KR970011370B1 - Lubricating composition - Google Patents
Lubricating composition Download PDFInfo
- Publication number
- KR970011370B1 KR970011370B1 KR1019890012929A KR890012929A KR970011370B1 KR 970011370 B1 KR970011370 B1 KR 970011370B1 KR 1019890012929 A KR1019890012929 A KR 1019890012929A KR 890012929 A KR890012929 A KR 890012929A KR 970011370 B1 KR970011370 B1 KR 970011370B1
- Authority
- KR
- South Korea
- Prior art keywords
- composition
- soap
- weight percent
- copolymer
- vinyl acetate
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/06—Mixtures of thickeners and additives
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
- C10M117/02—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
- C10M117/04—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen containing hydroxy groups
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
- C10M143/02—Polyethene
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
- C10M143/06—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation containing butene
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M145/00—Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
- C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M145/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of a saturated carboxylic or carbonic acid
- C10M145/08—Vinyl esters of a saturated carboxylic or carbonic acid
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M145/00—Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
- C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M145/10—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate
- C10M145/12—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate monocarboxylic
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/022—Ethene
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/026—Butene
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- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
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- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/06—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing conjugated dienes
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
- C10M2207/1245—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof used as thickening agent
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- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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- C10M2207/10—Carboxylix acids; Neutral salts thereof
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- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
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- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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- C10M2207/10—Carboxylix acids; Neutral salts thereof
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- C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an alcohol or ester thereof; bound to an aldehyde, ketonic, ether, ketal or acetal radical
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- C10M2209/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of saturated carboxylic or carbonic acid
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- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of saturated carboxylic or carbonic acid
- C10M2209/062—Vinyl esters of saturated carboxylic or carbonic acids, e.g. vinyl acetate
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- C10M2209/082—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type monocarboxylic
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- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
- C10M2209/084—Acrylate; Methacrylate
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
- C10M2209/086—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type polycarboxylic, e.g. maleic acid
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- C10N2010/00—Metal present as such or in compounds
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- C10N2010/02—Groups 1 or 11
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- C10N2010/00—Metal present as such or in compounds
- C10N2010/04—Groups 2 or 12
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- C10N2010/06—Groups 3 or 13
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
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- C10N2040/02—Bearings
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/06—Instruments or other precision apparatus, e.g. damping fluids
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- C10N2040/30—Refrigerators lubricants or compressors lubricants
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- C10N2040/32—Wires, ropes or cables lubricants
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- C10N2040/38—Conveyors or chain belts
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- C10N2040/42—Flashing oils or marking oils
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- C10N2040/50—Medical uses
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- D—TEXTILES; PAPER
- D07—ROPES; CABLES OTHER THAN ELECTRIC
- D07B—ROPES OR CABLES IN GENERAL
- D07B1/00—Constructional features of ropes or cables
- D07B1/14—Ropes or cables with incorporated auxiliary elements, e.g. for marking, extending throughout the length of the rope or cable
- D07B1/141—Ropes or cables with incorporated auxiliary elements, e.g. for marking, extending throughout the length of the rope or cable comprising liquid, pasty or powder agents, e.g. lubricants or anti-corrosive oils or greases
- D07B1/144—Ropes or cables with incorporated auxiliary elements, e.g. for marking, extending throughout the length of the rope or cable comprising liquid, pasty or powder agents, e.g. lubricants or anti-corrosive oils or greases for cables or cable components built-up from metal wires
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Forging (AREA)
Abstract
요약 없음No summary
Description
본 발명은 개서된 저온 및 고온 특성을 갖는 윤활 조성물, 이의 제조방법 및 이의 용도, 특히 개방 기어 윤활제로서의 이의 용도에 관한 것이다.The present invention relates to a lubricating composition having modified low temperature and high temperature properties, a process for its preparation and its use, in particular its use as an open gear lubricant.
종종, 윤활 조성물은 극한의 고온 및 저온에서 만족스러운 성능을 요구하는 용도에 사용된다. 상기 용도의 실예로는 채광 서블(shovel)상의 회전 기어, 볼 밀(ball mill)상의 거대한 개방기어 등이 있다. 상기 타입의 제품을 사용하는자의 주요 불만은 이들 제품이 차가운 온도에서 매우 깨지기 쉽고 보다 따뜻한 온도에서는 "불량 상태"("run-off")가 되기 쉽다는 것이다.Often, lubricating compositions are used in applications requiring satisfactory performance at extreme high and low temperatures. Examples of such applications include rotating gears on mining shovels, huge open gears on ball mills, and the like. The main complaint of using this type of product is that these products are very fragile at cold temperatures and prone to "run-off" at warmer temperatures.
상기 문제를 교정하기 위해 첨가제들의 다양한 조합이 제시되어 왔다. 예를들면, 미합중국 특허 제3,705,853호에는 윤활유, 농후제(thickner) 및 0.5 내지 200 범위의 용융지수를 갖는 에틸렌 삼원공중합체를 포함하는 그리이스 조성물이 개시되어 있다. 점도지수 개선제가 존재할 수 있지만, 에틸렌 공중합체를 함유하는 그리이스에 대해서는 전혀 언급된 바 없다(미합중국 특허 제 3,904,543 호 참조).Various combinations of additives have been proposed to correct the problem. For example, US Pat. No. 3,705,853 discloses a grease composition comprising a lubricating oil, a thicker and an ethylene terpolymer having a melt index in the range of from 0.5 to 200. Viscosity index improvers may be present, but no mention is made of greases containing ethylene copolymers (see US Pat. No. 3,904,543).
그러나, 에틸렌 공중합체를 다양한 윤활 조성물에 혼입시켜 왔다. 예를 들면, 미합중국 특허 제 4,115,343호에는 광물성 오일중의 유기실옥산 중합체의 저장 안정성 및 거품 방지 경향은 분산액에 에틸렌-비닐 아세테이트 공중합체(EVA)를 첨가하여 개선할 수 있다고 개시되어 있다. 또다른 예로서, 미합중국 특허 제3,250,714호에는 EVA가 광물성 윤활유에 대한 VI 개선제라고 개시되어 있다. 그러나 중합체의 용융지수에 대해서는 전혀 언급되어 있지 않다. 미합중국 특허 제 3,947,368 호에는 5 내지 580의 용융 지수를 갖는 EVA가 왁스성 윤활유중에 유동점 강하제로서 사용된다고 한다. 그러나 농후제가 존재하는 것에 대해서는 전혀 언급되어 있지 않다.However, ethylene copolymers have been incorporated into various lubricating compositions. For example, US Pat. No. 4,115,343 discloses that the storage stability and antifoaming tendency of organosiloxane polymers in mineral oils can be improved by adding ethylene-vinyl acetate copolymers (EVA) to the dispersion. As another example, US Pat. No. 3,250,714 discloses EVA as a VI improver for mineral lubricants. However, no mention is made of the melt index of the polymer. U.S. Patent No. 3,947,368 states that EVA having a melt index of 5 to 580 is used as the pour point depressant in waxy lubricants. However, no mention is made of the presence of thickeners.
