CN115926471B - Liquid silicone rubber with tackifying property on glass fiber base material and preparation method thereof - Google Patents
Liquid silicone rubber with tackifying property on glass fiber base material and preparation method thereof Download PDFInfo
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- CN115926471B CN115926471B CN202211354401.8A CN202211354401A CN115926471B CN 115926471 B CN115926471 B CN 115926471B CN 202211354401 A CN202211354401 A CN 202211354401A CN 115926471 B CN115926471 B CN 115926471B
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- 239000000463 material Substances 0.000 title claims abstract description 119
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 66
- 239000004944 Liquid Silicone Rubber Substances 0.000 title claims abstract description 59
- 239000003365 glass fiber Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title abstract description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000006229 carbon black Substances 0.000 claims abstract description 40
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 238000004132 cross linking Methods 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 16
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- -1 polysiloxane Polymers 0.000 claims description 66
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 52
- 229920001296 polysiloxane Polymers 0.000 claims description 49
- 238000002156 mixing Methods 0.000 claims description 48
- 229920002554 vinyl polymer Polymers 0.000 claims description 45
- 239000000758 substrate Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 25
- 230000002209 hydrophobic effect Effects 0.000 claims description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 17
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 17
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 125000003545 alkoxy group Chemical group 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 229920002545 silicone oil Polymers 0.000 claims description 8
- 125000005821 ethenylmethoxy group Chemical group [H]\[#6]([H])=[#6](\[H])C([H])([H])[#8]-* 0.000 claims description 7
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 6
- 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
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-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
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 238000006459 hydrosilylation reaction Methods 0.000 claims description 3
- 238000007142 ring opening reaction Methods 0.000 claims description 3
- 239000012808 vapor phase Substances 0.000 claims description 3
- 239000013067 intermediate product Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000011152 fibreglass Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 239000002318 adhesion promoter Substances 0.000 abstract description 7
- 238000003860 storage Methods 0.000 abstract description 5
- 239000003292 glue Substances 0.000 abstract description 4
- 238000003825 pressing Methods 0.000 abstract description 3
- 239000002585 base Substances 0.000 description 104
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 14
- 239000000047 product Substances 0.000 description 12
- 238000004898 kneading Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 8
- 229910021485 fumed silica Inorganic materials 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 241000872198 Serjania polyphylla Species 0.000 description 6
- 239000004945 silicone rubber Substances 0.000 description 6
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- 125000000524 functional group Chemical group 0.000 description 5
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- 239000005060 rubber Substances 0.000 description 2
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- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 description 1
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- 230000002411 adverse Effects 0.000 description 1
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- UCSBCWBHZLSFGC-UHFFFAOYSA-N tributoxysilane Chemical compound CCCCO[SiH](OCCCC)OCCCC UCSBCWBHZLSFGC-UHFFFAOYSA-N 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- OZWKZRFXJPGDFM-UHFFFAOYSA-N tripropoxysilane Chemical compound CCCO[SiH](OCCC)OCCC OZWKZRFXJPGDFM-UHFFFAOYSA-N 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a liquid silicone rubber with tackifying property on glass fiber base material and a preparation method thereof, wherein the liquid silicone rubber comprises the following components in percentage by mass: (0.6-1.5) A component and B component; the component A comprises the following components: 100 parts by weight of base material a and 1-2 parts by weight of catalyst; the component B comprises: 60 to 106 weight portions of base material b, 6 to 10 weight portions of cross-linking agent and 0.01 to 0.2 weight portion of cross-linking inhibitor; the mass ratio of the base material a is (1.2-1.8): 1 and white carbon black. The liquid silicone rubber with tackifying property for glass fiber base materials can realize good adhesion with the glass fiber base materials without adding an additional adhesion promoter or tackifier or primer, so that the problems of glue stock promotion, insufficient storage time and the like caused by the adhesion promoter or tackifier are avoided, convenience is brought to production, and the liquid silicone rubber is very suitable for production and application of glass fiber base material surface coating or mould pressing liquid silicone rubber products.
Description
Technical Field
The invention relates to the technical field of addition type liquid silicone rubber, in particular to liquid silicone rubber with tackifying property on glass fiber base materials and a preparation method thereof.
