CN106883919A - A kind of composite titan-based grease preparation method based on dimethyl silicone polymer - Google Patents
A kind of composite titan-based grease preparation method based on dimethyl silicone polymer Download PDFInfo
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- CN106883919A CN106883919A CN201710069175.1A CN201710069175A CN106883919A CN 106883919 A CN106883919 A CN 106883919A CN 201710069175 A CN201710069175 A CN 201710069175A CN 106883919 A CN106883919 A CN 106883919A
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- dimethyl silicone
- silicone polymer
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- mineral oil
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- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/06—Mixtures of thickeners and additives
-
- 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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
-
- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
-
- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
-
- 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
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/06—Organic compounds derived from inorganic acids or metal salts
- C10M2227/065—Organic compounds derived from inorganic acids or metal salts derived from Ti or Zr
-
- 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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
- C10M2229/0415—Siloxanes with specific structure containing aliphatic substituents used as base material
-
- 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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- 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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
-
- 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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
-
- 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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
-
- 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—Semi-solids; greasy
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The present invention relates to lubricating grease, the preparation method of specifically a kind of composite titan-based grease based on dimethyl silicone polymer.Mineral oil, dimethyl silicone polymer, 12 hydroxy stearic acids, benzoic acid are mixed and heated to 90 DEG C, insulated and stirred obtains mixture 1.Mixture 1 is warming up to 110 DEG C, titanate esters are added, by-product is blown out and condenses collection by insulated and stirred, period, to adding mineral oil, dimethyl silicone polymer to obtain mixture 2 in system again after 5h.Mixture 2 is to slowly warm up into 210 DEG C carries out high temperature refining, be warming up to keep 1 5min after required temperature after pour into rustless steel container, after naturally cooling to room temperature, add water and repeatedly stirring shearing, it is ground, be homogenized, obtain final product composite titan-based grease.The method is prepared, and composite titan-based grease dropping point is up to 330 DEG C and Stencil oil-dividing is few, and evaporation loss is small, and copper corrosion is qualified.
Description
Technical field
The present invention relates to lubricating grease, the preparation side of specifically a kind of composite titan-based grease based on dimethyl silicone polymer
Method.
Background technology
Lubricant has extremely important effect in the industrial production, and it can reduce friction so as to reduce unnecessary energy
Lose and protect Mechanical extension its service life.Composite titan-based grease has high-fire resistance and good shearing self-repairability,
There is good application prospect in fields such as industry, aviation, vehicles.Conventional composite titan-based grease is by single mineral oil system
Into its feature is for cost is relatively low, greasy property is good, but its heat-resisting, inoxidizability is general.And it is multiple to use 100% artificial oil to prepare
Close the heat resistance of titan-based grease preferably, but its cost is also substantially increased.
Existing Patent No. CN101307269A discloses a kind of preparation method of composite titan-based grease, and for preparing answers
Closing titan-based grease has the characteristic of low noise.But the performance of composite titan-based grease prepared by non-doping is not directed to, and
Grease dropping point prepared by the method is relatively low.
Patent No. CN100558866C discloses a kind of preparation method of composite titan-based grease, the composite titanium prepared
Base grease has good mechanical stability and extreme pressure anti-wear.But its dropping point is relatively low.
The content of the invention
The present invention proposes a kind of preparation method of the composite titan-based grease based on dimethyl silicone polymer, the method work
Skill is simple, raw material is easy to get, low cost, have good industrial prospect, and the composite titan-based grease dropping point prepared is up to 330 DEG C
And Stencil oil-dividing is few, evaporation loss is small, and copper corrosion is qualified.
The present invention is achieved by following technical proposals：
(1) mineral oil, dimethyl silicone polymer, 12- hydroxy stearic acids, benzoic acid are mixed and heated to 90 DEG C, insulation is stirred
Mix and obtain mixture 1.
(2) mixture 1 is warming up to 110 DEG C, adds titanate esters, by-product is blown out and condenses collection by insulated and stirred, period,
To adding mineral oil, dimethyl silicone polymer to obtain mixture 2 in system again after 5h.
(3) mixture 2 is to slowly warm up into 210 DEG C carries out high temperature refining, and 1-5min is kept after required temperature is warming up to
After pour into rustless steel container, after naturally cooling to room temperature, add water and repeatedly stirring shearing, it is ground, be homogenized, obtain final product compound
Titan-based grease.
In step (1) and (2), mineral oil is the one kind in KN4010,500SN, 150BS.
