CN106893618A - A kind of composite titan-based grease preparation method based on PSI - Google Patents
A kind of composite titan-based grease preparation method based on PSI Download PDFInfo
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- CN106893618A CN106893618A CN201710069128.7A CN201710069128A CN106893618A CN 106893618 A CN106893618 A CN 106893618A CN 201710069128 A CN201710069128 A CN 201710069128A CN 106893618 A CN106893618 A CN 106893618A
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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
- C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
- C10M107/50—Lubricating compositions characterised by the base-material being a macromolecular compound containing silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- 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
- C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
- C10M111/04—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a macromolecular organic compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
-
- 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
- C10M2207/14—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
- C10M2229/042—Siloxanes with specific structure containing aromatic substituents
-
- 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
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (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 PSI.Mineral oil, PSI, 12 hydroxy stearic acids, benzoic acid are mixed and heated to 95 DEG C, insulated and stirred obtains mixture 1.Mixture 1 is warming up to 120 DEG C, titanate esters are added, by-product is blown out and condenses collection by insulated and stirred, period, to adding mineral oil, PSI to obtain mixture 2 in system again after 5h.Mixture 2 is to slowly warm up into 220 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 336 DEG C and Stencil oil-dividing is few, and evaporation loss is small, and copper corrosion is qualified, with relatively low coefficient of friction.
Description
Technical field
The present invention relates to lubricating grease, the preparation of specifically a kind of composite titan-based grease based on PSI
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 is a kind of new lubricating grease, with many excellent
Performance, the conventional greases, effect is significant such as complex lithium grease can be replaced in many occasions.Compared with conventional grease,
Do not add additivated composite titan-based grease and show excellent physicochemical property yet, therefore extensively closed by domestic and international scientific research person
Note.
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 is not directed to the composite titan-based grease performance without additive, and the method
The grease dropping point of preparation 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 336 DEG C
And Stencil oil-dividing is few, evaporation loss is small, and copper corrosion is qualified, with relatively low coefficient of friction.
The present invention is achieved by following technical proposals：
(1) dimethylbenzene, acetone, dimethyldichlorosilane, diphenyl dichlorosilane and dichloromethyl phenylsilane are mixed
Uniformly, its temperature is maintained at 30 DEG C, the mixed liquor of water and acetone is added dropwise in mixed solution, react 12h.
(2) after reaction terminates, neutrality is washed to product using distilled water, is subsequently adding HMDO and tetramethyl
Base Ammonia, 10h is reacted at 100 DEG C, and reaction reuses distillation washing product 3-5 times after terminating.
(3) product after washing is fitted into and 135 DEG C, removed under reduced pressure solvent, until no liquid evaporates is heated in distilling apparatus
Go out, now residual solution is PSI.
(4) mineral oil, PSI, 12- hydroxy stearic acids, benzoic acid are mixed and heated to 95 DEG C, insulation
Stirring obtains mixture 1.
(5) mixture 1 is warming up to 120 DEG C, adds titanate esters, by-product is blown out and condenses collection by insulated and stirred, period,
To adding mineral oil, PSI to obtain mixture 2 in system again after 5h.
(6) mixture 2 is to slowly warm up into 220 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), dimethylbenzene, acetone, dimethyldichlorosilane, diphenyl dichlorosilane and dichloromethyl phenylsilane
The ratio between volume and the amount of material be：80mL：50mL：0.12-0.19mol：0.01-0.08mol：0.10mol.
In step (1), in water and acetone mixed solution, the volume ratio of water and acetone is 57.6：100, acetone and dimethylbenzene
Volume ratio be 5：4.
In step (2), tetramethyl ammonium hydroxide solution concentration is 25wt%, is 0.05- with the mass volume ratio of dimethylbenzene
0.1g：80mL.
In step (2), HMDO is 0.0375 with the mol ratio of dichloromethyl phenylsilane：1.
In step (3), the pressure in distilling apparatus is 1kPa.
In step (4) and (5), mineral oil is the one kind in KN4010,500SN, 150BS.
In step (4) and (5), the PSI being related to is the product of step (1)-(3).
In step (4), the time of insulated and stirred is 20min.
In step (5), period by-product blows out and condenses collection and refers to：Period, logical nitrogen blew out and cold the alcohols material of by-product
It is solidifying to collect.
The mass ratio of step (4) each material is, mineral oil：PSI：12- hydroxy stearic acids：Benzene
Formic acid=75-120：5-50：75.72：30.77.
