CN107892898A - A kind of preparation method of high heat conduction low-gravity flame-proof organosilicon casting glue - Google Patents
A kind of preparation method of high heat conduction low-gravity flame-proof organosilicon casting glue Download PDFInfo
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- CN107892898A CN107892898A CN201711096411.5A CN201711096411A CN107892898A CN 107892898 A CN107892898 A CN 107892898A CN 201711096411 A CN201711096411 A CN 201711096411A CN 107892898 A CN107892898 A CN 107892898A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K3/18—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
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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
- 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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention provides a kind of preparation method of composite graphite alkene high heat conduction low-gravity flame-proof organosilicon casting glue, is 1 by weight by component A and component B:12 mixtures mixed, when the mobility of mixture remains, fill into equipment, then carry out cold curing shaping or heating cure shaping.Component A includes as following weight percent：47.4% 61.6% vinyl silicone oil, 3% 12% modification heat conduction micro mist, 0.4% 0.6% catalyst, 35% 40% fire retardant；Component B as following weight percent than including：41.99% 57.992% vinyl silicone oil, 3% 12% graphene composite heat-conducting filler, 4% 6% containing hydrogen silicone oil, 0.005% 0.008% inhibitor, 35% 40% fire retardant.The present invention passes through the surface treatment to different heat fillings and compounding use, it is prepared into graphene composite heat-conducting filler, improve heat filling and organic silicon rubber scattering problem, graphene composite heat-conducting filler can increase the heat conductivility of organic casting glue, the compounding use obtained by simulating different-grain diameter and different-grain diameter, organic silicon potting adhesive of the invention have high heat conduction and low-gravity.
Description
Technical field
The invention belongs to organic silicon potting adhesive production technology field, is more particularly to a kind of graphene and other heat conduction are filled out
The hybrid technique of material.
Background technology
Due to the excellent thermal conductivity of graphene, it has also become the focus of all trades and professions research.Due to organic silicon rubber have it is excellent
Good electrical insulating property, high and low temperature resistance, weatherability and anti-flammability etc., are widely used in every field.With electronics
The raising of component density and degree of integration, cause power increasing, caused heat is more and more, requires potting glue accordingly
Heat conductivility just have higher requirement.Because organic silicon rubber does not have heat conductivility, generally needed to be added a certain amount of
Heat filling, but the addition of simple heat filling is larger, and it is poor with the compatibility of silicon rubber.Such filling will
The performance after the shaping of silicon rubber can be influenceed, makes the mechanical property of organic silicon rubber reduce, bonding force reduces, and hardness improves.
The content of the invention
It is an object of the invention to provide one kind for graphene, other heat fillings be modified, compound, preparing has
The production work of the composite graphite alkene high heat conduction low-gravity flame-proof organosilicon casting glue of good compatibility, mobility and thermal conductivity
Skill.
A kind of according to an aspect of the invention, there is provided composite graphite alkene high heat conduction low-gravity flame-proof organosilicon casting glue
Preparation method, by component A and component B by weight be 1:The mixture that 1-2 is mixed, in the mobility of the mixture
When remaining, fill into equipment, then carry out cold curing shaping or heating cure shaping,
The component A includes as following weight percent：47.4%-61.6% vinyl silicone oil, 3%-12%'s changes
Property heat conduction micro mist, 0.4%-0.6% catalyst, 35%-40% fire retardant,
The component B as following weight percent than including：41.99%-57.992% vinyl silicone oil, 3%-12%
Graphene composite heat-conducting filler, 4%-6% containing hydrogen silicone oil, 0.005%-0.008% inhibitor, 35%-40% resistance
Fire agent.
