CN105111443B - High transparency one-component condensed room temperature vulcanized silicone rubber composition and preparation method - Google Patents
High transparency one-component condensed room temperature vulcanized silicone rubber composition and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of high transparency one-component condensed room temperature vulcanized silicone rubber composition and preparation method, the composition is made of following components in parts by weight：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；Reinforced filling, 1~50 part；Crosslinking agent, 0.1~15 part；Catalyst, 0.1~5 part；Tackifier, 0.1~5 part.Light transmittance is up to more than 90% after product produced by the present invention cures, and mechanical strength is up to more than 2.0MPa after curing, and elongation at break is up to more than 300%.
Description
Technical field
The invention belongs to polymeric material field, and in particular to a kind of multiple reactionness end-group termination polymethyl-benzene base silica
Alkane, and it is related to the condensed room temperature vulcanized silicon of high transparency one-component comprising multiple reactionness end-group termination polymethylphenylsiloxane
Rubber composition and preparation method.
Background technology
Condensed room temperature vulcanized (hereinafter referred to as RTV-1) silicon rubber of one-component has the features such as easy to use, in-place molding,
There is excellent weatherability, resistance to ag(e)ing, high-low temperature resistant impact, and good electric property and biologically inert etc. after curing
Performance, is widely applied to aerospace, electric, automobile mechanical, the field such as health care and daily life.
Domestic common transparent RTV-1 silicon rubber is all to use α, alpha, omega-dihydroxy polydimethyl siloxane or alkane at present
Polymer based on epoxide end-blocking dimethyl silicone polymer, adds white carbon reinforcement, is configured to have certain printing opacity after curing
The silicon rubber of rate, such as Chinese patent CN102146208A, CN102408719A and CN103484056A.But poly dimethyl silicon
The index of refraction of oxygen alkane and white carbon difference is larger, and white carbon, which adds, can substantially reduce the light transmittance after product cures.Or pass through
α, the transparent organic filler of alpha, omega-dihydroxy polydimethyl siloxane cooperation are configured to the silicon rubber of higher light transmittance, such as Chinese patent
CN103525358A.But the hydroxy-end capped ladder-like polysiloxane therein used makes difficult, price as reinforcing agent
It is expensive, it is difficult to large-scale application.
The content of the invention
It is an object of the present invention to provide a kind of multiple reactionness end-group termination polymethylphenylsiloxane, its index of refraction exists
It is 1.4600 ± 0.0100 (index of refraction as described below is all tested under the conditions of 20 DEG C) at 20 DEG C, the viscosity at 25 DEG C is 1500
~500000cps (viscosity as described below is all tested under the conditions of 25 DEG C).
It is an object of the present invention to provide a kind of high transparency one-component condensed room temperature vulcanized silicone rubber composition.
It is a further object to provide a kind of high transparency one-component condensed room temperature vulcanized silicone rubber composition
Preparation method.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme：
A kind of multiple reactionness end-group termination polymethylphenylsiloxane, structure are as follows：
Wherein, a, b, c=0~1000, R1Selected from methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido,
One kind in formyloxy, acetoxyl group, propionyloxy, benzoyloxy group, R2Selected from methyl, ethyl, propyl group, vinyl, phenyl,
Methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido, formyloxy, acetoxyl group, propionyloxy, benzoyl
One kind in epoxide；The index of refraction of the multiple reactionness end-group termination polymethylphenylsiloxane is 1.46 ± 0.01, viscosity
For 1500~500000cps.
The present invention provides a kind of preparation method of multiple reactionness end-group termination polymethylphenylsiloxane, including following step
Suddenly：
Hydroxyl-terminated polymethylphenyl sioxane and crosslinking agent are added in reaction kettle, it is warming up to 40 under nitrogen protection~
100 DEG C, cyclohexanone oxime is added as catalyst, after reacting 2~8h, nitrogen protection is cooled to room temperature, and obtains multiple reactionness end group
It is spare to block polymethylphenylsiloxane.
A kind of high transparency one-component condensed room temperature vulcanized silicone rubber composition, is made of following components in parts by weight：
Component A：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；
Component B：Reinforced filling, 1~50 part；
Component C：Crosslinking agent, 0.1~15 part；
Component D：Catalyst, 0.1~5 part；
Component E：Tackifier, 0.1~5 part.
