KR20020023472A - Catalyst for recycle of monomer from disused plastic of polyethylene origin - Google Patents
Catalyst for recycle of monomer from disused plastic of polyethylene origin Download PDFInfo
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Abstract
Description
본 발명은, 폴리스틸렌(PS), 폴리메칠메타아크릴(PMMA)을 열분해하여 모노머를 분리, 회수시 회수효율 증대를 위한 촉매와 열분해 방법에 관한 것으로서, 보다 상세하게는, 폴리스틸렌, PMMA등 해중합형의 폐플라스틱으로부터 열분해에 의해 모노모를 회수하는 경우 모노모 회수율 증대를 위한 촉매와 열분해 속도의 촉진을 위한 가열방법을 얻을 수 있는 폴리스틸렌계 폐플라스틱으로부터 모노머 회수를 위한 촉매 및 열분해 방법에 관한 것이다.The present invention relates to a catalyst and a pyrolysis method for thermal recovery of polystyrene (PS) and polymethyl methacryl (PMMA) to increase the recovery efficiency when separating and recovering monomers, and more particularly, to depolymerization such as polystyrene and PMMA. When recovering monomo by pyrolysis from waste plastics, the present invention relates to a catalyst for pyrolysis and a pyrolysis method for recovering monomers from polystyrene-based waste plastics.
최근 폐플라스틱의 발생에 의한 환경 문제가 크게 제기되고 있으나 재활용율은 여전히 저조한 실정이다.Recently, environmental problems due to the generation of waste plastics have been raised, but the recycling rate is still low.
폐플라스틱의 재활용 방법은 원형 그대로 또는 가공하여 재활용하는 방법(Material Recycle), 소각 등의 열적 재활용(Thermal Recycle), 수지원료 등의 화학물질을 회수하는 방법(Chemical Recycle)으로 구분된다.The recycling method of waste plastics is divided into the original form or the process of recycling (Material Recycle), thermal recycling (incineration), and chemical recycling (eg, chemical recycling).
수지원료를 경제성 있게 회수하기 위한 방법이 개발된다면 부가가치가 큰 재활용 방법으로 평가될 수 있으나 아직은 기술개발 수준이 이에 미치지 못한 실정이다.If a method for economically recovering the support fee is developed, it can be evaluated as a high value-added recycling method, but the level of technology development is still far below this level.
본 발명은, 폐플라스틱중 폴리스틸렌, PMMA으로부터 원료물질 회수를 위한 화학적 리싸이클링을 목표로 열분해에 의한 모노머 회수 효율의 증대를 위한 촉매와 열분해 방법을 제공하는 것이다.The present invention provides a catalyst and pyrolysis method for increasing monomer recovery efficiency by pyrolysis, with the aim of chemical recycling for recovery of raw materials from polystyrene and PMMA in waste plastic.
폐플라스틱의 열분해 형태를 보면 폴리에틸렌(PE), 폴리프로필렌(PP)은 랜덤(rendom)분해, 폴리스틸렌(PS)과 PMMA는 해중합형으로서 모노머 형태로의 분해가 이루어진다. 따라서 폴리스틸렌, PMMA계의 플라스틱은 열분해조작을 통하여 비교적 쉽게 모노머를 회수할 수 있으며, 모노머 회수의 경제성을 높이기 위해서는 열분해 속도의 촉진과 모노머 회수율의 증대가 필수적이다.In the pyrolysis form of waste plastics, polyethylene (PE) and polypropylene (PP) are randomly decomposed, polystyrene (PS) and PMMA are depolymerized into monomers. Therefore, polystyrene and PMMA-based plastics can recover monomers relatively easily through pyrolysis operation, and in order to increase the economic efficiency of monomer recovery, it is necessary to promote the thermal decomposition rate and increase the monomer recovery rate.
폴리스틸렌을 촉매를 처리하지 않고 열분해 시켰을 때 열분해 생성물은 모노머를 비롯하여 파라핀, 올레핀 방향족의 생성물이 다양하게 분포되나 적정 촉매로처리하면 탄소-탄소간의 분해보다는 모노머 단위로 분해가 이루어져 모노머 회수율을 크게 높일 수 있다.When polystyrene is thermally decomposed without treating a catalyst, pyrolysis products include various monomers, paraffins, and olefin aromatic products.However, by treating with a proper catalyst, the decomposition of monomers can be increased by monomer units rather than carbon-carbon decomposition, thereby greatly increasing the monomer recovery rate. have.
