CN100549147C - Grease composition - Google Patents

Grease composition Download PDF

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CN100549147C
CN100549147C CNB2006100890282A CN200610089028A CN100549147C CN 100549147 C CN100549147 C CN 100549147C CN B2006100890282 A CNB2006100890282 A CN B2006100890282A CN 200610089028 A CN200610089028 A CN 200610089028A CN 100549147 C CN100549147 C CN 100549147C
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calcium
acid
base oil
complex grease
described composition
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CN101117604A (en
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李茂森
刘显秋
王磊
方春梅
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

Grease composition provided by the invention is mixed by aluminum complex grease and calcium sulfonate complex grease, and part by weight is 1: 0.2~7.0.Said aluminum complex grease is made up of compound aluminium soap viscosifying agent and base oil that phenylformic acid, lipid acid and aluminum alkoxide reaction generate, and wherein compound aluminium soap viscosifying agent accounts for 3%~15% of aluminum complex grease weight, and all the other are base oil.Said calcium sulfonate complex grease is made up of base oil, non-newtonian fluid high alkalinity calcium mahogany sulfonate and compound calcium viscosifying agent.In calcium sulfonate complex grease weight is 100%, and non-newtonian fluid high alkalinity calcium mahogany sulfonate weight is 20~50%, and compound calcium viscosifying agent weight is 2~10%, and all the other are base oil.Grease composition of the present invention had both had good high and low temperature, water resisting property and pumping, had good resistance to abrasion, mechanical stability, rust-preventing characteristic and good surface appearance again, can satisfy the naval vessel lubricating requirement.

