CN109054733A - A kind of bi-component self-adhesion add-on type electron pouring sealant and preparation method thereof - Google Patents
A kind of bi-component self-adhesion add-on type electron pouring sealant and preparation method thereof Download PDFInfo
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- CN109054733A CN109054733A CN201811091622.4A CN201811091622A CN109054733A CN 109054733 A CN109054733 A CN 109054733A CN 201811091622 A CN201811091622 A CN 201811091622A CN 109054733 A CN109054733 A CN 109054733A
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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
-
- 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
-
- 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
-
- 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
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- 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
Abstract
The invention discloses a kind of bi-component self-adhesion add-on type electron pouring sealants and preparation method thereof, a kind of method for preparing the high activity platinum complex that platinum content is 8130ppm-9020ppm is also disclosed simultaneously, the present invention joined 7.5% SiCw of the high activity platinum complex that platinum content is 8130ppm-9020ppm and aluminum oxide and gross mass in the preparation process of bi-component self-adhesion add-on type electronics sealed cans glue, the electronics sealed cans glue of method preparation of the invention has viscosity low, good fluidity, it is easy to operate, there is the characteristics of tack, there can be good adhesive property with substrate surface in the case where not needing pretreated situation, simultaneously, there is good heating conduction and firing resistance compared with prior art, effectively increase product quality.
Description
Technical field
The present invention relates to silicon rubber technical field, more particularly to a kind of bi-component self-adhesion add-on type electron pouring sealant and
Preparation method.
Background technique
With recently as the products such as electronics, electric appliance, weaving it is a large amount of outlet and domestic construction, automobile, electronics,
The industries such as medical treatment, daily use chemicals rapidly develop the thriving demand of organosilicon material, China's organosilicon industry, it has also become high
Mainstay industry in performance chemical industry field of new materials.Since silica gel resistance to acid and alkali is good, resistance to atmospheric aging, insulation, resistance to compression,
Moisture-proof shockproof characteristic, the silicon rubber of low viscosity are widely used in electrical appliance module encapsulating protection field always.However, current city
There is have shrinkage, may corrode to electronic device condensed type casting glue on field;Add-on type casting glue needs
The effect just having been had using silane coupling agent or tackifier in advance, it is not only expensive but also complicated for operation.
The patent of invention that China Patent No. is 201510103763.3 discloses a kind of electron pouring sealant and its preparation side
Method, including A glue and B glue, specific steps are as follows:) preparation of A glue: by castor oil 300kg, dioctyl phthalate 900kg, phosphoric acid
Three ester 500kg are placed in reaction kettle, are heated to 110 DEG C, and 40 DEG C are cooled to after vaccum dewatering, hexamethylene diisocyanate is then added
2000kg, amino-acid zinc 2kg, reaction 15min discharge to obtain A glue;(2) prepared by B glue: by polytetrahydrofuran diol 1000kg, adjacent benzene
Diformazan dioctyl phthalate 800kg, phosphotriester 600kg are added in reaction kettle, are heated to 130 DEG C, chlorination is added after vaccum dewatering
Paraffin -52,800kg is added dibutyl tin dilaurate (by 0.1% addition of B glue weight), is then cooled to 90 DEG C, is added
Discharging obtains B glue after 5kg ethyl alcohol, then vaccum dewatering 20min;(3) A glue, the mixing of B glue: A glue and B glue are mixed by weight 1:2
It closes uniformly, is subsequently poured into encapsulating mould solidification.The preparation process of this sealed cans glue, due to using conventional component and catalysis
Agent, therefore, the electron pouring sealant viscosity of preparation are less desirable, are easy to fall off with substrate surface.
The patent of invention that China Patent No. is 201310012160.3 discloses a kind of electron pouring sealant and its preparation side
Method, the specific steps of preparation method are as follows: (1) prepared by A glue: polyalcohol, plasticizer, phosphotriester are mixed, 110- is heated to
130 DEG C, it is cooled to 10-60 DEG C after water removal, isocyanates is then added, reacts and A glue is made;(2) B glue prepare: by polyalcohol,
Plasticizer, phosphotriester mixing, are heated to 110-130 DEG C, chlorinated paraffin -52 are added after water removal, is then cooled to 90-110
DEG C, then remove water to obtain B glue;(3) A glue, the mixing of B glue: A glue is uniformly mixed with B glue, is subsequently poured into encapsulating mould solidification.
