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KR930008925B1 - 형상기억 중합발포체 - Google Patents

형상기억 중합발포체 Download PDF

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KR930008925B1
KR930008925B1 KR1019890014058A KR890014058A KR930008925B1 KR 930008925 B1 KR930008925 B1 KR 930008925B1 KR 1019890014058 A KR1019890014058 A KR 1019890014058A KR 890014058 A KR890014058 A KR 890014058A KR 930008925 B1 KR930008925 B1 KR 930008925B1
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polymer
glass transition
transition point
foam
shape
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슝이찌 하야시
히로시 후지무라
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미쯔비시주우고오교오 가부시기가이샤
우에다 쇼오지
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
    • C08F299/02—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
    • C08F299/06—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates from polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
    • B29C44/34—Auxiliary operations
    • B29C44/56—After-treatment of articles, e.g. for altering the shape
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C61/00—Shaping by liberation of internal stresses; Making preforms having internal stresses; Apparatus therefor
    • B29C61/003—Shaping by liberation of internal stresses; Making preforms having internal stresses; Apparatus therefor characterised by the choice of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2075/00—Use of PU, i.e. polyureas or polyurethanes or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/04—Condition, form or state of moulded material or of the material to be shaped cellular or porous
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00—Foam properties
    • C08G2110/0008—Foam properties flexible
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2250/00—Compositions for preparing crystalline polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2280/00—Compositions for creating shape memory

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Shaping By String And By Release Of Stress In Plastics And The Like (AREA)

Abstract

내용 없음.

