CN113025265A - Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film - Google Patents
Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film Download PDFInfo
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- CN113025265A CN113025265A CN202011422093.9A CN202011422093A CN113025265A CN 113025265 A CN113025265 A CN 113025265A CN 202011422093 A CN202011422093 A CN 202011422093A CN 113025265 A CN113025265 A CN 113025265A
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- organic silicon
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- adhesive film
- stirring
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 44
- 239000010703 silicon Substances 0.000 title claims abstract description 44
- 239000003292 glue Substances 0.000 title claims abstract description 23
- 230000003287 optical effect Effects 0.000 title claims abstract description 22
- 239000002313 adhesive film Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000002904 solvent Substances 0.000 title abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003112 inhibitor Substances 0.000 claims abstract description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229920001971 elastomer Polymers 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000004593 Epoxy Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 239000008096 xylene Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 239000004945 silicone rubber Substances 0.000 claims description 2
- 239000013464 silicone adhesive Substances 0.000 claims 1
- 229920002050 silicone resin Polymers 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 1
- 238000003475 lamination Methods 0.000 abstract 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 12
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 5
- 229920002545 silicone oil Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002390 adhesive tape Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C09J11/06—Non-macromolecular additives organic
-
- 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
-
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
-
- 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
- C09J2483/00—Presence of polysiloxane
Abstract
The invention provides a preparation method of a solvent type organic silicon glue for manufacturing an optical transparent adhesive film, which comprises the following components in parts by weight: a) 70-130 parts of toluene or dimethylbenzene, 30-50 parts of silicon rubber, 60-90 parts of organic silicon resin, 0.1-3 parts of cross-linking agent, 0.1-0.5 part of inhibitor and 0.2-0.6 part of catalyst. The optical transparent adhesive film prepared by using the organic silicon rubber with the special structure and the cross-linking agent can provide high adhesive property and moderate hardness after the film is formed by the adhesive, so that the adhesive film has better flexibility, meets the requirement of full-lamination of a screen and replaces the traditional acrylic acid OCA film.
Description
Technical Field
The invention relates to the technical field of preparation of glue for optical transparent glue, in particular to a preparation method of organic silicon glue for optical transparent glue.
Background
The main stream of OCA products in the market still mainly comprises acrylic products, and the acrylic products have the advantages of high adhesive force and quick curing, and have the defect of poor weather resistance, and particularly, under the conditions of receiving light and damp and hot for a long time, the attached screen is easy to generate yellow spots or cracking phenomena. By means of the extremely low shrinkage rate, excellent long-term weather resistance, excellent optical performance, lower dielectric constant, easy coating, fast curing, low energy consumption, higher viscosity, higher bonding yield and reworkability of the organic silicon OCA optical adhesive, the organic silicon OCA optical bonding scheme is adopted by more and more display factories. And the organic silicon OCA product is completely nontoxic and has good biocompatibility, and completely meets the restriction requirements of European Union RoHS.
Currently, the silicone pressure sensitive adhesive technology available for OCA or LOCA is based on thermal cure systems, including peroxide cure and platinum catalyst cure systems.
The peroxide curing system has the advantages of low cost, high bonding strength and the like, but the pressure-sensitive adhesive state can be formed only by high curing temperature, such as over 160 ℃, and the problems of aging deformation, unstable peeling force and the like of the release film of the substrate caused by the high temperature can be solved. And the obtained pressure-sensitive adhesive film has high hardness and low transparency, and is difficult to meet the requirements of OCA on films.
The platinum curing system has the advantages of low vulcanization temperature, high transparency and the like, and is increasingly applied to the electronic field. However, the platinum vulcanization system has low cohesive force and a crude rubber structure limitation, so that high bonding force is difficult to obtain. In order to meet the requirements for preparing OCA laminating products, the raw materials of the system and related technologies need to be improved and innovated so as to improve cohesive strength and adhesive force.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of organic silicon glue for manufacturing an optical transparent adhesive film.
In order to achieve the purpose, the invention provides the following technical scheme:
the preparation method of the organic silicon glue for manufacturing the optical transparent adhesive film comprises the following steps:
a) adding toluene or xylene or a mixture thereof into a reaction kettle with stirring and heating, adding part of epoxy or hydroxyl-terminated silicon rubber crude rubber at the constant temperature of 40-60 ℃, and stirring for 4-6 hours until the raw rubber is uniformly dispersed;
b) adding organic silicon resin, and stirring for 1-3 hours;
c) adding inhibitor and cross-linking agent, stirring for 1-3 hr;
d) after stirring evenly, adding platinum catalyst, continuing stirring for 0.5-1 hour, filtering, detecting and discharging.
