KR100787403B1 - 개선된 녹방지성 및 내마모성을 가진 그리스 조성물 - Google Patents

개선된 녹방지성 및 내마모성을 가진 그리스 조성물 Download PDF

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KR100787403B1
KR100787403B1 KR1020037001912A KR20037001912A KR100787403B1 KR 100787403 B1 KR100787403 B1 KR 100787403B1 KR 1020037001912 A KR1020037001912 A KR 1020037001912A KR 20037001912 A KR20037001912 A KR 20037001912A KR 100787403 B1 KR100787403 B1 KR 100787403B1
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South Korea
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grease composition
benzotriazole
grease
hydroxy
calcium
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KR1020037001912A
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KR20030027014A (ko
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오자끼다까히로
시노다노리아끼
나까자와고우이찌
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쉘 인터내셔날 리서치 마챠피즈 비.브이.
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Abstract

베이스 오일 및 증점제를 함유하는 그리스 조성물로서, 그리스가 전체 그리스 조성물에 대해, 0.05 중량% 내지 30 중량% 의 소듐 티오설페이트, 및 0.1 중량% 이상의, 칼슘 살리실레이트, 마그네슘 살리실레이트, 칼슘 페네이트 및/또는 칼슘 술포네이트를 포함하는 군으로부터 선택되는 하나 이상의 첨가제 (A) 를 추가적으로 함유하는 그리스 조성물; 녹방지성 및 내마모성을 개선하기 위한 상기 그리스 조성물의 용도; 및 상기 그리스 조성물의 제조 방법.

Description

개선된 녹방지성 및 내마모성을 가진 그리스 조성물{GREASE COMPOSITION WITH IMPROVED RUST PREVENTION AND ABRASION RESISTANCE PROPERTIES}
본 발명은 개선된 녹방지성 및 내마모성을 가진 그리스 조성물에 관한 것이다.
극압 그리스는 그의 탁월한 내마모성 및 하중을 견디는 그의 성능 때문에, 예를 들어 자동차의 베어링 및 기어, 철 및 강철, 철도 및 각종 기타 공업용 기계 장치에서 다수의 용도를 갖는다.
전형적인 극압 그리스 조성물은, 일반적으로, 각종 유형의 그리스 중에, 올레핀 설파이드, 유지류의 설파이드, 황-인 기재의 극압제, 몰리브덴 디설파이드, 유기몰리브덴 화합물, 납 화합물 및 아연 디티오포스페이트와 같은 첨가제를 함유하는 것들이다.
최근 기술은 소듐 티오설페이트를 함유한 그리스를 개시했는데, 이는 탁월한 극압성을 갖는다: 일본 공개 특허 3-131690, 일본 공개 특허 11-35965 및 미국 특허 4,923,625 의 명세서.
그러나, 상기 선행 기술 문서에서의 내마모성은 불만족스러우며, 소듐 티오설페이트가 수분을 흡수하는 특성이 있기 때문에, 녹이 유도될 추가적인 가능성이 있다. 특히, 강철 장치 및 식료품 설비의 베어링 및 기어는, 다량의 수분이 있는 조건 하에 윤활되기 때문에, 녹의 생성이 촉진되며, 윤활화에 연관된 문제가 쉽게 발생한다.
따라서, 녹의 생성이 방지되며 또한 내마모성이 개선되면서도, 소듐 티오설페이트를 함유하는 그리스 조성물의 극압성이 잘 보존되는 그리스 조성물을 제공할 수 있는 것이 강하게 요망된다.
본 발명은, 베이스 오일 및 증점제를 함유하는 그리스 조성물로서, 그리스가 전체 그리스 조성물에 대해, 0.05 중량% 내지 30 중량% 의 소듐 티오설페이트, 및 0.1 중량% 이상의, 칼슘 살리실레이트, 마그네슘 살리실레이트, 칼슘 페네이트 및/또는 칼슘 술포네이트를 포함하는 군으로부터 선택되는 하나 이상의 첨가제 (A) 를 추가적으로 함유하는 그리스 조성물을 제공한다.
바람직한 구현예에서, 본 발명의 그리스 조성물은 전체 그리스 조성물에 대해, 0.1 중량% 이상의 벤조트리아졸 화합물 (B) 를 추가로 함유한다.