Background
The addition type liquid silicone rubber has simple injection molding process, rapid molding, no toxicity and no harm, and is widely applied to the fields of automobile parts, electronic appliances, industrial coating, infant products, tableware and the like. The adhesion of the addition type liquid silicone rubber with most of base materials is poor due to the inertia of the addition type liquid silicone rubber, and in order to improve the adhesion of the addition type liquid silicone rubber with the base materials, the surface of the adhesion base materials is pretreated in advance by using a primer in the prior art, so that the problems of complicated working procedures, environmental pollution and the like are caused; another common method is to add a tackifier to the liquid silicone rubber to improve its adhesion to the substrate, although simpler and more environmentally friendly than the primer method, the addition of the tackifier tends to have more or less impact on the size, including the flowability of the size, the transparency of the size, the storage stability of the size, and the like; considering how to start from the silicone rubber, the improvement of the adhesion of the silicone rubber to the base material is a good choice, so that the environment is protected, and the physical properties of the rubber material are not changed.
Industrial coating liquid silicone rubber is a liquid silicone rubber with wide application, such as wire and cable coating, glass fiber sleeve coating, glass fiber cloth coating and the like, wherein the liquid silicone rubber is often required to have good adhesion to glass fiber substrates, the traditional process is to improve the adhesion of the liquid silicone rubber and the glass fiber substrates by a primer or an adhesion promoter, and the traditional process is to use some epoxy or alkoxy adhesive additives or Si-H-based adhesives and the like, and the addition of the additives improves the adhesion of the liquid silicone rubber and the glass fiber substrates, but reduces the flowability or physical and mechanical strength of the rubber, and has adverse effects on the production and strength of products. Therefore, it is necessary to design a liquid silicone rubber with increased viscosity to a glass fiber substrate and a preparation method thereof.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the invention provides the liquid silicone rubber with the viscosity increasing effect on the glass fiber base material and the preparation method thereof, and the liquid silicone rubber with the viscosity increasing effect on the glass fiber base material can realize good adhesion with the glass fiber base material without adding an adhesive auxiliary agent or a tackifier or a primer, so that the problems of glue stock promotion, insufficient storage time and the like caused by the adhesive auxiliary agent or the tackifier are avoided, convenience is brought to production, and the liquid silicone rubber is very suitable for production and application of glass fiber base material surface coating or mould pressing liquid silicone rubber products.
In order to achieve the above purpose, the present invention provides the following technical solutions: a liquid silicone rubber with tackifying property on glass fiber base material comprises the following components in percentage by mass: (0.6-1.5) A component and B component;
The component A comprises the following components: 100 parts by weight of base material a and 1-2 parts by weight of catalyst;
the component B comprises the following components: 60 to 106 weight portions of base material b, 6 to 10 weight portions of cross-linking agent and 0.01 to 0.2 weight portion of cross-linking inhibitor;
the base material a comprises the following components in percentage by mass (1.2-1.8): 1 and white carbon black;
The base material b comprises the following components in percentage by mass (0.6-1.2): 1 and white carbon black;
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 1000-20000 mpa.s;
The vinyl alkoxy polysiloxane in the base material b is alpha, omega-divinyl polydimethylsiloxane with an alkoxy group on a side chain, and the viscosity of the vinyl alkoxy polysiloxane is 1000-20000 mpa.s at 25 ℃;
The vinyl alkoxy polysiloxane in the base material b is prepared by synthesizing an intermediate product through the hydrosilylation of tetramethyl tetra-vinyl cyclotetrasiloxane and trimethoxy silane, and then ring-opening with octamethyl cyclotetrasiloxane and a vinyl double-end socket to synthesize the corresponding vinyl methoxy polysiloxane;
the mol content of methoxy in the vinyl methoxy 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 gas phase white carbon black, and the specific surface area of the hydrophobic gas phase white carbon black is 100-350 m 2/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 ethynyl cyclohexanol.
The invention also provides a preparation method of the liquid silicone rubber with tackifying property on the glass fiber base material, which comprises the following steps:
1) Mixing vinyl polysiloxane, white carbon black, hexamethyldisilazane and water, mixing to remove hexamethyldisilazane and water to obtain a base material a, mixing vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, 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 mixing the base material B obtained in the step 1) with a crosslinking agent and a crosslinking inhibitor to obtain a component B;
3) The component A and the component B are mixed according to the mass ratio of 1: (0.6-1.5) and mixing to obtain the liquid silicone rubber with tackifying property to glass fiber base material.