According to a preferred embodiment of the invention, the composition is made of following components in parts by weight：
Component A：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；
Component B：Reinforced filling, 10~50 parts；
Component C：Crosslinking agent, 3~15 parts；
Component D：Catalyst, 0.2~4 part；
Component E：Tackifier, 0.5~5 part.
More preferred embodiment according to the present invention, the composition are made of following components in parts by weight：
Component A：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；
Component B：Reinforced filling, 10~30 parts；
Component C：Crosslinking agent, 3~10 parts；
Component D：Catalyst, 0.5~3 part；
Component E：Tackifier, 1~4 part.
According to a particular embodiment of the invention, the reinforced filling is that specific surface area is 30~400m2The vapor phase method of/g
Silica.
According to a particular embodiment of the invention, the structural formula of the crosslinking agent is as follows：
Wherein R1Selected from methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, diacetylmonoxime
Base, formyloxy, acetoxyl group, propionyloxy, benzoyloxy group, R2Selected from methyl, ethyl, propyl group, vinyl, phenyl, methoxy
Base, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido, formyloxy, acetoxyl group, propionyloxy, benzoyl oxygen
Base.
According to a particular embodiment of the invention, the catalyst is tetraisopropyl titanate, tetra-n-butyl titanate, metatitanic acid four
One kind or several in double (ethyl acetoacetate) complexs of isobutyl ester, stannous octoate, dibutyl tin laurate, dibutyl tin
Kind.
According to a particular embodiment of the invention, the tackifier are γ-amine propyl trimethoxy silicane, γ-amine propyl group
Triethoxysilane, γ-methacryloxypropyl trimethoxy silane, γ-glycidoxypropyl group triethoxysilane,
β-amine ethyl-γ -- amine propyl trimethoxy silicane, β-amine ethyl-γ -- amine propyl-triethoxysilicane, γ-urea propyl group three
One or more in Ethoxysilane, γ-isocyanate group propyl-triethoxysilicane.
Present invention also offers a kind of preparation method of high transparency one-component condensed room temperature vulcanized silicone rubber composition,
Comprise the following steps：
Multiple reactionness end-group termination polymethylphenylsiloxane, reinforced filling are stirred into 0.5~5h in disperser, then
>=80 DEG C are heated to, is evacuated to P≤- 0.08MPa, 1~12 removes low molecule and moisture when small, then cold under nitrogen protection
But to room temperature, crosslinking agent, catalyst and tackifier are added, be finally stirred under vacuo 0.5~5 it is small when discharge.
The present invention is further illustrated below.
A kind of multiple reactionness end-group termination polymethylphenylsiloxane, structure are as follows：
Wherein, a, b, c=0~1000, R1Selected from methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido,
One kind in formyloxy, acetoxyl group, propionyloxy, benzoyloxy group, R2Selected from methyl, ethyl, propyl group, vinyl, phenyl,
Methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido, formyloxy, acetoxyl group, propionyloxy, benzoyl
One kind in epoxide；The index of refraction of the multiple reactionness end-group termination polymethylphenylsiloxane is 1.46 ± 0.01, viscosity
For 1500~500000cps.
In the present invention, the index of refraction of the multiple reactionness end-group termination polymethylphenylsiloxane is by benzene in structural formula
The content of base determines that viscosity is determined by a, the link quantity of b, c.Preferred embodiment according to the present invention, the multiple reactionness
The viscosity of end-group termination polymethylphenylsiloxane is 5000~200000cps；It is furthermore preferred that the multiple reactionness end group envelope
The viscosity for holding polymethylphenylsiloxane is 20000~80000cps.
The present invention provides a kind of preparation method of multiple reactionness end-group termination polymethylphenylsiloxane, including following step
Suddenly：
Hydroxyl-terminated polymethylphenyl sioxane and crosslinking agent are added in reaction kettle, it is warming up to 40 under nitrogen protection~
100 DEG C, cyclohexanone oxime is added as catalyst, after reacting 2~8h, nitrogen protection is cooled to room temperature, and obtains multiple reactionness end group
It is spare to block polymethylphenylsiloxane.
In above-mentioned preparation method, hydroxyl-terminated polymethylphenyl sioxane, crosslinking agent, the mass ratio of cyclohexanone oxime are
100：1~10：0.01~0.5.
