Pirólise de pneus em fim de vida_ passando de um protótipo piloto para uma planta semi-industrial usando tecnologia Auger _ Energia e combustíveis

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<p></p><p>Informações</p><p></p><p>Métricas</p><p></p><p>Figuras</p><p></p><p>Ref.Resumo</p><p>Este trabalho, realizado no âmbito do</p><p>projeto BlackCycle, demonstra a</p><p>robustez de um reator de trado para a</p><p>pirólise de pneus em �m de vida (ELTs) a</p><p>ser considerado dentro do sétimo nível</p><p>de prontidão tecnológica (TRL-7). Para</p><p>este propósito, os produtos de pirólise</p><p>resultantes são comparados com</p><p>aqueles obtidos de uma instalação em</p><p>escala piloto variando dentro do quinto</p><p>nível de prontidão tecnológica (TRL-5).</p><p>Usando o mesmo tipo de ELTs,</p><p>caminhões de pneus (TTs), as condições</p><p>Energia e Combustíveis  Vol 38/Edição 17  Artigo</p><p>ENGENHARIA DE PROCESSOS | 23 de agosto de 2024</p><p>Pirólise de pneus em �m de vida: passando de um protótipo piloto</p><p>para uma planta semi-industrial usando tecnologia Auger</p><p> Clique para copiar o link do artigo</p><p>, , , , , , and</p><p></p><p>Citar</p><p></p><p>Compartilhar</p><p></p><p>Pular para</p><p></p><p>Colapso</p><p>Alberto Veses* Juan Daniel Martínez Alberto Sanchis José Manuel López Tomás García Gonzalo García Ramón Murillo</p><p> Abrir PDF</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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s.org/content/acs/en/privacy.html</p><p>http://www.acs.org/</p><p>https://pubs.acs.org/</p><p>https://cen.acs.org/</p><p>https://www.cas.org/</p><p>https://pubs.acs.org/action/ssoRequestForLoginPage</p><p>https://pubs.acs.org/</p><p>operacionais usadas na planta TRL-5 são tentadas para imitar aquelas esperadas em uma planta</p><p>semi-industrial: per�l de temperatura personalizado (450, 550 e 775 °C) e tempo de residência para</p><p>vapores (30 s) e sólidos (15 min). A taxa de massa de alimentação é de 4 e 400 kg/h para as plantas</p><p>piloto e semi-industrial, respectivamente. Os rendimentos de óleo de pirólise de pneu (TPO), gás de</p><p>pirólise de pneu (TPG) e negro de fumo bruto recuperado (RRCB) de ambas as plantas, bem como</p><p>suas principais propriedades e características, estão em bom acordo entre si. O TPO produzido por</p><p>ambas as plantas contém concentrações comparáveis de produtos químicos de valor agregado,</p><p>como benzeno, tolueno, xileno, etilbenzeno e limoneno. Há também um padrão muito semelhante</p><p>entre as curvas de destilação simuladas. O TPG obtido de ambas as plantas também é muito rico</p><p>em H e CH e tem um menor valor calorí�co de 52–54 MJ/Nm (base livre de N ). Embora os</p><p>RRCBs produzidos pelas duas plantas sejam mais exigentes e exijam mais mão de obra, eles têm</p><p>uma série de características comparáveis. Todas essas informações demonstram não apenas a</p><p>con�abilidade das campanhas experimentais para aumentar a escala do processo de pirólise, mas</p><p>também a robustez da planta em escala semi-industrial com base na tecnologia de trado a ser</p><p>classi�cada no TRL-7.</p><p>Esta publicação está licenciada sob</p><p>Copyright © 2024 Os autores. Publicado pela American Chemical Society</p><p>2 4</p><p>3</p><p>2</p><p> Edição Especial</p><p>Publicado como parte da edição especial da Energy & Fuels “2024 Pioneers in Energy Research: Robert</p><p>Brown”.</p><p>1. Introdução</p><p>Hoje, os pneus em �m de vida útil (ELTs) são vistos como uma grande fonte de produtos químicos de</p><p>valor agregado em vez de resíduos, o que supõe uma economia importante de matérias-primas e, ao</p><p>mesmo tempo, reduz a pegada ambiental.(1,2)Esses produtos valiosos podem ser extraídos por</p><p>pirólise para recuperar blocos de construção embutidos em pneus. Assim, a pirólise de ELTs produz</p><p>Assuntos</p><p>Compostos Aromáticos Biopolímeros Hidrocarbonetos Fabricação Pirólise</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/</p><p>https://pubs.acs.org/</p><p>https://cen.acs.org/</p><p>https://www.cas.org/</p><p>https://pubs.acs.org/action/ssoRequestForLoginPage</p><p>https://pubs.acs.org/</p><p>after this fractionation were later characterized for BTEX and limonene compounds according to the</p><p>procedures described above.</p><p>2.3.2. Raw Recovered Carbon Black</p><p>The RRCB was characterized by ultimate and proximate analyses and calori�c value determination</p><p>using the same procedures as indicated for the TTs. The volatile matter content is an important</p><p>indicator of the presence of carbonaceous deposits on the surface of the carbon particles as these</p><p>residues appear to promote the formation of hard agglomerates that severely degrade the quality of</p><p>the RRCB. Particular attention has therefore been paid to this parameter. The RRCB was also</p><p>characterized for BET surface area using a Micromeritics ASAP 2020 instrument according to ISO</p><p>9277 standard, with an instrument accuracy of 0.01 m /g. The BET surface area is calculated from</p><p>the physisorption of N up to a relative pressure of 0.3. The transmittance of the toluene extract was</p><p>also determined as it is one of the few analytical techniques for virgin CB that has been approved for</p><p>characterizing RRCB. It was determined in a PerkinElmer Lambda 25 UV/vis spectrophotometer</p><p>following the ASTM D1618-18 standard.</p><p>2.3.3. Tire Pyrolysis Gas</p><p>The permanent gases were analyzed on a Bruker 450 GC equipped with a TCD detector. Separation</p><p>was performed on two SS packed columns in series (Molsieve 13X, HayeSep Q). An initial oven</p><p>temperature of 60 °C was maintained for 10 min. The carrier gas was Ar at a column �ow rate of 30</p><p>mL /min. The detector temperature was set at 200 °C. Light hydrocarbons (C –C ) were quanti�ed in</p><p>a PerkinElmer Clarus 590 GC equipped with a �ame ionization detector (FID). Separation was</p><p>performed using a 30-m long and 0.32 mm wide alumina-chloride capillary column. Permanent gases</p><p>analyzed included hydrogen (H ), carbon dioxide (CO ), oxygen (O ), nitrogen (N ), and carbon</p><p>monoxide (CO), while light hydrocarbons included methane (CH ), ethane (C H ), ethylene (C H ),</p><p>propane (C H ), propylene (C H ), isobutane (C H ), n-butane (C H ), trans-2-butene (C H ), 1-</p><p>butene (C H ), isobutene (C H ), cis-2-butene (C H ), and 1,3-butadiene (C H ). Sulfur compounds</p><p>were analyzed on a PerkinElmer Clarus 590 GC equipped with an FPD detector. Separation was</p><p>performed using a 30 m Rt-Silica BOND capillary column. An initial oven temperature of 40 °C was</p><p>maintained for 2.5 min. A heating rate of 15 °C/min was then applied to reach a �nal oven</p><p>temperature of 180 °C. This temperature was maintained for 2 min. The carrier gas was He at a</p><p>constant column �ow rate of 2 mL /min. The injector and FPD temperatures were 250 and 300 °C,</p><p>respectively. Sulfur compounds analyzed included carbonyl sul�de (COS), hydrogen sul�de (H S),</p><p>2</p><p>2</p><p>N 1 4</p><p>2 2 2 2</p><p>4 2 6 2 4</p><p>3 8 3 6 4 10 4 10 4 8</p><p>4 8 4 8 4 8 4 6</p><p>N</p><p>2</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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disul�de (CS ), and methyl mercaptan (CH S). Certi�cated gas mixtures (Air Products) were</p><p>used for identi�cation and quanti�cation purposes.</p><p>3. Results and Discussion</p><p>3.1. Pyrolysis Conditions</p><p>Both plants were operated under very similar conditions in terms of the controlling variables involved</p><p>in auger pyrolyzers: temperature and residence time of solids and vapors in the reactor. (44−49) As</p><p>hot gas was used to heat the semi-industrial plant, a temperature pro�le was observed along the</p><p>reactor as the TTs are converted. On the other hand, the pilot plant was equipped with three</p><p>independent electrical resistances to provide the energy required for pyrolysis. A temperature pro�le</p><p>similar to that observed in the semi-industrial plant was therefore set. The temperatures observed for</p><p>both plants in the �rst, middle, and last sections of the reactor for both plants were 450, 550, and 775</p><p>°C, respectively, and the residence time of the rubber particles in the reactor was 15 min. Based on</p><p>previous tests carried out by our research group, this temperature pro�le had the added bene�t of</p><p>maximizing TPO production while ensuring a low volatile matter content in the RRCB. (38) The</p><p>temperature was measured using a series of thermocouples placed on the inner walls of the lower</p><p>part of the reactor. This allowed the temperature to be approximated by the temperature of the ELT</p><p>particles.