KR20040036144A - Liquidizing Method of Waste Polyurethane Foam Members and Manufacturing Method of Said Members Using Said Liquidized Products - Google Patents
Liquidizing Method of Waste Polyurethane Foam Members and Manufacturing Method of Said Members Using Said Liquidized Products Download PDFInfo
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- KR20040036144A KR20040036144A KR1020020064957A KR20020064957A KR20040036144A KR 20040036144 A KR20040036144 A KR 20040036144A KR 1020020064957 A KR1020020064957 A KR 1020020064957A KR 20020064957 A KR20020064957 A KR 20020064957A KR 20040036144 A KR20040036144 A KR 20040036144A
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- 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
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/16—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with inorganic material
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- 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
- C08J9/33—Agglomerating foam fragments, e.g. waste foam
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- 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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- 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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
Description
본 발명은 폐기될 폴리우레탄 발포재의 액화방법 및 동 방법으로 액화된 발포재를 주성분으로 하는 폴리우레탄 발포재의 제조방법에 관한 것이다.The present invention relates to a method for liquefying a polyurethane foam to be discarded and a method for producing a polyurethane foam mainly composed of a foam material liquefied by the same method.
통상 폴리우레탄 발포재는 제조공정상 제품의 불량률이 5∼7% 정도 발생되고 있으며, 시중에 액자틀, 가구용 알판 등 넓은 용도로 사용되고 있다. 그러나 폴리우레탄 발포재는 열경화성 수지이기 때문에, 통상의 열가소성 수지와는 달리 열에 의해 녹는 것이 불가능하다. 따라서 이들을 폐기할 때에는 대부분의 플라스틱의 폐기처리와 같이 당국의 허가를 받아 소각처리 하거나 매립하고 있는 실정이다.In general, polyurethane foam materials have a defective rate of about 5 to 7% in the manufacturing process, and are widely used in a wide range of applications such as picture frames and furniture plates. However, since polyurethane foam is a thermosetting resin, it is impossible to melt | dissolve by heat unlike a normal thermoplastic resin. Therefore, when disposing of them, they are incinerated or landfilled with permission from the authorities, such as most plastics.
본 발명과 관련된 종래의 기술은 아직 보고된 바가 없으며, 이와 유사한 기술로는 본 발명자들이 개발한 액화목재 제조방법(특허 제 173442호)과 액화목재를 이용한 폴리우레탄 발포재 제조방법(특허 제 239218호)을 들 수 있다. 그러나 이 방법은 목재 및 목질재료를 원료로 하여 목재성분을 함유하는 폴리우레탄 발포재를 제조하는 기술이며, 폐기 또는 불량 폴리우레탄 발포재를 재활용하는 기술은 아니다.The prior art related to the present invention has not been reported yet, and similar techniques include the liquefied wood manufacturing method developed by the present inventors (Patent No. 173442) and the polyurethane foam manufacturing method using the liquefied wood (Patent 239218). ). However, this method is a technique for producing a polyurethane foam containing wood components from wood and wood materials as a raw material, not a technology for recycling waste or bad polyurethane foam.
현재 폴리우레탄 발포재의 폐기는 소각 또는 매립에 의한 처리에만 의존되고 있다. 그러나 소각 또는 매립 방법은 유해가스의 발생에 의한 대기오염이나, 토양 및 수질오염 등 환경오염의 원인이 되고 있다.At present, the disposal of polyurethane foam relies only on treatment by incineration or landfilling. However, incineration or landfill methods cause environmental pollution such as air pollution and soil and water pollution caused by the generation of harmful gases.
본 발명자는 상기한 종래 기술의 단점을 극복하기 위한 방안을 연구하여 오던 중 폐기될 폴리우레탄 발포재를 액화하고, 이를 종래 폴리우레탄 발포재의 원료가 되는 폴리올을 대체하는 경우 대체에 따른 원가절감효과는 물론 소각 또는 매립으로 인한 2차 오염을 방지하여 환경개선에 크게 기여할 수 있음을 발견하고서 본 발명을 완성하게 되었다.The present inventors liquefied the polyurethane foam to be discarded during the study to overcome the disadvantages of the prior art described above, the cost reduction effect of the replacement when replacing the polyol which is a raw material of the conventional polyurethane foam Of course, the present invention was completed by discovering that the secondary pollution due to incineration or landfill can greatly contribute to environmental improvement.