그러므로, 상기 참고문헌중 어느 것에도 본 명세서에서 하기되는 조성물의 우수한 저온 슬럼프성(slumpability) 및 고온 접착성을 갖는 윤활 조성물이 교시되거나 개시되어 있지 않다.Therefore, none of the above references teaches or discloses lubricating compositions having good low temperature slumpability and high temperature adhesion of the compositions described herein.
가장 광의의 태양에 있어서 본 발명은 개선된 저온 및 고온 특성을 갖는 윤활 조성물에 관한 것이다. 더욱 특히, (1) 윤활유, (2) 농후제, (3) VI 개선제 및 (4) 비닐 아세테이트, 알킬 아크릴레이트, 또는 알킬 메타크릴레이트의 군으로부터 선택된 적어도 하나의 화합물과 에틸렌의 공중합체를 포함하는 윤활 조성물이 우수한 고온 접착성 및 저온 슬럼프성을 모두 갖는 것으로 확인되었다. 본 발명에 사용된 에틸렌 공중합체는 적어도 약 40g/10분의 용융지수를 가져야 하고 비닐 아세테이트, 알킬 아크릴레이트 또는 알킬 메타크릴레이트를 약 10 내지 약 40 중량%, 함유해야 한다. 바람직하게는 용융지수가 약 40 내지 약 10,000, 더욱 바람직하게는 약 40 내지 약 5000, 그리고 가장 바람직하게는 약 40 내지 약 2500g/10분이어야 한다.In the broadest aspect, the invention relates to a lubricating composition having improved low and high temperature properties. More particularly, a copolymer of ethylene with at least one compound selected from the group of (1) lubricants, (2) thickeners, (3) VI improvers and (4) vinyl acetate, alkyl acrylates, or alkyl methacrylates It was confirmed that the lubricating composition had both excellent high temperature adhesiveness and low temperature slumpability. The ethylene copolymer used in the present invention should have a melt index of at least about 40 g / 10 minutes and contain about 10 to about 40 weight percent of vinyl acetate, alkyl acrylate or alkyl methacrylate. Preferably the melt index should be about 40 to about 10,000, more preferably about 40 to about 5000, and most preferably about 40 to about 2500 g / 10 minutes.
또다른 태양에서 본 발명은 약 -20℃ 이하의 온도에서 윤활 조성물의 슬럼프성을 증가시키고 약 20℃ 이상의 온도에서 그의 접착성을 증가시키는 방법에 관한 것이다.In another aspect the present invention relates to a method of increasing the slumpability of a lubricating composition at a temperature of about −20 ° C. or less and increasing its adhesion at a temperature of about 20 ° C. or more.
본 발명의 필수성분은 윤활유, 농후제, VI 개선제 및 비닐 아세테이트, 알킬 아크릴레이트 또는 알킬 메타 크릴레이트의 군으로 부터 선택된 적어도 하나의 화합물과 에틸렌의 공중합체이다.Essential ingredients of the present invention are copolymers of ethylene with lubricating oils, thickeners, VI improvers and at least one compound selected from the group of vinyl acetates, alkyl acrylates or alkyl methacrylates.
매우 다양한 윤활유가 본 발명의 조성물을 제조하는데 이용될 수 있다. 따라서, 윤활유 기제는 통상적으로 사용되는 광물성 오일, 합성 탄화수소 오일 또는 합성 에스테르 오일 중의 어느 것일수 있다. 일반적으로 전형적인 용도에서는 40℃에서 약 10 내지 약 1,000cSt 범위의 점도를 갖는 오일이 요구되지만 상기 윤활유들은 40℃에서 약 5 내지 10,000cSt 범위의 점도를 갖는다. 윤활 조성물을 제조하는데 사용되는 광물성 윤활유 기제 원료는 파라핀성, 나프텐성 및 혼합된 기제 원유로 부터 유도된 통상적으로 정제된 기제 원료일 수 있다. 사용 될 수 있는 합성 윤활유로는 다-2-에틸헥실 세바케이트와 같은 이염기성 산의 에스테르, 테트라에텔렌 글리콜의 C13, 옥소산 디에스테르와 같은 글리콜의 에스테르 또는 세바크 산 1몰, 테트라에틸렌 글리콜 2몰 및 2-에틸헥사노산 2몰로 생성된 에스테르와 같은 복합 에스테르가 있다. 사용할 수 있는 다른 합성유로는 폴리알파올레핀 ; 알킬 벤젠[예, 벤젠을 테트라 프로필렌으로 또는 에틸렌 및 프로필렌 실리콘 오일의 공중합체(예, 에틸 페닐 폴리실옥산, 메틸 폴리실옥산 등)로 알킬화하여 얻은 알킬레이트 생성물(bottoms)] ; 폴리글리콜 오일(예, 부틸알콜과 프로필렌 옥사이드의 축합에 의해 얻어지는 오일) ; 및 카보네이트 에스테르(예, C8옥소 알콜과 에틸 카보네이트를 반응시켜 반 에스테르를 형성하고 이어서 이를 테트라에틸렌 글리콜 등과 반응시켜 얻은 생성물)가 있다. 다른 적절한 합성유로는 폴리페닐 에테르(예, 약 3 내지 7개의 에테르 결합 및 약 4 내지 8개의 페닐그룹을 갖는 에테르)가 있다(미합중국 특허 제3,424,678 호 컬럼 3 참조). 보통, 윤활유는 윤활 조성물의 대부분을 차지한다. 전형적으로, 윤활유의 양은 윤활 조성물의 약 50 내지 약 90 중량%, 바람직하게는 약 70 내지 약 85 중량%의 범위이다.A wide variety of lubricants can be used to prepare the compositions of the present invention. Thus, the lubricant base may be any of the mineral oils, synthetic hydrocarbon oils or synthetic ester oils commonly used. Generally, applications require oils having a viscosity in the range of about 10 to about 1,000 cSt at 40 ° C., but the lubricants have a viscosity in the range of about 5 to 10,000 cSt at 40 ° C. The mineral lubricant base stocks used to prepare the lubricating composition can be conventionally refined base stocks derived from paraffinic, naphthenic and mixed base crudes. Synthetic lubricants that may be used include esters of dibasic acids such as poly-2-ethylhexyl sebacate, C 13 of tetraethylene glycol, esters of glycols such as diester of oxo acid or 1 mole of sebacic acid, tetraethylene Complex esters such as esters produced with 2 moles of glycol and 2 moles of 2-ethylhexanoic acid. Other synthetic oils that can be used include polyalphaolefins; Alkyl benzenes (eg, alkylate products obtained by alkylation of benzene with tetrapropylene or with copolymers of ethylene and propylene silicone oils (eg ethyl phenyl polysiloxane, methyl polysiloxane, etc.); Polyglycol oils (eg, oils obtained by condensation of butyl alcohol and propylene oxide); And carbonate esters (e.g., products obtained by reacting a C 8 oxo alcohol with ethyl carbonate to form a half ester and then reacting it with tetraethylene glycol and the like). Other suitable synthetic oils are polyphenyl ethers (eg, ethers having about 3 to 7 ether bonds and about 4 to 8 phenyl groups) (see US Pat. No. 3,424,678 column 3). Usually, lubricants make up the majority of the lubricating composition. Typically, the amount of lubricant is in the range of about 50 to about 90 weight percent, preferably about 70 to about 85 weight percent of the lubricating composition.
