CN109370511A - A kind of silicone sealants and preparation method thereof - Google Patents
A kind of silicone sealants and preparation method thereof Download PDFInfo
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- CN109370511A CN109370511A CN201811248910.6A CN201811248910A CN109370511A CN 109370511 A CN109370511 A CN 109370511A CN 201811248910 A CN201811248910 A CN 201811248910A CN 109370511 A CN109370511 A CN 109370511A
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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
- 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
- C09J11/06—Non-macromolecular additives organic
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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
- C08K2003/2296—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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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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- Chemical & Material Sciences (AREA)
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- Sealing Material Composition (AREA)
Abstract
The present invention provides a kind of silicone sealants, are prepared by the raw material for including following components: α, 100 parts by weight of alpha, omega-dihydroxy polydimethyl siloxane；0.1 parts by weight of dimethicone~30 parts by weight；200 parts by weight of filler~1000 parts by weight；10 parts by weight of organosilicon cross-linking agent~30 parts by weight；0.05 parts by weight of titanium-containing catalyst~10 parts by weight；0~10 parts by weight of mill base；The filler is selected from one of silicon powder, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, magnesium hydroxide and aluminium nitride or a variety of.Compared with prior art, silicone sealants provided by the invention use certain content component, realize preferable interaction, make product on the basis of caking property is good and stablizes, and have high thermal conductivity, and excellent fireproof performance.The experimental results showed that, the PC/PC shear strength of silicone sealants provided by the invention is 1.44MPa~1.53MPa, shear strength is 1.27MPa~1.28MPa after bis- " 85 " agings, strength retention is 80% or more, thermal coefficient is 1.52W/ (m.K)~2.23W/ (m.K), and flame retardant rating UL94 is V-0.
Description
Technical field
The present invention relates to adhesive techniques fields, are to be related to a kind of silicone sealants and its preparation side more specifically
Method.
Background technique
Silicon rubber is that main chain is alternately arranged by silicon and oxygen atom, and the rubber there are two organic group is usually connected on silicon atom.
The property for constituting the silicon oxygen bond of silicon rubber main chain determines that silicon rubber has the advantages that not available for natural rubber and other rubber,
It has extensive operating temperature range (- 60 DEG C~260 DEG C), excellent high and low temperature resistance, while having excellent heat steady
Qualitative, weatherability, corrosion resistance, electrical insulation capability and gas permeability etc., in building, electronic apparatus, aerospace, auto industry
It is applied widely with every field such as medical instruments.
Organic silica gel in the prior art has good adhesive property and leakproofness；But sealing in the prior art
The general emphasis of agent considers caking property, and the high thermal conductivity of organic silica gel is not studied.And electronic field, lighting area etc. very
The multi-field thermal conductivity for organic silica gel, which all has, to be distinctly claimed, and is needed the higher capacity of heat transmission, is improved the heat dissipation of component
Efficiency, while component is risen again, protective effect is adhesively fixed.Currently, the organic silica gel thermal coefficient of common calcium carbonate system
Generally only 0.4W/ (m.K), it can not meet the cooling requirements of component；Therefore it provides a kind of high heat conduction organosilicon binder,
The technical problem urgently to be resolved as those skilled in the art.
Summary of the invention
In view of this, the present invention provides the purpose of the present invention is to provide a kind of silicone sealants and preparation method thereof
Silicone sealants on the basis of caking property is good and stablizes, there is high thermal conductivity, and excellent fireproof performance.
The present invention provides a kind of silicone sealants, are prepared by the raw material for including following components:
α, 100 parts by weight of alpha, omega-dihydroxy polydimethyl siloxane；
0.1 parts by weight of dimethicone~30 parts by weight；
200 parts by weight of filler~1000 parts by weight；
10 parts by weight of organosilicon cross-linking agent~30 parts by weight；
0.05 parts by weight of titanium-containing catalyst~10 parts by weight；
0~10 parts by weight of mill base；
The filler is in silicon powder, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, magnesium hydroxide and aluminium nitride
It is one or more.