Preferably, the weight percentages of the components in the step a) are as follows: 80-130 parts of toluene or xylene or a mixture thereof and 35-50 parts of raw silicone rubber.
Preferably, the weight portion of the organic silicon resin in the step b) is 65-85 portions, the molecular weight is 4000-8000, and the M/Q ratio is 0.6-1.0.
Preferably, the hydrogen content of the cross-linking agent in the step c) is 0.1-1.0%, the weight part is 0.3-2.5 parts, and the weight part of the inhibitor is 0.2-0.5 part.
Preferably, the weight part of the catalyst in the step d) is 0.2-0.6 part.
The beneficial effects brought by the invention are as follows: the combination of the improved raw organic silicon rubber, the organic silicon resin and the cross-linking agent is adopted to achieve the purposes of enhancing the bonding strength and reducing the hardness of the organic silicon pressure-sensitive adhesive, and the organic silicon OCA adhesive film is suitable for preparing an organic silicon OCA adhesive film:
1. adopts high molecular weight silicon rubber crude rubber containing epoxy and hydroxyl;
2. the organic silicon resin with proper molecular weight and M/Q ratio is adopted, so that the cohesive strength can be improved, and the hardness of the glue after film formation can be reduced;
3. the proper cross-linking agent is used for adjusting the film forming property and the cohesive strength of the glue;
4. the obtained organic silicon glue has high transparency, complete film forming and high bonding strength.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
The first embodiment is as follows:
the preparation method of the organic silicon glue for manufacturing the optical transparent adhesive film comprises the following steps:
a) adding 100 parts of toluene into a reaction kettle with stirring and heating functions, and heating to 40 ℃ for constant temperature;
b) adding 35 parts of epoxy or hydroxyl-terminated organic silicon raw rubber, and stirring for 4 hours;
c) adding 70 parts of organic silicon resin with the molecular weight of 4000 and the M/Q ratio of 0.7, and stirring for 1 hour;
d) 0.5 part of hydrogen-containing silicone oil having an average hydrogen content of 0.5% and 0.2 part of 10% ethynylcyclohexanol toluene solution were added and stirred for 1 hour.
e) 0.5 part of 5000ppm Karster catalyst was added thereto, and the mixture was stirred for 30 minutes.
Obtaining the organic silicon pressure-sensitive adhesive, and preparing the organic silicon pressure-sensitive adhesive into an adhesive tape for testing.
Example two:
the preparation method of the organic silicon glue for manufacturing the optical transparent adhesive film comprises the following steps:
a) adding 100 parts of toluene into a reaction kettle with stirring and heating functions, and heating to 40 ℃ for constant temperature;
b) adding 35 parts of epoxy or hydroxyl-terminated organic silicon raw rubber, and stirring for 4 hours;
c) adding 70 parts of organic silicon resin with the molecular weight of 4000 and the M/Q ratio of 0.8, and stirring for 1 hour;
d) 0.5 part of hydrogen-containing silicone oil having an average hydrogen content of 0.5% and 0.2 part of 10% ethynylcyclohexanol toluene solution were added and stirred for 1 hour.
e) 0.5 part of 5000ppm Karster catalyst was added thereto, and the mixture was stirred for 30 minutes.
Obtaining the organic silicon pressure-sensitive adhesive, and preparing the organic silicon pressure-sensitive adhesive into an adhesive tape for testing.
Example three:
the preparation method of the organic silicon glue for manufacturing the optical transparent adhesive film comprises the following steps:
a) adding 100 parts of toluene into a reaction kettle with stirring and heating functions, and heating to 40 ℃ for constant temperature;
b) adding 35 parts of epoxy or hydroxyl-terminated organic silicon raw rubber, and stirring for 4 hours;
c) adding 70 parts of organic silicon resin with the molecular weight of 6000 and the M/Q ratio of 0.8, and stirring for 1 hour;
d) 0.5 part of hydrogen-containing silicone oil having an average hydrogen content of 0.6% and 0.2 part of a 10% ethynylcyclohexanol toluene solution were added and stirred for 1 hour.
e) 0.5 part of 5000ppm Karster catalyst was added thereto, and the mixture was stirred for 30 minutes.
Obtaining the organic silicon pressure-sensitive adhesive, and preparing the organic silicon pressure-sensitive adhesive into an adhesive tape for testing.
