CN105111443A - High-transmittance single-component condensed room-temperature-vulcanized silicone rubber composition and preparation method thereof - Google Patents
High-transmittance single-component condensed room-temperature-vulcanized silicone rubber composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-transmittance single-component condensed room-temperature-vulcanized silicone rubber composition and a preparation method thereof. The composition comprises, by weight, 100 parts of multi-reactive terminal group terminated poly(methyl phenyl siloxane), 1-50 parts of a reinforcing filler, 0.1-15 parts of a cross-linking agent, 0.1-5 parts of a catalyst, and 0.1-5 parts of a tackifier. After being cured, the composition is higher than 90% in light transmittance, higher than 2.0Mpa in mechanical strength and higher than 300% in elongation at break.
Description
Technical field
The invention belongs to polymeric material field, be specifically related to a kind of multiple reactionness end-group termination PSI, and relate to the high transmission rate single-component condensed room temperature vulcanized silicone rubber composition and preparation method that comprise multiple reactionness end-group termination PSI.
Background technology
Single-component condensed room temperature vulcanized (hereinafter referred to as RTV-1) silicon rubber has easy to use, the features such as in-place mo(u)lding, there is after solidification excellent weathering resistance, ageing resistance, high-low temperature resistant impact, and the performance such as good electric property and biologically inert, be applied in aerospace widely, electric, automobile mechanical, the field such as health care and daily life.
Current domestic common transparent RTV-1 silicon rubber is all use α, polymkeric substance based on alpha, omega-dihydroxy polydimethyl siloxane or alkoxy end-capped polydimethylsiloxane, add white carbon black reinforcement, there is after being mixed with solidification the silicon rubber of certain transmittance, as Chinese patent CN102146208A, CN102408719A and CN103484056A.But the refractive index of polydimethylsiloxane and white carbon black difference is comparatively large, white carbon black add membership obviously reduce products solidifying after transmittance.Or by α, alpha, omega-dihydroxy polydimethyl siloxane coordinates transparent organic filler to be mixed with the silicon rubber of higher light transmittance, as Chinese patent CN103525358A.But the hydroxy-end capped ladder-like polysiloxane of use wherein makes difficulty as strengthening agent, expensive, is difficult to large-scale application.
Summary of the invention
An object of the present invention is to provide a kind of multiple reactionness end-group termination PSI, its refractive index is 1.4600 ± 0.0100 (the following stated refractive index is all tested under 20 DEG C of conditions) at 20 DEG C, and the viscosity at 25 DEG C is 1500 ~ 500000cps (the following stated viscosity is all tested under 25 DEG C of conditions).
An object of the present invention is to provide a kind of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition.
Another object of the present invention is to provide a kind of preparation method of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
A kind of multiple reactionness end-group termination PSI, structure is as follows:
wherein, a, b, c=0 ~ 1000, R
1be selected from the one in methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group, R
2be selected from the one in methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group; The refractive index of described multiple reactionness end-group termination PSI is 1.46 ± 0.01, and viscosity is 1500 ~ 500000cps.
The invention provides a kind of preparation method of multiple reactionness end-group termination PSI, comprise the following steps:
Hydroxyl-terminated polymethylphenyl sioxane and linking agent are added in reactor; be warming up to 40 ~ 100 DEG C under nitrogen protection, add cyclohexanone-oxime as catalyzer, after reaction 2 ~ 8h; nitrogen protection is cooled to room temperature, obtains multiple reactionness end-group termination PSI for subsequent use.
A kind of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition, is made up of the component of following weight parts:
Component A: multiple reactionness end-group termination PSI, 100 parts;
B component: reinforced filling, 1 ~ 50 part;
Component C: linking agent, 0.1 ~ 15 part;
Component D: catalyzer, 0.1 ~ 5 part;
Component E: tackifier, 0.1 ~ 5 part.
According to a preferred embodiment of the invention, described composition is made up of the component of following weight parts:
Component A: multiple reactionness end-group termination PSI, 100 parts;
B component: reinforced filling, 10 ~ 50 parts;
Component C: linking agent, 3 ~ 15 parts;
Component D: catalyzer, 0.2 ~ 4 part;
Component E: tackifier, 0.5 ~ 5 part.