The electron pouring sealant of the method preparation prepares electronics filling due to using the components such as polyalcohol, plasticizer, phosphotriester
Although sealing is easy to remove, viscosity is poor, lower with substrate binding force, and heating conduction is not very well, to be easy on substrate poly-
Heat-collecting capacity and flame retardant property is poor.
In consideration of it, add-on type glue casting glue is allowed to be able to achieve self-adhesion, energy and substrate surface in the case where not needing pretreated situation
There is good adhesive property to become a selection well, moreover, it is good thermally conductive to have electron pouring sealant
Performance and flame retardant property become the direction of industry research.
Summary of the invention
The purpose of the present invention is overcoming shortcoming in the prior art, a kind of bi-component self-adhesion add-on type electronics is provided
Casting glue and preparation method thereof, to solve the problems, such as above-mentioned background technique.
In order to solve the above technical problems, the present invention is solved by following technical proposals:
A kind of bi-component self-adhesion add-on type electron pouring sealant, component A and B component comprising following parts by weight:
Wherein, component A includes
Vinyl silicone oil: 100 parts;
High activity platinum complex: 0.1-0.4 parts;
B component includes:
The vinyl silicone oil is poly- the two of the dimethyl ethenyl silyloxy bi-end-blocking that viscosity is 500cp-800cp
Methylsiloxane.
The containing hydrogen silicone oil is the methyl end containing hydrogen silicone oil that hydrogen content is 0.45%-0.58%.
The high activity platinum complex is the platinum complex that platinum content is 8130ppm-9020ppm.
The present invention also provides it is a kind of prepare platinum content be 8130ppm-9020ppm high activity platinum complex method,
The following steps are included:
7.5-8.5 parts of chloroplatinic acid is added in step 1 in the reaction flask that quality is divided into 100 parts of vinyl double seal head
The platinum acid chloride solution mixed with 63-67 parts of dehydrated alcohols, 55-65 DEG C of heating water bath stir 1.3-1.6 hours;
The sodium bicarbonate that mass parts are 15-17 parts is added into reaction flask, stirs 1.2-1.5 hours, by institute for step 2
It obtains object to be filtered under diminished pressure, filtrate is evaporated under reduced pressure 2.2-2.5 hours under 70-79 DEG C of water-bath;
Step 3, into reaction flask be added dimethicone until gross mass part be 320 parts, stir evenly platinum obtained
Content is the platinum complex of 8130ppm-9020ppm.
The present invention also provides a kind of preparation methods of institute's bi-component self-adhesion add-on type electron pouring sealant, including following step
It is rapid:
Step 1 prepares component A, first by the dimethyl silicone polymer of the dimethyl ethenyl silyloxy bi-end-blocking
It is added in reaction kettle, adds the high activity platinum complex and filter obtained A component after stirring;
Step 2 prepares B component, first adds the dimethyl silicone polymer that the dimethyl ethenyl silyloxy blocks
Enter in reaction kettle, it is hydrogeneous to add glycidoxy-propyltrimethoxy silane, vinyl silane tri-butyl peroxy, methyl end
Silicone oil and ethynylcyclohexanol filter after stirring in a kettle and B component are made;
Step 3 matches glue, and A, B component are mixed according to mass ratio 1:1, is stirred evenly, is obtained bi-component tack and add
Form electron pouring sealant.
The present invention have the following advantages that compared with prior art and the utility model has the advantages that
1. it is living to joined the height that platinum content is 8130ppm-9020ppm in the preparation process of electron pouring sealant of the invention
Property platinum complex, and provide the preparation method of this high activity platinum complex, high activity platinum complex can be such that reaction more fills
Divide thoroughly, is conducive to improve production efficiency.