In step (1) and (2), the viscosity of dimethyl silicone polymer is 100-500mm2/s。
In step (1), the mass ratio of each material is, mineral oil：Dimethyl silicone polymer：12- hydroxy stearic acids：Benzene
Formic acid=75-110：5-50：75.72：30.77.
In step (1), the time of insulated and stirred is 30min.
In step (2), by-product is blown out and condenses collection and refers to by period：Period, logical nitrogen blew out the alcohols material of by-product
And condense collection.
Step (2) mineral oil in fluid, the addition of dimethyl silicone polymer are identical with step (1).
Titanate esters in step (2) are isopropyl titanate or tetrabutyl titanate, amount and the benzoic acid matter of the material of titanate esters
The ratio between amount is 0.25mol：30.77g.
The heating rate that 110 DEG C are warming up to described in step (2) is 2-10 DEG C/min.
Slow intensification in step (3) refers to that heating rate is 0.2-0.7 DEG C/min.
It is 5-10mL that water in step (3) adds the ratio between volume and benzoic acid Mass：30.77g.
The advantage of the invention is that：
1. the raw material that uses of the present invention be 12- hydroxy stearic acids, benzoic acid, lithium hydroxide, raw material simply, it is low cost, easy
So that complex lithium grease is easier industrialized production.
2. the present invention is using mineral oil and dimethyl silicone polymer both base oils of different nature, the lubricating grease of generation
It is provided simultaneously with the advantage of mineral oil and synthetic oil grease.
3. the present invention leads to nitrogen during the course of the reaction, both accessory substance isopropanol, n-butanol can be taken out of reaction system, and
Grease is oxidized under high temperature can be reduced, and plays a very good protection.
4. the present invention is added after the cooling period in preparation process reclaimed water, and preventing from adding at high temperature causes to emit kettle.
5. lubricating grease based on lubricating grease of the present invention, does not add any additive, adds the appropriate additive can be with
Obtain better performance.
6. the composite titan-based grease that prepared by the present invention, dropping point is high, and Stencil oil-dividing is few, and evaporation loss is small, and copper corrosion is closed
Lattice.
7. the composite titan-based grease coefficient of friction that prepared by the present invention is smaller, and abrasion condition is also smaller.
Specific embodiment
It is below presently preferred embodiments of the present invention, better understood when the present invention, but embodiments of the invention are not limited to
This, while its shown data does not represent the limitation to feature of present invention scope.
Embodiment 1：
100g mineral oil, 25g dimethyl silicone polymers, 75.72g12- hydroxy stearic acids, 30.77g benzoic acid are mixed and is added
Heat is to 90 DEG C, insulated and stirred 30min；110 DEG C are warming up to, 0.25mol isopropyl titanates are added, insulated and stirred, period leads to nitrogen
The alcohols material of by-product is blown out and collection is condensed, to addition 100g mineral oil, 25g dimethyl silicone polymers in system after 5h,
To be to slowly warm up to 210 DEG C carry out high temperature refining, be warming up to keep 3min after required temperature after pour into rustless steel container, it is natural
After being cooled to room temperature, 5mL water and repeatedly stirring shearing are added, ground, homogenizing obtains final product composite titan-based grease.
Embodiment 2：
110g mineral oil, 15g dimethyl silicone polymers, 75.72g12- hydroxy stearic acids, 30.77g benzoic acid are mixed and is added
Heat is to 90 DEG C, insulated and stirred 30min；110 DEG C are warming up to, 0.25mol isopropyl titanates are added, insulated and stirred, period leads to nitrogen
The alcohols material of by-product is blown out and collection is condensed, to addition 110g mineral oil, 15g dimethyl silicone polymers in system after 5h,
To be to slowly warm up to 210 DEG C carry out high temperature refining, be warming up to keep 3min after required temperature after pour into rustless steel container, it is natural
After being cooled to room temperature, 5mL water and repeatedly stirring shearing are added, ground, homogenizing obtains final product composite titan-based grease.
Embodiment 3：
90g mineral oil, 35g dimethyl silicone polymers, 75.72g12- hydroxy stearic acids, 30.77g benzoic acid are mixed and is added
Heat is to 90 DEG C, insulated and stirred 30min；110 DEG C are warming up to, 0.25mol isopropyl titanates are added, insulated and stirred, period leads to nitrogen
The alcohols material of by-product is blown out and collection is condensed, to 90g mineral oil, 35g dimethyl silicone polymers is added in system after 5h, delayed
It is slow be warming up to 210 DEG C and carry out high temperature refining, be warming up to keep 3min after required temperature after pour into rustless steel container, it is naturally cold
But it is ground to 5mL water and repeatedly stirring shearing after room temperature, is added, it is homogenized, obtain final product composite titan-based grease.