본 발명에 따른 그리스 조성물에서, 증점제는 우레아 화합물, 리튬 비누, 리튬 착물 비누 및 알루미늄 착물 비누와 같은 제제일 수 있으며, 이는 단독으로 또는 혼합물로서 사용될 수 있다. 우레아 결합을 가진 화합물에 더해, 우레아 화합물은 천연적으로 우레아 결합 및 우레탄 결합을 포함하는 화합물일 수 있다. 디우레아, 트리우레아 및/또는 테트라우레아 증점제가 편리하게 사용될 수 있다. 우레아-이미도 화합물도 또한 증점제로서 편리하게 사용될 수 있다.
본 발명의 바람직한 구현예에서는, 전체 그리스 조성물에 대해 2 내지 35 중량% 의 증점제가 사용된다.
본 발명에 따라 사용되는 베이스 오일로는 식물성 오일; 광물성 오일; 및 합성 오일, 예컨대 에스테르 오일, 에테르 오일 및 탄화수소 오일을 사용할 수 있다.
본 발명에 따라 사용되는 소듐 티오설페이트는 Na2S2O3 (무수물) 또는 Na2S2O3·5H2O (5 수화물), 또는 이들의 혼합물일 수 있다. 소듐 티오설페이트를 함유하는 시판용 첨가제 (예를 들어, Desilube 88, Desilube Technology Incorporated, USA) 도 사용할 수 있다.
첨가되는 소듐 티오설페이트의 양은 전체 그리스 조성물에 대해, 바람직하게는 0.2 중량% 내지 20 중량%, 더욱 바람직하게는 0.2 중량% 내지 10 중량%, 더욱 바람직하게는 0.2 중량% 내지 8 중량%, 가장 바람직하게는 0.5 중량% 내지 6 중량% 의 범위이다.
바람직하게는, 칼슘 살리실레이트, 마그네슘 살리실레이트, 칼슘 페네이트 및/또는 칼슘 술포네이트를 포함하는 군으로부터 선택되는 하나 이상의 첨가제 (A) 는 각각 전체 그리스 조성물에 대해, 0.1 중량% 내지 5 중량%, 더욱 바람직하게는 0.2 중량% 내지 3 중량%의 범위의 양으로 존재한다.
벤조트리아졸 화합물 (B) 는 전체 그리스 조성물에 대해, 바람직하게는 0.1 중량% 내지 5 중량%, 더욱 바람직하게는 0.2 중량% 내지 3 중량% 의 범위의 양으로 존재한다.
상기 언급된 첨가제 (A) 가 0.1 중량% 미만으로 존재하는 경우, 녹방지 효과가 불충분하며, 상기 언급된 첨가제 (B) 가 0.1 중량% 미만으로 존재하는 경우, 내마모성 촉진 효과가 불충분하다.
어느 하나의 첨가제가 5 중량% 초과로 존재하는 경우, 이들의 효과는 한계가 있거나 또는 추가적인 증가가 없다.
상기 언급된 벤조트리아졸 (B) 의 예는 1,2,3-벤조트리아졸, 2-(2'-히드록시-5'-메틸페닐)벤조트리아졸, 2-[2'-히드록시-3'-(3",4",5",6"-테트라히드로프탈이미도메틸)-5'-메틸페닐]벤조트리아졸, 2-(2'-히드록시-3',5'-디-tert-부틸페닐)벤조트리아졸, 2-(2'-히드록시-5'-tert-옥틸페닐)벤조트리아졸, 2-(2'-히드록시-3',5'-디-tert-아밀페닐)벤조트리아졸, 2-[2-히드록시-3,5-비스(α,α -디메틸벤질)페닐]-2H-벤조트리아졸 및 2-(2'-히드록시-3'-운데실-5'-메틸페닐)벤조트리아졸을 포함한다.
본 발명의 그리스 조성물은 추가적인 첨가제, 예를 들어, 산화방지제, 예컨대 아민 및 페놀; 극압 첨가제, 예컨대 올레핀 설파이드 및 유지류 설파이드; 극압/내마모제, 예컨대 포스파이트 및 포스페이트; 증점제, 예컨대 폴리부텐 및 폴리메타크릴레이트; 고체 윤활제, 예컨대 질화붕소 및 이황화몰리브덴; 및 각종 기타 첨가제를 추가로 함유할 수 있다.
