CN107915999A - A kind of addition thermal conductive fire retardant insulating silicon rubber and preparation method thereof - Google Patents
A kind of addition thermal conductive fire retardant insulating silicon rubber and preparation method thereof Download PDFInfo
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- CN107915999A CN107915999A CN201610887210.6A CN201610887210A CN107915999A CN 107915999 A CN107915999 A CN 107915999A CN 201610887210 A CN201610887210 A CN 201610887210A CN 107915999 A CN107915999 A CN 107915999A
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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
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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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Abstract
This application discloses a kind of addition thermal conductive fire retardant insulating silicon rubber and preparation method thereof, it includes 25~60 parts of vinyl polysiloxanes, 1.5~5 parts of hydrogen containing siloxanes, 35~75 parts of silicon powders, 0~2 part of mill base, 0.2~1 part of platinum catalyst and 0.01~0.03 part of inhibitor, the number is that the weight ratio of parts by weight, wherein vinyl polysiloxane and silicon powder is 1：(0.6~3).Pass through the production method of the addition thermal conductive fire retardant insulating silicon rubber of the application, adjust the proportioning between each component, the finished product for the thermal conductivity for adapting to different requirements can be made, obtained addition thermal conductive fire retardant insulating silicon rubber flame-retardant excellent performance, rubber mobility is good, and raw material are cheap and easy to get, it is adapted to industrialized production.
Description
Technical field
The application belongs to silastic material technical field, specifically, is related to a kind of addition thermal conductive fire retardant insulating silicon rubber
Glue and preparation method thereof.
Background technology
Compared with natural rubber and other synthetic rubber, silicon rubber has high- and low-temperature resistance, ageing-resistant, electric insulation, physiology
Inertia, a series of excellent properties such as release property is good, in aerospace, electric, chemical industry, machinery, building, communications and transportation, doctor
Health etc. is treated to be widely used.
In electronics field, electronic product often produces substantial amounts of heat when running, can serious shadow if shedding not in time
The operational efficiency and service life of product are rung, therefore in order to improve heat dissipation performance, conduction material can be filled in the product, reduces heat
Accumulation.Electronics is a kind of typical polymer composite with heat conductive flame-retarding silicon rubber, it is mainly led by being added into silica gel
Prepared by heat and fire-retardant filler, metal packing (such as Al, Ag, Cu) has higher thermal conductivity factor, but its is conductive,
Can not be suitable for electronic product, inorganic non-metallic such as carborundum also has high thermal conductivity, but its is expensive；It is big at present
Part with magnesia, aluminium oxide etc. is used as heat filling, but its fire resistance is often not fully up to expectations, and the viscosity of sizing material compared with
Height, it is inconvenient for use.
The content of the invention
In order to solve the above-mentioned technical problem, this application discloses a kind of addition thermal conductive fire retardant insulating silicon rubber, it includes
25~60 parts of vinyl polysiloxanes, 1.5~5 parts of hydrogen containing siloxanes, 35~75 parts of silicon powders, 0~2 part of mill base, 0.2~1
Part platinum catalyst and 0.01~0.03 part of inhibitor, the number are parts by weight, and wherein vinyl polysiloxane and silicon is micro-
The weight ratio of powder is 1：(0.6~3).
According to the embodiment of the application, the viscosity of above-mentioned vinyl polysiloxane is 500mPa.s~1000mPa.s,
There are at least two vinyl to be connected with silicon atom for it.
According to the embodiment of the application, the viscosity of above-mentioned hydrogen containing siloxane is 10mPa.s~100mPa.s, its hydrogen
The content of atom is 0.1%~1.6%, and at least three hydrogen atoms are connected with silicon atom, and the hydrogen containing siloxane is straight chain
Shape, dendritic or cricoid one or more.
According to the embodiment of the application, above-mentioned silicon powder is hydrophily silicon powder, its particle diameter is 3 μm~50 μm.
According to the embodiment of the application, above-mentioned platinum catalyst is isopropyl alcohol solution of chloroplatinic acid, chloroplatinic acid tetrahydrofuran
Solution, chloroplatinic acid-divinyl tetramethyl disiloxane complex or chloroplatinic acid -1,3,5,7- tetravinyls -1,3,5,7- tetra-
Methyl-cyclotetrasiloxane complex, the wherein content of Pt atoms are 100ppm~500000ppm.
