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KR960014933B1 - 인 함량이 낮은 윤활유 - Google Patents

인 함량이 낮은 윤활유 Download PDF

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Publication number
KR960014933B1
KR960014933B1 KR1019880002058A KR880002058A KR960014933B1 KR 960014933 B1 KR960014933 B1 KR 960014933B1 KR 1019880002058 A KR1019880002058 A KR 1019880002058A KR 880002058 A KR880002058 A KR 880002058A KR 960014933 B1 KR960014933 B1 KR 960014933B1
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South Korea
Prior art keywords
composition
copper
fat
phosphorus
soluble
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Expired - Fee Related
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KR1019880002058A
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KR880010106A (ko
Inventor
테렌스 콜클로흐
존 프레드릭 마쉬
프레드릭 알리스테어 깁슨
Original Assignee
엑손 케미칼 페이턴츠 아이엔씨
로버트 프랭크 노뜨오버
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Publication of KR880010106A publication Critical patent/KR880010106A/ko
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Publication of KR960014933B1 publication Critical patent/KR960014933B1/ko
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Abstract

내용없음.

Description

인 함량이 낮은 윤활유
본 발명은 윤활유 조성물, 특히 인이 포함되지 않았거나 또는 소량으로 함유된 자동차의 크랭크실용(crankcase) 윤활유에 관한 것이다.
인은 배출가스를 조절하는 촉매적 전환자에 보통 이용되는 촉매에 해로운 영향을 끼치기 때문에 윤활유내의 인 함량을 줄이기 위한 작업들이 유행하고 있다. 일반적으로 인 함량은 0.1%였으나 0.05wt% 이하의 수준으로 낮추거나 또는 모두 제거하기 위한 필요성이 증가하였다. 그러나 징크 디알킬 디티오포스페이트(ZDDP) 및 기타 인을 함유하는 부가제들이 마모방지(anti-wear) 및/또는 산화방지 부가제로서 널리 이용되었으며 이러한 성분들을 윤활유로부터 줄이거나 모두 제거하면 엔진성능은 떨어지게 된다.
본 발명은 구리, 황, 베어링 부식억제제를 포함하며 인이 전혀 없거나 소량 함유된 주목할만한 엔진성능을 나타내는 윤활유 조성물 및 농축물을 제공한다.
미합중국 출원 제2356661호는 코퍼 디알킬 디티오카바메이트 같은 지용성 유기 화합물로서 구리 50-1000ppm을 함유하며 티오카바메이트 같은 지용성 유기 황 화합물로서 오일내의 0.1-0.5wt% 황과 함께 인을 함유하는 화합물을 포함하는 윤활유에 관한 것이다.
황 화합물과 복합된 인을 함유하는 구리를 포함하는 구리 화합물을 윤활유에 부가하는 것이 미합중국 출원 제2343756호에 기재되었다. 0.1-0.5wt%의 황함량이 기재되었으며 0.5wt%를 초과하면 매우 해롭다고 기재되었다. 미합중국 출원 제2552580호에서는 티오인산염 제1동(cuprous thiophosphates)을 비교적 높은 수준으로 윤활유 조성물에 포함시켜 오일내에서의 인의 수준을 높이게 하였다.
미합중국 출원 제3346493호에서는 여러가지 다양한 금속을 함유하는 중합체 아민-금속 반응물이 윤활유 조성물내에서 청정제로 이용되었다. 그중 한 실시예에서, 그중에서도 특히 아실화된 질소 화합물의 구리염, 헥센산화물과 반응하는 ZDDP로서의인 0.075%와 송유산(tall oil acid)의 황화된 메틸에스테르를 포함하는 윤활유가 기재되었다. 기타 구리를 함유하는 윤활유보다 많은 인을 함유하거나 또는 황을 전혀 함유하지 않았다. 아민, 셀레나이드, 포스핀 또는 포스파이트와 함께 산화방지 안정화제로서의 모든 전이금속화합물 그룹이 미합중국 출원 제4122033호에 기재되었으며 이러한 것은 윤활유의 부가제와 같은 여러가지 경우에 이용될 수 있다. 앞서의 출원중 어느 하나도 최신식 윤활유에 요구되는 점들을 갖춘 완전히 제형화된 윤활유에 관한 것은 아니며, 특히 마모방지, 산화방지, 부식억제 성능을 유지하면서 인의 수준을 낮추는 것에 대해서는 기록하지 않았다.
재가 없는 분산제 및/또는 점도 지수를 개선하는 중합성 분산제, 디티오카바메이트 형태의 구리를 함유하지만 아연 및 0.01-0.5wt%의 인을 필요로 하는 윤활유 조성물이 유럽특허 출원 제24146호에 기재되었다. 티아디아졸 폴리설파이드가 임의의 성분으로 포함될 수 있다.
ZDDP 양을 감소시킨 것을 보충하기 위하여 디알킬디페닐아민과 황화폴리올레핀의 혼합물을 이용하여 인함량이 감소된(0.05% P까지) 오일이 미합중국 출원 제4330420호에 기재되었다. 구리 또는 티아디아졸 폴리설파이드를 이용하는 것은 기재되지 않았다.
4,4'-메틸렌 비스(2,6-디-t-부틸페놀)과 트리-sec-C4-12알킬 오르토보레이트의 반응생성물 및 ZDDP의 양을 0.05-0.11wt% P로 감소시키기 위한 윤활유내에서의 이 생성물의 용도가 유럽특허 출원 제89844호에 기재되었다.
금속이 특히, 구리 또는 황으로 가교된 입체 장해된 비스페놀인 경우 산화 억제제로서 비스(디티오벤질) 금속 유도체와 구리염, 티아디아졸 폴리설파이드, 테레프탈산을 포함하는 금속염 형태의 붕소를 함유하는 복소환식 화합물로 구성된 윤활유가 미합중국 특허 출원 제4490265호에 기재되었다. 인을 감소시키거나 또는 모두 제거하기 위한 필요성이 기재되어 있지 않으며 모든 실시예에서 윤활유는 0.05wt의 인을 함유한다. 이와 유사한 것이 미합중국 특허 출원 제4623474호이다.
