CN115926471A - Liquid silicone rubber capable of increasing viscosity of glass fiber base material and preparation method thereof - Google Patents
Liquid silicone rubber capable of increasing viscosity of glass fiber base material and preparation method thereof Download PDFInfo
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- CN115926471A CN115926471A CN202211354401.8A CN202211354401A CN115926471A CN 115926471 A CN115926471 A CN 115926471A CN 202211354401 A CN202211354401 A CN 202211354401A CN 115926471 A CN115926471 A CN 115926471A
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- glass fiber
- silicone rubber
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- liquid silicone
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- 239000000463 material Substances 0.000 title claims abstract description 134
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 68
- 239000004944 Liquid Silicone Rubber Substances 0.000 title claims abstract description 61
- 239000003365 glass fiber Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 230000001965 increasing effect Effects 0.000 title claims abstract description 40
- -1 polysiloxane Polymers 0.000 claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 43
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 42
- 239000006229 carbon black Substances 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 27
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 238000004132 cross linking Methods 0.000 claims abstract description 16
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 13
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 52
- 238000002156 mixing Methods 0.000 claims description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 229910021485 fumed silica Inorganic materials 0.000 claims description 18
- 230000002209 hydrophobic effect Effects 0.000 claims description 18
- 125000003545 alkoxy group Chemical group 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 229920002545 silicone oil Polymers 0.000 claims description 8
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 claims description 4
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 4
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 3
- 239000004971 Cross linker Substances 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 238000006459 hydrosilylation reaction Methods 0.000 claims description 3
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims description 3
- 238000007142 ring opening reaction Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 claims description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000012752 auxiliary agent Substances 0.000 abstract description 11
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- 229920001971 elastomer Polymers 0.000 abstract description 5
- 239000005060 rubber Substances 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 3
- 239000002585 base Substances 0.000 description 111
- 238000004898 kneading Methods 0.000 description 31
- 238000010438 heat treatment Methods 0.000 description 22
- 238000000034 method Methods 0.000 description 15
- 230000008569 process Effects 0.000 description 10
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 6
- 238000004513 sizing Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 239000004945 silicone rubber Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000005821 ethenylmethoxy group Chemical group [H]\[#6]([H])=[#6](\[H])C([H])([H])[#8]-* 0.000 description 2
- 239000006115 industrial coating Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Abstract
The invention discloses liquid silicone rubber capable of increasing viscosity of a glass fiber substrate and a preparation method thereof, wherein the liquid silicone rubber comprises the following components in percentage by mass: (0.6-1.5) of component A and component B; the component A comprises: 100 parts of base material a and 1-2 parts of catalyst; the component B comprises: 60-106 parts of base material b, 6-10 parts of cross-linking agent and 0.01-0.2 part of cross-linking inhibitor; the base material a is prepared from (1.2-1.8) by mass: 1 of vinyl polysiloxane and white carbon black. The liquid silicone rubber capable of increasing viscosity of the glass fiber substrate can realize good bonding with the glass fiber substrate without additionally adding a bonding auxiliary agent or a tackifier or a primer, so that the problems of rubber material change promotion, short storage time and the like caused by the bonding auxiliary agent or the tackifier are solved, convenience is brought to production, and the liquid silicone rubber is very suitable for production application of coating or mould pressing of the surface of the glass fiber substrate.
Description
Technical Field
The invention relates to the technical field of addition type liquid silicone rubber, in particular to liquid silicone rubber capable of increasing viscosity of a glass fiber substrate and a preparation method thereof.
Background
The addition type liquid silicone rubber has simple injection molding process, fast molding, no toxicity and no harm, and is widely applied to the fields of automobile parts, electronic and electric appliances, industrial coating, infant products, tableware and the like. The addition type liquid silicone rubber has poor cohesiveness with most base materials due to the inertia of the addition type liquid silicone rubber, and in order to improve the cohesiveness with the base materials, the surface of the bonding base material is pretreated in advance by using a primer in the prior art, which often causes the problems of complicated working procedures, environmental pollution and the like; in addition, a common method is to add a tackifier into the liquid silicone rubber to improve the adhesion between the liquid silicone rubber and the base material, although the method is simpler in process and more environment-friendly than a method using a primer, the addition of the tackifier often has more or less influence on the sizing material, including the fluidity of the sizing material, the transparency of the sizing material, the storage stability of the sizing material and the like; considering how to start from the silicon rubber, the method for improving the adhesion of the silicon rubber to the base material is a good choice, is not only environment-friendly, but also can ensure that the physical properties of the rubber material are not changed.