Preferably, the α, the kinematic viscosity of alpha, omega-dihydroxy polydimethyl siloxane are 1000mm2/ s~80000mm2/s。
Preferably, the kinematic viscosity of the dimethicone is 50mm2/ s~5000mm2/s。
Preferably, the organosilicon cross-linking agent is selected from methyltrimethoxysilane, vinyltrimethoxysilane, methyl three
One of Ethoxysilane, methyl orthosilicate and ethyl orthosilicate are a variety of.
Preferably, the titanium-containing catalyst is selected from tetrabutyl titanate, isopropyl titanate, the metatitanic acid tert-butyl ester and acetoacetate second
One of ester titanium compound is a variety of.
Preferably, the mill base is selected from one of black slurry, stock white and silver color slurry or a variety of.
The present invention also provides a kind of preparation methods of silicone sealants described in above-mentioned technical proposal, including following step
It is rapid:
A) it is de- to be subjected to vacuum after alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, filler and mill base mixing by α
Water obtains basestocks；
B) basestocks that step a) is obtained are mixed with organosilicon cross-linking agent, titanium-containing catalyst, it is viscous obtains organosilicon
Tie agent.
Preferably, the vacuum degree of vacuum dehydration described in step a) be -0.05MPa~-0.1MPa, temperature be 100 DEG C~
150 DEG C, the time is 60min~300min.
Preferably, the process of mixing described in step b) carries out in planetary mixer；The mixed revolving speed is 25HZ
~35HZ.
Preferably, the process of mixing described in step b) specifically:
Organosilicon cross-linking agent is added in the basestocks and carries out first time atmospheric agitation 10min~60min, adds and contains
Titanium catalyst carries out second of atmospheric agitation 10min~60min, then stirs 10min~60min under vacuum conditions, is had
Machine silicon bonding.
The present invention provides a kind of silicone sealants, are prepared by the raw material for including following components: α, alpha, omega-dihydroxy
100 parts by weight of dimethyl silicone polymer；0.1 parts by weight of dimethicone~30 parts by weight；200 parts by weight of filler~1000 weight
Part；10 parts by weight of organosilicon cross-linking agent~30 parts by weight；0.05 parts by weight of titanium-containing catalyst~10 parts by weight；0~10 weight of mill base
Measure part；The filler in silicon powder, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, magnesium hydroxide and aluminium nitride one
Kind is a variety of.Compared with prior art, silicone sealants provided by the invention use certain content component, realize preferable phase
Interaction makes product on the basis of caking property is good and stablizes, and has high thermal conductivity, and excellent fireproof performance.Experiment knot
Fruit shows that the PC/PC shear strength of silicone sealants provided by the invention is 1.44MPa~1.53MPa, after bis- " 85 " agings
Shear strength is 1.27MPa~1.28MPa, and for strength retention 80% or more, thermal coefficient is 1.52W/ (m.K)~2.23W/
(m.K), flame retardant rating UL94 is V-0.
In addition, silicone sealants provided by the invention are in application process to product to be bonded (such as electronic component) nothing
Corrosion, and no pollution to the environment.
In addition, preparation method provided by the invention is easy to operate, mild condition, it is suitable for large-scale production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of silicone sealants, are prepared by the raw material for including following components:
α, 100 parts by weight of alpha, omega-dihydroxy polydimethyl siloxane；
0.1 parts by weight of dimethicone~30 parts by weight；
200 parts by weight of filler~1000 parts by weight；
10 parts by weight of organosilicon cross-linking agent~30 parts by weight；
0.05 parts by weight of titanium-containing catalyst~10 parts by weight；
0~10 parts by weight of mill base；
The filler is in silicon powder, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, magnesium hydroxide and aluminium nitride
It is one or more.
In the present invention, the α, alpha, omega-dihydroxy polydimethyl siloxane are basic sizing material；The present invention is to the α, ω-
The source of dialkyl polydimethylsiloxane is not particularly limited, using commercial goods well known to those skilled in the art.