Step (5) mineral oil in fluid, the addition of PSI are identical with step (4).
Titanate esters in step (5) 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 120 DEG C are warming up to described in step (5) is 2-10 DEG C/min.
Slow intensification in step (6) is heating rate in 0.2-0.7 DEG C/min.
It is 4-8mL that water in step (6) adds the ratio between volume and benzoic acid Mass：30.77g.
The advantage of the invention is that：
1. the raw material that the present invention is used is 12- hydroxy stearic acids, benzoic acid, titanate esters, mineral oil, polymethyl-benzene base silica
Alkane, raw material is simple, low cost, be easy to get.
2. the present invention synthesizes PSI using solution, organic ammonium catalysis method against the current, with sulphuric acid catalysis method phase
Than safer.
3. the present invention uses mediation type base oil, is provided simultaneously with the advantage of mineral oil and synthetic oil grease.
4. the present invention leads to nitrogen during the course of the reaction, both accessory substance alcohols material can be taken out of reaction system, again can be with
Grease is oxidized under reducing high temperature, plays a very good protection.
5. lubricating grease based on the lubricating grease that prepared by 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, and antifriction quality, wear resistence are good.
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：
By 80mL dimethylbenzene, 50mL acetone, 0.157mol dimethyldichlorosilanes, 0.043mol diphenyl dichlorosilanes and
0.1mol dichloromethyl phenylsilanes are well mixed, and are incubated 30 DEG C, and the mixed liquor of 57.6ml water and 100ml acetone is added dropwise over
To in mixed solution, 12h is reacted at 30 DEG C；After reaction terminates, neutrality is washed to product using distilled water, is subsequently adding pregnancy
Base disiloxane 0.00375mol and tetramethyl ammonium hydroxide solution 0.077g, 10h is reacted at 100 DEG C, is reacted after terminating again
Product is washed using distillation 3-5 times；Product after washing is fitted into and is heated to 135 DEG C in distilling apparatus, removed under reduced pressure solvent, directly
Distillated to no liquid, now residual solution is PSI.
By 118.75gKN4010,6.25g PSI, 75.72g 12- hydroxy stearic acids, 30.77g benzene first
Acid is mixed and heated to 95 DEG C, insulated and stirred 20min；120 DEG C are warming up to, 0.25mol isopropyl titanates, insulated and stirred, phase is added
Between lead to nitrogen the alcohols material of by-product blown out and collections is condensed, to adding 118.75gKN4010,6.25g poly- in system after 5h
Methyl phenyl siloxane；Being to slowly warm up to 220 DEG C carries out high temperature refining, is poured into not after holding 3min being warming up to after required temperature
In rust steel container, after naturally cooling to room temperature, 4ml water and repeatedly stirring shearing are added, ground, homogenizing is obtained final product composite titan-based
Lubricating grease.
Embodiment 2：
PSI is prepared with embodiment 1.
By 112.5gKN4010,12.5g PSI, 75.72g 12- hydroxy stearic acids, 30.77g benzene first
Acid is mixed and heated to 95 DEG C, insulated and stirred 20min；120 DEG C are warming up to, 0.25mol tetrabutyl titanates, insulated and stirred, phase is added
Between lead to nitrogen the alcohols material of by-product is blown out and collections is condensed, after 5h in system addition the poly- first of 112.5gKN4010,12.5g
Base phenyl siloxane；Being to slowly warm up to 220 DEG C carries out high temperature refining, be warming up to after required temperature keep 3min after pour into it is stainless
In steel container, after naturally cooling to room temperature, 4ml water and repeatedly stirring shearing are added, ground, homogenizing obtains final product composite titan-based profit
Consistent lubricant.
Embodiment 3：
PSI is prepared with embodiment 1.
100gKN4010,25g PSI, 75.72g 12- hydroxy stearic acids, 30.77g benzoic acid are mixed
Conjunction is heated to 95 DEG C, insulated and stirred 20min；120 DEG C are warming up to, 0.25mol isopropyl titanates are added, insulated and stirred, period leads to
The alcohols material of by-product is blown out and condenses collection by nitrogen, to addition 100gKN4010,25g polymethyl-benzene base silicon in system after 5h
Oxygen alkane；Being to slowly warm up to 220 DEG C carries out high temperature refining, and rustless steel container is poured into after holding 3min being warming up to after required temperature
In, after naturally cooling to room temperature, 4ml water and repeatedly stirring shearing being added, ground, homogenizing obtains final product composite titan-based grease.