The industrial coating liquid silicone rubber is widely applied liquid silicone rubber, such as electric wire and cable coating, glass fiber sleeve coating, glass fiber cloth coating and the like, the liquid silicone rubber is often required to have good cohesiveness to a glass fiber base material, the traditional process is to improve the cohesiveness of the liquid silicone rubber and the glass fiber base material by a primer or a tackifier, and the traditional process is often to use some epoxy group or alkoxy group containing cementing aids, or Si-H group containing adhesives and the like, and although the addition of the aids improves the cohesiveness of the liquid silicone rubber and the glass fiber base material, the flowability or physical and mechanical strength of a sizing material can be reduced, and the production and strength of a product are adversely affected. Therefore, it is necessary to design a liquid silicone rubber having viscosity increasing effect on glass fiber base material and a preparation method thereof.
Disclosure of Invention
Aiming at the situation, the invention provides the liquid silicone rubber capable of increasing the viscosity of the glass fiber base material and the preparation method thereof, aiming at overcoming the defects of the prior art, the liquid silicone rubber capable of increasing the viscosity of the glass fiber base material provided by the invention can realize good bonding with the glass fiber base material without additionally adding a bonding auxiliary agent or a tackifier or a primer, thereby avoiding the problems of rubber material promotion, insufficient storage time and the like caused by the bonding auxiliary agent or the tackifier, bringing convenience for production, and being very suitable for the production application of the liquid silicone rubber product coated on the surface of the glass fiber base material or molded.
In order to achieve the purpose, the invention provides the following technical scheme: a liquid silicone rubber capable of increasing viscosity of a glass fiber substrate is prepared from the following components in percentage by mass of 1: (0.6-1.5) of component A and component B;
the component A comprises: 100 parts of base material a and 1-2 parts of catalyst;
the component B comprises: 60-106 parts of base material b, 6-10 parts of cross-linking agent and 0.01-0.2 part of cross-linking inhibitor;
the base material a is prepared from (1.2-1.8) by mass: 1 of vinyl polysiloxane and white carbon black;
the base material b is prepared from (0.6-1.2) by mass: 1 of vinyl alkoxy polysiloxane and white carbon black.
Preferably, the vinyl polysiloxane in the base material a is alpha, omega-divinyl polydimethylsiloxane, and the viscosity of the alpha, omega-divinyl polydimethylsiloxane at 25 ℃ is 1000-20000mPa.s;
the vinyl alkoxy polysiloxane in the base material b is alpha, omega-divinyl polydimethylsiloxane with alkoxy groups on side chains, and the viscosity of the vinyl alkoxy polysiloxane at 25 ℃ is 1000-20000mPa.s.
Preferably, the side chain alkoxy group of the vinylalkoxypolysiloxane in the base material b is selected from any one of methoxy, ethoxy, propoxy and butoxy.
Preferably, the vinylalkoxypolysiloxane in the base material b is prepared by firstly synthesizing 1, 3-divinyl-2, 4-dimethoxycyclotetrasiloxane by hydrosilylation with tetramethyltetravinylcyclotetrasiloxane and trimethoxysilylhydride, and then carrying out ring opening reaction with octamethylcyclotetrasiloxane and vinyl double end socket to synthesize the corresponding vinylmethoxypolysiloxane.
Preferably, the molar content of the methoxyl in the vinylmethoxy polysiloxane is 0.001-0.02 mmol/g.
Preferably, the white carbon black in the base material a and the base material b is hydrophobic fumed silica, and the specific surface area of the hydrophobic fumed silica is 100-350 m2/g.
Preferably, the catalyst is a platinum catalyst, and the platinum content of the platinum catalyst is 2500-6000 ppm.
Preferably, the cross-linking agent is hydrogen-containing silicone oil, and the hydrogen content of the hydrogen-containing silicone oil is 0.3-1.5 wt%.
Preferably, the crosslinking inhibitor is selected from any one of methylbutynol and ethynylcyclohexanol.