In the present invention, the α, the kinematic viscosity of alpha, omega-dihydroxy polydimethyl siloxane are preferably 1000mm2/ s~80000mm2/ s,
More preferably 1500mm2/ s~20000mm2/s.In the present invention, the silicone sealants include the α of 100 parts by weight, ω-
Dialkyl polydimethylsiloxane.
In the present invention, the dimethicone primarily serves plasticization；The present invention carrys out the dimethicone
Source is not particularly limited, using commercial goods well known to those skilled in the art.In the present invention, the dimethicone
Kinematic viscosity be preferably 50mm2/ s~5000mm2/ s, more preferably 100mm2/ s~1000mm2/s.In the present invention, described
Silicone sealants include 0.1 parts by weight~30 parts by weight dimethicone, preferably 5 parts by weight~20 parts by weight.
In the present invention, the filler is selected from silicon powder, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, magnesium hydroxide
With one of aluminium nitride or a variety of, preferably one of aluminium oxide, aluminium hydroxide and zinc oxide or a variety of.It is excellent in the present invention
In the embodiment of choosing, the filler is aluminium hydroxide and zinc oxide；The mass ratio of the aluminium hydroxide and zinc oxide is preferably 1:
(0.7~0.9), more preferably 1:0.8.In another two preferred embodiment of the present invention, the filler is aluminium oxide and hydrogen-oxygen
Change aluminium, wherein the aluminium oxide is ball-type aluminium oxide well known to those skilled in the art.
In the present invention, the partial size of the filler is preferably 1 μm~50 μm.The present invention is to the source of the filler without spy
Different limitation, using above-mentioned silicon powder well known to those skilled in the art, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, hydrogen-oxygen
Change the commercial goods of magnesium and aluminium nitride.In the present invention, the filler preferably passes through fatty acid treatment, and the present invention is to this
It is not particularly limited.The present invention uses above-mentioned particular kind of filler, cooperates other certain content components, can be realized preferable
Interaction, makes product on the basis of caking property is good and stablizes, and has high thermal conductivity, and excellent fireproof performance.At this
In invention, the silicone sealants include 200 parts by weight~1000 parts by weight filler, preferably 450 parts by weight~900 weights
Measure part.
In the present invention, the organosilicon cross-linking agent is preferably selected from methyltrimethoxysilane, vinyl trimethoxy silicon
One of alkane, methyltriethoxysilane, methyl orthosilicate and ethyl orthosilicate are a variety of, more preferably methyl trimethoxy oxygroup
Silane.In the present invention, the organosilicon cross-linking agent primarily serves crosslinking curing effect, with α, alpha, omega-dihydroxy polydimethyl silicon
Sealant is set to become elastomer after the reaction of oxygen alkane.The present invention is not particularly limited the source of the organosilicon cross-linking agent, uses
Above-mentioned methyltrimethoxysilane well known to those skilled in the art, vinyltrimethoxysilane, methyltriethoxysilane,
The commercial goods of methyl orthosilicate and ethyl orthosilicate.In the present invention, the silicone sealants include 10 parts by weight
The organosilicon cross-linking agent of~30 parts by weight, preferably 15 parts by weight~25 parts by weight.
In the present invention, the titanium-containing catalyst is preferably selected from tetrabutyl titanate, isopropyl titanate, the metatitanic acid tert-butyl ester and second
One of ethyl acetoacetic acid ethyl ester titanium compound is a variety of, more preferably ethylacetoacetate titanium compound.In the present invention, described
Titanium-containing catalyst, which primarily serves, accelerates cured effect.The present invention is not particularly limited the source of the titanium-containing catalyst, adopts
It is multiple with above-mentioned tetrabutyl titanate well known to those skilled in the art, isopropyl titanate, the metatitanic acid tert-butyl ester and ethylacetoacetate titanium
Close the commercial goods of object.In the present invention, the silicone sealants include 0.05 parts by weight~10 parts by weight titaniferous
Catalyst, preferably 5 parts by weight~10 parts by weight.
