KR101180580B1 - Selective Multistage Catalytic Pyrolysis Process for the Recycled Oil Recovery from Polymers - Google Patents
Selective Multistage Catalytic Pyrolysis Process for the Recycled Oil Recovery from Polymers Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/10—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal from rubber or rubber waste
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/02—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by distillation
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/14—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts
- C10G11/18—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts according to the "fluidised-bed" technique
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Abstract
본 발명은 고분자화합물의 고효율 열분해공법으로서, 열분해란 고분자화합물을 산소의 접촉없이 고열로 가열하여, 촉매의 작용으로 저분자로 분해하여 재생유 로 전환하거나, 지방족 혹은 방향족 단량체로 전환하는 반응이다. 그러나 생활계 혼합 폐합성수지에는 염화비닐수지(PVC)가 함유되어 있으며, 이 물질은 열분해온도가 비교적 낮고 분해시 다량의 부식성 염화수소를 방출함으로서, 생성된 재생유를 오염시켜 실용성을 저하시키게 되는 것이다. 본 발명은 선행발명인 특허출원 제2002-16586 및 특허출원 제2003-40640의 후속발명으로서, 재활용 재생유의 오염을 방지하기 위하여, 일단계로 염화비닐수지와 포리스틸렌수지 등의 분해온도가 낮은 수지류를 용융기에서 선택적으로 열분해하여, 생성물인 염화수소를 세정탑에서 중화하여 정화된 분해가스를 가스연소기로 열회수하고, 융해된 혼합페합성수지를 이단계 유동상분해기에 연속 투입하여 염소의 오염이 제거된 재생유를 분별증류탑에서 정제하여 연속 회수하며, 이때 분별증류탑하부로 낙하하는 고비점 왁스류를 다시 최종단계 고정상분해기에서 재분해하여 재생유로 회수하는 연속식 선택적 다단 촉매열분해공법에 관한 것이다.The present invention is a high-efficiency pyrolysis method of a polymer compound, wherein pyrolysis is a reaction in which a polymer compound is heated at high temperature without contact with oxygen, decomposed into low molecular weight by the action of a catalyst, and then converted into a regeneration oil or an aliphatic or aromatic monomer. However, vinyl chloride resin (PVC) is contained in the mixed waste plastics, and the material has a relatively low thermal decomposition temperature and releases a large amount of corrosive hydrogen chloride when decomposed, thereby contaminating the generated regenerated oil, thereby degrading practicality. The present invention is a follow-up invention of the patent application No. 2002-16586 and the patent application No. 2003-40640 of the prior invention, in order to prevent the contamination of recycled recycled oil, resins having low decomposition temperature such as vinyl chloride resin and polystyrene resin in one step Is selectively pyrolyzed in the melter, the product of hydrogen chloride is neutralized in the washing tower, and the purified cracked gas is heat-recovered with a gas burner, and the mixed mixed mixed resin is continuously introduced into a two-stage fluidized bed cracker to remove chlorine contamination. The present invention relates to a continuous selective multi-stage catalytic pyrolysis process in which regenerated oil is purified and recovered continuously in a fractionation tower, wherein high boiling point waxes falling to the bottom of the fractionation column are re-decomposed in a final stage fixed bed cracker and recovered as regeneration oil.
Description
본 발명이 속하는 기술분야는 고분자화합물의 열분해공법으로서, 열분해공법이란 염화비닐수지(PVC), 포리에티렌(PE), 포리프로피렌(PP) 등 지방족 고분자화합물과, 포리에티렌테레프타레이트(PET), 포리스티렌(PS), 아크리로나이트릴부타디엔스티렌(ABS)수지 등의 방향족 고분자화합물의 혼합물을 선별없이, 산소의 접촉없이 고열로 가열하여 저분자 탄화수소로 분해시켜 재생유로 전환하고, 단량체로도 회수할 수 있는 경제적이며, 고부가가치의 공법이다. The technical field of the present invention is a thermal decomposition method of a polymer compound, the thermal decomposition method is an aliphatic high molecular compound such as vinyl chloride resin (PVC), polyether (PE), polypropylene (PP), and polyether terephthalate ( PET), polystyrene (PS), and a mixture of aromatic polymer compounds such as acryronitrile butadiene styrene (ABS) resins are heated to high temperature without contact with oxygen, without being screened, and decomposed into low molecular hydrocarbons. It is an economical and high value-added process that can be recovered.