2. bi-component self-adhesion add-on type electron pouring sealant of the invention joined vinyl tri-tert during the preparation process
Peroxy-silane and glycidoxy-propyltrimethoxy silane, epoxy group can effectively reinforce silica gel to the bonding of nonmetallic materials, and
Peroxy can effectively reinforce the bonding to metal material, and the present invention has viscosity low, and good fluidity is easy to operate, there is tack
The characteristics of, there can be good adhesive property with substrate surface in the case where not needing pretreated situation.
3. the present invention joined filler aluminum oxide in the preparation process of bi-component self-adhesion add-on type electron pouring sealant
(Al2O3) and dosage be 7.5% SiCw of filler gross mass, SiCw can be interspersed in Al2O3Between particle, advantageously forms and lead
Ther mal network increases thermal conducting path, reduces the heat transmission resistance of sealed cans glue, improves the heating conduction and anti-flammability of sealed cans glue
Energy.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Specific implementation process of the invention is as follows:
Embodiment 1
A kind of bi-component self-adhesion add-on type electron pouring sealant, which is characterized in that the component A comprising following parts by weight and B group
Point:
Wherein, component A includes
Vinyl silicone oil: 100 parts;
0.1 part of high activity platinum complex;
B component includes:
The vinyl silicone oil is poly- the two of the dimethyl ethenyl silyloxy bi-end-blocking that viscosity is 500cp-800cp
Methylsiloxane.
The containing hydrogen silicone oil is the methyl end containing hydrogen silicone oil that hydrogen content is 0.45%-0.58%.
The high activity platinum complex is the platinum complex that platinum content is 8130ppm-9020ppm.
The present invention also provides a kind of preparation methods of bi-component self-adhesion add-on type electron pouring sealant, comprising the following steps:
Step 1 prepares component A, and first the dimethyl silicone polymer of dimethyl ethenyl silyloxy bi-end-blocking is added
In reaction kettle, adds the high activity platinum complex and filter obtained component A after stirring;
Step 2 prepares B component, and the dimethyl silicone polymer for first blocking dimethyl ethenyl silyloxy is added anti-
It answers in kettle, adds glycidoxy-propyltrimethoxy silane, vinyl silane tri-butyl peroxy, methyl end containing hydrogen silicone oil
And ethynylcyclohexanol, it is filtered after stirring in a kettle and B component is made;
Step 3 matches glue, and A, B component are mixed according to mass ratio 1:1, is stirred evenly, is obtained bi-component tack and add
Form electron pouring sealant.
The high activity platinum complex that platinum content is 8130ppm-9020ppm is prepared the present invention also provides a kind of
Method, which comprises the following steps:
7.5-8.5 parts of chloroplatinic acid is added in step 1 in the reaction flask that quality is divided into 100 parts of vinyl double seal head
The platinum acid chloride solution mixed with 63-67 parts of dehydrated alcohols, 55-65 DEG C of heating water bath stir 1.3-1.6 hours;
The sodium bicarbonate that mass parts are 15-17 parts is added into reaction flask, stirs 1.2-1.5 hours, by institute for step 2
It obtains object to be filtered under diminished pressure, filtrate is evaporated under reduced pressure 2.2-2.5 hours under 70-79 DEG C of water-bath;
Step 3, into reaction flask be added dimethicone until gross mass part be 320 parts, stir evenly platinum obtained
Content is the platinum complex of 8130ppm-9020ppm.
Embodiment 2
A kind of bi-component self-adhesion add-on type electron pouring sealant, component A and B component comprising following parts by weight:
Wherein, component A includes
Vinyl silicone oil: 100 parts;
0.3 part of high activity platinum complex;
B component includes:
Wherein, the vinyl silicone oil is the dimethyl ethenyl silyloxy bi-end-blocking that viscosity is 500cp-800cp
Dimethyl silicone polymer.
Wherein, the containing hydrogen silicone oil is the methyl end containing hydrogen silicone oil that hydrogen content is 0.45%-0.58%.
Wherein, the high activity platinum complex is the platinum complex that platinum content is 8130ppm-9020ppm.
Preparation method: with embodiment 1.