</p><p>Figure 4 shows the measured temperature in both plants, which can be considered similar in both the</p><p>initial and �nal sections of the reactor. In addition, three steps can be distinguished. The �rst step</p><p>corresponds to the heating of the reactor. The temperature in the �rst section is set a few degrees</p><p>higher than expected (450 °C). Once the feedstock is introduced into the reactor and the pyrolysis</p><p>process takes place, this temperature decreases until the desired temperature is reached. This</p><p>process takes about 30–45 min in the TRL-5 plant and 12–14 h in the TRL-7 plant. The second step</p><p>begins after this period, when a steady state with no signi�cant temperature variations is reached in</p><p>both plants. The �nal and third steps are the temperature drop pro�le. This step takes place after 10</p><p>and 24 h of testing for the pilot plant and the semi-industrial plant, respectively; and means that no</p><p>more energy is being supplied, and the test can be considered complete.</p><p>Figure 4</p><p>2 4</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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://pubs.acs.org/</p><p>Figure 4. Temperature pro�le: a) pilot plant and b) semi-industrial plant.</p><p>On the other hand, the mass �ow rate of the feedstock is the main operating parameter governing the</p><p>residence time of the vapors in the auger reactor. (50) The geometry of the reactor can therefore be</p><p>sued to estimate the degree of �lling of the reactor and the residence time of the vapors released</p><p>during pyrolysis, once their density has been calculated. For this purpose, an internal Aspen Hysys</p><p>model was used to determine the speci�c volume occupied by the volatile fraction considering both</p><p>condensable and noncondensable hydrocarbons inside the reactor. Comparable vapor residence</p><p>times of about 30 s were found in both plants using mass �ow rates of 4 and 400 kg/h of ELTs in the</p><p>pilot and semi-industrial plants, respectively.</p><p>3.2. Yields</p><p>Under the above operating conditions, the resulting yields from the pilot and semi-industrial plants for</p><p>TPO, RRCB, and TPG were determined to be 43.7 ± 2.2 and 41.5 ± 4.3 wt %, 40.5 ± 2.1 and 41.5 ± 4.2</p><p>wt %, and 16.2 ± 0.8 and 17.6 ± 1.6 wt %, respectively (Figure 5). These values were calculated as the</p><p>average of 3 identical experiments. It is worth noting that the resulting yields from both plants are</p><p>quite similar and serve to demonstrate that the semi-industrial plant works properly in an operational</p><p>environment. These yields were those expected under intermediate pyrolysis conditions, i.e, when the</p><p>heating rate of the particles and the residence time of the vapors were around 100 °C/min and 30 s,</p><p>respectively. A notable advantage of intermediate pyrolysis is its ability to handle a wide variety of</p><p>feedstock (coarse, shredded, chopped, or �nely ground materials), providing versatility and �exibility</p><p>compared to other pyrolysis conditions. (51) Similar yields have been reported in other pyrolysis</p><p>systems using throughputs between 4 and 100 kg/h of ELTs such as rotary kilns (1,20) and auger</p><p>reactors. (3,35,38,44,52−55)</p><p>Figure 5</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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bs.acs.org/action/ssoRequestForLoginPage</p><p>https://pubs.acs.org/</p><p>Figure 5. Pyrolysis yields.</p><p>It is well-known that temperature is probably the key parameter in pyrolysis, as it plays a very</p><p>important role not only in the depolymerization of the ELTs but also in the occurrence of secondary</p><p>reactions, especially at high values. On the one hand, the low temperature in the pyrolysis of ELTs</p><p>results in some unconverted rubber being �xed in the RRCB, seriously affecting its quality and</p><p>marketability. At low temperatures, the</p><p>TPO composition is expected to be very rich in primary</p><p>pyrolysis compounds, such as limonene. In contrast, high temperatures generally favor the</p><p>separation of rubber from the carbonaceous solid matrix (depolymerization), and the RRCB is</p><p>expected to consist mainly composed of carbon derived from CBs. In addition, the TPG yield is</p><p>increased at the expense of the TPO yield, which is very rich in aromatic compounds due to the</p><p>promotion of secondary reactions. The temperature pro�ling technique used in this work takes</p><p>advantage of both low and high temperatures. This strategy minimizes vapor phase cracking</p><p>reactions in the �rst heating section of the reactor prior to volatile evacuation, while subjecting the</p><p>RRCB to high devolatilization severity in the �nal heating section.</p><p>3.3. Properties of the Tire Pyrolysis Oil</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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2 shows the main properties of the TPO obtained from the pilot and semi-industrial plants. As</p><p>observed, the results are very similar, and there does not seem to be a major effect on the size of the</p><p>plant. For both samples, the carbon and hydrogen contents show good agreement, while the sulfur</p><p>and nitrogen contents are slightly higher in the TPO from the semi-industrial plant. Nevertheless,</p><p>these concentrations are expected in TPO (4,5) and are due in part to the presence of sulfur- and</p><p>nitrogen-containing compounds such as thiophene, benzothiazole, benzothiophene, and</p><p>benzonaphthothiophene, as well as benzothiazole and benzonitrile, respectively. (26) Sulfur and</p><p>nitrogen compounds in the TPO are attributed to some additives used in the vulcanization and</p><p>formulation of tires. (56,57) Based on the above results, both TPOs can be considered as a mixture of</p><p>pure hydrocarbons and hydrocarbons combined with nitrogen and sulfur.</p><p>Table 2. TPO Characterization</p><p>element/property pilot plant semi-industrial plant</p><p>carbon (wt %) 88.7 ± 0.3 87.5 ± 0.3</p><p>hydrogen (wt %) 10.2 ± 0.3 11.3 ± 0.3</p><p>nitrogen (wt %) 1.4 ± 0.0 0.6 ± 0.0</p><p>sulfur (wt %) 0.76 ± 0.04 0.96 ± 0.04</p><p>H/C 1.4 ± 0.03 1.5 ± 0.04</p><p>HHV (MJ/kg) 42.3 ± 1.2 41.5 ± 1.2</p><p>density at 25 °C (kg/m ) 975.7 ± 60 960.0 ± 60</p><p>viscosity at 40 °C (mPa.s) 7.0 ± 0.5 5.6 ± 0.5</p><p>pH 6.9 ± 0.1 7.3 ± 0.1</p><p>TAN (mg KOH/g) 6.2 ± 0.5 5.4 ± 0.5</p><p>water (ppm) 253 ± 20 170 ± 20</p><p>3</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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stForLoginPage</p><p>https://pubs.acs.org/</p><p>As expected, the high carbon and hydrogen content gives TPO a remarkable HCV, comparable to</p><p>crude oil from petroleum (40–42 MJ/kg). It is also worth highlighting the renewable content</p><p>embedded in the TPO given the presence of natural rubber in the ELTs. TPO is therefore considered to</p><p>be both a waste-based and renewable hydrocarbon liquid feedstock. Density and viscosity are not</p><p>only very similar between the TPO produced in the two plants but also show interesting values when</p><p>compared with those of petroleum-based fuels. These similarities have led to the widespread use of</p><p>TPO as an alternative to various fuels in a variety of energy systems such as furnaces, (58) boilers,</p><p>(59) and even internal combustion engines. (60,61) In this sense, motivating results have been</p><p>reported despite the challenges associated with sulfur, nitrogen, �ash point, �nal distillation point,</p><p>and polycyclic aromatic hydrocarbons, among others. (26,62) Interest in the production of transport</p><p>fuels from TPO has also been on the rise, and the results are very encouraging and interesting.</p><p>(7,63,64)</p><p>However, the use of TPO for the production of chemical commodities appears to be gaining</p><p>tremendous traction in achieving a more circular and resource-e�cient economy, or in other words, a</p><p>higher degree of circularity. (7,9,23) In general, the characteristics shown in this work for the TPO,</p><p>both at the pilot and semi-industrial scale, are fully consistent with those found in the literature for</p><p>different plant scales. (1,3,20,35,38,65) These results therefore demonstrate the robustness of the</p><p>semi-industrial plant to be considered within the seventh technology readiness level (TRL-7). Other</p><p>properties shown in Table 2 also con�rm the representativeness of the TPO, such as pH, TAN, and</p><p>water content, which are practically the same regardless of plant size. Although TPO is transportable</p><p>and storable, these characteristics are prone to possible risks of corrosion, deposits, and handling,</p><p>among others. (65)</p><p>The boiling point distribution for TPO obtained in the two plants is also shown in Figure 6. It can be</p><p>seen that both samples have the same pro�le, although the TPO from the pilot plant seems to</p><p>contain slightly heavier compounds than that derived from the semi-industrial plant. The initial boiling</p><p>point (IPB), the temperature at which 50% of the TPO is distilled (T50), and the �nal boiling point</p><p>(FBP) are 60 and 70 °C, 290 and 300 °C, and 592 and 590 °C for the TPO produced in the pilot plant</p><p>and semi-industrial plant, respectively. These high �nal temperatures are related to the presence of</p><p>high molecular weight compounds such as polycyclic aromatic hydrocarbons (PAHs) and</p><p>heterocyclic compounds, as shown elsewhere. (7,26) Figure 6 also shows that both TPOs contain a</p><p>signi�cant amount of gasoline-like, kerosene-like, and diesel-like compounds, as the cuts of these</p><p>streams are within their boiling point range. (66) It is worth noting that these data, especially those</p><p>from the semi-industrial plant, are useful as a database for further simulation and design of re�nery</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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under industrially relevant conditions with the aim of integrating the TPO into the petrochemical</p><p>industry.