본 발명의 선행발명인 특허출원 제2002-16586은 고정상 열분해촉매가 관내에 충전된 무교반 박막열분해장치로서, 이 공법은 혼합 폐합성수지를 용융하여 액상수지를 고정상 촉매를 통과하여 흘러 내려가게 함으로서 촉매열분해반응이 일어남으로서, 액상의 열가소성수지만을 반응시킬 수 있고, 고형물은 촉매표면에 침적되어 고정상이 막힐 우려가 있음으로서, 이를 여과시켜 제거함으로서 열경화성수지는 처리하지 못하는 제약이 있었다. Patent Application No. 2002-16586, which is a prior invention of the present invention, is an agitated thin film pyrolysis apparatus in which a fixed bed pyrolysis catalyst is filled in a tube, and this method melts a mixed waste synthetic resin so that the liquid resin flows down through the fixed bed catalyst to decompose the catalytic pyrolysis. As the reaction occurs, only the liquid thermoplastic resin can be reacted, and the solids may be deposited on the surface of the catalyst and the fixed phase may be blocked. Thereby, there is a limitation that the thermosetting resin cannot be treated by filtration.
특허출원 제2003-40640은 선행발명에서 처리하지 못하는 고형물을 촉매열분해하기 위하여, 공지의 열분해공법인 기류이송열분해기술을 개선하여 폐합성수지의 열분해에 적합한 공법을 개발하였다. 반응단계를 1단낙하열분해와 2단낙하열분해로 구분하여, 1단낙하열분해단계에서는 투입된 혼합 폐합성수지중에서 고열에 의하여 용융되는 열가소성수지를 우선 열분해하여 등유류를 주로한 연료유를 생성하고, 2단낙하열분해단계에서는 반응기 내에 고열의 촉매를 추가 도입함으로서 온도를 상승시켜, 전단계에서 반응하지 못한 분말상의 열경화성수지마저도 열분해시켜서, 저분자 탄화수소인 분해가스를 생성함으로서 액상과 분말상의 폐합성수지를 단일반응체계내에서 효과적으로 연속열분해하는 것이다. Patent application No. 2003-40640 has developed a method suitable for pyrolysis of waste synthetic resins by improving the airflow pyrolysis technique, which is a known pyrolysis method, for catalytic pyrolysis of solids that cannot be treated in the prior invention. The reaction stage is divided into one-stage falling pyrolysis and two-stage falling pyrolysis, and in the first-stage falling pyrolysis step, firstly pyrolyzes the thermoplastic resin melted by high heat in the mixed waste synthetic resin input to produce fuel oil mainly composed of kerosene. In the fall-fall pyrolysis step, a high-temperature catalyst is added to the reactor to increase the temperature, and thermally decompose the powdery thermosetting resin, which has not reacted in the previous stage, to generate cracked gas, which is a low molecular hydrocarbon, to form a liquid and powdery waste synthetic resin in a single reaction system. It is effective pyrolysis within.
종래의 공지의 기류이송열분해공법은 재생된 고온의 재생촉매를 반응가스나 불활성가스와 함께 순환시키는 수직관형 기류이송열분해반응기 내에, 액상 또는 분말상의 폐합성수지를 연속투입하여 고온의 재생촉매와 원료수지가 직접 접촉하여 열이 전달됨으로서 촉매열분해가 촉진되도록 하는 반응장치로서, 기류이송 열분해반응기는 상승식과 낙하식의 2가지 방법이 있으나, 이들 모두 반응 시간은 수초로서 매우 짧아서, 열분해 온도와 조건이 다양한 혼합합성수지를 단일 반응 단계로서 전부 열분해하기에는 어려움이 있다. 미국특허 제6,534,689는 이를 보완하는 방안으로서 낙하식 기류열분해기의 하부수기에서 다시 유동층 열분해를 시킴으로써 반응을 완결시키고자 하였다. 그러나 유동상을 형성시키기 위하여는 반응가스나 불활성가스를 유동상 하부로 송풍해야하며, 이는 생성 탄화수소 회수나, 염화수소가스 제거를 방해하여 실용성이 결여되는 것이다. Conventionally known air flow pyrolysis methods continuously inject liquid or powdered waste synthetic resin into a vertical tubular air flow pyrolysis reactor which circulates the regenerated high temperature regenerated catalyst together with the reaction gas or the inert gas, thereby regenerating the high temperature regeneration catalyst and the raw material resin. Is a reaction apparatus that promotes catalytic pyrolysis by direct contact with heat transfer, and there are two methods of air transfer pyrolysis reactors, a rising type and a falling type, but the reaction time is very short as several seconds, so that the pyrolysis temperature and conditions vary. It is difficult to pyrolyze the mixed synthetic resin as a single reaction step. U.S. Patent No. 6,534,689 intends to complete the reaction by performing fluidized bed pyrolysis again in the bottom water of the falling air stream pyrolysis unit as a complementary solution. However, in order to form a fluidized bed, a reaction gas or an inert gas needs to be blown to the lower part of the fluidized bed, which impedes practicality by impeding the recovery of generated hydrocarbons or removing hydrogen chloride gas.