In some embodiments, the vinyl silicone oil for strand two ends sealed linear silicones or side chain only
Containing two vinyl polysiloxanes, the vinyl silicone oil is selected from molecule both ends and all blocked with dimethyl ethenyl silyloxy
Dimethyl polysiloxane, methyl phenyl siloxane and the poly- silica of dimethyl that molecule both ends are all blocked with dimethylsilyloxy
The copolymer of alkane, the methyl vinyl silicone and dimethyl silica that molecule both ends are all blocked with dimethyl ethenyl silyloxy
The copolymer of alkane, the copolymer for the methyl vinyl silicone that molecule both ends are all blocked with trimethicone, molecule both ends are all
The methyl polysiloxane blocked with dimethyl ethenyl silyloxy.
In some embodiments, the vinyl silicone oil is 200-3000cps in 25 DEG C of viscosity.
In some embodiments, the containing hydrogen silicone oil is the polymethyl hydrogen siloxane that hydrogen content is 0.8%-1.6%.
In some embodiments, the platinum content in the catalyst is 3000-4500ppm, selected from chloroplatinic acid-different
Acetone, chloroplatinic acid-divinyl tetramethyl disiloxane catalyst and chloroplatinic acid-tetravinyl tetramethyl-ring tetrasiloxane catalysis
One kind in agent.
In some embodiments, the inhibitor accounts for the 0.005%- of the component A and the B component gross weight
0.008%, one kind in more vinyl polysiloxanes, 1-Ethynylcyclohexanol, maleic acid esters and BTA.
A kind of component A preparation method, comprises the following steps：
The preparation of modified heat conduction micropowder filler：Heat filling is added in high mixer, disperseed at a high speed under the conditions of 100 DEG C
60min, the ethanol solution of the ethanol solution containing surfactant and catalyst is added, be heat-treated under the conditions of 110 DEG C
60min, continue to cure 120min under the conditions of 130 DEG C, modified heat conduction micropowder filler be made,
Component A preparation：Vinyl silicone oil, graphene composite heat-conducting filler, modified heat conduction micro mist are added in mixer
And fire retardant, unlatching is scattered after 10min is stirred under the conditions of room temperature, -0.085MPa, disperses 60min, adds platinum catalyst
Continue to be dispersed with stirring uniformly, component A is made.
A kind of component B preparation method, comprises the following steps：
The preparation of graphene composite heat-conducting filler：50wt% ethanol solutions are added in mixer, add two kinds or two
The surfactant of the kind above, disperse stirring 10min, regulation pH value is 3-4 or so, adds graphene and heat filling, after
Continue after being dispersed with stirring 3h, grinding refinement, the gas grinds after drying curing under the conditions of 120 DEG C, obtained graphene composite heat-conducting is filled out
Material；
The preparation of modified heat conduction micropowder filler：Heat filling is added in high mixer, disperseed at a high speed under the conditions of 100 DEG C
60min, the ethanol solution of surfactant and the ethanol solution of catalyst are added, 60min are heat-treated under the conditions of 110 DEG C,
Continuation cures 120min under the conditions of 130 DEG C, and modified heat conduction micro mist is made,
Component B preparation：Vinyl silicone oil, graphene composite heat-conducting filler, modified heat conduction micro mist are added in mixer
And fire retardant, stir under the conditions of the room temperature, -0.085MPa and open after 10min scattered, disperse 60min, add containing hydrogen silicone oil and
Inhibitor continues to be dispersed with stirring uniformly, and B component is made.
In some embodiments, the surfactant be selected from γ-(methacryloxypropyl) propyl trimethoxy silicane,
In gamma-aminopropyl-triethoxy-silane, tetra isopropyl two (dioctyl phosphite) titanate esters, dodecyltrimethoxysilane
Two or more.
In some embodiments, the inorganic filler be selected from aluminum oxide, magnesia, silicon powder, boron nitride, zinc oxide,
It is several in aluminium nitride and titanium oxide.
In some embodiments, the graphene composite heat-conducting filler includes the coarse grain footpath ball-type that particle diameter is 60-70 μm
Filler, 6-10 μm of middle particle diameter needle-like filler and 0.4-0.8 μm of fine grain irregular shape filler.