</p><p>Figure 6</p><p>Figure 6. Boiling point distribution of TPO.</p><p>The concentrations of BTEX + styrene and limonene of the two TPOs are listed in Table 3. The</p><p>presence of these compounds is directly related to the amount of styrene–butadiene rubber (SBR)</p><p>and natural rubber (NR) in the ELTs, respectively. (6,26,67) It is interesting to note that NR is higher in</p><p>tires from heavy vehicles (27–30 wt %) than from light vehicles (15–22 wt %). (68,69) The opposite</p><p>applies to the composition of SBR. The concentration of these compounds is therefore highly</p><p>dependent on the source of the ELTs. The composition of TPO is also directly related to the reaction</p><p>temperature, as discussed above. In general, limonene production is maximized at low temperatures</p><p>(425–450 °C), whereas single-ring aromatics are maximized at higher temperatures as they are</p><p>favored by the occurrence of secondary cracking and aromatization reactions. As shown in Table 3,</p><p>some minor differences can be observed between the two TPOs with regard to the concentration of</p><p>the above-mentioned compounds. In this sense, BTEX and limonene account for 12.14 and 3.66 wt %</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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9.37 and 4.55 wt % of the TPO produced in the pilot and semi-industrial plants, respectively.</p><p>These results show once again the advantages of the temperature pro�le, in particular the low value</p><p>in the �rst section of the reactor, which prevents the severe cracking of the vapors before they are</p><p>condensed and collected.</p><p>Table 3. Composition of TPO, LF, and HF Fractions</p><p>pilot plant semi-industrial p</p><p>compound (wt%) TPO light fraction (LF) heavy fraction (HF) TPO lig</p><p>benzene 2.53 ± 0.03 6.15 ± 0.06 0.00 ± 0 1.54 ± 0.03 4</p><p>toluene 4.64 ± 0.04 9.85 ± 0.1 0.02 ± 0 3.69 ± 0.04 9</p><p>ethylbenzene 0.47 ± 0.01 1.08 ± 0.03 0.03 ± 0 0.56 ± 0.01 1</p><p>(p+m)-xylene 3.85 ± 0.1 7.08 ± 0.14 0.16 ± 0 3.13 ± 0.03 7</p><p>o-xylene 0.65 ± 0.04 2.04 ± 0.14 0.02 ± 0 0.45 ± 0.02 1</p><p>total BTEX 12.14 ± 0.2 26.20 ± 0.5 0.23 ± 0 9.37 ± 0.15 2</p><p>styrene 1.27 ± 0.05 1.00 ± 0.03 0.04 ± 0 0.55 ± 0.05 1</p><p>limonene 3.66 ± 0.07 10.72 ± 0.2 1.72 ± 0.03 4.55 ± 0.09 8</p><p>Table 3 also shows the concentration of BTEX + styrene and limonene for the light and heavy</p><p>fractions after fractionation at 235 °C of the TPO samples. Fractionation of organic liquid mixtures by</p><p>distillation is considered to be a simple strategy to carry out the initial rough separation of crude oils</p><p>in such a way that compounds with similar volatility are grouped together. It can be seen that the</p><p>BTEX concentration of the light fraction was more than doubled for both TPOs after fractional</p><p>distillation, while in the heavy fraction it was less than 0.4 wt %. The limonene concentration in the</p><p>light fraction was also very high for the two TPOs (10.72 and 8.08 wt %, respectively). The light</p><p>fraction yield at 235 °C was 27% and 31% for the TPOs produced at the pilot and semi-industrial scale</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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respectively. The</p><p>recovery of BTEX and limonene plays a key role in the development of ELTs</p><p>pyrolysis and its integration into the petrochemical industry as these compounds are widely used in</p><p>the production of various industrial and valuable products. Together with ole�ns (ethylene and</p><p>propylene), BTEX are part of the high-value chemicals (HVCs), important building blocks for the</p><p>production of plastics, resins, adhesives, cosmetics, inks, paints, pharmaceuticals, rubbers, and</p><p>thinners, among others. (7,57) Limonene also has important and diverse industrial applications.</p><p>These include the production of resins and various oxygenated derivatives.</p><p>The continuous fractionation process by atmospheric distillation of TPO has recently been</p><p>demonstrated by our research group under industrially relevant conditions with very promising</p><p>results. (7) In that work, the BTEX concentration in the overhead product was greater than 55 wt %,</p><p>paving the way for defossilization in the chemical and petrochemical sector. Details of how the pilot</p><p>distillation column for TPO was designed and operated are also given elsewhere. (8) The distillation</p><p>unit described in both works was tested and validated with TPO produced from the pilot and semi-</p><p>industrial scale plants. These papers demonstrate the technical feasibility of fractionating TPO using</p><p>an industrially relevant packed distillation column and provide valuable insights into the integration of</p><p>pyrolysis and distillation technologies. The results reported in those papers are expected to make a</p><p>signi�cant contribution to the circular economy by effectively combining these technologies to</p><p>process complex waste-based hydrocarbons, such as TPO.</p><p>3.4. Composition of Tire Pyrolysis Gas</p><p>The volumetric composition of the TPG (on an N -free basis) is summarized in Table 4. As can be</p><p>seen, both plants have very similar compositions and are particularly rich in hydrocarbons (C H )</p><p>accounting for approximately 64 and 72 vol % for the pilot and semi-industrial plants, respectively.</p><p>The most abundant C H is methane (C ) (32–34 vol %), followed by hydrogen (24–29 vol %), which</p><p>makes up more than half of the TPG. Ethane and ethylene (C ), propane and propylene (C ), n-butane</p><p>and butadiene compounds (C ), and higher molecular weight C H (>C ) are also found, with fairly</p><p>similar concentrations between the two plants. Carbon monoxide as well as sulfur compounds (COS</p><p>+ H S + CS + CH S) are also observed. The latter are the main contributors to the unpleasant odor,</p><p>as well as potential vectors of corrosivity and toxicity.</p><p>Table 4. TPG Composition in a Free N Basis</p><p>2</p><p>x y</p><p>x y 1</p><p>2 3</p><p>4 x y 4</p><p>2 2 4</p><p>2Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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stForLoginPage</p><p>https://pubs.acs.org/</p><p>gas (vol %) pilot plant semi-industrial plant</p><p>H 29.9 ± 0.6 24.1 ± 0.5</p><p>CH 32.6 ± 2.3 34.5 ± 2.5</p><p>COx 4.6 ± 0.1 3.1 ± 0.1</p><p>C 10.5 ± 0.9 13.3 ± 0.9</p><p>C 3.9 ± 0.2 6.6 ± 0.4</p><p>C 10.6 ± 0.9 9.0 ± 0.7</p><p>>C 6.7 ± 1.3 8.9 ± 1.8</p><p>COS 0.03 ± 0 0.02 ± 0</p><p>H S 1.2 ± 0.4 0.5 ± 0.2</p><p>CS 0.0 ± 0 0.0 ± 0</p><p>CH S 0.06 ± 0.01 0.02 ± 0</p><p>LCV (MJ/Nm ) 54.2 ± 2.5 52.2 ± 2.5</p><p>Therefore, gas scrubbers should be installed in large plants to prevent damage to equipment and</p><p>pipelines and to meet strict environmental regulations. In fact, the semi-industrial plant includes a</p><p>desulfurization system consisting of a scrubber with an NaOH solution that converts</p><p>the sulfur-</p><p>containing gases into soluble sodium salts. The scrubber achieves about 90% H S removal e�ciency</p><p>using a 50% H O/NaOH mixture. This solution is continuously recirculated until the pH falls below a</p><p>speci�ed level. When this occurs, the liquid in the scrubber is purged and fresh solution is introduced</p><p>to bring the pH back to the desired range.