In the present invention, the mill base is preferably selected from one of black slurry, stock white and silver color slurry or a variety of, more preferably
For stock white.In the present invention, the mill base primarily serves the effect of toning, and those skilled in the art can use need according to border
It asks, selects the color of mill base.The present invention is not particularly limited the source of the mill base, and use is well known to those skilled in the art
The commercial goods of above-mentioned black slurry, stock white and silver color slurry.In the present invention, the silicone sealants include 0~10
The mill base of parts by weight, preferably 2 parts by weight~10 parts by weight.
Silicone sealants provided by the invention use certain content component, realize preferable interaction, product is made to exist
Caking property is good and on the basis of stablizing, and has high thermal conductivity, and excellent fireproof performance.In addition, provided by the invention organic
In application process, the small molecule that dealcoholized type curing system generates will not be to product to be bonded (such as electronic component) for silicon bonding
Corrosion is generated, it is also pollution-free to environment；And there is good tensile strength after solidifying, all have to most of substrate good
Cementability.
The present invention also provides a kind of preparation methods of silicone sealants described in above-mentioned technical proposal, including following step
It is rapid:
A) it is de- to be subjected to vacuum after alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, filler and mill base mixing by α
Water obtains basestocks；
B) basestocks that step a) is obtained are mixed with organosilicon cross-linking agent, titanium-containing catalyst, it is viscous obtains organosilicon
Tie agent.
The present invention is first by α, after alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, filler and mill base mixing, into
Row vacuum dehydration, obtains basestocks.In the present invention, the α, alpha, omega-dihydroxy polydimethyl siloxane, are filled out dimethicone
Material and mill base with it is as described in the above technical scheme identical, details are not described herein.
The present invention is not particularly limited the mixed equipment, using planetary mixer well known to those skilled in the art
?；Purpose is to be uniformly mixed each raw material.
In the present invention, the vacuum degree of the vacuum dehydration is preferably -0.05MPa~-0.1MPa, more preferably -
0.09MPa~-0.1MPa；The temperature of the vacuum dehydration is preferably 100 DEG C~150 DEG C, more preferably 110 DEG C~120 DEG C；Institute
The time for stating vacuum dehydration is preferably 60min~300min, more preferably 150min~200min.
After completing the mixed process, the present invention it is also preferable to include:
Mixed material is cooled down, basestocks are obtained.In the present invention, the temperature of the cooling is preferably less than
Equal to 50 DEG C.
After obtaining the basestocks, the present invention mixes obtained basestocks and organosilicon cross-linking agent, titanium-containing catalyst
It closes, obtains silicone sealants.In the present invention, the organosilicon cross-linking agent and titanium-containing catalyst and institute in above-mentioned technical proposal
That states is identical, and details are not described herein.
In the present invention, the mixed process carries out preferably in planetary mixer.In the preferred embodiment of the invention
In, the planetary mixer is high speed dispersion planetary mixer.In the present invention, the mixed revolving speed be preferably 25HZ~
35HZ, more preferably 30HZ~35HZ.
In the present invention, the mixed process is preferred specifically:
Organosilicon cross-linking agent is added in the basestocks and carries out first time atmospheric agitation 10min~60min, adds and contains
Titanium catalyst carries out second of atmospheric agitation 10min~60min, then stirs 10min~60min under vacuum conditions, is had
Machine silicon bonding；
More preferably:
Organosilicon cross-linking agent is added in the basestocks and carries out first time atmospheric agitation 30min, adds titaniferous catalysis
Agent carries out second of atmospheric agitation 30min, then stirs 30min under vacuum conditions, obtains silicone sealants.In the present invention
In, the vacuum degree of the vacuum condition is preferably -0.05MPa~-0.1MPa, more preferably -0.09MPa~-0.1MPa.
Preparation method provided by the invention is easy to operate, mild condition, is suitable for large-scale production.
