CN108102386A - A kind of low stain silicone grease and preparation method thereof - Google Patents
A kind of low stain silicone grease and preparation method thereof Download PDFInfo
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- CN108102386A CN108102386A CN201810048550.9A CN201810048550A CN108102386A CN 108102386 A CN108102386 A CN 108102386A CN 201810048550 A CN201810048550 A CN 201810048550A CN 108102386 A CN108102386 A CN 108102386A
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- silicone oil
- filler
- low stain
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- silicone grease
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The present invention discloses a kind of low stain silicone grease and preparation method thereof, belongs to technical field of polymer materials.It is formed comprising following parts by weight：6~500 parts micro- 100 parts of silicone oil of crosslinking, processing of filler.Compared with the prior art, the phenomenon that sizing synthesized by the present invention is a kind of micro- crosslinking silicone oil of molecule under bound state, changes prior art free state molecule and is not easy to be bound, easy condensate oil, so that product is more stablized, oily pollution is efficiently solved the problems, such as.
Description
Technical field
The present invention relates to a kind of low stain silicone grease and preparation method thereof, belong to technical field of polymer materials.
Background technology
Silicone grease (or silicon cream) is oily based on silicone oil, adds in thickener, stabilizer and property-modifying additive and is ground through mixing
Grind the product being process.It has good waterproof seal, solvent resistance and creep resistance energy, does not corrode metal, with rubber
Glue has well adapting to property more, for bathing device, sealing ring, the waterproof sealing of electric industry and lubrication.From function
On can be divided into insulation silicone grease, lubrication silicone grease and heat-conducting silicone grease.
In recent years, silicone grease is widely used in the fields such as nuclear power engineering, thermal power project and hydroelectric project.Traditional silicone grease system
Standby base oil used is mostly using certain molecular weight silicone oil, and with the increase of molecular weight, the cone penetration of silicone grease reduces, under coating
Drop, although oily have a degree of decline from degree, since this silicone molecule for having certain degree of polymerization is in free state, silicon
The condensate oil of fat is not reduced effectively, so that the component and electronic component that are coated around silicone grease all can be because of condensate oils
And pollute, also resulting in colloid is dried, is hardened, so as to shorten the service life of silicone grease.
At present, on silicone grease to the pollution problem of contact interface there is not yet report.
The content of the invention
It is an object of the invention to overcome the shortcomings of in the prior art, a kind of low stain silicone grease is provided, which is controlling
While product oil is from spending, moreover it is possible to the precipitation of silicone oil is effectively reduced, so as to control oily pollution, improves the appearance of seal member,
Extend the service life of silicone grease and electronic component.
In order to realize foregoing invention purpose, technical scheme is as follows：A kind of low stain silicone grease, matches somebody with somebody by weight
Than being made of 100 parts of micro- crosslinking silicone oil and 6~500 parts of processing fillers；Micro- crosslinking silicone oil is by containing hydrogen silicone oil, vinyl
Silicone oil and catalyst are made；The processing filler is made of filler and inorganic agent.
Above-mentioned low stain silicone grease, micro- crosslinking silicone oil, by mass percentage composition be：Containing hydrogen silicone oil 0.2~
5%, vinyl silicone oil 94~99.5%, catalyst 0.05~1.0%.
Containing hydrogen silicone oil can be the full containing hydrogen silicone oil of methyl, the full containing hydrogen silicone oil of ethyl, part containing hydrogen silicone oil, double end hydrogen silicone oils and
At least one of single end hydrogen silicone oil.Vinyl silicone oil can be single-ended vinyl silicone oil, both-end vinyl silicone oil and side group ethylene
At least one of base silicone oil.
The upper low stain silicone grease, the catalyst are chloroplatinic acid.
Above-mentioned low stain silicone grease, the processing filler, by mass percentage composition be：Filler 89~98%, processing
Agent 2~11%.
Above-mentioned low stain silicone grease, the filler for fume colloidal silica, precipitated silica, aluminium oxide, zinc oxide,
At least one of boron nitride and aluminium nitride.
Above-mentioned low stain silicone grease, the inorganic agent are one kind in hexamethyldisilazane, KH-550 and KH-560.
Inorganic agent can not only eliminate the interaction force of the chemical bond on filler surface, can also improve compatible between filler and silicone oil
Property improves the stability of product.
