KR100250822B1 - Grease composition for rubber deterioration prevention - Google Patents
Grease composition for rubber deterioration prevention Download PDFInfo
- Publication number
- KR100250822B1 KR100250822B1 KR1019970068272A KR19970068272A KR100250822B1 KR 100250822 B1 KR100250822 B1 KR 100250822B1 KR 1019970068272 A KR1019970068272 A KR 1019970068272A KR 19970068272 A KR19970068272 A KR 19970068272A KR 100250822 B1 KR100250822 B1 KR 100250822B1
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- KR
- South Korea
- Prior art keywords
- grease
- sulfur
- extreme pressure
- grease composition
- diborate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000004519 grease Substances 0.000 title claims abstract description 67
- 239000000203 mixture Substances 0.000 title claims abstract description 38
- 230000006866 deterioration Effects 0.000 title abstract description 14
- 230000002265 prevention Effects 0.000 title description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011593 sulfur Substances 0.000 claims abstract description 18
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 18
- -1 borate compound Chemical class 0.000 claims abstract description 15
- 239000005069 Extreme pressure additive Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 239000005078 molybdenum compound Substances 0.000 claims abstract description 3
- 150000002752 molybdenum compounds Chemical class 0.000 claims abstract description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 12
- 239000011574 phosphorus Substances 0.000 claims description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims description 12
- 150000001340 alkali metals Chemical class 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 9
- QCJQWJKKTGJDCM-UHFFFAOYSA-N [P].[S] Chemical compound [P].[S] QCJQWJKKTGJDCM-UHFFFAOYSA-N 0.000 claims description 5
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical group [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 claims description 5
- MEKUERBZVYOCSL-UHFFFAOYSA-N dicalcium dioxidoboranyloxy(dioxido)borane Chemical group [Ca+2].[Ca+2].[O-]B([O-])OB([O-])[O-] MEKUERBZVYOCSL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000654 additive Substances 0.000 abstract description 6
- 238000005299 abrasion Methods 0.000 abstract description 4
- 230000000996 additive effect Effects 0.000 abstract description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 abstract 1
- 239000004202 carbamide Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 239000002199 base oil Substances 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- KHYKFSXXGRUKRE-UHFFFAOYSA-J molybdenum(4+) tetracarbamodithioate Chemical compound C(N)([S-])=S.[Mo+4].C(N)([S-])=S.C(N)([S-])=S.C(N)([S-])=S KHYKFSXXGRUKRE-UHFFFAOYSA-J 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 239000007866 anti-wear additive Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 3
- 229940114069 12-hydroxystearate Drugs 0.000 description 2
- 229940114072 12-hydroxystearic acid Drugs 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QVXGKJYMVLJYCL-UHFFFAOYSA-N 2,3-di(nonyl)-N-phenylaniline Chemical compound C(CCCCCCCC)C=1C(=C(C=CC1)NC1=CC=CC=C1)CCCCCCCCC QVXGKJYMVLJYCL-UHFFFAOYSA-N 0.000 description 1
- QFBYWORVYPLCIN-UHFFFAOYSA-N B([O-])([O-])OB([O-])[O-].[K+].[K+].[K+].[K+] Chemical compound B([O-])([O-])OB([O-])[O-].[K+].[K+].[K+].[K+] QFBYWORVYPLCIN-UHFFFAOYSA-N 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XYRMLECORMNZEY-UHFFFAOYSA-B [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S Chemical compound [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S XYRMLECORMNZEY-UHFFFAOYSA-B 0.000 description 1