본 발명에 따른 그리스 조성물은 소듐 티오설페이트, 및 칼슘 살리실레이트, 마그네슘 살리실레이트, 칼슘 페네이트 및/또는 칼슘 술포네이트를 포함하는 군으로부터 선택되는 하나 이상의 첨가제 (A) 및 베이스 오일에 혼입될 기타 추가의 첨가제를 미리 혼합하고, 혼합물을 베이스 오일 및 증점제를 함유하는 베이스 그리스 조성물에 첨가함으로써, 또는 각각의 첨가제를 개별적으로 베이스 그리스 조성물에 혼입시킴으로써 제조할 수 있다. 이는 고온 또는 저온 혼합에 이은, 첨가제 성분의 균일한 분산을 위한 균질화를 통해 수행될 수 있다.
본 발명의 그리스 조성물은 베어링, 기어 및 조인트, 예컨대 등속 조인트에 편리하게 사용될 수 있다.
본 발명은 이제 하기 실시예를 참고로 상술될 것이며, 이는 본 발명의 범주를 임의의 방식으로 한정하려는 것이 아니다.
실시예
그리스 조성물의 제조
실시예 및 비교예의 그리스는, 표 1 내지 9 에 기재된 제형에 따라서, 상기 언급된 (A) 및 (B) 에 해당하는 첨가제, 또는 기타 첨가제를 베이스 그리스에 첨가하여 이를 3 롤 분쇄기로 처리함으로써 수득했다. 베이스 그리스의 조성은 하기에 있다.
I. 우레아 베이스 그리스
디페닐메탄-4,4'-디이소시아네이트 (295.2 g) 및 옥틸아민 (304.8 g) 을 정제된 광물성 오일 (동점도, 100℃에서 약 15 ㎟/s; 5400 g) 에서 반응시키고; 수득한 우레아 화합물을 균일하게 분산시켜서, 일관성 (consistency) 289 (25℃, 60 W) 및 적점 263℃ 의 우레아 베이스 그리스를 수득했다. 우레아 화합물 함량은 10 중량% 였다.
II. 리튬 비누 베이스 그리스
일관성 268 (25℃, 60 W) 및 적점 199℃ 의 리튬 비누 베이스 그리스를, 리튬 12-히드록시스테아레이트 (600 g) 를 균일하게 분산시키고, 이를 정제된 광물성 오일 (동점도, 100℃에서 약 15 ㎟/s; 5400 g) 에 용해시킴으로써 수득했다. 리튬 비누 함량은 10 중량% 였다.
III. 리튬 착물 비누 베이스 그리스
12-히드록시스테아르산 (350 g) 및 수산화리튬 (50.5 g) 을 정제된 광물성 오일 (동점도, 100℃에서 약 11 ㎟/s; 4165 g) 에서 반응시킨 후, 일관성 281 (25℃, 60 W) 및 적점 259℃ 의 화합물 리튬 비누 베이스 그리스를, 아젤라산 (120.65 g) 및 수산화리튬 (59.0 g) 과 반응시키고 균일 분산 처리를 함으로써 수득했다. 리튬 착물 비누 함량은 10.4 중량% 였다.
IV. 알루미늄 착물 비누 베이스 그리스
벤조산 (158.22 g) 및 스테아르산 (334.8 g) 을 정제된 광물성 오일 (동점도, 100℃에서 약 11 ㎟/s; 4272 g) 에 용해시킨 후, 일관성 279 (25℃, 60 W) 및 적점 258℃ 의 화합물 알루미늄 비누 베이스 그리스를, 시판되는 시클릭 알루미늄 옥시드 프로필레이트 윤활액 [상표명: Arugoma (Algomer), Sengen Fain Kemikaru (Sengen Fine Chemicals) K.K. 제조] 을 첨가함으로써 반응을 수행하여 수득했으며; 생성된 비누를 처리하여 균일하게 분산시켰다. 알루미늄 착물 비누 함량은 11 중량% 였다. 벤조산 (BA) 및 스테아르산 (FA) 의 몰비는 BA/FA = 1.1:1 였으며, 알루미늄에 대한 벤조산과 스테아르산의 몰비는 (BA + FA)/Al = 1.9:1 였다.