구리염 형태일 수 있으며 황화될 수 있는 붕소함유 복소환식 화합물이 미합중국 특허 출원 제4627930호에 기재되었다. 티아디아졸 폴리설파이드와 카복실산 구리가 기재되었다. 비록 붕소함유 복소환식 화합물이 인이 없이 기재되었어도 0.05wt% P 미만을 함유하는 완전히 제형화된 오일이 기재되지는 않았다.
이와 유사하게 기재된 특허는 미합중국 출원 제462958호이다. 극심한 압력하에서 이용하기 위한 붕소 및 금속-붕소 유도체, 윤활유에 대한 마모방지 부가제 및 마찰감소 부가제, ZDDP를 함유하지 않는 조성물 등이 미합중국 출원 제4629579호에 기재되었으나 황, 구리와 함께 소량의 인을 함유하거나 전혀 갖지 않는 조성물에 대해서는 기재되지 않았다.
인이 적거나 전혀 없고 구리가 없는 윤활유 조성물이 WO-A-8604601, WO-A-8604602, WO-A-8606092호에 기재되어 있다.
본 발명은 인 함량이 적거나 또는 없고 다량의 및/또는 값비싼 형태의 산화 방지제를 사용할 필요가 없는 최신 오일로서 적당한 마모방지, 부식억제, 산화방지 성능을 갖는 윤활유를 제공한다.
본문에 사용된 '최신 오일'이란 것은 주요 공업국에서 크랭크실 윤활유로서 요구되는 점들에 부합되는 오일인 자동차의 크랭크실 윤활유를 말한다. 오일교환 시간이 길어지기 때문에 요구되는 고성능 엔진, 길어진 수명 및 높은 조작 온도 등은 모두 윤활유에 요구되는 개선된 성능에 기여한다. 본 발명은 특히 API, SAE, ASTM 연합으로 책정된 일반 차량용 오일의 SF API 요구 규격 및/또는 상업용 오일/디젤엔진용 CD API 요구 규격에 부합되거나 이보다 성능이 좋은 자동차 크랭크실 윤활유에 관한 것이다.
본 발명의 한 면으로, 대부분의 윤활유, 5-500ppm의 지용성 형태로 존재하는 부가된 구리,총 황함령이 0.5-2.0wt% 이상의 바람직하게는 0.5-1.0wt%가 되도록 부가된 하나 이상의 지용성 황-함유 화합물 및 유효량의 베어링 부식억제제로 구성되며, 0.01wt% 보다 적은 인을 함유하고 실질적으로 인이 전혀 없는 것이 바람직한 윤활유 조성물을 제공한다.
본 발명의 특히 바람직한 구체예에서 윤활유 조성물은 또한 하나 이상의 무희(ashless) 분산제 및/또는 하나 이상의 점도 지수 개선 분산제 및/과염기성 칼슘 또는 마그네슘 설포네이트 또는 페네이트 같은 제산제, 녹방지제 역할을 하는 과염기성 부가제를 함유한다.
경제적으로 얻을 수 있는 최신식 오일의 요구성능에 부합되고 산화를 조절할 수 있는 인이 적은 오일로 만드는 본 발명에 이용된 구리는 특별한 산화 촉매인 철로 부식되거나 또는 마모되므로서 오일내에 축적된 금속에 의해 자동차 엔진내에서 촉매화된다.
구리의 농도가 과도하게 낮으면 어떠한 경우에는 산화방지 효과가 충분치 못하게 된다. 구리의 농도가 과도하게 높다면 오일이 회분(ash)이 증가하고 베어링의 부식증가 경향이 눈에 띄게 증가될 것이다. 조성물에 부가되는 구리의 양은 일반적으로 10-400ppm 사이이며 10-300ppm이 대표적이고 예컨대 60-200ppm 같은 10-200ppm 사이가 바람직하다.
최신 엔진시험의 규격 조건에 대한 적당한 산화방지 및 마모방지 성능을 제공하기 위한 인이 소량이거나 또는 전혀 없고 소량의 지용성 구리 화합물로 구성된 본 발명의 조성물의 성능은 놀랍다. 여러가지 경우에 있어서 산화 촉진제 또는 촉매로서의 역할을 하는 구리 및 코발트, 크로뮴 같은 유사한 금속들은 효과적인 윤활유 산화방지제가 아니다. 유럽특허 출원 제24146호에는 최소한 0.01wt%의 인과 아연이 존재한다고 기재되었다.
놀랍게도 구리 화합물의 기능은 원래부터 산화제 활성을 갖는 칼슘 또는 마그네슘의 과염기성 부가제 같은 기타 금속 화합물 및 아연을 함유 조성물 내에서 효과적이다.
만일 구리 화합물에 인이 전혀없다면 본 발명에서 산화방지제로 이용되는 구리화합물은 윤활유에 적합한 유럽특허 출원 제24146호에 기재된 것들로부터 선택할 수 있다.
그러므로, 구리는 합성 또는 천연 카복실산의 지용성 구리염으로서 오일내로 혼합될 수 있다. 적합한 카복실산의 예로는 스테아린산 또는 팔미트산 같은 C10-C18지방산, 올레인산 같은 불포화산, 분자량이 200-500인 나프텐산 같은 분지된 카복실산, 네오데카논산 또는 2-에틸헥사논산, 예컨대 옥타데켄일 숙신산, 도데칸일 숙신산, 폴리이소부텐일 숙신산인 폴리알켄 치환된 숙신산 같이 알킬 또는 알켄일 치환된 디카복실산 등이 있다.
구리는 일반식이 (RR'NCSS)nCu인 지용성 코퍼 디티오카바메이트처럼 오일내로 혼합될 수 있다. 상기 일반식에서 n은 1 또는 2이고, R 및 R'는 동일하거나 상이한 바 알킬, 알켄일, 아릴, 아랄기, 알카릴 및 시클로알킬 라디칼 같은 C1-18, 바람직하게는 C2-12를 함유하는 하이드로카빌라디칼이다. 코퍼 머캅타이드, 디설파이드 및 티옥산테이트(thioxanthates) 같은 구리와 황을 포함하는 화합물들이 본 발명에서 이용하기에 적합하다. 코퍼 설포네이트, 페네이트, 아세틸아세토네이트가 이용될 수 있다.