- WJPZDRIJJYYRAH-UHFFFAOYSA-N [Zn].[Mo] Chemical class [Zn].[Mo] WJPZDRIJJYYRAH-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- XMDZAYCSAPTDNV-UHFFFAOYSA-N azane 1,2-di(nonyl)naphthalene Chemical compound N.C1=CC=CC2=C(CCCCCCCCC)C(CCCCCCCCC)=CC=C21 XMDZAYCSAPTDNV-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012990 dithiocarbamate Substances 0.000 description 1
- OYQYHJRSHHYEIG-UHFFFAOYSA-N ethyl carbamate;urea Chemical compound NC(N)=O.CCOC(N)=O OYQYHJRSHHYEIG-UHFFFAOYSA-N 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
-
- 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
- C10M137/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus
- C10M137/12—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus having a phosphorus-to-carbon bond
- C10M137/14—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus having a phosphorus-to-carbon bond containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
Description
본 발명은 고무 열화 방지용 그리이스 조성물에 관한 것으로, 보다 상세하게는 기존의 그리이스 조성물에 보레이트 (borate) 화합물을 첨가함으로써 극압성 향상을 위한 황(S)-인(P) 계 첨가제의 사용량을 대폭 줄여 고무 열화를 효과적으로 방지할 수 있는 그리이스 조성물에 관한 것이다.The present invention relates to a rubber composition for preventing rubber deterioration, and more particularly, by adding a borate compound to an existing grease composition, the amount of sulfur (S) -phosphorus (P) -based additives for improving extreme pressure is greatly reduced. A grease composition capable of effectively preventing rubber deterioration.
종래에는 극압이 걸리고 마찰계수 및 마모 계수가 낮아야 하는 등속 조인트 (C. V. Joint), 유니버설 조인트, 스프라인 샤프트, 산업용 기어 카프링 등과 같은 가혹한 조건의 윤활 개소에 황-인계 극압첨가제를 함유한 그리이스, 이유화 몰리브덴 (disulfurized molybden)을 함유한 극압 그리이스 또는 유기 몰리브덴-아연 화합물을 함유한 그리이스가 사용되고 있었다. 그러나 이러한 그리이스에는 다량의 황과 인이 함유되어 있으므로 고온에서 열화 및 분해되어 유리 황과 유리 인이 생성되고, 이들이 고무 열화에 촉진제 작용을 함으로서 고무 부스 (rubber boots)가 쉽게 팽윤 (swelling)되거나 경화되어 수명이 짧아지는 단점이 있었다.Grease containing sulfur-phosphoric extreme pressure additives in lubrication areas under severe conditions such as CV joints, universal joints, spline shafts, industrial gear couplings, etc., which require extreme pressure and low friction and wear coefficients. Extreme pressure greases containing disulfurized molybden or greases containing organic molybdenum-zinc compounds have been used. However, since these greases contain large amounts of sulfur and phosphorus, they deteriorate and decompose at high temperatures to produce free sulfur and free phosphorus, and they act as accelerators for rubber deterioration, making rubber boots easily swell or harden. There was a disadvantage that the life is shortened.
또한 그리이스에 몰리브덴 디티오카바메이트 (Mo-DTC) 와 몰리브덴 디티오포스페이트 (Mo-DTP)를 단독으로 또는 병용하여 첨가하여 사용하는 방법이 공지되어 있으나 이 또한 황 원자를 포함하고 있는 유기 몰리브덴이 분해될 때 생기는 이유화 몰리브덴으로 인한 고무의 열화가 심각한 문제로 대두되었다.Molybdenum dithiocarbamate (Mo-DTC) and molybdenum dithiophosphate (Mo-DTP) are known to be used alone or in combination with grease, but organic molybdenum containing sulfur atoms is also decomposed. The deterioration of rubber due to molybdenum wetting as a result of this problem has become a serious problem.
이에 본 발명자들은 종래의 그리이스 조성물이 다량의 황과 인을 함유함으로 인하여 야기되는 고무 물성의 열화를 방지하고자 노력하여 오던 중, 기존의 그리이스 화합물에 보레이트 화합물을 첨가하면 황-인계 극압 첨가제의 양을 대폭 줄이고도 극압성 및 마모 계수의 특성은 유지하거나 향상시키면서 고무열화를 방지할 수 있음을 알아내어 본 발명을 제조하였다.The present inventors have been trying to prevent the deterioration of the rubber properties caused by the conventional grease composition containing a large amount of sulfur and phosphorus, and when the borate compound is added to the existing grease compound, the amount of sulfur-phosphorus extreme pressure additive The present invention was made by finding that the rubber deterioration can be prevented while maintaining or improving the characteristics of the extreme pressure and the wear coefficient even with the drastic reduction.
