CN101117605A - Preparation method of composite titanium radical lubricating grease and product produced thereby - Google Patents
Preparation method of composite titanium radical lubricating grease and product produced thereby Download PDFInfo
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Abstract
The present invention provides a preparation method for compound titanium base grease lubricant, according to the sequence, the following steps are included: firstly, fatty acid and base oil are mixed together and heated, when the temperature is raised to 70 to 90 DEG C, the tetraiopropyl titanate is added in for reaction; secondly, when the temperature is raised to 130 to 150 DEG C, aromatic acid is added in for reaction; thirdly, cool oil is added in for reducing the temperature, and distilled water is added in; fourthly, the temperature is increased to 170 to 200 DEG C for high temperature refining, the rest cool oil is added in, the temperature is reduced, and the reactant is ground to get the end product. The product got from the present invention has obviously better mechanical stability, as well as better abrasion resistance under the extreme pressure than that got from the prior technology.
Description
Technical field
The present invention relates to the preparation of greases method, specifically, is the preparation method of composite titan-based grease, and the product that makes thus.
Background technology
As everyone knows, titanium elements is the content height in the earth's crust not only, and itself has environment friendly, in field widespread uses such as iron and steel, oil refining, chemical industry.In the lubricating grease field, at the beginning of the nineties in last century, the investigator of India has successfully developed the multi-functional composite titan-based grease of high-performance, is acknowledged as a quantum jump of lubricating grease industry.On use properties, the composite titan-based grease (basic fat) that does not add any functional additive with the interpolation of present widespread use overstocked anti-wear agent extreme pressure compound lithium base fat compare, extreme pressure property is quite even exceed; And this fat and traditional high-performance lubricating grease has good consistency, is considered to a class lubricating grease of multifunctional high-performance.
US 5,387, and 351 composite titan-based greases use isopropyl titanate, lipid acid and aromatic carboxylic acid to be raw material, prepare composite titan-based grease basis fat.Its product has good extreme pressure anti-wear, good non-corrosibility, and still, mechanical stability is still unsatisfactory.
US 6,172, added multiple functional additive in 012 composite titan-based grease, further strengthened the performance such as the extreme pressure anti-wear of composite titan-based grease basis fat, and still, this patent does not relate to the improvement of the mechanical stability of this fat.
Summary of the invention
The invention provides a kind of preparation method of composite titan-based grease, the mechanical stability of products obtained therefrom and extreme pressure anti-wear obviously are better than prior art.
The present invention also provides the lubricating grease that uses the inventive method to obtain.
The preparation method of composite titan-based grease provided by the invention may further comprise the steps in order:
(1) lipid acid is mixed with base oil and heat, when temperature rises to 70～95 ℃, add titanium isopropylate and react;
(2) be warming up to 130～150 ℃, add aromatic acid and react;
(3) add the cold oil cooling, add distilled water;
(4) be warming up to 170～200 ℃ and carry out the high temperature refining, add residue cold oil, cooling is ground, and obtains the finished product.
The cold oil that the base oil of step (1) and step (3) and (4) add is whole base oils, and the base oil of step (1) accounts for 50%～80% of whole base oil weight, preferred 55%～65%.
The reaction times of step (1) is about 30～90 minutes.
The reaction times of step (2) is about 10～60 minutes.
Step (3) adds an amount of cold oil reduces to below 100 ℃ temperature, and preferred 80～95 ℃, add excessive distilled water then, the remaining isopropoxy of isopropyl titanate is sloughed in water and titanium isopropylate reaction, finally forms the titanium soap.
Step (4) rises to 170～200 ℃ with temperature and carries out the high temperature refining, to improve the soap fibrous texture.The high temperature refining stopped heating after 20～100 minutes.Add residue cold oil, continue to stir, treat that temperature of charge is reduced to 85～100 ℃ after, grinding product obtains the finished product.
Said base oil is mineral oil, synthetic hydrocarbon oil or the like, and 100 ℃ of viscosity are 30～50mm2/s.
Said lipid acid is C
12～C
20Monocarboxylic acid, preferred stearic acid, or the mixture of stearic acid and ten dihydroxystearic acids, wherein the weight content of ten dihydroxystearic acids is 1%～15%, preferred 2%～10%.
Said aromatic acid is terephthalic acid or phenylformic acid, and weight is 20%～70% of fatty acid wt, preferred 30%～60%.
Titanium isopropylate weight be 70%～100% of fatty acid wt, preferred 80%～95%.