Description

형상기억 중합발포체
본 발명은, 형상기억성을 가진 중합발포체에 관한 것이다.
종래, 내부에 기포구조조직을 가진 폴리우레탄포옴으로 대표되는 중합발포체는, 탄력성, 단열성등의 포옴 특유의 성질을 이용한 여러가지의 제품이 시판되고 있다. 이들 포옴은 현장시공의 경우를 제외하고, 미리, 일정한 형상으로 성형된 포옴을, 그대로의 형상으로 사용에 제공되어 왔다.
한편, 통상의 중합성형체중에는, 성형형상과 변형형상을 온도조작으로 구분해서 쓰는 형상기억 중합성형체가 제안되고 있다.
형상기억 중합성형체는, 중합체의 유리전이점이상, 성형온도미만의 온도로 변형을 가하고, 그 형상을 유지한 상태에서 유리전이점 이하까지 냉각하므로서, 변형형상을 고정하고, 또, 유리전이점 이상에서 성형온도미만의 온도로 가열하므로서 원래의 성형형상을 회복하는 것으로서, 온도조작에 의해 변형형상과 성형형상을 구분해서 쓸수 있는 것이다.
그런데, 중합발포체는, 내부에 대량의 기포를 가지고 있기 때문에, 중량에 대해서 체적이 매우 크고, 예를들면, 공장에서 발포체를 제조하여 사용현장으로 반송할 경우에는, 그 체적이 반송의 지장으로 된다. 이와 같은 경우에는, 반송시에는 작은 체적으로 되고, 사용시에는 소정의 크기의 본래의 발포체를 얻을 수 있게 되면 매우 유효하다.
그러나, 이와 같은 변형형상과 성형형상을 그 용도에 따라서 구분해서 사용할 수 있는 형상기억 중합발포체는, 아직, 제안되어 있지 않았다.
본 발명은, 이와 같은 형상기억성을 구비한 중합발포체를 제공할려고 하는 것이다.
본 발명은, 중합체의 유리전이점이상에서 압축변형시킨 발포체를 유리전이점이하에서 고정하여 얻는 변형형상과, 다시 유리전이점이상의 온도로 승온해서 당초의 형상으로 복귀시킨 성형형상을 취할 수 있는 형상기억 중합발포체이다.
본 발명의 형상기억 중합발포체는, 종래의 발포성형체의 형상이외에, 압축변형 고정한 제 2의 형상을 취할 수 있다. 특히, 개방기포구조조직을 가진 중합발포체에 있어서는, 내부기포를 배출해서 비교적 작은 힘으로 큰 변형을 가져올 수 있게 할 수 있다. 또, 독립기포구조조직을 가진 중합발포체에 있어서는, 기포내의 기체를 압축해서 변형고정하면, 형상 회복시에 기체가 팽창하기 때문에 회복속도를 비약적으로 빠르게 할 수 있게 된다. 그리고, 이 2개의 형상에 있어서, 탄성율을 비롯한 여러가지의 물성을 선택할 수 있다.
이와 같이, 2개의 형상 및 그 형상에 있어서의 물성을 구분해서 쓰므로서, 형상기억 중합발포체를 여러가지의 용도에 적용할 수 있다. 특히, 중합체의 유리전이점을 실온 부근에 설정한 발포체에 대해서는, 가까운 가열수단, 예를들면, 드라이어등을 사용해서, 사용자가 좋아하는 형상으로 수시 간단하게 변형고정시킬 수 있다.
본 발명의 발포체에 사용할 수 있는 중합체로서는, 우레탄계중합체, 스티렌-부타디엔계중합체, 결정성디엔계중합체, 노르보르난계중합체 등을 들 수 있다. 그중에서도, 2관능의 디이소시아네이트, 2관능의 폴리올 및 활성수소기를 함유하는 2관능의 사슬연장제를 몰비로 2.00~1.10 : 1.00 : 1.00~0.10, 바람직하게는, 1.80~1.20 : 1.00 : 0.80~0.20으로 배합하고, 발포제를 첨가하여 프로폴리머법에 의해 합성한 폴리우레탄발포체로서, 중합체의 말단에는 [NCO]와 [OH]를 거의 등량 함유하고, -50~60℃의 범위의 유리전이점 및 3~50중량%의 결정화도를 가진 형상기억 중합발포체가 바람직하다.
이 중합체는, 말단에 잉여의 [NCO]를 실질적으로 함유하지 않으므로, 강직한 가교를 형성하는 앨러페네이트결합을 억제할 수 있어, 가공성의 자유도를 가진 가소성사슬형상 중합체를 얻을 수 있다. 또, 알맞는 정도의 결정화도를 부여하므로서, 이 사슬형상중합체에 대해서 필요로 하게 되는 탄성율을 부여할 수 있다.
여기서, 결정화도는 3~50중량%의 범위에 있는 것이 바람직하다. 결정화도를 3중량% 이하로 하면 유리전이점이상의 온도에서 고무탄성이 작아지고, 결정화도를 50중량% 이상으로 하면 유리전이점이상의 온도에서 고무탄성이 높아져서, 유리전이점전후 ±10℃의 온도에서의 탄성율의 비가 작아진다.
이 중합체에 사용가능한 원료를 다음에 예시하나, 이에 한정되는 것은 아니다.
먼저, 2관능의 이소시아네이트의 예로서는, 일반식으로 OCN-R-NCO로 표기할 수 있으며, R에는 벤젠고리를 1, 2개 가진 것과 전혀 가지고 있지 않는 것이 있으나, 모두 사용가능하며, 구체적으로는, 2,4-톨루엔디이소시아네이트, 4,4'-디페닐메탄디이소시아네이트, 카르보디이미드변성, 4,4'-디페닐메탄디이소시아네이트, 헥사메틸렌디이소시아네이트등을 들 수 있다.
2관능의 폴리올의 예로서는, 일반식으로 OH-R'-OH로 표기할 수 있으며, R'에는 벤젠고리를 1, 2개 가진 것과 전혀 가지고 있지 않는 것, 또는 상기 2관능의 폴리올에 2관능의 카르복시산 또는 고리형상에테르를 반응시킨 생성물등, 모두 사용가능하며, 구체적으로는, 폴리프로필렌글리콜, 1,4-부탄글리콜아디페이트, 폴리테트라메틸렌글리콜, 폴리에틸렌글리콜, 비스페놀-A＋프로필렌옥시드등을 들수 있다.
활성수소기를 함유한 2관능의 사슬연장제의 예로서는, 일반식으로 OH-R"-OH로 표기할 수 있으며, R"에는 (CH2)n기, 벤젠고리를, 1, 2개 가진 기등, 모두 사용가능하며, 구체적으로는, 에틸렌글리콜, 1,4-부탄글리콜 비스(2-히드록시에틸)히드로퀴논, 비스페놀-A＋에틸렌옥시드, 비스페놀-A＋프로필렌옥시드등을 들 수 있다.
이들 원료로부터 합성한 폴리우레탄 탄성중합체는, 일반식으로 다음과 같이 표기할 수 있다.
HOR"OCONH(RNHCOOR'OCONH)nRNHCOOR"OCONH-(RNHCOOROCONH)mRNHCOOR"OH
m=1~16, n=0~16.
발포방법은, 종래의 프레폴리머를 거쳐서 발포시키는 콘벤셔널법, 프로드(froth)법등을 사용할 수 있다.
발포제는, 화학적인 분해에 의해서 가스를 발생하는 분해형발포제와, 화학적변화없이도 휘발하는 증발형 발포제가 있으며, 모두 사용할 수 있다. 분해형발포제로서는, 중탄산나트륨, 탄산암모늄, 중탄산암모늄, 아질산암모늄, 아지드화합물, 붕수소화나트륨, 물과 반응해서 수소를 발생하는 경금속등의 무기계발포제, 및 트리클로로모노플로로메탄, 트리클로로트리플로로에탄, 염화메틸렌, 아조디카르본아미드, 아조비스포름아미드, N,N'-디니트로소펜타메틸렌테트라민등의 유기계발포제를 들 수 있다. 또, 증발형발포제로서는, 압축질소가스, 트리클로로모노플루오로메탄등을 들 수 있다.
[실시예]
이소시아네이트성분과 폴리올성분을 제 1 표에 기재한 바와 같이 배합하여, 무촉매로 반응시켜서 프레폴리머를 합성하고, 이어서, 사슬연장제 및 발포제를 제 1 표의 배합으로 첨가하여, 가열하므로서 큐어링을 실시하고, 현상기억폴리우레탄포옴을 얻었다. 발포제는 트리클로로모노플로로메탄(비등점 23.8℃)을 폴리우레탄 100부에 대해서 20부 배합하였다.
이 폴리우레탄포옴은, 20배로 팽창되어 있으며, 기본적물성은 제 1 표와 같다. 표중의 Tg는, 유리전이점(℃)를 표시한다. 결정화도(중량%)는, X선회절법에 의해 측정하였다.
다음에, 내경 15cm의 좁은 부분과 외경 10cm의 배관사이에 제 1 표의 예 38의 폴리우레탄포옴의 단열재를 시공하는 실험을 행하였다. 배관의 외경보다 약간 작은 내경 9.5cm이고, 두께 4cm의 원통형상의 폴리우레탄포옴을 준비하고, 그속에 배관을 삽입한 다음에, 폴리우레탄포옴을 약 50℃로 가열해서 외부로부터 압력을 가하고, 단열재의 직경을 12cm로 유지하면서, 실온까지 냉각하여 그대로 고정하였다. 이 배관을 좁은 부분에 삽입하고, 배관내부에 약 50℃의 가열가스를 보내어, 단열재를 원래의 형상으로 복귀시켰다. 이 결과, 폴리우레탄포옴의 탄성력에 의해, 단열재는 좁은 부분과 완전히 밀착하고, 배관을 좁은 부분내에 지지할 수 있었다.
[표 1]
Figure kpo00001
[표 1 (계속)]
Figure kpo00002
본 발명은, 상기 구성을 채용하므로서, 성형형상외에, 소정의 변형형상을 취할 수 있고, 간단한 가열조작에 의해, 성형형상으로 복귀시킬 수 있다. 특히, 형상기억 중합발포체에 개방기포를 내포시킬때에는, 작은 압력으로 큰 변형을 가져오게 할 수 있으므로, 큰 변형량과 그 사이의 물성의 변화를 활용해서 폭넓게 이용할 수 있다. 또, 독립기포를 내포시킨 형상기억 중합발포체는, 변형시에 기포내의 가스를 압축해서 고정하므로서, 형상회복속도를 높일 수 있어, 뛰어난 회복동작성을 활용할 수도 있다.