본 발명은 황-인계 극압 첨가제의 양을 대폭 줄이고도 극압성 및 마모 계수의 특성을 유지하거나 향상시킬 수 있는 그리이스 조성물을 제공하는 것을 목적으로 한다.It is an object of the present invention to provide a grease composition which can maintain or improve the properties of extreme pressure and wear coefficient even though the amount of sulfur-based extreme pressure additive is greatly reduced.
상기 목적을 달성하기 위하여 본 발명에서는 기존의 그리이스에 보레이트 화합물을 첨가하여 전체 그리이스 조성 중의 황 및 인 성분의 함량을 대폭 줄인 그리이스 조성물을 제공한다.In order to achieve the above object, the present invention provides a grease composition in which the content of sulfur and phosphorus in the overall grease composition is greatly reduced by adding a borate compound to the existing grease.
이하 본 발명은 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명은 극압성 및 저 마찰 계수를 가져야 하는 그리이스 조성물에 있어서, 기존의 그리이스에 보레이트 화합물이 0.3∼5 중량% 로 함유되고 전체 그리이스 중에서 황 성분과 인 성분의 함량이 각각 2 중량% 를 초과하지 않는 그리이스 조성물을 제공한다.The present invention provides a grease composition that must have extreme pressure and low friction coefficient, wherein the conventional grease contains 0.3 to 5% by weight of a borate compound and the sulfur and phosphorus contents of the whole grease do not exceed 2% by weight, respectively. Does not provide a grease composition.
본 발명의 그리이스 조성물은, 기존의 그리이스에 알칼리 금속 디보레이트 (diborate), 알칼리 금속 메타보레이트 (metaborate)를 혼합하여 사용하고 종래의 황-인계 극압 첨가제 및 유기 몰리브덴 화합물을 최소한으로 줄여 사용하는데 그 특징을 두고 있는바, 본 발명에서 사용되는 알칼리 금속 디보레이트로서는 칼륨 디보레이트 (potassium diborate), 알칼리 금속 메타보레이트로는 소듐 메타보레이트 (sodium metaborate)를 사용하는 것이 바람직하다.The grease composition of the present invention is used by mixing alkali metal diborate and alkali metal metaborate to the existing grease and using a minimal amount of conventional sulfur-phosphorus extreme pressure additives and organic molybdenum compounds. As the alkali metal diborate used in the present invention, potassium diborate is preferable, and sodium metaborate is preferably used as the alkali metal metaborate.
이 때 디보레이트 화합물과 메타보레이트 화합물의 함량은 전체 그리이스의 0.3∼5 중량% 가 적당한데, 함량이 5 중량% 를 초과하면 마모 계수가 낮아지는 효과도 없고 극압성이 향상되는 효과도 없다.At this time, the content of the diborate compound and the metaborate compound is 0.3 to 5% by weight of the total grease is appropriate, but if the content exceeds 5% by weight there is no effect of lowering the coefficient of wear and improving the extreme pressure.
또한 혼합하여 사용하는 디보레이트와 메타보레이트 화합물의 비율은 2 : 1 인 경우가 가장 효과적이다.In addition, the ratio of the diborate and metaborate compound used by mixing is most effective when it is 2: 1.
