CN112708396A - Preparation of integrated black silica gel OCA - Google Patents
Preparation of integrated black silica gel OCA Download PDFInfo
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- CN112708396A CN112708396A CN202011590722.9A CN202011590722A CN112708396A CN 112708396 A CN112708396 A CN 112708396A CN 202011590722 A CN202011590722 A CN 202011590722A CN 112708396 A CN112708396 A CN 112708396A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of silica gel OCA, in particular to preparation of black silica gel OCA. The preparation method of the integral black silica gel OCA comprises the following vinyl silicone oil, a tackifier, a cross-linking agent, a solvent, a pigment, a catalyst and an inhibitor, wherein the integral black silica gel OCA can be used like a common acrylic OCA and has all advantages of silica gel, meanwhile, the appearance of the integral black is particularly improved and attractive, the added black pigment is carbon black which is the most stable pigment and has high-quality properties of heat resistance, chemical resistance, light resistance and the like, the light absorption rate of fine particle carbon black is higher than that of coarse particle carbon black, so that the tinting strength is stronger, the structure of the carbon black is the form of carbon black aggregates, the more the general chains are, the denser the higher the structure is, otherwise, the lower the structure is, the high structure dispersion performance is good, and the covering capacity is strong.
Description
Technical Field
The invention relates to the technical field of silica gel OCA, in particular to preparation of black silica gel OCA.
Background
With the accelerated development of automobile intelligence, the vehicle-mounted display is developed towards large size, multi-screen, high definition, interactivity and multi-modality, and higher requirements are also placed on the performance of the display, including high contrast, low reflectivity, wide viewing angle, high brightness, touch control, fast response and the like. In addition, the novel design of the details and the structure of the vehicle-mounted display screen can also play an unexpected role in improving the product competitiveness. Therefore, an "integral black" technology capable of creating a novel, striking, beautiful and technological vehicle-mounted display effect will become one of the trends;
the 'integral black' effect can greatly improve the static aesthetic feeling of the display, the surface of the product looks more beautiful, luxurious and scientific, the quality of the displayed product is improved from the appearance, and better experience is brought to consumers. At the moment of rapid development of vehicle-mounted display technology, the 'integral black' will become one of trends;
in the full-lamination process of the optical element, a plurality of lamination processes are performed by adopting a wet glue coating mode, so that the advantages of easiness in reworking, difficulty in generating bubbles during lamination, good lamination for special-shaped pieces and the like are achieved, but the defects of complex thickness control, glue overflow, high process requirement, insufficient viscosity and the like exist, and the application of the process is limited.
Disclosure of Invention
The invention aims to provide a preparation method of an integral black silica gel OCA, which aims to solve the problems in the background technology.
In order to achieve the above object, in one aspect, the present invention provides an integral black silica gel OCA, which comprises the following raw materials: 10-60 parts of vinyl silicone oil, 10-40 parts of tackifier, 1-15 parts of cross-linking agent, 10-60 parts of solvent, 0.1-10 parts of pigment, 0.001-5 parts of catalyst and 0.001-5 parts of inhibitor.
As a further improvement of the technical scheme, the tackifier is selected from silicone resin, the silicone resin is at least one of silicone MQ resin, silicone VMQ resin and silicone HMQ resin, and the tackifier is mainly used in silica gel to improve initial adhesion and holding adhesion of products.
As a further improvement of the technical proposal, the cross-linking agent is selected from hydrogen-containing silicone oil, is reactive silicone oil containing two Si-H bonds, is convenient to generate cross-linking reaction with vinyl silicone oil, and plays a role in adjusting the Wukui cross-linking density.
As a further improvement of the technical scheme, the solvent is one or a mixture of more of toluene, benzene, xylene, ethanol, methanol and ethyl acetate, and is used as a medium for polymerization reaction, so that the reaction is mild, the temperature is easy to control, and meanwhile, the solvent can be used for reducing the cost and improving the benefit.
