CN114316894A - High-temperature-resistant silica gel protective film and preparation method thereof - Google Patents
High-temperature-resistant silica gel protective film and preparation method thereof Download PDFInfo
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- CN114316894A CN114316894A CN202111634756.8A CN202111634756A CN114316894A CN 114316894 A CN114316894 A CN 114316894A CN 202111634756 A CN202111634756 A CN 202111634756A CN 114316894 A CN114316894 A CN 114316894A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 239000000741 silica gel Substances 0.000 title claims abstract description 139
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 139
- 230000001681 protective effect Effects 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 19
- 239000002683 reaction inhibitor Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000007822 coupling agent Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 51
- 229920002554 vinyl polymer Polymers 0.000 claims description 49
- -1 polysiloxane Polymers 0.000 claims description 34
- 229920001296 polysiloxane Polymers 0.000 claims description 27
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 239000010703 silicon Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 229920002050 silicone resin Polymers 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims 1
- 239000013464 silicone adhesive Substances 0.000 claims 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims 1
- 230000009194 climbing Effects 0.000 abstract description 7
- 238000010030 laminating Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract description 2
- 238000004132 cross linking Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001723 curing Methods 0.000 description 5
- UEXCJVNBTNXOEH-UHFFFAOYSA-N Ethynylbenzene Chemical group C#CC1=CC=CC=C1 UEXCJVNBTNXOEH-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- BPSIOYPQMFLKFR-VIFPVBQESA-N trimethoxy-[3-[[(2r)-oxiran-2-yl]methoxy]propyl]silane Chemical compound CO[Si](OC)(OC)CCCOC[C@H]1CO1 BPSIOYPQMFLKFR-VIFPVBQESA-N 0.000 description 2
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- ZDWQSEWVPQWLFV-UHFFFAOYSA-N C(CC)[Si](OC)(OC)OC.[O] Chemical compound C(CC)[Si](OC)(OC)OC.[O] ZDWQSEWVPQWLFV-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 108010025899 gelatin film Proteins 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920006268 silicone film Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
The invention provides a high-temperature-resistant silica gel protective film which comprises a silica gel layer, wherein the silica gel layer comprises the following raw materials in parts by weight: 100 parts of low-viscosity silica gel; 0-100 parts of high-viscosity silica gel; 0.5-1.5 parts by weight of a crosslinking agent; 0.5-1 part by weight of platinum catalyst; 0.05 to 0.1 portion of reaction inhibitor; 0.5-1 part by weight of coupling agent; 100 portions and 200 portions of solvent. The invention also provides a preparation method. Through the addition of low-viscosity silica gel and the optimization of the using amount of the low-viscosity silica gel, the silica gel layer has viscosity, and in addition, the protective film prepared by laminating the silica gel layer on the base material has good exhaust performance and can dissipate heat in time, so that the high temperature resistance of the silica gel protective film is improved, the peeling force climbing degree of the protective film in a high-temperature environment of about 70 ℃ is reduced, and the follow-up protective film is prevented from being difficult to tear after being applied to a product and subjected to high temperature.
Description
Technical Field
The invention relates to the technical field of films, in particular to a high-temperature-resistant silica gel protective film and a preparation method thereof.
Background
The silica gel membrane is a membrane structure formed by using silica gel materials, has the advantages of high toughness, impact resistance and difficult deformation, and is widely applied to the packaging of various products. However, the existing silica gel film has poor high temperature resistance, and the phenomenon of obvious peeling force climbing is easily generated after high temperature, so that the follow-up protective film is difficult to tear off.
Disclosure of Invention
In order to achieve the above object, the present invention is achieved by the following technical solutions.
The invention provides a high-temperature-resistant silica gel protective film which comprises a silica gel layer, wherein the silica gel layer comprises the following raw materials in parts by weight:
preferably, the low-viscosity silica gel is vinyl polysiloxane, and the vinyl content is 0.15% -0.25%;
the general structural formula of the vinyl polysiloxane is as follows:
R(CH3)2SiO[Si(CH3)2O]n[Si(CH3)(CH=CH2)O]mSi(CH3)2R, wherein R is vinyl.
Preferably, the high-viscosity silica gel is prepared by mixing the following components in a weight ratio of 1: 2-4 mixtures of vinyl polysiloxanes with methyl MQ silicone resins; wherein the molar ratio of M groups to Q groups in the methyl MQ silicon resin is 0.6-0.8.
Preferably, the molecular weight of the vinylpolysiloxane is 100000-300000.
Preferably, the cross-linking agent is hydrogen-based silicone oil containing terminal hydrogen groups or terminal hydrogen groups; wherein, the hydrogen content is 0.5 to 2 percent.