본 발명의 조성물에서 그리이스로서는 기존의 그리이스가 모두 사용될 수 있는데, 예를 들어 리튬 그리이스, 칼슘 그리이스, 복합 칼슘 그리이스, 복합 리튬 그리이스, 복합 알루미늄 그리이스와 같은 비누계 그리이스; 벤토나이트 그리이스, 실리카 그리이스와 같은 무기질 그리이스; 우레아 그리이스, 우레아 우레탄 그리이스 등과 같은 합성 그리이스 등이 사용될 수 있다. 그러나 특히 내열성을 필요로 하는 등속 조인트에는 리튬 및 우레아 그리이스가 유용하다.As the grease in the composition of the present invention, all conventional greases can be used, for example, soap-based greases such as lithium grease, calcium grease, composite calcium grease, composite lithium grease, composite aluminum grease; Inorganic greases such as bentonite grease, silica grease; Synthetic greases such as urea grease, urea urethane grease and the like can be used. However, lithium and urea greases are particularly useful for constant velocity joints requiring heat resistance.
그리고 그리이스 조성물의 기유 (base oil)로서는 광유, 합성유 또는 이들의 혼합유가 모두 사용될 수 있다.And as a base oil of the grease composition, both mineral oil, synthetic oil or a mixture of these may be used.
본 발명의 그리이스는 전술한 바와 같이 종래의 황-인계 극압 첨가제를 최소로 사용하면서 디보레이트 화합물과 메타보레이트 화합물을 병용 사용함으로서, 종래 그리이스가 가지는 극압성과 마모 계수가 낮은 성질을 유지함과 동시에 고무 열화 방지에 훨씬 우수한 특성을 발현하게 된다.As described above, the grease of the present invention uses a diborate compound and a metaborate compound in combination with a minimum amount of a conventional sulfur-phosphorus extreme pressure additive, thereby maintaining rubber properties and at the same time deteriorating rubber at the same time. It exhibits even better properties for prevention.
다만 이 때 전체 그리이스 중에서 황 성분과 인 성분이 각각 2 중량% 이상 되면 고무 열화 방지에 효과가 적으므로, 이들 성분은 2 중량% 를 초과하지 않아야 한다.At this time, if the sulfur component and the phosphorus component in the total grease are each 2 wt% or more, it is less effective in preventing rubber deterioration, so these components should not exceed 2 wt%.
이와 같이 본 발명에서는 종래의 그리이스에 알칼리 금속 보레이트와 알칼리 금속 메타보레이트를 적절히 혼합 사용함으로서 후술하는 실시예 등에서 알 수 있는 바와 같이 이들 성분을 사용하지 않은 경우와 비교하여 고무 열화 방지 효과가 30∼50 % 향상된다. 이는 그리이스에 디보레이트, 메타보레이트 화합물을 첨가하여 황-인계 극압 및 마모 방지제의 양을 줄임으로써 황 또는 인 화합물이 고무 성분을 경화시키거나 팽윤시키는 것을 방지하는 것으로 생각된다.As described above, in the present invention, an alkali metal borate and an alkali metal metaborate are appropriately mixed with the conventional grease, and as shown in Examples described later, the rubber deterioration prevention effect is 30-50 compared with the case where these components are not used. % Is improved. This is believed to prevent the sulfur or phosphorus compound from curing or swelling the rubber component by adding diborate, metaborate compounds to the grease to reduce the amount of sulfur-phosphorus extreme pressure and antiwear agent.
