CN112940656A - Packaging adhesive for mini LED screen and preparation method thereof - Google Patents
Packaging adhesive for mini LED screen and preparation method thereof Download PDFInfo
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- CN112940656A CN112940656A CN202110224378.XA CN202110224378A CN112940656A CN 112940656 A CN112940656 A CN 112940656A CN 202110224378 A CN202110224378 A CN 202110224378A CN 112940656 A CN112940656 A CN 112940656A
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- mini led
- led screen
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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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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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Epoxy Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of mini LED screen packaging, and particularly discloses a mini LED screen packaging adhesive and a preparation method thereof. The packaging adhesive of the mini LED screen comprises a component A and a component B, wherein the component A is composed of organic silicon modified epoxy resin, an antioxidant and a defoaming agent; the component B consists of a curing agent and a catalyst. The organic silicon modified epoxy resin is obtained by carrying out hydrosilylation reaction on hydrogen-containing silicone oil and allyl glycidyl ether, and the organic silicon modified epoxy resin combines the advantages of organic silicon and epoxy resin, so that the cured mini LED screen packaging adhesive has good light transmittance, good mechanical property, high temperature resistance and yellowing resistance, and the preparation process has the advantages of simple operation, capability of curing at room temperature, good repeatability and controllability, no use of organic solvent, capability of curing at room temperature, saving of a large amount of cost and easiness in industrialization.
Description
Technical Field
The invention relates to the technical field of mini LED screen packaging glue, in particular to mini LED screen packaging glue and a preparation method thereof.
Background
The mini LED display screen is a novel display technology which is well-sought at present, has the characteristics of higher consistency, higher brightness and the like compared with the existing Liquid Crystal Display (LCD), has the display effect equivalent to that of an organic light-emitting diode (OLED), is not easy to burn, and has long service life. At present, a mini LED display screen is developed towards a large screen, but a large screen mini LED is faced with the problems of high packaging difficulty, low yield and the like, and besides the requirement that a packaging adhesive has good light transmittance and thermal stability, the packaging adhesive is also required to be flat, yellowing-resistant and good in air tightness.
The common mini LED packaging adhesive mainly comprises epoxy resin and organic silicon resin, wherein the epoxy resin is high in hardness, good in air tightness and high in reliability, is the mainstream mini LED packaging adhesive at present, but is poor in temperature resistance and yellowing resistance, and the organic silicon resin overcomes the defects of the epoxy resin, but is low in mechanical strength and weak in air tightness.
The epoxy resin for mini LED encapsulation has a plurality of different curing modes, which can be mainly divided into three modes of thermal curing, room temperature curing and UV curing. The thermosetting curing is rapid, the cured product has good mechanical properties, but the curing temperature is high, a large amount of energy is consumed, the cost is high, and the large-screen mini LED packaging is not facilitated; the UV curing can be realized only by short irradiation of UV rays, the reaction speed is very quick, and a large amount of energy consumption is avoided, but the curing mode requires specific groups in the epoxy resin, so that the curing mode is not beneficial to adjustment of researchers according to actual conditions and is difficult to apply to mini LED packaging on a large scale; the curing at room temperature can be realized only by placing for a period of time at room temperature, specific groups are not needed, the energy is saved, the environment is protected, and the method is suitable for packaging a large-screen mini LED, so that the development of the high-performance epoxy resin capable of being cured at room temperature has very important significance for the mini LED packaging.
Disclosure of Invention
The invention mainly aims to provide a packaging adhesive for a mini LED screen;
the invention also aims to provide a method for preparing the packaging adhesive for the mini LED screen. The packaging adhesive prepared by the method has the advantages of smooth surface, good light transmission, good mechanical property, high temperature resistance and yellowing resistance, can be cured at room temperature, and meets the requirements of the existing mini LED on the packaging adhesive.
The invention is realized by the following technical scheme:
the utility model provides an encapsulation of mini LED screen glues, includes the mass ratio and is 1: 0.3-1: 0.6 of a component A and a component B;
the component A consists of the following raw materials in parts by mass: 96-99% of organic silicon modified epoxy resin, 1-4% of antioxidant and 0.01-0.03% of defoaming agent, wherein the total mass fraction of the raw materials is 100%;
the component B consists of the following raw materials in parts by mass: 98-99% of curing agent and 1-2% of catalyst, wherein the total mass of the raw materials is 100%;
in the component A, the preparation process of the organosilicon modified epoxy resin is as follows: taking hydrogen-containing silicone oil and allyl glycidyl ether as raw materials, heating the allyl glycidyl ether, adding a Pt catalyst, adding the hydrogen-containing silicone oil into the allyl glycidyl ether, heating, carrying out stirring reaction, and obtaining the organic silicon modified epoxy resin after the reaction is finished.
