CN1364859A - Mixed lubricating grease with high extreme polar pressure thickener and its preparing method - Google Patents
Mixed lubricating grease with high extreme polar pressure thickener and its preparing method Download PDFInfo
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- CN1364859A CN1364859A CN 01102234 CN01102234A CN1364859A CN 1364859 A CN1364859 A CN 1364859A CN 01102234 CN01102234 CN 01102234 CN 01102234 A CN01102234 A CN 01102234A CN 1364859 A CN1364859 A CN 1364859A
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Abstract
The lubricating grease consists of base oil 45-67 wt%, thickener 10-20 wt% and extreme pressure wear resisting additive 23-35 wt%, where the base oil is mixture of low viscosity mineral oil with viscosity of 6-20 sq mm/s as 100 deg.c and high viscosity mineral oil with viscosity of 20-40 sq mm/s at 100 deg.c, the thickener is the mixture of polyurea thickener and composite calcium-base thickener, and the extreme pressure wear resisting additive is the mixture of molybdenum disulfide and antimony troxide. The lubricating grease of the present invention has excellent high temperature performance, colloid stability, mechanical stability, anticorrosion performance and very high extreme pressure antiwear performance.
Description
The invention belongs to lubricating grease, more particularly, the present invention is a kind of mixing thickened agent lubricant grease of high extreme pressure.
The lubricating grease kind is a lot, polyurea grease, compositing lithio ester, calcium grease, composite calcium-base fat, wilkinite fat is arranged, mix thickened agent lubricant grease or the like.As US 5,084, the 193 mixing thickened agent lubricant greases of introducing are to be mixed by calcium base viscosifying agent and polyurea thickening agent, and are added with various sulfur-bearing phosphorus additives, and this lubricating grease over-all properties is better.High extreme pressure grease generally all is single soap lubricating grease, and as US 5,015,401 lubricating grease of introducing are to be mixed by complex calcium lubricating grease interpolation molybdenumdisulphide and Calcium Fluoride (Fluorspan).Because the performance deficiency of complex calcium lubricating grease itself, it is the long-time easy hardening of placement surface in air.
The purpose of this invention is to provide a kind of multiple-effect and mix thickened agent lubricant grease with high dropping point, good mechanical stability, particularly high extreme pressure and antiwear behavior.
Another object of the present invention is to provide above-mentioned preparation of greases method.
Grease composition provided by the invention (is benchmark with lubricating grease weight) is: base oil 45～67%, and preferred 53～62%, viscosifying agent 10～20%, preferred 13～17%, extreme-pressure anti-friction additive 23～35%, preferred 25～30%.
Described base oil is the miscellany of low viscosity mineral oil and high viscosity mineral oil, and the weight ratio of the two is 1: 0.2～5, preferred 1: 0.5～2.Wherein 100 of the low viscosity Dormant oils ℃ of viscosity are 6～20mm
2/ s is preferably 8～14mm
2/ s.100 ℃ of viscosity of high viscosity Dormant oils are 20～40mm
2/ s is preferably 25～35mm
2/ s.
Described viscosifying agent is to be mixed by polyurea thickening agent and composite calcium-base viscosifying agent, wherein polyurea thickening agent is to be that 8～18 primary amine and isocyanate reaction form by carbon number, and the composite calcium-base viscosifying agent is to be formed by Glacial acetic acid and n-caprylic acid (or boric acid), ten dihydroxystearic acids (or stearic acid) and calcium hydroxide (or calcium oxide) reaction.The weight ratio of polyurea thickening agent and composite calcium-base viscosifying agent 1: 0.3～3, preferred 1: 0.7～2.
Described extreme-pressure anti-friction additive is to be mixed by molybdenumdisulphide, antimonous oxide, and the weight ratio of the two is 1: 0.2～1.2, preferred 1: 0.3～0.8.Can also contain lime carbonate in the extreme-pressure anti-friction additive, can further improve the extreme pressure and antiwear behavior of lubricating grease, wherein the weight ratio of lime carbonate and molybdenumdisulphide is 0～1: 1, preferred 0.2～0.8: 1.
Preparation of greases method provided by the invention comprises:
1) base oil is mixed with calcium hydroxide (or calcium oxide) and water, add Glacial acetic acid, n-caprylic acid (or boric acid) and ten dihydroxystearic acids (or stearic acid) respectively, the dehydration that heats up begins the homogenizing of lowering the temperature to 210～230 ℃, obtains composite calcium-base fat;
2) with base oil and aliphatic amide and the dissolved vulcabond mix, add suitable quantity of water, be warming up to 150～220 ℃ of reactions 0.5～3 hour, cooling is ground, and obtains areidofat;
3) composite calcium-base fat and areidofat are mixed, add molybdenumdisulphide, antimonous oxide and lime carbonate optionally, stir, promptly get lubricating grease of the present invention.