즉, 본 발명의 그리이스 조성물에서는 극압 및 마모 방지 첨가제가 극압을 받아 높은 온도에서 분해, 유리될 때 발생하는 활성 유황이나 인이 종래 그리이스보다 훨씬 적기 때문에, 이들 극압 및 마모 방지 첨가제가 고무 성분의 가류를 촉진시키거나 열화를 촉진시키는 것을 방지하여 준다. 최소한의 황이나 인이 금속 표면에 형성되어 융착 및 마모를 방지하는데, 이 때 디보레이트 및 메타보레이트 화합물이 분해되어 금속 표면에 무기물 층을 형성하여 더욱 효과를 증진시킨다고 생각된다. 또한 알칼리의 보레이트나 알칼리 메타 보레이트는 가류 촉진 및 고무 열화를 촉진하는 활성 유황이나 디티오카바메이트가 고무에 미치는 작용을 완화시키거나 차단하는 효과를 가진다.That is, in the grease composition of the present invention, since the active sulfur or phosphorus generated when extreme pressure and antiwear additive is decomposed and released at high temperature under extreme pressure is much smaller than that of conventional grease, these extreme pressure and antiwear additives are vulcanized in rubber components. To prevent or accelerate deterioration. Minimal sulfur or phosphorus is formed on the metal surface to prevent fusion and abrasion, at which time the diborate and metaborate compounds are decomposed to form an inorganic layer on the metal surface to further enhance the effect. In addition, alkali borate and alkali metaborate have the effect of alleviating or blocking the action of activated sulfur or dithiocarbamate on rubber to promote vulcanization and rubber deterioration.
한편, 본 발명의 그리이스 조성물에는 유기 몰리브덴 그라파이트 등의 고체 윤활제; 암모늄 디노닐나프탈렌 등의 방청제; 2,6-디-t-부틸-p-크레졸, 알킬화 디페닐아민, 디노닐 디페닐아민 등의 산화 방지제를 적당량 함께 첨가할 수 있다.On the other hand, the grease composition of the present invention includes a solid lubricant such as organic molybdenum graphite; Rust inhibitors such as ammonium dinonylnaphthalene; Antioxidants, such as 2, 6- di- t- butyl- p- cresol, alkylated diphenylamine, and dinonyl diphenylamine, can be added together in an appropriate amount.
이하 실시예에 의거하여 본 발명을 더욱 상세히 설명하기로 한다. 단 하기 실시예는 본 발명을 예시하는 것일 뿐 본 발명이 실시예에 의하여 제한되는 것은 아니다.The present invention will be described in more detail based on the following examples. However, the following examples are merely to illustrate the invention and the present invention is not limited by the examples.
실시예에 앞서 하기 제조예에서는 본 발명에 사용되는 기존의 그리이스를 제조하는 방법을 나타내었다.Prior to Examples The following preparation examples show a method for producing a conventional grease used in the present invention.
제조예 1. 리튬 그리이스의 제조Preparation Example 1 Preparation of Lithium Grease
100 ℃ 에서 점도가 18 cSt 이며 점도 지수가 80 이상인 정제 광유에 12-하이드록시 스테아린산과 수산화 리튬을 가열 반응시켜 12-하이드록시 스테아레이트를 제조하고, 이 12-하이드록시 스테아레이트의 함유량이 12 중량 % 가 되도록 기유 중에 균일하게 분산시켜 리튬 그리이스를 제조하였다.12-hydroxy stearic acid and lithium hydroxide were heated and reacted with purified mineral oil having a viscosity of 18 cSt and a viscosity index of 80 or more at 100 ° C. to prepare 12-hydroxy stearate, and the content of this 12-hydroxy stearate was 12% by weight. Lithium grease was prepared by uniformly dispersing in base oil to be%.
제조예 2. 우레아 그리이스의 제조Preparation Example 2 Preparation of Urea Grease
제조예 1에서 사용한 것과 동일한 기유 중에서 톨루엔디이소시아네이트와 아닐린을 반응시켜 우레아 화합물을 제조하고, 이 우레아 화합물이 180 중량 % 가 되도록 기유 중에 균일하게 분산시켜 우레아 그리이스를 제조하였다.A urea compound was prepared by reacting toluene diisocyanate and aniline in the same base oil as used in Preparation Example 1, and uniformly dispersed in base oil such that the urea compound was 180% by weight to prepare urea grease.