윤활 조성물은 또한 윤활유에 분산되어 기제(base) 그리이스를 형성하는 농후제를 함유한다. 그러나, 사용되는 특정한 농후제가 중요한 것은 아니며 광범위하게 변할 수 있다. 예를들면, 농후제는 알루미늄, 바륨, 칼슘, 리튬, 나트륨 비누, 또는 이들의 복합물(Complex)을 기본으로 한다. 비누 농후제는 광범위한 동물성 오일, 식물성 오일 및 그리이스 뿐만아니라 이들로 부터 유도되는 지방 산으로부터 유도될 수 있다. 상기 물질들은 본 분야에서 잘 알려져 있고 예를들어, 문헌[C. J. Boner, Manufacture and Application of Lubricating Greases, Chapter 4, Robert E. Krieger Publishing Company, Inc., New York(1971)]에 기술되어 있다. 염료, 폴리우레아 및 다른 유기농후제 뿐만아니라 카본블랙, 실리카 및 점토가 사용될 수 있다. 피롤리돈을 기본으로 하는 농후제 또한 사용될 수 있다. 바람직한 농후제는 점토, 피롤리돈, 알루미늄 비누, 바륨 비누, 칼슘 비누, 리튬 비누, 나트륨 비누 또는 이들 비누의 복합물을 기본으로 한다. 특히 바람직한 농후제는 리튬 비누, 칼슘 비누, 알루미늄 비누, 이들의 복합물 또는 이들의 혼합물을 기본으로 한다. 보다 바람직한 농후제는 리튬 비누, 칼슘 비누, 이들의 복합물 또는 이들의 혼합물을 기본으로 한다. 가장 바람직한 것은 12 내지 24개(바람직하게는 16 내지 20개)의 탄소 원자를 갖는 하이드록시 지방산을 혼입시킨 리튬 또는 리튬 복합물 농후제이다. 바람직한 하이드록시 지방산은 하이드록시 스테아르 산(예 : 9-하이드록시 또는 10-하이드록시 스테아르 산)이고 그중 12-하이드록시 스테아르산이 가장 바람직하다(미합중국 특허 제3,929,651 호를 참조하고, 이의 내용은 본 명세서에서 참고로 인용되었다). 윤활제 조성물중의 농후제 양은 전형적으로 약 1 내지 약 15 중량% 범위이다. 대부분의 경우 조성물중에 농후제가 약 1 내지 약 10 중량%, 바람직하게는 약 2 내지 약 5 중량% 존재한다.The lubricating composition also contains a thickening agent that is dispersed in the lubricating oil to form a base grease. However, the particular thickener used is not critical and can vary widely. For example, the thickener is based on aluminum, barium, calcium, lithium, sodium soap, or a complex thereof. Soap thickeners can be derived from a wide range of animal oils, vegetable oils and greases as well as fatty acids derived therefrom. Such materials are well known in the art and are described, for example, in C. J. Boner, Manufacture and Application of Lubricating Greases, Chapter 4, Robert E. Krieger Publishing Company, Inc., New York (1971). Carbon black, silica and clays can be used as well as dyes, polyureas and other organic agents. Thickeners based on pyrrolidone may also be used. Preferred thickeners are based on clays, pyrrolidones, aluminum soaps, barium soaps, calcium soaps, lithium soaps, sodium soaps or combinations of these soaps. Particularly preferred thickening agents are based on lithium soaps, calcium soaps, aluminum soaps, composites thereof or mixtures thereof. More preferred thickening agents are based on lithium soaps, calcium soaps, composites thereof or mixtures thereof. Most preferred are lithium or lithium composite thickeners incorporating hydroxy fatty acids having 12 to 24 (preferably 16 to 20) carbon atoms. Preferred hydroxy fatty acids are hydroxy stearic acid (such as 9-hydroxy or 10-hydroxy stearic acid), of which 12-hydroxy stearic acid is most preferred (see US Pat. No. 3,929,651, the contents of which are incorporated herein by reference). Cited for reference). The thickener amount in the lubricant composition typically ranges from about 1 to about 15 weight percent. In most cases there is about 1 to about 10 weight percent, preferably about 2 to about 5 weight percent thickener in the composition.
VI 개선제가 또한 윤활 조성물중에 존재한다. 점도 조절제는 윤활 조성물을 승온에서도 비교적 점성 사태로 남아있게 하고 저온에서도 유용성이 있게 함으로써 윤활 조성물에 고온 및 저온에서의 작용능력을 부여하는 장쇄, 일반적으로 고분자량 중합체(폴리에스테르 포함)이다. 점도 조절제는 또한 분산성의 배가와 같은 다른 성질 또는 기능을 포함하도록 유도할 수 있다. 본 발명에 유용한 지용성 점도 조절 중합체는 일반적으로 수평균 분자량 약 300 내지 약 106, 바람직하게는 약 500 내지 약 104, 및 보다 바람직하게는 약 1,000 내지 약 2,000을 갖는다. 윤활 조성물중에 존재하는 VI 개선제의 양은 사용된 특정 VI 개선제, 그의 분자량 등에 따라 변한다. 그러나, 전형적으로 윤활 조성물의 약 5 내지 약 40 중량%(바람직하게는 약 10 내지 약 30 중량%)가 VI개선제이다.VI improvers are also present in the lubricating composition. Viscosity modifiers are long chain, generally high molecular weight polymers (including polyesters) that render the lubricating composition functional at high and low temperatures by making the lubricating composition remain relatively viscous at elevated temperatures and useful at low temperatures. Viscosity modifiers may also induce to include other properties or functions, such as doubling of dispersibility. The fat soluble viscosity controlling polymers useful in the present invention generally have a number average molecular weight of about 300 to about 10 6 , preferably about 500 to about 10 4 , and more preferably about 1,000 to about 2,000. The amount of VI improver present in the lubricating composition varies depending on the particular VI improver used, its molecular weight, and the like. Typically, however, about 5 to about 40 weight percent (preferably about 10 to about 30 weight percent) of the lubricating composition is a VI improver.
적절한 VI 개선제는 탄화수소 중합체, 폴리에스테르 또는 이의 혼합물을 기초로 할 수 있다. 적절한 탄화수소 중합체 VI 개선제의 실예로는, C2내지 C30의 단량체(예, 알파 올레핀 및 내부 올레핀 모두를 비롯한 직쇄 또는 측쇄의 지방족, 방향족, 알킬-방향족, 지환족 등일 수 있는 C2내지 C8올리핀) 들 또는 그 이상의 단족 중합체 및 공중합체가 있다. 종종, VI개선제는 이소부틸렌의 중합체, 또는 에틸렌, 프로필렌, 부텐 또는 이소부틸렌과 C2내지 C30올레핀의 공중합체이다.Suitable VI modifiers may be based on hydrocarbon polymers, polyesters or mixtures thereof. Silye a suitable hydrocarbon polymer VI improvers is, C 2 to C 30 monomers (e.g., aliphatic, aromatic, alkyl of straight or branched chain, including both alpha olefins and internal olefins - C 2 to C 8 with the like aromatic, alicyclic Olefins) or more homopolymers and copolymers. Often VI improvers are polymers of isobutylene or copolymers of ethylene, propylene, butene or isobutylene with C 2 to C 30 olefins.