The beneficial effects of the invention are as follows:
1. the liquid silicone rubber with tackifying property for the glass fiber base material can realize good adhesion with the glass fiber base material without adding an additional adhesion promoter or tackifier or primer, so that the problems of glue stock promotion, insufficient storage time and the like caused by the adhesion promoter or tackifier are avoided, convenience is brought to production, and the liquid silicone rubber is very suitable for production and application of coating or molding the surface of the glass fiber base material;
2. The preparation method provided by the invention is simple and stable, does not need to additionally add bonding auxiliary agents, has low cost, and is suitable for large-scale production and application.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in various different ways 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," and the like are merely for convenience of description and to simplify the description, and do not denote or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature.
The technical scheme of the invention is clearly and completely described below.
The invention provides the following technical scheme: a liquid silicone rubber with tackifying property on glass fiber base material comprises the following components in percentage by mass: (0.6-1.5) A component and B component;
The component A comprises the following components: 100 parts by weight of base material a and 1-2 parts by weight of catalyst;
the component B comprises the following components: 60 to 106 weight portions of base material b, 6 to 10 weight portions of cross-linking agent and 0.01 to 0.2 weight portion of cross-linking inhibitor;
the base material a comprises the following components in percentage by mass (1.2-1.8): 1 and white carbon black;
The base material b comprises the following components in percentage by mass (0.6-1.2): 1 and white carbon black.
In the invention, the liquid silicone rubber with tackifying property to the glass fiber base material comprises the following components in percentage by mass: the component A and the component B (0.6 to 1.5) preferably comprise the following components in percentage by mass: the component A and the component B of the component 1; wherein, the A component comprises: 100 parts by weight of base material a and 1-2 parts by weight of catalyst;
the component B comprises the following components: 60 to 106 parts of base material b, 6 to 10 parts of cross-linking agent and 0.01 to 0.2 part of cross-linking inhibitor.
In the invention, the base material a consists of the following components in percentage by mass (1.2-1.8): 1 and white carbon black, preferably consisting of a mass ratio of 1.6:1 and white carbon black; the base material b consists of (0.6-1.2) 1 mass ratio of vinyl alkoxy polysiloxane and white carbon black, preferably 1.0:1 mass ratio of vinyl alkoxy polysiloxane and white carbon black.
In the present invention, the vinyl polysiloxane in the base material a is preferably α, ω -divinyl polydimethylsiloxane, and the viscosity of the α, ω -divinyl polydimethylsiloxane is preferably 1000 to 20000mpa.s, more preferably 1000 to 10000mpa.s at 25 ℃; the vinyl alkoxy polysiloxane in the base material b is preferably alpha, omega-divinyl polydimethyl alkoxy siloxane containing methoxy, more preferably the methoxy mole content is 0.01-0.015 mmol/g, and more preferably the viscosity is 10000-15000 mPa.s at 25 ℃.
In a preferred embodiment of the invention, the α, ω -divinyl polydimethylsiloxane in the base a has a viscosity of 1000 mpa.s at 25 ℃ and the α, ω -divinyl polydimethyl alkoxy siloxane in the base b has a viscosity of 10000mpa.s at 25 ℃ and a methoxy molar content of 0.01mmol/g; in another preferred embodiment of the invention, the α, ω -divinyl dimethicone in base a has a viscosity of 10000mpa.s at 25 ℃, the α, ω -divinyl dimethicone in base b has a viscosity of 12000mpa.s at 25 ℃ and a methoxy molar content of 0.013 mmol/g. The source of the vinyl polysiloxane is not particularly limited, and commercially available α, ω -divinyl polydimethylsiloxane as described above, which is well known to those skilled in the art, may be employed in the present invention.
In the invention, the white carbon black in the base material is preferably hydrophobic fumed white carbon black; the specific surface area of the hydrophobic fumed silica is preferably 100-250 m 2/g, more preferably 100-150 m 2/g.
In a preferred embodiment of the invention, the specific surface area of the hydrophobic fumed silica is 100m 2/g; in another preferred embodiment of the invention, the specific surface area of the hydrophobic fumed silica is 150m 2/g. The source of the white carbon black is not particularly limited, and commercially available products or self-made products of the above-mentioned hydrophobic vapor phase white carbon black 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 material 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 is not particularly limited in the present invention, and commercially available products of the above-mentioned platinum catalyst, which are well known to those skilled in the art, may be used.
In the present invention, the A component comprises 1 to 2 parts by weight of a catalyst, preferably 1.5 parts by weight.