Embodiment 4：
PSI is prepared with embodiment 1.
By 93.75gKN4010,31.25g PSI, 75.72g 12- hydroxy stearic acids, 30.77g benzene first
Acid is mixed and heated to 95 DEG C, insulated and stirred 20min；120 DEG C are warming up to, 0.25mol tetrabutyl titanates, insulated and stirred, phase is added
Between lead to nitrogen the alcohols material of by-product blown out and collections is condensed, to adding 93.75gKN4010,31.25g poly- in system after 5h
Methyl phenyl siloxane；Being to slowly warm up to 220 DEG C carries out high temperature refining, is poured into not after holding 3min being warming up to after required temperature
In rust steel container, after naturally cooling to room temperature, 4ml water and repeatedly stirring shearing are added, ground, homogenizing is obtained final product composite titan-based
Lubricating grease.
Embodiment 5：
By 80mL dimethylbenzene, 50mL acetone, 0.143mol dimethyldichlorosilanes, 0.057mol diphenyl dichlorosilanes and
0.1mol dichloromethyl phenylsilanes are well mixed, and are incubated 30 DEG C, and the mixed liquor of 57.6ml water and 100ml acetone is added dropwise over
To in mixed solution, 12h is reacted at 30 DEG C；After reaction terminates, neutrality is washed to product using distilled water, is subsequently adding pregnancy
Base disiloxane 0.00375mol and tetramethyl ammonium hydroxide solution 0.073g, 10h is reacted at 100 DEG C, is reacted after terminating again
Product is washed using distillation 3-5 times；Product after washing is fitted into and is heated to 135 DEG C in distilling apparatus, removed under reduced pressure solvent, directly
Distillated to no liquid, now residual solution is PSI.
By 118.75gKN4010,6.25g PSI, 75.72g 12- hydroxy stearic acids, 30.77g benzene first
Acid is mixed and heated to 95 DEG C, insulated and stirred 20min；120 DEG C are warming up to, 0.25mol isopropyl titanates, insulated and stirred, phase is added
Between lead to nitrogen the alcohols material of by-product blown out and collections is condensed, to adding 118.75gKN4010,6.25g poly- in system after 5h
Methyl phenyl siloxane；Being to slowly warm up to 220 DEG C carries out high temperature refining, is poured into not after holding 3min being warming up to after required temperature
In rust steel container, after naturally cooling to room temperature, 4ml water and repeatedly stirring shearing are added, ground, homogenizing is obtained final product composite titan-based
Lubricating grease.
Comparative example：
Comparative example is conventional type complex lithium grease, and PSI is not used in preparation process,
Test result shows that its dropping point is low compared with above-described embodiment, and Stencil oil-dividing and evaporativity are higher, and coefficient of friction is also big.
120gKN4010,75.72g 12- hydroxy stearic acids, 30.77g benzoic acid are mixed and heated to 95 DEG C, insulated and stirred
20min；120 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 adding 120gKN4010 in system after 5h；Being to slowly warm up to 220 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 4ml water and stir repeatedly and cut
Cut, ground, homogenizing obtains final product composite titan-based grease.
Composite titan-based grease performance test table：
PSI performance test table：
Claims (10)
1. a kind of composite titan-based grease preparation method based on PSI, it is characterised in that specific steps are such as
Under：
(1) mineral oil, PSI, 12- hydroxy stearic acids, benzoic acid are mixed and heated to 95 DEG C, insulated and stirred
Obtain mixture 1；
(2) mixture 1 is warming up to 120 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, PSI is added in system again；
(3) mixture 2 is to slowly warm up into 220 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 PSI as claimed in claim 1, it is special
Levy and be, 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 PSI as claimed in claim 1, it is special
Levy and be, in step (1), the time of insulated and stirred is 20min；In step (2), period by-product blows out and condenses collection and refers to：Phase
Between lead to nitrogen the alcohols material of by-product is blown out and collection is condensed.
4. a kind of composite titan-based grease preparation method based on PSI as claimed in claim 1, it is special
Levy and be, in step (1), the mass ratio of each material is, mineral oil：PSI：12- hydroxy stearic acids：
Benzoic acid=75-120：5-50：75.72：30.77；In step (2), mineral oil, the addition of PSI with step
Suddenly (1) is identical.