In a further improvement of this aspect, the pigment is selected from black pigments, the black pigment is at least one of carbon black, iron oxide black, copper chromium black and iron chromium black, the black pigment is preferably carbon black, carbon black is the most stable pigment and has excellent properties such as heat resistance, chemical resistance and light resistance, the fine particle carbon black has a higher absorbance than the coarse particle carbon black, and therefore has a stronger tinting strength, and the structure of carbon black, i.e., the morphology of carbon black aggregates, is generally denser with more chain branches and has a higher structure, and conversely, has a lower structure, and therefore has good high structural dispersibility and a strong hiding power.
As a further improvement of the technical scheme, the catalyst is selected from platinum catalysts, the platinum catalyst is at least one of platinum black, chloroplatinic acid or platinum/olefin siloxane coordination compounds, the platinum catalyst has the advantages of high catalytic activity, strong selectivity, convenient preparation of the catalyst, small usage amount, capability of being compounded with other metals or cocatalyst active components and the like through the change and improvement of a preparation method, optimized catalytic performance, wide application field, repeated regeneration and activation, long service life, capability of recycling and reusing the metal palladium of the waste catalyst and the like.
As a further improvement of the present technical solution, the inhibitor is at least one selected from the group consisting of methylbutynol, ethynyl cyclohexanol, and maleic acid containing alkynyl, and the inhibitor is a substance for retarding or reducing the speed of the chemical reaction, and slowing the polymerization reaction, thereby suppressing or moderating the chemical reaction.
In another aspect, the present invention provides a method for preparing an integral black silica gel OCA, which comprises any one of the above integral black silica gel OCA, and comprises the following steps:
s1, adding vinyl silicone oil, a tackifier, a cross-linking agent and a solvent, heating, and carrying out ultrasonic dispersion and mixing;
s2, cooling, sequentially adding the pigment, the catalyst and the inhibitor, and performing ultrasonic dispersion and mixing to prepare a glue solution;
s3, spreading the release film to enable the upper release surface to be upward, and smearing glue solution on the surface of the release film according to the required thickness;
and S4, curing according to the characteristics of the glue solution, and rolling to ensure that the lower surface of the release film is attached to the initially cured gel film after curing.
Preferably, in S1, the temperature rise is 100-120 ℃, and the ultrasonic dispersion time is 15-30 min.
Preferably, in the step S2, the temperature is reduced to 60-80 ℃, and the ultrasonic dispersion time is 10-20 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method of the integral black silica gel OCA can be used like common acrylic OCA, has all the advantages of silica gel, and particularly has the function of improving the display attractiveness due to the integral black appearance.
2. In the preparation method of the integral black silica gel OCA, the added black pigment is carbon black which is the most stable pigment and has high-quality properties of heat resistance, chemical resistance, light resistance and the like, the light absorption rate of fine particle carbon black is higher than that of coarse particle carbon black, so the tinting strength is stronger, the structure of the carbon black, namely the form of carbon black aggregates, is higher when the number of general chains is more and the structure is denser, and is higher when the number of general chains is more and the structure is lower, the high-structure dispersion performance is good, and the covering capability is strong.
Drawings
Fig. 1 is an overall flow chart of embodiment 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1 preparation of a one-piece black silica gel OCA, comprising:
first, preparation of glue solution
Adding 60 parts of vinyl silicone oil, 10 parts of tackifier, 1 part of cross-linking agent and 10 parts of solvent, heating to 100 ℃ and 120 ℃, carrying out ultrasonic dispersion mixing for 15-30min, cooling to 60-80 ℃, sequentially adding 10 parts of pigment, 5 parts of catalyst and 5 parts of inhibitor, and carrying out ultrasonic dispersion mixing for 10-20min to prepare glue solution.
Secondly, preparing a glue film
Spreading the release film to enable the upper release surface to be upward, coating glue solution on the surface of the release film according to the required thickness, curing according to the characteristics of the glue solution, and rolling to enable the lower surface of the release film to be attached to the initially cured gel film after curing.