In above-mentioned preparation method, the viscosity of the hydroxyl-terminated polymethylphenyl sioxane for 1000~
600000cps, index of refraction are 1.46 ± 0.02.According to a preferred embodiment of the invention, the hydroxy-end capped polymethyl-benzene base
The viscosity of siloxanes is 20000~80000, and index of refraction is 1.46 ± 0.015.In above-mentioned preparation method, the crosslinking
Agent is methyltrimethoxysilane, vinyl tributyl ketoximyl silane, three propionyloxy silane of ethyl, methyl triacetoxyl group silicon
Alkane.
A kind of high transparency one-component condensed room temperature vulcanized silicone rubber composition, is made of following components in parts by weight：
Component A：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；
Component B：Reinforced filling, 1~50 part；
Component C：Crosslinking agent, 0.1~15 part；
Component D：Catalyst, 0.1~5 part；
Component E：Tackifier, 0.1~5 part.
In the present invention, the reinforced filling is fumed silica, and specific surface area is 30~400m2.Vapor phase method
The index of refraction of silica is 1.46.
The index of refraction of the multiple reactionness end-group termination polymethylphenylsiloxane is 1.46 ± 0.01, if more reactions
Property end-group termination polymethylphenylsiloxane index of refraction be more than 1.47 or less than 1.45, then the index of refraction and be used as reinforced filling
Fumed silica index of refraction difference it is larger, can substantially reduce product cure after light transmittance.
The viscosity of the multiple reactionness end-group termination polymethylphenylsiloxane is 1500~500000cps, if more
The viscosity of reactive terminal group end-blocking polymethylphenylsiloxane is less than 1500cps, then sizing material cured strength is poor, workability
Decline；If the viscosity of multiple reactionness end-group termination polymethylphenylsiloxane is more than 500000cps, the product viscosity prepared
It is too big, it is difficult to construct；Therefore, the viscosity of multiple reactionness end-group termination polymethylphenylsiloxane is for 1500~500000cps
Suitably.Preferably, viscosity is 8000~100000cps；It is furthermore preferred that viscosity is 8000~80000cps.
In the present invention, if the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight, which uses, is less than 1 weight
The reinforced filling of part is measured, then the intensity after curing is low, without use value；If the multiple reactionness end-group termination of 100 parts by weight
Polymethylphenylsiloxane uses the reinforced filling more than 50 parts by weight, then the product viscosity prepared is too big, it is difficult to constructs；Cause
This, the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight is to close using the reinforced filling of 1~50 parts by weight
It is suitable.Preferably, the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight is filled out using the reinforcement of 10~50 parts by weight
Material；It is furthermore preferred that the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight uses the reinforcement of 10~30 parts by weight
Filler.
In the present invention, the crosslinking agent is that structure is
Wherein, R1Selected from methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido, formyloxy, second
Acyloxy, propionyloxy, benzoyloxy group, R2Selected from methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, ethyoxyl, the third oxygen
Base, phenoxy group, acetone oximido, butanone oximido, formyloxy, acetoxyl group, propionyloxy, benzoyloxy group.According to the present invention
Specific embodiment, the crosslinking agent are selected from methyltrimethoxysilane, phenyltrimethoxysila,e, phenyltriethoxy silane
Alkane, methyl tri acetylacetonate oximino silane, vinyl tributyl ketoximyl silane, propyl group triacetoxysilane, phenyl triacetoxyl group
Silane.
In the present invention, if the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight, which uses, is less than 0.1 weight
The crosslinking agent of part is measured, then fully crosslinked can not be cured；If the multiple reactionness end-group termination polymethyl-benzene base silica of 100 parts by weight
Alkane uses the crosslinking agent more than 15 parts by weight, then significantly extends hardening time, reduces workability；Therefore, 100 parts by weight is more
It is suitable that reactive terminal group, which blocks polymethylphenylsiloxane using the crosslinking agent of 0.1~15 parts by weight,.Preferably, 100 weight
The multiple reactionness end-group termination polymethylphenylsiloxane for measuring part uses the crosslinking agent of 3~15 parts by weight；It is furthermore preferred that 100 weights
The multiple reactionness end-group termination polymethylphenylsiloxane for measuring part uses the crosslinking agent of 3~10 parts by weight；It is furthermore preferred that 100 weights
The multiple reactionness end-group termination polymethylphenylsiloxane for measuring part uses the crosslinking agent of 3~8 parts by weight.