The present invention provides a kind of silicone sealants, are prepared by the raw material for including following components: α, alpha, omega-dihydroxy
100 parts by weight of dimethyl silicone polymer；0.1 parts by weight of dimethicone~30 parts by weight；200 parts by weight of filler~1000 weight
Part；10 parts by weight of organosilicon cross-linking agent~30 parts by weight；0.05 parts by weight of titanium-containing catalyst~10 parts by weight；0~10 weight of mill base
Measure part；The filler in silicon powder, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, magnesium hydroxide and aluminium nitride one
Kind is a variety of.Compared with prior art, silicone sealants provided by the invention use certain content component, realize preferable phase
Interaction makes product on the basis of caking property is good and stablizes, and has high thermal conductivity, and excellent fireproof performance.Experiment knot
Fruit shows that the PC/PC shear strength of silicone sealants provided by the invention is 1.44MPa~1.53MPa, after bis- " 85 " agings
Shear strength is 1.27MPa~1.28MPa, and for strength retention 80% or more, thermal coefficient is 1.52W/ (m.K)~2.23W/
(m.K), flame retardant rating UL94 is V-0.
In addition, silicone sealants provided by the invention are in application process to product to be bonded (such as electronic component) nothing
Corrosion, and no pollution to the environment.
In addition, preparation method provided by the invention is easy to operate, mild condition, it is suitable for large-scale production.
In order to further illustrate the present invention, it is described in detail below by following embodiment.Following embodiment of the present invention
The partial size of aluminium hydroxide used, zinc oxide and ball-type aluminium oxide is 1 μm~50 μm
Embodiment 1
Raw material used in the embodiment of the present invention 1 and each raw material sources and dosage ginseng are shown in Table 1.
Raw material and each raw material sources and usage data used in 1 embodiment of the present invention 1 of table
It (1) is 1500mm by kinematic viscosity2The α of/s, alpha, omega-dihydroxy polydimethyl siloxane, kinematic viscosity 350mm2/s
Dimethicone, aluminium hydroxide, zinc oxide and stock white put into high speed dispersion planetary mixer and stir evenly, 110
DEG C, vacuum dehydration 3h under -0.09~-0.1MPa, then be cooled to 50 DEG C hereinafter, obtaining basestocks.
(2) under 30HZ revolving speed, methyltrimethoxysilane atmospheric agitation is added in the basestocks that step (1) obtains
30min adds ethylacetoacetate titanium compound atmospheric agitation 30min, then under the vacuum condition of -0.09~-0.1MPa
30min is stirred to uniform, discharging obtains silicone sealants.
Embodiment 2
Raw material used in the embodiment of the present invention 2 and each raw material sources and dosage ginseng are shown in Table 2.
Raw material and each raw material sources and usage data used in 2 embodiment of the present invention 2 of table
It (1) is 1500mm by kinematic viscosity2The α of/s, alpha, omega-dihydroxy polydimethyl siloxane, kinematic viscosity 350mm2/s
Dimethicone, ball-type aluminium oxide, aluminium hydroxide and stock white put into high speed dispersion planetary mixer and stir evenly,
120 DEG C, vacuum dehydration 3h under -0.09~-0.1MPa, then 50 DEG C are cooled to hereinafter, obtaining basestocks.
(2) under 30HZ revolving speed, methyltrimethoxysilane atmospheric agitation is added in the basestocks that step (1) obtains
30min adds ethylacetoacetate titanium compound atmospheric agitation 30min, then under the vacuum condition of -0.09~-0.1MPa
30min is stirred to uniform, discharging obtains silicone sealants.
Embodiment 3
Raw material used in the embodiment of the present invention 3 and each raw material sources and dosage ginseng are shown in Table 3.
Raw material and each raw material sources and usage data used in 3 embodiment of the present invention 3 of table
It (1) is 20000mm by kinematic viscosity2The α of/s, alpha, omega-dihydroxy polydimethyl siloxane, kinematic viscosity 350mm2/
Dimethicone, ball-type aluminium oxide, aluminium hydroxide and the stock white of s, which is put into high speed dispersion planetary mixer, to stir evenly,
The vacuum dehydration 3h at 120 DEG C, -0.09~-0.1MPa, then 50 DEG C are cooled to hereinafter, obtaining basestocks.