According to the embodiment of the application, above-mentioned inhibitor is methyl butynol, ethynylcyclohexanol, the horse containing alkynyl
Come rich maleic acid sour or derivatives thereof, containing alkynyl or derivatives thereof, more vinyl polysiloxanes, pyridine, unsaturated acyl amine,
Organophosphor or phosphite ester.
According to the embodiment of the application, above-mentioned mill base is the pigment using vinyl polysiloxane as decentralized medium.
The application further discloses a kind of production method of addition thermal conductive fire retardant insulating silicon rubber, comprises the following steps：
(1) 100 parts of vinyl polysiloxanes and 1 part of silazane input Cheng are closed into machine, stirring after five minutes, then puts into 100 parts
The silicon powder, is stirred 30 minutes；
(2) 1 part of silazane is continuously added, is stirred 5 minutes, adds 100 parts of silicon powders, is stirred 30 minutes；
(3) repeat step (2)；
(4) 3 parts of silazane are added, when stirring 1 is small；
(5) repeat step (4), stirring form the first sizing material；
(6) kneader is warming up to 145 DEG C, and adds water and clean the first sizing material 4 times, amount of water during cleaning is the every time
The 1% of the weight of one sizing material；
(7) affiliated kneader is vacuumized, and when keeping vacuum 2 small for 145 DEG C, extracts moisture and lower-molecular substance out, then
It is cooled to less than 70 DEG C；
(8) vinyl polysiloxane is added into first sizing material, until the vinyl polysiloxane is total
The ratio of parts by weight and the parts by weight of the silicon powder is 1：0.6~3, form the second sizing material；
(9) 100 part of second sizing material is taken, is stirred, obtains with the more parts of inhibitor, hydrogen containing siloxane and platinum catalyst
To finished product.
By the production method of the addition thermal conductive fire retardant insulating silicon rubber of the application, the proportioning between each component is adjusted, can
The finished product for the thermal conductivity for adapting to different requirements, obtained addition thermal conductive fire retardant insulating silicon rubber flame-retardant excellent performance, glue is made
Expect that mobility is good, and raw material are cheap and easy to get, are adapted to industrialized production.
Embodiment
Below will disclose the application multiple embodiments, as clearly stated, it is many material object on details will with
Illustrate in the lump in lower narration.It should be appreciated, however, that the details on these material objects is not applied to limit the application.That is,
In some embodiments of the application, the details in these practices is non-essential.
On its " first " used herein, " second " etc., the meaning of order or cis-position is not especially censured, also non-use
To limit the application, it is just for the sake of difference with the component of constructed term description or operation.
The application provides a kind of addition thermal conductive fire retardant insulating silicon rubber, it include 25~60 parts of vinyl polysiloxanes,
1.5~5 parts of hydrogen containing siloxanes, 35~75 parts of silicon powders, 0~2 part of mill base, 0.2~1 part of platinum catalyst and 0.01~0.03 part
Inhibitor, the number are that the weight ratio of parts by weight, wherein vinyl polysiloxane and silicon powder is 1：(0.6~
3)。
Specifically, the viscosity of vinyl polysiloxane is 500mPa.s~1000mPa.s, it has at least two ethene
Base is connected with silicon atom, and vinyl is located at the end of the chain or side chain, it is preferable that vinyl is located at the end of the chain；The viscosity of hydrogen containing siloxane
For 10mPa.s~100mPa.s, the content of its hydrogen atom is 0.1%~1.6%, at least three hydrogen atoms and silicon atom phase
Even, the hydrogen containing siloxane is straight-chain, dendritic or cricoid one or more mix, it is preferable that hydrogeneous poly- silica
Alkane is straight-chain, and hydrogen atom content is 0.4%~0.75%；Silicon powder is hydrophily silicon powder, its particle diameter is 3 μm~50 μm.
Platinum catalyst is isopropyl alcohol solution of chloroplatinic acid, chloroplatinic acid tetrahydrofuran solution, chloroplatinic acid-divinyl tetramethyl disiloxane are matched somebody with somebody
Compound or chloroplatinic acid -1,3,5,7- tetravinyls -1,3, wherein 5,7- tetramethyls-cyclotetrasiloxane complex, Pt atoms contain
Measure as 100ppm~500000ppm.Inhibitor is methyl butynol, ethynylcyclohexanol, containing the maleic acid of alkynyl or its derivative
Thing, rich maleic acid containing alkynyl or derivatives thereof, more vinyl polysiloxanes, pyridine, unsaturated acyl amine, organic phosphine or phosphorous
Acid esters, preferably methyl butynol, ethynylcyclohexanol.Mill base is the pigment using vinyl polysiloxane as decentralized medium.