According to a particular embodiment of the invention, the catalyst is tetraisopropyl titanate, tetra-n-butyl titanate, metatitanic acid four
One kind or several in double (ethyl acetoacetate) complexs of isobutyl ester, stannous octoate, dibutyl tin laurate, dibutyl tin
Kind.In the present invention, if, if the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight use be less than 0.1
The catalyst of parts by weight, then without catalyst effect；If the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight
Using the catalyst more than 5 parts by weight, then curing rate is too fast, and product can not normal use；Therefore, 100 parts by weight is how anti-
Answering property end-group termination polymethylphenylsiloxane is suitable using the catalyst of 0.1~5 parts by weight.Preferably, 100 parts by weight
Multiple reactionness end-group termination polymethylphenylsiloxane use 0.2~4 parts by weight catalyst；It is furthermore preferred that 100 parts by weight
Multiple reactionness end-group termination polymethylphenylsiloxane use 0.5~3 parts by weight catalyst；It is furthermore preferred that 100 parts by weight
Multiple reactionness end-group termination polymethylphenylsiloxane use 1~3 parts by weight catalyst.
According to a particular embodiment of the invention, the tackifier are γ-amine propyl trimethoxy silicane, γ-amine propyl group
Triethoxysilane, γ-methacryloxypropyl trimethoxy silane, γ-glycidoxypropyl group triethoxysilane,
β-amine ethyl-γ -- amine propyl trimethoxy silicane, β-amine ethyl-γ -- amine propyl-triethoxysilicane, γ-urea propyl group three
One or more in Ethoxysilane, γ-isocyanate group propyl-triethoxysilicane.In the present invention, if 100 weights
The multiple reactionness end-group termination polymethylphenylsiloxane for measuring part uses the tackifier for being less than 0.1 parts by weight, then can not play increasing
Viscous effect；If the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight uses the thickening more than 5 parts by weight
Agent, then can influence the intensity after curing；Therefore, the multiple reactionness end-group termination polymethylphenylsiloxane of 100 parts by weight uses
The tackifier of 0.1~5 parts by weight are suitable.Preferably, the multiple reactionness end-group termination polymethyl-benzene base silica of 100 parts by weight
Alkane uses the tackifier of 0.5~5 parts by weight；It is furthermore preferred that the multiple reactionness end-group termination polymethyl-benzene base silica of 100 parts by weight
Alkane uses the tackifier of 1~4 parts by weight.
Present invention also offers a kind of preparation method of high transparency one-component condensed room temperature vulcanized silicone rubber composition,
Comprise the following steps：
Multiple reactionness end-group termination polymethylphenylsiloxane, reinforced filling are stirred into 0.5~5h in disperser, then
>=80 DEG C are heated to, is evacuated to P≤- 0.08MPa, 1~12 removes low molecule and moisture when small, then cold under nitrogen protection
But to room temperature, crosslinking agent, catalyst and tackifier are added, be finally stirred under vacuo 0.5~5 it is small when discharge.
The high transparency one-component condensed room temperature vulcanized silicone rubber composition of the present invention has carried out light transmittance, stretching by force
Degree, elongation at break etc. are tested.Light transmittance is directly tested using light transmittance haze detection instrument, and tensile strength and elongation at break are pressed
Tested according to GT/T 528-2009 methods.
Compared with prior art, the present invention with following beneficial effect：
1) present invention uses the multiple reactionness end-group termination polymethyl-benzene base silicon identical with reinforced filling white carbon index of refraction
Polymer based on oxygen alkane, light transmittance can be used for electric coating up to more than 90% after obtained product cures,
Optical element assembles, the field such as lamps and lanterns sealing bonding；And the preparation side of multiple reactionness end-group termination polymethylphenylsiloxane
Method is simple, and reaction condition is easily controllable.
2) using white carbon, obtained product has good thixotropy, and mechanical strength is reachable after curing as reinforced filling
More than 2.0MPa, elongation at break are bonded common materials good up to more than 300%.
