WO1995000582A1 - Procedes de recyclage des dechets de mousse de polystyrene - Google Patents
Procedes de recyclage des dechets de mousse de polystyrene Download PDFInfo
- Publication number
- WO1995000582A1 WO1995000582A1 PCT/CN1994/000051 CN9400051W WO9500582A1 WO 1995000582 A1 WO1995000582 A1 WO 1995000582A1 CN 9400051 W CN9400051 W CN 9400051W WO 9500582 A1 WO9500582 A1 WO 9500582A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- solvent
- polystyrene
- mixed solvent
- waste
- mixed
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/16—Making expandable particles
- C08J9/18—Making expandable particles by impregnating polymer particles with the blowing agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Definitions
- the invention relates to a method for recycling polystyrene foam plastic waste.
- the present invention relates to a method for recovering polystyrene foam plastic (PSF) waste by a gelation defoaming method, and then to preparing a modified polystyrene plastic (MP S) method or regenerating expandable polymer A method of styrene (EPS) beads and a mixed solvent used in the above method.
- PSF polystyrene foam plastic
- MP S modified polystyrene plastic
- EPS styrene
- thermoplastic method to recover PSF waste to produce recycled modified PS molding compounds includes the following three methods: namely, the method of hot-shaping granules after mechanical glass crushing, hot-pressing or 'hot-melt crushing, and modification aids.
- Agent hot-shaping granulation method and sol method after material extrusion and steam extrusion method can process PS F waste into molding compounds or modified molding compounds, there are certain shortcomings.
- the thermal shaping granulation method after mechanical crushing the specific gravity of the crushed material pile is too small, it is difficult to mix with the modified materials, and the equipment efficiency is very low; When heated, the resin is severely degraded by thermal oxygen and has low efficiency and large capacity during pre-heat pressing or hot-melt.
- the solvent such as banana water
- the solvent has too much volatility loss, is flammable, It is explosive, the on-site chemical is not safe, and the amount of solvent is up to 1.5-2 times the amount of PSF.
- the viscosity of the sol increases, and the rate of dissolved material decreases significantly. Due to the high viscosity of the resulting sol, handling was difficult.
- the above methods are not economically cost-effective to transport PS foam in long-distance fields.
- EPS is the original commodity form of PSF. Some people think that using PSF waste section to regenerate EPS is the best way to use waste PSF reasonably. For example, GB 1021250 uses waste PSF to substitute 30-50% styrene, dissolves in styrene for suspension polymerization, and makes EPS in one step. Alternatively, as described in GB 988, 289 and GB 988, 290, waste PSF is hot melted, defoamed, mechanically crushed, and shaped into pellets. The foaming agent is added to the autoclave with water as a dispersion medium, and EPS is produced in a two-step process.
- the two-step hot melt defoaming device has low efficiency, severe hot gas cracking, and deep product color.
- Proposed EPS regeneration method. (CN 91108317) The defoamer has a boiling point of ⁇ , which is too large, unsafe, and air-drying of pellets, which is not suitable for large-scale production; Chen Huaijiu, Wuhan University, etc.
- the developed method (Plastics Industry 1991, (2): 13) is to soften and break the PSF into beads' pellets, and directly mold it after adding a foaming agent.
- an object of the present invention is to provide a method for recycling polystyrene foam (PSF) waste.
- PSF polystyrene foam
- Another object of the present invention is to provide a method for preparing modified polystyrene by recycling polystyrene foam (PSF) waste.
- PSF polystyrene foam
- Another object of the present invention is to provide a polystyrene foam (P s ).
- Another object of the present invention is to provide a gelled mixed solvent used in a series of methods for recycling polystyrene foam (PSF) waste.
- PSF polystyrene foam
- the waste foam is treated with a high boiling point mixed solvent with less solvent volatilization and a small amount of use.
- the obtained gel mass is neither sticky to the hand nor the container, and is convenient and safe to handle.
- Solvents can be recovered through vacuum evaporation equipment known to those skilled in the art, and reused, which is economical. Summary of the Invention
- the present invention provides a more economical and reasonable method for recycling waste in situ to regenerate P S or MP S or regenerate E P S and a mixed solvent used in the recycling method.