A kind of preparation method of low stain silicone grease, comprises the following steps：
1) containing hydrogen silicone oil, vinyl silicone oil are added in reaction kettle, stirred evenly；Catalyst is added in, stirring is opened, 60
1~3h is reacted at~200 DEG C, treats temperature less than 50 DEG C, blowing obtains micro- crosslinking silicone oil；
2) filler being added in reaction kettle, stirring adds in inorganic agent at 40~70 DEG C, stirs 2h, then it is warming up to 100~
200 DEG C, start vacuum system, filler must be handled when reaction 2 is small under -0.065~-0.85MPa；
3) by 100 parts of micro- crosslinking silicone oil and 6~500 parts of processing fillers, micro- crosslinking silicone oil and processing filler are added in into stirring
In device, under the rotating speed of 30~3000rpm, temperature is controlled to be mixed under 40~95 DEG C, the vacuum degree of -0.08~-0.095MPa,
Scattered 0.5~3h, filtering obtain low stain silicone grease.
The present invention has the following advantages compared with prior art：
1st, the sizing synthesized by the present invention is a kind of micro- crosslinking silicone oil of molecule under bound state, is changed existing
The phenomenon that technology free state molecule is not easy to be bound, easy condensate oil so that product is more stablized, efficiently solves oily pollution
Problem.
2nd, when the present invention is dispersed with stirring in blender, the vacuum degree is -0.080~-0.095MPa.Decompression is pulled out low
Purpose be remaining low molecule in removal system.Silicone grease can gradually rise temperature under high speed mixing, in high temperature, vacuum degree
Under, it is more advantageous to low molecular abjection.
3rd, the present invention is in micro- crosslinking silicone oil is synthesized, including following mass percentage composition：Containing hydrogen silicone oil 0.2~5%, second
Alkenyl silicone oil 94~99.5%, catalyst 0.05~1.0%.The mass percent of containing hydrogen silicone oil increases or vinyl silicone oil
Mass percent reduce, can crosslink density be caused to increase, declined with the comixing compatibility of filler.On the contrary, containing hydrogen silicone oil
Mass percent is reduced or the mass percent of vinyl silicone oil increases, and can cause crosslink density inadequate, so as to rise
The effect moved to bound molecule.Catalyst quality percentage increases, and can accelerate the progress of cross-linking reaction, prevent crosslinking points from equal
Even distribution, the molecule content under free state increases, so as to solve the problems, such as oily pollution.On the contrary, the quality percentage of catalyst
Than reducing, and it is unable to catalytic reaction.
4th, for the present invention in synthesis handles filler, the vacuum degree is -0.065~-0.85MPa.Low mesh is pulled out in decompression
Be the low molecules such as the moisture in the excessive inorganic agent of removal, filler.Vacuum degree is too low, it is impossible to effectively remove low molecule；Very
Reciprocal of duty cycle is excessively high, and dry filler will be carried over.
Specific embodiment
Embodiment 1
(1) micro- crosslinking silicone oil is prepared
1) 0.2 part of containing hydrogen silicone oil, 99.3 parts of vinyl silicone oil, 0.5 part of chloroplatinic acid are weighed according to parts by weight；
2) containing hydrogen silicone oil, vinyl silicone oil are added in reaction kettle, stirred evenly, then chloroplatinic acid is added in into reaction kettle
In, it is uniformly mixed, opens heating, 2.5h is reacted at 150 DEG C, cool down, when temperature is less than 50 DEG C, blowing obtains micro- crosslinking silicon
Oil, sealing are for use.
(2) processing filler is prepared
1) 89 parts of fume colloidal silica, 11 parts of hexamethyldisilazane are weighed according to parts by weight；
2) fume colloidal silica is added in reaction kettle, heating, stirring add in hexamethyldisilazane at 45 DEG C, stir
2h is mixed, then heats up and starts vacuum system, temperature control is 180 DEG C, and vacuum degree is that must handle to fill out when reaction 1.5 is small under -0.08MPa
Material, sealing are for use.
(3) low stain silicone grease is prepared
By weight, 6 parts micro- 100 parts of silicone oil of crosslinking, processing of filler are taken, is added in blender, speed of agitator is
3000rpm, reaction temperature are 70 DEG C, and vacuum degree is that scattered 0.5h is mixed under -0.08MPa, and filtering, discharge to obtain low stain silicone grease.
(4) performance test of low stain silicone grease
1st, pollution is tested
Sample preparation：In clean stainless steel surface coating silicone grease disk (disk diameter 30mm, thickness 1mm).
Experimental condition：By sample preparation into silicone grease disk be put into 80 DEG C of baking oven, constant temperature for 24 hours, re-test silicone oil be precipitated after
The difference of the radius R of circle and silicone grease wafer radius that is formed of oily pollution border, i.e.,：(R-15)mm.
2nd, according to GB/T269-1991, its cone penetration is measured.
3rd, according to HG/T2509-93, its volatile matter and oily from degree is measured.
As a result such as table 1.