</p><p>Table 4 also includes the lower calori�c value (LCV) of both TPGs (52–54 MJ/Nm ), which shows the</p><p>great potential not only to meet the energy needs of pyrolysis but also to generate electricity and/or</p><p>2</p><p>4</p><p>2</p><p>3</p><p>4</p><p>4</p><p>2</p><p>2</p><p>4</p><p>3</p><p>2</p><p>2</p><p>3</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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as reported elsewhere. (3,70) It should be noted once again that the TPG produced in the</p><p>semi-industrial plant is used as a fuel in an industrial burner in order to self-sustain the pyrolysis</p><p>process by means of the resulting �ue gases; in fact, around 70% of the TPG produced is used for</p><p>this purpose. This is achieved by supplying a constant amount of air that is supplied to the burner, as</p><p>the blower operates under consistent conditions. A control valve regulates the TPG supply to the</p><p>burner, allowing the system to automatically adjust the valve opening and the amount of TPG</p><p>supplied once the temperature is set. As a result, the TPG cleaning system worked e�ciently and</p><p>avoided the risks associated with corrosion during operation. The semi-industrial plant also</p><p>represents an excellent example of energy integration and therefore energy e�ciency, as the energy</p><p>required by the process, namely the energy for pyrolysis, is supplied by the TPG. Future integration</p><p>with re�nery and petrochemical units such as distillation can also bring signi�cant bene�ts by</p><p>replacing part of the operation with TPG.</p><p>3.5. Properties of the Raw Recovered Carbon Black</p><p>It is well-known that RRCB contains different grades of CB and is therefore considered to be a</p><p>complex mixture of many and heterogeneous carbon particles. It also includes inorganic elements</p><p>and exogenous carbonaceous deposits. (10,71,72) The recovery and use of RRCB is particularly</p><p>important not only because of the huge and growing CB market, (73) but also because of the carbon</p><p>footprint associated with its production (2.4 kg CO /kgCB). (31) The RRCB therefore has particular</p><p>interest in the achievement of a sustainable and circular economy. Table 5 summarizes some of the</p><p>characteristics of the RRCBs produced in the pilot and semi-industrial plants. It can be seen that</p><p>comparable values were found, which once again con�rms the robustness of the semi-industrial</p><p>scale plant.</p><p>Table 5. RRCB Characterization</p><p>analysis pilot plant semi-industrial plant</p><p>Proximate, dry basis (wt %)</p><p>ash (wt %) 14.7 ± 1.5 16.6 ± 1.7</p><p>volatile matter (wt %) 1.6 ± 0.1 4.6 ± 0.4</p><p>�xed carbon (wt %) 83.8 ± 0.4 76.4 ± 0.4</p><p>2</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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pilot plant semi-industrial plant</p><p>Ultimate, dry basis (wt %)</p><p>carbon 84.5 ± 0.4 80.1 ± 0.4</p><p>hydrogen 0.4 ± 0.0 1.7 ± 0.1</p><p>nitrogen 0.3 ± 0.0 0.4 ± 0.0</p><p>sulfur 2.8 ± 0.3 3.3 ± 0.3</p><p>Calori�c value</p><p>HCV (MJ/kg) 29.6 ± 1.0 27.8 ± 1.0</p><p>Others</p><p>S (m /g) 54.0 ± 0.3 56.9 ± 0.3</p><p>transmittance of toluene extract (%) 40.5 ± 1.2 0.12 ± 0.01</p><p>However, there is a noticeable difference between the volatile matter levels (1.6 wt % for the pilot</p><p>plant and 4.6 wt % for the semi-industrial plant). Volatile matter is generally associated with the</p><p>presence of carbonaceous deposits in the RRCB coming from nondevolatilized rubber and/or</p><p>condensed hydrocarbon compounds in the surface. The transmittance of the toluene extract</p><p>obtained by the ASTM D1618 method is a representative indicator of the presence of these</p><p>carbonaceous deposits on the RRCB, or, in other words, of the organic impurity content. In this case,</p><p>the transmittance of the toluene extract was lower for the solid obtained in the semi-industrial plant</p><p>(0.1%) than that for the solid obtained in the pilot plant (40%), as expected due to the higher volatile</p><p>content of the sample. It is desirable to keep the volatile matter as low as possible to improve the</p><p>quality of the RRCB. However, in industrial-scale plants, adequate control of the reactor to prevent the</p><p>occurrence of this volatile matter in the RRCB is more complex than that in laboratory and pilot scale</p><p>plants. This challenge could be overcome by intensive milling, as the volatile matter tends to both</p><p>break and separate from the CB matrix when ground into powder, resulting in dust-free, free-�owing</p><p>BET</p><p>2</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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de pirólise de pneus (TPO) e gás de pirólise de pneus (TPG), que vêm de borracha natural e</p><p>sintética contida em pneus. Além disso, uma fração carbonácea sólida é obtida, que inclui os negros</p><p>de fumo (CBs) usados na fabricação de pneus. De acordo com a norma ASTM D8178, este produto</p><p>deve ser denominado negro de fumo recuperado bruto (RRCB). Uma vez que o RRCB tenha sido</p><p>intensamente moído e tanto o aço quanto os tecidos tenham sido removidos, ele deve ser denotado</p><p>como negro de fumo recuperado (rCB). Como o TPG (15–30% em peso) é usado principalmente para</p><p>fornecer os requisitos de energia do processo,(3)produtos comercializáveis da pirólise de ELTs são</p><p>TPO (35–45% em peso) e RRCB (35–45% em peso). TPO representa um pool químico não apenas</p><p>para a recuperação de compostos valiosos, como aromáticos de anel único e limoneno(4−7)mas</p><p>também como matéria-prima na indústria de CB.(8)Em geral, essa mistura complexa de</p><p>hidrocarbonetos aromáticos, alifáticos, polares e heteroatômicos parece ser muito atraente como</p><p>substituição de diversas fontes fósseis em unidades de re�naria.(9)Espera-se que o RRCB</p><p>desempenhe um papel muito interessante na substituição do CB virgem como agente de reforço em</p><p>vários produtos poliméricos, bem como em outras aplicações relacionadas a catalisadores e</p><p>carvões projetados como carvão ativado.(10,11−13)</p><p>A pirólise é um processo antigo usado há séculos para carbonizar madeira e sintetizar carvão</p><p>vegetal.(14)Os primeiros desenvolvimentos usando ELTs como matéria-prima datam da década de</p><p>70, com a primeira crise do petróleo.(15)Desde então, a pirólise de ELTs tem sido estudada em todo</p><p>o mundo há anos, com atenção especial à in�uência das variáveis reguladoras tanto no rendimento</p><p>quanto nas propriedades dos produtos resultantes usando instalações em escala laboratorial.(4,16)</p><p>Na escala piloto, estudos limitados são encontrados na literatura.(1,3,17−19,21,22)Além disso, as</p><p>informações em escala industrial são praticamente inexistentes, e os dados disponíveis são</p><p>encontrados apenas nos sites dos provedores de tecnologia. Dados técnicos sobre a pirólise de ELTs</p><p>em escala industrial são certamente escassos na literatura, considerando que mais de 50 anos de</p><p>pesquisa intensiva se passaram desde os primeiros relatórios. Essas lacunas de informação são</p><p>frequentemente chamadas de “vale da morte”, que é dividido em técnico e comercial ( Figura 1 ). O</p><p>Grupo de Pesquisa Ambiental do Instituto de Carboquímica (ICB-CSIC) trabalha há anos na transição</p><p>entre instalações em escala laboratorial e plantas piloto de processos termoquímicos para a</p><p>valorização e reciclagem de diferentes tipos de resíduos. Essa experiência também pode ser vista</p><p>como uma ponte sobre o “vale da morte” técnico entre os níveis de prontidão tecnológica (TRLs) dos</p><p>primeiros: de 1 a 3, para 4–5. Com este pano de fundo, e em estreita</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/</p><p>https://pubs.acs.org/</p><p>https://cen.acs.org/</p><p>https://www.cas.org/</p><p>https://pubs.acs.org/action/ssoRequestForLoginPage</p><p>https://pubs.acs.org/</p><p>rCB granules. This reduces the size of the fused agglomerates, and the interactions between the CB</p><p>particles are reduced, ultimately improving the quality of the material, such as dispersibility when</p><p>used in rubber formulations.</p><p>Based on the above results, the ASTM D8178 standard distinguishes between RRCB and rCB, as</p><p>mentioned in Section 1, in order to differentiate between those with low and high reinforcing</p><p>properties, respectively. In addition, the mechanical grinding of RRCB is expected to form chemical</p><p>bonds that provide new oxygenated functional groups whose nature and relative quantity can change</p><p>depending on the reaction time, as reported elsewhere. (74) The presence of these functional groups</p><p>after milling is expected to increase the surface activity of the rCB; resulting in stronger bonds are</p><p>formed when used, for example, in polymer formulations. (71) The milling step, as well as</p><p>palletization to improve handling and shipping, have been used by industrial companies involved in</p><p>the pyrolysis of ELTs in order to provide rCBs with a comparable performance to N300, N500, N600,</p><p>and N700 CB grades. (75) The BET surface area of the RRCB produced in both plants was similar to</p><p>values of 54 and 57 m /g. These values are in the range of the commercial CB. The versatility of the</p><p>auger reactor con�guration is highlighted with regard to the use of different potential temperature</p><p>pro�les, in particular the high temperature in the tail section of the reactor as a strategy to minimize</p><p>the presence of exogenous carbon deposits in the RRCB. Although this plan is currently being</p><p>con�rmed by the accumulation of hours in the semi-industrial plant, the results obtained so far</p><p>con�rm the potential of this strategy to maximize the bene�ts of all the products obtained.