- the key of this method is to take advantage of the gelation and defoaming phenomenon of PS waste in a high boiling point mixed solvent, and the resulting gel mass is not sticky to hands and containers, and is easy to handle.
- the recovered polystyrene gel material can not only directly collect the PS resin by recovering the solvent by evaporation under reduced pressure, but also can easily add various auxiliaries and easily stir and mix, and then remove the solvent to obtain MP S or follow the "two-step method" "Impregnated foaming agent to regenerate EPS.
- the gelled mixed solvent used in the present invention is less volatile and has a boiling point higher than 10o.
- C's hydrophobic organic solvent In essence, it is compounded with a good solvent of PS and a suitable amount of non-solvent of PS.
- the mixing ratio is not strictly regulated, and the criteria for smooth and defoaming the PSF gel are economical.
- the total amount of the good solvent in the gelled mixed solvent is usually 5-50%, preferably 30-50%, which is mainly determined by the operating temperature. When the operating temperature is low, the amount of good solvent should be appropriately increased, otherwise it can be appropriately reduced.
- the term "Gao boiling point" refers to a mixed solvent of gelling ioo e C higher than the boiling point of the hydrophobic organic solvent.
- Suitable good solvents in the present invention are: aromatic hydrocarbons, such as toluene, xylene, diethylbenzene, carbon decaaromatic oil, etc .; 3 ⁇ 4 aromatic hydrocarbons, such as chlorobenzene, o-difluorobenzene, etc .; esters, such as butyl acetate, pentyl acetate, etc. Esters, etc. as well as tar solvent oil, etc.
- Suitable non-solvents include alkanes, such as petroleum distillates above C8, various gasolines, solvent gasoline, kerosene, diesel, etc., and fermentations, such as isopropanol, n-butanol, and pentanolase.
- alkanes such as petroleum distillates above C8, various gasolines, solvent gasoline, kerosene, diesel, etc.
- fermentations such as isopropanol, n-butanol, and pentanolase.
- the invention relates to a method for recycling polystyrene foam (PSF) waste, which includes the following steps: adding polystyrene foam (PSF) waste to a boiling point higher than 100 "C
- the gelled mixed solvent is used in an amount sufficient to defoam the polystyrene foam (PSF) waste into a gel material, and generally 100 parts of polystyrene foam (PSF) is discarded. About 60 parts of the mixed solvent is obtained; the solvent is recovered through the desolventizing device; and polystyrene (PS) is obtained.
- the PSF waste is added to the high-boiling-point gelatinized mixed solvent prepared by the present invention to make it quickly Defoaming into a gelatinous material; the solvent will be recovered by a vacuum evaporation device known to those skilled in the art, such as a vented reel extruder; while recovering the mixed solvent, the pellets are thermoformed to obtain recycled polystyrene ⁇ PS pellets. If the original branch is relatively pure, the obtained pellets can be molded into transparent polystyrene products.
- the physical-chemical method of recovering the waste foam family is to use the gelation and defoaming phenomenon of P S F in a P S good solvent-non-solvent mixed solution.
- the mechanism is that PS is easily combined with the prepared gelled mixture to cause dissolution; ⁇
- the strength of the gel film is not sufficient to withstand the combined force of the surface tension of the gel film, the buoyancy of the bubble, and the mechanical squeeze force At this time, the gel film will break and defoam to form a gel mass.
- the remaining gelled mixed waves still maintain easy flow dynamics, and it is easy to continue to play the role of gelling and defoaming.
- modified resin and additives before hot shaping the pellets, and then recover the mixed solvent through multi-stage flash evaporation while thermoforming.
- the modified polystyrene (MPS) finished product is obtained by discharging, cooling, pelletizing and packaging.
- the recovered solvent can be recycled for gelation, defoaming and recovery of PS foam.
- the resins used for toughening and modification are various styrene-butadiene copolymers, such as SB, SBS, MB S, and styrene-butadiene rubber, and the amount is 5-20%.
- the conditions for desolvothermal shaping granules are: operating temperature is 15 0 3 0 0 C, operating residual pressure is 7 6 0 -2 0 Torr.
- the regenerated PS prepared by the method of the present invention can be further impregnated with a foaming agent to regenerate expandable polystyrene (EPS).