3) raw material is made, and preparation method is workable, and production equipment is conventional equipment, and production process three wastes produce,
It is environmentally protective.
Brief description of the drawings：
Fig. 1 is the infrared spectrum of high transparency one-component condensed room temperature vulcanized silicone rubber composition prepared by embodiment 1
Figure.
Embodiment
With reference to the embodiment of the present invention, the invention will be further elaborated.
Embodiment 1
By the 80000cps hydroxyl-terminated polymethylphenyl sioxanes of 1000g indexs of refraction 1.4715 and 60g methyl trimethoxy oxygen
Base silane is added in reaction kettle, is heated to 80 DEG C under nitrogen protection, is added 2g cyclohexanone oximes, react 6h at 80 DEG C, rolled over
Light rate is that the multiple reactionness end-group termination polymethylphenylsiloxane of 1.4657 viscosity 78000cps is spare.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane according to the preparation method in patent CN102070785A from
System.
By 100 parts by weight multiple reactionness end-group termination polymethylphenylsiloxane obtained above, 10 weight part ratio surfaces
Product 150m2The hydrophily fumed silica of/g, which is placed in disperser, stirs 5h, is heated to 110 DEG C of temperature, be evacuated to-
0.085MPa, 1 removes low molecule and moisture when small, is then cooled to room temperature under nitrogen protection, adds 3 parts by weight methyl three
Methoxy silane, 2 parts by weight tetra-n-butyl titanates, 1 parts by weight γ-amine propyl trimethoxy silicane, it is small finally to vacuumize stirring 2
When after discharge and be sealed.
Fig. 1 shows the infrared of high transparency one-component condensed room temperature vulcanized silicone rubber composition manufactured in the present embodiment
Spectrogram.From figure 1 it appears that 2842cm-1For the absworption peak of silica methyl after end-blocking, 1590cm-1And 1414cm-1For silicon
The absworption peak of phenyl, 1256cm-1For the absworption peak of silicon methyl, 1084cm-1And 1009cm-1For the absworption peak of silica silicon, nothing
3400cm-1The absworption peak of left and right, illustrates that silicone hydroxyl has blocked and finishes.
Obtained RTV-1 silicon rubber surface drying time 55min, is fully cured rear light transmittance 96%, tensile strength 2.1MPa, breaks
Elongation 450% is split, after normality is stored 12 months, properties are with just preparing product without significant difference.
Embodiment 2
By the 20000cps hydroxyl-terminated polymethylphenyl sioxanes of 1000g indexs of refraction 1.4702 and three fourth of 30g vinyl
Ketoximinosilanes are added in reaction kettle, are heated to 40 DEG C under nitrogen protection, are added 1g cyclohexanone oximes, react 4h at 40 DEG C, obtain
Multiple reactionness end-group termination polymethylphenylsiloxane to the viscosity 19800cps that index of refraction is 1.4632 is spare.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane according to the preparation method in patent CN102070785A from
System.
By 100 parts by weight viscosity multiple reactionness end-group termination polymethylphenylsiloxane obtained above, 15 weight part ratios
Surface area 200m2The hydrophily fumed silica of/g, which is placed in disperser, stirs 3h, is heated to 120 DEG C of temperature, vacuumizes
Extremely -0.088MPa, 3 remove low molecule and moisture when small, are then cooled to room temperature under nitrogen protection, add 3 parts by weight second
Alkenyl tributanoximo silane, 1 parts by weight methyl tri acetylacetonate oxime silane, 0.1 parts by weight dibutyl tin laurate, 0.5 weight
Part γ-amine propyl trimethoxy silicane, finally vacuumize stirring 0.5 it is small when after discharge and be sealed.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 35min, is fully cured rear light transmittance 94%, tensile strength
2.3MPa, elongation at break 330%, after normality is stored 12 months, properties are with just preparing product without significant difference.
Embodiment 3
By the 5000cps hydroxyl-terminated polymethylphenyl sioxanes of 1000g indexs of refraction 1.4687 and three propionyl oxygen of 40g ethyls
Base silane is added in reaction kettle, is heated to 40 DEG C under nitrogen protection, is added 0.1g cyclohexanone oximes, react 2h at 40 DEG C, obtain
Index of refraction is that the multiple reactionness end-group termination polymethylphenylsiloxane of 1.4587 viscosity 4800cps is spare.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane according to the preparation method in patent CN102070785A from
System.