이와는 다르게 최종 마무리된 윤활유 조성물에서의 구리가 지용성 화합물 형태이라면 삽입될 구리는 기름에 녹지않는 형태일 수 있다. "부가된 구리"란 예컨대 구리 함유 성분이 마모되거나 부식되는 것 같이 사용되는 동안 오일내에 축적된 구리는 포함하지 않는 것이다.
본 발명의 윤활유 조성물은 부가된 지용성 황 화합물을 함유한다. 이러한 황 화합물의 바람직한 한 부류는 바람직하게는 일반식(RR'NCSS)nM의 디티오카바메이트(식중, R, R' 및 n은 상기한 바와 같고 M은 아연, 몰리브데늄 또는 (상기한 바와 같이) 구리와 같은 적당한 금속 또는 임의 치환된 하이드로카빌 라디칼임)이다. 바람직한 디티오카바메이트는 디아밀 디티오카바메이트 같은 바람직하게 C2-12를 함유하는 디알킬 디티오카바메이트이다. 특히 바람직한 화합물은 징크 디아밀 디티오카바메이트이다.
황은 또한 머캅타이드 특히 지방족 머캅단의 머캅타이드(상기한 바와 같이 코퍼 머캅타이드를 포함하는), 황화 올레핀(예컨대 US-A-4119540, US-A-4119550, US-A-4191659, US-E-4147640호) 황화 Diels-Alder 부가물(예컨대, US-A-3632566, US-A-3498915, US-A-27331) 및 특히 예컨대 고래기름 같은 고래기름 치환체와 같은 황화된 불포화 알콜 및 에스테르 등을 포함하는 황화된 불포화 유기 화합물, 디- 및 폴리설파이드, 티오에테르, 티오페놀, 티옥산테이트(상기한 바와 같이 코퍼 티옥산테이트를 포함하는), 황화 에스테르, 티오에스테르, 티오아미드 등이 포함되는 황화물 및 벤조티아졸과 특히 머캅토벤조티아졸 같은 티아졸류와 티아디아졸 같은 황화물의 형태로 주입될 수 있다.
광물성 윤활유(Mineral lubricating oil)는 황을 함유하는 반면에 합성 윤활유는 황이 없으므로 총 황 성분이 0.5-1.0wt% 이상되게 하기 위하여 황함유 화합물로서 부가되는 황의 양은 베이스스톡(Basestock)과 윤활유 조성물에 들어있는 기타 성분들의 황함량에 따라서 달라진다.
본 발명의 윤활유 조성물은 이롭게도 총 0.5-0.7wt%의 S과 가장 바람직하게 부가되는 지용성 황함유 화합물로서 0.5wt%의 S을 함유한다. 이 조성물은 바람직하게 0.01-0.5wt%의 Zn, 바람직하게는 0.05-0.2wt%의 Zn을 함유한다. 특히 바람직한 조성물은 0.5-3wt%의 징크 디티오카바메이트를 함유한다.
베어링 부식억제제는 Cu/Pb 베어링 같은 베어링에서 부딪힐 수 있는 구리 얼룩과 높은 질량 감소와 같은 부식 문제점들을 억제하는데 효과적이다. 이러한 부가제들은 오일의 마모방지 성능을 촉진한다고 발견되었다. 바람직한 베어링 부식억제제는 B(OR)3, (RO)2B-O-B(OR)2, (ROBO)3(RO)2BOR'OB(OR)2및 이들 혼합물(여기서 R은 치환되거나 또는 비치환된 알킬, 아릴 또는 아랄킬 그룹 또는 두 그룹 R이 치환되거나 또는 비치환된 알킬렌 그룹을 형성하며 R'은 치환되거나 또는 비치환된 알킬렌 그룹이다) 같은 보레이트 에스테르이며 이러한 물질들은 예컨대 알콕시 알칸올 (US-A-4440656에서와 같이 모두 단쇄 알칸올이고 장쇄 알콜), 폴리에테르알칸올 같은 알콜류 ; 예컨대 US-A-2866811호에서의 2-에틸헥산올, 2-에틸헥산-1,3-디올, 부탄-1,2-디올, 부탄-1,3-디올, 글리세롤 및 아크릴산 폴리올 같은 모노-, 디- 및 트리하이드록시 알칸올 ; 예컨대 올레인산과 트리스(하이드록시메틸)-아미노메탄으로부터 유도된 옥사졸린류 ; 글리세릴 모노-올레이트 같은 하이드록시 에스테르 ; 에폭사이드와 예컨대 t-도데실-메캅토에탄올 같은 모캅탄을 반응시켜 얻을 수 있는 황-함유 알콜 ; 1차 아민(예컨대 올레일아민) 또는 2차 아민을 에틸렌 또는 프로필렌옥사이드와 US-A-4406802 화합물을 반응시켜 얻은 하이드록시아민, 트리에탄올아민 및 트리이소프로판올아민인 알칸올아민 같은 아미노알콜 등으로부터 유도될 수 있다. 바람직한 알콜은 2-메틸펜탄-1,3-디올, 부탄-1,2-디올, 부탄-1,3-디올 및 유사한 1,2 및 1,3 디올과 에톡시에탄올이다.
본 발명의 바람직한 일면으로 0.01-10wt%, 바람직하게는 0.1-5wt%의 보레이트 에스테르, 특히 예컨대 트리스(에톡시에틸)오르토보레이트 에스테르 또는 메타보레이트 에스테르 같은 폴리에테르알칸올 또는 알콕시알칸올, 또는 부탄-1,3-디올 같은 디올의 바이보레이트를 함유한다.