이소부틸렌의 중합체 또는 부텐과 이소부틸렌의 공중합체가 바람직하며, 이소부틸렌의 중합체가 특히 바람직하다. 사용될 수 있는 다른 중합체로는 C6및 고급 알파 올레핀의 단독중합체 및 공중합체 ; 어택터 폴리프로필렌 ; (예를들어, 이소프렌 및/또는 부타디엔 및 이들의 수소화 유도체와)스티렌의 수소화 중합체, 공중합체 및 삼원공중합체가 있다. 중합체는 분쇄(mastication), 압출, 산화, 열분해(degradation) 등에 의해 분자량을 낮출 수 있으며 산소를 함유할 수 있다.Polymers of isobutylene or copolymers of butene and isobutylene are preferred, and polymers of isobutylene are particularly preferred. Other polymers that can be used include homopolymers and copolymers of C 6 and higher alpha olefins; Attacker polypropylene; Hydrogenated polymers, copolymers and terpolymers (for example with isoprene and / or butadiene and hydrogenated derivatives thereof). The polymer may lower the molecular weight by oxygenation, extrusion, oxidation, degradation, and the like and may contain oxygen.
적절한 VI개선제로는 또한 폴리에스테르 V.I.개선제(이는 일반적으로 메타크릴 산, 아크릴 산, 말레산, 말레산 부수물, 푸마르 산 등과 같은 에틸렌형 불포화 C3내지 C8모노-및 디카복실산의 에스테르의 중합체 이다)가 있다. 사용될 수 있는 불포화 에스테르의 실예로는 데실 아크릴레이트, 라우릴 아크릴레이트, 스테아릴 아크릴레이트, 데실 메타크릴레이트, 디아밀 푸마레이트, 세틸 메타크릴레이트 등 및 이의 혼합물과 같은 적어도 1개의 탄소원자 및 바람직하게는 12 내지 20개의 탄소원자를 갖는 지방족 포화 모노 알콜의 에스테르가 있다. 다른 에스테르로는 비닐 아세테이트, 비닐 라우레이트, 비닐 스테아레이트 등 및 이의 혼합물과 같은 C2내지 C22지방 산 또는 모노카복실 산의 비닐 알콜 에스테르가 있다. C2내지 C22지방 산 또는 모노카복실 산은 포화된 것이 바람직하다. 비닐 아세테이트와 디알킬 푸마레이트의 공중합체와 같은 비닐 알콜 에스테르와 불포화 산 에스테르의 공중합체 또한 사용될 수 있다.Suitable VI improvers also include polyester VI improvers (which are generally polymers of esters of ethylenically unsaturated C 3 to C 8 mono- and dicarboxylic acids such as methacrylic acid, acrylic acid, maleic acid, maleic acid accompany, fumaric acid, etc.). Is). Examples of unsaturated esters that can be used include at least one carbon atom and preferred, such as decyl acrylate, lauryl acrylate, stearyl acrylate, decyl methacrylate, diamyl fumarate, cetyl methacrylate and the like and mixtures thereof. Preferably there are esters of aliphatic saturated mono alcohols having 12 to 20 carbon atoms. Other esters include vinyl alcohol esters of C 2 to C 22 fatty acids or monocarboxylic acids such as vinyl acetate, vinyl laurate, vinyl stearate and the like and mixtures thereof. The C 2 to C 22 fatty acid or monocarboxylic acid is preferably saturated. Copolymers of vinyl alcohol esters with unsaturated acid esters, such as copolymers of vinyl acetate and dialkyl fumarate, may also be used.
윤활 조성물은 또한 비닐 아세테이트, 알킬 아크릴 레이트 또는 알킬 메타크릴레이트의 군으로 부터 선택된 적어도 하나의 화합물과 에틸렌의 공중합체를 함유한다. 비닐 아세테이트가 바람직한 에틸렌 공중합체이다. 상기 공중합체는 적어도 약 40g/10분의 용융지수를 가져야 하고 약 10 내지 40 중량%, 바람직하게는 약 10 내지 약 30 중량%의 공중합체 함량을 가져야 한다. 상기 용융지수가 바람직하게는 약 40 내지 약 10,000, 더욱 바람직하게는, 약 40 내지 약 5000, 및 가장 바람직하게는 약 40 내지 약 2,500g/10분의 범위이어야 한다. 첨가되는 공중합체의 양은 조성물의 총중량을 기준으로 약 1 내지 약 20 중량%(바람직하게는 약 1 내지 약 10 중량%) 범위이어야 한다.The lubricating composition also contains a copolymer of ethylene with at least one compound selected from the group of vinyl acetate, alkyl acrylates or alkyl methacrylates. Vinyl acetate is the preferred ethylene copolymer. The copolymer should have a melt index of at least about 40 g / 10 minutes and have a copolymer content of about 10 to 40 weight percent, preferably about 10 to about 30 weight percent. The melt index should preferably range from about 40 to about 10,000, more preferably from about 40 to about 5000, and most preferably from about 40 to about 2,500 g / 10 minutes. The amount of copolymer added should range from about 1 to about 20 weight percent (preferably from about 1 to about 10 weight percent) based on the total weight of the composition.
사용된 특정 VI개선제 및 중합체는 시중에서 다양한 화학약품 공급처로 부터 쉽게 구입할 수 있다. 따라서 이들의 제조방법은 본 분야의 숙련된자에게는 잘 알려져 있다.The specific VI improvers and polymers used are readily available from various chemical suppliers on the market. Therefore, their production methods are well known to those skilled in the art.
윤활 조성물은 또한 소량의 보조 첨가제들(특수 목적을 위해 혼입되는 부식 방지제, 극한 압력 내마모제, 유동점 강하제, 점조제(tackiness agent), 산화 방지제, 염료 등을 포함하나, 이들로 제한되는 것은 아님)을 함유할 수 있다. 상기 첨가제들의 총량은 전형적으로 윤활 조성물의 총량을 기준으로 약 2 내지 약 5 중량% 범위이다. 또한, 이황화 몰리브덴 및 흑연과 같은 고체 윤활제가 상기 조성물내에 존재할 수 있으며 전형적으로 이황화 몰리브덴의 경우 약 1 내지 약 5중량%(바람직하게는 약 1.5 내지 약 3 중량%)이고, 흑연 경우 약 3 내지 약 15 중량%(바람직하게는 약 6 내지 약 12 중량%)이다.The lubricating composition also contains small amounts of auxiliary additives (including, but not limited to, corrosion inhibitors, extreme pressure wear agents, pour point depressants, tackiness agents, antioxidants, dyes, etc., incorporated for special purposes). can do. The total amount of the additives typically ranges from about 2 to about 5 weight percent based on the total amount of the lubricating composition. In addition, solid lubricants such as molybdenum disulfide and graphite may be present in the composition and are typically from about 1 to about 5 weight percent (preferably from about 1.5 to about 3 weight percent) for molybdenum disulfide and from about 3 to about 15 weight percent (preferably about 6 to about 12 weight percent).