According to more preferred embodiment of the present invention, described composition is made up of the component of following weight parts:
Component A: multiple reactionness end-group termination PSI, 100 parts;
B component: reinforced filling, 10 ~ 30 parts;
Component C: linking agent, 3 ~ 10 parts;
Component D: catalyzer, 0.5 ~ 3 part;
Component E: tackifier, 1 ~ 4 part.
According to a particular embodiment of the invention, described reinforced filling is specific surface area is 30 ~ 400m
2the fumed silica of/g.
According to a particular embodiment of the invention, the structural formula of described linking agent is as follows:
wherein R
1be selected from methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group, R
2be selected from methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group.
According to a particular embodiment of the invention, described catalyzer is one or more in titanium isopropylate, tetra-n-butyl titanate, tetrabutyl titanate, stannous octoate, dibutyl tin laurate, two (methyl aceto acetate) title complex of dibutyl tin.
According to a particular embodiment of the invention, described tackifier are γ-amine propyl trimethoxy silicane, γ-amine propyl-triethoxysilicane, γ-methacryloxypropyl trimethoxy silane, γ-glycidoxypropyl group triethoxyl silane, β-amine ethyl-γ--amine propyl trimethoxy silicane, β-amine ethyl-γ--one or more in amine propyl-triethoxysilicane, γ-urea propyl-triethoxysilicane, γ-isocyanate group propyl-triethoxysilicane.
Present invention also offers a kind of preparation method of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition, comprise the following steps:
Multiple reactionness end-group termination PSI, reinforced filling are stirred 0.5 ~ 5h in decollator; then be heated to >=80 DEG C; be evacuated to P≤-0.08MPa; within 1 ~ 12 hour, remove low molecule and moisture; then room temperature is cooled under nitrogen protection; add linking agent, catalyzer and tackifier again, be finally uniformly mixed discharging in 0.5 ~ 5 hour under vacuo.
The present invention is further illustrated below.
A kind of multiple reactionness end-group termination PSI, structure is as follows:
wherein, a, b, c=0 ~ 1000, R
1be selected from the one in methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group, R
2be selected from the one in methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group; The refractive index of described multiple reactionness end-group termination PSI is 1.46 ± 0.01, and viscosity is 1500 ~ 500000cps.
In the present invention, the refractive index of described multiple reactionness end-group termination PSI is determined by the content of phenyl in structural formula, and viscosity is determined by the link quantity of a, b, c.According to the preferred embodiment of the invention, the viscosity of described multiple reactionness end-group termination PSI is 5000 ~ 200000cps; Preferred, the viscosity of described multiple reactionness end-group termination PSI is 20000 ~ 80000cps.
The invention provides a kind of preparation method of multiple reactionness end-group termination PSI, comprise the following steps:
Hydroxyl-terminated polymethylphenyl sioxane and linking agent are added in reactor; be warming up to 40 ~ 100 DEG C under nitrogen protection, add cyclohexanone-oxime as catalyzer, after reaction 2 ~ 8h; nitrogen protection is cooled to room temperature, obtains multiple reactionness end-group termination PSI for subsequent use.
In above-mentioned preparation method, the mass ratio of hydroxyl-terminated polymethylphenyl sioxane, linking agent, cyclohexanone-oxime is 100:1 ~ 10:0.01 ~ 0.5.
In above-mentioned preparation method, the viscosity of described hydroxyl-terminated polymethylphenyl sioxane is 1000 ~ 600000cps, and refractive index is 1.46 ± 0.02.According to a preferred embodiment of the invention, the viscosity of described hydroxyl-terminated polymethylphenyl sioxane is 20000 ~ 80000, and refractive index is 1.46 ± 0.015.In above-mentioned preparation method, described linking agent is methyltrimethoxy silane, vinyl tributyl ketoximyl silane, ethyl three propionyloxy silane, methyl triacetoxysilane.
A kind of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition, is made up of the component of following weight parts:
Component A: multiple reactionness end-group termination PSI, 100 parts;
B component: reinforced filling, 1 ~ 50 part;
Component C: linking agent, 0.1 ~ 15 part;
Component D: catalyzer, 0.1 ~ 5 part;
Component E: tackifier, 0.1 ~ 5 part.
In the present invention, described reinforced filling is fumed silica, and specific surface area is 30 ~ 400m
2.The refractive index of fumed silica is 1.46.