</p><p>3.6. Scale-Up Analysis and Product Consistency in Tire Pyrolysis</p><p>This section deals with the scaling up of the pyrolysis process from pilot to semi-industrial scale,</p><p>with a focus on the consistency of yields and characteristics across different particle sizes.</p><p>Con�rmation of scale-up: the observed consistency in product composition indicates</p><p>successful scale-up of the pyrolysis process from laboratory to semi-industrial scale. This</p><p>suggests that the operating parameters, such as temperature pro�les and residence times, are</p><p>su�ciently robust to accommodate variations in particle size without signi�cantly altering the</p><p>�nal product composition.</p><p>Mass and energy transfer: in an auger reactor, e�cient mass and energy transfer can be</p><p>achieved due to the inherent mechanical forces that enhance particle mixing. This helps to</p><p>maintain uniform temperature distribution and consistent reaction conditions throughout the</p><p>reactor. The continuous movement of the particles, regardless of their size, exposed them to a</p><p>constant thermal environment, resulting in successful pyrolysis reactions.</p><p>2</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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thermal conductivity of the feedstock in the reactor plays a crucial role in ensuring uniform</p><p>heat distribution. Although larger particles may take longer to heat up, the overall heat transfer</p><p>mechanisms in the auger reactor are satisfactorily controlled by the feed mass rate to ensure</p><p>that both the interior and surface of the particles reach the temperatures required for pyrolysis.</p><p>Residence time: optimizing residence time for both vapors and solids is critical for effective</p><p>pyrolysis. In this work, the residence time of the vapors was optimized to avoid the occurrence</p><p>of secondary reactions, which was ultimately controlled by the feed mass rate. Auger reactors</p><p>have the advantage that the residence time of the solids can be easily controlled by varying the</p><p>rotation speed, ensuring complete pyrolysis of both small and large particles. The auger reactor</p><p>design facilitates uniform residence time distribution, which contributes to the observed</p><p>similarity in product yields.</p><p>Thus, the scale-up process maintained the integrity of the pyrolysis reaction across different particle</p><p>sizes, con�rming the robustness and e�ciency of the process. In addition, it is important to consider</p><p>other types of technologies available at an industrial level in order to provide a more realistic view of</p><p>the processes being carried out. In the context of pyrolysis of ELTs, �xed bed reactors, particularly</p><p>moving bed technology and rotary kiln reactors, are the most commonly used and accessible</p><p>options. When these results are compared with other industrial plants, several observations can be</p><p>made. Pyrum Innovations AG using a moving bed technology at TRL-9 (5000 ton/y for reactor)</p><p>produces 31, 44, and 25 wt % of TPO, RRCB and TPG, respectively (76) This indicates a slightly lower</p><p>TPO yield but a higher RRCB yield compared to the auger technology described in this work. These</p><p>differences can be directly related to the reactor design and operating conditions as the volatile</p><p>residence time is much higher with moving bed technology.</p><p>On the other hand, studies relating to rotary kiln technology (17) report yields of 15 ± 3 wt % TPG, 40</p><p>± 4 wt % TPO, and 45 ± 4 wt % RRCB at approximately 450 °C using mixtures of different types of ELTs</p><p>with a particle sizes in the range of 5–20 mm. These results are in close agreement with our �ndings,</p><p>particularly in TPO and TPG, although the RRCB yield is slightly higher in the rotary kiln. Another</p><p>relevant study (1) describes a semi-industrial prototype (TRL-7) operating at 550 °C using 50 to 300</p><p>mm particles, achieving yields of 14.5 ± 2 wt % TPG, 37.5 ± 1 wt % TPO, and 48.0 ± 2 wt % RRCB. That</p><p>prototype, like the auger reactor, operates at a similar TRL level and has comparable yields in the TPO</p><p>and TPG but again has a higher RRCB.</p><p>The consistent yields across these different reactor types: moving bed, rotary kiln, and auger, suggest</p><p>robustness in the operating parameters such as temperature pro�les and residence times. The</p><p>variation in RRCB and TPO yields can be attributed to differences in reactor design and the e�ciency</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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mass and energy transfer mechanisms. In particular, the continuous mixing and movement of the</p><p>auger reactor facilitate uniform thermal conditions, which may contribute to its distinctive yield</p><p>distribution. These �ndings underline the effectiveness of our TRL-7 auger reactor in the wider</p><p>context of industrial pyrolysis technologies.</p><p>3.7. Technical Issues and Concerns</p><p>Details of different reactor designs for the pyrolysis of ELTs, including operating principles, and even</p><p>throughputs are found elsewhere. (77) Accordingly, �xed beds and rotary kilns are currently the most</p><p>widely used technologies worldwide, and both are found on an industrial scale with several suppliers.</p><p>(5) However, the auger pyrolyzer detailed in this work clari�es the exogenous risks associated with</p><p>scale and provides key information to consider this technology as reliable, being possible included</p><p>among the different options for pyrolysis of ELTs on an industrial scale. Although the semi-industrial</p><p>plant has been demonstrated to be capable of working �awlessly and according to the expected</p><p>pattern based on the pilot plant (TRL-5), some concerns and issues are raised in order to move</p><p>forward a higher level of technological maturity.</p><p>During process control, special attention should be focused on pressure, especially at the vapor</p><p>outlet. No variations in this parameter is an essential indicator that the pyrolysis process is</p><p>being carried out correctly. The ducts that evacuate the gaseous fraction can be a key factor in</p><p>ensuring long-term operation, and special attention must be paid to during maintenance,</p><p>cleaning and overhaul work.</p><p>It is highly recommended that the ELTs particles are free of steel and textile contamination in</p><p>order to avoid clogging and ensure the correct operation.</p><p>The presence of corrosive agents such as sulfur-containing compounds in both TPO and TPG</p><p>makes mandatory the use of stainless steel in pipelines and other mechanical elements of the</p><p>plant which could be in direct contact with these compounds.</p><p>The presence of different thermocouples and pressure sensors along the reactor certainly</p><p>provides more information about what is happening during the process, making control</p><p>procedures and decisions more e�cient and timely.</p><p>4. Conclusions</p><p>This work shows a detailed comparison of the yields and characteristics of the resulting products</p><p>derived from pyrolysis of end-of-life tires between a pilot prototype (4 kg/h) and a semi-industrial</p><p>plant (400 kg/h) both using the auger technology. The pilot prototype, ranked within the �fth</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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readiness level (TRL-5), has been operated and revamped over time for the Environmental</p><p>Research Group of the Instituto de Carboqumica (ICB-CSIC) and has served to provide key data for</p><p>setting technical speci�cations of the semi-industrial plant. In this sense, the yields and properties of</p><p>tire pyrolysis oil, tire pyrolysis gas, and raw recovered carbon black are notoriously similar between</p><p>the two plants. These resemblances support the reliability and robustness of the semi-industrial</p><p>plant to be considered within the seventh level of technology readiness (TRL-7).</p><p>Author Information</p><p>Corresponding Author</p><p>Alberto Veses - Instituto de Carboquímica (ICB-CSIC), C/Miguel Luesma Castán 4, Zaragoza</p><p>50018, Spain;  https://orcid.org/0000-0002-7589-2643; Email: a.veses@icb.csic.es</p><p>Authors</p><p>Juan Daniel Martínez - Instituto de Carboquímica (ICB-CSIC), C/Miguel Luesma Castán 4,</p><p>Zaragoza 50018, Spain;  https://orcid.org/0000-0001-5075-5135</p><p>Alberto Sanchís - Instituto de Carboquímica (ICB-CSIC), C/Miguel Luesma Castán 4, Zaragoza</p><p>50018, Spain</p><p>José Manuel López - Instituto de Carboquímica (ICB-CSIC), C/Miguel Luesma Castán 4,</p><p>Zaragoza 50018, Spain</p><p>Tomás García - Instituto de Carboquímica (ICB-CSIC), C/Miguel Luesma Castán 4, Zaragoza</p><p>50018, Spain</p><p>Gonzalo García - Greenval Technologies S.L, C/Ayala 10, Madrid 28001, Spain</p><p>Ramón Murillo - Instituto de Carboquímica (ICB-CSIC), C/Miguel Luesma Castán 4, Zaragoza</p><p>50018, Spain;  https://orcid.org/0000-0002-0299-506X</p><p>Notes</p><p>The authors declare no competing �nancial interest.