KR100256634B1 - 충전 화합물 - Google Patents

충전 화합물 Download PDF

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KR100256634B1
KR100256634B1 KR1019940701542A KR19940701542A KR100256634B1 KR 100256634 B1 KR100256634 B1 KR 100256634B1 KR 1019940701542 A KR1019940701542 A KR 1019940701542A KR 19940701542 A KR19940701542 A KR 19940701542A KR 100256634 B1 KR100256634 B1 KR 100256634B1
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South Korea
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compound according
weight
filling
star
filling compound
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KR1019940701542A
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English (en)
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라이마르휴크터
위르겐켈하우스
요한네스안드레스
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한스 크리스토프 빌크, 미하엘 베르크만
헨켈 코만디트게젤샤프트 아우프 악티엔
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Application filed by 한스 크리스토프 빌크, 미하엘 베르크만, 헨켈 코만디트게젤샤프트 아우프 악티엔 filed Critical 한스 크리스토프 빌크, 미하엘 베르크만
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
    • H01B7/28—Protection against damage caused by moisture, corrosion, chemical attack or weather
    • H01B7/282—Preventing penetration of fluid, e.g. water or humidity, into conductor or cable
    • H01B7/285—Preventing penetration of fluid, e.g. water or humidity, into conductor or cable by completely or partially filling interstices in the cable
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract

본 발명은 방사상 물질을 함유함을 특징으로 하는 케이블, 스트립, 플러그 등과 같은 전기 및 광학 장치용 충진제에 관한 것이다. 특히, 올리고머화도가 3이상인 올리고-데세-1-엔을 함유한다. 여기에 미세 규산 및 고분자량 폴리올레핀 또는 수화 폴리이소프렌과 같은 점도 향상제를 가한다면 -50℃에서 원뿔형 투과성 및 80℃이하에서의 유동내성과 같은 열적 특성이 향상된 충진 화합물을 수득할 수 있다.