Description

Grease composition
Technical field
The present invention relates to lubricating grease.
Background technology
The lubricating grease that is used for equipments waterborne such as naval vessel, submarine requires to have good high and low temperature, water resisting property, pumping, rust-preventing characteristic, mechanical stability and resistance to abrasion, selects compound aluminium soap multiviscosisty high viscosity refined mineral oil lubricating grease to suit.Refining high viscosity mineral oil can satisfy the requirement that has between high temperature, low temperature and the friction pair of lubricating grease than heavy oil film; Compound aluminium soap can satisfy the high temperature of lubricating grease, anti-water, pumping requirement.But the resistance to abrasion of this kind lubricating grease, mechanical stability and rust-preventing characteristic are relatively poor, and outward appearance is gelatin.
Complex calcium sulfonate grease has good high-temperature, mechanical stability, extreme pressure anti-wear and rust-preventing characteristic, and shortcoming is a long storage, the grease consistency hardening.
USP 4132658 patents are by adding excessive aluminum compound, to improve oilness; By the part homogeneous, to improve the rheopexy of fat, product is sheared not softening; Kept 1 hour for 185~195 ℃ in the saponification section, to improve water resisting property; Keep for some time for 60 ℃ at cooling section, to improve the outward appearance of product.But the improvement of its outward appearance and resistance to abrasion is also not obvious.Because adopt the part homogeneous, grease consistency is softer, the first thickening phenomenon of deliquescing again can appear in the shear history, and grease thickening can make moment increase in the use, and this is disadvantageous.
Summary of the invention
The invention provides a kind of grease composition, this lubricating grease had both had good high and low temperature, water resisting property and pumping, had good resistance to abrasion, mechanical stability, rust-preventing characteristic and good surface appearance again, satisfied the naval vessel lubricating requirement.
Lubricating grease provided by the invention is mixed in proportion by aluminum complex grease and calcium sulfonate complex grease and forms, and part by weight is 1: 0.2~7.0, and preferably 1: 0.5~3.0.
Said aluminum complex grease is made up of compound aluminium soap viscosifying agent and base oil that phenylformic acid, lipid acid and aluminum alkoxide reaction generate, and wherein compound aluminium soap viscosifying agent accounts for 3%~15% of aluminum complex grease weight, and all the other are base oil.
Said base oil is 100 ℃ of viscosity 10~40mm 2The refined mineral oil of/s.
Said lipid acid is C 8~C 20Monocarboxylic acid, as ten dihydroxystearic acids or stearic acid, preferably stearic acid.The mol ratio of phenylformic acid and lipid acid is 1: 0.8~1.2.
Said aluminum alkoxide is aluminium isopropoxide or aluminium isopropoxide tripolymer.The mole number of aluminum alkoxide is phenylformic acid and lipid acid mole number sum 0.5~0.7 times.
Aluminum complex grease can prepare in accordance with the following methods: lipid acid and phenylformic acid are mixed with the part base oil and heat up, at 90~110 ℃, add aluminum alkoxide, reacted about 10~60 minutes, add entry reaction 5~30 minutes, be warming up to 170~200 ℃, kept 20~40 minutes, add the residue base oil and be cooled to about 100 ℃, get final product.
Said calcium sulfonate complex grease is made up of base oil, non-newtonian fluid high alkalinity calcium mahogany sulfonate and compound calcium viscosifying agent.In calcium sulfonate complex grease weight is 100%, and non-newtonian fluid high alkalinity calcium mahogany sulfonate weight is 20~50%, and compound calcium viscosifying agent weight is 2~10%, and all the other are base oil.