하나 또는 그 이상의 용매(전형적으로 약 10 내지 약 40 중량%)가 윤활 조성물의 분배특성을 개선하기 위해 윤활 조성물에 희석제로서 첨가될 수 있다. 적절한 용매로는 순수 탄화수소 용매, 혼합된 탄화수소 용매, 염화 탄화수소 용매 또는 이들의 혼합물(이들은 전형적으로 약 30℃ 내지 약 300℃의 대기압 비점을 갖는다)이 있다.One or more solvents (typically about 10 to about 40 weight percent) may be added as a diluent to the lubricating composition to improve the dispensing properties of the lubricating composition. Suitable solvents include pure hydrocarbon solvents, mixed hydrocarbon solvents, chlorinated hydrocarbon solvents or mixtures thereof, which typically have an atmospheric boiling point of about 30 ° C to about 300 ° C.
적절한 순수 탄화수소 용매로는 톨루엔, 오르토크실렌, 메타-크실렌, 메시틸렌, 에틸벤젠, 부틸벤젠, 헥산, 헵탄, 옥탄, 이소옥탄 등 또는 이들의 혼합물이 있다. 전형적으로 이들 용매는 약 -25℃ 이하(바람직하게는 -40℃ 이하)의 고형화 점(또는 융점)을 갖는다.Suitable pure hydrocarbon solvents include toluene, orthoxylene, meta-xylene, mesitylene, ethylbenzene, butylbenzene, hexane, heptane, octane, isooctane and the like or mixtures thereof. Typically these solvents have a solidification point (or melting point) of about −25 ° C. or less (preferably −40 ° C. or less).
적절한 혼합된 탄화수소 용매로는 등유, 바솔(Varsol), 나프타 등 또는 이의 혼합물이 있다. 전형적으로 이들 용매는 약 -25℃이하, 바람직하게는 약 -40℃ 이하의유동점을 갖는다.Suitable mixed hydrocarbon solvents include kerosene, Varsol, naphtha and the like or mixtures thereof. Typically these solvents have a flow point of about −25 ° C. or less, preferably about −40 ° C. or less.
적절한 염화탄화수소 용매로는 n-프로필클로라이드, 이소프로필 클로라이드, n-부틸클로라이드, 이소-부틸클로라이드, 2급-부틸클로라이드, 펜틸클로라이드, 헥실클로라이드, 디클로로메탄, 트리클로로메탄, 1,1-디클로로에탄, 1,2-디클로로에탄, 트리클로로에틸렌, 클로로벤젠 등 및 이의 혼합물이 있으며, 1,1,1-트리클로로에탄이 특히 바람직하다.Suitable hydrocarbon chloride solvents include n-propylchloride, isopropyl chloride, n-butylchloride, iso-butylchloride, secondary-butylchloride, pentyl chloride, hexyl chloride, dichloromethane, trichloromethane, 1,1-dichloroethane , 1,2-dichloroethane, trichloroethylene, chlorobenzene and the like and mixtures thereof, with 1,1,1-trichloroethane being particularly preferred.
본 발명의 윤활 조성물은 보통 먼저 윤활유 중에 농후제를 약 1 내지 약 8시간 또는 그이상(바람직하게는 약 1 내지 약 4시간)동안 분산 또는 혼합시키고 이어서 승온(예, 사용된 특정 농후제에 따라 약 60℃ 내지 약 260℃)에서 상기 혼합물이 농후화 될때까지 가열하여 제조한다. 다음에 상기 혼합물을 주위온도(전형적으로 약 25℃)로 냉각시키면서 VI개선제, 에틸렌 공중합체 및 다른 첨가제를 첨가한다. VI개선제 및 에틸렌 공중합체를 함께 또는 어떤 순서로든 개별적으로 첨가할 수 있지만, 목적하는 저온 및 고온 특성을 갖는 윤활 조성물을 얻기 위해서 하기한 바와 같이 첨가하는 것이 바람직하다.The lubricating compositions of the present invention usually first disperse or mix the thickener in the lubricant for about 1 to about 8 hours or more (preferably about 1 to about 4 hours) and then at elevated temperatures (e.g., depending on the specific thickener used). From about 60 ° C. to about 260 ° C. until the mixture is enriched. The VI improver, ethylene copolymer and other additives are then added while cooling the mixture to ambient temperature (typically about 25 ° C.). Although the VI improver and the ethylene copolymer can be added together or separately in any order, it is preferred to add as described below to obtain a lubricating composition having the desired low temperature and high temperature properties.
상기 혼합물이 냉각됨에 따라, 약 120℃ 내지 약 180℃ 온도에서 에틸렌 공중합체(예, EVA)를 첨가하는 것이 바람직하다. 에틸렌 공중합체를 상기 범위밖의 온도에서 첨가할 수 있지만, 상기 공중합체는 보다 저온에서는 합착하는 경향이 있어 혼합물중에 적절히 분산되지 않는다. 보다 고온에서는 상기 공중합체는 열적으로 불안정하다. VI개선제를 약 80℃내지 약 190℃ 온도에서 첨가하는 것이 바람직하다. 또한 목적하는 그리이스 점조도 및 오일 점도 특성을 얻기 위해서 상기 후자의 온도 범위내에서 추가의 윤활유를 첨가할 수 있다. 다른 첨가제들(상기 언급한 보조 첨가제 및 고체 윤활제)은 보통 약 50℃ 내지 약 100℃ 온도에서 첨가한다. 마지막으로, 요구되는 분배능력을 제공하기 위해 주위온도 내지 약 50℃(바람직하게는 약 25℃ 내지 약 40℃)에서 상기 혼합물에 용매를 첨가한다. 용매 첨가 경우 과잉 증발을 피하기 위해 저온이 바람직하다. 보통, 상기 성분들을 첨가하는 도중에 조성물을 블렌딩하거나 혼합한다.As the mixture cools, it is preferred to add ethylene copolymers (eg EVA) at temperatures of about 120 ° C to about 180 ° C. The ethylene copolymer can be added at a temperature outside the above range, but the copolymer tends to coalesce at lower temperatures and does not disperse properly in the mixture. At higher temperatures the copolymer is thermally unstable. Preferably, the VI improver is added at a temperature of about 80 ° C to about 190 ° C. It is also possible to add additional lubricants within the latter temperature range in order to obtain the desired grease consistency and oil viscosity properties. Other additives (above mentioned additives and solid lubricants) are usually added at a temperature of about 50 ° C to about 100 ° C. Finally, solvent is added to the mixture at ambient temperature to about 50 ° C. (preferably between about 25 ° C. and about 40 ° C.) to provide the required dispensing capacity. Low temperature is preferred in case of solvent addition to avoid excessive evaporation. Usually, the composition is blended or mixed during the addition of the components.
