CN104830436A - Preparation method of composite titanium-based lubricating grease with high dropping point - Google Patents
Preparation method of composite titanium-based lubricating grease with high dropping point Download PDFInfo
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- CN104830436A CN104830436A CN201510230077.2A CN201510230077A CN104830436A CN 104830436 A CN104830436 A CN 104830436A CN 201510230077 A CN201510230077 A CN 201510230077A CN 104830436 A CN104830436 A CN 104830436A
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Abstract
The invention relates to a technical field of lubricating grease preparation, and especially relates to a preparation method of composite titanium-based lubricating grease with a high dropping point. The preparation method comprises the following steps: adding fatty acid and a certain amount of base oil into a reactor, heating to a temperature of 90 to 180 DEG C to dissolve the fatty acid, introducing nitrogen gas into the reactor to expel the air completely, adding n-butyl titanate to carry out reactions for 1 to 3 hours; after the reactions, adding aromatic acid; keeping on carrying out reactions for 1 to 7 hours, then heating to a temperature of 200 to 250 DEG C to carry out high-temperature refining for 5 to 10 minutes, then adding a certain amount of base oil to cool the product, adding a certain amount of distilled water into the reactor when the temperature of the system is cooled to the room temperature, evenly stirring, then heating to a temperature of 120 DEG C, and finally grinding and homogenizing the products so as to obtain the composite titanium-based lubricating grease with a high dropping point.
Description
Technical field
The present invention relates to lubricating grease preparing technical field, refer in particular to a kind of preparation method of high dropping point composite titan-based grease.
Background technology
Lubricating grease is the important component part of industrial lubricants, and current lubricating grease industry development grows, and has formed a series of grease product wide in variety; Composite titan-based grease is a kind of product innovation, compared with conventional composite lithium soap grease, even if do not add functional agent, also shows fabulous physical and chemical performance; Composite titan-based grease is comparatively large at the turnout of India, great variety of goods, but the domestic research for composite titan-based grease is still immature.
The existing patent No. is the preparation method that CN103113969A discloses a kind of composite titan-based grease, and the composite titan-based grease prepared has good self-healing properties.
The patent No. is the preparation method that CN100558866C discloses a kind of composite titan-based grease, and the composite titan-based grease prepared has good mechanical stability and extreme pressure anti-wear.
But the grease dropping point that the method involved by above patent is prepared is on the low side, and do not relate to a large amount of alcohol how processing and produce in saponification reaction process, discharge a large amount of alcohol not in time, not only bad for the carrying out of saponification reaction, and residual alcohol also can affect the physical and chemical performance of lubricating grease in grease, do not relate to the oxidation how reducing grease in high temperature refining yet.
Summary of the invention
The present invention proposes a kind of preparation method of composite titan-based grease, the method technique is simple, raw material is easy to get, cost is low, be easy to suitability for industrialized production, the composite titan-based grease of preparation, and dropping point is high, Stencil oil-dividing amount is few, corrosion-free to copper sheet.
The present invention is achieved by following technical proposals:
(1) add in reactor by lipid acid and a certain amount of base oil, be warming up to 90-180 DEG C of heating for dissolving, logical nitrogen drains air, adds tetrabutyl titanate and reacts.
(2), after reacting 1-3 h, aromatic acid is added.
(3) be warming up to 200-250 DEG C after continuing reaction 1-7 h and carry out high temperature refining 5-10 min, again add a certain amount of base oil and cool, add a certain amount of distilled water when being cooled to room temperature and stir, then 120 DEG C are heated to, through grinding, homogenizing, obtains composite titan-based grease.
Oxidized in order to reduce grease, reaction starts until reaction terminates logical nitrogen protection, and nitrogen flow keeps 15 ml/min.
Composite titan-based grease is made up of 30-90 part base oil, 3-21 part lipid acid, 2-9 part aromatic acid, 5-40 part tetrabutyl titanate by weight.
Preparing composite titan-based grease base oil used is 150 BS, 350 SN, 500 SN, KN 4010 or silicone oil.
Lipid acid described in step (1) is stearic acid or 12-oxystearic acid.
Aromatic acid described in step (2) is phthalic acid or phenylformic acid.
Base oil in step (1) accounts for the 30-80% of base oil total mass.
The consumption of the water in step (3) is the 1-15% of lipid acid, tetrabutyl titanate, aromatic acid three total mass.
In composite titan-based grease, composite titanium soap is reticular fiber structure, and forms stable soap-oil dispersion system in base oil.