The viscosifying agent that is generated by metatitanic acid four isopropyl esters, lipid acid, aromatic acid and water reaction accounts for 6%～20% of lubricating grease gross weight, preferred 8%～15%.
According to the dropping point of technology products obtained therefrom of the present invention all more than 280 ℃; Mechanical stability good (100,000 times cut off softening rate less than 10%), the sintering load of basic fat can reach 3090N (315kg), illustrates that mechanical stability and extreme pressure anti-wear have surpassed prior art.
The composite titan-based grease that the present invention obtains can be applicable to have vast market prospect on steel mill, cement mill, power station, packaging industry, chemical plant and the automobile.
Embodiment
Following raw material is the commercial goods.
Embodiment 1
237g huge port lithium material, 46g stearic acid mixture (wherein 4g ten dihydroxystearic acids) are added in the still, be heated to 75 ℃, 45 gram isopropyl titanates are added, be incubated 90 minutes.After insulation finishes, continue heating and make temperature rise to 135 ℃, add the 27g terephthalic acid, this temperature insulation 20 minutes.After insulation finishes, stop to heat and adding 50g cold oil, when temperature in the kettle drops to 80 ℃, add 5g distilled water, and recover heating, make temperature in the kettle rise to 175 ℃, and high temperature was refined 45 minutes under this temperature.After the high temperature refining, stop heating, will remain cold oil 230g and add, treat that temperature of charge drops to 90 ℃ after, with the product grinding, obtain product, its physico-chemical property sees Table one.
Embodiment 2
340g huge port lithium material, 48g stearic acid mixture (wherein 2g ten dihydroxystearic acids) are added in the still, be heated to 90 ℃, the 40g isopropyl titanate is added, be incubated 45 minutes.After insulation finishes, continue heating and make temperature rise to 140 ℃, add the 29g terephthalic acid, this temperature insulation 40 minutes.After insulation finishes, stop to heat and adding 50g cold oil, when temperature in the kettle drops to 90 ℃, add 8g distilled water, and recover heating, make temperature in the kettle rise to 190 ℃, and high temperature was refined 35 minutes under this temperature.After the high temperature refining, stop heating, will remain cold oil 250g and add, treat that temperature of charge drops to 100 ℃ after, with the product grinding, obtain product, its physico-chemical property sees Table one.
Embodiment 3
330g huge port lithium material, 49g stearic acid mixture (wherein 1g ten dihydroxystearic acids) are added in the still, be heated to 75 ℃, the 50g isopropyl titanate is added, be incubated 60 minutes.After insulation finishes, continue heating and make temperature rise to 150 ℃, add the 23g terephthalic acid this temperature insulation 60 minutes.After insulation finishes, stop to heat and adding 50g cold oil, when temperature in the kettle drops to 90 ℃, add 8g distilled water, and recover heating, make temperature in the kettle rise to 185 ℃, and high temperature was refined 60 minutes under this temperature.After the high temperature refining, stop heating, will remain cold oil 280g and add, treat that temperature of charge drops to 90 ℃ after, with the product grinding, obtain product, its physico-chemical property sees Table one.
Embodiment 4
350g huge port lithium material, 41g stearic acid are added in the still, be heated to 75 ℃, the 52g isopropyl titanate is added, be incubated 70 minutes.After insulation finishes, continue heating and make temperature rise to 150 ℃, add the 26g terephthalic acid this temperature insulation 50 minutes.After temperature in the kettle drops to 90 ℃ of insulations and finishes, add 8g distilled water, and recover heating, make temperature in the kettle rise to 195 ℃, and high temperature refining 60 minutes under this temperature.After the high temperature refining, stop heating, will remain cold oil 240g and add, treat that temperature of charge drops to 90 ℃ after, with the product grinding, obtain product, its physico-chemical property sees Table one.
Embodiment 5
340g huge port lithium material, 41g stearic acid are added in the still, be heated to 75 ℃, the 52g isopropyl titanate is added, be incubated 70 minutes.After insulation finishes, continue heating and make temperature rise to 130 ℃, add the 26g phenylformic acid this temperature insulation 45 minutes.After temperature in the kettle drops to 90 ℃ of insulations and finishes, add 8g distilled water, and recover heating, make temperature in the kettle rise to 185 ℃, and high temperature refining 60 minutes under this temperature.After the high temperature refining, stop heating, will remain cold oil 240g and add, treat that temperature of charge drops to 90 ℃ after, with the product grinding, obtain product, its physico-chemical property sees Table one.