The production method of the addition thermal conductive fire retardant insulating silicon rubber of the description below the application.First, by 100 parts of vinyl
Polysiloxanes and 1 part of silazane input Cheng close machine, and stirring after five minutes, then puts into 100 parts of silicon powders, stirs 30 minutes, by three
Stir evenly.1 part of silazane is continuously added, is stirred 5 minutes, adds 100 parts of silicon powders, is stirred 30 minutes, repeats this operation.
After stirring, add 3 parts of silazane, stirring 1 it is small when, again add 3 parts of silazane, and stir 1 it is small when, stir evenly to be formed
First sizing material.Then kneader is warming up to 145 DEG C, and adds water and clean the first sizing material 4 times, each amount of water is the first glue
The 1% of the weight of material.After cleaning, kneader is vacuumized, and when 145 DEG C of constant temperature keep vacuum 2 small, extraction moisture and
Lower-molecular substance, is cooled to less than 70 DEG C.Then continue to add vinyl polysiloxane into the first sizing material so that vinyl
The ratio of the total weight parts of polysiloxanes and the total weight parts of silicon powder is 1：(0.6~3), forms the second sizing material.Finally take out
100 part of second sizing material, is uniformly mixed with suitable inhibitor, hydrogen containing siloxane and platinum catalyst, obtains finished product.
The application is described in detail with reference to embodiment.
Embodiment 1
100 parts of viscositys are put into Cheng for vinyl polysiloxane, the 1 part of silazane of 500mPa.s and close machine, stirring is after five minutes
100 parts of silicon powders are added, wherein silicon powder includes the silicon powder and 10 μm of silicon powder that particle diameter is 3 μm, and the proportioning of the two is 7：
3, vinyl polysiloxane, silazane and silicon powder are stirred 30 minutes.It is further continued for adding 1 part of silazane, stirs 5 minutes, then
100 parts of silicon powders are added, are stirred 30 minutes.1 part of silazane is subsequently added into, is stirred 5 minutes, adds 100 parts of silicon powders, stirring 30
Minute.Add 3 parts of silazane, when stirring 1 is small after, add 3 parts of silazane again, when stirring 1 is small, form the first sizing material.Connect
And kneader is warming up to 145 DEG C, and add water and clean the first sizing material 4 times, amount of water during cleaning is 4 parts every time.Clean
Bi Hou, vacuumizes kneader, and moisture and silazane are taken away, adds the ethene that 400 parts of viscositys are 500mPa.s
Based polysiloxane so that the parts by weight ratio of vinyl polysiloxane and silicon powder is 1：0.6, form the second sizing material.Take 100
Part the second sizing material, with 0.03 part of methyl butynol, 1 part of platinum catalyst, 2 parts of viscositys be 50mPa.s, hydrogen content be 0.75% to contain
Hydrogen polysiloxanes and 1 part of grey mill base fully mix, that is, obtain finished product.
Embodiment 2
100 parts of viscositys are put into Cheng for vinyl polysiloxane, the 1 part of silazane of 500mPa.s and close machine, stirring is after five minutes
100 parts of silicon powders are added, wherein silicon powder includes silicon powder, 30 μm of silicon powder and 10 μm of the silicon powder that particle diameter is 50 μm,
The proportioning of three is 3：4：3, vinyl polysiloxane, silazane and silicon powder are stirred 30 minutes.It is further continued for adding 1 part of silicon nitrogen
Alkane, is stirred 5 minutes, adds 100 parts of silicon powders, is stirred 30 minutes.1 part of silazane is subsequently added into, is stirred 5 minutes, adds 100
Part silicon powder, is stirred 30 minutes.Add 3 parts of silazane, when stirring 1 is small after, add 3 parts of silazane again, when stirring 1 is small,
Form the first sizing material.Then kneader is warming up to 145 DEG C, and adds water and clean the first sizing material 4 times, every time adding during cleaning
Water is 4 parts.After cleaning, after cleaning, kneader is vacuumized, moisture and silazane are taken away, then added
Enter the vinyl polysiloxane that 50 parts of viscositys are 500mPa.s so that the parts by weight ratio of vinyl polysiloxane and silicon powder
For 1：2, form the second sizing material.100 part of second sizing material is taken, with 0.02 part of ethynylcyclohexanol, 0.5 part of platinum catalyst, 5 parts of viscositys
The hydrogen containing siloxane for being 0.45% for 100mPa.s, hydrogen content and 1 part of grey mill base fully mix, that is, obtain finished product.