Example 2 preparation of a one-piece black silica gel OCA, comprising:
first, preparation of glue solution
Adding 48 parts of vinyl silicone oil, 17.5 parts of tackifier, 4 parts of cross-linking agent and 22 parts of solvent, heating to 100 ℃ and 120 ℃, carrying out ultrasonic dispersion mixing for 15-30min, then cooling to 60-80 ℃, sequentially adding 7.5 parts of pigment, 4 parts of catalyst and 4 parts of inhibitor, and carrying out ultrasonic dispersion mixing for 10-20min to prepare glue solution.
Secondly, preparing a glue film
Spreading the release film to enable the upper release surface to be upward, coating glue solution on the surface of the release film according to the required thickness, curing according to the characteristics of the glue solution, and rolling to enable the lower surface of the release film to be attached to the initially cured gel film after curing.
Example 3 preparation of a one-piece black silica gel OCA, comprising:
first, preparation of glue solution
Adding 35 parts of vinyl silicone oil, 25 parts of tackifier, 8 parts of cross-linking agent and 35 parts of solvent, heating to 100 ℃ and 120 ℃, carrying out ultrasonic dispersion mixing for 15-30min, cooling to 60-80 ℃, sequentially adding 5 parts of pigment, 3 parts of catalyst and 3 parts of inhibitor, and carrying out ultrasonic dispersion mixing for 10-20min to prepare glue solution.
Secondly, preparing a glue film
Spreading the release film to enable the upper release surface to be upward, coating glue solution on the surface of the release film according to the required thickness, curing according to the characteristics of the glue solution, and rolling to enable the lower surface of the release film to be attached to the initially cured gel film after curing.
Example 4 preparation of a one-piece black silica gel OCA, comprising:
first, preparation of glue solution
Adding 22 parts of vinyl silicone oil, 32.5 parts of tackifier, 12 parts of cross-linking agent and 48 parts of solvent, heating to 100 ℃ and 120 ℃, carrying out ultrasonic dispersion mixing for 15-30min, then cooling to 60-80 ℃, sequentially adding 2.5 parts of pigment, 2 parts of catalyst and 2 parts of inhibitor, and carrying out ultrasonic dispersion mixing for 10-20min to prepare glue solution.
Secondly, preparing a glue film
Spreading the release film to enable the upper release surface to be upward, coating glue solution on the surface of the release film according to the required thickness, curing according to the characteristics of the glue solution, and rolling to enable the lower surface of the release film to be attached to the initially cured gel film after curing.
Example 5 preparation of a one-piece black silica gel OCA, comprising:
first, preparation of glue solution
Adding 10 parts of vinyl silicone oil, 40 parts of tackifier, 15 parts of cross-linking agent and 60 parts of solvent, heating to 100 ℃ and 120 ℃, carrying out ultrasonic dispersion mixing for 15-30min, cooling to 60-80 ℃, sequentially adding 0.1 part of pigment, 0.001 part of catalyst and 0.001 part of inhibitor, and carrying out ultrasonic dispersion mixing for 10-20min to prepare a glue solution.
Secondly, preparing a glue film
Spreading the release film to enable the upper release surface to be upward, coating glue solution on the surface of the release film according to the required thickness, curing according to the characteristics of the glue solution, and rolling to enable the lower surface of the release film to be attached to the initially cured gel film after curing.