The invention also provides a preparation method of the liquid silicone rubber capable of increasing viscosity of the glass fiber base material, which comprises the following steps:
1) Mixing vinyl polysiloxane, white carbon black, hexamethyldisilazane and water, carrying out mixing to remove hexamethyldisilazane and water to obtain a base material a, mixing vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, carrying out mixing to remove hexamethyldisilazane and water to obtain a base material b;
2) Mixing the base material a obtained in the step 1) with a catalyst to obtain a component A, and simultaneously mixing the base material B obtained in the step 1) with a cross-linking agent and a cross-linking inhibitor to obtain a component B;
3) Mixing the component A and the component B according to the mass ratio of 1: (0.6-1.5) to obtain the liquid silicone rubber which has viscosity-increasing effect on the glass fiber base material.
The invention has the beneficial effects that:
1. the liquid silicone rubber capable of increasing viscosity of the glass fiber substrate can realize good bonding with the glass fiber substrate without additionally adding a bonding auxiliary agent or a tackifier or a primer, so that the problems of rubber material change promotion, insufficient storage time and the like caused by the bonding auxiliary agent or the tackifier are avoided, convenience is brought to production, and the liquid silicone rubber is very suitable for production application of coating or mould pressing of the surface of the glass fiber substrate;
2. the preparation method provided by the invention is simple and stable, does not need to additionally add a bonding auxiliary agent, is low in cost, and is suitable for large-scale production and application.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the description is to be regarded as illustrative in nature and not as restrictive.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the illustrated embodiments, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first", "second", "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
The technical solution of the present invention is clearly and completely described below.
The invention provides the following technical scheme: a liquid silicone rubber capable of increasing viscosity of a glass fiber substrate is prepared from the following components in percentage by mass of 1: (0.6-1.5) of component A and component B;
the component A comprises: 100 parts of base material a and 1-2 parts of catalyst;
the component B comprises: 60-106 parts of base material b, 6-10 parts of cross-linking agent and 0.01-0.2 part of cross-linking inhibitor;
the base material a is prepared from (1.2-1.8) by mass: 1 of vinyl polysiloxane and white carbon black;
the base material b is prepared from (0.6-1.2) by mass: 1 of vinyl alkoxy polysiloxane and white carbon black.
In the invention, the liquid silicone rubber for increasing viscosity of the glass fiber substrate is prepared from the following components in percentage by mass of 1: (0.6-1.5) of a component A and a component B, preferably by mass ratio of 1:1, component A and component B; wherein the component A comprises: 100 parts of base material a and 1-2 parts of catalyst;
the component B comprises: 60 to 106 portions of base material b,6 to 10 portions of cross linker and 0.01 to 0.2 portion of cross linking inhibitor.
In the invention, the base material a is prepared from the following components in percentage by mass (1.2-1.8): 1, preferably 1.6:1 of vinyl polysiloxane and white carbon black; the base material b consists of vinylalkoxypolysiloxane and white carbon black in a mass ratio of (0.6-1.2) to 1, and preferably consists of vinylalkoxypolysiloxane and white carbon black in a mass ratio of 1.0.
In the present invention, the vinyl polysiloxane in the base a is preferably α, ω -divinylpolydimethylsiloxane, and the viscosity of the α, ω -divinylpolydimethylsiloxane at 25 ℃ is preferably 1000 to 20000mpa.s, more preferably 1000 to 10000mpa.s; the vinylalkoxypolysiloxane in the base b is preferably methoxy-containing alpha, omega-divinylpolydimethylalkoxysiloxane, more preferably the molar methoxy group content is 0.01 to 0.015mmol/g, and even more preferably the viscosity at 25 ℃ is 10000 to 15000mPa.s.
In a preferred embodiment of the invention, the viscosity of α, ω -divinylpolydimethylsiloxane in the base a at 25 ℃ is 1000mpa.s, the viscosity of α, ω -divinylpolydimethylsiloxane in the base b at 25 ℃ is 10000mpa.s, and the molar content of methoxy groups is 0.01mmol/g; in another preferred embodiment of the invention, the viscosity of α, ω -divinylpolydimethylsiloxane in the base a at 25 ℃ is 10000mpa.s, the viscosity of α, ω -divinylpolydimethylsiloxane in the base b at 25 ℃ is 12000mpa.s, and the molar content of methoxy groups is 0.013mmol/g. Wherein the source of the vinyl polysiloxane is not particularly limited in the present invention, and commercially available products of the above-mentioned α, ω -divinylpolydimethylsiloxane well known to those skilled in the art may be used.