Embodiment 3
A kind of bi-component self-adhesion add-on type electron pouring sealant, component A and B component comprising following parts by weight:
Wherein, component A includes
Vinyl silicone oil: 100 parts;
0.4 part of high activity platinum complex;
B component includes:
Wherein, the vinyl silicone oil is the dimethyl ethenyl silyloxy bi-end-blocking that viscosity is 500cp-800cp
Dimethyl silicone polymer.
Wherein, the containing hydrogen silicone oil is the methyl end containing hydrogen silicone oil that hydrogen content is 0.45%-0.58%.
Wherein, the high activity platinum complex is the platinum complex that platinum content is 8130ppm-9020ppm.
Preparation method: with embodiment 1.
It, can be in the preparation method of the bi-component self-adhesion add-on type electron pouring sealant of embodiment 1 to 3 in the present invention
During step 1 prepares component A, by the polydimethylsiloxanes of 100 parts of dimethyl ethenyl silyloxy bi-end-blocking
Aluminum oxide (the Al of alkane and 175-185 parts by weight2O3) and beta-silicon carbide whisker (SiCw) mixing of 15-35 parts by weight after it is same
Reaction kettle is added in high activity platinum complex after mixing together, reaction temperature is 110 degrees Celsius, vacuum degree 0.06-0.1MPa,
Component A is made after reaction 2 hours.In order to guarantee the mobility of casting glue, the mass fraction of SiCw is usually no more than 10%.When
When the mass fraction of SiCw is 7.5%, the viscosity of casting glue increases to 5800mPas from 3500rnPas, is keeping flowing
Keep the viscosity of casting glue best under dynamic implementations.
It is learnt through overtesting, with SiCw dosage gradually increasing within the scope of 5%-10%, the thermal conductivity of casting glue has
It changes significantly, thermal conductivity takes the lead in increasing comparatively fast, increases eased up later.When SiCw dosage is the 5% of filler gross mass, fill
The thermal conductivity of sealing is increased to 0.623W/mK from 0.565W/mK, this is because SiCw is not only a kind of highly heat-conductive material,
Or a kind of monocrystalline staple fiber with certain draw ratio, can be interspersed between Al2O3 particle, advantageously form heat conduction network,
Thermal conducting path is increased, the heat transmission resistance of material is reduced, when SiCw dosage is 7.5%, the heat of casting glue can be greatly improved
Conductance continues growing the dosage of SiCw, and due to having formed relatively effective thermal conducting path, the thermal conductivity of casting glue increases
Trend slows down.Moreover, SiCw dosage can excessively be such that the viscosity of casting glue increases, and its electrical insulating property is influenced, therefore, SiCw is closed
Suitable dosage is the 7.5% of filler gross mass.
It, can be in the preparation method of the bi-component self-adhesion add-on type electron pouring sealant of embodiment 1 to 3 in the present invention
In the step of step 3 matches glue, it is added the inhibitor C AS 1604-35-9TMDO/3 that mass parts are 0.3-0.5%, 7,11- tri-
Methyl dodecyne -3- alcohol, can be crosslinked rapidly in lower temperature, improve the stability of product, improve the resistance to combustion of sealed cans glue
Property, and be conducive to reduce the reaction temperature of reaction kettle, it is conducive to save the energy, the curingprocess rate of reduction and control potting compound extends
The working life of vulcanizing system had both met the requirement of process operation, in turn avoided that vulcanizate is tacky, improved the quality of sealed cans glue.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination, letter
Change, should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of bi-component self-adhesion add-on type electron pouring sealant, which is characterized in that component A and B component comprising following parts by weight:
Wherein, component A includes
Vinyl silicone oil: 100 parts;
High activity platinum complex: 0.1-0.4 parts;
B component includes:
2. a kind of bi-component self-adhesion add-on type electron pouring sealant according to claim 1, it is characterised in that: the vinyl
Silicone oil is the dimethyl silicone polymer for the dimethyl ethenyl silyloxy bi-end-blocking that viscosity is 500cp-800cp.
3. a kind of bi-component self-adhesion add-on type electron pouring sealant according to claim 1, it is characterised in that: the Silicon Containing Hydrogen
Oil is the methyl end containing hydrogen silicone oil that hydrogen content is 0.45%-0.58%.