The refractive index of described multiple reactionness end-group termination PSI is 1.46 ± 0.01, if the refractive index of multiple reactionness end-group termination PSI is greater than 1.47 or be less than 1.45, then this refractive index differs comparatively large with the refractive index of the fumed silica as reinforced filling, obviously can reduce the transmittance after products solidifying.
The viscosity of described multiple reactionness end-group termination PSI is 1500 ~ 500000cps, if the viscosity of multiple reactionness end-group termination PSI is less than 1500cps, then sizing material cured strength is poor, and workability declines; If the viscosity of multiple reactionness end-group termination PSI is greater than 500000cps, then the product viscosity prepared is too large, is difficult to construction; Therefore, the viscosity of multiple reactionness end-group termination PSI is 1500 ~ 500000cps is suitable.Preferably, viscosity is 8000 ~ 100000cps; Preferred, viscosity is 8000 ~ 80000cps.
In the present invention, if the multiple reactionness end-group termination PSI of 100 weight parts uses the reinforced filling being less than 1 weight part, then the intensity after solidification is low, does not have use value; If the multiple reactionness end-group termination PSI of 100 weight parts uses the reinforced filling being greater than 50 weight parts, then the product viscosity prepared is too large, is difficult to construction; Therefore, the multiple reactionness end-group termination PSI of 100 weight parts uses the reinforced filling of 1 ~ 50 weight part to be suitable.Preferably, the multiple reactionness end-group termination PSI of 100 weight parts uses the reinforced filling of 10 ~ 50 weight parts; Preferred, the multiple reactionness end-group termination PSI of 100 weight parts uses the reinforced filling of 10 ~ 30 weight parts.
In the present invention, described linking agent is structure
Wherein, R
1be selected from methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group, R
2be selected from methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group.According to a particular embodiment of the invention, described linking agent is selected from methyltrimethoxy silane, phenyltrimethoxysila,e, phenyl triethoxysilane, methyl tri acetylacetonate oximino silane, vinyl tributyl ketoximyl silane, propyl group triacetoxysilane, phenyl triacetoxysilane.
In the present invention, if the multiple reactionness end-group termination PSI of 100 weight parts uses be less than the linking agent of 0.1 weight part, then cannot crosslinking curing completely; If the multiple reactionness end-group termination PSI of 100 weight parts uses the linking agent being greater than 15 weight parts, then significantly extend set time, reduce workability; Therefore, the multiple reactionness end-group termination PSI of 100 weight parts uses the linking agent of 0.1 ~ 15 weight part to be suitable.Preferably, the multiple reactionness end-group termination PSI of 100 weight parts uses the linking agent of 3 ~ 15 weight parts; Preferred, the multiple reactionness end-group termination PSI of 100 weight parts uses the linking agent of 3 ~ 10 weight parts; Preferred, the multiple reactionness end-group termination PSI of 100 weight parts uses the linking agent of 3 ~ 8 weight parts.
According to a particular embodiment of the invention, described catalyzer is one or more in titanium isopropylate, tetra-n-butyl titanate, tetrabutyl titanate, stannous octoate, dibutyl tin laurate, two (methyl aceto acetate) title complex of dibutyl tin.In the present invention, if, if the multiple reactionness end-group termination PSI of 100 weight parts uses the catalyzer being less than 0.1 weight part, then catalyst-free effect; If the multiple reactionness end-group termination PSI of 100 weight parts uses the catalyzer being greater than 5 weight parts, then curing speed is too fast, and product cannot normally use; Therefore, the multiple reactionness end-group termination PSI of 100 weight parts uses the catalyzer of 0.1 ~ 5 weight part to be suitable.Preferably, the multiple reactionness end-group termination PSI of 100 weight parts uses the catalyzer of 0.2 ~ 4 weight part; Preferred, the multiple reactionness end-group termination PSI of 100 weight parts uses the catalyzer of 0.5 ~ 3 weight part; Preferred, the multiple reactionness end-group termination PSI of 100 weight parts uses the catalyzer of 1 ~ 3 weight part.