In the invention, the white carbon black in the base material is preferably hydrophobic fumed silica; the specific surface area of the hydrophobic fumed silica is preferably 100-250 m 2 (ii) g, more preferably 100 to 150m 2 /g。
In a preferred embodiment of the present invention, the hydrophobic fumed silica has a specific surface area of 100m 2 (iv) g; in another preferred embodiment of the present invention, the hydrophobic fumed silica has a specific surface area of 150m 2 (ii) in terms of/g. The source of the white carbon black is not particularly limited in the present invention, and any commercially available or self-made product of the above hydrophobic fumed silica known to those skilled in the art may be used.
In the present invention, the a component includes 100 parts by weight of the base a.
In the present invention, the catalyst is preferably a platinum catalyst; the platinum content of the platinum catalyst is preferably 2500 to 6000ppm, more preferably 5200ppm. The source of the catalyst in the present invention is not particularly limited, and a commercially available product of the above platinum catalyst known to those skilled in the art may be used.
In the present invention, the A component includes 1 to 2 parts by weight of the catalyst, preferably 1.5 parts by weight.
In the present invention, the base B of the B component is not the same as the vinyl polysiloxane used in the base a of the A component described above, and is specifically described herein.
In the present invention, the B component comprises 60 to 106 parts by weight of the base material B, preferably 90.94 to 95.94 parts by weight.
In the invention, the vinyl alkoxy polysiloxane in the base material b is formed by 1, 3-divinyl-2, 4-dimethoxytetramethylcyclotetrasiloxane and octamethylcyclotetrasiloxane through ring-opening condensation under the catalysis of alkali and is terminated by a vinyl double-end socket, so that alkoxy functional groups are successfully introduced into a main chain of the vinyl polysiloxane; wherein the 1, 3-divinyl-2, 4-dimethoxytetramethylcyclotetrasiloxane is obtained by hydrosilylation of tetramethyltetravinylcyclotetrasiloxane and trimethoxyhydrosilane; wherein, the trimethoxy hydrosilane is also any one of triethoxy hydrosilane, tripropoxy hydrosilane or tributoxy hydrosilane, and is preferably trimethoxy hydrosilane. The sources of the trimethoxyhydrosilane, octamethylcyclotetrasiloxane, and vinyl double block and the like are not particularly limited in the present invention, and the above-mentioned commercially available products known to those skilled in the art can be used.
In a preferred embodiment of the invention, the vinyl alkoxy polysiloxane is preferably vinyl methoxy polysiloxane, more preferably the molar content of methoxy groups is 0.013mmol/g, and the viscosity at 25 ℃ is 12000mPa.s.
According to the invention, functional groups such as alkoxy and the like are introduced to the main chain of the vinyl polysiloxane, so that the polarity of vinyl polysiloxane molecules is greatly increased, and the alkoxy functional groups can generate similar compatibility with polar groups on the surface of the glass fiber substrate under the action of high temperature, so that the two groups can be well bonded.
In the invention, the weight portion of the base material B in the component B is 60-106 parts, preferably 90.94-95.94 parts, wherein the mass ratio of the vinyl alkoxy polysiloxane to the white carbon black is (0.6-1.2): 1, wherein the molar content of the methoxyl in the vinylmethoxypolysiloxane is preferably 1.0 to 1, and more preferably 0.001 to 0.02mmol/g, and preferably 0.01 to 0.015mmol/g.
The invention realizes good bonding between the liquid silicone rubber and the glass fiber base material by adjusting the molar content of alkoxy in the vinyl alkoxy polysiloxane and the dosage of the vinyl alkoxy polysiloxane, and is very suitable for the production of glass fiber coated liquid silicone rubber products.
In the present invention, the crosslinking agent is preferably a hydrogen-containing silicone oil; the hydrogen content of the hydrogen-containing silicone oil is preferably 0.1 to 1.0wt%, and more preferably 0.5wt%. The source of the crosslinking agent in the present invention is not particularly limited, and commercially available products of the above hydrogen-containing silicone oil known to those skilled in the art can be used.
In the present invention, the B component includes 6 to 10 parts by weight of a crosslinking agent, preferably 8 to 9 parts by weight.
In the present invention, the crosslinking inhibitor is preferably one selected from the group consisting of methylbutynol and ethynylcyclohexanol, and more preferably ethynylcyclohexanol. The source of the crosslinking inhibitor in the present invention is not particularly limited, and commercially available products of the above-mentioned methylbutynol and ethynylcyclohexanol, which are well known to those skilled in the art, may be used.