Comparative example
With heating in 300 gram huge port lithium material, 45g stearic acid, the 26g terephthalic acid adding still, when rising to 90～95 ℃, temperature adds isopropyl titanate 44.2 grams.Heat temperature raising slowly rises to about 100 ℃ temperature of reaction system.Reaction is about 2 hours under this temperature, continues then slowly to be warming up to 200 ℃, stops heating, will remain cold oil 260g and add, treat that temperature is reduced to 100 ℃ after, with the product grinding, obtain product.Its physicochemical property sees Table one.
Table one product physicochemical property
| Experimental project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example | Experimental technique |
| Drawing cone in-degree (60 times), 0.1mm | 286 | 295 | 320 | 266 | 283 | 360 | GB/T269 |
| Prolong Drawing cone in-degree (100,000 times) | 288 | 324 | 328 | 292 | 301 | 427 | GB/T269 |
| Dropping point, ℃ | 282 | 281 | 284 | 280 | 281 | 280 | GB/T3498 |
| Corrosion (T 2Copper sheet, 100 ℃, 24h) | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified | GB/T7326 second method |
| Stencil oil-dividing (100 ℃, 24h) | 1.38 | 1.74 | 0.79 | 1.74 | 1.71 | 1.03 | SH/T0324 |
| Four-ball test P D N d 60 40mm | 2450 0.45 | 3090 0.40 | 2450 0.40 | 2450 0.50 | 2450 0.50 | 1960 0.53 | SH/T0202 SH/T0204 |
Claims (18)
1. the preparation method of a composite titan-based grease may further comprise the steps in order:
(1) lipid acid is mixed with base oil and heat, when temperature rises to 70～95 ℃, add titanium isopropylate and react;
(2) be warming up to 130～150 ℃, add aromatic acid and react;
(3) add the cold oil cooling, add distilled water;
(4) be warming up to 170～200 ℃ and carry out the high temperature refining, add residue cold oil, cooling is ground.
2. according to the described preparation method of claim 1, it is characterized in that the reaction times of step (1) is 30～90 minutes.
3. according to the described preparation method of claim 1, it is characterized in that the reaction times of step (2) is 10～60 minutes.
4. according to the described preparation method of claim 1, it is characterized in that step (3) adds cold oil reduces to below 100 ℃ temperature.
5. according to the described preparation method of claim 1, it is characterized in that the high temperature refining time of step (4) is 20～100 minutes.
6. according to the described preparation method of claim 1, it is characterized in that the base oil of step (1) accounts for 50%～70% of whole base oil weight.
7. according to the described preparation method of claim 1, it is characterized in that 100 ℃ of viscosity of said base oil are 30～50mm
2/ s.
8. according to the described preparation method of claim 1, it is characterized in that said base oil is mineral oil or synthetic hydrocarbon oil.
9. according to the described preparation method of claim 1, it is characterized in that said lipid acid is stearic acid, or the mixture of stearic acid and ten dihydroxystearic acids, wherein the weight content of ten dihydroxystearic acids is 1%～15%.
10. according to the described preparation method of claim 9, it is characterized in that said lipid acid is the mixture of stearic acid and ten dihydroxystearic acids, wherein the weight content of ten dihydroxystearic acids is 2%～10%.
11., it is characterized in that said aromatic acid is terephthalic acid or phenylformic acid according to the described preparation method of claim 1.
12., it is characterized in that the weight of aromatic acid is 20%～70% of fatty acid wt according to the described preparation method of claim 1.
13., it is characterized in that the weight of aromatic acid is 30%～60% of fatty acid wt according to the described preparation method of claim 12.
14., it is characterized in that the weight of titanium isopropylate is 70%～100% of fatty acid wt according to the described preparation method of claim 1.
15., it is characterized in that the weight of titanium isopropylate is fatty acid wt 80%～95% according to the described preparation method of claim 15.
16., it is characterized in that the viscosifying agent that is generated by metatitanic acid four isopropyl esters, lipid acid, aromatic acid and water reaction accounts for 6%～20% of lubricating grease gross weight according to the described preparation method of claim 1.
17., it is characterized in that viscosifying agent accounts for 8%～15% of lubricating grease gross weight according to the described preparation method of claim 16.