According to a particular embodiment of the invention, described tackifier are γ-amine propyl trimethoxy silicane, γ-amine propyl-triethoxysilicane, γ-methacryloxypropyl trimethoxy silane, γ-glycidoxypropyl group triethoxyl silane, β-amine ethyl-γ--amine propyl trimethoxy silicane, β-amine ethyl-γ--one or more in amine propyl-triethoxysilicane, γ-urea propyl-triethoxysilicane, γ-isocyanate group propyl-triethoxysilicane.In the present invention, if the multiple reactionness end-group termination PSI of 100 weight parts uses the tackifier being less than 0.1 weight part, then viscosifying action cannot be played; If the multiple reactionness end-group termination PSI of 100 weight parts uses the tackifier being greater than 5 weight parts, then can affect the intensity after solidification; Therefore, the multiple reactionness end-group termination PSI of 100 weight parts uses the tackifier of 0.1 ~ 5 weight part to be suitable.Preferably, the multiple reactionness end-group termination PSI of 100 weight parts uses the tackifier of 0.5 ~ 5 weight part; Preferred, the multiple reactionness end-group termination PSI of 100 weight parts uses the tackifier of 1 ~ 4 weight part.
Present invention also offers a kind of preparation method of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition, comprise the following steps:
Multiple reactionness end-group termination PSI, reinforced filling are stirred 0.5 ~ 5h in decollator; then be heated to >=80 DEG C; be evacuated to P≤-0.08MPa; within 1 ~ 12 hour, remove low molecule and moisture; then room temperature is cooled under nitrogen protection; add linking agent, catalyzer and tackifier again, be finally uniformly mixed discharging in 0.5 ~ 5 hour under vacuo.
High transmission rate single-component condensed room temperature vulcanized silicone rubber composition of the present invention has carried out the tests such as transmittance, tensile strength, elongation at break.Transmittance adopts transmittance haze detection instrument directly to test, and tensile strength and elongation at break are tested according to GT/T528-2009 method.
The present invention compared with prior art, has following beneficial effect:
1) polymkeric substance based on the multiple reactionness end-group termination PSI that employing of the present invention is identical with reinforced filling white carbon black refractive index, after obtained products solidifying, transmittance is up to more than 90%, may be used for electric coating, the fields such as optical element is assembled, and light fixture sealing is bonding; And the preparation method of multiple reactionness end-group termination PSI is simple, reaction conditions is easy to control.
2) use white carbon black as reinforced filling, obtained product has good thixotropy, and after solidification, mechanical strength can reach more than 2.0MPa, and elongation at break can reach more than 300%, well bonding to common materials.
3) raw material obtains, and preparation method is workable, and production unit is conventional equipment, and production process is produced without the three wastes, environmental protection.
Accompanying drawing illustrates:
Fig. 1 is the infrared spectrogram of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition prepared by embodiment 1.
Embodiment
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1
The 80000cps hydroxyl-terminated polymethylphenyl sioxane of 1000g refractive index 1.4715 and 60g methyltrimethoxy silane are added in reactor; 80 DEG C are heated under nitrogen protection; add 2g cyclohexanone-oxime; at 80 DEG C, react 6h, obtaining refractive index is that the multiple reactionness end-group termination PSI of the viscosity 78000cps of 1.4657 is for subsequent use.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane is according to the preparation method's self-control in patent CN102070785A.
By the above-mentioned obtained multiple reactionness end-group termination PSI of 100 weight part, 10 weight part ratio surface-area 150m
2the wetting ability fumed silica of/g is placed in decollator and stirs 5h; be heated to temperature 110 DEG C; be evacuated to-0.085MPa; within 1 hour, remove low molecule and moisture; then be cooled to room temperature under nitrogen protection, then add 3 weight part methyltrimethoxy silanes, 2 weight part tetra-n-butyl titanates; 1 weight part γ-amine propyl trimethoxy silicane, finally vacuumizes stirring discharging sealing preservation after 2 hours.
Fig. 1 shows the infrared spectrogram of high transmission rate single-component condensed room temperature vulcanized silicone rubber composition prepared by the present embodiment.As can be seen from Figure 1,2842cm
-1for the absorption peak of silica methyl after end-blocking, 1590cm
-1and 1414cm
-1for the absorption peak of silicon phenyl, 1256cm
-1for the absorption peak of silicon methyl, 1084cm
-1and 1009cm
-1for the absorption peak of silica silicon, without 3400cm
-1the absorption peak of left and right, silicone hydroxyl is described, and end-blocking is complete.
Obtained RTV-1 silicon rubber surface drying time 55min, completely transmittance 96%, tensile strength 2.1MPa after solidification, elongation at break 450%, after normality deposits 12 months, properties and firm formulated product are without significant difference.