Description

충전 화합물
본 발명은 케이블, 커넥터, 플러그 등의 형태의 전기 및 광학 장치용 충전 화합물, 및 이렇게 제조된 어셈블리에 관한 것이다.
케이블, 커넥터, 플러그 등의 형태의 전기 및 광학 장치는 외부로부터 침투되는 해로운 영향, 특히 물, 및 설치 동안 또는 열에 노출된 결과인 기계적 손상에 대하여 보호되어야 한다. 이는 일정 지점에 침투된 수분이 퍼져 전선의 성능에 악영향을 미치기 때문이다. 이러한 문제점은 공지되어 있으며 이를 해결하기 위한 여러 가지 방법이 이미 제안되어 있다. 즉, EP 0 206 234-B1호에는 65~90중량％의 광물유, 2~25중량％의 유기증점제, 더욱 구체적으로는 폴리-α-올레핀, 2~10중량％의 고분산성 실리카, 및 임의로 0.2~10중량％의 중공성 미세 비드 및 0.1~5중량％의 분산제로 구성된 충전 화합물이 기재되어 있다. 실제로 동일한 조성물이 FR-PS 2 644 004호에 기재되어 있다.
상기 조성물이 성능 및 가공성의 면에서 케이블 산업의 엄격한 필요조건을 만족시킬 수 있지만, 더욱 더 엄격한 필수 조건이, 특히 가혹한 온도영향과 관련된 조건이, 특정한 분야에 요구되고 있다. 즉, 한편으로는 충전 화합물은 초저온에서도 유연성이 있어야 하며, 다른 한편으로는 초고온에서도 유동되지 않아야 한다. 또한, 충전 화합물은 인화점이 높아야 한다.
케이블, 커넥터, 플러그 등의 형태의 전기 및 광학 장치용 충전 화합물에 일반적으로 기대되는 다른 요구 조건도 역시 만족시켜야 한다. 관련된 특정 분야에 따라, 이러한 다른 요구 조건은 예를 들면 하기에 관한 것일 수 있다.
-유전 상수
-유전 강도
-저항율
-주위 물질에 의한 충전제 흡수도
-물(증기) 침투도
따라서, 본 발명의 목적은 극한 온도에서 향상된 특성을 나타내나, 통상적인 필요 조건을 여전히 만족시키며, 특히 가공이 용이한 충전 화합물을 제공하는 것이다.
본 발명에 의해 제공된 상기 과제에 대한 해결책은 청구범위에 기재되어 있고, 충전 화합물의 기재로서 성상(星狀) 물질(stellate substance)의 선택하는 것이 필수적이다.
본 명세서에서, "성상(星狀) 물질"은 이상적으로 3이상의 분지, 더욱 구체적으로 고분자 중합성 사슬, 예를 들면 HC-(CH2-O-CO-CaH19)3이 단일의 분지점에서 방사상으로 뻗어있는 분지 분자 구조를 가진 물질을 의미한다.
그러나, "성상 물질"은 또한 분지점 간의 간격이 측쇄 길이와 비교하여 더 작은 여러 개의 분지점을 가진 분지 물질도 포함하기로 한다. 측쇄 형성원자에 대한 주쇄 형성 원자의 비는 1 : 3 이하이어야 한다. 분자식이 H-[CH2CH(C8H17)-]3H인 트리데크-1-엔의 경우에는 1 : 4이다. 성상 물질은 ASTM D445에 따라 측정한 40℃에서의 점도가 10~500㎟/s(cST), 바람직하게는 20~60㎟/s(cST)이어야 한다. ASTM D97에 따른 유동점은 -25℃미만, 바람직하게는 -50℃미만이어야 한다.
적당한 성상 물질의 한 예는 트리올과 모노카르복실산의 폴리에스테르 CH3-C(-CH2-O-CO-알킬)3이다. 이는 공류제(公留劑 : entraining agent)로서 톨루엔과 함께 산 촉매의 존재 하에 100~200℃에서 제조할 수 있다.
이들과 같은 폴리올 에스테르가 합성 윤활유의 제조에 사용되는 것은 공지되어 있다.
그러나, 성상 물질은 폴리-α-올레핀인 것이 바람직하다. 첫 번째 단계로 에틸렌을 올리고머 중합해서 데크-1-엔(dec-1-ene)을 얻는다. 그 다음, 데크-1-엔을 증류하고 촉매적 수소화 반응을 행하여 이중 결합을 제거한다. 탄소와 산소막으로 구성된 지방족 액체는 이러한 방법으로 수득한다. 바람직한 폴리-α-올레핀은 구조식이 H-[CH2-CH(C8H17)-]nH(n≥3)인 올리고데크-1-엔이다. 이는 헨켈 사로부터 입수 가능하다(Emery).
성상 물질에 이외에, 대부분의 충전 화합물은 광물유를 함유한다. 본 명세서에서, 광물유란 포화탄화수소 혼합물로 필수적으로 구성되어 있는 석유, 갈탄, 무연탄, 목재 및 토탄(土炭)과 같은 광물성 원료의 액체 증류 생성물을 의미한다. 광물유는 성상 물질을 기준으로 0~10중량％, 바람직하게는 1~5중량％의 양으로 첨가해야 한다. 고분산성 실리카는 추가의 성분으로서 성상 물질을 기준으로 0~15중량％, 바람직하게는 0.5~6중량％의 양으로 첨가하는 것이 바람직하다. 본 명세서에서, 고분산성 실리카는 다른 고분산성 실리카가 사용될 수도 있을지라도 주로 발열성 실리카를 의미한다. 이들은 입자 크기가 바람직하게는 0.007~0.05㎛, 더욱 바람직하게는 0.007~0.014㎛이며, 겉보기 밀도는 20~120g/ℓ, 바람직하게는 35~40g/ℓ이다. 적당한 실리카는 Cab-O-Sil(Cabot Corporation), Aerosil (Degussa AG) 및 HDK(Wacker-Chemie)의 형태로 시판되고 있다.