Example four:
the preparation method of the organic silicon glue for manufacturing the optical transparent adhesive film comprises the following steps:
a) adding 100 parts of toluene into a reaction kettle with stirring and heating functions, and heating to 40 ℃ for constant temperature;
b) adding 35 parts of epoxy or hydroxyl-terminated organic silicon raw rubber, and stirring for 4 hours;
c) adding 75 parts of organic silicon resin with the molecular weight of 7000 and the M/Q ratio of 0.7, and stirring for 1 hour;
d) 0.4 part of hydrogen-containing silicone oil having an average hydrogen content of 0.6% and 0.2 part of a 10% ethynylcyclohexanol toluene solution were added and stirred for 1 hour.
e) 0.5 part of 5000ppm Karster catalyst was added thereto, and the mixture was stirred for 30 minutes.
Obtaining the organic silicon pressure-sensitive adhesive, and preparing the organic silicon pressure-sensitive adhesive into an adhesive tape for testing.
Comparative example 1:
the method comprises the following steps:
a) adding 100 parts of toluene into a reaction kettle with stirring and heating functions, and heating to 40 ℃ for constant temperature;
b) adding 35 parts of common organic silicon crude rubber, and stirring for 4 hours;
c) adding 70 parts of organic silicon resin with the molecular weight of 7000 and the M/Q ratio of 0.8, and stirring for 1 hour;
d) 0.4 part of hydrogen-containing silicone oil having an average hydrogen content of 1.5% and 0.2 part of a 10% ethynylcyclohexanol toluene solution were added and stirred for 1 hour.
e) 0.5 part of 5000ppm Karster catalyst was added thereto, and the mixture was stirred for 30 minutes.
Table 1 test results of performance of the obtained organic silicon optical transparent glue
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be made by those skilled in the art without inventive work within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (9)
1. The preparation method of the organic silicon glue for manufacturing the optical transparent adhesive film is characterized by comprising the following steps of:
adding toluene or xylene or a mixture thereof into a reaction kettle with stirring and heating, adding raw silicon rubber at the constant temperature of 40-60 ℃, and stirring for 4-6 hours until the raw silicon rubber is uniformly dispersed;
adding organic silicon resin, and stirring for 1-3 hours;
adding inhibitor and cross-linking agent, stirring for 1-3 hr;
after stirring evenly, adding platinum catalyst, continuing stirring for 0.5-1 hour, filtering, detecting and discharging.
2. The method for preparing the silicone glue used for manufacturing the optical clear adhesive film according to claim 1, wherein the components in the step a) are in parts by weight: 70-130 parts of toluene or xylene or a mixture thereof and 30-50 parts of raw silicone rubber.
3. The method for preparing silicone glue used for making an optical clear adhesive film according to claim 1, wherein the silicone resin in step b) is 60 to 90 parts by weight.
4. The method for preparing silicone glue used for preparing OCA according to claim 1, wherein in step c), the hydrogen content of the cross-linking agent is 0.1-1.5%, the weight part is 0.1-3 parts, and the weight part of the inhibitor is 0.1-0.5 part.
5. The method for preparing silicone glue used for making an optical clear adhesive film according to claim 1, wherein the weight part of the catalyst in the step d) is 0.2-0.6.
6. The method for preparing silicone adhesive used to make an optical clear adhesive film according to claim 1, wherein the silicone crude rubber has a molecular weight of 60-100 ten thousand, a vinyl content of 0.016% -0.9%, and a partial epoxy or hydroxyl capping.
7. The method as claimed in claim 1, wherein the organic silicon resin has a M/Q ratio of 0.5-1.2 and a molecular weight of 3000-20000.
8. The method for preparing silicone glue used for making optical clear adhesive film according to claim 1, wherein the inhibitor is alkynol inhibitor.
9. The method as claimed in claim 6, wherein the platinum catalyst has a platinum content of 2000-10000 ppm.
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CN202011422093.9A CN113025265A (en) | 2020-12-08 | 2020-12-08 | Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film |
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CN202011422093.9A CN113025265A (en) | 2020-12-08 | 2020-12-08 | Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film |
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Cited By (2)
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CN115232601A (en) * | 2022-07-01 | 2022-10-25 | 深圳市宝力新材料有限公司 | Preparation and application of semiconductor type organic silicon OCA optical cement |
CN116041965A (en) * | 2022-12-09 | 2023-05-02 | 太湖金张科技股份有限公司 | High impact resistance organic silica gel film |
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Cited By (2)
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CN115232601A (en) * | 2022-07-01 | 2022-10-25 | 深圳市宝力新材料有限公司 | Preparation and application of semiconductor type organic silicon OCA optical cement |
CN116041965A (en) * | 2022-12-09 | 2023-05-02 | 太湖金张科技股份有限公司 | High impact resistance organic silica gel film |
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