In the present invention, the base material B in the B component is different from the vinyl polysiloxane used in the base material a in the above-mentioned A component, and is specifically described herein.
In the invention, the component B comprises 60 to 106 parts by weight of 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 ring-opening condensation of 1, 3-divinyl-2, 4-dimethoxy tetramethyl cyclotetrasiloxane and octamethyl cyclotetrasiloxane under the catalysis of alkali and end-capping of vinyl double end caps, so that alkoxy functional groups are successfully introduced into a vinyl polysiloxane main chain; wherein the 1, 3-divinyl-2, 4-dimethoxy tetramethyl cyclotetrasiloxane is obtained by hydrosilylation of tetramethyl tetravinyl cyclotetrasiloxane and trimethoxy hydrosilane; wherein the trimethoxy silane is any one of triethoxy silane, tripropoxy silane and tributoxy silane, and preferably trimethoxy silane. The sources of the trimethoxy hydrosilane, octamethyl cyclotetrasiloxane, vinyl double-headed and the like are not particularly limited, and the commercial products mentioned above, which are well known to those skilled in the art, may be used in the present invention.
In a preferred embodiment of the invention, the vinyl alkoxy polysiloxane is preferably a vinyl methoxy polysiloxane, more preferably having a methoxy molar content of 0.013mmol/g and a viscosity of 12000mPa.s at 25 ℃.
According to the invention, the polarity of vinyl polysiloxane molecules is greatly increased by introducing functional groups such as alkoxy and the like into the vinyl polysiloxane main chain, and the alkoxy functional groups can have similar compatibility with the polar groups on the surface of the glass fiber substrate under the action of high temperature, so that the vinyl polysiloxane main chain and the vinyl polysiloxane main chain are well bonded.
In the invention, the weight part of the base material B in the component B is 60-106 weight parts, preferably 90.94-95.94 weight parts, wherein the mass ratio of the vinyl alkoxy polysiloxane to the white carbon black is (0.6-1.2): 1, wherein preferably 1.0:1, more preferably vinylmethoxy polysiloxane, wherein the molar content of methoxy groups in the vinylmethoxy polysiloxane is in the range of 0.001 to 0.02mmol/g, preferably 0.01 to 0.015 mmol/g.
The invention realizes good adhesion of the liquid silicone rubber and the glass fiber base material by adjusting the molar content of the 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 hydrogen-containing silicone oil; the hydrogen content of the hydrogen-containing silicone oil is preferably 0.1 to 1.0wt%, more preferably 0.5wt%. The source of the crosslinking agent is not particularly limited, and commercially available products of the above-mentioned hydrogen-containing silicone oils, which are well known to those skilled in the art, may 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 of methylbutinol and ethynyl cyclohexanol, more preferably ethynyl cyclohexanol. The source of the crosslinking inhibitor is not particularly limited in the present invention, and commercially available products of the above-mentioned methylbutinol and ethynyl cyclohexanol, which are well known to those skilled in the art, may be employed.
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, the polarity of vinyl polysiloxane molecules is greatly increased by introducing functional groups such as alkoxy and the like into the vinyl polysiloxane main chain, and the alkoxy functional groups can have similar compatibility with the polar groups on the surface of the glass fiber substrate under the action of high temperature, so that the vinyl polysiloxane main chain and the polar groups can be well bonded, and the vinyl polysiloxane main chain are very suitable for the production of glass fiber coating liquid silicone rubber products.
The invention also provides a preparation method of the liquid silicone rubber with tackifying property on the glass fiber base material, which comprises the following steps:
1) Mixing vinyl polysiloxane, white carbon black, hexamethyldisilazane and water, mixing to remove hexamethyldisilazane and water to obtain a base material a, mixing vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, 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 mixing the base material B obtained in the step 1) with a crosslinking agent and a crosslinking inhibitor to obtain a component B;
3) The component A and the component B are mixed according to the mass ratio of 1: (0.6-1.5) and mixing to obtain the liquid silicone rubber with tackifying property to glass fiber base material.
Firstly, mixing vinyl polysiloxane/vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, and carrying out mixing to remove the hexamethyldisilazane and the water to obtain a 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 will not be described herein.
In the invention, the mass ratio of vinyl polysiloxane, white carbon black, hexamethyldisilazane and water in the base material a is preferably (1.2-1.8): 1: (0.2-0.3): (0.04 to 0.06), more preferably 1.6:1:0.25:0.05; the mass ratio of the vinyl alkoxy polysiloxane, 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 apparatus for the mixing and subsequent kneading is not particularly limited, and a kneader known to those skilled in the art may be used.