실리카를 첨가하면 특히, 가소성 흐름 행동이 나타난다. 이는 자신의 중량 하에서 충전 화합물이 유동할 수 없다는 특성을 의미하는 것이다. 따라서, 항복점 미만의 전단응력치에서는, 분산계가 고체와 같이 행동하며 그 자체로서 탄성적으로 변형된다. 분산액은 항복점을 초과하는 경우에만 유동한다.
추가 성분으로서 고분자량의 폴리올레핀은 0~10중량％, 바람직하게는 0.05~2중량％인 것이 추천할 만하다. 고분자량의 폴리올레핀은 분자량은 50만 이상, 바람직하게는 2백만보다 큰 알켄의 단일중합체 및 공중합체인 것으로 이해한다. 적당한 고분자량의 폴리올레핀은 폴리에틸렌, 폴리프로필렌, 폴리이소부틸렌, 및 바람직하게는 폴리부텐 및 혼합물 및 그의 공중합체이다. 바람직한 구현예에서는, 실리카 및 고분자량의 폴리올레핀 모두를 첨가한다.
그러나, 부가 성분으로서, 성상 물질에 성상 물질을 기준으로 1~20중량％의 양으로 1종 이상의 점도 지수 향상제를 가하는 것이 훨씬 유용할 수 있다. 따라서, 점도 거동은 일반적인 경우에서와 같이 점도가 온도가 증가함에 따라 감소하지 않는 정도까지 향상된다. 점도 지수 향상제는 평균 분자량이 10,000~100,000, 바람직하게는 10,000~20,000인 중합체이다.
공지의 점도 지수 향상제는 폴리이소부텐, 디엔 중합체, 에틸렌과 프로필렌의 공중합체, 및 폴리알킬 스티렌이다. 공지의 점도 지수 향상제 중에서, 본 발명의 목적에 적당한 화합물은 무엇보다도 하기의 두 가지 성질 때문에 선택된다: 케이블 재료에 대해 불활성이어야 하며, 저온에서는 성상 물질에 용해성이 열등하고 고온에서는 용해성이 탁월하다. 이소프렌 및 스티렌의 수소화 공중합체(쉘비스(Shellvis) 50, Shell 사 제품)가 특히 유용한 것으로 판명되었다.
또한, 본 발명에 따른 충전 화합물은 분산 보조제를 함유할 수 있다. 적당한 분산 보조제는 중축합물, 더욱 구체적으로는 소수성 및 친수성 성분기재의 중축합물이다. 즉, 이량체 지방산 또는 상응하는 디아민으로부터 적어도 부분적으로 합성된 중축합물을 사용할 수 있다. 적당한 중축합물은 이량체 지방산과 디아민의 폴리아미드 또는 이량체 지방산과 다가 알코올(2가 또는 3가)의 폴리에스테르이다. 혼합형도 사용할 수 있다. 아미노말단의 폴리중축합물이 바람직하다. 예를 들면, 장쇄의 디카르복실산과 하나 이상의 디아민 또는 트리아민과의 중축합물, 더욱 구체적으로는 이량체 지방산, 삼량체 지방산, 단량체 지방산과 탄소수 2~36의 1차 또는 2차의 디아민(이량체 지방성 아민)과의 축합 생성물이 적합하다. 디카르복실산과 피페라진과 같은 고리형 디아민과의 중축합물도 사용할 수 있다. 이량체 지방산도 세박산 또는 아디프산과 같은 단쇄의 디카르복실산으로 어느 정도 대체할 수도 있다. 많은 경우에, 중축합물은 말단이 아미노기인 것이 바람직하다. 아민가는 80~400, 더욱 구체적으로는 190~230인 것이 바람직하다. 예를 들면, 바람직한 재료는 이러한 특성 값 및 점도 0.3 내지 4Pas(75℃)을 갖지만, 다른 적당한 생성물의 점도는 150℃에서 0.7~1.2Pas이다. 원한다면, 올리고머 분산제를 지방산 에스테르 및/또는 지방 알코올 에테르로 완전히 또는 부분적으로 대체할 수도 있다.
본 발명에 따른 충전 화합물은 또다른 성분으로서 이러한 제제에 일반적으로 포함되는 보조제를 함유할 수 있다. 예를 들면, 항산화제, 염료 또는 부식 방지제를 함유할 수 있다.
충전 화합물은 효과적이지만 소극적인 혼합기를 사용하여 제조할 수 있는데, 이 혼합기는 소위 탁류 믹서와 같이 저속에서도 효과적으로 배합할 수 있다.
본 발명에 따른 충전 화합물은 실온에서부터 60℃ 이하까지의 완만하게 상승한 온도에서 용이하게 펌프될 수 있다. 이동 동안에는 분리되거나 공기가 혼입되거나 액포가 관찰되지 않는다. 본 발명의 충전 화합물은 어려움없이 금형에 부울 수도 있으며, 금형은 기포없이 완전히 채워진다.
본 발명에 따른 충전 화합물은 해로운 영향, 특히 수분의 침투에 대하여 케이블, 플러그, 커넥터, 통신 케이블 또는 광학 케이블과 같은 여러 가지 종류의 전기 성분의 보호에 적당하다. 충전 화합물은 또한 방치 동안에 굽힘 및 저온에 노출된 결과 나타날 수 있는 기계적 손상에 대하여 광학적 유리 케이블을 보호하는데 적당하다. 본 발명에 따른 충전 화합물은 예를 들면, 전선 또는 성분이 설치 동안에 탈절연되거나 손상되고 재절연되어야 하는 경우에 수리 밀봉제로 사용할 수 있다.