Said base oil is meant that 100 ℃ of viscosity are 6～20mm
2/ s, preferred 8～14mm
2The low viscosity Dormant oils of/s and 100 ℃ of viscosity are 20～40mm
2/ s, preferred 25～35mm
2The high viscosity Dormant oils of/s.Wherein the allocation proportion of low viscosity Dormant oils in calcium grease and areidofat can be 0.2～2: 1, preferred 0.5～1.5: 1; The allocation proportion of high viscosity Dormant oils in calcium grease and areidofat can be 0.5～5: 1, preferred 0.7～2: 1.
Specifically, lubricating grease of the present invention can adopt following method preparation:
1) preparation of composite calcium-base fat.With required low viscosity Dormant oils and high viscosity Dormant oils 50～80% mixing at normal temperatures separately with calcium hydroxide (or calcium oxide) and water, add Glacial acetic acid respectively, n-caprylic acid or boric acid, ten dihydroxystearic acids or stearic acid, whenever after adding a kind of acid, preferably reaction earlier is after about 5～15 minutes, add another kind of acid again, after three kinds of acid all add, heat up, water is discharged from reactant, add all the other 20～50% low viscosity Dormant oils and high viscosity Dormant oils, be warmed up to 210～230 ℃, begin the circulation cooling, and carry out homogenizing in about 120 ℃, homogenization pressures is generally 0.6～0.8MPa, the homogenizing time obtains calcium grease for being generally 10～50 minutes.
2) preparation of areidofat.Earlier with aliphatic amide and high viscosity Dormant oils Hybrid Heating to 60～80 ℃ in the normal pressure still, simultaneously in another container with vulcabond and low viscosity Dormant oils heating for dissolving, pour in the normal pressure still, stir, add suitable quantity of water, be warming up to 150～220 ℃ of reactions 0.5～3 hour, cooling is ground, and obtains areidofat.
3) preparation of mixing thickened agent lubricant grease.About 70～80 ℃ with step 1), 2) calcium grease of preparation and areidofat and various additive mix and stir, and goes out still in about 50 ℃, promptly gets grease product.
Lubricating grease result of performance test of the present invention shows, have excellent high-temperature performance, colloid stability energy, mechanical stability energy, Corrosion Protection and excellent especially extreme pressure and antiwear behavior, be applicable to working parts such as drill bit, bearing, heavy loading gear, constant velocity cardan joint.
Further specify characteristics of the present invention below by example.
Example 1
With 8.0Kg 500SN oil (100 ℃ of viscosity 11mm
2/ s) with 4.0Kg 150BS oil (100 ℃ of viscosity 29mm
2/ s), 1.8Kg calcium hydroxide and 5.0Kg water add in the normal pressure still, stir, add the 2.2Kg Glacial acetic acid at normal temperatures, stir, and reacted about 10 minutes, add the 0.5Kg n-caprylic acid, stir, add ten dihydroxystearic acid 2.2Kg, heat to about 110 ℃, water is discharged, add 5.4Kg 500SN oil and 2.6Kg 150SN oil at last, continue to be warmed up to 220 ℃, circulation cooling, and normal temperature grinding get calcium grease 26.7Kg.
Amino dodecane 3.0Kg and 150BS oil 13.3Kg are added in the normal pressure still, and be heated to 70 ℃, in container A, add vulcabond (MDI) 2.1Kg and 500SN oil 6.7Kg simultaneously, be heated to MDI and dissolve fully.MDI oil solution in the container A is poured in the still, stirred, add entry 500ml, heat to 195 ℃, constant temperature 0.5 hour, circulation cooling and normal temperature grind, and get areidofat 25.1Kg.
Calcium grease 725g is mixed with areidofat 725g, stir, add 290g molybdenumdisulphide again, the lime carbonate of 160g antimonous oxide and 100g, stirring promptly gets grease product.
Example 2
To mix with areidofat 1087.5g by the calcium grease 362.5g that example 1 method makes, stir, add 285g molybdenumdisulphide again, the lime carbonate of 165g antimonous oxide and 200g, stirring promptly gets grease product.