In the present invention, the mixing process is preferably specifically:
Kneading the mixture for 2-3 hours at 20-30 ℃ in advance, then heating to 95-105 ℃ to continue kneading for 0.4-0.6 hour, and then heating to 135-150 ℃ to perform vacuum kneading for 2-4 hours to obtain a base material;
More preferably:
Kneading the mixed material for 2.5 hours at 25 ℃, then heating to 100 ℃ to continue kneading for 0.5 hour, and then heating to 140-150 ℃ to perform vacuum kneading for 3 hours to obtain a base material; in the present invention, the vacuum degree of the vacuum kneading is preferably 0.08 to 0.1MPa. The invention adopts the mixing process to ensure that the vinyl polysiloxane and the white carbon black are uniformly kneaded, and simultaneously remove low volatile matters such as hexamethyldisilazane, water and the like.
After the base material is obtained, the obtained base material a is mixed with a catalyst to obtain a component A; and mixing the obtained base material B with a cross-linking agent and a cross-linking inhibitor to obtain a component B. The specific process of mixing the base material a with the catalyst and the specific process of mixing the base material B with the cross-linking agent and the cross-linking inhibitor are not particularly limited, and the technical scheme of mechanical stirring or manual stirring, which are well known to those skilled in the art, can be adopted, so that each component in the component A and each component in the component B are uniformly mixed 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 A component and the B component are mixed according to the mass ratio of 1:1, and obtaining the liquid silicone rubber. The specific process of mixing the component A and the component B is not particularly limited, and the technical scheme of mechanical stirring or manual stirring 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 with tackifying property on glass fiber base materials, which comprises the following components in percentage by mass: (0.6-1.5) A component and B component; the component A comprises the following components: 100 parts by weight of base material a and 1-2 parts by weight of catalyst; the component B comprises the following components: 60 to 106 parts of base material b, 6 to 10 parts of cross-linking agent and 0.01 to 0.2 part of cross-linking inhibitor. The base material a comprises the following components in percentage by mass (1.2-1.8): 1 and white carbon black; the base material b consists of vinyl alkoxy polysiloxane and white carbon black with the mass ratio of (0.6-1.2) 1.
Compared with the prior art, the liquid silicone rubber with tackifying property for the glass fiber substrate can realize good adhesion with the glass fiber substrate without adding an additional adhesion promoter or tackifier or primer, so that the problems of glue stock promotion, insufficient storage time and the like caused by the adhesion promoter or tackifier are avoided, convenience is brought to production, and the liquid silicone rubber is very suitable for production and 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 bonding auxiliary agents, has low cost, and is suitable for large-scale production and application.
In order to further illustrate the present invention, the following examples are provided. The raw materials used in the following examples of the present invention are all commercially available.
Example 1
1) Preparation of base a: 80 parts by weight of alpha, omega-divinyl polydimethylsiloxane with viscosity (25 ℃) of 1000mPa.s, 50 parts by weight of hydrophobic fumed silica with specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hour at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (vacuum degree of 0.08-0.1 MPa) to obtain a base material a;
2) Preparation of base material b: 30 parts by weight of alpha, omega-divinyl polydimethyl trimethoxysiloxane (the methoxy molar content is 0.01 mmol/g) with the viscosity of 10000 Pa.s (25 ℃) and 50 parts by weight of hydrophobic gas phase white carbon black with the specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hours at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (the vacuum degree is 0.08-0.1 MPa), so as to obtain a base material b;
3) And (3) preparation of the component A: taking 100g of the base material a obtained in the step 1), adding 1g of a catalyst, and stirring for 10-30 min to obtain the component A.
4) And (3) preparation of a component B: 90.94g of the base material B obtained in the step 2), 6g of hydrogen-containing silicone oil (hydrogen content is 0.5%) and 0.06g of ethynyl cyclohexanol are taken and stirred for 10-30 min, so that a component B is obtained.