본 발명에 따른 충전 화합물은 여러 가지의 기술적 특성을 나타낸다. 즉, 그의 절연 저항은 특정한 부피 저항 인자와 같이 높다. 그의 유전 상수는 낮으며, 즉 2.3 미만, 심지어는 2미만으로 조정할 수 있다. 바람직한 충전 화합물의 비중은 1미만이다. 이들은 전기 성분 및 케이블에 사용되는 여러 가지 종류의 플라스틱과 혼화 가능하다. 즉, 충전 화합물의 성분은 플라스틱에 거의 침투되지 않으며 표준 케이블 외장 재료에 영향을 미치지 않는다. 충전 화합물은 100℃이하의 온도에서 완전히 안정하며 이러한 온도에서는 손상의 경우에도 유동되지 않는다. 또한, 충전 화합물은 유연성이 있으며 저온의 응력 하에서 나타나는 균열이 없이 흐름 특성의 극적인 변화 없이 -50℃ 이하의 온도에서 그의 유연성을 유지한다. 또한, 본 발명에 따른 충전 화합물은 가공이 용이하며, 즉, 이들은 적절한 압력하의 60℃미만의 온도에서 가장 접근하기 어려운 지점까지 충전될 케이블 외장에 도입될 수 있다.
본 발명에 따른 모든 충전 화합물은 하기의 조건을 만족한다:
·DIN ISO 2592에 따른 인화점(℃) : 〉 200℃;
·DIN 53483에 따른 20℃에서의 유전 상수 : 〈 2.3;
·DIN 53482에 따른 100℃에서의 부피 저항률(cm): 〉 1010;
·20℃에서의 점도 : 〈20Pa.s(D=20s-1에서);
·DIN 51580에 따른 원뿔형 투과성 : 〉 250[1/10mm] (-40℃ 에서), 또는 〉 200mm/10 (-50℃에서) ; 및
·케이블 외장 PE의 중량 증가(70℃/10d) : 〈5％.
상기한 특성은 하기의 방법으로 측정한다:
-측정 온도에서 측정될 물질의 한정된 기포가 없는 부피(〉100㎖)를 칭량한 밀도. 계산은 공지의 방법으로 행한다.
-중량 증가는 DIN 57472(40×40×3mm의 시험판을 충전화합물 중에서 70℃에서 10일간 보관한다)에 따라 측정한다. 그 차는 중력계로 측정한다.
-인화점은 DIN ISO 2592에 따라 측정한다.
적하 움직임은 하기의 네트(net)/시이브(sieve)시험으로 측정한다:
-Fed. 시험법 STD. No. 791B,
-JIS K 2220, p.7, 또는
-CNET ST LAA/ELR/CSD/543.
이들 모두는 메쉬의 넓이가 250㎛인 원추형 철망을 통해 10g의 충전 화합물로부터 오일을 분리하는 것을 기준으로 한 것이다. 본 경우에는, 시험 시간과 온도를 24시간 및 +80℃로 고정시켰다.
유리한 특성, 무엇보다도 저온에서의 유연성 및 내구성에 대하여 나타내기 위하여, 본 발명에 따른 화합물을 하기의 시험법에 따라 비교예와 비교하였다:
방법 Ⅰ
유동 내성(FTM STD No. 791 B 또는 JIS, K 2220, p.7에 따른 적하시험으로 측정).
방법 Ⅱ
DIN 51580에 따른 원뿔형 투과성.
방법 Ⅲ
유동 곡선/점도의 측정
장치 : 콘트라베스(Contraves) DIN 125
본 발명을 하기의 실시예로 나타내었다:
A) 사용된 성분 :
a) 합성 오일(α-올레핀 공중합체, SAP 601(Shell사 제품))
전형적인 데이타 :
40℃에서의 동적 점도(㎟/s) : 30.5㎟/s
인화점 : 238℃ ASTM D92.
유동점 : -68℃ ASTM D97.
b) 쉘비스(Shellvis) 50(Shell사 제품; 스티렌/이소프렌 공중합체 (수소화됨))
c) 실리카 : Cab-o-Sil M5(Cabot사 제품)
전형적인 값 : 표면 BET 200±25㎡/g
입자 크기 : 약 14·10-9m
d) A247(Henkel Corp., USA 제품)
광물유 및 에스테르 중 고분자량 폴리(이소)부텐의 용액 5.6％.
B) 특성을 가진 충전 화합물의 제조.
621.6kg의 SAP 601을 용량 1000ℓ의 난류 믹서에 도입하고, 78.4kg의 쉘비스 50을 실온에서 첨가하고 혼합하여 균일하게 분포시킨다. 간접 증기를 사용하여 120~130℃로 승온시킨 후, 모든 고형입자가 용해될 때까지 혼합한다. 이는 유리판 상의 코팅 및 점도 및 항복점의 시험에 의해 입증된다. 긍정적인 결과가 수득되면 진공을 가하고 생성물을 필터를 통해 기포 없이 적당한 팩으로 흐르게한다.
[실시예 2]
658kg의 SAP 601을 믹서에 도입하고(실시예 1 참고), 7kg의 A247을 실온에서 가하고 균일하게 분포시키거나 용해시킨다. 간접 증기로 약 120~130℃로 가열하면서 35kg의 Cab-O-Sil M5를 일부 가하고 혼합하여 균일하게 분포시킨다. 그의 확인 및 특성을 실시예 1과 같이 수행한다. 배기 후, 생성물을 필터를 통해 기포 없이 적당한 팩으로 흐르게 한다.
[표 1]