Preferably, the platinum catalyst is a platinum-a, w-bis (n-octyl) polymethylvinylsiloxane complex; wherein the platinum content is 3000ppm-4000 ppm.
Preferably, the reaction inhibitor is an alkynol catalytic reaction inhibitor.
Preferably, the silane coupling agent is at least one selected from r-glycidoxypropyltrimethoxysilane and r-methacryloxypropyltrimethoxysilane.
Preferably, the solvent is selected from at least one of toluene, xylene and ethyl acetate.
The invention also provides a preparation method of the high-temperature-resistant silica gel protective film, which comprises the following steps:
s1, weighing low-viscosity silica gel, high-viscosity silica gel, a cross-linking agent, a platinum catalyst, a reaction inhibitor, a coupling agent and a solvent according to the measurement;
s2, mixing and stirring the low-viscosity silica gel, the high-viscosity silica gel and the solvent;
s3, adding a cross-linking agent, a platinum catalyst, a reaction inhibitor and a coupling agent into the mixed solution prepared in the step S2, and uniformly stirring to prepare a silica gel liquid;
and S4, coating the silica gel glue solution prepared in the step S3 on a base material, and heating and curing to obtain the silica gel protective film.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a high-temperature-resistant silica gel protective film, which is characterized in that a silica gel layer has viscosity through the addition of low-viscosity silica gel and the optimization of the dosage of the low-viscosity silica gel, and in addition, the protective film prepared by coating the silica gel layer on a base material has good exhaust performance and can dissipate heat in time, so that the high temperature resistance of the silica gel protective film is improved, the peeling force climbing degree of the protective film in a high-temperature environment of about 70 ℃ is reduced, and the problem that the subsequent protective film is difficult to tear after being applied to a product and subjected to high temperature is avoided.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood and to be implemented according to the content of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings. The detailed description of the present invention is given in detail by the following examples and the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 is a flow chart of the steps of the preparation method of the present invention.
Detailed Description
The foregoing and other objects, features, aspects and advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings, which will enable those skilled in the art to practice the present invention with reference to the accompanying specification. In the drawings, the shape and size may be exaggerated for clarity, and the same reference numerals will be used throughout the drawings to designate the same or similar components. In the following description, terms such as center, thickness, height, length, front, back, rear, left, right, top, bottom, upper, lower, and the like are used based on the orientation or positional relationship shown in the drawings. In particular, "height" corresponds to the dimension from top to bottom, "width" corresponds to the dimension from left to right, and "depth" corresponds to the dimension from front to back. These relative terms are for convenience of description and are not generally intended to require a particular orientation. Terms concerning attachments, coupling and the like (e.g., "connected" and "attached") refer to a relationship wherein structures are secured or attached, either directly or indirectly, to one another through intervening structures, as well as both movable or rigid attachments or relationships, unless expressly described otherwise.
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
The invention provides a high-temperature-resistant silica gel protective film which comprises a silica gel layer, wherein the silica gel layer comprises the following raw materials in parts by weight:
in the embodiment, the silica gel layer has viscosity by adding the low-viscosity silica gel and optimizing the using amount of the low-viscosity silica gel, and in addition, the protective film prepared by laminating the silica gel layer on the base material has good exhaust performance, can dissipate heat in time, further improves the high temperature resistance of the silica gel protective film, reduces the climbing degree of the peeling force of the protective film in a high-temperature environment of about 70 ℃, and avoids the problem that the subsequent protective film is difficult to tear after being applied to a product at high temperature. The initial viscosity and the stripping force of the prepared silica gel layer are improved by adding the high-viscosity silica gel and optimizing the dosage of the high-viscosity silica gel.
In one embodiment, the low-viscosity silica gel has a viscosity of 0.1-1.5 g/inc; the viscosity of the high-viscosity silica gel to the steel plate is 700-800 g/inc.
In one embodiment, the low viscosity silica gel is vinyl polysiloxane, and the vinyl content is 0.15% -0.25%;
the general structural formula of the vinyl polysiloxane is as follows:
R(CH3)2SiO[Si(CH3)2O]n[Si(CH3)(CH=CH2)O]mSi(CH3)2R, wherein R is vinyl. Specifically, m in the structural general formula of the vinyl polysiloxane is related to the content of vinyl, and n is related to the molecular weight of the vinyl polysiloxane. The vinyl polysiloxane contains terminal vinyl groups for the crosslinking reaction. When the vinyl content is within the range of 0.15-0.25%, the crosslinking degree is controlled, and the high temperature resistance of the silica gel protective film is improved. Furthermore, the content of vinyl is 0.18-0.22%, the molecular network structure of the product is compact, the high temperature resistance effect is achieved, and the climbing of the viscosity between the product and a stuck object is small.