이에 본 발명의 목적은 폴리우레탄 발포재의 대체 원료로서 사용하기 위해 폐기될 폴리우레탄 발포재을 액화하는 방법을 제공함에 있다.It is therefore an object of the present invention to provide a method of liquefying polyurethane foam to be discarded for use as an alternative raw material of polyurethane foam.
본 발명의 다른 목적은 원가절감효과는 물론 소각 또는 매립으로 인한 2차 오염을 방지하기 위해 상기 액화된 폴리우레탄 발포재를 주성분으로 하는 폴리우레탄 발포재의 제조방법을 제공함에 있다.Another object of the present invention is to provide a method for producing a polyurethane foam containing the liquefied polyurethane foam as a main component to prevent secondary pollution due to incineration or landfill as well as a cost reduction effect.
도 1은 불량 또는 폐기되는 폴리우레탄 발포재를 액체화한 후 이를 원료로 제조된 재생 폴리우레탄 발포재1 is a recycled polyurethane foam made of a raw material after liquefying polyurethane foam that is defective or discarded
본 발명은 폐기되는 폴리우레탄 발포재의 액화방법으로서,The present invention is a method of liquefying the polyurethane foam to be discarded,
적당한 크기로 절단된 폴리우레탄발포재를 용매인 페놀, 프로필렌카보네이트, 또는 다가알콜에 투입하고 소정 촉매의 존재하에 100∼150℃에서 반응시켜 액화함을 특징으로 하는 폴리우레탄 발포재의 액화방법을 포함한다.Method for liquefying a polyurethane foam material characterized in that the polyurethane foam material cut to a suitable size is added to a solvent phenol, propylene carbonate or polyhydric alcohol and reacted at 100 to 150 ℃ in the presence of a predetermined catalyst to liquefy. .
상기 용매 중 다가알콜의 예로는 폴리에틸렌글리콜(바람직하게는 평균분자량 400~1,000), 에틸렌글리콜 등이 있으며 이들에 한정되는 것은 아니다.Examples of the polyhydric alcohol in the solvent include polyethylene glycol (preferably, the average molecular weight 400 ~ 1,000), ethylene glycol and the like, but is not limited thereto.
사용가능한 촉매로는 황산, 염산 등의 다양한 무기산 및 염화철 등이 있으나 바람직하게는 액화수율의 면에서 황산을 사용한다.Examples of the catalyst that can be used include various inorganic acids such as sulfuric acid and hydrochloric acid, and iron chloride. Preferably, sulfuric acid is used in terms of liquefaction yield.
상기 폐폴리우레탄발포재를 상기 선택된 용매 중에 바람직하기로 폐기폴리우레탄 발포재의 2~3배 중량의 용매를 투입하고 적량의 촉매(바람직하게는 용매 중량의 1~2%)를 가하여 100∼150℃하에 바람직하기로는 20분 이상, 보다 바람직하기로는 20∼40분 액화시켜 액화폴리우레탄발포재를 얻을 수 있다.The waste polyurethane foaming material is preferably in the selected solvent, and a solvent having 2-3 weights of the waste polyurethane foaming material is added thereto, and an appropriate amount of catalyst (preferably 1 to 2% of the weight of the solvent) is added to 100 to 150 ° C. It is preferably 20 minutes or more, more preferably 20 to 40 minutes to liquefy to obtain a liquefied polyurethane foaming material.
상기 반응을 위한 장치로는 스테인레스 용기에 의한 고압반응기 또는 환류냉각기가 부착된 반응기에 의한 상압반응기 등의 공지의 제조장치가 이용가능하다.As the apparatus for the reaction, a known production apparatus such as a high pressure reactor using a stainless vessel or an atmospheric pressure reactor using a reactor equipped with a reflux cooler may be used.
또한 본 발명은 폴리우레탄 발포재의 제조방법에 있어서,In addition, the present invention is a method for producing a polyurethane foam,
(a) 적당한 크기로 절단된 폐폴리우레탄발포재를 용매인 페놀, 프로필렌카보네이트, 또는 다가알콜에 투입하고 소정 촉매의 존재하에 100∼150℃에서 반응시켜액화하는 단계와,(a) injecting a waste polyurethane foam cut to a suitable size into a solvent phenol, propylene carbonate or polyhydric alcohol and reacted at 100 to 150 ℃ in the presence of a predetermined catalyst to liquefy;
(b) 전기 (a)단계의 액화된 발포재를 단독으로 또는 통상적인 폴리올을 소정비율로 혼합한 것에 통상적인 정포제, 발포촉매를 혼합하여 1차 교반하는 단계, 및(b) mixing the liquefied foamed material of step (a) alone or a conventional polyol in a predetermined ratio, followed by mixing the conventional foam stabilizer and the foaming catalyst with primary stirring, and
(c) 디이소시아네이트를 혼합하여 2차 교반하여 발포하는 단계를 포함함을 특징으로 하는 폴리우레탄 발포재의 제조방법을 포함한다.(c) mixing the diisocyanate, followed by foaming by secondary stirring.