Its advantage is：The graphene composite heat-conducting filler that the present invention is obtained using physical mixed, can form densification
Interstitital texture, good thermal conducting path is formed, and handle by the compounding of other inorganic fillers and intercalation etc., in certain journey
Weaken the electric conductivity of graphene on degree, ensure the insulating properties of electron pouring sealant.Using two or more surface active
Agent can assign the more preferable feature of heat filling and operability.
The shape of the graphene composite heat-conducting filler of the present invention is mixed with sheet, spherical, aciculiform and irregular shape, with
The heat filling mix and match of a variety of different shapes and particle diameter uses, and its role is to each component is inserted with certain proportion
Seam mixing, builds more complete, effective heat conduction network in ultimate product, increases heat conduction network Connection Density, improves product
Heat conductivility.
The hydrogen-containing siloxane of the present invention is polymethyl hydrogen siloxane, hydrogen content 0.38%-1.36%, if hydrogen content mistake
Low that the degree of cross linking can be caused inadequate, material can not solidify；Cause the degree of cross linking too high if hydrogen content is too high, under mechanical properties of polymer
Drop, material hardness increase.Hydrogen-containing siloxane includes at least two organopolysiloxanes being connected with silicon atom, to ensure well
Mechanical property preferred molar ratio：Si-H/Si-Vi=1：3, preferably silicon hydrogen content≤0.5wt%.
Vinyl silicone oil has certain limitation in 25 DEG C of viscosity, it is desirable to which viscosity is between 200-3000cps, if viscosity
Crossing conference influences the viscosity of block polymer, causes that whole electronic original part can not be full of when early embedding sophisticated electronic original paper,
If the too low mechanical properties decrease that can influence polymer of viscosity.
The present invention contributes to the surface of each component pre- using the ethanol solution of surfactant and the ethanol solution of catalyst
Processing and uniform mixing afterwards.
The present invention by be surface-treated graphene composite heat-conducting filler carry out improve heat filling disperse with organic silicon rubber
Problem, graphene composite heat-conducting filler can be realized, while insulating properties are met, increase the heat conductivility of organic casting glue,
The obvious proportion for reducing product simultaneously.The compounding use obtained by simulating different-grain diameter and different-grain diameter, of the invention has
Machine silicon casting glue has high heat conduction and low-gravity.
Embodiment
Embodiment one,
The preparation of modified heat conduction micropowder filler：By 100 parts of heat filling boron nitride, aluminum oxide, magnesia, zinc oxide, silicon
Micro mist and titanium oxide are added in high mixer, are disperseed 60min at a high speed under the conditions of 100 DEG C, are added 5 parts of 40wt% γ-(methyl-props
Alkene acyl-oxygen) ethanol solution of propyl trimethoxy silicane, the second of 5 parts of 40wt% tetra isopropyls two (dioctyl phosphite) titanate esters
Alcoholic solution, 0min is heat-treated at 110 DEG C, and 120min is cured at 130 DEG C, modified heat conduction micropowder filler is made.
The preparation of graphene composite heat-conducting filler：800 parts of 50wt% ethanol solutions are added in planetary mixer, add 2
Part γ-(methacryloxypropyl) propyl trimethoxy silicane, 2 parts of tetra isopropyl two (dioctyl phosphite) titanate esters, it is scattered to stir
10min, regulation pH value to 3-4 or so are mixed, then is individually added into the heat fillings such as 100 parts of graphenes, boron nitride, aluminium nitride, is continued
After being dispersed with stirring 3h, refined by sand mill by grinding.Carried out after mixture is dried into curing at 120 DEG C using gas grinding machine
Pulverize.Obtain graphene composite heat-conducting filler.
Component A preparation：54.5% vinyl-polymethylsiloxane is added in planetary mixer, 0.1% graphene is answered
Heat filling is closed, 5% is modified heat conduction micropowder filler, 40% fire retardant, is opened after stirring 10min under the conditions of room temperature, -0.085MPa
Open scattered, scattered 60min.0.4% is added, platinum content is that 3000ppm platinum catalyst continues to be dispersed with stirring uniformly, and A is made
Component.