열분해반응은 고온의 인화성 증기가 발생하는 민감한 촉매반응으로서, 또한 열분해 반응온도가 생성되는 저분자 탄화수소의 발화점을 상회하여, 종래의 열분해 반응장치로는 인화 및 발화위험성이 높고, 촉매의 오염 및 손실로 인한 활성 저하로 분해가스 및 타르상 탄화물의 과도한 생성과 장치의 기계적 취약성 및 고난도 운전기법이 요구됨으로 인하여 실용화가 되지 못하였다. 또한 페프라스틱 발생량의 절반에 달하는 생활계 혼합폐합성수지에는 염화비닐수지(PVC)가 함유되어 있으며, 이 물질은 열분해온도가 비교적 낮고 분해시 다량의 부식성 가스인 염화수소를 방출함으로서 생성된 분해가스를 오염시켜, 회수 재생유의 재활용을 저해하는 요소가 되는 것이다. 또한 분해가스를 재활용하지 못함으로서 에너지 효율이 저조하여 손익 분기점에 못미쳐 경제성이 저하되었던 것이다.Pyrolysis is a sensitive catalytic reaction in which high-temperature flammable vapors are generated. In addition, the pyrolysis reaction temperature exceeds the ignition point of low molecular hydrocarbons, and the pyrolysis reaction apparatus has a high risk of ignition and ignition. Due to the deterioration of the activity due to excessive generation of cracked gas and tar phase carbide, mechanical fragility of the device and a high degree of difficulty operation technique was not practical. In addition, vinyl chloride resin (PVC) is contained in the life-cycle mixed synthetic resin, which accounts for half of the amount of plastics produced, and this material contaminates the decomposition gas generated by releasing a large amount of corrosive gas, hydrogen chloride, during decomposition. As a result, it is a factor that hinders the recycling of recovered recycled oil. In addition, due to the inability to recycle cracked gas, energy efficiency was low, falling short of the break-even point, resulting in economic deterioration.
본 발명은 자동투입기로 원료투입시 질소밀봉실을 통과시켜 산소의 유입을 완전차단하여 화재발생요인을 근원적으로 예방하였으며, 재생유의 오염을 방지하기 위하여, 일단계 용융기에서 염화비닐수지와 포리스틸렌수지 등의 분해온도가 낮은 수지류를 선택적으로 분해하여, 생성물인 염화수소를 배출시켜 세정탑에서 중화하고 정화된 분해가스를 가스연소기로 연소시켜 열분해 열원으로 사용하여 열회수함으로서 에너지 효율을 향상시켜 경제성을 제고시켰으며, 용융기에서 융해되어 미분해된 폴리올레핀 등 열가소성수지를 이단계 유동상분해기에 연속 투입하여 예열된 촉매상에서 급속 열분해시킴으로서 타르 및 탄화물의 생성을 최소화하고, 생성되는 분해증기를 일관공정으로 연속적으로 분별증류탑으로 도입시키고 탑내에서는 충전층을 통하여 증기가 상승하며 저비점유와 왁스를 연속적으로 분리시켜 염소의 오염이 없는 정제된 고품질의 재생유를 분별증류탑 측면 회수변을 통하여 연속 회수하며, 최종단계로 분별증류탑하부의 고정상분해기 상부로 낙하하는 고비점 왁스류를 촉매상에서 재분해하여 저분자로 전환된 재생유를 충전층을 통하여 상승시켜 회수변을 통하여 고품질의 재생유를 고수율로 회수하게 되는 것이다.The present invention prevents the influx of fire by fundamentally preventing the inflow of oxygen by passing the nitrogen sealing chamber when the raw material is fed into the automatic feeder, and to prevent contamination of the regenerated oil, the vinyl chloride resin and the polystyrene in the first stage melter. It selectively decomposes resins with low decomposition temperature such as resins, discharges hydrogen chloride as a product, neutralizes them in the washing tower, burns the purified decomposition gas with a gas burner, and uses it as a heat source for pyrolysis to improve energy efficiency. The thermoplastic resins, such as polyolefins melted in the melter and undigested polyolefin, are continuously introduced into the two-stage fluidized bed cracker to rapidly pyrolyze on the preheated catalyst, thereby minimizing the generation of tar and carbides, and producing the cracked steam in a consistent process. Continuously introduced into the fractionation column, the packed bed in the tower As the vapor rises, low boiling point and wax are separated continuously, and purified high-quality recycled oil without chlorine contamination is continuously recovered through the side of the distillation column, and finally falls to the top of the fixed bed cracker under the distillation column. The high boiling point waxes are re-decomposed on the catalyst to raise the regenerated oil converted into the low molecular weight through the packed bed to recover the high quality regenerated oil through the recovery valve in high yield.