18. the lubricating grease of claim 1 preparation.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766511A (en) * | 2012-07-10 | 2012-11-07 | 华北电力大学 | Composite calcium sulfonate-titanium composite lubricating grease and preparation method thereof |
| CN103113969A (en) * | 2013-02-21 | 2013-05-22 | 尹继辉 | Modified composite titanium-based grease of micron-nano particles and preparation method thereof |
| CN104164288A (en) * | 2014-08-05 | 2014-11-26 | 中国石油化工股份有限公司 | Compound titanium-based bearing grease composition and preparation method thereof |
| CN104232275A (en) * | 2014-09-24 | 2014-12-24 | 路伯润滑油（苏州）有限公司 | Complex titanium and calcium sulfonate lubricating grease and preparation method thereof |
| CN104342243A (en) * | 2014-09-24 | 2015-02-11 | 路伯润滑油（苏州）有限公司 | Compound titanium-based lubricant and preparation method thereof |
| CN104611095A (en) * | 2015-01-24 | 2015-05-13 | 黑龙江多邦科技开发有限公司 | Compound titanium-based lubricating grease and preparation method thereof |
| CN104830436A (en) * | 2015-05-08 | 2015-08-12 | 江苏大学 | Preparation method of composite titanium-based lubricating grease with high dropping point |
| CN104927977A (en) * | 2015-05-08 | 2015-09-23 | 江苏大学 | Preparation method of low noise compound titanium-based grease |
| CN105062625A (en) * | 2015-08-11 | 2015-11-18 | 新乡市恒星化工有限责任公司 | Preparation method of environment-friendly compound titanium-based grease |
| CN105623801A (en) * | 2015-12-11 | 2016-06-01 | 禾泰特种新材料（苏州）有限公司 | Biodegradable grease composition and preparation method thereof |
| CN110903883A (en) * | 2019-11-15 | 2020-03-24 | 中国人民解放军陆军勤务学院 | Composite titanium-based lubricating grease and preparation method thereof |
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2006
- 2006-07-31 CN CNB2006100890297A patent/CN100558866C/en active Active
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766511B (en) * | 2012-07-10 | 2014-01-15 | 华北电力大学 | Composite calcium sulfonate-titanium composite lubricating grease and preparation method thereof |
| CN102766511A (en) * | 2012-07-10 | 2012-11-07 | 华北电力大学 | Composite calcium sulfonate-titanium composite lubricating grease and preparation method thereof |
| CN103113969A (en) * | 2013-02-21 | 2013-05-22 | 尹继辉 | Modified composite titanium-based grease of micron-nano particles and preparation method thereof |
| CN104164288A (en) * | 2014-08-05 | 2014-11-26 | 中国石油化工股份有限公司 | Compound titanium-based bearing grease composition and preparation method thereof |
| CN104342243B (en) * | 2014-09-24 | 2016-10-26 | 路伯润滑油（苏州）有限公司 | A kind of composite titan-based grease and preparation method thereof |
| CN104232275A (en) * | 2014-09-24 | 2014-12-24 | 路伯润滑油（苏州）有限公司 | Complex titanium and calcium sulfonate lubricating grease and preparation method thereof |
| CN104342243A (en) * | 2014-09-24 | 2015-02-11 | 路伯润滑油（苏州）有限公司 | Compound titanium-based lubricant and preparation method thereof |
| CN104611095A (en) * | 2015-01-24 | 2015-05-13 | 黑龙江多邦科技开发有限公司 | Compound titanium-based lubricating grease and preparation method thereof |
| CN104927977A (en) * | 2015-05-08 | 2015-09-23 | 江苏大学 | Preparation method of low noise compound titanium-based grease |
| CN104830436A (en) * | 2015-05-08 | 2015-08-12 | 江苏大学 | Preparation method of composite titanium-based lubricating grease with high dropping point |
| CN104927977B (en) * | 2015-05-08 | 2017-11-17 | 江苏大学 | A kind of preparation method of low noise composite titan-based grease |
| CN104830436B (en) * | 2015-05-08 | 2017-11-17 | 江苏大学 | A kind of preparation method of high dropping point composite titan-based grease |
| CN105062625A (en) * | 2015-08-11 | 2015-11-18 | 新乡市恒星化工有限责任公司 | Preparation method of environment-friendly compound titanium-based grease |
| CN105623801A (en) * | 2015-12-11 | 2016-06-01 | 禾泰特种新材料（苏州）有限公司 | Biodegradable grease composition and preparation method thereof |
| CN110903883A (en) * | 2019-11-15 | 2020-03-24 | 中国人民解放军陆军勤务学院 | Composite titanium-based lubricating grease and preparation method thereof |
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| CN100558866C (en) | 2009-11-11 |
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