Component B preparation：49.9% vinyl-polymethylsiloxane is added in planetary mixer, 0.1% graphene is answered
Heat filling is closed, 5% is modified heat conduction micropowder filler, 40% fire retardant, is opened after stirring 10min under the conditions of room temperature, -0.085MPa
Open scattered, scattered 60min.Add 5% containing hydrogen silicone oil and inhibitor 1-Ethynylcyclohexanol continues to be dispersed with stirring uniformly, B is made
Component.
There is catalyst in component A, there is inhibitor in B component, but be free of catalyst, close casting glue component A will be formulated
(shift to an earlier date 1 hour in the present embodiment) by both according to 1 before embedding is carried out with casting glue B component:1 ratio is mixed,
When component A and component B mobility remain, component A and component the B mixture blended together are filled into the space of equipment, by component A
Colloidal substance and component B colloidal substance carry out cross-linking reaction under catalyst action, curing molding, inhibitor control solidification
Time, to certain operating time is actually used, not yet embedding after mixing is avoided just to have been cured.
By A, B component according to 1：1 mixed-forming, test data result such as table one.
Table one, embodiment product parameters result
| Embodiment one | |
| Mix viscosity (mpas) | 1900 |
| Density (g/cm3) | 1.3 |
| Operating time (min) | 60 |
| Dielectric strength (KV/mm) | 10 |
| Dielectric constant (100HZ) | 2.8 |
| Thermal conductivity (level) (w/mk) | 7.5 |
| Tensile strength (psi) | 125 |
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, do not taking off
On the premise of conceiving from the invention, various modifications and improvements can be made, these belong to protection scope of the present invention.
Claims (11)
1. a kind of preparation method of composite graphite alkene high heat conduction low-gravity flame-proof organosilicon casting glue, it is characterised in that by component A
It is 1 by weight with component B:The mixture that 1-2 is mixed, when the mobility of the mixture remains, fill into equipment,
Cold curing shaping or heating cure shaping are carried out again,
The component A includes as following weight percent：47.4%-61.6% vinyl silicone oil, 3%-12% modification are led
Hot micropowder filler, 0.4%-0.6% catalyst, 35%-40% fire retardant,
The component B includes as following weight percent：41.99%-57.992% vinyl silicone oil, 3%-12% graphite
Alkene composite heat-conducting filler, 4%-6% containing hydrogen silicone oil, 0.005%-0.008% inhibitor, 35%-40% fire retardant.
2. the preparation method of composite graphite alkene high heat conduction low-gravity flame-proof organosilicon casting glue according to claim 1, its
It is characterised by, the vinyl silicone oil only gathers for the linear silicones or side chain of strand two ends sealed containing two vinyl
Siloxanes, the vinyl silicone oil are selected from the poly- silica of dimethyl that molecule both ends are all blocked with dimethyl ethenyl silyloxy
Alkane, the methyl phenyl siloxane and the copolymer of dimethyl polysiloxane that molecule both ends are all blocked with dimethylsilyloxy, point
The methyl vinyl silicone and the copolymer of dimethyl siloxane that sub- both ends are all blocked with dimethyl ethenyl silyloxy, point
The copolymer for the methyl vinyl silicone that sub- both ends are all blocked with trimethicone, dimethyl ethenyl is all used at molecule both ends
The methyl polysiloxane of silyloxy end-blocking.
3. the preparation method of the fire-retardant organic silicon potting adhesive of composite graphite alkene high heat conduction low-gravity according to claim 2,
Characterized in that, the vinyl silicone oil is 200-3000cps in 25 DEG C of viscosity.