윤활 조성물의 성분들은 본 분야의 숙련된자에 의해 쉽게 선택될 수 있는 다수의 방법으로 혼합하거나, 블렌딩하거나, 또는 분쇄할 수 있다. 적절한 수단으로는 외부 혼합기, 롤 밀, 내부 혼합기, 벤버리 혼합기, 스크류-압출기, 아거(auger), 콜로이드 밀, 균질화기 등이 있다.The components of the lubricating composition can be mixed, blended or ground in a number of ways that can be readily selected by those skilled in the art. Suitable means include external mixers, roll mills, internal mixers, Benbury mixers, screw-extruders, augers, colloid mills, homogenizers and the like.
본 발명의 윤활 조성물은 고온 및 저온 모두에서 양호한 윤활 작용을 요구하는 본질적으로 어떠한 용도에서도 적절히 사용될 수 있다. 상기 용도의 실례로는 개방기어, 롤러, 베아링, 와이어 로프, 케이블 등이 있다. 그러나 상기 조성물은 특히 개방 기어 윤활제로서의 용도로 아주 적합하다.The lubricating composition of the present invention can be suitably used in essentially any application that requires good lubrication at both high and low temperatures. Examples of such applications include open gears, rollers, bearings, wire ropes, cables and the like. However, the composition is particularly well suited for use as an open gear lubricant.
또다른 태양에서, 본 발명은 윤활 조성물의 약 -20℃ 이하의 온도에서의 슬럼프성 및 약 20℃ 이상의 온도에서의 접착성을 증가시키는 방법에 관한 것이며, 여기에서, 상기 조성물은 (a) 윤활유, (b) 농후제, 및 (c) VI개선제를 함유하고 상기 방법은 비닐 아세테이트, 알킬 아크릴레이트 또는 알킬 메타크릴레이트의 군으로부터 선택된 적어도 하나의 화합물과 에틸렌의 공중합체(이는 적어도 약 40g/10분(바람직하게는 약 40 내지 약 10,000, 더욱 바람직하게는 약 40 내지 약 5,000, 및 가장 바람직하게는 약 40 내지 2,500g/10분)의 용융지수를 갖고 상기 조성물에 대한 비닐 아세테이트, 알킬 아크릴레이트 또는 알킬 메타크릴레이트 함량 약 10 내지 약 40 중량%, 바람직하게는 약 10 내지 약 30 중량%를 갖는다)를 첨가하는 것을 포함한다.In another aspect, the present invention relates to a method of increasing slumpability at a temperature of about −20 ° C. or lower and adhesion at a temperature of about 20 ° C. or higher of the lubricating composition, wherein the composition comprises (a) a lubricant (b) a thickener, and (c) a VI enhancer, the process comprising copolymers of ethylene with at least one compound selected from the group of vinyl acetate, alkyl acrylates or alkyl methacrylates, which is at least about 40 g / 10 Vinyl acetate, alkyl acrylates for the composition with a melt index of minutes (preferably about 40 to about 10,000, more preferably about 40 to about 5,000, and most preferably about 40 to 2,500 g / 10 minutes) Or about 10 to about 40 weight percent, preferably about 10 to about 30 weight percent, alkyl methacrylate content).
본 발명은 본 명세서에 첨부된 특허 청구 범위의 범주를 제안하고자 하지 않는 하기의 실시예들을 참고로 하여 보다 잘 이해될 것이다.The invention will be better understood by reference to the following examples which are not intended to suggest the scope of the claims appended hereto.
실시예 1-기제 그리이스 조성물의 제조Example 1-Preparation of Base Grease Composition
기제 그리이스 조성물은 호바트 혼합(Hobart mixing) 장치중에서 제조한다. 개방 혼합 용기는 열복사 및 단열 장치가 갖추어져 있다. 용기에 12-하이드록시 스테아르산 300g 및 100SUS(@100℉) 수소 처리된 나프텐 증류물(엑손 오일 1502로 시판되고 있음) 915g을 첨가하고 이 혼합물을 일정하게 교반하면서 70℃로 가열하였다. 상기 혼합물을, 70℃에서 1시간에 걸쳐 물 150g 중의 LiOH·H0O 45g을 서서히 첨가하여 중화시키며, 이때 온도는 70°내지 110℃로 유지시킨다. 알칼리 첨가가 완결된후, 온도를 150℃로 상승시키고, 탈수가 완결될때까지 이 온도를 유지시킨다. 알칼리 함량은 산 적정에 의해 0.2질량%(NaOH당량으로 표현됨)로 측정되었으며, 이는 중화가 완결되었음을 나타낸다. 이어서 혼합물의 온도를 190℃ 내지 200℃로 상승시키고 이 범위의 온도로 약 30분간 유지시킨다. 이 "굽기(cook-out)"에 이어 상기 혼합물을 펜실바니아 수지(Pennsylvania Resin, 2600 SUS @210℉) 500g 및 폴리부텐(100℃에서 800cSt)500g을 서서히 첨가하여 약 120℃로 냉각시키고 이어서 펜 수지(Penn Resin) 345g 및 폴리부텐 86g을 첨가하여 목적하는 오일 점도(40℃에서 약 1000 cSt)를 얻는다. 다음에 광물성 오일대 VI개선제의 목적하는 비를 유지시키면서 좀더 부드러운 그리이스 점조도를 얻기 위해 추가의 오일(3000g)을 6개의 500g분취량(각 분취량은 1502 오일 195g, 펜 수지 180g 및 폴리부텐 125g을 함유함)으로 첨가한다. 상기 오일 첨가는 분리된 오일 상의 형성을 피하기 위해 서서히 실시한다. 이어서 상기 조성물을 사르롯떼(charlotte) 콜로이드 밀을 1회 통과시킨다. 분쇄 생성물은 ASTM D217로 측정한 결과 298 밀리미터/10 원추제 침투도를 갖는다.The base grease composition is prepared in a Hobart mixing apparatus. Open mixing vessels are equipped with thermal radiation and thermal insulation. 300 g of 12-hydroxy stearic acid and 915 g of 100SUS (@ 100 ° F.) hydrogenated naphthenic distillate (commercially available as Exxon Oil 1502) were added and the mixture was heated to 70 ° C. with constant stirring. The mixture is neutralized by slowly adding 45 g of LiOH.H 0 O in 150 g of water at 70 ° C. over 1 hour at which time the temperature is maintained between 70 ° and 110 ° C. After the alkali addition is complete, the temperature is raised to 150 ° C. and maintained at this temperature until dehydration is complete. Alkali content was determined by acid titration to 0.2% by mass (expressed as NaOH equivalent), indicating that neutralization was complete. The temperature of the mixture is then raised to 190 ° C. to 200 ° C. and held at this temperature for about 30 minutes. Following this “cook-out” the mixture was cooled to about 120 ° C. by slowly adding 500 g of Pennsylvania Resin (2600 SUS @ 210 ° F.) and 500 g of polybutene (800 cSt at 100 ° C.), followed by pen resin. 345 g (Penn Resin) and 86 g polybutene are added to obtain the desired oil viscosity (about 1000 cSt at 40 ° C.). Next, to obtain a smoother grease consistency while maintaining the desired ratio of mineral oil to VI improver, add 500 additional 500 g aliquots (195 g of 1502 oil, 180 g of pen resin and 125 g of polybutene). Containing). The oil addition is carried out slowly to avoid the formation of a separate oil phase. The composition is then passed through a charlotte colloid mill once. The milled product has a 298 millimeter / 10 cone cone penetration as measured by ASTM D217.