한편 베어링 부식억제제는 티아디아졸 머캅탄 특히 C5-50을 함유하는 티아디아졸 폴리설파이드, 이들의 중합체 또는 유도체이다. 바람직한 물질은 US-A-2719125, 2719126 및 3087932호에 기재된 것과 같은 1, 3, 4 티아디아졸 폴리설파이드이다. 특히 바람직한 화합물은 2, 5-비스(t-옥타디티오)-1,3,4-티아디아졸인 Amoco 150 또는 2,5-비스(노닐디티오)-1,3,4-티아디아졸인 Amoco 158이다. 이와 유사한 기타 적합한 물질은 US-A-3821236, 3904537, 4097387, 4107059, 4136043, 4188299, 4193882호에 기재된 것들이다. 티아디아졸 머캅탄의 유도체들은 에스테르, 할로겐화 카복실산과의 축합생성물, 알데히드와 아민의 반응생성물, 알콜 또는 머캅탄, 아민염, 디티오카바메이트, 무회 분산제와의 반응 혼합물(예컨대, US-A-4140643 및 US-A-4136043) 및 할로겐화 황 및 올레핀과의 반응생성물 같이 이용된다.
이러한 물질들은 윤활유 조성물의 0.01-10wt%, 바람직하게는 0.1-5.0wt% 정도 존재한다.
본 윤활유 조성물은 소량의 인, 0.01wt% 미만, 바람직하게는 0.005wt% 미만의 인을 함유하지만 실질적으로 인이 전혀없는 윤활유 조성물이 바람직하다.
바람직한 일면으로서 본 윤활유 조성물은 다음으로 더욱 구성된다.
(A)(i) 장쇄 탄화수소 치환된 모노 및 디카복실산 또는 이들 무수물의 지용성 염, 아미드, 이미드, 옥사졸린 및 에스테르 또는 이들의 혼합물 ; (ii) 폴리아민이 직접 붙은 장쇄 지방족 탄화수소 ; 및 (iii) 1-2.5몰의 포름알데히드로 치환된 장쇄 탄화수소 페놀과 폴리알킬렌 폴리아민을 0.5-2몰 비로 축합시켜 만든 Mannich 축합 생성물 ; (여기서, 장쇄 탄화수소 그룹은 C2-C5모노올레핀의 중합체이고 이 중합체의 분자량은 700-5000임)로부터 바람직하게 선택된 무회의 질소 또는 에스테르 함유 분산제 화합물인 무회의 분산제 화합물 1-10wt% 및/또는 (B)(a) 비닐 알콜의 C4-24불포화 에스테르 또는 C3-C10불포화 모노- 또는 디-카복실산과 C4-20을 갖는 불포화 질소 함유 단량체와의 중합체 ; (b) 아민, 하이드록시아민 또는 알콜로 중화된 불포화 C3-C10모노-또는 디-카복실산과 C2-C20올레핀의 중합체 ; 및 (c) C4-C20불포화 질소 함유 단량체 위에 접목되거나 또는 불포화산이 중합체 주쇄에 접목되어 더욱 반응한 뒤 상기 카복실산이 아민, 하이드록시아민 또는 알콜과 반응하는 에틸렌과 C3-C20올레핀의 중합체를 포함하는 질소 또는 에스테르를 함유하는 점도지수 개선 중합체 분산제 0.3-10wt%.
질소를 함유하는 분산제 부가제는 예컨대 US-A-3275554, US-A-3565804, US-A-3442808, US-A-3442808, GB-A-983040 또는 BE-A-658236호에서 나타내진 것과 같은 크랭크실 모터 오일용 슬러지 분산제로서 업계에 공지된 것이다.
가장 널리 이용되는 분산제는 예컨대 폴리이소부텐일 숙신산 무수물과 US-A-3202678, 3154560, 3172892, 3024195, 3024237, 3219666, 3216936 및 BE-A-662875호에 기재된 아민 같은 알켄일 숙신산 무수물을 반응시켜 형성된 것이다.
한편 무회 분산제는 장쇄 탄화수소 치환된 카복실산으로부터 유도된 에스테르 및 모노하이드릭, 폴리하이드릭 알콜 같은 하이드록시 화합물로부터 유도된 에스테르 또는 예컨대 US-A-3522179호에서 제조한 바와 같은 페놀 및 나프톨같은 방향족 화합물이다.
분산제를 만들기 위한 앞서 언급한 장쇄 탄화수소 치환된 카복실산과 반응할 수 있는 하이드록시아민에는 2-아미노-1-부탄올, 2-아미노-2-메틸-1-프로판올, P-(베타-하이드록시에틸)-아닐린, 2-아미노-1-프로판, 3-아미노-1-프로판올, 2-아미노-2-메틸-1,3-프로판-디올, 2-아미노-2-에틸-1,3-프로판디올, N-(베타-하이드록시-프로필)-N'-(베타-아미노에틸)-피페라진, 트리스(하이드록시메틸)아미노-메탄(트리스메틸올아미노메탄 이라고도 함), 2-아미노-1-부탄올, 에탄올 아민, 베타-(베타-하이드록시에톡시)-에틸아민 등이 있다.
바람직한 분산제는 예컨대 펜타에리트리톨, 트리스메틸올아미노메탄, 폴리옥시프로필렌 디아민 같은 폴리옥시에틸렌 및 폴리옥시프로필렌 아민류, 테트라에틸렌 펜타아민 같은 폴리에틸렌 아민류와 폴리이소부텐일숙신산 무수물로부터 유도된 것들이거나 이들의 결합물이다. 한가지 특히 바람직한 분사제 결합물은 (A)폴리이소부텐일 숙신산 무수물과 (B)펜타에리트리톨 같은 하이드록시 화합물 (C) 폴리옥시프로필렌 디아민 같은 폴리옥시알킬렌 폴리아민 및 (D) 폴리에티렌 디아민 및 테트라에틸렌 펜타아민 같은 폴리알킬렌 폴리아민의 결합물을 US-A-3894763호에 기재된 바와 같이 (A) 1당량 당 약 0.01-약 2당량의 (C)와 약 0.01-약 4당량의 (B) 및 (D)를 사용하여 만든다. 또다른 바람직한 분산제 결합물은 (A) 폴리이소부텐일 숙신산 무수물과 (B) 테트라에틸렌 펜타이민 같은 폴리알킬렌 폴리아민 및 (C) US-A-3632511호에 기재된 펜타에리트리톨 또는 트리스메틸올 아미노메탄 같은 폴리하이드록시-치환된 지방족 1차 아민 또는 폴리하이드릭 알콜의 결합물이다.