</p><p>Acknowledgments</p><p>Este site usa cookies para melhorar sua experiência de usuário. 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work is part of the BLACKCYCLE project (For the circular economy of tire domain: recycling end</p><p>of life tires into secondary raw materials or tires and other product applications) which has received</p><p>funding from the European Union’s Horizon 2020 research and innovation programme under grant</p><p>agreement No 869625. The authors would also like to thank the Regional Government of Aragon</p><p>(DGA) for the support provided under the research groups support programme and CSIC for the</p><p>interdisciplinary thematic platforms SusPlast and</p><p>SosEcoCir. The authors also thank the teams of</p><p>Greenval and Sisener Ingenieros for their collaboration in the experimental campaign at the TRL-7</p><p>plant.</p><p>Symbols</p><p>symbol meaning</p><p>BTEX benzene, toluene, ethyl-benzene, xylenes</p><p>CB carbon black</p><p>CO carbon dioxide</p><p>CH methane</p><p>CH S methyl mercaptan</p><p>CO carbon oxides (e.g., CO, CO )</p><p>C2, C3, C4 hydrocarbons with two, three, and four carbon atoms</p><p>>C4 higher C hydrocarbons</p><p>COS carbonyl sul�de</p><p>2</p><p>4</p><p>4</p><p>x 2</p><p>4</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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carbon disul�de</p><p>CSIC Spanish Council for Scienti�c Research</p><p>ELTs end-of-life tires</p><p>FBP �nal boiling point</p><p>FCC �uid catalytic cracking</p><p>FID �ame ionization detector</p><p>GC gas chromatograph</p><p>H hydrogen</p><p>H S hydrogen sul�de</p><p>H-1, 2, 3 hopper 1, 2, 3</p><p>HF heavy Fraction</p><p>HHV higher heating value</p><p>IPB initial boiling point</p><p>LF light fraction</p><p>2</p><p>2</p><p>2</p><p>Este site usa cookies para melhorar sua experiência de usuário. 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temperature (typically in degrees Celsius)</p><p>TAN total acid number</p><p>TCD thermal conductivity detector</p><p>TIC temperature indicator controller</p><p>TPG tire pyrolysis gas</p><p>TPO tire pyrolysis oil</p><p>TRLs technology readiness levels</p><p>TTs truck tires</p><p>References</p><p>This article references 77 other publications.</p><p>1. 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On Fractioning the Tire Pyrolysis Oil in a</p><p>Pilot-Scale Distillation Plant under Industrially Relevant Conditions. Energy Fuels 2023, 37, 2886– 2896,</p><p>DOI: 10.1021/acs.energyfuels.2c03850</p><p>8. Daniel Martínez, J.; Sanchís, A.; Veses, A.; Soledad Callén, M.; Manuel López, J.; García, T.; Murillo, R. Design and</p><p>operation of a packed pilot scale distillation column for tire pyrolysis oil: Towards the recovery of value-added raw</p><p>materials. Fuel 2024, 358, 130266,  DOI: 10.1016/j.fuel.2023.130266</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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Martínez, J. D. An overview of the end-of-life tires status in some Latin American countries: Proposing pyrolysis</p><p>for a circular economy. Renewable Sustainable Energy Rev. 2021, 144, 111032,  DOI: 10.1016/j.rser.2021.111032</p><p>16. Arabiourrutia, M.; Lopez, G.; Artetxe, M.; Alvarez, J.; Bilbao, J.; Olazar, M. Waste tyre valorization by catalytic</p><p>pyrolysis – A review. Renewable Sustainable Energy Rev. 2020, 129, 109932,  DOI: 10.1016/j.rser.2020.109932</p><p>17. Xu, J.; Yu, J.; He, W.; Huang, J.; Xu, J.; Li, G. Recovery of carbon black from waste tire in continuous commercial</p><p>rotary kiln pyrolysis reactor. Sci. Total Environ. 2021, 772, 145507,  DOI: 10.1016/j.scitotenv.2021.145507</p><p>18. Roy, C.; Chaala, A.; Darmstadt, H. The vacuum pyrolysis of used tires: End-uses for oil and carbon black</p><p>products. J. Anal. Appl. Pyrolysis 1999, 51, 201– 221,  DOI: 10.1016/S0165-2370(99)00017-0</p><p>19. Oliveira Neto, G. C.; Chaves, L. E.; Pinto, L. F.; Santana, J. C.; Amorim, M. P.; Rodrigues, M. J. Economic,</p><p>Environmental and Social Bene�ts of Adoption of Pyrolysis Process of Tires: A Feasible and Ecofriendly Mode to</p><p>Reduce the Impacts of Scrap Tires in Brazil. Sustainability 2019, 11, 2076,  DOI: 10.3390/su11072076</p><p>20. Li, S. Q.; Yao, Q.; Chi, Y.; Yan, J. H.; Cen, K. F. Pilot-Scale Pyrolysis of Scrap Tires in a Continuous Rotary Kiln</p><p>Reactor. Ind. Eng. Chem. Res. 2004, 43, 5133– 5145,  DOI: 10.1021/ie030115m</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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1</p><p>Figura 1. Esquema geral dos conceitos do TRL.</p><p>Re�narias ao redor do mundo estão cada vez mais interessadas em matéria-prima alternativa ao</p><p>petróleo bruto, principalmente de resíduos. O objetivo �nal é substituir alguns de seus insumos e,</p><p>assim, contribuir até certo ponto para a desfossilização do setor químico, permitindo a transição de</p><p>uma economia de carbono linear para uma circular.(23−25)Neste sentido, estudos que mostram o</p><p>potencial de utilização do TPO em unidades-chave de re�no, como a destilação,(7,8,26)</p><p>craqueamento catalítico �uido (FCC),(23,27)e hidrotratamento,(28,29)entre outros, estão se tornando</p><p>mais comuns. Os resultados obtidos neste campo são muito encorajadores com relação à</p><p>possibilidade de misturar TPO em baixas concentrações com �uxos de petróleo bruto convencionais</p><p>para produzir produtos derivados de alta qualidade sem alterar as condições operacionais</p><p>necessárias.(9)No entanto, essas unidades de re�naria operam com rendimentos muito altos, então</p><p>as quantidades de TPO também precisam ser signi�cativas para demonstrar a viabilidade dessas</p><p>rotas. Portanto, o desenvolvimento de plantas de pirólise semi-industriais, seguindo os diferentes</p><p>estágios dos TRLs com base na experiência adquirida em pesquisa e desenvolvimento (P&D), ou</p><p>seja, em protótipos em escala piloto extensivamente estudados, é considerado um passo essencial</p><p>para garantir uma economia verdadeiramente circular para ELTs.</p><p>Da mesma forma, o RRCB está atraindo considerável atenção como substituto do CB virgem em</p><p>diversas formulações de borracha.(10,30)Como agente de reforço, mais de 90% da produção</p><p>mundial de CB é usada na fabricação de borracha, principalmente pneus.(31)Assim, a recuperação</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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y.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/content/acs/en/privacy.html</p><p>http://www.acs.org/</p><p>https://pubs.acs.org/</p><p>https://cen.acs.org/</p><p>https://www.cas.org/</p><p>https://pubs.acs.org/action/ssoRequestForLoginPage</p><p>https://pubs.acs.org/</p><p>21. 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Ca-based Catalysts for the</p><p>Production of High-Quality Bio-Oils from the Catalytic Co-Pyrolysis of Grape Seeds and Waste Tyres. Catalysts</p><p>2019, 9, 992,  DOI: 10.3390/catal9120992</p><p>42. Veses, A.; Aznar, M.; Martínez, I.; Martínez, J. D.; López, J. M.; Navarro, M. V.; Callén, M. S.; Murillo, R.; García, T.</p><p>Catalytic pyrolysis of wood biomass in an auger reactor using calcium-based catalysts. Bioresour. Technol. 2014,</p><p>162, 250– 258,  DOI: 10.1016/j.biortech.2014.03.146</p><p>43. Veses, A.; Aznar, M.; López, J. M.; Callén, M. S.; Murillo, R.; García, T. Production of upgraded bio-oils by</p><p>biomass catalytic pyrolysis in an auger reactor using low cost materials. Fuel 2015, 141, 17– 22,</p><p>DOI: 10.1016/j.fuel.2014.10.044</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>Este site usa cookies para melhorar sua experiência de usuário. 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Martínez, J. D.; Ramos, Á.; Armas, O.; Murillo, R.; García, T. Potential for using a tire pyrolysis liquid-diesel fuel</p><p>blend in a light duty engine under transient operation. Appl. Energy 2014, 130, 437– 446,</p><p>DOI: 10.1016/j.apenergy.2014.05.056</p><p>62. Lopez, G.; Alvarez, J.; Amutio, M.; Mkhize, N. M.; Danon, B.; van der Gryp, P.; Görgens, J. F.; Bilbao, J.; Olazar, M.</p><p>Waste truck-tyre processing by �ash pyrolysis in a conical spouted bed reactor. Energy Convers. Manage. 2017,</p><p>142, 523– 532,  DOI: 10.1016/j.enconman.2017.03.051</p><p>63. Straka, P.; Auersvald, M.; Vrtiška, D.; Kittel, H.; Šimáček, P.; Vozka, P. Production of transportation fuels via</p><p>hydrotreating of scrap tires pyrolysis oil. Chem. Eng. J. 2023, 460, 141764,  DOI: 10.1016/j.cej.2023.141764</p><p>64. Ayanŏlu, A.; Yumruta̧, R. Rotary kiln and batch pyrolysis of waste tire to produce gasoline and diesel like fuels.</p><p>Energy Convers. Manage. 