CN106750319A - A kind of selective self bonding add-on type liquid silicon rubber tackifier and preparation method thereof - Google Patents
A kind of selective self bonding add-on type liquid silicon rubber tackifier and preparation method thereof Download PDFInfo
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- CN106750319A CN106750319A CN201611215986.XA CN201611215986A CN106750319A CN 106750319 A CN106750319 A CN 106750319A CN 201611215986 A CN201611215986 A CN 201611215986A CN 106750319 A CN106750319 A CN 106750319A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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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
- 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
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Abstract
The present invention provides a kind of selective self bonding add-on type liquid silicon rubber tackifier, and the tackifier structural formula is as follows：
Description
Background technology
The present invention relates to add-on type liquid silicon rubber tackifier, more particularly to a kind of selective self bonding add-on type liquid
Silicon rubber tackifier and preparation method thereof, belong to technical field of polymer materials.
Technical field
Addition-type silicon rubber is a kind of nonpoisonous and tasteless, with excellent weather resistance and electrical insulating property organosilicon material, wide at present
It is general to be applied to the industries such as electronic apparatus, machinery, automobile, daily kitchen and medical treatment.Some industries need to use different substrate materials with
The product of rubber composition.Such as traditional plastics+silica gel, silica gel+stainless steel, silica gel+glass, if it is desired to realize that these should
With, it will usually realized with silane coupling agent pretreating substrates or to tackifier are added in sizing material.Production work can be increased using silane coupling agent
Sequence, and solvent volatilization can cause environmental pollution；And tackifier are added without there is above mentioned problem, simple to operate, adhesive property
It is reliable and stable, therefore as domestic and international study hotspot.
Common silane coupler（Such as KH560, KH570 etc.）Can be as a kind of tackifier, by being used alone or compounding
The bonding to different substrate materials is capable of achieving, but can there is the easy moisture absorption in such tackifier, become cloudy in sizing material storage, and bonding force declines
The shortcomings of.Chinese patent CN105001422 uses hydrogeneous phenyl silicone oil high and KH560 and KH570, by hydrosilylation,
A kind of tackifier for being bonded the plastics such as various metals and makrolon are synthesized, it is to avoid conventional common coupling agent is in add-on type silicon
The unstable and hypodynamic shortcoming of bonding is stored in rubber, but there is problems with the tackifier of this type：By routine
Metal die compression molding prepares the product that different substrate materials are combined with add-on type liquid silicon rubber, such as plastics+silicon rubber；Can then make
It is bonding with common metal mould into silicon rubber, it is unfavorable for the demoulding, so as to limit its range of application.
The silicon nitrogen heterocycles tackifier of the olefin-containing base of the synthesis of European patent EP 1002834, are capable of achieving to PC, PP and phenolic aldehyde
Deng the bonding of working of plastics, again can be from the metal die demoulding of chromium plating.But this tackifier can become cloudy in adding silicon rubber, glue is influenceed
The outward appearance and viscosity of material；Rubber mobility is deteriorated, processing difficulties.Simultaneously because the tackifier contain N element, the sulphur of sizing material can be influenceed
Change performance, therefore usually need high temperature（More than 100 DEG C）Vulcanization.
Therefore develop in a kind of product of different substrate materials and the rubber composition prepared for compression molding, both will not be with
Common metal mould is bonded, and the new tackifier that the outward appearance of processability and sizing material etc. is not interfered with again is significant.
The content of the invention
Present invention seek to address that the tackifier of prior art by compression molding for preparing different substrate materials and silicon rubber
Exist when in the product of combination：Silicon rubber is bonding with common metal mould, is unfavorable for the demoulding；Add tackifier influence sizing material
Outward appearance, processing difficulties, influence sizing material curability the problems such as, there is provided one kind will not be Nian Jie with common metal mould, and plus
Selective self bonding addition-type silicon rubber tackifier that work is good, do not influence sizing material outward appearance and preparation method thereof.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions；
A kind of selective self bonding add-on type liquid silicon rubber tackifier, the tackifier structural formula is as follows：
A kind of method for preparing above-mentioned selective self bonding add-on type liquid silicon rubber tackifier, methods described includes following steps
Suddenly：
（1）During 50~100 parts of containing hydrogen silicone oil and 10~20 parts of compounds of phenols containing vinyl benzene added into reaction bulb together, stir
Mix uniform, obtain reaction mass；
（2）At ambient temperature, to step（1）0.02~0.04 part of platinum catalyst is added in the reaction mass for obtaining, is continued
It is stirred until homogeneous；
（3）Step（2）Material is obtained to be reacted 4~6 hours under the conditions of 100~120 DEG C；
（4）After reaction terminates, 0.25~0.5 part of activated carbon is added, stirred 3~5 hours, and filtered, filtrate is standby；
（5）By step（4）At 120~150 DEG C, vacuum is to slough low point under the conditions of -0.098~-0.099MPa to gained filtrate
Sub- material, selective self bonding add-on type liquid silicon rubber tackifier are obtained final product to not there is cut to flow out.