Embodiment 2
(1) micro- crosslinking silicone oil is prepared
1) 5 parts of containing hydrogen silicone oil, 94.7 parts of vinyl silicone oil, 0.3 part of chloroplatinic acid are weighed according to parts by weight；
2) containing hydrogen silicone oil, vinyl silicone oil are added in reaction kettle, stirred evenly, then chloroplatinic acid is added in into reaction kettle
In, it is uniformly mixed, opens heating, 2h is reacted at 130 DEG C, cool down, when temperature is less than 50 DEG C, blowing obtains micro- crosslinking silicone oil,
Sealing is for use.
(2) processing filler is prepared
1) 98 parts of zinc oxide, 2 parts of KH-560 are weighed according to parts by weight；
2) zinc oxide is added in reaction kettle, heating, stirring add in KH-560 at 70 DEG C, stir 2h, then the startup that heats up
Vacuum system, temperature control are 160 DEG C, when vacuum degree is that -0.08MPa reactions 1.5 are small, obtain processing filler, sealing is for use.
(3) low stain silicone grease is prepared
By weight, 500 parts micro- 100 parts of silicone oil of crosslinking, processing of filler are taken, is added in blender, speed of agitator is
30rpm, reaction temperature are 95 DEG C, and vacuum degree is that scattered 3h is mixed under -0.095MPa, and filtering, discharge to obtain low stain silicone grease.
(4) performance test of low stain silicone grease
With embodiment 1, as a result such as table 1.
Embodiment 3
(1) micro- crosslinking silicone oil is prepared
1) 3 parts of containing hydrogen silicone oil, 96.9 parts of vinyl silicone oil, 0.1 part of chloroplatinic acid are weighed according to parts by weight；
2) containing hydrogen silicone oil, vinyl silicone oil are added in reaction kettle, stirred evenly, then chloroplatinic acid is added in into reaction kettle
In, it is uniformly mixed, opens heating, 3h is reacted at 120 DEG C, cool down, when temperature is less than 50 DEG C, blowing obtains micro- crosslinking silicone oil,
Sealing is for use.
(2) processing filler is prepared
1) 95 parts of boron nitride, 5 parts of KH-550 are weighed according to parts by weight；
2) boron nitride is added in reaction kettle, heating, stirring add in KH-550 at 50 DEG C, stir 2h, then the startup that heats up
Vacuum system, temperature control are 160 DEG C, when vacuum degree is that -0.08MPa reactions 1.5 are small, obtain processing filler, sealing is for use.
(3) low stain silicone grease is prepared
By weight, 200 parts micro- 100 parts of silicone oil of crosslinking, processing of filler are taken, is added in blender, speed of agitator is
50rpm, reaction temperature are 95 DEG C, and vacuum degree is that scattered 2h is mixed under -0.095MP, and filtering, discharge to obtain low stain silicone grease.
(4) performance test of low stain silicone grease
With embodiment 1, as a result such as table 1.
The comparison of 1 Examples 1 to 3 test result of table
From the comparison of Examples 1 to 3 as can be seen that the oil of embodiment 2~3 from degree for 0, the pollution of embodiment 2 is also controlled
System is within 3mm, therefore embodiment 2 is preferred embodiment.
Comparative example 1
By weight, 500 parts of the processing filler that 100 parts of the methyl-silicone oil of 5000cp, embodiment 2 is taken to prepare, adds in stirring
In device, speed of agitator 30rpm, reaction temperature is 95 DEG C, and vacuum degree is that scattered 3h is mixed under -0.095MPa, and filtering discharges
Silicone grease.
The performance test of silicone grease is with embodiment 1, as a result such as table 2.
Comparative example 2
By weight, 500 parts of the processing filler that 100 parts of the methyl-silicone oil of 20000cp, embodiment 2 is taken to prepare, adds in stirring
In device, speed of agitator 30rpm, reaction temperature is 95 DEG C, and vacuum degree is that scattered 3h is mixed under -0.095MPa, and filtering discharges
Silicone grease.
The performance test of silicone grease is with embodiment 1, as a result such as table 2.
Comparative example 3
By weight, 500 parts of the processing filler that 100 parts of the methyl-silicone oil of 50000cp, embodiment 2 is taken to prepare, adds in stirring
In device, speed of agitator 30rpm, reaction temperature is 95 DEG C, and vacuum degree is that scattered 3h is mixed under -0.095MPa, and filtering discharges
Silicone grease.
The performance test of silicone grease is with embodiment 1, as a result such as table 2.