Embodiment 3
With embodiment 1, following adjustment is only done, the ratio of vinyl polysiloxane and the parts by weight of silicon powder is adjusted to
1：3, the content of methyl butynol is adjusted to 0.01 part, and the content of platinum catalyst is adjusted to 0.2 part, the content of hydrogen containing siloxane
1 part is adjusted to, remaining step and components unchanged, that is, obtain finished product.
Embodiment 4
With embodiment 1, following adjustment is only done, the viscosity of vinyl polysiloxane is adjusted to 1000mPa.s, vinyl gathers
The ratio of the parts by weight of siloxanes and silicon powder is adjusted to 1：2, the content of hydrogen containing siloxane is adjusted to 1 part, remaining step
And components unchanged, that is, obtain finished product.
Embodiment 5
With embodiment 1, following adjustment is only done, the ratio of vinyl polysiloxane and the parts by weight of silicon powder is adjusted to
1：1, mill base number is adjusted to 0, remaining step and components unchanged, that is, obtain finished product.
Embodiment 6
With embodiment 1, following adjustment is only done, the ratio of vinyl polysiloxane and the parts by weight of silicon powder is adjusted to
1：1.5, remaining step and components unchanged obtain finished product.
Embodiment 7
With embodiment 2, following adjustment is only done, the ratio of vinyl polysiloxane and the parts by weight of silicon powder is adjusted to
1：2.3, the content of platinum catalyst is adjusted to 0.4 part, remaining step and components unchanged, that is, obtain finished product.
Embodiment 8
With embodiment 2, following adjustment is only done, the ratio of vinyl polysiloxane and the parts by weight of silicon powder is adjusted to
1：2.8, the content of platinum catalyst is adjusted to 0.3 part, remaining step and components unchanged, that is, obtain finished product.
Embodiment 9
With embodiment 2, following adjustment is only done, silicon powder is changed to mix particle diameter for 30 μm of silicon powder and 10 μm of silicon powder
Close, the two ratio is 7：3, remaining step and components unchanged obtain finished product.
Embodiment 10
1 is adjusted to embodiment 9, and by the ratio of vinyl polysiloxane and the parts by weight of silicon powder：2.3, platinum is urged
The content of agent is adjusted to 0.4 part, remaining step and components unchanged, that is, obtain finished product.
Embodiment 11
1 is adjusted to embodiment 9, and by the ratio of vinyl polysiloxane and the parts by weight of silicon powder：2.5, platinum is urged
The content of agent is adjusted to 0.4 part, remaining step and components unchanged, that is, obtain finished product.
Embodiment 12
1 is adjusted to embodiment 9, and by the ratio of vinyl polysiloxane and the parts by weight of silicon powder：2.8, platinum is urged
The content of agent is adjusted to 0.3 part, remaining step and components unchanged, that is, obtain finished product.
Finished product made from above-mentioned 12 embodiments is detected, test respectively the thermal conductivity of each finished product, fire-retardant rank and
Material viscosity, test result are as follows：
In conclusion in one or more embodiments of the application, pass through the addition thermal conductive fire retardant insulating silicon of the application
The production method of rubber, adjusts the proportioning between each component, and the finished product for the thermal conductivity for adapting to different requirements, obtained addition can be made
Type heat conductive flame-retarding electrically insulating silicone rubber excellent fireproof performance, rubber mobility is good, and raw material are cheap and easy to get, is adapted to industry metaplasia
Production.
Some preferred embodiments of the present invention have shown and described in described above, but as previously described, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations,
Modification and environment, and above-mentioned teaching or the technology or knowledge of association area can be passed through in the scope of the invention is set forth herein
It is modified., then all should be in this hair and changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention
In the protection domain of bright appended claims.