2016, 111, 261– 270,  DOI: 10.1016/j.enconman.2015.12.070</p><p>65. Martínez, J. D.; Campuzano, F.; Agudelo, A. F.; Cardona-Uribe, N.; Arenas, C. N. Chemical recycling of end-of-life</p><p>tires by intermediate pyrolysis using a twin-auger reactor: Validation in a laboratory environment. J.</p><p>Anal. Appl.</p><p>Pyrolysis 2021, 159, 105298,  DOI: 10.1016/j.jaap.2021.105298</p><p>66. Martínez, J. D.; Lapuerta, M.; García-Contreras, R.; Murillo, R.; García, T. Fuel Properties of Tire Pyrolysis Liquid</p><p>and Its Blends with Diesel Fuel. Energy Fuels 2013, 27, 3296– 3305,  DOI: 10.1021/ef400602e</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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CB de ELTs é vista como uma ação concreta de uma perspectiva de economia circular. Também</p><p>vale destacar que qualquer produto de cor preta contém CB, e por esta e outras razões, espera-se</p><p>que o mercado de CB continue crescendo nos próximos anos. A indústria de CB é caracterizada não</p><p>apenas pelo manuseio de quantidades muito grandes de materiais, mas também pela entrega de</p><p>propriedades consistentes ao longo do tempo e volumes de produção constantes. Nesse sentido, a</p><p>pirólise de ELTs deve progredir na produção e caracterização de RRCB de plantas semi-industriais</p><p>para preencher a lacuna deixada por protótipos em escala piloto e, assim, atender aos requisitos</p><p>impostos pelo setor. Em todos os casos, o RRCB deve ser convertido em rCB para atender à norma</p><p>ASTM D8178 para o melhor desempenho como agente de reforço em formulações de borracha.</p><p>A incorporação de TPO e RRCB em aplicações práticas em escala industrial promove a pirólise como</p><p>um mecanismo para o gerenciamento circular de produtos complexos de �m de vida, como ELTs.</p><p>Isso signi�ca que TPO e RRCB podem oferecer benefícios técnicos e econômicos reais, bem como</p><p>uma contribuição con�ável para reduzir as pegadas de carbono. Espera-se que ambos os produtos</p><p>de pirólise contribuam para o fechamento do ciclo na indústria de pneus e borracha. Até onde os</p><p>autores sabem, não há trabalhos na literatura que se concentrem no aumento de escala do processo</p><p>de pirólise de ELTs, embora deva ser mencionado que há informações muito úteis disponíveis para</p><p>biomassa.(32)Estudos detalhando as condições operacionais e os rendimentos e propriedades reais</p><p>dos produtos resultantes em uma escala semi-industrial fornecem um importante ímpeto para a</p><p>pirólise avançar em direção a uma economia circular para pneus. Além disso, espera-se que os</p><p>desa�os associados aos riscos impostos por fatores exógenos, como a dinâmica do mercado, a</p><p>con�abilidade da infraestrutura e a cadeia de suprimentos, sejam esclarecidos.(33)A escalabilidade</p><p>dos processos de pirólise é superada com dados con�áveis provenientes de campanhas</p><p>experimentais usando plantas semi-industriais, pois não há uma estratégia simples de aumento de</p><p>escala para levar esse tipo de processo termoquímico à maturidade.(34)</p><p>Como um passo à frente, este trabalho descreve pela primeira vez na literatura os rendimentos e</p><p>propriedades dos produtos obtidos da pirólise de ELTs usando duas escalas de reatores diferentes</p><p>com base na tecnologia auger sob condições operacionais semelhantes. A este respeito, os</p><p>resultados obtidos na planta em escala semi-industrial (400 kg/h) são su�cientemente robustos</p><p>para serem classi�cados no sétimo nível de prontidão tecnológica (TRL-7). Esses resultados são</p><p>totalmente comparáveis com aqueles obtidos em uma instalação em escala piloto (4 kg/h) que tem</p><p>sido intensamente estudada por nosso grupo de pesquisa,(3,35,36,39,43) and it aligns with the</p><p>characteristics of the �fth technology readiness level (TRL-5). In particular, the experimental</p><p>conditions in the TRL-5 facility have been meticulously selected to allow an accurate comparison,</p><p>including a similar volatile residence time (controlled by the feed rate of 4 kg/h) and the same</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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Menares, T.; Herrera, J.; Romero, R.; Osorio, P.; Arteaga-Pérez, L. E. Waste tires pyrolysis kinetics and reaction</p><p>mechanisms explained by TGA and Py-GC/MS under kinetically-controlled regime. Waste Manage. 2020, 102, 21–</p><p>29,  DOI: 10.1016/j.wasman.2019.10.027</p><p>68. Quek, A.; Balasubramanian, R. Liquefaction of waste tires by pyrolysis for oil and chemicals─A review. J. Anal.</p><p>Appl. Pyrolysis 2013, 101, 1– 16,  DOI: 10.1016/j.jaap.2013.02.016</p><p>69. Sienkiewicz, M.; Kucinska-Lipka, J.; Janik, H.; Balas, A. Progress in used tyres management in the European</p><p>Union: A review. Waste Manage. 2012, 32, 1742– 1751,  DOI: 10.1016/j.wasman.2012.05.010</p><p>70. Czajczyńska, D.; Krzẏyńska, R.; Jouhara, H.; Spencer, N. Use of pyrolytic gas from waste tire as a fuel: A review.</p><p>Energy 2017, 134, 1121– 1131,  DOI: 10.1016/j.energy.2017.05.042</p><p>71. Martínez, J. D.; Cardona-Uribe, N.; Murillo, R.; García, T.; López, J. M. Carbon black recovery from waste tire</p><p>pyrolysis by demineralization: Production and application in rubber compounding. Waste Manage 2019, 85, 574–</p><p>584,  DOI: 10.1016/j.wasman.2019.01.016</p><p>72. Cardona-Uribe, N. ; Betancur, M. ; Martínez, JD Rumo à valorização química do negro de fumo recuperado</p><p>derivado da pirólise de pneus em �m de vida . Sustainable Mater. Technol. 2021 , 28 , e00287</p><p>DOI: 10.1016/j.susmat.2021.e00287</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Scholar</p><p>| Google Acadêmico</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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pro�le along the reactor (450, 550, and 775 °C). The auger reactor is an emerging and</p><p>promising technology that offers a small speci�ed reactor size, low carrier gas �ow rate, and minimal</p><p>energy requirements. (44) Auger reactors also show an interesting versatility in the handling of solids</p><p>with poor �owability, such as ELTs. (45,46) They are easy to operate with different arrangements of</p><p>temperature distribution along the reactor, enabling the integration with different heat transfer media,</p><p>among others. The results reported in this work are expected to provide a major breakthrough in the</p><p>circular economy of tires and rubber products, while highlighting the bene�ts of the auger technology</p><p>at the semi-industrial scale.</p><p>2. Materials and Methods</p><p>2.1. Feedstock: End-Of-Life Tires</p><p>Both the pilot plant (TRL-5) and the semi-industrial plant (TRL-7) used granules of ELTs from truck</p><p>tires (TTs) without steel or textile �bers. However, the particle size of the TTs used in the pilot plant</p><p>was lower (2–4 mm) than that used in the semi-industrial plant (20–60 mm). This feedstock was</p><p>provided by Estato Umweltservice GmbH. Table 1 summarizes the characteristics of the feedstock in</p><p>terms of ultimate and proximate analyses and the higher calori�c value (HCV), carried out in</p><p>accordance with standards UNE-EN 15407 (Thermo Flash 1112), UNE-EN 15402-3 (IKA C-2000), and</p><p>UNE-EN 15400 (Parr 6400), respectively. The characterization data of the ELT samples reported in</p><p>Table 1 are found clearly in line with previously published data sets in the literature. (4,5,12)</p><p>Proximate analysis is a useful indicator for predicting the �nal product yields, as the volatile matter is</p><p>expected to be completely converted to TPG and TPO, leaving �xed carbon and ash in the RRCB</p><p>fraction.</p><p>Table 1. ELT Characterization</p><p>analysis, as received basis sample TT</p><p>Proximate (wt %)</p><p>moisture (wt %) 1.0</p><p>ash (wt %) 5.9</p><p>volatile matter (wt %) 65.0</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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stForLoginPage</p><p>https://pubs.acs.org/</p><p>analysis, as received basis sample TT</p><p>�xed carbon (wt %) 28.1</p><p>Ultimate (wt %)</p><p>carbon 84.5</p><p>hydrogen 7.11</p><p>nitrogen 0.49</p><p>sulfur 1.72</p><p>Calori�c value</p><p>HCV (MJ/kg) 37.5</p><p>2.2. Plants’ Description</p><p>2.2.1. Pilot Plant</p><p>The pilot plant used in this work is based on the single-auger technology and has been continuously</p><p>revamped and used for years by our research group for the pyrolysis not only of ELTs (3), (35−38) but</p><p>also of biomass (40,42,43) and polystyrene waste. (37) The plant is located in the laboratories of the</p><p>Instituto de Carboqumica (ICB) in Zaragoza, Spain. It can process up to 10 kg/h of shredded rubber.