In the above, the silicone resin is at least one of silicone MQ resin, silicone VMQ resin and silicone HMQ resin, and the tackifier is mainly used in silica gel to improve the initial adhesion and the holding adhesion of the product;
the cross-linking agent is selected from hydrogen-containing silicone oil, is reactive silicone oil containing two Si-H bonds, is convenient to generate cross-linking reaction with vinyl silicone oil, and plays a role in adjusting and comprehending cross-linking density;
the solvent is one or a mixture of more of toluene, benzene, xylene, ethanol, methanol or ethyl acetate, and is used as a medium for polymerization reaction, so that the reaction is mild, the temperature is easy to control, and meanwhile, the cost can be reduced, and the benefit is improved;
the pigment is selected from black pigment, the black pigment is at least one of carbon black, iron oxide black, copper chromium black and iron chromium black, the black pigment is preferably carbon black, the carbon black is the most stable pigment and has excellent properties of heat resistance, chemical resistance, light resistance and the like, the light absorption rate of fine particle carbon black is higher than that of coarse particle carbon black, so the tinting strength is stronger, the structure of the carbon black, namely the form of carbon black aggregate, the structure is higher as the chain branches are more and more dense, and the structure is lower as the chain branches are more and more dense, the high structure dispersion performance is good, and the covering capability is strong;
the catalyst is selected from platinum catalysts, the platinum catalyst is at least one of platinum black, chloroplatinic acid or platinum/olefin siloxane coordination compounds, the platinum catalyst has the advantages of high catalytic activity, strong selectivity, convenient catalyst preparation, small usage amount, capability of being compounded with other metals or cocatalyst active components and the like through the change and improvement of a preparation method, optimized catalytic performance, wide application field, repeated regeneration and activation, long service life, capability of recycling and reusing the metal palladium of the waste catalyst and the like;
the inhibitor is at least one selected from the group consisting of methylbutynol, ethynylcyclohexanol, and maleic acid containing an alkynyl group, and is a substance that retards or slows the rate of the chemical reaction, thereby inhibiting or moderating the chemical reaction.
The integral black silica gel OCA prepared by the invention has better integral black effect, and the detection indexes of the integral black silica gel OCA prepared by the invention are shown in table 1:
TABLE 1
As shown in Table 1, in examples 1-5, when 35 parts of vinyl silicone oil, 25 parts of tackifier, 8 parts of crosslinking agent, 35 parts of solvent, 5 parts of pigment, 3 parts of catalyst and 3 parts of inhibitor are used, the adhesive film obtained has higher cohesive strength, better tinctorial strength and better stripping force and initial adhesion.
Comparative example 1 preparation of an integral black silica gel OCA, comprising:
first, preparation of glue solution
Adding 35 parts of vinyl silicone oil, 25 parts of tackifier, 8 parts of cross-linking agent and 35 parts of solvent, heating to 100 ℃ and 120 ℃, carrying out ultrasonic dispersion mixing for 15-30min, cooling to 60-80 ℃, sequentially adding 3 parts of catalyst and 3 parts of inhibitor, and carrying out ultrasonic dispersion mixing for 10-20min to prepare glue solution.
Secondly, preparing a glue film
Spreading the release film to enable the upper release surface to be upward, coating glue solution on the surface of the release film according to the required thickness, curing according to the characteristics of the glue solution, and rolling to enable the lower surface of the release film to be attached to the initially cured gel film after curing.
In the integrated black silica gel OCA prepared by the invention, the adhesive force and the strength of an adhesive film are better, and in order to verify the related technical scheme, the applicant performs the following tests:
comparative example 1: by adopting the method of example 3, the relevant indexes of the prepared integral black silica gel OCA are detected under the condition of removing the colorant, and the concrete results are shown in Table 2;
TABLE 2
As shown in Table 2, in comparative example 1, the integral black silica gel OCA was prepared with a significant decrease in cohesive strength and poor in peel strength and initial tack when the colorant was removed, and it can be seen that the colorant is an important factor for changing the tack and strength of the integral black silica gel OCA
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. An integral black silica gel OCA comprises the following raw materials: 10-60 parts of vinyl silicone oil, 10-40 parts of tackifier, 1-15 parts of cross-linking agent, 10-60 parts of solvent, 0.1-10 parts of pigment, 0.001-5 parts of catalyst and 0.001-5 parts of inhibitor.
2. The integral black silica OCA of claim 1, wherein: the tackifier is selected from silicone resin, and the silicone resin is at least one of silicone MQ resin, silicone VMQ resin and silicone HMQ resin.