Above-mentioned containing hydrogen silicone oil, the compound of phenols containing vinyl benzene and platinum catalyst are measured in parts by mass.
The mass fraction of the hydrogen of the containing hydrogen silicone oil is 0.60~1.50%.Preferably, the quality of the hydrogen of the containing hydrogen silicone oil
Fraction is 1.00~1.50%.The mass fraction of the hydrogen of containing hydrogen silicone oil is 1.00~1.50%, and reactivity is high, and adhesive strength is more
It is high.
Further, described phenols containing vinyl benzene compound is 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes.
Described platinum catalyst includes toluene solution, the vinylsiloxane chelate of chloroplatinic acid and the load of chloroplatinic acid
Type platinum catalyst.The wherein vinylsiloxane chelate of the preferential chloroplatinic acid of platinum catalyst, as of the invention containing vinyl
Phenol compound and the catalyst of containing hydrogen silicone oil reaction, its catalysis activity are higher.
The platinum catalyst platinum content is 20000~30000ppm.Ensure that the addition in later stage is appropriate without influenceing other
Performance and with preferable storage stability.
Described activated carbon is powdered.
In step（3）In, the reaction time is 5 hours；The reaction temperature is 100 DEG C.Can guarantee that what is obtained under the conditions of this
The quality of tackifier avoids the unnecessary time from wasting and energy waste simultaneously, and improve production efficiency reduces production cost.
The invention has the advantages that：
1st, when tackifier of the invention are added in liquid silastic and prepare add-on type liquid silicon rubber, liquid silastic will not become
Muddiness, does not influence outward appearance；After addition, liquid silastic viscosity B coefficent is small, can still flow freely, and curability keeps constant, Europe
The silicon nitrogen heterocycles tackifier of the olefin-containing base synthesized in continent patent EP1002834 are containing N element, it is necessary to by high temperature vulcanized ability
Bonding is realized, and tackifier of the invention can also solidify at ambient temperature, and energy consumption greatly reduces；Addition has increasing of the present invention
The add-on type liquid silicon rubber that stick is made and other different substrate materials（Plastics）When combination prepares product by compression molding, Gu
The selectivity bonding to the working of plastics such as PC, PP, PBT and nylon 6 is capable of achieving after change；And do not have bonding to metal die, so as to protect
Hold preferable release property.
Tackifier water white transparency of the invention, smell is low, stable storage, can be to conventional organic substrate, such as makrolon, Buddhist nun
Dragon, polypropylene and polybutylene terephthalate (PBT) etc. form preferably bonding.
2nd, the preparation method of tackifier of the invention is simple, and energy consumption is low, is adapted to large-scale production.
Specific embodiment
The present invention is illustrated with reference to specific embodiment.
Embodiment 1
A kind of method for preparing above-mentioned middle selective self bonding add-on type liquid silicon rubber tackifier, methods described includes following
Step：
（1）During 50 parts of containing hydrogen silicone oil and 10 parts of 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes added into reaction bulb together, stirring
Uniformly；
（2）0.02 part of platinum catalyst is added at ambient temperature, is continued to be stirred until homogeneous and is obtained mixed reactant；
（3）Step（2）Mixed reactant is obtained to be reacted 5 hours under the conditions of 120 DEG C；
（4）After reaction terminates, 0.25 part of activated carbon is added, stirred 3 hours, and filter；
（5）By gained filtrate at 120 DEG C, vacuum is to slough lower-molecular substance under the conditions of -0.098MPa, to not there is distillate flow
Go out to obtain final product.