(2) under 30HZ revolving speed, methyltrimethoxysilane atmospheric agitation is added in the basestocks that step (1) obtains
30min adds ethylacetoacetate titanium compound atmospheric agitation 30min, then under the vacuum condition of -0.09~-0.1MPa
30min is stirred to uniform, discharging obtains silicone sealants.
Comparative example 1
Raw material used in comparative example 1 and each raw material sources and dosage ginseng are shown in Table 4.
Raw material and each raw material sources and usage data used in 4 comparative example 1 of table
It (1) is 20000mm by kinematic viscosity2The α of/s, alpha, omega-dihydroxy polydimethyl siloxane, kinematic viscosity 350mm2/
Dimethicone, nanometer calcium carbonate and the stock white of s, which is put into high speed dispersion planetary mixer, to stir evenly, 120 DEG C ,-
Vacuum dehydration 3h under 0.09~-0.1MPa, then 50 DEG C are cooled to hereinafter, obtaining basestocks.
(2) under 30HZ revolving speed, methyltrimethoxysilane atmospheric agitation is added in the basestocks that step (1) obtains
30min adds ethylacetoacetate titanium compound atmospheric agitation 30min, then under the vacuum condition of -0.09~-0.1MPa
30min is stirred to uniform, discharging obtains silicone sealants.
Embodiment is measured according to test method described in " measurement of GB/T7124-2008 adhesive tensile shear strength "
1~3 and the obtained PC/PC shear strength of silicone sealants of comparative example 1；According to " GB/T 2423.50-2012 environment examination
Test " described in steady damp heat test method measurement Examples 1 to 3 and the obtained shearing mould of silicone sealants of comparative example 1
Block kept for 500 hours at 85 DEG C, 85%RH after shear strength；According to " ISO 22007-2-2015 plastics thermal conductivity and heat
The measurement of diffusivity " described in test method measurement Examples 1 to 3 and the obtained silicone sealants of comparative example 1 it is thermally conductive
Coefficient；Examples 1 to 3 and right is measured according to test method described in " measurement of GB/T2408-2008 Plastics Combustion performance "
The flame retardant rating for the silicone sealants that ratio 1 obtains.Test result ginseng is shown in Table 5.
The properties data for the silicone sealants that 5 Examples 1 to 3 of table and comparative example 1 provide
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 |
| Shear strength MPa | 1.48 | 1.44 | 1.53 | 1.62 |
| Bis- " 85 " shear strength MPa afterwards | 1.27 | 1.27 | 1.28 | 1.17 |
| Bis- " 85 " shear strength conservation rate % afterwards | 85.8 | 88.2 | 83.7 | 72.2 |
| Thermal coefficient W/ (m.K) | 1.52 | 2.23 | 1.75 | 0.43 |
| Flame retardant rating UL94 | V-0 | V-0 | V-0 | HB |
As shown in Table 5, the silicone sealants that the embodiment of the present invention 1~3 the provides basis good and stable in caking property
On, there is high thermal conductivity, and excellent fireproof performance；The shear strength (PC/PC) of product is 1.44MPa~1.53MPa, double
Shear strength is 1.27MPa~1.28MPa after " 85 " 500 hours, and shear strength property retention rate is 80% or more, thermal coefficient
It is V-0 for 1.52W/ (m.K)~2.23W/ (m.K), flame retardant rating UL94.
The above description of the disclosed embodiments, enables those skilled in the art to implement or use the present invention.It is right
A variety of modifications of these embodiments will be readily apparent to those skilled in the art, and as defined herein one
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will
It will not be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed herein
Widest scope.
Claims (10)
1. a kind of silicone sealants are prepared by the raw material for including following components:
α, 100 parts by weight of alpha, omega-dihydroxy polydimethyl siloxane；
0.1 parts by weight of dimethicone~30 parts by weight；
200 parts by weight of filler~1000 parts by weight；
10 parts by weight of organosilicon cross-linking agent~30 parts by weight；
0.05 parts by weight of titanium-containing catalyst~10 parts by weight；
0~10 parts by weight of mill base；
The filler is selected from one of silicon powder, aluminium oxide, aluminium hydroxide, zinc oxide, magnesia, magnesium hydroxide and aluminium nitride
Or it is a variety of.