In one embodiment, the high-viscosity silica gel is prepared by mixing the following components in a weight ratio of 1: 2-4 mixtures of vinyl polysiloxanes with methyl MQ silicone resins; wherein the molar ratio of M groups to Q groups in the methyl MQ silicon resin is 0.6-0.8. The vinyl content of the high-viscosity silica gel is identical to that of the low-viscosity silica gel. Specifically, the tackifying effect is achieved by adding 2-4 parts of methyl MQ silicone resin to 1 part of vinyl polysiloxane. Further, the molar ratio of the M groups to the Q groups in the methyl MQ silicone resin is 0.6-0.7.
Further, the molecular weight of the vinyl polysiloxane in the low-viscosity silica gel and/or the high-viscosity silica gel is 100000-300000 so as to improve the high-temperature resistance of the silica gel.
In one embodiment, the crosslinking agent is hydrogen-based silicone oil containing terminal hydrogen groups or terminal hydrogen groups to perform a crosslinking reaction with vinyl groups; wherein, the hydrogen content is 0.5 to 2 percent. Further, the hydrogen content is 0.6-1.5%. More preferably, the hydrogen radical content is from 0.8% to 1.2%. The curing effect is controlled by controlling the content of amino groups so as to fully cure.
In one embodiment, the platinum catalyst is a platinum-a, w-bis (n-octyl) polymethylvinylsiloxane complex; wherein the platinum content is 3000ppm-4000 ppm. Specifically, the platinum catalyst is prepared by carrying out coordination exchange on a Kaersi catalyst by using siloxane oligomer containing long-chain alkyl and vinyl, and can effectively catalyze addition reaction at the temperature of more than 80 ℃, improve the catalytic activity of the catalyst, accelerate crosslinking reaction and improve the reaction rate. Further, the platinum content is 3500ppm to 4000 ppm.
In one embodiment, the reaction inhibitor is an alkynol catalytic reaction inhibitor to inhibit the crosslinking reaction rate and allow sufficient coating time during the coating process of the silica gel glue prepared from the raw materials.
Further, the reaction inhibitor is at least one selected from phenylacetylene, 1-ethynyl-1-cyclohexanol, tetramethyltetravinylcyclotetrasiloxane, 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol, 3, 5-dimethyl-1-hexynyl-3-ol, and 3-methyl-1-dodecynyl-3-ol.
In one embodiment, the silane coupling agent is at least one selected from r-glycidoxypropyltrimethoxysilane and r-methacryloxypropyltrimethoxysilane, so as to increase the adhesion of the silica gel solution to the substrate during the coating process of the silica gel solution.
In one embodiment, the solvent is at least one selected from toluene, xylene and ethyl acetate, so that the prepared silica gel liquid has good dispersion uniformity and coating leveling property. Preferably, the solvent is a mixture of toluene and ethyl acetate.
The invention provides a preparation method of the high-temperature-resistant silica gel protective film, which comprises the following steps as shown in figure 1:
s1, weighing low-viscosity silica gel, high-viscosity silica gel, a cross-linking agent, a platinum catalyst, a reaction inhibitor, a coupling agent and a solvent according to the measurement;
s2, mixing and stirring the low-viscosity silica gel, the high-viscosity silica gel and the solvent;
s3, adding a cross-linking agent, a platinum catalyst, a reaction inhibitor and a coupling agent into the mixed solution prepared in the step S2, and uniformly stirring to prepare a silica gel liquid;
and S4, coating the silica gel glue solution prepared in the step S3 on a base material, and heating and curing to obtain the silica gel protective film.
Further, in step S4, heat curing is performed in the oven at a temperature of 150 ℃ and 160 ℃ for a curing time of 30-120S.
In order to illustrate the invention herein, specific examples are set forth below. It should be understood that these examples are for illustrative purposes only and are not to be construed as limiting the invention in any way.
Example 1
The invention provides a high-temperature-resistant silica gel protective film which comprises a silica gel layer, wherein the silica gel layer comprises the following raw materials in parts by weight:
wherein the low-viscosity silica gel is vinyl polysiloxane, the vinyl content is 0.2%, and the molecular weight of the vinyl polysiloxane of the low-viscosity silica gel is 200000; the weight ratio of the high-viscosity silica gel is 1: 3, the molar ratio of M groups to Q groups in the methyl MQ silicon resin is 0.7, the molecular weight of the vinyl polysiloxane of the high-viscosity silica gel is 200000, the vinyl content is 0.2%, and the molecular weight of the methyl MQ silicon resin is 5000.