Toluene solution of the platinum catalyst of the present embodiment from chloroplatinic acid.The hydrogeneous mass fraction of described containing hydrogen silicone oil is
0.60%。
Embodiment 2
A kind of method for preparing above-mentioned middle selective self bonding add-on type liquid silicon rubber tackifier, methods described includes following
Step：
（1）During 80 parts of containing hydrogen silicone oil and 15 parts of 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes added into reaction bulb together, stirring
Uniformly；
（2）0.02 part of platinum catalyst is added at ambient temperature, is continued to be stirred until homogeneous and is obtained mixed reactant；
（3）Step（2）Mixed reactant is obtained to be reacted 5 hours under the conditions of 130 DEG C；
（4）After reaction terminates, 0.4 part of activated carbon is added, stirred 3 hours, and filter；
（5）By gained filtrate at 120~150 DEG C, vacuum evaporates to slough lower-molecular substance under the conditions of -0.099MPa to not having
Distribute and obtain final product.
The platinum catalyst of the present embodiment selects the vinylsiloxane chelate of chloroplatinic acid, and described containing hydrogen silicone oil is hydrogeneous
Mass fraction is 1.50%.
Embodiment 3
A kind of method for preparing above-mentioned middle selective self bonding add-on type liquid silicon rubber tackifier, methods described includes following
Step：
（1）During 100 parts of containing hydrogen silicone oil and 13 parts of 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes added into reaction bulb together, stirring
Uniformly；
（2）0.03 part of platinum catalyst is added at ambient temperature, is continued to be stirred until homogeneous and is obtained mixed reactant；
（3）Step（2）Mixed reactant is obtained to be reacted 5 hours under the conditions of 100 DEG C；
（4）After reaction terminates, 0.5 part of activated carbon is added, stirred 5 hours, and filter；
（5）By gained filtrate at 140 DEG C, vacuum is to slough lower-molecular substance under the conditions of -0.099MPa, to not there is distillate flow
Go out to obtain final product.
Toluene solution of the platinum catalyst of the present embodiment from chloroplatinic acid.The hydrogeneous mass fraction of described containing hydrogen silicone oil is
0.80%。
Embodiment 4
A kind of method for preparing above-mentioned middle selective self bonding add-on type liquid silicon rubber tackifier, methods described includes following
Step：
（1）During 100 parts of containing hydrogen silicone oil and 10 parts of 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes added into reaction bulb together, stirring
Uniformly；
（2）0.04 part of platinum catalyst is added at ambient temperature, is continued to be stirred until homogeneous and is obtained mixed reactant；
（3）Step（2）Mixed reactant is obtained to be reacted 6 hours under the conditions of 110 DEG C；
（4）After reaction terminates, 0.35 part of activated carbon is added, stirred 4 hours, and filter；
（5）By gained filtrate at 150 DEG C, vacuum is to slough lower-molecular substance under the conditions of -0.098MPa, to not there is distillate flow
Go out to obtain final product.
Vinylsiloxane chelate of the platinum catalyst of the present embodiment from chloroplatinic acid.Described containing hydrogen silicone oil is hydrogeneous
Mass fraction is 1.00%.
Embodiment 5
A kind of method for preparing above-mentioned middle selective self bonding add-on type liquid silicon rubber tackifier, methods described includes following
Step：
（1）During 100 parts of containing hydrogen silicone oil and 20 parts of 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes added into reaction bulb together, stirring
Uniformly；
（2）0.02 part of platinum catalyst is added at ambient temperature, continues to be stirred until homogeneous to obtain mixed reactant；
（3）Step（2）The mixed reactant for obtaining reacts more than 4~6 hours under the conditions of 120 DEG C；
（4）After reaction terminates, 0.25 part of activated carbon is added, stirred 3 hours, and filter；
（5）By gained filtrate at 120 DEG C, vacuum flows out to slough lower-molecular substance under the conditions of -0.099MPa to not there is cut
Obtain final product.
Toluene solution of the platinum catalyst of the present embodiment from chloroplatinic acid.The hydrogeneous mass fraction of described containing hydrogen silicone oil is
1.50%。
Embodiment 6
A kind of method for preparing above-mentioned middle selective self bonding add-on type liquid silicon rubber tackifier, methods described includes following
Step：
（1）During 50 parts of containing hydrogen silicone oil and 15 parts of 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes added into reaction bulb together, stirring
Uniformly；
（2）0.02 part of platinum catalyst is added at ambient temperature, continues to be stirred until homogeneous；
（3）Step（2）Reacted more than 4 hours under the conditions of 120 DEG C；
（4）After reaction terminates, 0.45 part of activated carbon is added, stirred 5 hours, and filter；
（5）By gained filtrate at 140 DEG C, vacuum is to slough lower-molecular substance under the conditions of -0.098MPa, to not there is distillate flow
Go out to obtain final product.