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
Example 2
1) Preparation of base a: as in example 1;
2) Preparation of base material b: 40 parts by weight of alpha, omega-divinyl polydimethyl trimethoxysiloxane (the methoxy molar content is 0.01 mmol/g) with the viscosity of 10000 Pa.s (25 ℃) and 50 parts by weight of hydrophobic fumed silica with the specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hours at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (the vacuum degree is 0.08-0.1 MPa), so as to obtain a base material b;
3) And (3) preparation of the component A: as in example 1;
4) And (3) preparation of a component B: as in example 1;
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
Example 3
1) Preparation of base a: as in example 1;
2) Preparation of base material b: 50 parts by weight of alpha, omega-divinyl polydimethyl trimethoxysiloxane (the methoxy molar content is 0.01 mmol/g) with the viscosity of 10000 Pa.s (25 ℃) and 50 parts by weight of hydrophobic gas phase white carbon black with the specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hours at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (the vacuum degree is 0.08-0.1 MPa), so as to obtain a base material b;
3) And (3) preparation of the component A: as in example 1;
4) And (3) preparation of a component B: as in example 1;
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
Example 4
1) Preparation of base a: as in example 1;
2) Preparation of base material b: 60 parts by weight of alpha, omega-divinyl polydimethyl trimethoxysiloxane (the methoxy molar content is 0.01 mmol/g) with the viscosity of 10000 Pa.s (25 ℃) and 50 parts by weight of hydrophobic gas phase white carbon black with the specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hours at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (the vacuum degree is 0.08-0.1 MPa), so as to obtain a base material b;
3) And (3) preparation of the component A: as in example 1;
4) And (3) preparation of a component B: as in example 1;
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
Example 5
1) Preparation of base a: as in example 1;
2) Preparation of base material b: 50 parts by weight of alpha, omega-divinyl polydimethyl trimethoxysiloxane (the methoxy molar content is 0.012 mmol/g) with the viscosity of 10000 Pa.s (25 ℃) and 50 parts by weight of hydrophobic gas phase white carbon black with the specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hours at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (the vacuum degree is 0.08-0.1 MPa), so as to obtain a base material b;
3) And (3) preparation of the component A: as in example 1;
4) And (3) preparation of a component B: as in example 1;
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
Example 6
1) Preparation of base a: as in example 1;
2) Preparation of base material b: 50 parts by weight of alpha, omega-divinyl polydimethyl trimethoxysiloxane (the methoxy molar content is 0.015 mmol/g) with the viscosity of 10000 Pa.s (25 ℃) and 50 parts by weight of hydrophobic fumed silica with the specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hours at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (the vacuum degree is 0.08-0.1 MPa), so as to obtain a base material b;
3) And (3) preparation of the component A: as in example 1;
4) And (3) preparation of a component B: as in example 1;
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
Example 7
1) Preparation of base a: as in example 1;
2) Preparation of base material b: 50 parts by weight of alpha, omega-divinyl polydimethylsiloxane (the molar content of methoxy is 0.015 mmol/g) with the viscosity of 15000mPa.s (25 ℃) and 50 parts by weight of hydrophobic gas phase white carbon black with the specific surface area of 150m 2/g are put into a kneader, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are kneaded for 2.5 hours at 25 ℃, then the temperature is raised to 100 ℃ for continuous kneading for 0.5 hours, and then the temperature is raised to 140-150 ℃ for kneading for 3 hours under vacuum (the vacuum degree is 0.08-0.1 MPa), so as to obtain a base material b;
3) And (3) preparation of the component A: as in example 1;
4) And (3) preparation of a component B: as in example 1;
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
Example 8
1) Preparation of base a: as in example 1;
2) Preparation of base material b: 50 parts by weight of alpha, omega-divinyl polydimethylsiloxane with viscosity (25 ℃) of 15000mPa.s, 50 parts by weight of hydrophobic fumed silica with specific surface area of 150m 2/g, 10 parts by weight of hexamethyldisilazane and 2 parts by weight of water are put into a kneader, kneaded for 2.5 hours at 25 ℃, then continuously kneaded for 0.5 hour at 100 ℃, and then kneaded for 3 hours at 140-150 ℃ under vacuum (vacuum degree of 0.08-0.1 MPa) to obtain a base material b;
3) And (3) preparation of the component A: as in example 1;
4) And (3) preparation of a component B: as in example 1;
5) Preparation of liquid silicone rubber with tackifying properties for glass fiber substrates: and (2) 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.
The liquid silicone rubber with tackifying property on glass fiber base materials prepared in the embodiments 1 to 8 of the invention is tested for various properties, including adhesion test on glass fiber base materials, and the test method is as follows: the liquid silicone rubber sizing material prepared by mixing the AB components is coated on the surface of the glass fiber substrate in advance, then baked for 10min in a baking oven at 150 ℃, and the bonding strength is measured, and the results are shown in tables 1-2.