한편, 폐플라스틱은 열전도성이 낮고 특히 폴리스틸렌의 열분해시엔 코킹현상이 심하여 전열면에 부착되거나 촉매상에 석출되어 장애를 일으키므로 열분해를 위한 가열시엔 열전달율을 높이고 코킹 현상을 줄이는 방안이 중요하다.On the other hand, waste plastics have low thermal conductivity and particularly coking phenomenon during the thermal decomposition of polystyrene, which is attached to the heat transfer surface or precipitates on the catalyst, thus causing an obstacle, so it is important to increase the heat transfer rate and reduce the coking phenomenon when heating for pyrolysis.
폴리스틸렌, PMMA계의 폐플라스틱과 같이 해중합형의 폐플라스틱은 열부해 생성오일 중에 모노머의 함유 정도는 열분해 조건과 촉매처리 여부에 따라 차이가 나타난다. 그리고 폐플라스틱은 열전도성이 낮고 또한 열분해시 코킹현상으로 인한 열전달율의 저하 등의 장애점이 크다.The waste plastics of depolymerization type, such as polystyrene and PMMA waste plastics, are different from each other due to thermal decomposition conditions and catalyst treatment. In addition, waste plastics have low thermal conductivity and have high obstacles such as lowering of heat transfer rate due to coking phenomenon during pyrolysis.
따라서, 본 발명은 폴리스틸렌, PMMA계의 폐플라스틱으로부터 고부가가치의 모노머 회수를 위한 적정 촉매와 열분해 방법을 제공하는 것이다.Accordingly, the present invention provides an appropriate catalyst and pyrolysis method for recovering high value-added monomers from waste plastics of polystyrene and PMMA.
도 1은 본 발명에 따른 폐플라스틱의 열분해에 의한 모노머 회수 실험장치 개념도이다.1 is a conceptual diagram of a monomer recovery experiment by pyrolysis of waste plastics according to the present invention.
* 도면중 주요 부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : 질소가스 2 : 가열로1: nitrogen gas 2: heating furnace
3 : 열분해 반응기 4 : 폐플라스틱+촉매3: pyrolysis reactor 4: waste plastic + catalyst
5 : 온도제어 6 : 분리조5: temperature control 6: separation tank
7 : 응축기 8 : 오일회수조7: condenser 8: oil recovery tank
본 발명에서 폐플라스틱의 열분해 촉진과 코킹현상 감소를 위한 가열 방법은 열분해 오일의 일정량을 열분해 반응기에 환류시켜 폐플라스틱과 잘혼합, 가열함으로써 환류 오일이 팽윤제, 용매로의 역할에 의한 것이고, 모노머 회수율 증대는 적정 촉매에 의해 달성하는 것이다.In the present invention, a heating method for promoting pyrolysis of waste plastic and reducing coking phenomenon is by refluxing a predetermined amount of pyrolysis oil into a pyrolysis reactor to mix and heat the waste plastic well, and thus the reflux oil acts as a swelling agent and a solvent. The increase in recovery is achieved by the titration catalyst.
도 1은 본 발명에 따른 폐플라스틱의 열분해에 의한 모노머 회수 실험장치 개념도에 관한 것이다. 이 도면에서 볼 수 있는 바와 같이 폐플라스틱중 해중합형인 폴리스틸렌, PMMA를 대상으로 하여 폐플라스틱과 각종 촉매 일정량을 열분해반응기(3)에 넣고 450℃로 가열한다.1 is a conceptual diagram of a monomer recovery experimental apparatus by pyrolysis of waste plastics according to the present invention. As can be seen from this figure, waste plastics and various catalysts are put in a pyrolysis reactor 3 for polystyrene and PMMA, which are depolymerized waste plastics, and heated to 450 ° C.
분해된 가스상은 응축기(7)에서 응축하여 오일을 회수(8)하고 비응축성 가스를 분리한다. 회수 오일은 일정량 열분해 반응기에 환류시켜 폐플라스틱과 혼합, 가열한다. 그리고, 회수오일을 2차적 증류 처리를 통하여 오일과 모노머를 분리한다.The decomposed gas phase condenses in the condenser 7 to recover oil 8 and separates the non-condensable gas. The recovered oil is refluxed in a constant amount of pyrolysis reactor, mixed with waste plastic and heated. The oil is separated from the monomer through the secondary oil distillation.
[실시예 1]Example 1
도 1에 표시된 장치의 열분해 반응기(3)에 폴리스틸렌 20g과 각종의 촉매 1g을 넣고 균일하게 혼합하면서 반응기내의 온도를 450℃로 유지, 열분해 하여 생성된 가스상을 응축함으로서 오일을 회수한다. 회수 오일을 2차 증류 과정을 통하여 모노머와 오일을 분리한다. 촉매 종류별 모노머 회수효과를〈표 1〉에 비교하였다.Into the pyrolysis reactor 3 of the apparatus shown in FIG. 1, 20 g of polystyrene and 1 g of various catalysts were added and mixed uniformly, while maintaining the temperature in the reactor at 450 ° C. to pyrolyze the resulting gas phase to recover oil. The recovered oil is subjected to secondary distillation to separate monomers and oil. The monomer recovery effect by catalyst type was compared to <Table 1>.