녹방지성, 극압성 및 마모성은, 녹방지 시험 (습도 시험) 및 4 구 시험 (EP 시험 및 내마모성 시험) 을 수행하여 확인했다.
습도 시험
그리스의 샘플을, 시험편의 표면에 코팅되는 그리스의 양이 JIS (일본 산업 표준) K2220 5.17 습도 시험에 따라 처방된 바와 같이 0.30 g ±0.05 g 이 되도록, 시험편의 전체 표면 상에 균일하게 코팅했다. 그리스가 적용된 강철판을 온도 49℃, 상대 습도 95% 이상의 습도 캐비넷 내에 정치시키고, 2 주 후 녹 정도를 JIS K2246 등급으로 나타냈다.
등급 생성된 녹%
A 등급 0
B 등급 1 내지 10
C 등급 11 내지 25
D 등급 26 내지 50
E 등급 51 내지 100
EP 시험
팽창 하중 (N) 을, ASTM (American Society for Testing Materials) D2596 에 따라 4 구 시험으로 시험했다.
시험 조건: 회전속도: 1770 ± 60 rpm
온도: 27℃ ±8℃
시간: 10 ±0.2 초
내마모성 시험
4 구 시험에 사용된 구체 상의 마모 자국의 직경을 ASTM D2266 에 따라 측정했다.
시험 조건: 회전속도: 1200 ±50 rpm
온도: 75℃±1.7℃
하중: 40 ±2 kgf (392 ±2 N)
시간: 60 ±1 분
첨가제
하기 표에서, *1 내지 *10 는 하기와 같다:
Desilube 88, *1 는 Desilube Technology Incorporated 로부터의, 소듐 티오설페이트를 함유하는 무기성 S-P 첨가제에 대한 상표명이다.
하기 제품은 본 발명에 따라 상기 언급된 첨가제 (A) 에 해당한다.
SAP001, *2 는 Infineum Limited 로부터의, 칼슘 살리실레이트에 대한 상표명이다.
SAP007, *3 는 Infineum Limited 로부터의, 마그네슘 살리실레이트에 대한 상표명이다.
OLOA219, *4 는 Oronaito Japan (K.K) 로부터의, 칼슘 페네이트에 대한 상표명이다.
NA-SUL 729, *5 는 King Industrias Incorporated 로부터의, 칼슘 술포네이트에 대한 상표명이다.
하기 제품은 본 발명에 따라 상기 언급된 첨가제 (B) 에 해당한다.
BT-120, *6 는 Shirokita‡ Kagaku (Shirokita Chemicals) (K.K.) 으로부터의, 1,2,3-벤조트리아졸에 대한 상표명이다.
하기는 (A) 및 (B) 이외의 첨가제이다.
NA-SUL ZS, *7 은 King Industries Incorporated 로부터의, 아연 술포네이트에 대한 상표명이다.
Dailuba Z-500, *8 은 Dainippon Inki Kagaku Kogyo (Dainippon Ink and Chemicals) (K.K) 로부터의, 광물성 오일에 희석된 아연 나프테네이트 (아연 금속 5%) 에 대한 상표명이다.
NA-SUL SS, *9 은 King Industries Incorporated 로부터의, 소듐 술포네이트에 대한 상표명이다.
NA-SUL 707, *10 은 King Industries Incorporated 로부터의, 리튬 술포네이트에 대한 상표명이다.
Figure 112003004475186-pct00001
Figure 112003004475186-pct00002
Figure 112003004475186-pct00003
Figure 112003004475186-pct00004
Figure 112003004475186-pct00005
Figure 112003004475186-pct00006
Figure 112003004475186-pct00007
Figure 112003004475186-pct00008
Figure 112003004475186-pct00009
발명의 효과
표 1 내지 5 에서의 실시예 및 표 6 내지 9 에서의 비교예로부터 명백하듯이, 소듐 티오설페이트가 혼합된 그리스 조성물에 상기 언급된 첨가제 (A) 가 첨가된 본 발명에 따른 그리스 조성물은 탁월한 극압성을 가지며, 그의 녹방지 성능은 크게 증가된다. 상기 언급된 첨가제 (A) 및 상기 언급된 벤조트리아졸 화합물 (B) 를 소듐 티오설페이트가 혼합된 그리스에 첨가한 그리스 조성물 또한 탁월한 극압성 및 녹방지성을 가지며, 추가적으로 탁월한 내마모성을 갖는다. 내마모성의 증가는 특히 우레아 그리스, 리튬 비누 그리스 및 리튬 착물 비누 그리스에서 뛰어났다. 소듐 티오설페이트는 식품 첨가제로서 오래전부터 인지되어 있었고, 해독제로서도 공지되어 있기 때문에, 인간 신체에서 뿐 아니라 지구 환경에도 순한 첨가제이다. 따라서, 본 발명에 따른 조성물은 환경 친화적인 탁월한 그리스이다.