Said non-newtonian fluid high alkalinity calcium mahogany sulfonate is to be formed by newton's height alkalescence calcium mahogany sulfonate and transforming agent reaction, and transforming agent wherein can be that carbon number is C 1-C 5Fatty Alcohol(C12-C14 and C12-C18), lipid acid, aliphatic ketone, alkanoic, low molecule ether, alkylamine, and water, boric acid, alkyl or aryl phosphoric acid, phosphonic acids, carbonic acid gas, phenol, cycloalkanol, aromatic alcohol, C 1-C 5The cycloalkanes amine that alkyl replaces, aromatic amine etc., also can be the mixture of above-mentioned two or more compound, the mixture of two or more in the compounds such as preferable formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, Virahol, n-propyl alcohol, ethylene glycol monomethyl ether, phenol, acetaldehyde, ketone, methylamine, ethamine, propylamine, 3-methyl cyclohexylamine, aniline and water.
Said compound calcium viscosifying agent is to be formed by ten dihydroxystearic acids, boric acid and calcium hydroxide reaction, wherein the mol ratio of ten dihydroxystearic acids, boric acid is 1: 0.8~1.2, and the mole number of calcium hydroxide is ten dihydroxystearic acids and boric acid mole number sum 1~1.2 times.
Calcium sulfonate complex grease can be by following prepared: part base oil, high alkalinity calcium mahogany sulfonate newton's body and transforming agent are mixed, about 30~90 minutes of 80~100 ℃ of reactions, make high alkalinity calcium mahogany sulfonate newton body be converted into non-newtonian fluid, as the part viscosifying agent of calcium sulfonate complex grease.Add the residue base oil, add ten dihydroxystearic acids, boric acid aqueous solution and calcium hydroxide aqueous solution and reacted about 30~90 minutes, be warmed up to 170~210 ℃, kept 20~40 minutes, circulation is cooled to about 100 ℃, gets final product.
Lubricating grease of the present invention has good high and low temperature, water resisting property, pumping, rust-preventing characteristic, mechanical stability and resistance to abrasion, poisonous element such as not phosphorous and volatilization obnoxious flavour in the composition do not add any additives and can satisfy the lubricated of naval vessel waterborne and underwater submarine.
Embodiment
The following example is used to illustrate the present invention, but the invention is not restricted to these embodiment.
Embodiment 1
With 100 ℃ of viscosity 30mm 2The refined mineral oil 50kg of/s, stearic acid 5.6kg and phenylformic acid 2.4kg add in the system fat still, stirring is warming up to 80 ℃, add aluminium isopropoxide 4.82kg, 90~110 ℃ of scope internal reactions 30 minutes, add entry 0.5kg reaction 10 minutes, be warming up to 190 ℃, kept 30 minutes, add remaining 42kg refined mineral oil, be cooled to 100 ℃, (calculate principle: product weight is considered as equaling the weight sum of base oil and two kinds of acid to obtain the about 100kg of aluminum complex grease.Because pure reactive aluminum is emitted Virahol, remaining aluminium accounting example is very little, and base oil high temperature has vaporization losses), material changes the mediation still over to.
With 100 ℃ of viscosity 30mm 2The refined mineral oil 20kg of/s, T106 high alkaline calcium sulfonate 40kg, water 4kg and acetic acid 0.6kg add in the still, 80~95 ℃ of reactions down, treat the material retrogradation, with the Fourier transformation infrared spectrometer test, at 881-886cm -1There is the absorption peak of calcite type calcium carbonate at the place, in still, add remaining 38kg base oil, ten dihydroxystearic acid 2kg, boric acid 0.42kg and calcium hydroxide 0.54kg, saponification reaction 40 minutes, being warmed up to 200 ℃ kept 20 minutes, circulation is cooled to 100 ℃, and (calculate principle: product weight is considered as equaling the weight sum of base oil and T106 and ten dihydroxystearic acids to obtain the about 100kg of calcium sulfonate complex grease.Because the weight of the calcium in boric acid and the calcium hydroxide is less, offset with the vaporization losses of base oil), material changes the mediation still over to.
Aluminum complex grease mixes with calcium sulfonate complex grease in the still, stir, circulating evenly gets final product being in harmonious proportion.Resulting product physicochemical property is detected, the results are shown in Table 1.
Embodiment 2