In the preparation process of the organic silicon modified epoxy resin, the hydrogen-containing silicone oil is long-chain linear structure and does not contain phenyl, and the hydrogen content is 0.18-0.75%.
In the preparation process of the organic silicon modified epoxy resin, the molar ratio of Si-H to vinyl is 1: 1.1-1: 1.3. The content of the Pt catalyst is 2 ppm-10 ppm.
In the preparation process of the organic silicon modified epoxy resin, the hydrogen-containing silicone oil is added into allyl glycidyl ether in a dropwise manner, and the dropwise adding speed is 2.5-6 g/min. The heating temperature range of the allyl glycidyl ether is 70-90 ℃; the temperature range after temperature rise is 110-120 ℃. The stirring reaction time is 1-3 hours.
Preferably, in the component A, the antioxidant is one or more than two of triphenyl phosphite, trioctyl phosphite, 2, 6-di-tert-butyl-4-methylphenol and bisdodecyl thiodipropionate; the defoaming agent is a silicone defoaming agent, and more preferably one or more of Tego900, Tego910, Tego940 and Tego 961.
Preferably, the curing agent in the component B is a modified alicyclic amine curing agent, and more preferably one or more of R-2265, R-2266, R-2269 and R-3301; the catalyst is one or more than two of 2,4, 6-tri (dimethylamino methyl) phenol, triethanolamine and trimethyl amino methyl phenol.
A method for preparing the packaging adhesive of the mini LED screen comprises the following steps:
(1) uniformly mixing the organic silicon modified epoxy resin, the antioxidant and the defoaming agent to obtain a component A, and uniformly mixing the curing agent and the catalyst to obtain a component B;
(2) and uniformly mixing the component A and the component B, and then standing at room temperature to obtain the cured mini LED screen packaging adhesive.
Preferably, the standing time in the step (2) is 2-6 hours, and preferably 3-5 hours.
Compared with the prior art, the invention has the following beneficial effects:
(1) the organic silicon modified epoxy resin is obtained through hydrosilylation, the long-chain silicon-oxygen-silicon bond is branched into the epoxy resin, and the organic silicon modified epoxy resin combines the advantages of organic silicon and the epoxy resin, so that the cured packaging adhesive has good light transmission, mechanical property, thermal stability and flatness.
(2) The adopted hydrogen-containing silicone oil is long-chain linear and phenyl-free hydrogen-containing silicone oil, the prepared organic silicon modified epoxy resin is long-chain modified epoxy resin, the steric hindrance is small, the curing is easy to carry out at room temperature, and meanwhile, the cured packaging adhesive is not easy to yellow because the organic silicon modified epoxy resin does not contain phenyl.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the invention as claimed is not limited to the examples. The room temperature is 20-30 ℃. The curing agent used in the invention is produced by Guangzhou Ruizi chemical industry.
Example 1
The embodiment provides a preparation method of a packaging adhesive of a mini LED screen.
(1) Preparing organic silicon modified epoxy resin: 45.62g of allyl glycidyl ether were taken in a 150ml three-necked flask (equipped with a magnetic stirrer and a thermocouple), warmed to 80 ℃ and 3ppm of catalyst were added. Then, 80.00g of hydrogen-containing silicone oil (hydrogen content: 0.36%) was added dropwise to the flask over 20 minutes. And after the dropwise addition of the raw materials is finished, timing is started, and the reaction temperature is controlled to be 110 ℃. Reacting for 2 hours to obtain clear and transparent,Viscous silicone-modified epoxy resin. And (5) detecting. n isD H1.4421, epoxy value 0.288mol/100 g.
(2) Preparation of component A: 98g of organic silicon modified epoxy resin, 1.97g of antioxidant triphenyl phosphite and 0.03g of Tego962 defoaming agent are put into a beaker and mixed and stirred uniformly.
(3) Preparation of the component B: 98.00g of gR-2269 and 2.00g of 2,4, 6-tris (dimethylaminomethyl) phenol are put into a beaker and mixed and stirred uniformly.
(4) Curing of the organosilicon modified epoxy resin: mixing the component A and the component B according to the mass ratio of 1: 0.4, stirring evenly, and standing for 4 hours at room temperature to realize solidification.
Example 2
The embodiment provides a preparation method of a packaging adhesive of a mini LED screen.