298밀리미터/10 침투도를 갖는 생성물의 3000g 분취량을 혼합용기에 되돌려 보내고 상기 1502/펜 수지/폴리부텐블렌드의 6개의 추가의 500g 분취량을 첨가한다. 상기 혼합 용기가 너무 작아 적절한 점조도를 갖는 기제 그리이스를 얻기가 어려우므로 생성물 약 1000g을 혼합용기로 부터 제거하고 남아 있는 생성물에 또다른 블렌드 500g 분취량을 첨가한다. 생성된 최종 기제 그리이스는 ASTM D217로 측정한 결과 367 밀리미터/10의 점조도를 갖고 하기의 조성을 갖는다.A 3000 g aliquot of the product having a 298 millimeter / 10 permeability is returned to the mixing vessel and six additional 500 g aliquots of the 1502 / pen resin / polybutene blend are added. Since the mixing vessel is so small that it is difficult to obtain a base grease with an appropriate consistency, about 1000 g of product is removed from the mixing vessel and another 500 g aliquot of blend is added to the remaining product. The resulting base grease has a consistency of 367 millimeters / 10 as measured by ASTM D217 and has the following composition.
수산화 리튬·H2O0.25중량%Lithium hydroxide · H 2 O0.25% by weight
12-하이드록시 스테아르 산1.69중량%12-hydroxystearic acid1.69 wt%
100SUS@100℉ 수소 처리된 나프텐 증류물38.22중량%100SUS @ 100 ℉ Hydrotreated Naphthenic Distillate38.22% by weight
펜실바니아 수지(2600 SUS @210℉)35.31중량%PA resin (2600 SUS @ 210 ℉) 35.31 wt%
폴리부텐(800 cSt @100℃)24.53중량%Polybutene (800 cSt @ 100 ° C) 24.53 wt%
실시예 2 및 3(하기)에서 이용된 윤활 조성물은 다음과 같이 상기 기제 그리이스로 부터 제조한다. 기제 그리이스 약 400g을 125℃에서 필요량의 하기 시판 중합체의 각각과 혼합된다. 이어서 ASTM D217에 의해 상기 각 혼합물의 60 스트로크 작업 침투도를 측정했다.The lubricating composition used in Examples 2 and 3 (below) is prepared from the base grease as follows. About 400 g of base grease is mixed at 125 ° C. with each of the requisite amounts of the following commercially available polymers. The 60 stroke working penetration of each of these mixtures was then measured by ASTM D217.
[표 1]TABLE 1
이어서 상기 혼합물을 냉각시키고 트리클로로에탄과 혼합하여 시험 조성물의 25 중량%의 최종 용매 농도를 얻는다.The mixture is then cooled and mixed with trichloroethane to give a final solvent concentration of 25% by weight of the test composition.
실시예 2-저온 슬럼프성에 대한 다양한 중합체의 영향Example 2 Influence of Various Polymers on Low Temperature Slump Properties
실시예 1에서 제조된 각 중합체 개질된 조성물의 슬럼프(즉, 유동)경향은 원추체 항복치(Cone Yield Value)로 부터 측정한다. 원추체 항복을 측정하기 위해서 직경 90밀리미터, 깊이 60 밀리미터의 둥근 용기를 상기 각 조성물의 샘플로 채우고 필요하다면 표면을 스팩튤러로 매끈하게 한다. 각 샘플을 -40℃에서 4시간 동안 냉각 침지시키고 있어서 표준 그리이스 침입도계로 침투로를 측정하였으며, 그 설명을 ASTM D217에 제공되어 있다. 상기 측정을 위해 기부가 62 밀리미터인 특수 우향-각 원추체를 사용하였다. 상기 원추체 및 손잡이의 총무게는 66.7g이었다. 표준 원추체를 사용하는 보통 시험에서 이용되는 5초후 대신에 10초후에 -40℃에서 침투도 측정을 실시하였다. 상기 측정은 샘플의 과도한 가온을 피가기 위해서 냉각 상자로 부터 샘플을 제거한 후 1분안에 이루어진다. 원추체 항복은 하기의 계산식을 사용하여 -40℃에서의 침투도를 계산한다.The slump (ie flow) tendency of each polymer modified composition prepared in Example 1 is determined from the cone yield value. To measure cone yield, a round container of 90 mm in diameter and 60 mm in depth is filled with a sample of each of the above compositions and the surface is smoothed with a spatula if necessary. Each sample was chilled for 4 hours at −40 ° C. so that the penetration furnace was measured with a standard grease penetrometer and a description is provided in ASTM D217. For this measurement a special right-angle cone with a base of 62 millimeters was used. The total weight of the cone and handle was 66.7 g. Permeability measurements were made at −40 ° C. after 10 seconds instead of 5 seconds used in the normal test using standard cones. The measurement is made within 1 minute of removing the sample from the cooling box to avoid excessive warming of the sample. Conical yield yields the penetration at −40 ° C. using the following formula.
과거 경험상 약 80미만의 원추체 항복치가 양호한 슬럼프성을 갖는 윤활제의 특징임을 나타낸다.Past experience indicates that less than about 80 cone yield values are characteristic of lubricants with good slumpability.
각 샘플의 원추체 항복치를 측정하여 그 결과를 표2에 요약하였다.The cone yield of each sample was measured and the results are summarized in Table 2.
[표 2]TABLE 2
(1) 용매 첨가전의 60 스트로크 작업 침투도.(1) 60 stroke working penetration before adding solvent.
(2) 최종 생성물에 대한 -40℃에서의 침투도.(2) Penetration degree at -40 ° C for the final product.
(3) 34 및 43의 항복치를 제공하는 두개의 샘플의 평균.(3) Average of two samples giving yields of 34 and 43.
(4) 중합체가 기제 그리이스 중에 분산될 수 없기 때문에 샘플을 제조하지 못함.(4) Samples could not be prepared because the polymer could not be dispersed in the base grease.
표2의 자료는 중합체 A-F를 함유하는 샘플들이 -40℃ 및 2 중량% 농도에서 양호한 슬럼프성을 가짐을 보여준다. 그러나, 6 중량%의 농도에서 중합체 E를 함유하는 샘플은 불량한 슬럼프성을 갖고 중합체 F를 함유하는 샘플은 제조할 수 없었다.The data in Table 2 shows that samples containing polymer A-F have good slumpability at -40 ° C and 2% by weight concentration. However, samples containing polymer E at a concentration of 6% by weight had poor slumpability and samples containing polymer F could not be prepared.
실시예 3-고온 접착성에 대한 다양한 중합체의 영향Example 3 Influence of Various Polymers on High Temperature Adhesion
별개의 알루미늄 판들에 각 샘플 10g을 펴서 실시예 1에서 제조한 샘플들의 접착성을 측정하였다. 이어서 판들을 순환 오븐안에 65℃에서 24시간 동안 수직으로 매달았다. 이어서 각 판의 무게 변화를 용매를 제외한 기준으로 계산하고 표면 덮음 정도를 육안으로 측정하였다. 이 시험의 결과는 표 3에 나타나 있다.The adhesiveness of the samples prepared in Example 1 was measured by spreading 10 g of each sample on separate aluminum plates. The plates were then suspended vertically at 65 ° C. for 24 hours in a circulation oven. Subsequently, the weight change of each plate was calculated on the basis of excluding the solvent, and the degree of surface covering was visually measured. The results of this test are shown in Table 3.