상기 단계 (a)는 앞서 이미 설명한 바와 같다.Step (a) is as described above.
상기 단계 (b)는 액화된 발포재 단독 또는 발포재 원료로 사용되는 폴리올, 예를 들면 폴리프로필렌글리콜 등을 혼합하여 공지의 정포재, 예를 들면 실록산폴리옥시알킬렌코폴리머와 공지의 발포촉매로 예를 들면 1.4-디아자(2,2,2)비시클로옥탄 등을 적량 혼합하여 1차 교반하는 과정을 포함한다.Step (b) is a mixture of liquefied foam alone or a polyol used as a foam material, for example, polypropylene glycol, and the like to form a known foam stabilizer, for example, a siloxane polyoxyalkylene copolymer and a known foam catalyst. For example, 1.4-diaza (2,2,2) bicyclooctane etc. are mixed suitably, and the process of primary stirring is included.
상기 단계 (c)는 디이소시아네이트, 예를 들면 메틸렌디페닐디이소시아네이트(MDI)를 적량 혼합하여 2차 교반하여 발포하는 단계를 포함한다.The step (c) includes a step of mixing a suitable amount of diisocyanate, for example methylene diphenyl diisocyanate (MDI), followed by foaming by secondary stirring.
이하 본 발명의 내용을 실시예에 의해 보다 상세하게 설명하기로 한다. 다만 이들 실시예는 본 발명의 내용을 이해하기 위해 제시되는 것일 뿐 본 발명의 권리범위가 이들 실시예에 한정되어지는 것으로 해석되어져서는 아니된다.Hereinafter, the content of the present invention will be described in more detail with reference to Examples. However, these examples are only presented to understand the content of the present invention, and the scope of the present invention should not be construed as being limited to these embodiments.
<실시예 1><Example 1>
폴리우레탄 발포재 제조 공정에서 발생한 불량 폴리우레탄 발포재를 가로, 세로 및 높이가 약 20mm 정도가 되게 절단하였다(다만 절편의 크기는 액체화 작업에 용이하도록 당업자에 의해 적의 선택될 사항으로 특별한 한정을 요하지는 아니한다). 잘게 절단된 폴리우레탄 발포재 260g과 프로필렌카보네이트(BASF사, 끓는점 240~243℃) 520g 및 촉매로 염화철 20g(시약일급)을 환류냉각기와 온도계가 부착된 4ℓ용 삼구플라스크에 넣고 100℃에서 60분간 반응시켜 흑갈색의 액체를 얻었다. 그런 다음, 100메쉬의 그물에 통과시켜 폴리우레탄 발포재 액화물을 얻었으며 그 결과는 하기 표 1에 나타낸 바와 같다.The defective polyurethane foams generated in the polyurethane foam manufacturing process were cut to have a width, length, and height of about 20 mm. (However, the size of the sections is not limited to those selected by those skilled in the art to facilitate the liquefaction operation. Is not). 260 g of finely cut polyurethane foam, 520 g of propylene carbonate (BASF, boiling point 240 ~ 243 ℃) and 20g of iron chloride (catalyst grade) with catalyst are placed in a 4L three-necked flask equipped with reflux cooler and thermometer for 60 minutes at 100 ℃ The reaction was carried out to obtain a dark brown liquid. Then, it was passed through a mesh of 100 mesh to obtain a polyurethane foam liquefaction and the results are shown in Table 1 below.
<실시예 2><Example 2>
상기 실시예 1에서와 동일한 크기의 불량 폴리우레탄 발포재 350g과 프로필렌카보네이트 700g 및 촉매로 황산(시약일급) 10㎖를 환류냉각기와 온도계가 부착된 4ℓ용 삼구플라스크에 넣고 100℃에서 30분간 반응시켜 흑갈색의 액체를 얻었다. 그런 다음, 100메쉬의 그물에 통과시켜 폴리우레탄 발포재 액화물을 얻었으며 그 결과는 하기 표 1에 나타낸 바와 같다.350 g of poor polyurethane foam of the same size as in Example 1, 700 g of propylene carbonate, and 10 ml of sulfuric acid (reagent) were put into a 4 L three-necked flask equipped with a reflux cooler and a thermometer and reacted at 100 ° C. for 30 minutes. A dark brown liquid was obtained. Then, it was passed through a mesh of 100 mesh to obtain a polyurethane foam liquefaction and the results are shown in Table 1 below.