Claims (2)

  1. 중합체의 유리전이점이상에서 압축변형시킨 중합체 발포체를 유리전이점이하에서 고정해서 얻는 변형형상과, 압축된 중합체 발초체를 다시 유리전이점이상의 온도로 승온해서 당초의 형상으로 복귀시킨 성형형상을 취할 수 있는 형상기억 폴리우레탄 중합발포체.
  2. 제 1 항에 있어서, 2,4-톨루엔디이소시아네이트, 4,4'-디페닐메탄디이소시아네이트, 카르보디이미드변성 4,4-디페닐메탄디이소시아네이트, 헥사메틸렌디이소시아네이트로 이루어진 군에서 선택된 2관능의 이소시아네이트, 폴리프로필렌글리콜, 1,4-부탄글리콜아디페이트, 폴리테트라메틸렌글리콜, 폴리에틸렌글리콜, 비스페놀-A＋프로필렌옥시드로 이루어지는 군에서 선택된 2관능의 폴리올, 및, 에틸렌글리콜, 1,4-부탄글리콜 비스(2-히드록시에틸)히드로퀴논, 비스페놀-A＋에틸렌옥시드, 비스페놀-A＋프로필렌옥시드로 이루어지는 군에서 선택된 활성수소기를 함유한 2관능의 사슬연장제를 몰비로 2.00~1.10 : 1.00 : 1.00~0.10로 배합하고, 발포제를 첨가해서 프레폴리머법에 의해 합성한 폴리우레탄 발포체로서, 중합체의 말단에는 [NCO]와 [OH]를 등량 함유하고, -50~60℃의 범위의 유리전이점 및 3~50중량%의 결정화도를 가진 것을 특징으로 하는 형상기억 폴리우레탄 중합발포체.
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EP0361418A2 (en) 1990-04-04
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KR900004789A (ko) 1990-04-13
DE68920247T2 (de) 1995-05-04
DE68920247T3 (de) 1999-03-25
JPH0739506B2 (ja) 1995-05-01
CA1319238C (en) 1993-06-22
US5049591A (en) 1991-09-17
DE68920247D1 (de) 1995-02-09
EP0361418A3 (en) 1991-08-28
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