〈표 1〉PS의 열분해 및 촉매에 의한 모노머 회수 효과<Table 1> Thermal recovery of PS and monomer recovery effect by catalyst
(wt.%)(wt.%)
〈표 1〉에서 무촉매의 경우 스틸렌 모노머의 수율은 18%로서 가장 낮으며 촉매 처리 없이 열분해 하는 경우는 스틸렌 모노머나 다이머까지 완전히 분해되지 못하는 것으로 간주된다.In Table 1, the yield of styrene monomer is the lowest as 18% in the case of the non-catalyst, and it is considered that the pyrolysis without catalytic treatment does not completely decompose styrene monomer or dimer.
SiO2, Al2O3, 활성탄 중 BTX 수율은 활성탄이 높고 스틸렌 모노머 수율은 알루미나가 높다.The yield of BTX in SiO 2 , Al 2 O 3 and activated carbon is high in activated carbon and the yield of styrene monomer is high in alumina.
제올라이트게 고체상 촉매의 경우 모노머 회수율은 산강도와 관계가 있어 산의 강도가 큰 것일수록 모노머 회수율은 적게 나타난다.In the case of zeolite crab solid catalyst, the monomer recovery rate is related to the acid strength, so that the higher the acid strength, the lower the monomer recovery rate.
고체염기 촉매는 모노머 수율이 높아 BaO가 73%, 알루미나에 BaO(5wt.%)를 담지시킨 BaO/Al2O3가 79%로 가장 높다. 그리고 탈수소 촉매인 NiO, ZnO, Ag-ZSM-5의 경우 ZnO가 65%의 수율로 비교적 높다.The solid base catalyst has a high yield of monomers, the highest being BaO of 73%, and BaO / Al 2 O 3 having BaO (5 wt.%) Loaded on alumina is the highest at 79%. In the case of NiO, ZnO, and Ag-ZSM-5 which are dehydrogenation catalysts, ZnO is relatively high with a yield of 65%.
[실시예 2]Example 2
PMMA 20g과 각종의 촉매 1g을 450℃로 예열된 열분해 반응기(3)에 넣고 온도를 유지하면서 열분해 하여 생성오일을 얻고 이로부터 2차 증류에 의한 방법으로 모노머를 분리하였으며 그 결과를 〈표 2〉에 나타냈다.20 g of PMMA and 1 g of various catalysts were put in a pyrolysis reactor (3) preheated to 450 ° C. and pyrolyzed while maintaining the temperature to obtain a product oil. The monomers were separated from the monomers by secondary distillation. Indicated.
〈표 2〉PMMA의 열분해 및 촉매에 의한 모노머 회수 효과Table 2: Effect of pyrolysis and catalyst recovery of PMMA
PMMA의 경우 열분해에 의해 비교적 쉽게 모노머 회수가 가능하며 BaO, ZnO와 같은 고체 염기 촉매가 효과가 크게 나타난다.In the case of PMMA, monomer recovery is relatively easy by pyrolysis, and solid base catalysts such as BaO and ZnO show a great effect.
[실시에 3][Example 3]
폴리스틸렌 20g을 열분해 반응기(3)에 넣고 450℃로 가열 폴리스틸렌의 열분해가 완료되는 시간과 열분해 오일의 5wt.% 정도를 열분해 반응기에 환류하여 폴리스틸렌과 혼합, 열분해 하였을 경우의 열분해 소요시간을 비교하였고 각 경우의 조작을 반복시 전열면에 코킹 현상 정도를 비교하였다.20 g of polystyrene was added to the pyrolysis reactor (3), and the time required for pyrolysis of the polystyrene was completed and about 5 wt.% Of the pyrolysis oil was refluxed in the pyrolysis reactor and mixed with the polystyrene. When the operation was repeated, the degree of caulking phenomenon was compared to the heat transfer surface.
폴리스틸렌만을 열분해 할 경우 소요시간을 1시간 이상이 소요되었으나 환류시켜 폴리스틸렌과 혼합, 열분해할 경우에 40∼50분 소요되었다.Pyrolysis of only polystyrene took more than 1 hour, but it took 40 to 50 minutes when refluxed and mixed with polystyrene.