<실시예 3><Example 3>
상기 실시예 1에서와 동일한 크기의 불량 폴리우레탄 발포재 2g과 페놀 5㎖ 및 촉매로 황산(시약일급) 0.1㎖를 스테인레스 내압용기에 넣고 뚜껑을 닫은 후 150℃에서 30분간 반응시켜 흑갈색의 액체를 얻었다. G4 규격의 글래스필터로 상기 액체를 흡인 여과시켜 액상의 폴리우레탄발포재를 제조하였으며 그 결과는 하기 표 1에 나타낸 바와 같다.2 g of the poor polyurethane foam of the same size as in Example 1, 5 ml of phenol and 0.1 ml of sulfuric acid (reagent) were added to a stainless pressure vessel in a stainless pressure vessel, and the lid was reacted for 30 minutes at 150 ° C. to give a dark brown liquid. Got it. A liquid polyurethane foam was prepared by suction filtering the liquid with a glass filter of G4 standard, and the results are shown in Table 1 below.
<실시예 4><Example 4>
상기 실시예 1에서와 동일한 크기의 불량 폴리우레탄 발포재 2g과 폴리에틸렌글리콜(DAEJUNG, 분자량 400) 100g에 에틸렌글리콜(DAEJUNG) 50g의 비율로 혼합한 다가알콜류의 용매 6g 및 촉매로 황산(시약일급) 0.1㎖를 스테인레스 내압용기에 넣고 뚜껑을 닫은 후 150℃에서 40분간 반응시켜 흑갈색의 액체를 얻었다. G4 규격의 글래스필터로 상기 액체를 흡인 여과시켜 액상의 폴리우레탄발포재를 제조하였으며 그 결과는 하기 표 1에 나타낸 바와 같다.6 g of a solvent of polyhydric alcohols mixed with 2 g of a poor polyurethane foam having the same size as in Example 1 and 100 g of polyethylene glycol (DAEJUNG, molecular weight 400) at 50 g of ethylene glycol (DAEJUNG) and a sulfuric acid (reagent) 0.1 ml was put in a stainless pressure vessel, the lid was closed and reacted at 150 ° C. for 40 minutes to obtain a dark brown liquid. A liquid polyurethane foam was prepared by suction filtering the liquid with a glass filter of G4 standard, and the results are shown in Table 1 below.
<표 1>TABLE 1
*1 폐 PU : 폐기되는 폴리우레탄 발포재* 1 Waste PU: Polyurethane foam discarded
<실시예 5>Example 5
상기 실시예 1, 2, 3, 4의 방법에 의해 제조된 폴리우레탄 발포재의 액화물을 단독으로 또는 폴리우레탄 발포재 제조에 통상적으로 사용하는 폴리올을 적정비율 혼합하고, 통상의 폴리우레탄 발포재 제조에 사용하는 정포제와 발포촉매를 혼합한 후 1차 교반하였다. 이 혼합물에 MDI(메틸렌 디페닐 디이소시아네이트) 100 중량부를 혼합하여 2차 교반하여 발포시켰다. 혼합과 교반이 시작된 후 1분내에 수지화 공정이 종료되고 발포하기 시작하였다. 상세한 발포조건과 제조된 발포재의 밀도는 하기 표 2에 나타낸 바와 같으며, 이때 제조된 폴리우레탄발포재의 시제품은 도 1과 같다.The liquefaction of the polyurethane foam prepared by the method of Examples 1, 2, 3, and 4 alone or a polyol commonly used in polyurethane foam production is mixed in an appropriate ratio to prepare a normal polyurethane foam The foam stabilizer and foaming catalyst used in the above were mixed, followed by primary stirring. To this mixture, 100 parts by weight of MDI (methylene diphenyl diisocyanate) was mixed and foamed by second stirring. Within one minute after mixing and stirring began, the resination process was terminated and foaming began. Detailed foaming conditions and the density of the prepared foam is as shown in Table 2, wherein the prototype of the prepared polyurethane foam is shown in FIG.
