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 PDF

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Publication number
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
parts
adhesive film
stirring
preparing
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郭俊宝
蘧建星
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Jiangsu Keqi Polymer Materials Research Institute Co ltd
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Jiangsu Keqi Polymer Materials Research Institute Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38Pressure-sensitive adhesives [PSA]
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/10Transparent films; Clear coatings; Transparent materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00Crosslinking
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2483/00Presence 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

Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film
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
Figure RE-GDA0003079935240000061
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.
CN202011422093.9A 2020-12-08 2020-12-08 Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film Pending CN113025265A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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Application publication date: 20210625