</p><p>The ELTs particles are fed by means of an agitated hopper that can hold approximately 25 kg of</p><p>rubber. The outer part of the reactor is surrounded by 3 independent electrical resistances, which</p><p>provide the energy for the pyrolysis process. The reactor also has two outlets to direct the resulting</p><p>vapors released during pyrolysis to the condenser. Various inert gas (N ) inlets are located at</p><p>strategic points in the reactor to ensure that air intrusions are minimized. The N �ow rate used to</p><p>maintain the inert atmosphere was set at 550 lN/h, using 6 independent gas mass �ow controllers</p><p>(Bronkhorst model: F-201CV-20K-AGD-22-V) with a �ow capacity between 20 and 1000 lN/h of N .</p><p>This N stream, which has been experimentally shown to have no signi�cant effect on volatile</p><p>residence time, yield, or product properties in the range of 300 to 2000 lN/h, helps to prevent volatile</p><p>accumulation and reduces the risk of undesirable phenomena such as backmixing.</p><p>2</p><p>2</p><p>2</p><p>2</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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condensed stream leaves the condenser by gravity, and it is stored in a small tank that is</p><p>periodically �ushed. The noncondensed gas leaves the reactor through the top and, after expansion</p><p>to recover liquid droplets, is sent to a �are where it is burned. A sample is taken for GC analysis prior</p><p>to �aring. The pilot plant is also equipped with a control and acquisition system to control feed rate</p><p>and solids residence time and to monitor the pressure and temperature at various key points. A</p><p>simpli�ed scheme is shown in Figure 2. A number of different pyrolysis processes have been</p><p>successfully carried out using this equipment and more information can be found elsewhere. (41) It</p><p>is worth noting that more than 300 h of operation has been accumulated, and more than 1000 kg of</p><p>TTs has been processed, demonstrating the feasibility and competitiveness of this technology for the</p><p>pyrolysis of ELTs.</p><p>Figure 2</p><p>Figure 2. Simpli�ed scheme of the pyrolysis pilot plant.</p><p>2.2.2. Semi-Industrial Plant</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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 semiindustrial-scale plant is located at the “Parque Tecnológico de Reciclado (PTR)” in Zaragoza,</p><p>Spain. The plant is owned by Greenval Technologies SL, making use of a license from the “Consejo</p><p>Superior de Investigaciones Cientí�cas (CSIC)”. The Environmental Research Group of the “Instituto</p><p>de Carboqumica (ICB)” belongs to CSIC. The semi-industrial plant is based on the single-auger</p><p>technology using the results and operational features of the pilot plant described above. A simpli�ed</p><p>scheme of the semi-industrial plant is shown in Figure 3. This plant was developed as a prototype to</p><p>re�ect the full-scale system, including all critical components and subprocesses. Extensive testing</p><p>has been carried out under real operating conditions, including replication of input materials (ELTs)</p><p>and operating parameters (temperature, mass �ow rate, etc.), and this paper presents some of that</p><p>work. The high throughput, stability, e�ciency, and security metrics con�rm that the technology</p><p>operates in a reliable and secure manner, supporting its classi�cation as TRL-7. The reactor geometry</p><p>of both plants can be considered similar according to the rule of partial similarity based on a</p><p>dimensional analysis. (34) This plant was designed for pyrolysis of ELTs at mass �ow rates of up to</p><p>800 kg/h, i.e., an upscale factor of 80 compared to the pilot plant. The feeding system consists of</p><p>three hoppers. The �rst one is used to load the ELTs, and then an endless screw introduces the</p><p>feedstock into the other two hoppers, which are connected to the pyrolyzer. These hoppers are</p><p>sealed and inerted under an N atmosphere. The con�guration of these twin hoppers enables a</p><p>continuous operation, so while one is being �lled, the other is continuously feeding the ELTs to the</p><p>pyrolyzer.</p><p>Figure 3</p><p>2</p><p>Este site usa cookies para melhorar</p><p>sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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ure 3. Simpli�ed scheme of the pyrolysis semi-industrial plant.</p><p>The heating of the auger reactor is provided by the combustion of TPG and supported by an auxiliary</p><p>lique�ed petroleum gas (LPG) burner. The resulting �ue gases are routed to an external chamber to</p><p>provide countercurrent heating, i.e., from the RRCB outlet to the ELT inlet. A temperature pro�le is</p><p>then observed along the reactor. N is used at various points in the plant to prevent possible leaks</p><p>and blockages caused by the accumulation of gas �ows. One of the points of injection is at the solid</p><p>discharge point to prevent contact of volatile materials with the RRCB. The N �ow rate is controlled</p><p>by manual valves and an electronic �ow meter. The TPO is recovered by two condensers and an</p><p>expansion system that removes the oil droplets present in the gas. The TPG is compressed and</p><p>stored in a gas tank that fed the burner. It should be noted that the experimental campaign carried</p><p>out in the semi-industrial plant lasted more than 100 h of operation and a total of 28 tonnes of ELTs</p><p>were processed.</p><p>2.3. Characterization of Products</p><p>2.3.1. Tire Pyrolysis Oil</p><p>The elemental composition of TPO derived from both plants was determined from ultimate analysis</p><p>using the UNE-EN 15407:2011 standard (Thermo Flash 1112). The HCV was also measured</p><p>2</p><p>2</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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to the UNE-EN 15400:2011 standard (Parr 6400). In addition, pH and the total acid number</p><p>(TAN) were determined using a Mettler Toledo T50 analyzer. TPO was also characterized in terms of</p><p>density (by gravimetry), viscosity (using a Brook�eld LVDV-E apparatus following the standard ASTM</p><p>D445), and water content (Crison Titromatic, ASTM E203). It should be noted that the results shown</p><p>in this study are summarized as the average of at least 5 measurements to ensure adequate</p><p>reproducibility.</p><p>In addition, the boiling point distribution was determined according to ASTM D2887 standard using a</p><p>PerkinElmer Clarus 590 gas chromatograph (GC) equipped with an on-column injector (POC), a wide-</p><p>range FID detector, and a 10 m Elite-2887 column (0.53 mm ID and 2.65 μm df). An initial oven</p><p>temperature of 45 °C was maintained for 2 min. A heating rate of 15 °C/min was then applied to</p><p>reach a �nal oven temperature of 325 °C. This temperature was maintained for 15 min. The carrier</p><p>gas was He at a constant column �ow of 7 mL/min. The POC injector followed a temperature</p><p>program of 5 °C above the oven temperature, and the wide-range FID temperature was set at 350 °C.</p><p>Sample volume injected was 0.5 μL in splitless mode using an auto sampler. The ASTM D2887</p><p>quantitative calibration mixture containing C to C n-para�n was injected to obtain a correlation</p><p>curve between retention time and boiling point.</p><p>A quanti�cation of some relevant compounds present in TPO was also carried out by GC the same</p><p>instrument as for that the boiling point distribution but with a different con�guration. Benzene,</p><p>toluene, ethylbenzene, o-xylene, m-xylene, p-xylene, and limonene were detected and quanti�ed. A</p><p>wide-range FID detector and a 60 m DB-5 ms capillary column (0.25 mm ID and 0.25 μm df) were</p><p>used. An initial oven temperature of 40 °C was maintained for 1 min. A heating rate of 5 °C/min was</p><p>then applied to reach a �nal oven temperature of 290 °C. The carrier gas was He at a constant</p><p>column �ow rate of 1 mL/min. The split/splitlee injector and wide-range FID temperatures were 300</p><p>and 325 °C, respectively. The sample volume injected was 0.5 μL using an autosampler and a split</p><p>ratio of 1:30. A quantitative calibration mixture containing 0.2 mass % each of benzene, toluene,</p><p>ethylbenzene, o-xylene, m-xylene, and p-xylene (BTEX) and 0.26 mass % of limonene was injected to</p><p>obtain the response factors of the FID detector for each compound.</p><p>The TPO from the pilot plant (TRL-5) and the semi-industrial plant (TRL-7) was also separated into</p><p>light and heavy fractions at atmospheric pressure using a laboratory distillation unit. A �ask</p><p>containing 250 mL of TPO was gradually heated from room temperature to 235 °C. The temperature</p><p>of the vapor phase was measured with a specially placed thermocouple. The condensed vapors were</p><p>collected in a �ask located after the cooling system to obtain the light fraction (LF). The heavy</p><p>fraction (HF) was collected as the residual oil in the original �ask. The resulting fractions obtained</p><p>6 44</p><p>Este site usa cookies para melhorar sua experiência de usuário. Ao continuar a usar o site, você está aceitando nosso uso de cookies. 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