또한, 전열면에 형성되는 코킹 현상도 다소 감소하였다. 열분해 오일의 환류 조작에 의해 열분해 시간의 단축과 코킹 현상을 줄일 수 있는 것은 환류 오일이 열매체 및 용매의 작용에 기인되는 것으로 간주된다.In addition, the coking phenomenon formed on the heat transfer surface was also slightly reduced. It is considered that reflux oil is due to the action of the heat medium and the solvent to shorten the pyrolysis time and reduce the coking phenomenon by the reflux operation of the pyrolysis oil.
이상 설명한 바와 같이, 본 발명에 따르면, 폴리스틸렌으로부터 모노머 회수는 촉매처리 없이 열분해 하는 경우에 비하여 고체염기 촉매를 사용하여 모노머 회수율의 3배 이상으로 증가시킬 수 있다. 그리고, 폐플라스틱은 열전도성이 낮고 특히 폴리스틸렌은 열분해시의 코킹성이 크므로 열분해 오일을 일부 환류하여 폴리스틸렌과 혼합, 열분해 함으로서 열분해 속도를 높이고 코킹현상을 줄일 수 있는 폴리스틸렌계 폐플라스틱으로부터 모노머 회수를 위한 촉매 및 열분해 방법이 제공된다.As described above, according to the present invention, the monomer recovery from the polystyrene can be increased by three times or more of the monomer recovery rate using a solid base catalyst as compared with the case of pyrolysis without the catalytic treatment. In addition, since waste plastics have low thermal conductivity and polystyrene has high coking property during pyrolysis, partial recovery of monomers from polystyrene waste plastics which can increase pyrolysis rate and reduce coking phenomenon by mixing and pyrolyzing the pyrolysis oil with polystyrene is performed. Catalysts and pyrolysis methods are provided.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100891378B1 (en) * | 2008-08-27 | 2009-04-02 | (주)알앤이 | Recovering method of methyl methacrylate and alumina from waste artificial marvel |
| WO2013015676A3 (en) * | 2011-07-22 | 2013-04-25 | Bahar Bin Mohd Nor Shamsul | Thermal de-polymerization process of plastic waste materials |
| WO2013096815A1 (en) * | 2011-12-21 | 2013-06-27 | Swaminathan Ramesh | Method for recycling a plastic |
| WO2022220634A1 (en) * | 2021-04-16 | 2022-10-20 | 한국화학연구원 | Method for recovering styrene monomers from waste polystyrene |
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| KR19980013642A (en) * | 1996-08-01 | 1998-05-15 | 윤조희 | Method of recovering monomers and dimers from plastic by-products or waste plastics |
| JPH11246867A (en) * | 1998-03-03 | 1999-09-14 | Pipe Kankyo Service:Kk | Oil conversion from waste plastic mixture |
| JP2000191825A (en) * | 1998-12-25 | 2000-07-11 | San Kaihatsu Kk | Process for recovering styrene monomer from polystyrene resin waste |
| KR20010096422A (en) * | 2000-04-06 | 2001-11-07 | 사토 다투미 | Method for recovering styrene monomer from impact-resistant polystyrene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR19980013642A (en) * | 1996-08-01 | 1998-05-15 | 윤조희 | Method of recovering monomers and dimers from plastic by-products or waste plastics |
| JPH11246867A (en) * | 1998-03-03 | 1999-09-14 | Pipe Kankyo Service:Kk | Oil conversion from waste plastic mixture |
| JP2000191825A (en) * | 1998-12-25 | 2000-07-11 | San Kaihatsu Kk | Process for recovering styrene monomer from polystyrene resin waste |
| KR20010096422A (en) * | 2000-04-06 | 2001-11-07 | 사토 다투미 | Method for recovering styrene monomer from impact-resistant polystyrene |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100891378B1 (en) * | 2008-08-27 | 2009-04-02 | (주)알앤이 | Recovering method of methyl methacrylate and alumina from waste artificial marvel |
| WO2013015676A3 (en) * | 2011-07-22 | 2013-04-25 | Bahar Bin Mohd Nor Shamsul | Thermal de-polymerization process of plastic waste materials |
| WO2013096815A1 (en) * | 2011-12-21 | 2013-06-27 | Swaminathan Ramesh | Method for recycling a plastic |
| WO2013096794A1 (en) * | 2011-12-21 | 2013-06-27 | Swaminathan Ramesh | Catalyst for decomposing a plastic |
| US9802184B2 (en) | 2011-12-21 | 2017-10-31 | Swaminathan Ramesh | Method for recycling a plastic |
| WO2022220634A1 (en) * | 2021-04-16 | 2022-10-20 | 한국화학연구원 | Method for recovering styrene monomers from waste polystyrene |
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