알켄일 숙신산 폴리아민 형태의 분산제는 US-A-3087936호와 3254025호에서 생각하였듯이 아실화된 질소화합물 1몰당 붕소의 원자비율이 0.1-10이 되게하는 양의 산화붕소, 할로겐화붕소, 붕산 및 붕산의 에스테르 같은 붕소화합물로 더욱 변형될 수 있다. US-A-4113639에 기재된 것과 같이 분산제의 혼합물이 이용될 수도 있다.
오일은 1.0-10wt%, 더욱 바람직하게는 2.0-7.0wt%의 이러한 분산제를 함유할 수 있다.
예컨대 알킬 메타아크릴레이트와 N-비닐피롤리돈 또는 디메틸아미노알킬 메타아크릴레이트의 공중합체, 알킬푸마레이트-비닐아세테이트, N-비닐 피롤리딘 공중합체, US-A-4149984호에서와 같이 알킬렌 폴리아민 또는 알콜과 더욱 반응할 무수말레인산 같은 활성 단량체와 에틸렌-프로필렌의 포스트-그라프티드인터폴리마 ; 또는 알콜 및 아민과 후에 반응하는 스티렌/말레인산 무수물 중합체, US-A-3702300호에서와 같이 아실화된 중합체의 에톡시화 유도체 같은 점도지수개선 중합체 분산제를 0.3-10% 부가하며 이러한 분산성을 얻게된다.
마그네슘 및/또는 칼슘을 함유하는 부가제는 종종 윤활유 조성물에 혼자 이용되거나 또는 나트륨을 함유하는 것과 같은 알카리토금속 부가제 또는 기타 알카리금속 부가제와 결합되어 이용될 수 있다. 이들은 또한 술폰산, 알킬페놀, 황화알킬페놀, 알킬살리실레이트, 나프테네이트 및 기타 지용성 모노- 및 디-카복실산 등의 금속염의 형태로 존재할 수 있다.
고 염기성 알카리토금속 알카릴 설포네이트는 예컨대 US-A-3150088호 및 3150089호에 나타낸 것이 일반적이다. 본 발명의 목적으로, 바람직한 알카리토 설포네이트는 총 염기수(TBN, ASTM D 2896법으로 측정한)가 300-400범위인 마그네슘 또는 칼슘 알킬 방향족 설포네이트이다.
알킬치환된 살리실산 또는 나프텐산 또는 이들의 혼합물 또는 이 둘과 알킬치환된 페놀과의 혼합물 등으로부터 쉽게 유도될 수 있는 메틸렌 및 황으로 가교된 물질과 같은 다가의 금속알킬 살리실레이트 및 나프토네이트 물질이 또한 포함된다. 염기성 황화 살리실레이트 및 이의 제조방법의 US-A-3595791호에 기재되었다.
황화된 금속 페네이트는 다음 일반식으로 대표되는 천연 또는 염기성 화합물 또는 이러한 화합물의 중합체 형태로 이야기할 수 있는 "페놀 설파이드의 금속염"으로 생각할 수 있다.
Figure kpo00001
식중, R은 알킬 라디칼, n 및 X는 서로 1-4까지의 정수이고 모든 R그룹내의 평균 탄소원자수는 오일내의 적당한 용해도를 맞추기 위하여 최소한 약 9이다. x=1 또는 2, n=0,1 또는 2.
각각의 R그룹은 5-40, 바람직하게는 8-20개의 탄소원자를 함유한다. 금속염은 황화된 금속 페네이트에 원하는 알칼리도를 부여하기에 충분한 양의 금속 함유 물질을 알킬 페놀설파이드와 반응시켜 제조된다.
황화된 알킬 페놀은 상기 페놀을 중화시키거나, 만일 원한다면 업계에 공지된 방법으로 생성물의 원하는 알카리도를 얻도록 과염기화시키기에 충분한 양의 산화물, 수산화물 및 착화물 등이 포함되는 금속 함유 물질과 반응시켜 전환된다. 바람직한 방법은 글리콜에테르내의 금속 용액을 이용한 중화이다.
상기한 마그네슘 및 칼슘 함유 부가제는 비록 다른면으로는 이롭지만 윤활유의 산화를 증가시킨다. 고염기성 설포네이트에 대해서는 특히 그러하다.
그러므로 본 발명의 바람직한 구체예는 2-8000ppm의 칼슘 및/또는 마그네슘을 함유하는 크랭크실 윤활유 조성물을 제공한다.
마그네슘 및/또는 칼슘은 일반적으로 설포네이트 및 페네이트 같은 염기성 또는 천연 청정제로 존재하며 바람직한 부가제는 염기성 마그네슘 또는 칼슘설포네이트이다. 이러한 부가제로부터 500-5000ppm의 칼슘 및/또는 마그네슘을 함유한 오일이 바람직하다.
본 발명의 이들 조성물은 이와 다를 수도 있고 이에 부가하여 예컨대 바륨, 나트륨, 칼륨 또는 리튬을 함유하는 것과 같은 기타 유사한 금속을 함유한 청정부가제를 함유할 수 있다.
본 윤활유 조성물에 이용되는 윤활유는 광물성 윤활유 또는 합성윤활유 또는 이들의 혼합물일 수 있다. 적합한 합성 오일에는 디(2-에틸-헥실)세바세이트, 아셀레이트 및 아디페이트 같은 디에스테르오일 ; 디카복실산 글리콜 및 1염기산 또는 모노하이드릭알콜로 형성된 것과 같은 착물 에스테르오일 ; 실리콘오일 ; 설파이드에스테르 ; 유기 카보네이트 ; 탄화수소 오일 및 기타 업계에 공지된 합성 오일이 있다. 본 발명은 특히 광물성 윤활유에 유용하며 일반적으로 이용되는 것보다 낮은 산화방지 특성을 갖는 베이스스톡 오일을 이용할 수 있다는 부가적인 잇점을 갖는다.