The platinum catalyst of the present embodiment selects loaded platinum catalyst.The hydrogeneous mass fraction of described containing hydrogen silicone oil is
1.30%。
In above-described embodiment, it is more excellent that the platinum catalyst platinum content is controlled to 20000~30000ppm.Activated carbon is selected
Powdered active carbon.
In order to better illustrate the present invention, the tackifier that the present invention obtains embodiment 1-6 are used to prepare add-on type liquid
Silicon rubber, and add-on type liquid silicon rubber will be prepared for stainless steel, aluminium, plating straight-chromiun stainless steel, PC, nylon 6 and PBT substrate
It is bonded.
Add-on type liquid silicon rubber preparation method is as follows：100 parts of viscosity be 8000mPa.s, by CH2CH(CH3)2SiO1/2
In the dimethyl silicone polymer of chain link end-blocking, it is 200m to add 25 parts of specific surface areas2At the fume colloidal silica of/g, 6 parts of surfaces
Reason agent；Kneaded in kneader it is homogeneous after, depressurize it is lower 150 DEG C mixing 2h, be made into base-material.System in above-described embodiment 1-6 is taken respectively
Standby 1.5 parts of the tackifier for obtaining, are separately added into the base-materials for taking 100 parts of coolings, 2 parts of viscosity be 30mPa.s, by（CH3）3SiO1/2Chain
Section end-blocking（CH3）2SiO/CH3HSiO copolymers（Contain 18 SiH in 1 molecule）, 0.1 part of tetramethyl tetravinyl ring silicon
Oxygen alkane, 0.3 part of platinum mass fraction is 0.2% platinum-vinyl siloxane complex, mixes homogeneous, is made into add-on type liquid silicon rubber
Glue.
Contrast groups 1 and contrast groups 2 are set simultaneously, and contrast groups prepare add-on type liquid silicon with using the tackifier of embodiment 1-6
The contrast groups 1 that are distinguished as of rubber are not added with tackifier, and contrast groups 2 add tackifier KH570 and KH560, the add-on type liquid of contrast groups 1
It is prepared by silicon rubber：
In 100 parts of viscosity 8000mPa.s, by CH2CH(CH3)2SiO1/2In the dimethyl silicone polymer of chain link end-blocking, 25 parts are added
Specific surface area 200m2The fume colloidal silica of/g, 6 parts of surface conditioning agents；Kneaded in kneader it is homogeneous after, depressurize it is lower 150 DEG C
Mixing 2h, is made into base-material.In base-material after 100 parts of coolings, 2 parts of viscosity 30mPa.s of addition,（CH3）3SiO1/2Chain link end-blocking
（CH3）2SiO/CH3HSiO copolymers（Contain 18 SiH in 1 molecule）, 0.1 part of tetramethyl tetravinyl cyclosiloxane, 0.3
Part platinum mass fraction is 0.2% platinum-vinyl siloxane complex, mixes homogeneous, is made into add-on type liquid silicon rubber.
It is prepared by the add-on type liquid silicon rubber of contrast groups 2：
By 100 parts of viscosity 8000mPa.s, by CH2CH(CH3)2SiO1/2In the dimethyl silicone polymer of chain link end-blocking, 25 parts are added
Specific surface area 200m2The fume colloidal silica of/g, 6 parts of surface conditioning agents；Kneaded in kneader it is homogeneous after, depressurize it is lower 150 DEG C
Mixing 2h, is made into base-material.In base-material after 100 parts of coolings, 0.75 part of KH570,0.75 part of KH560,2 parts of viscosity are added
30mPa.s、（CH3）3SiO1/2Chain link end-blocking（CH3）2SiO/CH3HSiO copolymers（Contain 18 SiH in 1 molecule）, 0.1
Part tetramethyl tetravinyl cyclosiloxane, 0.3 part of platinum mass fraction is 0.2% platinum-vinyl siloxane complex, and mixing is equal
One, it is made into add-on type liquid silicon rubber.
Number in the present invention is mass parts.
Contrast groups 1, contrast groups 2 and existed using the add-on type liquid rubber that embodiment of the present invention 1-6 tackifier are prepared
Solidify 2h under the conditions of 120 DEG C, be bonded, its bonding result is carried out with stainless steel, aluminium, plating straight-chromiun stainless steel, PC, nylon 6 and PBT substrate
It is as shown in table 1 below：
Tackifier addition addition-type silicon rubber can be to conventional organic substrate as obtained in the data of upper table 1 can be seen that the present invention（Such as
Makrolon, nylon, polypropylene and polybutylene terephthalate (PBT) etc.）Preferably bonding is formed, and to common metal mould not
With bonding, preferable release property is kept；Can be used for addition-type silicon rubber to particular plastic have bonding and to common metal mould
Tool non-binding field.