- EPS expandable polystyrene
- the PS pellets are coarsely crushed and sieved and dispersed in water according to conventional methods.
- the material is cooled, discharged, rinsed, and drained to obtain recycled EPS bead pellets.
- Such Tu EPS granules according to conventional methods and pre-expanded molded work force mouth c
- the quality of the recycled waste produced by this legal system is not particularly strict, and waste can be used in a wider range.
- foamed plastic products for different purposes can be made, such as sandwich panels, buoys, life-saving appliances, insulation, insulation materials or packaging materials. Larger specific gravity can also be used as the ground material branch of cold storage.
- the liquid foaming agent for EPS is C 3 -C 6 alkanes or
- the amount is 3 "15% by weight.
- flame retardants can be added to make flame retardant Variety.
- Commonly used flame retardants are pentabromo-chlorocyclohexane, hexabromocyclododecane, and other brominated flame retardants such as tribromophenol, tetrabromobisphenol A, pentabromophenyl, decabromodiphenyl ether, etc.
- antimony trihalide, aluminum hydride, thorium hydride and the like can be added. Dosage is generally ⁇ 35% by weight.
- the method for modifying the recovered polystyrene (PS) described above includes the following sequential steps:
- the polystyrene foam plastic (PSF) waste is mixed with a gelling mixed solvent with a boiling point higher than 1.0 ⁇ 0 "(gelation mixed solvent) to defoam the polystyrene foamed plastic (PSF) waste into a gel material.
- the gelled mixed solvent is substantially prepared by using a good solvent of polystyrene (PS) and a non-solvent of polystyrene (PS) in proportion, and the total amount of the good solvent is mixed according to the mixing.
- Total solvent volume is 5-50%; 5 "20% toughened modified resin is added to said polystyrene gelatin; the solvent is recovered through a solvent removal device; and modified polystyrene (MPS) is obtained.
- the method for recovering polystyrene (PS) to regenerate expandable polystyrene (EPS) in the present invention includes the following sequential steps:
- the polystyrene foamed plastic (PSF) waste is mixed with a boiling point higher than 100 ° (: a gelling mixed solvent) to defoam the polystyrene foamed plastic (PSF) waste into a gel material.
- the gelled mixed solvent is substantially prepared by using a good solvent of polystyrene (PS) and a non-solvent of polystyrene (PS) in proportion, wherein the total amount of the good solvent is mixed according to the mixing Total solvent volume is 5-50%;
- an alkane having a liquid foaming agent of C 3 -C 6 or a substituted alkane having a boiling point of ⁇ 60 (inclusive) is used in an amount of 3 to 15% of the total weight of the polystyrene. .
- an alkane having a liquid foaming agent of C 3 -C 6 or a substituted alkane having a boiling point of ⁇ 60 (inclusive) is used in an amount of 3 to 15% of the total weight of the polystyrene. .
- 1 3 0 -1 4 0 “(heating and stirring in an aqueous medium to spheroidize to obtain expandable polystyrene beads.
- Example 3 Take 8 mL of n-octane and 2 mL of xylene and mix according to the method described in Example 1. A mixed solvent is obtained. 12.5 g of PSF is added in less than 5 minutes to obtain 19.8 g of gel. The combined latent capacity was 5 8% and the solvent loss rate was 0.8%.
- Example 3 Take 8 mL of n-octane and 2 mL of xylene and mix according to the method described in Example 1. A mixed solvent is obtained. 12.5 g of PSF is added in less than 5 minutes to obtain 19.8 g of gel. The combined latent capacity was 5 8% and the solvent loss rate was 0.8%.
- Example 3 Take 8 mL of n-octane and 2 mL of xylene and mix according to the method described in Example 1. A mixed solvent is obtained. 12.5 g of PSF is added in less than 5 minutes to obtain 19.8 g of gel. The combined latent capacity was 5 8% and the solvent loss rate was 0.8%.
- Blend a xylene-kerosene mixed solvent When the xylene content reaches 30% (V / V), the PS F slowly defoams when the operating temperature is only 10'C. Conversely, when xylene The total amount is only 10%, and when the operating temperature is 4 5 'C, the PSF gel can be defoamed slowly.