(1) Preparing organic silicon modified epoxy resin: 45.62g of allyl glycidyl ether were taken in a 150ml three-necked flask (equipped with a magnetic stirrer and a thermocouple), warmed to 80 ℃ and charged with 5ppm of a catalyst. Then, 80.00g of hydrogen-containing silicone oil (hydrogen content: 0.36%) was added dropwise to the flask over 30 minutes. And after the dropwise addition of the raw materials is finished, timing is started, and the reaction temperature is controlled to be 120 ℃. Reacting for 1h to obtain the clear, transparent and viscous organic silicon modified epoxy resin. And (5) detecting. n isD H1.4478, the epoxy value is 0.290mol/100 g.
(2) Preparation of component A: 97g of organic silicon modified epoxy resin, 2.97g of antioxidant triphenyl phosphite and 0.03g of Tego962 defoaming agent are put into a beaker and mixed and stirred uniformly.
(3) Preparation of the component B: 99.00g of gR-2269 and 1.00g of 2,4, 6-tris (dimethylaminomethyl) phenol are put into a beaker, mixed and stirred uniformly.
(4) Curing of the organosilicon modified epoxy resin: mixing the component A and the component B according to the mass ratio of 1: 0.4, stirring evenly, and standing for 4 hours at room temperature to realize solidification.
Example 3
The embodiment provides a preparation method of a packaging adhesive for a mini LED screen
(1) Preparing organic silicon modified epoxy resin: and taking 25.00g of allyl glycidyl ether was placed in a 150ml three-necked flask equipped with a magnetic stirrer and a thermocouple, warmed to 80 ℃ and 3ppm of catalyst was added. 102.21g of hydrogen-containing silicone oil (hydrogen content: 0.18%) was then added dropwise to the flask over 20 minutes. And after the dropwise addition of the raw materials is finished, timing is started, and the reaction temperature is controlled to be 110 ℃. Reacting for 2h to obtain the clear, transparent and viscous organic silicon modified epoxy resin. And (5) detecting. n isD H1.4218, the epoxy value is 0.172mol/100 g.
(2) Preparation of component A: 98g of organic silicon modified epoxy resin, 1.97g of antioxidant triphenyl phosphite and 0.03g of Tego910 defoaming agent are put into a beaker and mixed and stirred uniformly.
(3) Preparation of the component B: 98.00gR-2269 and 2.00g trimethylaminomethylphenol were put in a beaker and mixed and stirred well.
(4) Curing of the organosilicon modified epoxy resin: mixing the component A and the component B according to the mass ratio of 1: 0.3, stirring evenly, and standing for 5 hours at room temperature to realize solidification.
Example 4
The embodiment provides a preparation method of a packaging adhesive for a mini LED screen
(1) Preparing organic silicon modified epoxy resin: 25.00g of allyl glycidyl ether were taken in a 150ml three-necked flask (equipped with a magnetic stirrer and a thermocouple), warmed to 80 ℃ and charged with 5ppm of a catalyst. 102.21g of hydrogen-containing silicone oil (hydrogen content: 0.18%) was then added dropwise to the flask over 30 minutes. And after the dropwise addition of the raw materials is finished, timing is started, and the reaction temperature is controlled to be 120 ℃. Reacting for 1h to obtain the clear, transparent and viscous organic silicon modified epoxy resin. And (5) detecting. n isD H1.4274, epoxy value 0.181mol/100 g.
(2) Preparation of component A: 97g of organic silicon modified epoxy resin, 1.97g of antioxidant triphenyl phosphite and 0.03g of Tego940 defoaming agent are put in a beaker and mixed and stirred uniformly.
(3) Preparation of the component B: 99.00gR-2265 and 1.00g trimethylaminomethylphenol were put in a beaker and mixed and stirred well.
(4) Curing of the organic modified epoxy resin: mixing the component A and the component B according to the mass ratio of 1: 0.3, stirring evenly, and standing for 5 hours at room temperature to realize solidification.
Example 5
The embodiment provides a preparation method of a packaging adhesive for a mini LED screen
(1) Preparing organic silicon modified epoxy resin: 60.00g of allyl glycidyl ether were taken in a 150ml three-necked flask (equipped with a magnetic stirrer and a thermocouple), warmed to 80 ℃ and 3ppm of catalyst were added. Then, 58.88g of hydrogen-containing silicone oil (hydrogen content: 0.75%) was added dropwise to the flask over 20 minutes. And after the dropwise addition of the raw materials is finished, timing is started, and the reaction temperature is controlled to be 110 ℃. Reacting for 2h to obtain the clear, transparent and viscous organic silicon modified epoxy resin. And (5) detecting. n isD H1.4633, epoxy value is 0.443mol/100 g.