[표 3]TABLE 3
(1) 표 2로 부터의 값.(1) Values from Table 2.
(2) 중량 손실은 트리클로로에탄이 없는 생성물을 기준으로 한다.(2) Weight loss is based on products without trichloroethane.
표 3의 자료는 2500 MI EVA(중합체 A 및 B)를 함유하는 샘플들이 48 내지 69% 범위의 중량 손실을 나타내면서 2 및 6 중량%의 농도에서 기능을 잘 수행함을 나타낸다. 그러나 가장 중요한 것은 시험의 끝부분에서 남아 있는 조성물이 뚜렷이 표면을 드러냄이 없이 판상에 고르게 분포된 접착성 코팅물을 형성했다는 것이다. 중합체 D(39 MI EVA)를 함유하는 샘플 또한 2 중량%의 농도에서 역시 기능을 잘 수행하였다. SBS 416(중합체 E) 및 LLDPE(중합체 F)를 함유하는 샘플은 모두 시험 종결시에 육안으로 볼수 있는 어떤 큰 드러난 지역을 보이면서 기능은 불량하게 수행되었다. 따라서, 중합체 A, B 및 D를 함유하는 윤활 조성물만이 65℃에서 양호한 접착성을 제공하였다.The data in Table 3 show that samples containing 2500 MI EVA (polymers A and B) perform well at concentrations of 2 and 6 wt% with weight loss ranging from 48 to 69%. But most importantly, the remaining composition at the end of the test formed an evenly distributed adhesive coating on the plate without revealing a surface. Samples containing Polymer D (39 MI EVA) also performed well at concentrations of 2% by weight. The samples containing SBS 416 (Polymer E) and LLDPE (Polymer F) both performed poorly, showing some large exposed areas visible to the naked eye at the end of the test. Thus, only lubricating compositions containing polymers A, B and D provided good adhesion at 65 ° C.
표 2 및 3의 자료는 고온에서의 양호한 접착성 및 저온에서의 양호한 슬럼프성이 중합체 A, B 및 D를 함유하는 샘플들 즉, 적어도 약 40g/분(가장 바람직하게는 약 40 내지 약 2500g/10분)의 용융지수를 가지며 비닐아세테이트 약 10 내지 40 중량%(바람직하게는 약 10 약 30 중량%)를 함유하는 에틸렌-비닐 아세테이트 공중합체 경우에 얻어진다는 것을 보여준다.The data in Tables 2 and 3 show that samples with good adhesion at high temperatures and good slump at low temperatures contain polymers A, B and D, ie at least about 40 g / min (most preferably about 40 to about 2500 g / 10 minutes) and a ethylene-vinyl acetate copolymer containing about 10 to 40% by weight of vinyl acetate (preferably about 10 to about 30% by weight).
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GB9420312D0 (en) * | 1994-10-08 | 1994-11-23 | Exxon Research Engineering Co | Lubricating grease for open gears, cables, etc |
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US8318993B2 (en) | 2002-03-05 | 2012-11-27 | Exxonmobil Research And Engineering Company | Lubricant blend composition |
JP4202051B2 (en) * | 2002-05-31 | 2008-12-24 | Thk株式会社 | Lubricant supply device, guide device equipped with the same, and lubricating grease used therefor |
FI125285B (en) | 2009-05-20 | 2015-08-14 | Kone Corp | Method and apparatus for lubrication of strands from yarns |
FI125317B (en) * | 2010-05-20 | 2015-08-31 | Kone Corp | Metal rope, lift provided with a metal rope and use of a lubricant for lubricating a metal rope |
US20120004153A1 (en) * | 2010-06-30 | 2012-01-05 | Chevron U.S.A. Inc. | Lithium Complex Grease with Improved Thickener Yield |
US8796189B2 (en) | 2011-10-14 | 2014-08-05 | Chevron U.S.A. Inc. | Gear lubricant |
JP6624681B2 (en) * | 2016-05-25 | 2019-12-25 | コスモ石油ルブリカンツ株式会社 | Grease composition |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3705853A (en) * | 1970-09-23 | 1972-12-12 | Mobil Oil Corp | Grease compositions |
AU457980B2 (en) * | 1970-11-18 | 1975-02-13 | Esso Research And Engineering Company | Lithium soap grease |
FR2313440A1 (en) * | 1975-06-06 | 1976-12-31 | Rhone Poulenc Ind | HOMOGENOUS DISPERSIONS OF DIORGANOPOLYSILOXANIC COMPOSITIONS IN MINERAL OILS |
DE3033107A1 (en) * | 1980-09-03 | 1982-04-08 | The British Petroleum Co., Ltd., London | Light-coloured open gear lubricating grease - contg. clay thickener, polymer, particulate mineral and extreme pressure additives |
-
1989
- 1989-08-31 CA CA000610023A patent/CA1334965C/en not_active Expired - Lifetime
- 1989-09-05 NO NO893563A patent/NO174348C/en unknown
- 1989-09-06 DE DE8989309012T patent/DE68902115T2/en not_active Expired - Lifetime
- 1989-09-06 ES ES89309012T patent/ES2043028T3/en not_active Expired - Lifetime
- 1989-09-06 AT AT89309012T patent/ATE78289T1/en active
- 1989-09-06 EP EP89309012A patent/EP0359466B1/en not_active Expired - Lifetime
- 1989-09-07 AU AU41161/89A patent/AU4116189A/en not_active Abandoned
- 1989-09-07 FI FI894232A patent/FI894232A/en not_active Application Discontinuation
- 1989-09-07 KR KR1019890012929A patent/KR970011370B1/en active IP Right Grant
- 1989-09-07 MY MYPI89001218A patent/MY105037A/en unknown
- 1989-09-08 JP JP1231795A patent/JPH02175796A/en active Pending
- 1989-09-08 AR AR89314886A patent/AR244320A1/en active
Also Published As
Publication number | Publication date |
---|---|
EP0359466B1 (en) | 1992-07-15 |
AU4116189A (en) | 1990-03-15 |
MY105037A (en) | 1994-07-30 |
NO893563D0 (en) | 1989-09-05 |
NO174348C (en) | 1994-04-20 |
FI894232A (en) | 1990-03-09 |
JPH02175796A (en) | 1990-07-09 |
KR900004920A (en) | 1990-04-13 |
AR244320A1 (en) | 1993-10-29 |
CA1334965C (en) | 1995-03-28 |
DE68902115D1 (en) | 1992-08-20 |
FI894232A0 (en) | 1989-09-07 |
EP0359466A1 (en) | 1990-03-21 |
NO893563L (en) | 1990-03-09 |
NO174348B (en) | 1994-01-10 |
ES2043028T3 (en) | 1993-12-16 |
DE68902115T2 (en) | 1992-12-03 |
ATE78289T1 (en) | 1992-08-15 |
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