5. a kind of composite titan-based grease preparation method based on PSI as claimed in claim 1, it is special
Levy and be, the titanate esters in step (2) are isopropyl titanate or tetrabutyl titanate, the amount and benzoic acid Mass of the material of titanate esters
The ratio between be 0.25mol：30.77g；The heating rate that 120 DEG C are warming up to described in step (2) is 2-10 DEG C/min.
6. a kind of composite titan-based grease preparation method based on PSI as claimed in claim 1, it is special
Levy and be, the slow intensification in step (3) is heating rate in 0.2-0.7 DEG C/min；Water in step (3) adds volume and benzene
Formic acid mass ratio is 4-8mL：30.77g.
7. a kind of composite titan-based grease preparation method based on PSI as claimed in claim 1, it is special
Levy and be, the preparation method of the PSI is as follows：
(1) dimethylbenzene, acetone, dimethyldichlorosilane, diphenyl dichlorosilane and dichloromethyl phenylsilane are well mixed,
Its temperature is maintained at 30 DEG C, the mixed liquor of water and acetone is added dropwise in mixed solution, react 12h；
(2) after reaction terminates, neutrality is washed to product using distilled water, is subsequently adding HMDO and tetramethyl hydrogen
Ammonium hydroxide solution, 10h is reacted at 100 DEG C, and reaction reuses distillation washing product 3-5 times after terminating；
(3) product after washing is fitted into and is heated to 135 DEG C in distilling apparatus, removed under reduced pressure solvent, until no liquid is distillated, this
When residual solution be PSI.
8. a kind of composite titan-based grease preparation method based on PSI as claimed in claim 7, it is special
Levy and be, in step (1), dimethylbenzene, acetone, dimethyldichlorosilane, diphenyl dichlorosilane and dichloromethyl phenylsilane
The ratio between volume and the amount of material be：80mL：50mL：0.12-0.19mol：0.01-0.08mol：0.10mol；In step (1),
In water and acetone mixed solution, the volume ratio of water and acetone is 57.6：100, acetone is 5 with the volume ratio of dimethylbenzene：4.
9. a kind of composite titan-based grease preparation method based on PSI as claimed in claim 7, it is special
Levy and be, in step (2), tetramethyl ammonium hydroxide solution concentration is 25wt%, is 0.05- with the mass volume ratio of dimethylbenzene
0.1g：80mL；In step (2), HMDO is 0.0375 with the mol ratio of dichloromethyl phenylsilane：1.
10. a kind of composite titan-based grease preparation method based on PSI as claimed in claim 7, it is special
Levy and be, in step (3), the pressure in distilling apparatus is 1kPa.
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| CN201710069128.7A CN106893618A (en) | 2017-02-08 | 2017-02-08 | A kind of composite titan-based grease preparation method based on PSI |
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| CN201710069128.7A CN106893618A (en) | 2017-02-08 | 2017-02-08 | A kind of composite titan-based grease preparation method based on PSI |
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| CN (1) | CN106893618A (en) |
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| CN110358089A (en) * | 2018-04-11 | 2019-10-22 | 苏州润特新材料科技有限公司 | A kind of preparation method of alkylaryl modified silicon oil |
| CN115197765A (en) * | 2022-06-22 | 2022-10-18 | 中国民用航空飞行学院 | Zirconium phosphate composite titanium-based lubricating grease and preparation method thereof |
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| CN104830436A (en) * | 2015-05-08 | 2015-08-12 | 江苏大学 | Preparation method of composite titanium-based lubricating grease with high dropping point |
| CN103304818B (en) * | 2013-06-26 | 2015-09-02 | 江苏大学 | A kind of preparation method of methyl phenyl silicone oil |
| CN105585957A (en) * | 2014-10-22 | 2016-05-18 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish, and preparing method and applications thereof |
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| CN103304818B (en) * | 2013-06-26 | 2015-09-02 | 江苏大学 | A kind of preparation method of methyl phenyl silicone oil |
| CN105585957A (en) * | 2014-10-22 | 2016-05-18 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish, and preparing method and applications 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358089A (en) * | 2018-04-11 | 2019-10-22 | 苏州润特新材料科技有限公司 | A kind of preparation method of alkylaryl modified silicon oil |
| CN115197765A (en) * | 2022-06-22 | 2022-10-18 | 中国民用航空飞行学院 | Zirconium phosphate composite titanium-based lubricating grease and preparation method thereof |
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Application publication date: 20170627 |