본 발명의 윤활유 조성물은 만일 이들중 인이 전혀없다면 예컨대 올레인산 및 이들의 유도체 즉, N-올레일사르코신, 올레인산 이합체 및 삼합체, 레시틴, 솔비탄 모노-올레이트, 도데실 숙신산 무수물 또는 에톡시화된 알킬페놀 등과 같은 녹억제제 ; 비닐 아세테이트와 코코낫 오일 알콜의 푸마르산 에스테르와의 공중합체 같은 유동점 강하제 ; 및 올레핀 공중합체 또는 폴리메타아크릴레이트 같은 점도지수 개선제 등의 전형적인 기타 윤활유 부가물을 함유한다.
구리가 없는 오일에서 징크 디알킬디티오포스페이트에 때때로 기타 산화방지제를 부가할 필요가 있는데 이는 오일의 산화적 안정성을 증대시키기 위해서이다. 특히 베이스스톡의 산화적 안정성이 나쁠 경우에 이러한 보충 산화방지제가 포함되며 오일에 부가되는 보충 산화방지제의 양은 0.1-1.5wt%이다. 이용되는 보충 산화방지제에는 페놀, 입체장해된 페놀, 비스-페놀 및 황화된 페놀, 카테콜(catechol), 알킬화 카테콜 및 황화된 알킬 카테콜, 디페닐아민 및 알킬디페닐아민, 페닐-1-나프탈아민 및 이들의 알킬화 유도체 등이 포함된다.
소량의 구리를 포함시키면 일반적으로 보충 산화방지제를 이용할 필요가 없게 된다. 그러나 실제로 인이 전혀 사용되지 않았다면 이러한 보충 산화방지제가 오일내에 존재하는 경우 특히 극심한 조건하에서 조작될 때 이 보충 산화방지제는 본 발명의 일면에 포함된다.
윤활유용 부가제는 일반적으로 벌크 윤활유에 합침시키기 위하여 오일내의 농축물 형태로 제공된다. 그러므로 본 발명은 (1) 0.1wt% 미만의 인 : (2) 1-50wt%의 지용성 황함유 화합물 ; (3) 0.005-2wt%의 구리 ; 및 (4) 0.1-20wt%의 베어링 부식억제제 및 임의로 (5) (a) 0-60, 예컨대 10-60wt%의 무회의 분산제 화합물 (b) 일반적으로 다른 점도지수 개선제가 따로 부가된다 하더라도 0-40, 예컨대 3-40wt%의 점도지수 개선 중합체 분산제로 구성된 그룹으로부터 선택된 분산제를 함유하는 오일용액으로 구성된 농축물을 제공한다.
이 농축물은 또한 앞서 기재한 점도지수 개선제 및 청정제 같은 기타 부가제들을 함유할 수 있다. 특히 바람직한 농축물은 마그네슘 및/또는 칼슘을 함유하는 부가제를 포함하며 그러므로 본 발명은 0.01-8wt%의 칼슘 및/또는 마그네슘으로 더욱 구성된 농축물을 제공한다.
다음 실시예는 단지 본 발명을 예시할 뿐이며 본 발명의 보다 상세한 일면을 나타낼 것이다.
[비교실시예 I-VI 및 실시예 1-4]
다음 본 발명의비교실시예와 실시예에서의 제제는 윤활유 조성물에 적합하고 0.3wt%의 황을 함유하는 희석오일과 균형을 맞춰 표 1에 수득된 양의 부가제를 결합하여 제조하였다. 사용된 부가제들은 다음과 같다 :
A는 21%의 다기능 에틸렌-프로필렌 공중합체를 함유하는 오일용액 및 0.29 wt% N을 함유하는 분산제 V.I. 부가제.
B는 폴리이소부텐일 라디칼을 갖고 분자량이 약 950인 붕소화된 폴리이소부텐일 숙신아미드의 50wt% 오일용액으로 구성되고 1.6wt%의 N과 0.35wt%의 B를 함유하는 무회 분산제.
C는 TBN가 400이고 마그네슘 함량이 9.2wt%, 황함량이 1.7wt%인 과염기성의 마그네슘 설포네이트의 오일용액.
D는 TBN이 300, 칼슘 함량이 11.9wt%이며 황함량이 .9wt%인 과염기성의 칼슘 설포네이트의 오일용액.
E는 4wt% 구리를 함유하는 코퍼 올레이트의 오일용액.
F는 오일내에서의 입체 장해로된 메틸렌 비스-페놀 산화방지제의 30wt% 용액.
G는 Ciba-Geigy의 상표 Irganox L-57인 알킬화된 디페닐아민 산화방지제.
H는 6wt% 아연과 12wt% 황을 함유하는 징크 디아밀디티오카바메이트의 50wt% 오일용액.
J는 5wt% 붕소로 구성된 에톡시 에탄올로 만든 오르토보레이트 에스테르.
K는 Amoco Chemical Company의 상표 Amoco 158인 33wt% 황으로 구성된 2,5-비스(노닐디티오)-1,3,4-티아디아졸.
L은 옥토에이트인 몰리브데늄 12wt%를 함유하는 오일용액.
M은 Emery Corporation에서 만든 상표 Emery 9844인 황화된 에스테르 고래기름 치환체이며 11.5wt%의 황으로 구성되었다.
제제는 다음 표준 시험법에 따라 시험하였다 :
ASTM STP 315M part III에 따르는 Seq. IIID 엔진시험으로 캠(cam)과 리프터(lifter)의 최대 및 평균 마모량을 측정하였다. 이 시험에서 최대 마모량이 0.02cm(0.08in.) 이상, 평균 마모량이 0.01cm(0.004 in.) 이상이면 성공한 것이다.
seq. IID 시험에서 동적 점성도 증가는 40℃에서 64시간 내에 증가된 퍼센테이지로서 측정된다. 64시간 내에 증가된 점도가 375%를 넘지 않으면 성공한 것이다.
ASTM STP 509A PE IV에 기초한 CRC-L-38 스크리너 엔진시험으로 베어링 질량 감소(BWL)를 측정하였다. BWL이 40mg을 넘지 않으면 이 시험은 성공한 것이다.