3. The integral black silica OCA of claim 1, wherein: the cross-linking agent is selected from hydrogen-containing silicone oil and is reactive silicone oil containing two Si-H bonds.
4. The integral black silica OCA of claim 1, wherein: the solvent is one or more of toluene, benzene, xylene, ethanol, methanol and ethyl acetate.
5. The integral black silica OCA of claim 1, wherein: the pigment is selected from black pigments, the black pigments are at least one of carbon black, iron oxide black, copper chromium black and iron chromium black, and the black pigments are preferably carbon black.
6. The integral black silica OCA of claim 1, wherein: the catalyst is selected from platinum catalysts, and the platinum catalyst is at least one of platinum black, chloroplatinic acid or platinum/olefin siloxane coordination compound.
7. The integral black silica OCA of claim 1, wherein: the inhibitor is selected from at least one of methylbutinol, ethynyl cyclohexanol and maleic acid containing alkynyl.
8. The preparation of an integrated black silica gel OCA is characterized in that: comprising the integral black silica OCA according to any one of claims 1 to 7, in the following operating steps:
s1, adding vinyl silicone oil, a tackifier, a cross-linking agent and a solvent, heating, and carrying out ultrasonic dispersion and mixing;
s2, cooling, sequentially adding the pigment, the catalyst and the inhibitor, and performing ultrasonic dispersion and mixing to prepare a glue solution;
s3, spreading the release film to enable the upper release surface to be upward, and smearing glue solution on the surface of the release film according to the required thickness;
and S4, curing according to the characteristics of the glue solution, and rolling to ensure that the lower surface of the release film is attached to the initially cured gel film after curing.
9. The preparation of integral black silica OCA according to claim 8, wherein: in the step S1, the temperature rise is 100-120 ℃, and the ultrasonic dispersion time is 15-30 min.
10. The preparation of integral black silica OCA according to claim 8, wherein: in the step S2, the temperature is reduced to 60-80 ℃, and the ultrasonic dispersion time is 10-20 min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060128881A1 (en) * | 2002-12-04 | 2006-06-15 | Rhodia Chimie | Single-component adhesive silicone elastomer composition which can be crosslinked by polyaddition |
| CN102408869A (en) * | 2011-08-04 | 2012-04-11 | 绵阳惠利电子材料有限公司 | Halogen-free flame-retardant addition type organosilicon potting compound for electronic appliances |
| CN110343483A (en) * | 2019-07-12 | 2019-10-18 | 太仓斯迪克新材料科技有限公司 | A kind of rapid curing silicone pressure sensitive gluing agent and adhesive tape |
| CN110577661A (en) * | 2019-09-26 | 2019-12-17 | 昆山市中迪新材料技术有限公司 | Silicone membrane, heat-conducting silicone sheet and preparation method thereof |
| CN209816025U (en) * | 2018-12-30 | 2019-12-20 | 苏州桐力光电股份有限公司 | Integrated black touch display module |
-
2020
- 2020-12-29 CN CN202011590722.9A patent/CN112708396A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060128881A1 (en) * | 2002-12-04 | 2006-06-15 | Rhodia Chimie | Single-component adhesive silicone elastomer composition which can be crosslinked by polyaddition |
| CN102408869A (en) * | 2011-08-04 | 2012-04-11 | 绵阳惠利电子材料有限公司 | Halogen-free flame-retardant addition type organosilicon potting compound for electronic appliances |
| CN209816025U (en) * | 2018-12-30 | 2019-12-20 | 苏州桐力光电股份有限公司 | Integrated black touch display module |
| CN110343483A (en) * | 2019-07-12 | 2019-10-18 | 太仓斯迪克新材料科技有限公司 | A kind of rapid curing silicone pressure sensitive gluing agent and adhesive tape |
| CN110577661A (en) * | 2019-09-26 | 2019-12-17 | 昆山市中迪新材料技术有限公司 | Silicone membrane, heat-conducting silicone sheet and preparation method thereof |
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Application publication date: 20210427 |