The comparison of 2 comparative example 1~3 of table and 2 test result of embodiment
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Embodiment 2 | |
| Cone penetration, 0.1mm | 210 | 197 | 186 | 196 |
| Fugitive constituent (200 DEG C, for 24 hours), % | 1.02 | 0.83 | 0.69 | 0.71 |
| Oil is from degree (200 DEG C, for 24 hours), % | 0.43 | 0.12 | 0.10 | 0 |
| Pollution (80 DEG C, 10h), mm | 12.8 | 10.9 | 10.2 | 2.9 |
The present invention is can be seen that with the comparison of embodiment 2 low stain silicon is synthesized using micro- crosslinking silicone oil from comparative example 1~3
It is oily to be significantly reduced from degree after fat.The oil of embodiment 2 from degree for 0, less than the test data of comparative example 1~3, embodiment 2
Pollution data are controlled also superior to the test data of comparative example 1~3 within 3mm.
Claims (7)
1. a kind of low stain silicone grease, which is characterized in that by weight ratio, by 100 parts of micro- crosslinking silicone oil and 6~500 parts of processing
Filler is made；Micro- crosslinking silicone oil is made of containing hydrogen silicone oil, vinyl silicone oil and catalyst；The processing filler is by filling out
Material and inorganic agent are made.
2. low stain silicone grease according to claim 1, which is characterized in that micro- crosslinking silicone oil, by mass percentage
It forms and is：Containing hydrogen silicone oil 0.2~5%, vinyl silicone oil 94~99.5%, catalyst 0.05~1.0%.
3. low stain silicone grease according to claim 1 or 2, which is characterized in that the catalyst is chloroplatinic acid.
4. low stain silicone grease according to claim 1 or 2, which is characterized in that the processing filler, by mass percentage
It forms and is：Filler 89~98%, inorganic agent 2~11%.
5. low stain silicone grease according to claim 1, which is characterized in that the filler is fume colloidal silica, precipitation
At least one of method white carbon, aluminium oxide, zinc oxide, boron nitride and aluminium nitride.
6. low stain silicone grease according to claim 1, which is characterized in that the inorganic agent for hexamethyldisilazane,
One kind in KH-550 and KH-560.
7. the preparation method of any one of the claim 1-6 low stain silicone grease, which is characterized in that comprise the following steps：
1) containing hydrogen silicone oil, vinyl silicone oil are added in reaction kettle, stirred evenly；Catalyst is added in, opens stirring, 60~
1~3h is reacted at 200 DEG C, treats temperature less than 50 DEG C, blowing obtains micro- crosslinking silicone oil；
2) filler is added in reaction kettle, stirring adds in inorganic agent at 40~70 DEG C, stirs 2h, then is warming up to 100~200
DEG C, start vacuum system, when reaction 2 is small under -0.065~-0.85MPa, obtain processing filler；
3) by 100 parts of micro- crosslinking silicone oil and 6~500 parts of processing fillers, micro- crosslinking silicone oil and processing filler are added in blender,
Under the rotating speed of 30~3000rpm, control temperature mixes under 40~95 DEG C, the vacuum degree of -0.08~-0.095MPa, is scattered
0.5~3h, filtering, obtains low stain silicone grease.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810048550.9A CN108102386A (en) | 2018-01-18 | 2018-01-18 | A kind of low stain silicone grease and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810048550.9A CN108102386A (en) | 2018-01-18 | 2018-01-18 | A kind of low stain silicone grease and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080213578A1 (en) * | 2006-07-12 | 2008-09-04 | Shin-Etsu Chemical Co., Ltd. | Heat conductive silicone grease composition and cured product thereof |
| CN105838079A (en) * | 2016-04-13 | 2016-08-10 | 成都硅宝科技股份有限公司 | Heat-conducting silicone grease composition with low oil separation degree and preparation method thereof |
| CN106221236A (en) * | 2016-07-26 | 2016-12-14 | 深圳市金无曼工业新材料有限公司 | Can the double-component heat-conducting silicone grease prepared of room temperature or gelation of heating and preparation method thereof |
-
2018
- 2018-01-18 CN CN201810048550.9A patent/CN108102386A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080213578A1 (en) * | 2006-07-12 | 2008-09-04 | Shin-Etsu Chemical Co., Ltd. | Heat conductive silicone grease composition and cured product thereof |
| CN105838079A (en) * | 2016-04-13 | 2016-08-10 | 成都硅宝科技股份有限公司 | Heat-conducting silicone grease composition with low oil separation degree and preparation method thereof |
| CN106221236A (en) * | 2016-07-26 | 2016-12-14 | 深圳市金无曼工业新材料有限公司 | Can the double-component heat-conducting silicone grease prepared of room temperature or gelation of heating and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 橡胶工业原材料与装备简明手册编审委员会: "《橡胶工业原材料与装备简明手册》", 30 November 2016, 北京理工大学出版社 * |
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Application publication date: 20180601 |