결과는 표 2에 수록하였다. 이 결과로 본 발명의 인이 함유되지 않은 윤활유가 산화방지, 마모방지, 베어링 부식억제를 나타낸다는 것을 보여준다. 비교실시예 I, II 및 III은 베어링 부식억제제가 없어 마모성능이 부적당하다는 것을 보여준다. 비교실시예 IV는 몰리브데늄 부가제를 부가하면 마모성능이 개선된다는 것을 나타낸다. 비교실시예 V는 비록 통상적인 양의 공지된 기타의 산화방지제를 넣었어도 구리 산화방지제가 없으면 성능이 떨어진다는 것을 나타낸다.
비교실시예 V과 실시예 2를 비교해보면 구리를 사용하면 산화방지 성능이 개선될 뿐만 아니라 마모방지 성능도 놀랍게 개선된다는 것을 알 수 있다. 본 발명의 실시예에서 제제의 성능은 단지 개개 부가제들의 성능을 종합한 것이 아니라 통상적인 오일에 이용되는 수준보다 낮은 수준의 인을 함유하지만 보다 개선된 마모방지, 산화방지 및 베어링 부식억제 성능을 나타낸다.
Figure kpo00002
Figure kpo00003
[비교실시예 VII-IX 및 실시예 5-7]
최신식 엔진의 크랭크실용 윤활유 성능의 주된 인자는 산화를 억제하고, 특히 과도한 점도증가를 피하는 것이다. 점도증가를 억제하는 본 발명의 조성물의 효과는 상기 실시예 1-4에서 시범된 Seq. IIID 엔진 시험으로 실행되었다. 내연기관의 산화, 철 접촉 조건을 실행하기 위해 고안된 벤치 시험-ERCOT 시험-으로 더욱 실현하였다.
ERCOT 시험에서, 페릭 아세틸 아세토네이트로서 철 40ppm를 함유하는 300g 미만의 오일 조성물을 165℃에서 공기를 1분당 1.7ℓ로 통과시켜 산화시키고 Hakke 점도계를 이용하여 64시간 동안 증가된 점도 차이를 측정하였다. 결과는 센티포아즈(cp)로 나타냈다.
비교실시예 VII-IX는 WO-A-8604601호의 실시에 11, WO-A-8604602호의 실시예 13 및 WO-A-06092호의 실시예 IX을 따랐으나 이 실시에에 정의된 유사한 물질을 이용하였다. 비교실시예에서는 구리를 이용하지 않았으며, 다음 표 3은 점도 조절에 부적당하다는 것을 나타내는 반면 실시예 5-7에서 본 발명의 조성물은 엔진오일이 소모되는 시간까지인 장시간 동안 산화되는 조건하에 있게되는 최신 오일에 이용하기에 효과적이었다.
앞서 정의된 성분들의 일부분으로 다음과 같은 부가제들이 사용되었다 :
N은 분산제 B와 유사한 분산제이지만 폴리이소부텐일 라디칼의 분자량은 약 1300이고 이 분산제는 1.46wt%의 N과 0.32wt%의 B를 함유한다.
P은 7.0wt%의 P와 7.7wt%의 Zn을 함유하는 디이소옥틸 징크 디티오포스페이트의 오일용액(90% 활성성분)으로 구성된 마모방지 부가제이다.
Figure kpo00004
농축물- 상기 제제를 제공하기 위한 대표적인 농축물
Figure kpo00005
농축물은 조작을 용이하게 하기 위한(점도감소) 약간의 희석 오일을 함유할 수도 있다.

Claims (24)

  1. 다량의 윤활유가 지용성 형태로 부가된 구리 5-500ppm(중량 기준), 총 황함량이 0.5-2.0wt%가 되도록 부가된 하나 이상의 지용성 황함유 화합물 및 유효량의 베어링 부식 억제제로 구성되며 0.01wt% 미만의 인을 함유하는 자동차 엔진에 사용하는 크랭크실 윤활유 조성물.
  2. 제1항에 있어서, 부가된 구리의 양이 10-400ppm인 조성물.
  3. 제2항에 있어서, 부가된 구리의 양이 10-200ppm인 조성물.
  4. 제3항에 있어서, 부가된 구리의 양이 60-200ppm인 조성물.
  5. 제1항 내지 제4항에 있어서, 구리가 C10-C18지방산, 불포화 카복실산, 분자량이 200-500인 나프텐산 또는 알킬 또는 알케닐 치환된 디카복실산의 구리염 형태로 오일에 혼합되거나 또는 일반식 (RR'NCSS)nCu[식중, n이 1 또는 2이고, R 및 R'가 동일하거나 상이한 바 C1-18을 함유하는 하이드로카빌 라디칼임]의 지용성 코퍼 디티오카바메이트, 코퍼 설포네이트, 코퍼 페네이트 또는 코퍼 아세틸아세토네이트로 오일에 혼합되는 조성물.
  6. 제1항에 있어서, 지용성 황 화합물이 일반식 (RR'NCSS)nM(식중, R, R' 및 n은 제5항에서의 정의한 바와 같고 M은 금속임)의 디티오카바메이트 또는 머캅타이트, 황화된 불포화 유기 화합물, 설파이드, 티오에테르, 티오페놀, 티옥산테이트, 황화된 에스테르, 티오에스테르, 티오아미드, 티아졸 또는 티아디아졸인 조성물.
  7. 제6항에 있어서, 지용성 화합물이 C2-12를 함유하는 디알킬 디티오카바메이트인 조성물.
  8. 제1항에 있어서, 지용성 황함유 화합물로 부가된 0.1-0.5wt%의 황을 포함하여 총 황함량이 0.5-1.0wt%인 조성물.
  9. 제1항에 있어서, 0.01-0.5wt%의 Zn을 함유하는 조성물.
  10. 제6항에 있어서, 0.5-3wt%의 징크 디티오카바메이트를 함유하는 조성물.
  11. 제1항에 있어서, 베어링 부식억제제가 하기 일반식의 하나 이상의 보레이트 및/또는 C5-50을 함유하는 티아디아졸 폴리설파아드 및 이들의 유도체 또는 중합체로 구성되는 조성물.