In the present invention, the B component includes 0.01 to 0.2 parts by weight of a crosslinking inhibitor, preferably 0.08 parts by weight.
According to the invention, functional groups such as alkoxy and the like are introduced into the main chain of vinyl polysiloxane, so that the polarity of vinyl polysiloxane molecules is greatly increased, and the alkoxy functional groups can have similar compatible action with polar groups on the surface of a glass fiber substrate under the action of high temperature, so that the alkoxy functional groups and the polar groups can be well bonded, and the preparation method is very suitable for the production of glass fiber coated liquid silicone rubber products.
The invention also provides a preparation method of the liquid silicone rubber capable of increasing viscosity of the glass fiber base material, which comprises the following steps:
1) Mixing vinyl polysiloxane, white carbon black, hexamethyldisilazane and water, carrying out mixing to remove hexamethyldisilazane and water to obtain a base material a, mixing vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, carrying out mixing to remove hexamethyldisilazane and water to obtain a base material b;
2) Mixing the base material a obtained in the step 1) with a catalyst to obtain a component A, and simultaneously mixing the base material B obtained in the step 1) with a cross-linking agent and a cross-linking inhibitor to obtain a component B;
3) Mixing the component A and the component B according to the mass ratio of 1: (0.6-1.5) to obtain the liquid silicone rubber which has viscosity increasing effect on the glass fiber base material.
The invention firstly mixes vinyl polysiloxane/vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, and carries out mixing to remove hexamethyldisilazane and water, thus obtaining the base material. In the present invention, the vinyl polysiloxane and the white carbon black are the same as those described in the above technical solution, and are not described herein again.
In the present invention, the mass ratio of the vinyl polysiloxane, the white carbon black, the hexamethyldisilazane and the water in the base material a is preferably (1.2 to 1.8): 1: (0.2-0.3): (0.04 to 0.06), more preferably 1.6: 1:0.25:0.05; the mass ratio of the vinylalkoxypolysiloxane, the white carbon black, the hexamethyldisilazane and the water in the base material b is preferably (0.6-1.2): 1: (0.2-0.3): (0.04 to 0.06), more preferably 1.0:1:0.25:0.05.
the equipment for the mixing and subsequent mixing process is not particularly limited in the present invention, and a kneader well known to those skilled in the art may be used.
In the present invention, the mixing process preferably includes:
kneading the mixed material at 20-30 ℃ for 2-3 h in advance, heating to 95-105 ℃ for further kneading for 0.4-0.6 h, heating to 135-150 ℃ for vacuum kneading for 2-4 h to obtain a base material;
more preferably:
kneading the mixed material at 25 ℃ for 2.5h, heating to 100 ℃ for further kneading for 0.5h, heating to 140-150 ℃ for vacuum kneading for 3h to obtain a base material; in the present invention, the degree of vacuum of the vacuum kneading is preferably 0.08 to 0.1MPa. The purpose of the mixing process adopted by the invention is to uniformly knead the vinyl polysiloxane and the white carbon black and simultaneously remove low volatile matters such as hexamethyldisilazane, water and the like.
After the base material is obtained, mixing the obtained base material a with a catalyst to obtain a component A; and simultaneously mixing the obtained base material B with a cross-linking agent and a cross-linking inhibitor to obtain a component B. The invention has no special limitation on the specific process of mixing the base material a and the catalyst and the specific process of mixing the base material B, the cross-linking agent and the cross-linking inhibitor, and can adopt the technical scheme of mechanical stirring or manual stirring which is well known to a person skilled in the art, so as to uniformly mix each component in the component A and each component in the component B respectively.
After the component A and the component B are obtained, the component A and the component B are mixed according to the mass ratio of 1: (0.6-1.5) mixing to obtain liquid silicone rubber; preferably, the component A and the component B are mixed according to the mass ratio of 1:1, mixing to obtain the liquid silicone rubber. The specific process of mixing the component A and the component B is not particularly limited in the invention, and the technical scheme of mechanical stirring or manual stirring which is well known to those skilled in the art can be adopted, so that the component A and the component B are uniformly mixed.
The preparation method provided by the invention has the advantages of simple process and formula, stable production, no need of additional bonding auxiliary agent, low cost, few added components, easiness in repetition and suitability for large-scale production and application.