The cross-linking agent is hydrogen-based silicone oil containing terminal hydrogen groups or terminal hydrogen groups; wherein the hydrogen radical content is 1%.
The platinum catalyst is a platinum-a, w-di (n-octyl) polymethylvinylsiloxane complex; wherein the platinum content is 3000 ppm.
The reaction inhibitor is phenylacetylene.
The coupling agent is r-glycidol ether oxygen propyl trimethoxy silane.
The solvent is xylene.
Preparing a silica gel protective film, comprising the following steps:
(1) weighing low-viscosity silica gel, high-viscosity silica gel, a cross-linking agent, a platinum catalyst, a reaction inhibitor, a coupling agent and a solvent according to the weight;
(2) mixing and stirring the low-viscosity silica gel, the high-viscosity silica gel and the solvent;
(3) adding a cross-linking agent, a platinum catalyst, a reaction inhibitor and a coupling agent into the mixed solution prepared in the step (2), and uniformly stirring to prepare a silica gel liquid;
(4) and (4) coating the silica gel glue solution prepared in the step (3) on a base material through a coating machine, coating the dry glue solution with the thickness of 10 mu m, crosslinking and curing at 160 ℃, and baking for 2min to prepare the silica gel protective film.
Example 2
The invention provides a high-temperature-resistant silica gel protective film which comprises a silica gel layer, wherein the silica gel layer comprises the following raw materials in parts by weight:
wherein the low-viscosity silica gel is vinyl polysiloxane, the vinyl content is 0.2%, and the molecular weight of the vinyl polysiloxane of the low-viscosity silica gel is 200000; the weight ratio of the high-viscosity silica gel is 1: 3, the molar ratio of M groups to Q groups in the methyl MQ silicon resin is 0.7, the molecular weight of the vinyl polysiloxane of the high-viscosity silica gel is 200000, the vinyl content is 0.2%, and the molecular weight of the methyl MQ silicon resin is 5000.
The preparation method and the rest process parameters are the same as the example 1.
Example 3
The invention provides a high-temperature-resistant silica gel protective film which comprises a silica gel layer, wherein the silica gel layer comprises the following raw materials in parts by weight:
wherein the low-viscosity silica gel is vinyl polysiloxane, the vinyl content is 0.2%, and the molecular weight of the vinyl polysiloxane of the low-viscosity silica gel is 200000; the weight ratio of the high-viscosity silica gel is 1: 3, the molar ratio of M groups to Q groups in the methyl MQ silicon resin is 0.7, the molecular weight of the vinyl polysiloxane of the high-viscosity silica gel is 200000, the vinyl content is 0.2%, and the molecular weight of the methyl MQ silicon resin is 5000.
The preparation method and the rest process parameters are the same as the example 1.
Example 4
The invention provides a high-temperature-resistant silica gel protective film which comprises a silica gel layer, wherein the silica gel layer comprises the following raw materials in parts by weight:
wherein the low-viscosity silica gel is vinyl polysiloxane, the vinyl content is 0.2%, and the molecular weight of the vinyl polysiloxane of the low-viscosity silica gel is 200000; the weight ratio of the high-viscosity silica gel is 1: 3, the molar ratio of M groups to Q groups in the methyl MQ silicon resin is 0.7, the molecular weight of the vinyl polysiloxane of the high-viscosity silica gel is 200000, the vinyl content is 0.2%, and the molecular weight of the methyl MQ silicon resin is 5000.
The preparation method and the rest process parameters are the same as the example 1.
Comparative example 1
A silica gel protective film, which is different from embodiment 1 in that: the vinyl content of the low-viscosity silica gel and the high-viscosity silica gel was 0.05%.
Comparative example 2
A silica gel protective film, which is different from embodiment 1 in that: the vinyl content of the low-viscosity silica gel and the high-viscosity silica gel is 0.1%.
Comparative example 3
A silica gel protective film, which is different from embodiment 1 in that: the vinyl content of the low-viscosity silica gel and the high-viscosity silica gel is 0.3%.
Example 5
The silicone protective films of examples 1 to 4 and comparative examples 1 and 3 were subjected to a 180 ° peel force test. And (3) testing by adopting a universal tensile machine according to the GBT-2791-.
Watch 1
As can be seen from the above Table I, in example 1, compared with example 2, the amount of the crosslinking agent is increased within the range, the influence on the peel strength is not large, the peel improvement at 70 ℃ is slightly increased, but the 44H climbing measured at 70 ℃ is still controlled within 50%.