Example 3
With 2.7Kg 500SN oil 2.7Kg 150BS oil, 0.8Kg calcium hydroxide and 3Kg water add in the normal pressure still, stir, add the 0.9Kg Glacial acetic acid at normal temperatures, stir, and reacted about 10 minutes, add 0.2Kg boric acid, stir, add ten dihydroxystearic acid 0.9Kg, heat to about 100 ℃, water is discharged, add 1.3Kg 500SN oil and 1.3Kg 150SN oil at last, continue to be warmed up to 220 ℃, circulation cooling, and normal temperature grinding get calcium grease 10.8Kg.
Stearylamine 1.2Kg and 150BS oil 4.1Kg are added in the normal pressure still, and be heated to 70 ℃, in container A, add vulcabond (MDI) 0.6Kg and 500SN oil 4.1Kg simultaneously, be heated to MDI and dissolve fully.MDI oil solution in the container A is poured in the still, stirred, add entry 300g, heat to 180 ℃, constant temperature 1 hour, circulation cooling and normal temperature grind, and get areidofat 10.0Kg.
Calcium grease 200g is mixed with areidofat 200g, stir, add 65.8g molybdenumdisulphide again, the 40.5g antimonous oxide, stirring promptly gets grease product.
Example 4
According to the method for example 1, preparation 120Kg lubricating grease in the 100L still.Wherein composite calcium-base viscosifying agent content is 7.25%, and carbamido thickening agent content is 7.0%, and molybdenumdisulphide content is 14.5%, and antimonous oxide content is 8.0%, and calcium carbonate powders content is 5.0%, and the 150BS oil-contg is 19.4%, and the 500SN oil-contg is 38.9%.
Example 5
This example is the performance test of grease product, the results are shown in Table 1.
Table 1
As can be seen from Table 1, grease product of the present invention has high dropping point, favorable mechanical stability and excellent extreme pressure property.
Claims (13)
1. the mixing thickened agent lubricant grease of a high extreme pressure is a benchmark with lubricating grease weight, comprising: base oil 45～67%, viscosifying agent 10～20%, extreme-pressure anti-friction additive 23～35%, wherein said base oil are 100 ℃ of viscosity 6～20mm
2The low viscosity mineral oil of/s and 100 ℃ of viscosity 20～40mm
2The miscellany of the high viscosity mineral oil of/s, described viscosifying agent are polyurea thickening agent and composite calcium-base viscosifying agent mixture, and described extreme-pressure anti-friction additive is the mixture of molybdenumdisulphide and antimonous oxide.
2. lubricating grease according to claim 1 is characterized in that, comprises base oil 53～62%, viscosifying agent 13～17%, extreme-pressure anti-friction additive 25～30%.
3. lubricating grease according to claim 1 is characterized in that, 100 ℃ of viscosity of low viscosity Dormant oils are 8～14mm
2/ s, 100 ℃ of viscosity of high viscosity Dormant oils are 25～35mm
2/ s.
4. lubricating grease according to claim 1 is characterized in that, the weight ratio of low viscosity mineral oil and high viscosity mineral oil is 1: 0.2～5.
5. lubricating grease according to claim 4 is characterized in that, the weight ratio of low viscosity mineral oil and high viscosity mineral oil is 1: 0.5～2.
6. lubricating grease according to claim 1, it is characterized in that, described polyurea thickening agent is to be that 8～18 primary amine and isocyanate reaction form by carbon number, and the composite calcium-base viscosifying agent is to be formed by Glacial acetic acid and n-caprylic acid (or boric acid), ten dihydroxystearic acids (or stearic acid) and calcium hydroxide (or calcium oxide) reaction.
7. lubricating grease according to claim 1 is characterized in that, the weight ratio 1: 0.3～3 of polyurea thickening agent and composite calcium-base viscosifying agent.
8. lubricating grease according to claim 7 is characterized in that, the weight ratio 1: 0.7～2 of polyurea thickening agent and composite calcium-base viscosifying agent.
9. lubricating grease according to claim 1 is characterized in that, the weight ratio of molybdenumdisulphide and antimonous oxide is 1: 0.2～1.2 in the described extreme-pressure anti-friction additive.
10. lubricating grease according to claim 9 is characterized in that, the weight ratio of molybdenumdisulphide and antimonous oxide is 1: 0.3～0.8 in the described extreme-pressure anti-friction additive.
11. lubricating grease according to claim 1 is characterized in that, can also contain lime carbonate in the described extreme-pressure anti-friction additive, wherein the weight ratio of lime carbonate and molybdenumdisulphide is 0～1: 1.