The saponification reaction of composite titan-based grease: be that equimolecular titanic acid ester and lipid acid, aromatic acid react in theory, then generate alkali formula bisgallic acid titanium soap with two molecular water reactions, be broadly divided into two stages: one is saponification complex reaction, one is saponification reaction.The principal element affecting grease dropping point is the performance of base oil and viscosifying agent; Proportioning raw materials, temperature of reaction, high temperature refining temperature, cooling method etc. are very large to the one-tenth fat influential effect of lubricating grease.
The soap-oil dispersion system that composite titan-based grease is mainly made up of base oil and viscosifying agent (lipid acid, aromatic acid, tetrabutyl titanate), simply can liken into that sponge sucks in water, it is generally acknowledged that what play lubrication is base oil, soap-oil dispersion system that viscosifying agent and base oil combine with viscosifying agent.
The invention has the advantages that:
1. the raw material that the present invention adopts is stearic acid, aromatic acid, tetrabutyl titanate, and raw material is simple, cost is low, be easy to get, and makes the easier suitability for industrialized production of composite titan-based grease.
2. the present invention adds water after adopting high temperature refining and reheats process, and one-tenth ester is effective, speed is fast.
3. the present invention's logical nitrogen in reaction process, both the propyl carbinol generated in reaction can be taken out of system, be conducive to the carrying out reacted, under can reducing high temperature again, grease is oxidized, plays a very good protection.
4. the composite titan-based grease prepared of the present invention, dropping point is high, Stencil oil-dividing amount is few, corrosion-free to copper sheet.
embodiment:
Be below preferred embodiment of the present invention, can understand the present invention better, but embodiments of the invention be not limited thereto, shown in it, data do not represent the restriction to characteristic range of the present invention simultaneously.
embodiment1
:
(1) join in still by 9.85 g stearic acid, 150 g 150 BS, be heated to 90 DEG C and make it fully dissolve, logical nitrogen drains air, is added in still by 11.15 g tetrabutyl titanates.
(2) be incubated 1 h, 4.00 g phenylformic acid are added in still.
(3) continue insulation 3 h, continue to be heated to 200 DEG C, high temperature refines 5 min, stops heating, again 75 g 150 BS are added and cool, add 1.25 g distilled water upon cooling to room temperature, be uniformly mixed, be heated to 120 DEG C, again through grinding, homogenizing, obtains composite titan-based grease.
embodiment 2:
(1) join in still by 39.39 g 12-oxystearic acids, 100 g KN 4010, be heated to 120 DEG C and make it fully dissolve, logical nitrogen drains air, is added in still by 44.61 g tetrabutyl titanates.
(2) be incubated 3 h, 16.00 g phenylformic acid are added in still;
(3) insulation 3 h is continued, continue to be heated to 220 DEG C, high temperature refines 7 min, stops heating, then is added by 50 g KN 4010 and cool, add 5.00 g distilled water upon cooling to room temperature, be uniformly mixed, be heated to 120 DEG C, then through grinding, homogenizing, obtains composite titan-based grease.
embodiment 3:
(1) join in still by 68.92 g 12-oxystearic acids, 50 g silicone oil, be heated to 90 DEG C and make it fully dissolve, logical nitrogen drains air, adds in still by 93.80 g tetrabutyl titanates;
(2) be incubated 3 h, 28.01 g phthalic acids are added in still;
(3) continue insulation 7 h, continue to be heated to 250 DEG C, high temperature refines 10 min, stops heating, again 25 g silicone oil are added and cool, add 8.75 g distilled water upon cooling to room temperature, be uniformly mixed, be heated to 120 DEG C, again through grinding, homogenizing, obtains composite titan-based grease.
embodiment 4:
(1) join in still by 39.39 g 12-oxystearic acids, 75 g 350 SN, be heated to 180 DEG C and make it fully dissolve, logical nitrogen drains air, adds in still by 44.61 g tetrabutyl titanates;
(2) be incubated 3 h, 16.00 g phenylformic acid are added in still;
(3) continue insulation 3 h, continue to be heated to 200 DEG C, high temperature refines 7 min, stops heating, again 75g 350 SN is added and cool, add 15.0 g distilled water upon cooling to room temperature, be uniformly mixed, be heated to 120 DEG C, again through grinding, homogenizing, obtains composite titan-based grease.
embodiment 5:
(1) join in still by 68.92 g stearic acid, 60 g 500 SN, be heated to 150 DEG C and make it fully dissolve, logical nitrogen drains air, adds in still by 93.80 g tetrabutyl titanates;
(2) be incubated 3 h, 28.01 g phthalic acids are added in still;
(3) continue insulation 7 h, continue to be heated to 230 DEG C, high temperature refines 5 min, stops heating, again 15 g 500 SN are added and cool, add 17.5 g distilled water upon cooling to room temperature, be uniformly mixed, be heated to 120 DEG C, again through grinding, homogenizing, obtains composite titan-based grease.