By the multiple reactionness end-group termination polymethylphenylsiloxane of the above-mentioned preparation of 100 parts by weight, 12 weight part ratio surfaces
Product 380m2The hydrophily fumed silica of/g, which is placed in disperser, stirs 0.5h, is heated to 80 DEG C of temperature, be evacuated to-
0.090MPa, 1 removes low molecule and moisture when small, is then cooled to room temperature under nitrogen protection, adds 3 parts by weight propyl group three
Acetoxylsilane, 1 parts by weight phenyl triacetoxysilane, 0.1 parts by weight of octanoic acid stannous, 1 parts by weight β-amine ethyl-γ --
Amine propyl-triethoxysilicane, finally vacuumize stirring 1 it is small when after discharge and be sealed.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 75min, is fully cured rear light transmittance 92%, tensile strength
2.3MPa, elongation at break 370%, after normality is stored 12 months, properties are with just preparing product without significant difference.
Embodiment 4
By the 120000cps hydroxyl-terminated polymethylphenyl sioxanes of 1000g indexs of refraction 1.4714 and 40g methyl trimethoxy oxygen
Base silane is added in reaction kettle, is heated to 70 DEG C under nitrogen protection, is added 4g cyclohexanone oximes, react 6h at 70 DEG C, rolled over
Light rate is that the multiple reactionness end-group termination polymethylphenylsiloxane of 1.4668 viscosity 108000cps is spare.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane according to the preparation method in patent CN102070785A from
System.
By the multiple reactionness end-group termination polymethylphenylsiloxane of the above-mentioned preparation of 100 parts by weight, 10 weight part ratio surfaces
Product 50m2The hydrophily fumed silica of/g, which is placed in disperser, stirs 0.5h, is heated to 90 DEG C of temperature, be evacuated to-
0.080MPa, 6 remove low molecule and moisture when small, are then cooled to room temperature under nitrogen protection, add 3 parts by weight phenyl three
Ethoxysilane, 0.2 parts by weight dibutyl tin laurate, 0.5 parts by weight γ-urea propyl-triethoxysilicane, finally takes out true
Discharge and be sealed after when sky stirring 3 is small.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 45min, is fully cured rear light transmittance 96%, tensile strength
2.1MPa, elongation at break 550%, after normality is stored 12 months, properties are with just preparing product without significant difference.
Comparative example 1
By the 80000cps hydroxyl endblocked polydimethylsiloxanes of 1000g indexs of refraction 1.4067 and 40g methyl trimethoxy epoxides
Silane is added in reaction kettle, is heated to 70 DEG C under nitrogen protection, is added 2g cyclohexanone oximes, react 6h at 70 DEG C, obtain refractive power
Rate is that the multiple reactionness end-group termination polymethylphenylsiloxane of 1.4032 viscosity 77800cps is spare.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane according to the preparation method in patent CN102070785A from
System.
By the how alkoxy end-capped dimethyl silicone polymer of the above-mentioned preparation of 100 parts by weight, 10 weight part ratio surface areas
150m2The hydrophily fume colloidal silica of/g stirs 1h in disperser, and 120 DEG C of heating-up temperature, is evacuated to -0.085MPa,
1h removes low molecule and moisture, is cooled to room temperature under nitrogen protection, adds 3 parts by weight methyltrimethoxysilane, 1 parts by weight titanium
Sour four isobutyl esters, 1 parts by weight γ-amine propyl trimethoxy silicane are vacuumized to discharge after stirring 0.5h and are sealed.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 25min, is fully cured rear light transmittance 55%, tensile strength
1.7MPa, elongation at break 450%.
Comparative example 2
By the 20000cps hydroxyl endblocked polydimethylsiloxanes of 1000g indexs of refraction 1.4466 and 30g methyl triacetyl oxygen
Base silane is added in reaction kettle, is heated to 40 DEG C under nitrogen protection, is added 0.1g cyclohexanone oximes, react 2h at 40 DEG C, obtain
Index of refraction is that the multiple reactionness end-group termination polymethylphenylsiloxane of 1.4132 viscosity 18800cps is spare.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane according to the preparation method in patent CN102070785A from
System.