＜실시예 1＞<Example 1>
용량 150 L 되는 실험용 반응기에 100 ℃ 에서 점도가 18 cSt 인 기유 89.2 kg 을 넣고 12-하이드록시 스테아린산 14.2 kg 을 넣은 후 가열하여 85∼90 ℃ 의 온도가 되도록 하여 균일하게 용해한 다음 90 ℃ 온수 10 kg 에 2.0 kg 의 리튬 하이드록사이드를 넣어 용해한 수용액을 반응기에 서서히 넣으면서 교반하였다. 계속하여 교반하면서 가열하여 130 ℃ 가 되었을 때 반응이 완결되었는지 알기 위한 중화값이 적합하면 다시 교반 하면서 200∼205 ℃ 가 될 때까지 계속 가열하였다. 이 때 반응에서 발생한 물을 증발시키고, 냉각수로 반응기를 냉각하여 130 ℃ 가 되었을 때, 그리이스에 유기 몰리브덴 화합물인 몰리반 A (Mo-DTC, 반텔 빌트사 제품) 1 kg 과 칼슘 디보레이트 2 kg, 소듐 메타보레이트1 kg 을 차례로 교반하면서 넣어 균일하게 분산시켰다. 냉각을 계속하여 온도가 80 ℃ 정도 되었을 때 극압 첨가제인 RC2515 [레인 케미 (RHEIN CHEMIE)사 제품] 5 kg 과 황-인계 마모방지제인 RC3180 [레인 케미사 제품] 1 kg 을 차례로 교반하면서 균일하게 분산시켜서 본 발명의 그리이스 조성물을 제조하였다.89.2 kg of base oil having a viscosity of 18 cSt at 100 ° C. and 14.2 kg of 12-hydroxy stearic acid were added to an experimental reactor having a capacity of 150 L, heated, brought to a temperature of 85 to 90 ° C., dissolved uniformly, and 10 kg of hot water at 90 ° C. 2.0 kg of lithium hydroxide was added to the solution, followed by stirring while slowly dissolving the aqueous solution into the reactor. When the mixture was heated with continuous stirring to reach a temperature of 130 ° C., if a neutralization value suitable for knowing whether the reaction was completed, heating was continued until the temperature reached 200 to 205 ° C. while stirring again. At this time, the water generated in the reaction was evaporated, and the reactor was cooled with cooling water to reach 130 ° C., 1 kg of molybdenum A (Mo-DTC, manufactured by Vantel-Bilt), 2 kg of calcium diborate, 1 kg of sodium metaborate was added sequentially while stirring to disperse uniformly. When cooling is continued and the temperature is about 80 ° C, uniformly dispersing 5 kg of extreme pressure additive RC2515 [from Rain Chemie] and 1 kg of sulfur-based anti-wear RC3180 [from Rain Chemie] The grease composition of the present invention was prepared.
＜실시예 2∼3＞<Examples 2-3>
각 성분의 함량을 하기 표 1 과 같이 조절한 것을 제외하고는 상기 실시예 1 과 동일한 방법으로 반응을 수행하여 본 발명의 그리이스 조성물을 제조하였다.Except that the content of each component was adjusted as shown in Table 1, the reaction was carried out in the same manner as in Example 1 to prepare a grease composition of the present invention.
＜실시예 4＞<Example 4>
용량 150 L 되는 실험용 반응기에 100 ℃ 에서 점도가 18 cSt 인 기유 73.8 kg 및 아닐린 8.1 kg 을 넣고 상온에서 약 10 분 동안 잘 교반하여 용해시켰다. 그런 다음 톨루엔디이소시아네이트 8.0 kg 을 제트 분사식으로 소량씩 넣으면서 교반하면 반응열이 발생하여 온도가 50∼60 ℃ 가 된다. 이 때 시간은 약 30∼40 분 소요되며, 톨루엔 디이소시아네이트를 넣고 난 후 약 10 분간 가열 없이 교반을 계속한 다음 160 ℃ 가 될 때까지 계속 가열하고, 30 분 동안 정치한 후 냉각하여 120 ℃ 가 되었을 때 유기몰리브덴 화합물인 몰리반 A (Mo-DTC) 1 kg, 칼슘 디보레이트 2 kg 및 소듐 메타보레이트 1 kg 을 차례로 넣어 잘 교반, 분산시켰다.Into an experimental reactor having a capacity of 150 L, 73.8 kg of base oil having a viscosity of 18 cSt and 8.1 kg of aniline were added at 100 ° C. and stirred for about 10 minutes at room temperature for dissolution. Then, stirring and stirring a small amount of toluene diisocyanate 8.0 kg by jet jet type, the reaction heat is generated, the temperature is 50 ~ 60 ℃. At this time, it takes about 30 to 40 minutes. After adding toluene diisocyanate, stirring is continued without heating for about 10 minutes, and it is continued to heat up to 160 ℃, and it is allowed to stand for 30 minutes before cooling to 120 ℃. When 1 mol of Molyban A (Mo-DTC) which is an organomolybdenum compound, 2 kg of calcium diborate, and 1 kg of sodium metaborate were added in order, the mixture was well stirred and dispersed.