Claims (8)
1. a kind of addition thermal conductive fire retardant insulating silicon rubber, it is characterised in that including 25~60 parts of vinyl polysiloxanes, 1.5
~5 parts of hydrogen containing siloxanes, 35~75 parts of silicon powders, 0~2 part of mill base, 0.2~1 part of platinum catalyst and 0.01~0.03 part of suppression
Preparation, the number are parts by weight, wherein the weight ratio of the vinyl polysiloxane and the silicon powder is 1：
0.6~3.
2. addition thermal conductive fire retardant insulating silicon rubber as claimed in claim 1, it is characterised in that the vinyl polysiloxane
Viscosity be 500mPa.s~1000mPa.s, its have at least two vinyl be connected with silicon atom.
3. addition thermal conductive fire retardant insulating silicon rubber as claimed in claim 1, it is characterised in that the hydrogen containing siloxane
Viscosity is 10mPa.s~100mPa.s, and the content of its hydrogen atom is 0.1%~1.6%, at least three hydrogen atoms and silicon atom
It is connected, the hydrogen containing siloxane is straight-chain, dendritic or cricoid one or more.
4. addition thermal conductive fire retardant insulating silicon rubber as claimed in claim 1, it is characterised in that the silicon powder is hydrophily
Silicon powder, its particle diameter are 3 μm~50 μm.
5. addition thermal conductive fire retardant insulating silicon rubber as claimed in claim 1, it is characterised in that the platinum catalyst is chlorine platinum
Sour aqueous isopropanol, chloroplatinic acid tetrahydrofuran solution, chloroplatinic acid-divinyl tetramethyl disiloxane complex or chloroplatinic acid-
1,3,5,7- tetravinyl -1,3,5,7- tetramethyls-cyclotetrasiloxane complex, the wherein content of Pt atoms for 100ppm~
500000ppm。
6. addition thermal conductive fire retardant insulating silicon rubber as claimed in claim 1, it is characterised in that the inhibitor is methyl fourth
Alkynol, ethynylcyclohexanol, maleic acid containing alkynyl or derivatives thereof, rich maleic acid containing alkynyl or derivatives thereof, more ethene
Based polysiloxane, pyridine, unsaturated acyl amine, organophosphor or phosphite ester.
7. addition thermal conductive fire retardant insulating silicon rubber as claimed in claim 1, it is characterised in that the mill base is with the second
Alkenyl polysiloxanes is the pigment of decentralized medium.
A kind of 8. production method of addition thermal conductive fire retardant insulating silicon rubber as claimed in claim 1, it is characterised in that including
Following steps：
(1) 100 parts of vinyl polysiloxanes and 1 part of silazane input Cheng are closed into machine, stirring after five minutes, then puts into 100 parts
The silicon powder, is stirred 30 minutes；
(2) 1 part of silazane is continuously added, is stirred 5 minutes, adds 100 parts of silicon powders, is stirred 30 minutes；
(3) repeat step (2)；
(4) 3 parts of silazane are added, when stirring 1 is small；
(5) repeat step (4), stirring form the first sizing material；
(6) kneader is warming up to 145 DEG C, and adds water cleaning first sizing material 4 times, every time amount of water during cleaning
For the 1% of the weight of first sizing material；
(7) kneader is vacuumized, and when keeping vacuum 2 small for 145 DEG C, extracts moisture and lower-molecular substance out, then cool down
To less than 70 DEG C；
(8) vinyl polysiloxane is added into first sizing material, until the gross weight of the vinyl polysiloxane
The ratio of part and the parts by weight of the silicon powder is 1：0.6~3, form the second sizing material；
(9) 100 parts of second sizing materials are taken, is stirred, obtains with the more parts of inhibitor, hydrogen containing siloxane and platinum catalyst
To finished product.
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| CN201610887210.6A CN107915999A (en) | 2016-10-11 | 2016-10-11 | A kind of addition thermal conductive fire retardant insulating silicon rubber and preparation method thereof |
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| CN105670298A (en) * | 2016-03-07 | 2016-06-15 | 惠州赛力珑新材料有限公司 | Addition-type silicon rubber and bonding method thereof |
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| CN103965641A (en) * | 2013-02-01 | 2014-08-06 | 常州化学研究所 | Preparation method of addition type heatproof liquid silicone rubber composition |
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Application publication date: 20180417 |