100 parts by weight are stained with to the multiple reactionness end-group termination polymethylphenylsiloxane for stating preparation, 15 weight part ratio tables
Area 200m2The hydrophobic fumed white carbon of/g stirs 2h in disperser, 90 DEG C of heating-up temperature, be evacuated to-
0.090MPa, 1h remove low molecule and moisture, are cooled to room temperature under nitrogen protection, add 6 parts by weight phenyltrimethoxysila,es,
0.2 parts by weight dibutyl tin laurate, 0.5 parts by weight γ-urea propyl-triethoxysilicane, discharges after vacuumizing stirring 3h
It is sealed.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 35min, light transmittance 75%, tensile strength 2.2MPa, fracture are stretched
Long rate 250%.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modifications and embodiment, these modifications and embodiment will fall in principle disclosed in the present application
Within scope and spirit.
Claims (9)
1. a kind of multiple reactionness end-group termination polymethylphenylsiloxane, it is characterised in that its structure is as follows：
Wherein, a, b, c=0~1000, R1Selected from methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido, first
One kind in acyloxy, acetoxyl group, propionyloxy, benzoyloxy group,
R2Selected from methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone
One kind in oximido, formyloxy, acetoxyl group, propionyloxy, benzoyloxy group；
The preparation method of the multiple reactionness end-group termination polymethylphenylsiloxane, comprises the following steps：Will be hydroxy-end capped
Polymethylphenylsiloxane is added in reaction kettle with crosslinking agent, and 40~100 DEG C are warming up under nitrogen protection, is added cyclohexanone oxime and is made
For catalyst, after reacting 2~8h, nitrogen protection is cooled to room temperature, and obtains multiple reactionness end-group termination polymethylphenylsiloxane
It is spare；
Wherein hydroxyl-terminated polymethylphenyl sioxane, crosslinking agent, the mass ratio of cyclohexanone oxime are 100：1~10：0.01~
0.5；
The viscosity of the hydroxyl-terminated polymethylphenyl sioxane is 20000~80000cps, index of refraction for 1.46 ±
0.015；
The crosslinking agent is methyltrimethoxysilane, vinyl tributyl ketoximyl silane, three propionyloxy silane of ethyl, first
Base triacetoxysilane；
The index of refraction of the multiple reactionness end-group termination polymethylphenylsiloxane is 1.46 ± 0.01 at 20 DEG C, at 25 DEG C
Under viscosity be 8000~80000cps.
A kind of 2. high transparency one-component of the multiple reactionness end-group termination polymethylphenylsiloxane comprising described in claim 1
Condensed room temperature vulcanized silicone rubber composition, it is characterised in that the composition is made of following components in parts by weight：
Component A：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；
Component B：Reinforced filling, 1~50 part；
Component C：Crosslinking agent, 0.1~15 part；
Component D：Catalyst, 0.1~5 part；
Component E：Tackifier, 0.1~5 part.
3. high transparency one-component condensed room temperature vulcanized silicone rubber composition according to claim 2, it is characterised in that
The composition is made of following components in parts by weight：
Component A：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；
Component B：Reinforced filling, 10~50 parts；
Component C：Crosslinking agent, 3~15 parts；
Component D：Catalyst, 0.2~4 part；
Component E：Tackifier, 0.5~5 part.
4. high transparency one-component condensed room temperature vulcanized silicone rubber composition according to claim 2, it is characterised in that
The composition is made of following components in parts by weight：
Component A：Multiple reactionness end-group termination polymethylphenylsiloxane, 100 parts；
Component B：Reinforced filling, 10~30 parts；
Component C：Crosslinking agent, 3~10 parts；
Component D：Catalyst, 0.5~3 part；
Component E：Tackifier, 1~4 part.
5. high transparency one-component condensed room temperature vulcanized silicone rubber composition according to claim 2, it is characterised in that
The reinforced filling is that specific surface area is 30~400m2The fumed silica of/g.
6. high transparency one-component condensed room temperature vulcanized silicone rubber composition according to claim 2, it is characterised in that
The structural formula of the crosslinking agent is as follows：
Wherein, R1Selected from methoxyl group, ethyoxyl, propoxyl group, phenoxy group, acetone oximido, butanone oximido, formyloxy, acetyl oxygen
Base, propionyloxy, benzoyloxy group, R2Selected from methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, ethyoxyl, propoxyl group, benzene
Epoxide, acetone oximido, butanone oximido, formyloxy, acetoxyl group, propionyloxy, benzoyloxy group.