4. the preparation method of the fire-retardant organic silicon potting adhesive of composite graphite alkene high heat conduction low-gravity according to claim 1,
Characterized in that, the polymethyl hydrogen siloxane that it is 0.8%-1.6% that the containing hydrogen silicone oil, which is hydrogen content,.
5. the preparation method of the fire-retardant organic silicon potting adhesive of composite graphite alkene high heat conduction low-gravity according to claim 1,
Characterized in that, the catalyst is platinum catalyst, the platinum content in the catalyst is 3000-4500ppm, is selected from
Chloroplatinic acid-isopropyl acetone, chloroplatinic acid-divinyl tetramethyl disiloxane and chloroplatinic acid-tetravinyl tetramethyl-ring tetrasiloxane
In one kind.
6. the preparation method of the fire-retardant organic silicon potting adhesive of composite graphite alkene high heat conduction low-gravity according to claim 1,
Characterized in that, the inhibitor accounts for the 0.005%-0.008% of the gross weight of the component A and the B component, selected from more second
One kind in alkenyl polysiloxanes, 1-Ethynylcyclohexanol, maleic acid esters and BTA.
7. a kind of component A preparation method, it is characterised in that comprise the following steps：
The preparation of modified heat conduction micropowder filler：Heat filling is added in high mixer, disperses 60min at a high speed under the conditions of 100 DEG C,
The ethanol solution of surfactant and the ethanol solution of catalyst are added, 60min is heat-treated under the conditions of 110 DEG C, continues
120min is cured under the conditions of 130 DEG C, modified heat conduction micro mist is made；
Component A preparation：Vinyl silicone oil, graphene composite heat-conducting filler, modified heat conduction micro mist and resistance are added in mixer
Agent is fired, unlatching is scattered after 10min is stirred under the conditions of room temperature, -0.085MPa, disperses 60min, adds platinum catalyst continuation
It is dispersed with stirring uniformly, component A is made.
8. a kind of component B preparation method, it is characterised in that comprise the following steps：
The preparation of graphene composite heat-conducting filler：50wt% ethanol solutions are added in mixer, add two kinds or two kinds with
Upper surface activating agent, disperse stirring 10min, regulation pH value is 3-4 or so, adds graphene and heat filling, continues to stir
After scattered 3h, grinding refinement, the gas grinds after drying curing under the conditions of 120 DEG C, graphene composite heat-conducting filler is made；
The preparation of modified heat conduction micro mist：Heat filling is added in high mixer, disperses 60min at a high speed under the conditions of 100 DEG C, then add
Enter the ethanol solution of surfactant and the ethanol solution of catalyst, 60min is heat-treated under the conditions of 110 DEG C, continue at 130 DEG C
Under the conditions of cure 120min, modified heat conduction micropowder filler is made,
Component B preparation：Vinyl silicone oil, graphene composite heat-conducting filler, modified heat conduction micro mist and resistance are added in mixer
Agent is fired, unlatching is scattered after 10min is stirred under the conditions of room temperature, -0.085MPa, disperses 60min, adds containing hydrogen silicone oil and suppression
Agent continues to be dispersed with stirring uniformly, and B component is made.
9. the preparation method of the graphene composite heat-conducting filler according to claim 7 or 8, it is characterised in that the surface
Activating agent is selected from γ-(methacryloxypropyl) propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane, tetra isopropyl two
Two or more in (dioctyl phosphite) titanate esters, dodecyltrimethoxysilane.
10. the preparation method of the graphene composite heat-conducting filler according to claim 7 or 8, it is characterised in that described inorganic
Filler is several in aluminum oxide, magnesia, silicon powder, boron nitride, zinc oxide, aluminium nitride and titanium oxide.
11. the preparation method of graphene composite heat-conducting filler according to claim 8, it is characterised in that the graphene
Inorganic filler in composite heat-conducting filler includes the coarse grain footpath ball-shaped filling material that particle diameter is 60-70 μm, 6-10 μm of middle particle diameter needle-like
Filler and 0.4-0.8 μm of fine grain irregular shape filler.
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