Claims (10)

  1. 베이스 오일 및 증점제를 함유하는 그리스 조성물로서, 그리스가 전체 그리스 조성물에 대해, 0.05 중량% 내지 30 중량% 의 소듐 티오설페이트, 및 0.1 중량% 내지 5 중량% 의, 칼슘 살리실레이트, 마그네슘 살리실레이트, 칼슘 페네이트, 칼슘 술포네이트 및 이들의 조합물로 이루어진 군으로부터 선택되는 첨가제 (A) 를 추가적으로 함유하는 그리스 조성물.
  2. 삭제
  3. 제 1 항에 있어서, 상기 첨가제 (A) 가 각각 전체 그리스 조성물에 대해, 0.2 중량% 내지 3 중량% 의 양으로 존재하는 그리스 조성물.
  4. 제 1 항에 있어서, 전체 그리스 조성물에 대해, 0.1 중량% 내지 5 중량% 의 벤조트리아졸 화합물 (B) 를 추가로 함유하는 그리스 조성물.
  5. 삭제
  6. 제 4 항에 있어서, 상기 벤조트리아졸 화합물 (B) 가 전체 그리스 조성물에 대해, 0.2 중량% 내지 3 중량% 의 양으로 존재하는 그리스 조성물.
  7. 제 4 항에 있어서, 상기 벤조트리아졸 화합물 (B) 가 1,2,3-벤조트리아졸, 2-(2'-히드록시-5'-메틸페닐)벤조트리아졸, 2-[2'-히드록시-3'-(3",4",5",6"-테트라히드로프탈이미도메틸)-5'-메틸페닐]벤조트리아졸, 2-(2'-히드록시-3',5'-디-tert-부틸페닐)벤조트리아졸, 2-(2'-히드록시-5'-tert-옥틸페닐)벤조트리아졸, 2-(2'-히드록시-3',5'-디-tert-아밀페닐)벤조트리아졸, 2-[2-히드록시-3,5-비스(α,α-디메틸벤질)페닐]-2H-벤조트리아졸 및 2-(2'-히드록시 -3'-운데실-5'-메틸페닐)벤조트리아졸로부터 선택되는 그리스 조성물.
  8. 제 1 항에 있어서, 증점제가 우레아 화합물, 리튬 비누, 리튬 착물 비누, 알루미늄 착물 비누 및 이들의 조합물로 이루어진 군으로부터 선택되는 비누인 그리스 조성물.
  9. 녹방지성 및 내마모성을 개선하기 위한, 제 1 항에 따른 그리스 조성물의 사용 방법.
  10. 소듐 티오설페이트, 및 칼슘 살리실레이트, 마그네슘 살리실레이트, 칼슘 페네이트, 칼슘 술포네이트 및 이들의 조합물로 이루어진 군으로부터 선택되는 첨가제 (A) 를 미리 혼합하고, 혼합물을 베이스 오일 및 증점제를 함유하는 베이스 그리스에 첨가하는 방법이거나, 또는 소듐 티오설페이트 및 상기 첨가제 (A) 를 개별적으로 상기 베이스 그리스에 혼입시키는 방법인, 제 1 항에 따른 그리스 조성물의 제조 방법.
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JP4634585B2 (ja) 2011-02-16
RU2263137C2 (ru) 2005-10-27
CA2418850A1 (en) 2002-02-14
AU7981501A (en) 2002-02-18
HUP0302687A2 (hu) 2003-11-28
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EP1307532B1 (en) 2006-07-05
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