The invention provides liquid silicone rubber capable of increasing viscosity of a glass fiber substrate, which is prepared from the following components in percentage by mass: (0.6-1.5) and a component A and a component B; the component A comprises: 100 parts of base material a and 1-2 parts of catalyst; the component B comprises: 60 to 106 portions of base material b,6 to 10 portions of cross linker and 0.01 to 0.2 portion of cross linking inhibitor. The base material a is prepared from (1.2-1.8) by mass: 1 of vinyl polysiloxane and white carbon black; the base material b consists of vinyl alkoxy polysiloxane and white carbon black in a mass ratio of (0.6-1.2) to 1.
Compared with the prior art, the liquid silicone rubber capable of increasing viscosity of the glass fiber substrate can realize good bonding with the glass fiber substrate without additionally adding a bonding auxiliary agent or a tackifier or a primer, so that the problems of rubber material change promotion, insufficient storage time and the like caused by the bonding auxiliary agent or the tackifier are avoided, convenience is brought to production, and the liquid silicone rubber is very suitable for production application of glass fiber substrate surface coating or mould pressing liquid silicone rubber products.
In addition, the preparation method provided by the invention is simple and stable, does not need to additionally add a bonding auxiliary agent, is low in cost and is suitable for large-scale production and application.
In order to further illustrate the present invention, the following examples are provided for illustrative purposes. The starting materials used in the following examples of the present invention are all commercially available products.
Example 1
1) Preparation of base material a: 80 parts by weight of an alpha, omega-divinylpolydimethylsiloxane having a viscosity (25 ℃) of 1000mPas and 50 parts by weight of a specific surface area of 150m 2 Putting hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water into a kneader, kneading for 2.5h at 25 ℃, heating to 100 ℃, continuing kneading for 0.5h, heating to 140-150 ℃, and kneading for 3h under vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material a;
2) Preparation of base material b: 30 parts by weight of an alpha, omega-divinylpolydimethyltrimethoxysilane having a viscosity (25 ℃) of 10000mPa.s (the molar content of methoxyl groups is 0.01 mmol/g) and 50 parts by weight of a specific surface area of 150m 2 Perg of hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are introduced into a kneader at 25 DEGKneading for 2.5h, heating to 100 ℃, continuing to knead for 0.5h, heating to 140-150 ℃ and kneading for 3h under vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of the component A: taking 100g of the base material a obtained in the step 1), adding 1g of catalyst, and stirring for 10-30 min to obtain a component A.
4) Preparation of the component B: taking 90.94g of the base material B obtained in the step 2), 6g of hydrogen-containing silicone oil (with the hydrogen content of 0.5%) and 0.06g of ethynyl cyclohexanol, and stirring for 10-30 min to obtain a component B.
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1, and uniformly mixing to obtain the product.
Example 2
1) Preparation of base material a: the same as example 1;
2) Preparation of base material b: 40 parts by weight of an alpha, omega-divinylpolydimethyltrimethoxysilane having a viscosity (25 ℃) of 10000mPa.s (the molar content of methoxyl groups is 0.01 mmol/g) and 50 parts by weight of a specific surface area of 150m 2 Putting the hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water into a kneader, kneading for 2.5 hours at 25 ℃, heating to 100 ℃, continuing kneading for 0.5 hour, heating to 140-150 ℃, and kneading for 3 hours in vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of component A: the same as example 1;
4) Preparation of the component B: the same as example 1;
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1, and uniformly mixing to obtain the product.
Example 3
1) Preparation of base material a: the same as example 1;
2) Preparation of base material b: 50 parts by weight of an alpha, omega-divinylpolydimethyltrimethoxysilane having a viscosity (25 ℃) of 10000mPa.s (the molar content of methoxyl groups is 0.01 mmol/g) and 50 parts by weight of a specific surface area of 150m 2 Per g of hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water were added to the kneadingKneading for 2.5h at 25 ℃, heating to 100 ℃ for further kneading for 0.5h, heating to 140-150 ℃ for kneading for 3h under vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of the component A: the same as example 1;
4) Preparation of the component B: the same as example 1;
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1, and uniformly mixing to obtain the product.
Example 4
1) Preparation of base material a: the same as example 1;
2) Preparation of base material b: 60 parts by weight of an alpha, omega-divinylpolydimethyltrimethoxysilane having a viscosity (25 ℃) of 10000mPa.s (molar content of methoxy groups: 0.01 mmol/g) and 50 parts by weight of a specific surface area of 150m 2 Putting hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water into a kneader, kneading for 2.5h at 25 ℃, heating to 100 ℃, continuing kneading for 0.5h, heating to 140-150 ℃, and kneading for 3h under vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of component A: the same as example 1;
4) Preparation of the component B: the same as example 1;
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1, and uniformly mixing to obtain the product.