Embodiment 2
The 20000cps hydroxyl-terminated polymethylphenyl sioxane of 1000g refractive index 1.4702 and 30g vinyl tributyl ketoximyl silane are added in reactor; 40 DEG C are heated under nitrogen protection; add 1g cyclohexanone-oxime; at 40 DEG C, react 4h, obtaining refractive index is that the multiple reactionness end-group termination PSI of the viscosity 19800cps of 1.4632 is for subsequent use.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane is according to the preparation method's self-control in patent CN102070785A.
By the above-mentioned obtained multiple reactionness end-group termination PSI of 100 weight part viscosity, 15 weight part ratio surface-area 200m
2the wetting ability fumed silica of/g is placed in decollator and stirs 3h; be heated to temperature 120 DEG C; be evacuated to-0.088MPa; within 3 hours, remove low molecule and moisture, be then cooled to room temperature under nitrogen protection, then add 3 parts by weight of ethylene base tributanoximo silanes; 1 weight part methyl tri acetylacetonate oxime silane; 0.1 weight part dibutyl tin laurate, 0.5 weight part γ-amine propyl trimethoxy silicane, finally vacuumizes stirring discharging sealing preservation after 0.5 hour.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 35min, completely transmittance 94%, tensile strength 2.3MPa after solidification, elongation at break 330%, after normality deposits 12 months, properties and firm formulated product are without significant difference.
Embodiment 3
The 5000cps hydroxyl-terminated polymethylphenyl sioxane of 1000g refractive index 1.4687 and 40g ethyl three propionyloxy silane are added in reactor; 40 DEG C are heated under nitrogen protection; add 0.1g cyclohexanone-oxime; at 40 DEG C, react 2h, obtaining refractive index is that the multiple reactionness end-group termination PSI of the viscosity 4800cps of 1.4587 is for subsequent use.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane is according to the preparation method's self-control in patent CN102070785A.
By the multiple reactionness end-group termination PSI of the above-mentioned preparation of 100 weight part, 12 weight part ratio surface-area 380m
2the wetting ability fumed silica of/g is placed in decollator and stirs 0.5h; be heated to temperature 80 DEG C; be evacuated to-0.090MPa; within 1 hour, remove low molecule and moisture, be then cooled to room temperature under nitrogen protection, then add 3 weight part propyl group triacetoxysilanes; 1 weight part phenyl triacetoxysilane; the sub-tin of 0.1 parts by weight of octanoic acid, 1 weight part β-amine ethyl-γ--amine propyl-triethoxysilicane, finally vacuumizes stirring discharging sealing preservation after 1 hour.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 75min, completely transmittance 92%, tensile strength 2.3MPa after solidification, elongation at break 370%, after normality deposits 12 months, properties and firm formulated product are without significant difference.
Embodiment 4
The 120000cps hydroxyl-terminated polymethylphenyl sioxane of 1000g refractive index 1.4714 and 40g methyltrimethoxy silane are added in reactor; 70 DEG C are heated under nitrogen protection; add 4g cyclohexanone-oxime; at 70 DEG C, react 6h, obtaining refractive index is that the multiple reactionness end-group termination PSI of the viscosity 108000cps of 1.4668 is for subsequent use.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane is according to the preparation method's self-control in patent CN102070785A.
By the multiple reactionness end-group termination PSI of the above-mentioned preparation of 100 weight part, 10 weight part ratio surface-area 50m
2the wetting ability fumed silica of/g is placed in decollator and stirs 0.5h; be heated to temperature 90 DEG C; be evacuated to-0.080MPa; within 6 hours, remove low molecule and moisture; then be cooled to room temperature under nitrogen protection, then add 3 weight part phenyl triethoxysilanes, 0.2 weight part dibutyl tin laurate; 0.5 weight part γ-urea propyl-triethoxysilicane, finally vacuumizes stirring discharging sealing preservation after 3 hours.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 45min, completely transmittance 96%, tensile strength 2.1MPa after solidification, elongation at break 550%, after normality deposits 12 months, properties and firm formulated product are without significant difference.
Comparative example 1
The 80000cps hydroxyl endblocked polydimethylsiloxane of 1000g refractive index 1.4067 and 40g methyltrimethoxy silane are added in reactor; 70 DEG C are heated under nitrogen protection; add 2g cyclohexanone-oxime; at 70 DEG C, react 6h, obtaining refractive index is that the multiple reactionness end-group termination PSI of the viscosity 77800cps of 1.4032 is for subsequent use.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane is according to the preparation method's self-control in patent CN102070785A.