    B(OR)3, (RO)2B-O-B(OR)2, (ROBO)3또는 (RO)2BOR|1OB(OR)2
    식중, R은 치환되거나 비치환된 알킬, 아릴 또는 아랄킬 그룹 또는 두개의 그룹 R이 함께 치환된 또는 비치환된 알킬렌 그룹을 형성하고 R1은 치환되거나 또는 비치환된 알킬렌 그룹임.
  12. 제11항에 있어서, 0.01-10wt%의 보레이트 에스테르를 함유하는 조성물.
  13. 제11항 또는 제12항에 있어서, 보레이트 에스테르가 트리스(에톡시에틸)오르토보레이트 에스테르 또는 부탄-1,3-디올의 바이보레이트인 조성물.
  14. 제11항에 있어서, 0.01-10wt%의 2,5-비스(t-노닐디티오)-1,3,3-티아디아졸을 함유하는 조성물.
  15. 제1항에 있어서, 0.005wt% 미만의 인을 함유하는 조성물.
  16. 제15항에 있어서, 실질적으로 인을 함유하지 않는 조성물.
  17. 제1항에 있어서, (A) 1-10wt%의 무회(ashless) 분산제 화합물 및/또는 (B) 질소 또는 에스테르를 함유하는 0.3-10wt%의 점도지수 개선 중합체 분산제를 추가로 포함하는 조성물.
  18. 제1항에 있어서, 2-8000ppm의 칼슘 및/또는 마그네슘을 포함하는 조성물.
  19. 제18항에 있어서, 염기성 칼슘 및/또는 마그네슘 설포네이트로서 500-5000ppm의 칼슘 및/또는 마그네슘을 포함하는 조성물.
  20. 제1항에 있어서, 하나 이상의 녹억제제, 유동점 강하제(pour point depressan ts), 추가의 산화방지제 및 점도지수 개선제를 추가로 포함하는 조성물.
  21. (1) 0-.1wt% 미만의 인 ; (2) 1-50wt%의 지용성 황함유 화합물 ; (3) 0.005-2wt%의 구리 ; (4) 0.1-20wt%의 베어링 부식억제제 ; 및 (5) 0-60wt%의 무회 분산제 및/또는 점도지수 개선 중합체 분산제를 함유하는 오일용액으로 구성된 농축물.
  22. 제21항에 있어서, 0.01-8wt%의 칼슘 및/또는 마그네슘을 추가로 포함하는 조성물.
  23. 지용성 황함유 화합물, 베어링 부식억제제, 무회 분산제 및/또는 점도지수 개선 중합체, 분산제 및 칼슘 및/또는 마그네슘 함유 청정제로 구성되고 아연과 인을 함유하지 않는 윤활유 조성물에서 산화방지제로 사용되는 지용성 구리의 용도.
  24. 산화, 마모 및 부식을 억제시키고 최소한 API 엔진 요구 규격의 표준 규격 SF 및/또는 CD의 품질 규격에 부합될 수 있도록 0.01wt% 미만의 인을 함유하는 자동차 엔진용 크랭크실 윤활유 조성물에 사용되는, 지용성 형태로 존재하는 부가된 구리 5-500ppm, 총 0.5-2.0wt%의 황 및 베어링 부식억제제 조합물(combination)의 용도.
KR1019880002058A 1987-02-27 1988-02-27 인 함량이 낮은 윤활유 Expired - Fee Related KR960014933B1 (ko)

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EP0444830A1 (en) * 1990-02-26 1991-09-04 Ethyl Petroleum Additives Limited Succinimide composition
EP0814148B1 (en) * 1992-12-21 2002-10-02 Oronite Japan Limited Low phosphorous engine oil compositions and additive compositions
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GB9405903D0 (en) * 1994-03-24 1994-05-11 Exxon Chemical Patents Inc Lubricating compositions
GB9409756D0 (en) * 1994-05-16 1994-07-06 Exxon Chemical Patents Inc Lubricating compositions
GB0021041D0 (en) * 2000-08-29 2000-10-11 Exxonmobil Res & Eng Co Low phosphorus lubricating oil composition
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JP2004083746A (ja) 2002-08-27 2004-03-18 Nippon Oil Corp 内燃機関用潤滑油組成物
JP4578115B2 (ja) 2004-02-04 2010-11-10 Ｊｘ日鉱日石エネルギー株式会社 潤滑油組成物
JP2005220197A (ja) * 2004-02-04 2005-08-18 Nippon Oil Corp 鉛含有金属材料と接触する潤滑油組成物
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JP4663288B2 (ja) * 2004-10-19 2011-04-06 Ｊｘ日鉱日石エネルギー株式会社 鉛含有金属材料と接触する潤滑油組成物
WO2006043527A1 (ja) * 2004-10-19 2006-04-27 Nippon Oil Corporation 潤滑油組成物
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US20100081591A1 (en) * 2008-09-30 2010-04-01 Chevron Oronite Company Llc Lubricating oil compositions
EP2559748B1 (en) * 2011-08-19 2016-06-08 Infineum International Limited Lubricating oil composition
JP6480323B2 (ja) * 2015-12-28 2019-03-06 Ｊｘｔｇエネルギー株式会社 潤滑油組成物
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US20250115825A1 (en) * 2022-02-28 2025-04-10 Chevron Oronite Company Llc Lubricating oil compositions
US20240141250A1 (en) 2022-10-18 2024-05-02 Infineum International Limited Lubricating Oil Compositions
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AU1235188A (en) 1988-09-01
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EP0280580A2 (en) 1988-08-31
SG50093G (en) 1993-06-25
DE3875630T2 (de) 1993-03-18
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DK103788A (da) 1988-08-28
ATE82020T1 (de) 1992-11-15
GB8704682D0 (en) 1987-04-01
DK103788D0 (da) 1988-02-26
BR8800835A (pt) 1988-10-04
JP2505019B2 (ja) 1996-06-05
ES2045102T3 (es) 1994-01-16
EP0280580B1 (en) 1992-11-04
AU603186B2 (en) 1990-11-08
EP0280580A3 (en) 1989-07-12
NO880846D0 (no) 1988-02-26

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