Example 5
1) Preparation of base material a: the same as example 1;
2) Preparation of base material b: 50 parts by weight of an alpha, omega-divinylpolydimethyltrimethoxysilane having a viscosity (25 ℃) of 10000mPa.s (the molar content of methoxyl groups is 0.012 mmol/g) and 50 parts by weight of a specific surface area of 150m 2 Putting hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water into a kneader, kneading for 2.5h at 25 ℃, heating to 100 ℃, continuing kneading for 0.5h, heating to 140-150 ℃, and kneading for 3h under vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of the component A: the same as example 1;
4) Preparation of the component B: the same as example 1;
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1 and mixing uniformly to obtain the product.
Example 6
1) Preparation of base material a: the same as example 1;
2) Preparation of base material b: 50 parts by weight of α, ω -divinylpolydimethyltrimethoxysilane (molar content of methoxy group: 0.015 mmol/g) having a viscosity (25 ℃ C.) of 10000 mPas and 50 parts by weight of a specific surface area of 150m 2 Putting hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water into a kneader, kneading for 2.5h at 25 ℃, heating to 100 ℃, continuing kneading for 0.5h, heating to 140-150 ℃, and kneading for 3h under vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of component A: the same as example 1;
4) Preparation of the component B: the same as example 1;
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1, and uniformly mixing to obtain the product.
Example 7
1) Preparation of base material a: the same as example 1;
2) Preparation of base material b: 50 parts by weight of alpha, omega-divinylpolydimethyltrimethoxysiloxane having a viscosity (25 ℃) of 15000mPa.s (molar methoxy content 0.015 mmol/g) and 50 parts by weight of specific surface area 150m 2 Putting hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water into a kneader, kneading for 2.5h at 25 ℃, heating to 100 ℃, continuing kneading for 0.5h, heating to 140-150 ℃, and kneading for 3h under vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of component A: the same as example 1;
4) Preparation of the component B: the same as example 1;
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1 and mixing uniformly to obtain the product.
Example 8
1) Preparation of base material a: the same as example 1;
2) Preparation of base material b: 50 parts by weight of an alpha, omega-divinylpolydimethylsiloxane having a viscosity (25 ℃ C.) of 15000mPa.s and 50 parts by weight of a specific surface area of 150m 2 Putting the hydrophobic fumed silica, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water into a kneader, kneading for 2.5 hours at 25 ℃, heating to 100 ℃, continuing kneading for 0.5 hour, heating to 140-150 ℃, and kneading for 3 hours in vacuum (the vacuum degree is 0.08-0.1 MPa) to obtain a base material b;
3) Preparation of component A: the same as example 1;
4) Preparation of the component B: the same as example 1;
5) Preparing liquid silicone rubber with tackifying property on glass fiber base materials: mixing the component A obtained in the step 3) and the component B obtained in the step 4) according to the weight ratio of 1:1, and uniformly mixing to obtain the product.
The liquid silicone rubber with tackifying property to the glass fiber base material prepared in the embodiments 1-8 of the invention is tested for various performances, including the adhesion test to the glass fiber base material, and the test method is as follows: liquid silicone rubber prepared by mixing the AB components is coated on the surface of a glass fiber base material in advance, then is baked in an oven at 150 ℃ for 10min, and the bonding strength is measured, and the results are shown in tables 1-2.