With 100 ℃ of viscosity 10mm 2The refined mineral oil 56kg of/s, stearic acid 2.8kg and phenylformic acid 1.2kg add in the system fat still, stirring is warming up to 80 ℃, add aluminium isopropoxide 2.4kg,, add entry 0.25kg reaction 10 minutes 90~110 ℃ of scope internal reactions 30 minutes, be warming up to 190 ℃, kept 30 minutes, and added remaining 50kg refined mineral oil, be cooled to 100 ℃, obtain the about 110kg of aluminum complex grease, material changes the mediation still over to.
With 100 ℃ of viscosity 30mm 2The refined mineral oil 4kg of/s, T106 high alkaline calcium sulfonate 10kg, water 0.8kg and ethylene glycol monomethyl ether 0.3kg add in the still, 80~95 ℃ of reactions down, treat the material retrogradation, with the Fourier transformation infrared spectrometer test, at 881-886cm -1There is the absorption peak of calcite type calcium carbonate at the place, in still, add remaining 30kg base oil, ten dihydroxystearic acid 5kg, boric acid 1kg and calcium hydroxide 1.3kg, saponification reaction 90 minutes, being warmed up to 180 ℃ kept 40 minutes, circulation is cooled to 100 ℃, obtain the about 50kg of complex calcium sulfonate base, material changes the mediation still over to.
Aluminum complex grease mixes with calcium sulfonate complex grease in the still, stir, circulating evenly gets final product being in harmonious proportion.Resulting product physicochemical property is detected, the results are shown in Table 1.
Embodiment 3
With 100 ℃ of viscosity 20mm 2The refined mineral oil 57kg of/s, stearic acid 9.1kg and phenylformic acid 3.9kg add in the system fat still, stirring is warming up to 80 ℃, add aluminium isopropoxide 7.84kg,, add entry 0.8kg reaction 10 minutes 90~110 ℃ of scope internal reactions 30 minutes, be warming up to 190 ℃, kept 30 minutes, and added remaining 30kg refined mineral oil, be cooled to 100 ℃, obtain the about 100kg of aluminum complex grease, material changes the mediation still over to.
Proportion of composing and prepared 500kg lubricating grease according to preparation calcium sulfonate complex grease among the embodiment 1 change in the mediation still.
Aluminum complex grease mixes with calcium sulfonate complex grease in the still, stir, circulating evenly gets final product being in harmonious proportion.Resulting product physicochemical property is detected, the results are shown in Table 1.
Comparative example
With 100 ℃ of viscosity 30mm 2The refined mineral oil 50kg of/s, stearic acid 5.6kg and phenylformic acid 2.4kg add in the system fat still, stirring is warming up to 80 ℃, add aluminium isopropoxide 4.82kg, 90~110 ℃ of scope internal reactions 30 minutes, add entry 0.5kg reaction 10 minutes, be warming up to 190 ℃, kept 30 minutes, add remaining 42kg refined mineral oil, be cooled to 100 ℃, material changes the mediation still over to.Stir, circulate evenly, wrapped product.The product physicochemical property sees Table 1.
Table 1 product physicochemical property
Analysis project Example 1 Example 2 Example 3 Comparative example Test method
Outward appearance Evenly bright Evenly bright Evenly bright Be gelatin Range estimation
Drawing cone in-degree (0.1mm) 280 290 255 270 GB/T269
Prolongation Drawing cone in-degree (10,000 times, 0.1mm) softening rate, % -2 -4 +1 -15 GB/T269
Prolongation Drawing cone in-degree (100,000 times, 0.1mm) softening rate, % +7 +9 +5 +20 GB/T269
Dropping point (℃) >280 >280 >280 >280 GB/T4929
Corrosion (100 ℃, 24h, T 2Copper sheet) 1b 1b 1b 4a GB/T7326 first method
Rust-preventing characteristic (52 ℃, 48h, level) 1 1 1 3 GB/T5018
Anti-water spray (weight loss %) 21 18 23 19 SH/T0643
Similar viscosity (0 ℃, 200s -1,Pa.s) 17 34 15 28 SH/T0048
Four-ball test (392N, 60min), mm 0.43 0.50 0.39 0.92 SH/T0204
As can be seen from Table 1, lubricating grease of the present invention need not add any additives, promptly have good high and low temperature, water resisting property, pumping, rust-preventing characteristic, mechanical stability and resistance to abrasion, poisonous element such as not phosphorous and volatilization obnoxious flavour are specially adapted to the lubricated of naval vessel waterborne and underwater submarine in the composition.