By the how alkoxy end-capped polydimethylsiloxane of the above-mentioned preparation of 100 weight part, 10 weight part ratio surface-area 150m
2the wetting ability thermal silica of/g stirs 1h in decollator; Heating temperature 120 DEG C; be evacuated to-0.085MPa; 1h removes low molecule and moisture; be cooled to room temperature under nitrogen protection, add 3 weight part methyltrimethoxy silanes, 1 weight part tetrabutyl titanate; 1 weight part γ-amine propyl trimethoxy silicane, vacuumizes discharging sealing after stirring 0.5h and preserves.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 25min, completely transmittance 55%, tensile strength 1.7MPa after solidification, elongation at break 450%.
Comparative example 2
The 20000cps hydroxyl endblocked polydimethylsiloxane of 1000g refractive index 1.4466 and 30g methyl triacetoxysilane are added in reactor; 40 DEG C are heated under nitrogen protection; add 0.1g cyclohexanone-oxime; at 40 DEG C, react 2h, obtaining refractive index is that the multiple reactionness end-group termination PSI of the viscosity 18800cps of 1.4132 is for subsequent use.
In the present invention, hydroxyl-terminated polymethylphenyl sioxane is according to the preparation method's self-control in patent CN102070785A.
100 weight parts are stained with the multiple reactionness end-group termination PSI stating preparation, 15 weight part ratio surface-area 200m
2the hydrophobic fumed white carbon black of/g stirs 2h in decollator; Heating temperature 90 DEG C; be evacuated to-0.090MPa; 1h removes low molecule and moisture; be cooled to room temperature under nitrogen protection, add 6 weight part phenyltrimethoxysila,e, 0.2 weight part dibutyl tin laurate; 0.5 weight part γ-urea propyl-triethoxysilicane, vacuumizes discharging sealing after stirring 3h and preserves.
Obtained dealcoholized RTV-1 silicone rubber surface drying time 35min, transmittance 75%, tensile strength 2.2MPa, elongation at break 250%.
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only the present invention's preferably embodiment, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (9)
1. a multiple reactionness end-group termination PSI, is characterized in that its structure is as follows:
wherein, a, b, c=0 ~ 1000, R
1be selected from the one in methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group,
R
2be selected from the one in methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group; The refractive index of described multiple reactionness end-group termination PSI is 1.46 ± 0.01 at 20 DEG C, and the viscosity at 25 DEG C is 1500 ~ 500000cps.
2. comprise a high transmission rate single-component condensed room temperature vulcanized silicone rubber composition for multiple reactionness end-group termination PSI according to claim 1, it is characterized in that described composition is made up of the component of following weight parts:
Component A: multiple reactionness end-group termination PSI, 100 parts;
B component: reinforced filling, 1 ~ 50 part;
Component C: linking agent, 0.1 ~ 15 part;
Component D: catalyzer, 0.1 ~ 5 part;
Component E: tackifier, 0.1 ~ 5 part.
3. high transmission rate single-component condensed room temperature vulcanized silicone rubber composition according to claim 2, is characterized in that described composition is made up of the component of following weight parts:
Component A: multiple reactionness end-group termination PSI, 100 parts;
B component: reinforced filling, 10 ~ 50 parts;
Component C: linking agent, 3 ~ 15 parts;
Component D: catalyzer, 0.2 ~ 4 part;
Component E: tackifier, 0.5 ~ 5 part.
4. high transmission rate single-component condensed room temperature vulcanized silicone rubber composition according to claim 2, is characterized in that described composition is made up of the component of following weight parts:
Component A: multiple reactionness end-group termination PSI, 100 parts;
B component: reinforced filling, 10 ~ 30 parts;
Component C: linking agent, 3 ~ 10 parts;
Component D: catalyzer, 0.5 ~ 3 part;
Component E: tackifier, 1 ~ 4 part.
5. high transmission rate single-component condensed room temperature vulcanized silicone rubber composition according to claim 2, is characterized in that described reinforced filling be specific surface area is 30 ~ 400m
2the fumed silica of/g.