7. high transparency one-component condensed room temperature vulcanized silicone rubber composition according to claim 2, it is characterised in that
The catalyst is tetraisopropyl titanate, tetra-n-butyl titanate, tetrabutyl titanate, stannous octoate, di lauric dibutyl
One or more in double (ethyl acetoacetate) complexs of tin, dibutyl tin.
8. high transparency one-component condensed room temperature vulcanized silicone rubber composition according to claim 2, it is characterised in that
The tackifier are γ-amine propyl trimethoxy silicane, γ-amine propyl-triethoxysilicane, γ-methacryloxy third
Base trimethoxy silane, γ-glycidoxypropyl group triethoxysilane, β-amine ethyl-γ -- amine propyl trimethoxy silicane,
β-amine ethyl-γ -- amine propyl-triethoxysilicane, γ-urea propyl-triethoxysilicane, γ-three second of isocyanate group propyl group
One or more in oxysilane.
9. the preparation side of claim 2-8 any one of them high transparency one-component condensed room temperature vulcanized silicone rubber compositions
Method, it is characterised in that comprise the following steps：
Multiple reactionness end-group termination polymethylphenylsiloxane, reinforced filling are stirred into 0.5~5h in disperser, then heated
To >=80 DEG C, P≤- 0.08MPa is evacuated to, 1~12 removes low molecule and moisture when small, is then cooled under nitrogen protection
Room temperature, adds crosslinking agent, catalyst and tackifier, be finally stirred under vacuo 0.5~5 it is small when discharge.
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| CN106190012B (en) * | 2016-08-08 | 2019-02-05 | 广州机械科学研究院有限公司 | A kind of transparent high-intensitive Self-leveling piptonychia alcohol type single-component organic silicon glue and preparation method thereof |
| CN106519246B (en) * | 2016-11-21 | 2022-03-25 | 成都硅宝科技股份有限公司 | Polyalkoxy-terminated polysiloxanes and method for the production thereof |
| CN109929247A (en) * | 2017-12-18 | 2019-06-25 | 中蓝晨光化工研究设计院有限公司 | A kind of organosilicon coating glue and preparation method for rail traffic |
| CN109232894B (en) * | 2018-09-21 | 2021-04-06 | 广州天宸高新材料有限公司 | Methoxy-terminated methylphenyl polysiloxane resin, organic silicon coating adhesive, preparation method and application |
| CN111925529B (en) * | 2020-06-10 | 2022-04-12 | 湖北航天化学技术研究所 | POSS (polyhedral oligomeric silsesquioxane) modified silane terminated liquid fluororubber, adhesive and preparation method |
| CN113337174B (en) * | 2021-06-15 | 2022-02-11 | 常州大学 | Preparation method of super-hydrophobic coating with high light transmittance and high haze |
| CN115746305B (en) * | 2022-11-17 | 2023-09-19 | 万华化学集团股份有限公司 | Phenyl polysiloxane and preparation method and application thereof |
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| US5266631A (en) * | 1991-06-13 | 1993-11-30 | Shin-Etsu Chemical Co., Ltd. | Process of producing room temperature curable organopolysiloxane composition |
| US20040002571A1 (en) * | 2002-07-01 | 2004-01-01 | Shin-Etsu Chemical Co. Ltd. | Room temperature curable organopolysiloxane compositions |
| CN103408941A (en) * | 2013-08-23 | 2013-11-27 | 山东永安胶业有限公司 | Transparent dealcoholized single-component room temperature vulcanized silicone rubber and preparation method thereof |
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| US5266631A (en) * | 1991-06-13 | 1993-11-30 | Shin-Etsu Chemical Co., Ltd. | Process of producing room temperature curable organopolysiloxane composition |
| US20040002571A1 (en) * | 2002-07-01 | 2004-01-01 | Shin-Etsu Chemical Co. Ltd. | Room temperature curable organopolysiloxane compositions |
| CN103408941A (en) * | 2013-08-23 | 2013-11-27 | 山东永安胶业有限公司 | Transparent dealcoholized single-component room temperature vulcanized silicone rubber and preparation method thereof |
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