4. a kind of bi-component self-adhesion add-on type electron pouring sealant according to claim 1, it is characterised in that: the high activity
Platinum complex is the platinum complex that platinum content is 8130ppm-9020ppm.
5. a kind of prepare as platinum content is the method for the high activity platinum complex of 8130ppm-9020ppm, spy in claim 4
Sign is, comprising the following steps:
7.5-8.5 parts of chloroplatinic acid and 63- is added in step 1 in the reaction flask that quality is divided into 100 parts of vinyl double seal head
The platinum acid chloride solution of 67 parts of dehydrated alcohols mixing, 55-65 DEG C of heating water bath stir 1.3-1.6 hours;
The sodium bicarbonate that mass parts are 15-17 parts is added into reaction flask, stirs 1.2-1.5 hours, gains is subtracted for step 2
Press filtration, filtrate are evaporated under reduced pressure 2.2-2.5 hours under 70-79 DEG C of water-bath;
Dimethicone is added until gross mass part is 320 parts into reaction flask in step 3, and stirring evenly platinum content obtained is
The platinum complex of 8130ppm-9020ppm.
6. a kind of preparation method of bi-component self-adhesion add-on type electron pouring sealant, which comprises the following steps:
Step 1 prepares component A, first the dimethyl silicone polymer of the dimethyl ethenyl silyloxy bi-end-blocking is added anti-
It answers in kettle, adds the high activity platinum complex and filter obtained component A after stirring;
Step 2 prepares B component, and reaction first is added in the dimethyl silicone polymer of dimethyl ethenyl silyloxy sealing end
In kettle, glycidoxy-propyltrimethoxy silane, vinyl silane tri-butyl peroxy, methyl end containing hydrogen silicone oil and second are added
Alkynyl cyclohexanol filters after stirring in a kettle and B component is made;
Step 3 matches glue, and A, B component are mixed according to mass ratio 1:1, stirs evenly, obtains bi-component tack add-on type
Electron pouring sealant.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112063362A (en) * | 2020-09-21 | 2020-12-11 | 湘潭市特种线缆股份有限公司 | Bi-component organic silicon pouring sealant and preparation method thereof |
CN115746699A (en) * | 2022-11-24 | 2023-03-07 | 杭州之江有机硅化工有限公司 | Transparent organic silicon coating adhesive composition and preparation method and application thereof |
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EP0269454A2 (en) * | 1986-11-28 | 1988-06-01 | Toray Silicone Company, Ltd. | Silicone pressure-sensitive adhesive composition |
CN103131381A (en) * | 2013-03-06 | 2013-06-05 | 广州市高士实业有限公司 | High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof |
CN103756631A (en) * | 2013-11-28 | 2014-04-30 | 常熟市恒信粘胶有限公司 | Double-component self-adhesive addition type flame retardant heat conducting room temperature curing organic silicon pouring sealant |
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2018
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EP0269454A2 (en) * | 1986-11-28 | 1988-06-01 | Toray Silicone Company, Ltd. | Silicone pressure-sensitive adhesive composition |
CN103131381A (en) * | 2013-03-06 | 2013-06-05 | 广州市高士实业有限公司 | High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof |
CN103756631A (en) * | 2013-11-28 | 2014-04-30 | 常熟市恒信粘胶有限公司 | Double-component self-adhesive addition type flame retardant heat conducting room temperature curing organic silicon pouring sealant |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112063362A (en) * | 2020-09-21 | 2020-12-11 | 湘潭市特种线缆股份有限公司 | Bi-component organic silicon pouring sealant and preparation method thereof |
CN115746699A (en) * | 2022-11-24 | 2023-03-07 | 杭州之江有机硅化工有限公司 | Transparent organic silicon coating adhesive composition and preparation method and application thereof |
CN115746699B (en) * | 2022-11-24 | 2023-10-31 | 杭州之江有机硅化工有限公司 | Transparent organic silicon coating adhesive composition and preparation method and application thereof |
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Application publication date: 20181221 |