As is clear from the comparison among examples 1, 3 and 4, the high viscosity silica gel was increased in the range, and the peel strength before and after the high temperature was improved, but the 44H climbing percentage at 70 ℃ was not much different.
As can be seen from the comparison between example 1 and comparative examples 1 to 3, the protective silicone film has the best high temperature resistance when the vinyl content of the low-viscosity silica gel and the high-viscosity silica gel is 0.15% to 0.25%.
In conclusion, the peeling force of the silica gel protective film provided by the invention rises to within 50% when the silica gel protective film is subjected to the ring test at 70 ℃ for 44H, so that the silica gel protective film is prevented from being difficult to tear due to high temperature in the application process.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can readily practice the invention as shown and described in the drawings and detailed description herein; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the scope of the invention as defined by the appended claims; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
2. the high temperature resistant silica gel protective film according to claim 1, wherein the low viscosity silica gel is vinyl polysiloxane, and the vinyl content is 0.15% -0.25%;
the general structural formula of the vinyl polysiloxane is as follows:
R(CH3)2SiO[Si(CH3)2O]n[Si(CH3)(CH=CH2)O]mSi(CH3)2R, wherein R is vinyl.
3. The high temperature resistant silica gel protective film according to claim 2, wherein the high viscosity silica gel is prepared by mixing the following components in a weight ratio of 1: 2-4 mixtures of vinyl polysiloxanes with methyl MQ silicone resins; wherein the molar ratio of M groups to Q groups in the methyl MQ silicon resin is 0.6-0.8.
4. The protective film according to claim 3, wherein the molecular weight of the vinylpolysiloxane in the low-viscosity silica gel and/or the high-viscosity silica gel is 100000-300000.
5. The high temperature resistant silicone adhesive protective film according to claim 1, wherein the cross-linking agent is hydrogen-based silicone oil containing terminal hydrogen groups or terminal hydrogen groups; wherein, the hydrogen content is 0.5 to 2 percent.
6. The high temperature resistant silica gel protective film according to claim 1, wherein the platinum catalyst is a platinum-a, w-di (n-octyl) polymethylvinylsiloxane complex; wherein the platinum content is 3000ppm-4000 ppm.
7. The high temperature resistant silica gel protective film according to claim 1, wherein the reaction inhibitor is an alkynol catalytic reaction inhibitor.
8. The protective film according to claim 1, wherein the silane coupling agent is at least one selected from the group consisting of gamma-glycidoxypropyltrimethoxysilane and gamma-methacryloxypropyltrimethoxysilane.
9. The high temperature resistant silica gel protective film according to claim 1, wherein the solvent is at least one selected from toluene, xylene, and ethyl acetate.
10. The method for preparing the high temperature resistant silica gel protective film according to any one of claims 1 to 9, comprising the following steps:
s1, weighing low-viscosity silica gel, high-viscosity silica gel, a cross-linking agent, a platinum catalyst, a reaction inhibitor, a coupling agent and a solvent according to the measurement;
s2, mixing and stirring the low-viscosity silica gel, the high-viscosity silica gel and the solvent;
s3, adding a cross-linking agent, a platinum catalyst, a reaction inhibitor and a coupling agent into the mixed solution prepared in the step S2, and uniformly stirring to prepare a silica gel liquid;
and S4, coating the silica gel glue solution prepared in the step S3 on a base material, and heating and curing to obtain the silica gel protective film.
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CN202111634756.8A CN114316894A (en) | 2021-12-29 | 2021-12-29 | High-temperature-resistant silica gel protective film and preparation method thereof |
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CN113388362A (en) * | 2021-07-22 | 2021-09-14 | 江苏斯迪克新材料科技股份有限公司 | Low-climbing organic silicon pressure-sensitive adhesive and preparation method and application thereof |
CN113845860A (en) * | 2021-09-27 | 2021-12-28 | 江苏斯迪克新材料科技股份有限公司 | Silica gel protective film and preparation method thereof |
CN113845861A (en) * | 2021-09-30 | 2021-12-28 | 苏州世华新材料科技股份有限公司 | Low-climbing organic silicon protective film and preparation method thereof |
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CN113388362A (en) * | 2021-07-22 | 2021-09-14 | 江苏斯迪克新材料科技股份有限公司 | Low-climbing organic silicon pressure-sensitive adhesive and preparation method and application thereof |
CN113845860A (en) * | 2021-09-27 | 2021-12-28 | 江苏斯迪克新材料科技股份有限公司 | Silica gel protective film and preparation method thereof |
CN113845861A (en) * | 2021-09-30 | 2021-12-28 | 苏州世华新材料科技股份有限公司 | Low-climbing organic silicon protective film and preparation method thereof |
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