Claims (8)
1. a preparation method for high dropping point composite titan-based grease, is characterized in that concrete steps are as follows:
(1) add in reactor by lipid acid and a certain amount of base oil, be warming up to 90-180 DEG C of heating for dissolving, logical nitrogen drains air, adds tetrabutyl titanate and reacts;
(2), after reacting 1-3 h, aromatic acid is added;
(3) be warming up to 200-250 DEG C after continuing reaction 1-7 h and carry out high temperature refining 5-10 min, again add a certain amount of base oil to cool, add a certain amount of distilled water when being cooled to room temperature to stir, then 120 DEG C are heated to, through grinding, homogenizing, obtains high dropping point composite titan-based grease.
2. the preparation method of a kind of high dropping point composite titan-based grease as claimed in claim 1, is characterized in that: oxidized in order to reduce grease, and reaction starts until reaction terminates logical nitrogen protection, and nitrogen flow keeps 15 ml/min.
3. the preparation method of a kind of high dropping point composite titan-based grease as claimed in claim 1, is characterized in that: composite titan-based grease is made up of 30-90 part base oil, 3-21 part lipid acid, 2-9 part aromatic acid, 5-40 part tetrabutyl titanate by weight.
4. the preparation method of a kind of high dropping point composite titan-based grease as described in claim 1 or 3, is characterized in that: preparing composite titan-based grease base oil used is 150 BS, 350 SN, 500 SN, KN 4010 or silicone oil.
5. the preparation method of a kind of high dropping point composite titan-based grease as described in claim 1 or 3, is characterized in that: described lipid acid is stearic acid or 12-oxystearic acid.
6. the preparation method of a kind of high dropping point composite titan-based grease as described in claim 1 or 3, is characterized in that: described aromatic acid is phthalic acid or phenylformic acid.
7. the preparation method of a kind of high dropping point composite titan-based grease as claimed in claim 1, is characterized in that: the base oil in step (1) accounts for the 30-80% of the base oil total mass added.
8. the preparation method of a kind of high dropping point composite titan-based grease as claimed in claim 1, is characterized in that: the consumption of the water in step (3) is the 1-15% of lipid acid, tetrabutyl titanate, aromatic acid three total mass.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883919A (en) * | 2017-02-08 | 2017-06-23 | 江苏大学 | A kind of composite titan-based grease preparation method based on dimethyl silicone polymer |
| CN106893618A (en) * | 2017-02-08 | 2017-06-27 | 江苏大学 | A kind of composite titan-based grease preparation method based on PSI |
| 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 |
| CN116426328A (en) * | 2023-05-29 | 2023-07-14 | 泰奥星（天津）有限公司 | Lubricating grease, preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6172012B1 (en) * | 1998-03-13 | 2001-01-09 | Indian Oil Corporation Limited | Titanium complex grease composition including performance additives and process for preparation thereof |
| CN1814718A (en) * | 2005-01-31 | 2006-08-09 | 中国石油化工股份有限公司 | High-dropping-point lubricating grease and prefabricated soap making method |
| CN101117605A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Preparation method of composite titanium radical lubricating grease and product produced thereby |
| CN101899355A (en) * | 2009-05-27 | 2010-12-01 | 中国石油化工股份有限公司 | Lubricating oil composite with oxidation resistance and preparation method thereof |
-
2015
- 2015-05-08 CN CN201510230077.2A patent/CN104830436B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6172012B1 (en) * | 1998-03-13 | 2001-01-09 | Indian Oil Corporation Limited | Titanium complex grease composition including performance additives and process for preparation thereof |
| CN1814718A (en) * | 2005-01-31 | 2006-08-09 | 中国石油化工股份有限公司 | High-dropping-point lubricating grease and prefabricated soap making method |
| CN101117605A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Preparation method of composite titanium radical lubricating grease and product produced thereby |
| CN101899355A (en) * | 2009-05-27 | 2010-12-01 | 中国石油化工股份有限公司 | Lubricating oil composite with oxidation resistance and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 王基铭主编: "《石油炼制辞典》", 30 September 2013, 北京：中国石化出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883919A (en) * | 2017-02-08 | 2017-06-23 | 江苏大学 | A kind of composite titan-based grease preparation method based on dimethyl silicone polymer |
| CN106893618A (en) * | 2017-02-08 | 2017-06-27 | 江苏大学 | A kind of composite titan-based grease preparation method based on PSI |
| 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 |
| CN116426328A (en) * | 2023-05-29 | 2023-07-14 | 泰奥星（天津）有限公司 | Lubricating grease, preparation method and application thereof |
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| CN104830436B (en) | 2017-11-17 |
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Granted publication date: 20171117 Termination date: 20180508 |