TABLE 1 data on the properties of the liquid silicone rubbers obtained in examples 1 to 8 according to the invention
As can be seen from Table 1:
1) As can be seen from comparison of examples 1-4, the bonding strength of the silicone rubber to the glass fiber substrate is gradually increased along with the increasing of the dosage of the alpha, omega-divinylpolydimethyltrimethoxysiloxane in the base material b, and the mutual cohesive failure degree is gradually increased, which shows that the bonding of the silicone rubber to the glass fiber substrate is gradually increased along with the increasing of the trimethoxy content, and the tensile strength and the tearing strength are also gradually increased, mainly because the mutual cohesive force among the polysiloxane molecular chains is gradually increased after the introduction of the trimethoxy group, so that the tensile strength and the tearing strength are correspondingly increased, and the exercise elongation is correspondingly reduced just because the mutual cohesive force among the molecular chains is increased;
2) Comparing examples 3, 5 and 6, it can be seen that, as the molar content of trimethoxy in the molecule increases, the adhesive force of the silicone rubber to the glass fiber substrate gradually increases, and the cohesive failure in example 6 reaches 100%;
3) As can be seen by comparing examples 6 and 7, the physical combination of the silicone rubbers is improved with increasing viscosity of the α, ω -divinylpolydimethyltrimethoxysiloxane, especially in example 7, which results in 100% cohesive failure and optimum physical and mechanical properties.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The liquid silicone rubber capable of increasing viscosity of glass fiber base materials is characterized by comprising the following components in percentage by mass: (0.6-1.5) of component A and component B;
the component A comprises: 100 parts of base material a and 1-2 parts of catalyst;
the component B comprises: 60 to 106 portions of base material b,6 to 10 portions of cross linker and 0.01 to 0.2 portion of cross linking inhibitor;
the base material a is prepared from (1.2-1.8) by mass: 1 of vinyl polysiloxane and white carbon black;
the base material b is prepared from (0.6-1.2) by mass: 1 and white carbon black.
2. The liquid silicone rubber for increasing the viscosity of a glass fiber substrate according to claim 1, wherein the vinyl polysiloxane in the base material a is α, ω -divinyl polydimethylsiloxane, and the viscosity of the α, ω -divinyl polydimethylsiloxane at 25 ℃ is 1000 to 20000mPa.s;
the vinyl alkoxy polysiloxane in the base material b is alpha, omega-divinyl polydimethylsiloxane with side chains containing alkoxy groups, and the viscosity of the vinyl alkoxy polysiloxane at 25 ℃ is 1000-20000mPa.s.
3. The liquid silicone rubber for increasing the viscosity of a glass fiber substrate according to claim 2, wherein the pendant alkoxy group of the vinylalkoxypolysiloxane in the base b is selected from any one of methoxy, ethoxy, propoxy and butoxy groups.
4. The liquid silicone rubber for increasing the viscosity of glass fiber substrates as claimed in claim 2, wherein the vinylalkoxypolysiloxane in the base material b is the corresponding vinylmethoxypolysiloxane which is synthesized by first synthesizing 1, 3-divinyl-2, 4-dimethoxycyclotetrasiloxane through hydrosilylation with tetramethyltetravinylcyclotetrasiloxane and trimethoxysilane and then synthesizing the corresponding vinylmethoxypolysiloxane through ring opening with octamethylcyclotetrasiloxane and vinyl double-head.
5. The liquid silicone rubber capable of increasing the viscosity of a glass fiber substrate according to claim 4, wherein the molar content of the methoxyl in the vinylmethoxypolysiloxane is 0.001-0.02 mmol/g.
6. The liquid silicone rubber capable of increasing viscosity of glass fiber base material according to claim 1, wherein the white carbon black in the base material a and the base material b is hydrophobic fumed silica, and the specific surface area of the hydrophobic fumed silica is 100-350 m 2 /g。
7. The liquid silicone rubber for increasing the viscosity of a glass fiber substrate according to claim 1, wherein the catalyst is a platinum catalyst, and the platinum content of the platinum catalyst is 2500-6000 ppm.
8. The liquid silicone rubber for increasing the viscosity of a glass fiber substrate according to claim 1, wherein the crosslinking agent is hydrogen-containing silicone oil, and the hydrogen content of the hydrogen-containing silicone oil is 0.3 to 1.5wt%.
9. The liquid silicone rubber for increasing the viscosity of a glass fiber substrate according to claim 1, wherein the crosslinking inhibitor is any one selected from the group consisting of methylbutynol and ethynylcyclohexanol.
10. The preparation method of the liquid silicone rubber capable of increasing viscosity of the glass fiber substrate is characterized by comprising the following steps:
1) Mixing vinyl polysiloxane, white carbon black, hexamethyldisilazane and water, carrying out mixing to remove hexamethyldisilazane and water to obtain a base material a, mixing vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, carrying out mixing to remove hexamethyldisilazane and water to obtain a base material b;
2) Mixing the base material a obtained in the step 1) with a catalyst to obtain a component A, and simultaneously mixing the base material B obtained in the step 1) with a cross-linking agent and a cross-linking inhibitor to obtain a component B;
3) Mixing the component A and the component B according to the mass ratio of 1: (0.6-1.5) to obtain the liquid silicone rubber which has viscosity increasing effect on the glass fiber base material.
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