- Granular melt flow index 34.9g / 10min (200.C 500g)
- the used PSF waste cannot be contaminated with a large amount of oil (for example, a convenient lunch box without removing oil). It was plugged into the recovered light-colored mixed solvent, and the gel mass obtained by gelation and defoaming was sent to a steam-extracting twin-screw extruder, and the material was made under reduced pressure (feed end 180, 101 KPa; End 2 8 0 e C, 2.00 KPa), while recovering the solvent. The obtained granules are coarsely crushed and sieved by a shearing plastic pulverizer.
- 1 cubic meter of gelled mixed solvent can make 1 ton of PSF discarded.
- the material is transformed into a gel mass, that is, the aggregate of 80 to 100 cubic meters of waste foam can be reduced to a gel mass of 2 cubic meters.
- the mixed solvent used is less volatile, so that it can be used to secure materials at the site of waste foam accumulation, which solves the problem of low transportation efficiency.
- the obtained gel material is non-stick, easy to work, and suitable for large-tonnage production.
- this solution is also conducive to ensuring quality.
- the toughened PS plastic that is recycled and recycled is easy to be colored, or at the same time, it can be filled and modified, and flame retardant modified.
- the obtained plastic is not only suitable for making stationery, toys, and various daily necessities, but also can be used for molding various electronic and electrical parts.
- the method according to the present invention requires neither mechanical equipment nor energy, and can defoam the foam waste at any time and place, so that the volume is reduced to 1/50-1 0 0 of the original deposit, which is fundamentally solved. Difficulty in collecting and transporting foam waste; this method also avoids thermal degradation of hot melt defoaming, and the recovered product is light in color and high in quality.
- the method of the invention not only solves the problems of collection and transportation of dispersed wastes, but also can regenerate MPS or EPS at the same time, turning waste into treasure, which not only has the social benefits of treating environmental pollution, but also has a high cost due to the value of recycled products. Lower, has very significant economic benefits.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP50229895A JPH09503235A (ja) | 1993-06-24 | 1994-06-24 | ポリスチレン発泡プラスチック廃棄物の回収利用方法 |
AU69934/94A AU6993494A (en) | 1993-06-24 | 1994-06-24 | Processes for recycling waste polystyrene foam |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN93111865A CN1096735A (zh) | 1993-06-24 | 1993-06-24 | 凝胶化脱泡法回收聚苯乙烯废泡料制改性聚苯乙烯塑料 |
CN93111865.4 | 1993-12-17 | ||
CN93115420A CN1103874A (zh) | 1993-12-17 | 1993-12-17 | 凝胶化脱泡法回收聚苯乙烯废泡料再生可发性聚苯乙烯 |
CN93115420.0 | 1993-12-17 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1995000582A1 true WO1995000582A1 (fr) | 1995-01-05 |
Family
ID=25743089
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/CN1994/000051 WO1995000582A1 (fr) | 1993-06-24 | 1994-06-24 | Procedes de recyclage des dechets de mousse de polystyrene |
Country Status (3)
Country | Link |
---|---|
JP (1) | JPH09503235A (fr) |
AU (1) | AU6993494A (fr) |
WO (1) | WO1995000582A1 (fr) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5859072A (en) * | 1995-05-15 | 1999-01-12 | Seiken Chemical Co., Ltd. | Process for treating expanded polystyrene |