6. high transmission rate single-component condensed room temperature vulcanized silicone rubber composition according to claim 2, is characterized in that the structural formula of described linking agent is as follows:
Wherein, R
1be selected from methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group, R
2be selected from methyl, ethyl, propyl group, vinyl, phenyl, methoxyl group, oxyethyl group, propoxy-, phenoxy group, acetone oximido, butanone oximido, methanoyl, acetoxyl group, propionyloxy, benzoyloxy group.
7. high transmission rate single-component condensed room temperature vulcanized silicone rubber composition according to claim 2, is characterized in that described catalyzer is one or more in titanium isopropylate, tetra-n-butyl titanate, tetrabutyl titanate, stannous octoate, dibutyl tin laurate, two (methyl aceto acetate) title complex of dibutyl tin.
8. high transmission rate single-component condensed room temperature vulcanized silicone rubber composition according to claim 2, is characterized in that described tackifier are γ-amine propyl trimethoxy silicane, γ-amine propyl-triethoxysilicane, γ-methacryloxypropyl trimethoxy silane, γ-glycidoxypropyl group triethoxyl silane, β-amine ethyl-γ--amine propyl trimethoxy silicane, β-amine ethyl-γ--one or more in amine propyl-triethoxysilicane, γ-urea propyl-triethoxysilicane, γ-isocyanate group propyl-triethoxysilicane.
9. the preparation method of the high transmission rate single-component condensed room temperature vulcanized silicone rubber composition described in any one of claim 2-8, is characterized in that comprising the following steps:
Multiple reactionness end-group termination PSI, reinforced filling are stirred 0.5 ~ 5h in decollator; then be heated to >=80 DEG C; be evacuated to P≤-0.08MPa; within 1 ~ 12 hour, remove low molecule and moisture; then room temperature is cooled under nitrogen protection; add linking agent, catalyzer and tackifier again, be finally uniformly mixed discharging in 0.5 ~ 5 hour under vacuo.
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| CN106190012A (en) * | 2016-08-08 | 2016-12-07 | 广州机械科学研究院有限公司 | A kind of transparent high intensity Self-leveling piptonychia alcohol type single-component organic silicon glue and preparation method thereof |
| CN106519246A (en) * | 2016-11-21 | 2017-03-22 | 成都硅宝科技股份有限公司 | Polyalkyloxy-terminated polysiloxane and preparation method thereof |
| CN109232894A (en) * | 2018-09-21 | 2019-01-18 | 广州天宸高新材料有限公司 | Methoxy group methyl phenyl silicone resin, organosilicon coating glue and preparation method and application |
| 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 |
| CN111925529A (en) * | 2020-06-10 | 2020-11-13 | 湖北航天化学技术研究所 | POSS (polyhedral oligomeric silsesquioxane) modified silane terminated liquid fluororubber, adhesive and preparation method |
| CN113337174A (en) * | 2021-06-15 | 2021-09-03 | 常州大学 | Preparation method of super-hydrophobic coating with high light transmittance and high haze |
| CN115746305A (en) * | 2022-11-17 | 2023-03-07 | 万华化学集团股份有限公司 | Phenyl polysiloxane and preparation method and application thereof |
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| 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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| CN106190012A (en) * | 2016-08-08 | 2016-12-07 | 广州机械科学研究院有限公司 | A kind of transparent high intensity Self-leveling piptonychia alcohol type single-component organic silicon glue and preparation method thereof |
| CN106519246A (en) * | 2016-11-21 | 2017-03-22 | 成都硅宝科技股份有限公司 | Polyalkyloxy-terminated polysiloxane 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 |
| CN109232894A (en) * | 2018-09-21 | 2019-01-18 | 广州天宸高新材料有限公司 | Methoxy group methyl phenyl silicone resin, organosilicon coating glue and preparation method and application |
| CN111925529A (en) * | 2020-06-10 | 2020-11-13 | 湖北航天化学技术研究所 | POSS (polyhedral oligomeric silsesquioxane) modified silane terminated liquid fluororubber, adhesive and preparation method |
| 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 |
| CN113337174A (en) * | 2021-06-15 | 2021-09-03 | 常州大学 | Preparation method of super-hydrophobic coating with high light transmittance and high haze |
| CN115746305A (en) * | 2022-11-17 | 2023-03-07 | 万华化学集团股份有限公司 | Phenyl polysiloxane and preparation method and application thereof |
| 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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