Claims (10)

  1. 하기의 성상 물질(stellate substance)을 함유하는 것을 특징으로 하는 케이블, 커넥터, 플러그 등의 형태의 전기 및 광학 장치용 충전 화합물:
    성상 물질은 3이상의 분지가 단일의 분지점에서 방사상으로 뻗어 있는 분지 분자 구조를 갖는 물질, 또는 분지점 간의 간격이 측쇄 길이와 비교하여 좁은 여러개의 분지점을 가진 분지된 물질로서, 이 성상 물질에서, 측쇄 형성 원자에 대한 주쇄 형성 원자의 비는 1 : 3 이하이며,
    ASTM D445에 따른 40℃에서의 상기 성상 물질의 점도는 10 내지 500㎟/s(cST)이고; 상기 충전 화합물은 성상 물질을 기준으로 0.5중량％이하의 양으로 실리카, 클레이 또는 금속 비누와 같은 틱소트로피제를 함유한다.
  2. 제1항에 있어서, 성상 물질이 올리고머화도가 3이상인 폴리-α-올레핀인 것을 특징으로 하는 충전 화합물.
  3. 제1항에 있어서, 성상 물질을 기준으로 1~5중량％의 광물유가 첨가되는 것을 특징으로 하는 충전 화합물.
  4. 제1항 내지 3항 중의 어느 한 항에 있어서, 고분산성 실리카 및/또는 고분자량의 폴리올레핀이 첨가되는 것을 특징으로 하는 충전화합물.
  5. 제4항에 있어서, 성상 물질을 기준으로 고분산성 실리카의 함량 0.5 중량％이하 및/또는 고분자량의 폴리올레핀 함량 0.05~2중량％인 것을 특징으로 하는 충전 화합물.
  6. 제1항 내지 3항중의 어느 한 항에 있어서, 점도 지수 향상제가 성상 물질을 기준으로 1~20중량％의 양으로 첨가되는 것을 특징으로 하는 충전 화합물.
  7. 제1항에 있어서, -50℃에서의 원뿔형 투과성이 200이상이고, 80℃이상에서 유동 내성을 나타냄을 특징으로 하는 충전 화합물.
  8. 제7항에 있어서, 제1항 내지 6항 중의 어느 한 항에 따른 성분임을 특징으로 하는 충전 화합물.
  9. 제1항 내지 8항 중의 어느 한 항에 따른 충전 화합물을 함유하는 케이블, 케넥터, 플러그 등의 형태의 전기 및 광학 장치.
  10. 광학 케이블 제조용 전선 충전 화합물인 제1항 내지 8항 중의 어느 한 항에 따른 충전 화합물.
KR1019940701542A 1991-11-07 1992-10-29 충전 화합물 KR100256634B1 (ko)

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PCT/EP1992/002475 WO1993009208A1 (de) 1991-11-07 1992-10-29 Füllmasse

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FI942103A0 (fi) 1994-05-06
CA2123200A1 (en) 1993-05-13
DE4136617A1 (de) 1993-05-13
EP0739974A2 (de) 1996-10-30
EP0612345A1 (de) 1994-08-31
EP0739974A3 (de) 1996-11-20
US6258885B1 (en) 2001-07-10
ES2097932T3 (es) 1997-04-16
WO1993009208A1 (de) 1993-05-13
DE4136617C2 (de) 1997-08-14
DK0612345T3 (da) 1997-08-18
JPH07501089A (ja) 1995-02-02
JP3081644B2 (ja) 2000-08-28
EP0612345B1 (de) 1997-02-05
EP0541007A1 (de) 1993-05-12
ATE148739T1 (de) 1997-02-15
FI942103A (fi) 1994-05-06
DE59208023D1 (de) 1997-03-20

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