1) 염화비닐수지가 함유된 혼합합성수지에서 재생유를 실용적으로 회수함으로서 약삼백만톤/년에 달하는 폐합성수지를 종말처리하지 않고 대체에너지로 재활용할 수 있게 되어 환경보호와 원유 수입대체효과를 달성한다.. 1) By practically recovering recycled oil from mixed synthetic resin containing vinyl chloride resin, it is possible to recycle waste synthetic resin of about 3 million tons / year as alternative energy without end-processing to achieve environmental protection and crude oil import substitution effect. ..
2) 염화비닐수지는 4대 범용수지중의 하나로서 선택적 다단 촉매열분해공법으로 염화수소와 재생유가 경제적으로 분리 회수됨으로서, 폐염화비닐수지의 재활용실용화를 달성한다.2) Vinyl chloride resin is one of the four general-purpose resins, so that hydrogen chloride and recycled oil are separated and recovered economically by selective multi-stage catalytic pyrolysis method, thereby achieving practical use of waste vinyl chloride resin.
[도 1]은 고분자화합물에서 재생유를 회수하기 위한 연속식 선택적 다단 촉매열분해공법의 공정도이다. 1 is a process diagram of a continuous selective multistage catalytic pyrolysis method for recovering regenerated oil from a polymer compound.
별첨도면에 의하여 상세히 설명하면;If described in detail by the accompanying drawings;
(101)자동투입기에 투입된 압축포장된 혼합합성수지를 질소가 충전된 밀봉실을 통하여 (102)용융기에 연속적으로 공급하여 용융시키고, 부분 열분해된 분해가스와 염화비닐수지가 열분해하여 생성된 염화수소를 증기관을 통하여 (108)세정탑으로 유입시켜 순환되는 세정수에 의하여 급냉하고 가성소다로 중화하며, 용융기내에 잔류하는 미분해된 융해수지는 (103)유동상분해기로 연속투입하여 예열된 촉매와 접촉시켜 급속 열분해시키며, 염소에 오염되지 않은 생성된 분해증기는 (104)분별증류탑으로 일관공정으로 연속 도입하여 충전층을 통하여 탑정으로 상승하며 탑정에서 하강하는 환류액에 의하여 응축과 기화가 반복하여 분별증류가 일어나 분해가스와 저비점유는 탑정으로 상승하고 고비점 왁스는 탑하부로 하강하여 정제된 재생유는 탑측면의 회수변을 통하여 유출시켜 (106)냉각기를 통하여 냉각되며 (107)재생유조로 유입되어 저장된다. 분별증류탑 하부로 하강하는 왁스는 (105)고정상분해기로 유입되어 촉매상에서 재분해하여 저분자로 전환되어 충전층을 통하여 상승하여 재생유 회수변을 통하여 회수된다. 유동상분해기에 잔류하는 분해잔사는 활성이 저하된 폐촉매와 혼합되어 측면 배출구로 연속배출된다. 분해가스와 저비점유분은 탑정으로 배출되어 응축기를 통하여 응축되어 환류되고, 미응축 분해가스는 (108)세정탑을 통하여 정화되어 (109)가스저장조에 유입 저장되며 (110)가스연소기에 공급되어 연소시켜 열분해 열원으로 사용하여 열회수하여 에너지 효율을 향상시킨다. (101) Compression-packed mixed synthetic resin fed into an automatic feeder is continuously supplied to a melter through a sealed chamber filled with nitrogen (102) and melted, and hydrogen chloride produced by thermal decomposition of partially pyrolyzed decomposition gas and vinyl chloride resin is steamed. It is quenched by the circulating washing water and neutralized with caustic soda through (108) through the washing tower, and unresolved molten resin remaining in the melter is continuously introduced into the (103) fluidized-phase cracker and contacted with the preheated catalyst. The resulting cracked steam, which is not contaminated with chlorine, is introduced into the (104) fractionation column continuously in a consistent process and ascends to the column through the packed bed and is repeatedly fractionated by condensation and vaporization by reflux from the column. Distillation causes cracked gas and low boiling point to rise to the top and high boiling wax drops to the bottom of the column. Cooling through the outlet was 106 cooler through the waterside is stored is introduced into 107 oil bath playback. Wax descending to the bottom of the fractional distillation column is introduced into the (105) stationary bed cracker, re-decomposes on a catalyst, is converted into low molecules, and is raised through a packed bed to be recovered through a reclaimed oil recovery valve. The decomposed residues remaining in the fluidized bed cracker are mixed with the deactivated waste catalyst and continuously discharged to the side outlet. The cracked gas and the low boiling fraction are discharged to the tower top, condensed and refluxed through the condenser, and the uncondensed cracked gas is purified through the washing tower (108), flowed into the gas storage tank (109) and supplied to the gas combustor, and burned. It is used as a pyrolysis heat source to heat recovery to improve energy efficiency.