Claims (18)

1. a grease composition is mixed by aluminum complex grease and calcium sulfonate complex grease, and the weight ratio of the two is 1: 0.2~7.0.
2. according to the described composition of claim 1, it is characterized in that the weight ratio of mixture of aluminum complex grease and calcium sulfonate complex grease is 1: 0.5~3.0.
3. according to claim 1 or 2 described compositions, it is characterized in that said aluminum complex grease is made up of compound aluminium soap viscosifying agent and base oil that phenylformic acid, lipid acid and aluminum alkoxide reaction generate.
4. according to the described composition of claim 3, it is characterized in that wherein compound aluminium soap viscosifying agent accounts for 3%~15% of aluminum complex grease weight, all the other are base oil.
5. according to the described composition of claim 3, it is characterized in that said base oil is 100 ℃ of viscosity 10~40mm 2The mineral oil of/s.
6. according to the described composition of claim 3, it is characterized in that said lipid acid is C 8~C 20Monocarboxylic acid.
7. according to the described composition of claim 6, it is characterized in that said lipid acid is ten dihydroxystearic acids or stearic acid.
8. according to the described composition of claim 3, it is characterized in that the mol ratio of phenylformic acid and lipid acid is 1: 0.8~1.2.
9. according to the described composition of claim 3, it is characterized in that said aluminum alkoxide is aluminium isopropoxide or aluminium isopropoxide tripolymer.
10. according to the described composition of claim 3, it is characterized in that the mole number of aluminum alkoxide is phenylformic acid and lipid acid mole number sum 0.5~0.7 times.
11. according to the described composition of claim 3, it is characterized in that, the preparation method of aluminum complex grease comprises: lipid acid and phenylformic acid are mixed with the part base oil and heat up, add aluminum alkoxide at 90~110 ℃, reacted 10~60 minutes, add entry reaction 5~30 minutes, be warming up to 170~200 ℃, kept 20~40 minutes, and added the residue base oil, the circulation cooling.
12., it is characterized in that said calcium sulfonate complex grease is made up of base oil, non-newtonian fluid high alkalinity calcium mahogany sulfonate and compound calcium viscosifying agent according to claim 1 or 2 described compositions.
13., it is characterized in that according to the described composition of claim 12, be 100% in calcium sulfonate complex grease weight, non-newtonian fluid high alkalinity calcium mahogany sulfonate weight is 20%~50%, and compound calcium viscosifying agent weight is 2%~10%, and all the other are base oil.
14., it is characterized in that said non-newtonian fluid high alkalinity calcium mahogany sulfonate is to be formed by newton's height alkalescence calcium mahogany sulfonate and transforming agent reaction according to the described composition of claim 13, transforming agent wherein is that carbon number is C 1-C 5Fatty Alcohol(C12-C14 and C12-C18), lipid acid, aliphatic ketone, alkanoic, low molecule ether, alkylamine, or water, boric acid, alkyl or aryl phosphoric acid, phosphonic acids, carbonic acid gas, phenol, cycloalkanol, aromatic alcohol, C 1-C 5Cycloalkanes amine, aromatic amine that alkyl replaces, or the mixture of above-mentioned two or more compound.
15. according to the described composition of claim 14, it is characterized in that said transforming agent is two or more the mixture in formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, Virahol, n-propyl alcohol, ethylene glycol monomethyl ether, phenol, acetaldehyde, ketone, methylamine, ethamine, propylamine, 3-methyl cyclohexylamine, aniline or the water.
16., it is characterized in that said compound calcium viscosifying agent is to be formed by ten dihydroxystearic acids, boric acid and calcium hydroxide reaction according to the described composition of claim 12.
17., it is characterized in that wherein the mol ratio of ten dihydroxystearic acids and boric acid is 1: 0.8~1.2 according to the described composition of claim 16, the mole number of calcium hydroxide is ten dihydroxystearic acids and boric acid mole number sum 1~1.2 times.
18. according to the described composition of claim 12, it is characterized in that, the preparation method of calcium sulfonate complex grease comprises: part base oil, high alkalinity calcium mahogany sulfonate newton's body and transforming agent are mixed, about 30~90 minutes of 80~100 ℃ of reactions, make high alkalinity calcium mahogany sulfonate newton body be converted into non-newtonian fluid, as the part viscosifying agent of calcium sulfonate complex grease; Add the residue base oil, add ten dihydroxystearic acids, boric acid aqueous solution and calcium hydroxide aqueous solution and reacted about 30~90 minutes, be warmed up to 170~210 ℃, kept 20~40 minutes, the circulation cooling.
CNB2006100890282A 2006-07-31 2006-07-31 Grease composition Active CN100549147C (en)

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Families Citing this family (5)

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Publication number Priority date Publication date Assignee Title
DE102010006745A1 (en) * 2010-02-02 2011-08-04 Fuchs Petrolub AG, 68169 Greases containing lignosulfonate, their preparation and use
CN106032477B (en) * 2015-03-11 2019-01-08 中国石油化工股份有限公司 Lubricant composition and preparation method thereof
TW201908474A (en) * 2017-07-24 2019-03-01 美商坎圖爾公司 Extremely high pressure metal sulfonate grease
CN110408459A (en) * 2019-07-22 2019-11-05 纳拓润滑技术(上海)有限公司 A kind of high-performance composite aluminum base bentonite grease and preparation method thereof
CN114133975B (en) * 2021-11-22 2023-03-14 江西优宝新材料科技有限公司 Food-grade lubricating grease and preparation method thereof

Non-Patent Citations (4)

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复合磺酸钙基润滑脂的结构组成及应用. 益建国.汽车工艺与材料,第3期. 2005 *
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