이를 계속 냉각하여 80 ℃ 가 되었을 때 극압 첨가제인 RC2515 5 kg, 마모방지제인 RC3180 1 kg 을 차례로 잘 교반하면서 넣어 분산시킨 다음 3-롤 분쇄 (3-Roll Mill)하여 균질화시켜서 본 발명의 그리이스 조성물을 제조하였다.When the mixture was cooled to 80 ° C., 5 kg of the extreme pressure additive RC2515 and 1 kg of the anti-wear additive RC3180 were added and stirred in order, followed by dispersing, followed by 3-roll milling to homogenize the grease composition of the present invention. Prepared.
＜실시예 5∼6＞<Examples 5-6>
각 성분의 함량을 하기 표 1 과 같이 조절한 것을 제외하고는 상기 실시예 4와 동일한 방법으로 반응을 수행하여 본 발명의 그리이스 조성물을 제조하였다.The grease composition of the present invention was prepared by performing the reaction in the same manner as in Example 4, except that the content of each component was adjusted as in Table 1 below.
[비교예 1∼3]Comparative Examples 1-3
각 성분의 함량을 하기 표 1 과 같이 조절한 것을 제외하고는 상기 실시예 1 과 동일한 방법으로 반응을 수행하여 그리이스 조성물을 제조하였다.A grease composition was prepared by performing the reaction in the same manner as in Example 1, except that the content of each component was adjusted as in Table 1 below.
[비교예 4∼6]Comparative Examples 4 to 6
각 성분의 함량을 하기 표 1 과 같이 조절한 것을 제외하고는 상기 실시예 4와 동일한 방법으로 반응을 수행하여 그리이스 조성물을 제조하였다.A grease composition was prepared by carrying out the reaction in the same manner as in Example 4, except that the content of each component was adjusted as in Table 1 below.
＜시험예＞<Test Example>
살기 실시예 및 비교예의 그리이스 조성물을 이용하여 하기와 같은 방법으로 테스트를 수행하여 그 결과를 하기 표 2에 나타내었다.Tests were carried out in the following manner using the grease compositions of the living examples and the comparative examples, and the results are shown in Table 2 below.
1) ASTM D4289 : 고무 시편을 미리 경도, 부피, 밀도를 측정한 후 시료 그리이스에 침적하여 100 ℃ 에서, 70 시간 동안 유지한 후 경도, 부피 등을 측정하여 침적 전후의 변화를 측정하였다.1) ASTM D4289: After measuring the hardness, volume, and density of rubber specimens, the samples were immersed in sample grease and kept at 100 ° C. for 70 hours, and then measured before and after the deposition by measuring hardness, volume, and the like.
2) 쉘-4구 극압 테스트 : ASTM D2586 에 규정된 방법으로 시험기 회전 수 1760 RPM, 시료 온도 18∼35 ℃ 로 하고 10 초 간격으로 부하를 증가시키면서 융착이 일어날 때까지 시험하였다.2) Shell-four-ball extreme pressure test: The test was conducted in a manner specified in ASTM D2586 at 1760 RPM of the tester and a sample temperature of 18 to 35 DEG C, and the test was carried out while increasing the load at 10 second intervals until fusion occurred.