12. the described preparation of greases method of claim 1 comprises:
1) base oil is mixed with calcium hydroxide (or calcium oxide) and water, add Glacial acetic acid, n-caprylic acid (or boric acid) and ten dihydroxystearic acids (or stearic acid) respectively, the dehydration that heats up begins the homogenizing of lowering the temperature to 210～230 ℃, obtains composite calcium-base fat;
2) base oil is mixed with aliphatic amide, vulcabond, add suitable quantity of water, be warming up to 150～220 ℃ of reactions 0.5～3 hour, cooling is ground, and obtains areidofat;
3) composite calcium-base fat and areidofat are mixed, add molybdenumdisulphide, antimonous oxide and lime carbonate optionally, stir, promptly get lubricating grease of the present invention;
Said base oil comprises that 100 ℃ of viscosity are 6～20mm
2The low viscosity Dormant oils of/s and 100 ℃ of viscosity are 20～40mm
2The high viscosity Dormant oils of/s, wherein the allocation proportion of low viscosity Dormant oils in calcium grease and areidofat is 0.2～2: 1, the allocation proportion of high viscosity Dormant oils in calcium grease and areidofat is 0.5～5: 1.
13. lubricating grease according to claim 12 is characterized in that, said base oil comprises that 100 ℃ of viscosity are 8～14mm
2The low viscosity Dormant oils of/s and 100 ℃ of viscosity are 25～35mm
2The high viscosity Dormant oils of/s, wherein the allocation proportion of low viscosity Dormant oils in calcium grease and areidofat is 0.5～1.5: 1, the allocation proportion of high viscosity Dormant oils in calcium grease and areidofat is 0.7～2: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011022345A CN1141368C (en) | 2001-01-18 | 2001-01-18 | Mixed lubricating grease with high extreme polar pressure thickener and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011022345A CN1141368C (en) | 2001-01-18 | 2001-01-18 | Mixed lubricating grease with high extreme polar pressure thickener and its preparing method |
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| Publication Number | Publication Date |
|---|---|
| CN1364859A true CN1364859A (en) | 2002-08-21 |
| CN1141368C CN1141368C (en) | 2004-03-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358984C (en) * | 2005-08-05 | 2008-01-02 | 鞍山海华油脂化学有限公司 | Composite calcium sulphonate lubricating grease |
| CN100358986C (en) * | 2005-08-05 | 2008-01-02 | 鞍山海华油脂化学有限公司 | Composite high temperature areidofat |
| CN100358987C (en) * | 2005-08-05 | 2008-01-02 | 鞍山海华油脂化学有限公司 | High extreme pressure lithium base lubricating grease |
| CN101705140B (en) * | 2009-11-09 | 2012-08-08 | 鞍山海华油脂化学有限公司 | High-temperature grease and preparation method thereof |
| CN102703176A (en) * | 2012-04-27 | 2012-10-03 | 上海德古润滑油有限公司 | Leakproof lubricant for reducer |
| CN103254965A (en) * | 2012-02-21 | 2013-08-21 | 中国石油化工股份有限公司 | Complex-calcium-based tetrapolyurea lubricating grease and preparation method thereof |
| CN106833862A (en) * | 2016-12-12 | 2017-06-13 | 安徽省东至县东鑫冲压件有限责任公司 | A kind of press preparation of greases method |
-
2001
- 2001-01-18 CN CNB011022345A patent/CN1141368C/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358984C (en) * | 2005-08-05 | 2008-01-02 | 鞍山海华油脂化学有限公司 | Composite calcium sulphonate lubricating grease |
| CN100358986C (en) * | 2005-08-05 | 2008-01-02 | 鞍山海华油脂化学有限公司 | Composite high temperature areidofat |
| CN100358987C (en) * | 2005-08-05 | 2008-01-02 | 鞍山海华油脂化学有限公司 | High extreme pressure lithium base lubricating grease |
| CN101705140B (en) * | 2009-11-09 | 2012-08-08 | 鞍山海华油脂化学有限公司 | High-temperature grease and preparation method thereof |
| CN103254965A (en) * | 2012-02-21 | 2013-08-21 | 中国石油化工股份有限公司 | Complex-calcium-based tetrapolyurea lubricating grease and preparation method thereof |
| CN102703176A (en) * | 2012-04-27 | 2012-10-03 | 上海德古润滑油有限公司 | Leakproof lubricant for reducer |
| CN102703176B (en) * | 2012-04-27 | 2015-08-05 | 上海德古润滑油有限公司 | Leakproof lubricant for reducer |
| CN106833862A (en) * | 2016-12-12 | 2017-06-13 | 安徽省东至县东鑫冲压件有限责任公司 | A kind of press preparation of greases method |
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| Publication number | Publication date |
|---|---|
| CN1141368C (en) | 2004-03-10 |
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