Claims (10)
1. a kind of selective self bonding add-on type liquid silicon rubber tackifier, it is characterised in that：The tackifier structural formula is such as
Under：
In formula, m+n+x=5~15.
2. a kind of preparation method of selective self bonding add-on type liquid silicon rubber tackifier described in claim 1, its feature
It is：Methods described comprises the steps：
（1）During 50~100 parts of containing hydrogen silicone oil and 10~20 parts of compounds of phenols containing vinyl benzene added into reaction bulb together, stir
Mix uniform, obtain reaction mass；
（2）At ambient temperature, to step（1）0.02~0.04 part of platinum catalyst is added in the reaction mass for obtaining, is continued
It is stirred until homogeneous；
（3）Step（2）The material for obtaining reacts more than 4~6 hours under the conditions of 100~120 DEG C；
（4）After reaction terminates, activated carbon is added, stir and filter, filtrate is standby；
（5）By gained filtrate at 120~150 DEG C, vacuum is to slough lower-molecular substance under the conditions of -0.098~-0.099MPa,
Tackifier needed for obtaining.
3. the preparation method of a kind of selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：The mass fraction of the hydrogen of the containing hydrogen silicone oil is 0.60~1.50%.
4. the preparation method of a kind of selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：The mass fraction of the hydrogen of the containing hydrogen silicone oil is 1.00~1.50%.
5. a kind of method for preparing selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：The described compound of phenols containing vinyl benzene is 1- pi-allyl -3- methoxyl group -4- hydroxy benzenes.
6. the preparation method of a kind of selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：Described platinum catalyst is the toluene solution of chloroplatinic acid, the vinylsiloxane chelate of chloroplatinic acid and negative
Any one in load type platinum catalyst.
7. the preparation method of a kind of selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：The platinum catalyst is the vinylsiloxane chelate of chloroplatinic acid.
8. the preparation method of a kind of selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：The platinum content of the platinum catalyst is 20000~30000PPM.
9. the preparation method of a kind of selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：Described activated carbon is powdered.
10. the preparation method of a kind of selective self bonding add-on type liquid silicon rubber tackifier according to claim 2,
It is characterized in that：In step（3）In, the reaction time is 5 hours；The reaction temperature is 100 DEG C.
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| CN201611215986.XA CN106750319A (en) | 2016-12-26 | 2016-12-26 | A kind of selective self bonding add-on type liquid silicon rubber tackifier and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880585A (en) * | 2019-02-28 | 2019-06-14 | 浙江新安化工集团股份有限公司 | A kind of liquid silastic and preparation method thereof of pair of selective bonding of plastic basis material |
| CN112979961A (en) * | 2019-12-17 | 2021-06-18 | 中蓝晨光化工研究设计院有限公司 | Preparation method of macromolecular silicone rubber tackifier |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0776946A2 (en) * | 1995-11-29 | 1997-06-04 | Dow Corning Toray Silicone Co., Ltd. | Heat resistant polyorganosiloxane compositions |
| CN1303889A (en) * | 1999-12-20 | 2001-07-18 | 陶氏康宁东丽硅氧烷株式会社 | Composition of silicone rubber for insert moulding or double mould cavity moulding |
-
2016
- 2016-12-26 CN CN201611215986.XA patent/CN106750319A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0776946A2 (en) * | 1995-11-29 | 1997-06-04 | Dow Corning Toray Silicone Co., Ltd. | Heat resistant polyorganosiloxane compositions |
| CN1303889A (en) * | 1999-12-20 | 2001-07-18 | 陶氏康宁东丽硅氧烷株式会社 | Composition of silicone rubber for insert moulding or double mould cavity moulding |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880585A (en) * | 2019-02-28 | 2019-06-14 | 浙江新安化工集团股份有限公司 | A kind of liquid silastic and preparation method thereof of pair of selective bonding of plastic basis material |
| CN112979961A (en) * | 2019-12-17 | 2021-06-18 | 中蓝晨光化工研究设计院有限公司 | Preparation method of macromolecular silicone rubber tackifier |
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Application publication date: 20170531 |