3) 4구 마모 테스트 (4-Ball Wear Test) : ASTM D2596 에 규정된 방법으로 하중 40 kg, 1760 RPM, 온도 90 ℃ 의 조건하에서 1 시간 동안 가동한 다음 볼 마모 지름 (Ball Wear diameter)을 측정하였다.3) 4-Ball Wear Test: The ball wear diameter is measured after operating for 1 hour under the load of 40 kg, 1760 RPM and 90 ° C by the method specified in ASTM D2596. It was.
상기 실시예의 결과 표 1 로부터 다음과 같은 사실을 알 수 있었다.As a result of the above Example, Table 1 shows the following facts.
즉, 같은 종류의 극압제를 사용하더라도 알칼리 디보레이트 및 알칼리 메타 보레이트를 병용했을 때 극압성이 20∼30 % 향상되었으며, 같은 종류의 그리이스를 사용한 경우에 종래 극압 및 내마모 방지제를 단독으로 사용했거나 본 발명의 보레이트 화합물을 병용했을 때나 마모 성질에는 큰 차이가 없으면서 본 발명의 보레이트 화합물을 병용했을 때가 고무 열화 방지성이 30∼50% 향상되었다.That is, even when the same type of extreme pressure agent is used, when the alkali diborate and alkali metaborate are used together, the extreme pressure property is improved by 20 to 30%, and when the same type of grease is used, the conventional extreme pressure and anti-wear agent is used alone or When the borate compound of the present invention was used in combination or when the borate compound of the present invention was used in combination without any significant difference in wear properties, the rubber deterioration resistance was improved by 30 to 50%.
이상에서 살펴본 바와 같이 본 발명의 그리이스 조성물은 그리이스 조성물에 보레이트 (borate) 화합물을 첨가하여 극압성 향상을 위한 황(S)-인(P)계 첨가제의 사용량을 대폭 줄임으로써 고무의 열화를 효과적으로 방지할 수 있으며, 황-인계 첨가제의 사용량이 줄었음에도 극압성 및 마모 계수의 특성은 유지되어 등속 조인트 등의 각종 윤활 개소에 유용하게 사용될 수 있는 그리이스 조성물이다.As described above, the grease composition of the present invention effectively prevents deterioration of rubber by adding a borate compound to the grease composition and drastically reducing the amount of sulfur (S) -phosphorus (P) -based additive for improving extreme pressure. Although the amount of sulfur-based additive is reduced, the characteristics of extreme pressure and abrasion coefficient are maintained, and thus the grease composition can be usefully used for various lubrication points such as constant velocity joints.
Claims (5)
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| KR1019970068272A KR100250822B1 (en) | 1997-12-12 | 1997-12-12 | Grease composition for rubber deterioration prevention |
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| KR1019970068272A KR100250822B1 (en) | 1997-12-12 | 1997-12-12 | Grease composition for rubber deterioration prevention |
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|---|---|
| KR19990049344A KR19990049344A (en) | 1999-07-05 |
| KR100250822B1 true KR100250822B1 (en) | 2000-04-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1019970068272A Expired - Fee Related KR100250822B1 (en) | 1997-12-12 | 1997-12-12 | Grease composition for rubber deterioration prevention |
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| Country | Link |
|---|---|
| KR (1) | KR100250822B1 (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR960031581A (en) * | 1995-02-18 | 1996-09-17 | 구연찬 | Grease composition with extreme pressure and low friction |
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1997
- 1997-12-12 KR KR1019970068272A patent/KR100250822B1/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR960031581A (en) * | 1995-02-18 | 1996-09-17 | 구연찬 | Grease composition with extreme pressure and low friction |
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| KR19990049344A (en) | 1999-07-05 |
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