TABLE 1 various performance data of liquid Silicone rubbers prepared in examples 1 to 8 of the present invention
As can be seen from table 1:
1) As can be seen from comparative examples 1 to 4, as the amount of α, ω -divinyl polydimethylsiloxane in the base material b increases, the adhesion strength of the silicone rubber to the glass fiber substrate increases gradually, and the degree of cohesive failure between each other increases gradually, which means that as the amount of trimethoxy increases, the adhesion of the silicone rubber to the glass fiber substrate increases gradually, and the tensile strength and tear strength also increase gradually, mainly due to the gradual increase of the cohesive force between polysiloxane molecules after the introduction of the trimethoxy group, resulting in a corresponding increase in tensile strength and tear strength, and also due to the increase of cohesive force between the molecules, resulting in a corresponding decrease in exercise elongation;
2) As can be seen from comparing examples 3, 5 and 6, as the molar content of trimethoxy in the molecule increases, the adhesion of the silicone rubber to the glass fiber substrate gradually increases, and the cohesive failure reaches 100% in example 6;
3) As can be seen from comparison of examples 6 and 7, the physical combination of the silicone rubber is improved with an increase in the viscosity of the α, ω -divinyl polydimethylsiloxane, with the best results in example 7, 100% cohesive failure, and the best physical mechanical properties.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A liquid silicone rubber with tackifying property on glass fiber base material is characterized by comprising the following components in percentage by mass: (0.6-1.5) A component and B component;
The component A comprises the following components: 100 parts by weight of base material a and 1-2 parts by weight of catalyst;
the component B comprises the following components: 60 to 106 weight portions of base material b, 6 to 10 weight portions of cross-linking agent and 0.01 to 0.2 weight portion of cross-linking inhibitor;
the base material a comprises the following components in percentage by mass (1.2-1.8): 1 and white carbon black;
The base material b comprises the following components in percentage by mass (0.6-1.2): 1 and white carbon black;
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 1000-20000 mpa.s;
The vinyl alkoxy polysiloxane in the base material b is alpha, omega-divinyl polydimethylsiloxane with an alkoxy group on a side chain, and the viscosity of the vinyl alkoxy polysiloxane is 1000-20000 mpa.s at 25 ℃;
The vinyl alkoxy polysiloxane in the base material b is prepared by synthesizing an intermediate product through the hydrosilylation of tetramethyl tetra-vinyl cyclotetrasiloxane and trimethoxy silane, and then ring-opening with octamethyl cyclotetrasiloxane and a vinyl double-end socket to synthesize the corresponding vinyl methoxy polysiloxane;
the mol content of methoxy in the vinyl methoxy polysiloxane is 0.001-0.02 mmol/g.
2. The liquid silicone rubber with tackifying properties for glass fiber substrates according to claim 1, wherein the white carbon black in the base material a and the base material b is hydrophobic vapor phase white carbon black, and the specific surface area of the hydrophobic vapor phase white carbon black is 100-350 m 2/g.
3. The liquid silicone rubber with tackifying properties to glass fiber substrates according to claim 1, wherein the catalyst is a platinum catalyst having a platinum content of 2500-6000 ppm.
4. The liquid silicone rubber with tackifying property to glass fiber base material according to claim 1, wherein the crosslinking agent is hydrogen-containing silicone oil, and the hydrogen content of the hydrogen-containing silicone oil is 0.3-1.5 wt%.
5. A liquid silicone rubber having a tackiness to a glass fiber substrate according to claim 1, wherein said crosslinking inhibitor is selected from any one of methylbutinol and ethynyl cyclohexanol.
6. A method of preparing a liquid silicone rubber having a tackifying property for fiberglass substrates as claimed in any one of claims 1-5, comprising the steps of:
1) Mixing vinyl polysiloxane, white carbon black, hexamethyldisilazane and water, mixing to remove hexamethyldisilazane and water to obtain a base material a, mixing vinyl alkoxy polysiloxane, white carbon black, hexamethyldisilazane and water, 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 mixing the base material B obtained in the step 1) with a crosslinking agent and a crosslinking inhibitor to obtain a component B;
3) The component A and the component B are mixed according to the mass ratio of 1: (0.6-1.5) and mixing to obtain the liquid silicone rubber with tackifying property to glass fiber base material.
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