Comparative example：
Comparative example is conventional type composite titan-based grease, and dimethyl silicone polymer is not added in preparation process, is surveyed
Test result shows that its dropping point is low compared with above-described embodiment, and Stencil oil-dividing and evaporativity are higher.
110g mineral oil, 75.72g12- hydroxy stearic acids, 30.77g benzoic acid are mixed and heated to 90 DEG C, insulated and stirred
30min；110 DEG C are warming up to, 0.25mol isopropyl titanates, insulated and stirred is added, period leads to nitrogen and blows the alcohols material of by-product
Go out and condense collection, to 110g mineral oil is added in system after 5h, being to slowly warm up to 210 DEG C carries out high temperature refining, is being warming up to
Poured into rustless steel container after keeping 3min after required temperature, after naturally cooling to room temperature, add 5mL water and stir repeatedly and cut
Cut, ground, homogenizing obtains final product composite titan-based grease.
Test result：
Claims (7)
1. a kind of composite titan-based grease preparation method based on dimethyl silicone polymer, it is characterised in that comprise the following steps that：
(1) mineral oil, dimethyl silicone polymer, 12- hydroxy stearic acids, benzoic acid are mixed and heated to 90 DEG C, insulated and stirred is obtained
To mixture 1；
(2) mixture 1 is warming up to 110 DEG C, adds titanate esters, by-product is blown out and condenses collection by insulated and stirred, period, after 5h
Mixture 2 is obtained to mineral oil, dimethyl silicone polymer is added in system again；
(3) mixture 2 is to slowly warm up into 210 DEG C carries out high temperature refining, is being warming up to after required temperature to be fallen after holding 1-5min
Enter in rustless steel container, after naturally cooling to room temperature, add water and repeatedly stirring shearing, ground, homogenizing is obtained final product composite titan-based
Lubricating grease.
2. a kind of composite titan-based grease preparation method based on dimethyl silicone polymer as claimed in claim 1, its feature
It is that in step (1) and (2), mineral oil is the one kind in KN4010,500SN, 150BS.
3. a kind of composite titan-based grease preparation method based on dimethyl silicone polymer as claimed in claim 1, its feature
It is that in step (1) and (2), the viscosity of dimethyl silicone polymer is 100-500mm2/s。
4. a kind of composite titan-based grease preparation method based on dimethyl silicone polymer as claimed in claim 1, its feature
It is that in step (1), the mass ratio of each material is, mineral oil：Dimethyl silicone polymer：12- hydroxy stearic acids：Benzene first
Acid=75-110：5-50：75.72：30.77；In step (1), the time of insulated and stirred is 30min.
5. a kind of composite titan-based grease preparation method based on dimethyl silicone polymer as claimed in claim 1, its feature
It is that in step (2), by-product is blown out and condense collection and refers to by period：Period, logical nitrogen blew out simultaneously the alcohols material of by-product
Condensation is collected；Step (2) mineral oil in fluid, the addition of dimethyl silicone polymer are identical with step (1).
6. a kind of composite titan-based grease preparation method based on dimethyl silicone polymer as claimed in claim 1, its feature
Be that the titanate esters in step (2) are isopropyl titanate or tetrabutyl titanate, the amount and benzoic acid Mass of the material of titanate esters it
Than being 0.25mol：30.77g；The heating rate that 110 DEG C are warming up to described in step (2) is 2-10 DEG C/min.
7. a kind of composite titan-based grease preparation method based on dimethyl silicone polymer as claimed in claim 1, its feature
It is that the slow intensification in step (3) refers to that heating rate is 0.2-0.7 DEG C/min；Water in step (3) adds volume and benzene
Formic acid mass ratio is 5-10mL：30.77g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710069175.1A CN106883919A (en) | 2017-02-08 | 2017-02-08 | A kind of composite titan-based grease preparation method based on dimethyl silicone polymer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710069175.1A CN106883919A (en) | 2017-02-08 | 2017-02-08 | A kind of composite titan-based grease preparation method based on dimethyl silicone polymer |
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| CN106883919A true CN106883919A (en) | 2017-06-23 |
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| CN201710069175.1A Pending CN106883919A (en) | 2017-02-08 | 2017-02-08 | A kind of composite titan-based grease preparation method based on dimethyl silicone polymer |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2017
- 2017-02-08 CN CN201710069175.1A patent/CN106883919A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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