2. silicone sealants according to claim 1, which is characterized in that the α, alpha, omega-dihydroxy polydimethyl silicon oxygen
The kinematic viscosity of alkane is 1000mm2/ s~80000mm2/s。
3. silicone sealants according to claim 1, which is characterized in that the kinematic viscosity of the dimethicone is
50mm2/ s~5000mm2/s。
4. silicone sealants according to claim 1, which is characterized in that the organosilicon cross-linking agent is selected from methyl trimethoxy
One of oxysilane, vinyltrimethoxysilane, methyltriethoxysilane, methyl orthosilicate and ethyl orthosilicate or
It is a variety of.
5. silicone sealants according to claim 1, which is characterized in that the titanium-containing catalyst is selected from the positive fourth of metatitanic acid
One of ester, isopropyl titanate, the metatitanic acid tert-butyl ester and ethylacetoacetate titanium compound are a variety of.
6. silicone sealants according to claim 1, which is characterized in that the mill base be selected from black slurry, stock white and
One of silver color slurry is a variety of.
7. a kind of preparation method of the described in any item silicone sealants of claim 1~6, comprising the following steps:
A) α is carried out vacuum dehydration, obtained after alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, filler and mill base mixing
To basestocks；
B) basestocks that step a) is obtained are mixed with organosilicon cross-linking agent, titanium-containing catalyst, obtains silicone sealants.
8. preparation method according to claim 7, which is characterized in that the vacuum degree of vacuum dehydration described in step a) be-
0.05MPa~-0.1MPa, temperature are 100 DEG C~150 DEG C, and the time is 60min~300min.
9. preparation method according to claim 7, which is characterized in that the process of mixing described in step b) is in planet stirring
It is carried out in machine；The mixed revolving speed is 25HZ~35HZ.
10. preparation method according to claim 9, which is characterized in that the process of mixing described in step b) specifically:
Organosilicon cross-linking agent is added in the basestocks and carries out first time atmospheric agitation 10min~60min, adds titaniferous and urges
Agent carries out second of atmospheric agitation 10min~60min, then stirs 10min~60min under vacuum conditions, obtains organosilicon
Binder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154269A (en) * | 2019-12-31 | 2020-05-15 | 杭州之江新材料有限公司 | Low-modulus heat-conducting organopolysiloxane composition and preparation method and application thereof |
| CN112724921A (en) * | 2020-12-25 | 2021-04-30 | 杭州之江新材料有限公司 | Low-viscosity heat-conducting flame-retardant silicone rubber sealant and preparation method thereof |
| CN113863002A (en) * | 2021-09-22 | 2021-12-31 | 世联汽车内饰（苏州）有限公司 | Preparation method of deodorizing fabric |
Citations (1)
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| CN106833504A (en) * | 2017-02-10 | 2017-06-13 | 深圳市森日有机硅材料股份有限公司 | A kind of heat conduction single-component dealcoholization-type RTV fluid sealants and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106833504A (en) * | 2017-02-10 | 2017-06-13 | 深圳市森日有机硅材料股份有限公司 | A kind of heat conduction single-component dealcoholization-type RTV fluid sealants and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154269A (en) * | 2019-12-31 | 2020-05-15 | 杭州之江新材料有限公司 | Low-modulus heat-conducting organopolysiloxane composition and preparation method and application thereof |
| CN112724921A (en) * | 2020-12-25 | 2021-04-30 | 杭州之江新材料有限公司 | Low-viscosity heat-conducting flame-retardant silicone rubber sealant and preparation method thereof |
| CN112724921B (en) * | 2020-12-25 | 2022-07-05 | 杭州之江新材料有限公司 | Low-viscosity heat-conducting flame-retardant silicone rubber sealant and preparation method thereof |
| CN113863002A (en) * | 2021-09-22 | 2021-12-31 | 世联汽车内饰（苏州）有限公司 | Preparation method of deodorizing fabric |
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