<표 2>TABLE 2
* 1 폐 PU 액화물 : 페기되는 폴리우레탄 발포재의 액화물* 1 waste PU liquefaction: liquefaction of the polyurethane foam to be discarded
* 2 polyol : 폴리프로필렌글리콜* 2 polyol: polypropylene glycol
* 3 정포제 : 실록산폴리옥시알킬렌코폴리머* 3 foam stabilizer: siloxane polyoxyalkylene copolymer
* 4 촉매 : 1,4-디아자(2,2,2)비시클로옥탄(DABCO33-LV)* 4 catalyst: 1,4-diaza (2,2,2) bicyclooctane (DABCO33-LV)
* 5 MDI : 메틸렌 디페닐 디이소시아네이트* 5 MDI: methylene diphenyl diisocyanate
본 발명에 의하면 폐기될 폴리우레탄 발포재를 액화하여 통상적인 폴리우레탄발포재의 원료인 폴리프로필렌글리콜을 대체할 수 있을 뿐만 아니라, 폐자원을 활용하므로 소각이나 매립으로 인한 2차 오염을 방지할 수 있다.According to the present invention, the polyurethane foam to be disposed of can be liquefied to replace polypropylene glycol, which is a raw material of a conventional polyurethane foam, and waste resources can be used to prevent secondary pollution due to incineration or landfill. .
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Cited By (5)
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KR200449321Y1 (en) * | 2008-04-18 | 2010-06-30 | 김민성 | Helmet with goggle |
WO2014138827A1 (en) * | 2013-03-11 | 2014-09-18 | Vivan Gilceu Antonio | Method for manufacturing road signs from pressed polyurethane waste |
KR101583510B1 (en) * | 2014-10-22 | 2016-01-08 | 이성훈 | Blu mount apparatus |
JP2019510865A (en) * | 2016-04-05 | 2019-04-18 | コンポジット テック ホールディングス リミテッド | Recycling of polymer matrix composites |
KR102377611B1 (en) * | 2021-09-07 | 2022-03-22 | 동세철 | Manufacturing method for environment-friendly bio polyurethane resin of enhanced cold resistance synthesized with waste resin of the polyurethane fiber process and the bio polyurethane resin thereof |
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ZA875927B (en) * | 1986-08-27 | 1989-04-26 | Dow Chemical Co | Flexible polyurethane foams based on difunctional polyols and mdi and method for preparing the same |
KR0177154B1 (en) * | 1989-06-06 | 1999-05-15 | 야마구찌 도시아끼 | Process for producing rigid polyurethane foam |
DE3928330A1 (en) * | 1989-08-26 | 1991-02-28 | Bayer Ag | LIQUID POLYISOCYANATE MIXTURES, A METHOD FOR THE PRODUCTION THEREOF AND THEIR USE IN THE PRODUCTION OF POLYURETHANE FOAMS |
KR960005071B1 (en) * | 1992-11-25 | 1996-04-20 | 이대우 | Swelling liquid rubber on water |
JPH07126430A (en) * | 1993-10-29 | 1995-05-16 | Showa Highpolymer Co Ltd | Method for liquefying waste plastics |
WO1996005002A1 (en) * | 1994-08-15 | 1996-02-22 | Shinmaywa Industries, Ltd. | Heavy metal-containing waste treating process and apparatus |
KR19980032323A (en) * | 1996-10-08 | 1998-07-25 | 전종한 | Recycling method of waste rigid polyurethane foam and producing polyurethane foam with improved thermal insulation from recycled polyol obtained by this method |
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Cited By (6)
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KR200449321Y1 (en) * | 2008-04-18 | 2010-06-30 | 김민성 | Helmet with goggle |
WO2014138827A1 (en) * | 2013-03-11 | 2014-09-18 | Vivan Gilceu Antonio | Method for manufacturing road signs from pressed polyurethane waste |
KR101583510B1 (en) * | 2014-10-22 | 2016-01-08 | 이성훈 | Blu mount apparatus |
JP2019510865A (en) * | 2016-04-05 | 2019-04-18 | コンポジット テック ホールディングス リミテッド | Recycling of polymer matrix composites |
JP2022046640A (en) * | 2016-04-05 | 2022-03-23 | コンポジット テック ホールディングス リミテッド | Recycling of polymer matrix composite |
KR102377611B1 (en) * | 2021-09-07 | 2022-03-22 | 동세철 | Manufacturing method for environment-friendly bio polyurethane resin of enhanced cold resistance synthesized with waste resin of the polyurethane fiber process and the bio polyurethane resin thereof |
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