AU2001260362B2 (en) * | 2000-05-15 | 2005-07-14 | M-I Finland Oy | A drag reducing composition |
CN108484961A (zh) * | 2018-05-04 | 2018-09-04 | 林宗平 | 一种利用回收聚苯乙烯制品制造可发性聚苯乙烯的方法 |
US11407878B2 (en) | 2014-10-03 | 2022-08-09 | Polystyvert Inc. | Processes for recycling polystyrene waste |
US11407877B2 (en) | 2018-10-26 | 2022-08-09 | Polystvert Inc. | Processes for recycling polystyrene waste and/or polystyrene copolymer waste |
CN115889427A (zh) * | 2022-11-01 | 2023-04-04 | 上海睿聚环保科技有限公司 | 一种废弃pa66安全气囊的回收利用方法 |
US11680149B2 (en) | 2017-11-20 | 2023-06-20 | Polystyvert Inc. | Processes for recycling polystyrene waste |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001302843A (ja) * | 1999-10-15 | 2001-10-31 | Tamotsu Akita | 発泡スチロール処理用溶剤及びこれを用いた発泡スチロールの処理方法 |
AU2002349608A1 (en) | 2002-05-14 | 2003-11-11 | Shigenobu Hamano | Solvent for treating polystyrene resin and method of treating polystyrene resin with the same |
JP4774293B2 (ja) * | 2005-12-21 | 2011-09-14 | 積水化成品工業株式会社 | スチレン系樹脂発泡性粒子とその製造方法及び型内発泡成形品 |
KR101476674B1 (ko) * | 2013-07-12 | 2014-12-26 | 최성진 | 발포 폴리스티렌 감용제 조성물 |
JP2016010906A (ja) * | 2014-06-27 | 2016-01-21 | サンライフ株式会社 | 発泡ポリスチレンからの難燃剤の除去方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1030431A (zh) * | 1987-07-04 | 1989-01-18 | 李华鼎 | 用废聚苯乙烯泡沫生产涂饰剂 |
CN1060298A (zh) * | 1990-09-29 | 1992-04-15 | 化学工业部晨光化工研究院一分院 | 一步法聚甲醛熔融后处理工艺 |
CN1061228A (zh) * | 1991-10-15 | 1992-05-20 | 化工部成都有机硅应用研究技术服务中心 | 再生可发性聚苯乙烯制法 |
CN1072704A (zh) * | 1991-11-23 | 1993-06-02 | 刘贞秋 | 聚苯乙烯废弃物树脂漆及生产方法 |
-
1994
- 1994-06-24 AU AU69934/94A patent/AU6993494A/en not_active Abandoned
- 1994-06-24 WO PCT/CN1994/000051 patent/WO1995000582A1/fr active Application Filing
- 1994-06-24 JP JP50229895A patent/JPH09503235A/ja not_active Expired - Lifetime
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1030431A (zh) * | 1987-07-04 | 1989-01-18 | 李华鼎 | 用废聚苯乙烯泡沫生产涂饰剂 |
CN1060298A (zh) * | 1990-09-29 | 1992-04-15 | 化学工业部晨光化工研究院一分院 | 一步法聚甲醛熔融后处理工艺 |
CN1061228A (zh) * | 1991-10-15 | 1992-05-20 | 化工部成都有机硅应用研究技术服务中心 | 再生可发性聚苯乙烯制法 |
CN1072704A (zh) * | 1991-11-23 | 1993-06-02 | 刘贞秋 | 聚苯乙烯废弃物树脂漆及生产方法 |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5859072A (en) * | 1995-05-15 | 1999-01-12 | Seiken Chemical Co., Ltd. | Process for treating expanded polystyrene |
AU2001260362B2 (en) * | 2000-05-15 | 2005-07-14 | M-I Finland Oy | A drag reducing composition |
US11407878B2 (en) | 2014-10-03 | 2022-08-09 | Polystyvert Inc. | Processes for recycling polystyrene waste |
US11680149B2 (en) | 2017-11-20 | 2023-06-20 | Polystyvert Inc. | Processes for recycling polystyrene waste |
CN108484961A (zh) * | 2018-05-04 | 2018-09-04 | 林宗平 | 一种利用回收聚苯乙烯制品制造可发性聚苯乙烯的方法 |
US11407877B2 (en) | 2018-10-26 | 2022-08-09 | Polystvert Inc. | Processes for recycling polystyrene waste and/or polystyrene copolymer waste |
EP4245779A3 (fr) * | 2018-10-26 | 2023-10-25 | Polystyvert Inc. | Procédés de recyclage de déchets de polystyrène et/ou de déchets de copolymère de polystyrène |
US12018132B2 (en) | 2018-10-26 | 2024-06-25 | Polystyvert Inc. | Processes for recycling polystyrene waste and/or polystyrene copolymer waste |
CN115889427A (zh) * | 2022-11-01 | 2023-04-04 | 上海睿聚环保科技有限公司 | 一种废弃pa66安全气囊的回收利用方法 |
Also Published As
Publication number | Publication date |
---|---|
AU6993494A (en) | 1995-01-17 |
JPH09503235A (ja) | 1997-03-31 |
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