[도 1]의 공정도의 각장치의 부호는 다음과 같다;
(101) 자동투입기 (106) 냉각기
(102) 용융기 (107) 재생유조
(103) 유동상분해기 (108) 세정탑
(104) 분별증류탑 (109) 가스조
(105) 고정상분해기 (110) 가스연소기 The code | symbol of each apparatus of the process diagram of FIG. 1 is as follows;
(101) Automatic Input Machine (106) Cooler
(102) Melter (107) Regeneration Tank
(103) Fluidized Bed Crackers (108) Cleaning Towers
(104) Fractionation distillation tower (109) Gas tank
(105) Stationary phase crackers (110) Gas burners
Claims (1)
가) 일단계로 용융기에서 염화비닐수지와 포리스틸렌수지 등의 분해온도가 낮은 수지를 섭씨300도 이하에서 선택적으로 열분해하여 생성된 염화수소를 세정탑에서 중화 세정한후, 분해가스는 가스연소기에서 연소시켜 열분해 열원으로 열회수하고,
나) 이단계로 용융기에서 분해되지 않고 융해된 잔류 고분자화합물을 유동상분해기로 연속 투입하여 섭씨700도 이하에서 예열된 촉매와의 직접접촉으로 폴리올레핀계 등의 열가소성수지를 급속 열분해하여 탄화물 생성을 최소화 시키고, 일관공정으로 분별증류탑으로 연속적으로 도입하여 염소 오염 및 저비점유와 왁스가 제거되어 정제된 재생유를 탑측면 회수변을 통하여 연속 회수하며,
다) 삼단계로 분별증류탑하부의 고정상분해기로 낙하하는 고비점 왁스류를 섭씨500도 이하에서 촉매상에서 연속 재분해하여 저분자로 전환하여 충전층을 통하여 상승시켜 회수변을 통하여 정제된 재생유를 회수하는,
이상의 단계별 선택적 열분해 및 질소밀봉과 분해가스 열회수를 특징으로하는 고분자화합물의 연속식 선택적 다단 촉매열분해공법. In order to completely prevent the influx of oxygen through the nitrogen sealing chamber and to inject the polymer compound through the automatic feeding machine continuously, it is possible to fundamentally prevent fire factors, and to selectively catalytically decompose vinyl chloride resin, thermoplastic resin and wax at each stage. ,
In the first stage, hydrogen chloride produced by selectively pyrolyzing resins with low decomposition temperatures such as vinyl chloride resin and polystyrene resin in the melter at less than 300 degrees Celsius is neutralized and cleaned in the washing tower, and the decomposition gas is Burn and heat recovery to pyrolysis heat source,
B) Minimize the formation of carbides by rapid thermal decomposition of thermoplastic resins such as polyolefins through direct contact with catalyst preheated below 700 degrees Celsius by continuously injecting residual polymer compound which is not decomposed in the melter into the fluidized bed decomposer. And continuously introduced into the fractionation tower by a consistent process to remove the chlorine contamination, low boiling point and wax, and to recover the purified regenerated oil through the tower side recovery valve,
C) The high boiling point waxes falling into the fixed bed cracker at the bottom of the fractionation distillation column in three stages are continuously re-decomposed on the catalyst at below 500 degrees Celsius, converted to low molecular weight, raised through the packed bed, and recovered through the recovery bed. doing,
Continuous selective multistage catalytic pyrolysis of polymer compounds characterized by selective pyrolysis and nitrogen sealing and cracked gas heat recovery as described above.
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