(2) Preparation of component A: 98g of organic silicon modified epoxy resin, 1.97g of antioxidant triphenyl phosphite and 0.03g of Tego940 defoaming agent are put in a beaker and mixed and stirred uniformly.
(3) Preparation of the component B: 98.00g of gR-2266 and 2.00g of 2,4, 6-tris (dimethylaminomethyl) phenol are put into a beaker, mixed and stirred uniformly.
(4) Curing of the organosilicon modified epoxy resin: mixing the component A and the component B according to the mass ratio of 1: 0.5, stirring evenly, and standing for 3 hours at room temperature to realize solidification.
Example 6
The embodiment provides a preparation method of a packaging adhesive for a mini LED screen
(1) Preparing organic silicon modified epoxy resin: 60.00g of allyl glycidyl ether were taken in a 150ml three-necked flask (equipped with a magnetic stirrer and a thermocouple), warmed to 80 ℃ and charged with 5ppm of a catalyst. Then, 58.88g of hydrogen-containing silicone oil (hydrogen content: 0.75%) was added dropwise to the flask over 30 minutes. And after the dropwise addition of the raw materials is finished, timing is started, and the reaction temperature is controlled to be 120 ℃. Reacting for 1h to obtain the clear, transparent and viscous organic silicon modified epoxy resin. And (5) detecting. n isD H1.4646, the epoxy value is 0.451mol/100 g.
(2) Preparation of component A: 97g of organic silicon modified epoxy resin, 2.97g of antioxidant triphenyl phosphite and 0.03g of Tego962 defoaming agent are put into a beaker and mixed and stirred uniformly.
(3) Preparation of the component B: 99.00g of gR-2269 and 1.00g of 2,4, 6-tris (dimethylaminomethyl) phenol are put into a beaker, mixed and stirred uniformly.
(4) Curing of the organosilicon modified epoxy resin: mixing the component A and the component B according to the mass ratio of 1: 0.5, stirring evenly, and standing for 3 hours at room temperature to realize solidification.
Example 7
The performance indexes of the packaging adhesive of the mini LED screen obtained in the embodiment 1, the embodiment 2, the embodiment 3, the embodiment 4, the embodiment 5 and the embodiment 6 are shown in the following table 1:
TABLE 1 Properties of the encapsulant for mini LED panels obtained in examples 1-6
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The utility model provides a packaging adhesive of mini LED screen which characterized in that, includes the mass ratio and is 1: 0.3-1: 0.6 of a component A and a component B;
the component A consists of the following raw materials in parts by mass: 96-99% of organic silicon modified epoxy resin, 1-4% of antioxidant and 0.01-0.03% of defoaming agent, wherein the total mass of the raw materials is 100%;
the component B consists of the following raw materials in parts by mass: 98-99% of curing agent and 1-2% of catalyst, wherein the mass fraction of the raw materials is 100%;
in the component A, the preparation process of the organosilicon modified epoxy resin is as follows: taking hydrogen-containing silicone oil and allyl glycidyl ether as raw materials, heating the allyl glycidyl ether, adding a Pt catalyst, adding the hydrogen-containing silicone oil into the allyl glycidyl ether, heating, carrying out stirring reaction, and obtaining the organic silicon modified epoxy resin after the reaction is finished.
2. The packaging adhesive for the mini LED screen according to claim 1, wherein the molar ratio of the hydrogen-containing silicone oil to the allyl glycidyl ether is 1: 1.1-1: 1.3.
3. The packaging adhesive for the mini LED screen according to claim 1, wherein the hydrogen-containing silicone oil is a long-chain linear structure and phenyl-free hydrogen-containing silicone oil, and the hydrogen content is 0.18% -0.75%; the content of the Pt catalyst is 2 ppm-10 ppm.
4. The packaging adhesive for the mini LED screen according to claim 1, wherein the hydrogen-containing silicone oil is added into allyl glycidyl ether in a dropwise manner, and the dropwise adding speed is 2.5-6 g/min; the heating temperature range of the allyl glycidyl ether is 70-90 ℃; the temperature range after the temperature rise is 110-120 ℃; the stirring reaction time is 1-3 hours.
5. The packaging adhesive for the mini LED screen according to claim 1, wherein in the component A, the antioxidant is one or more of triphenyl phosphite, trioctyl phosphite, 2, 6-di-tert-butyl-4-methylphenol and bisdodecyl thiodipropionate; the defoaming agent is an organic silicon defoaming agent.
6. The packaging adhesive for the mini LED screen according to claim 5, wherein the defoaming agent is one or more than two of Tego900, Tego910, Tego940 and Tego 961.
7. The packaging adhesive for the mini LED screen according to claim 1, wherein the curing agent in the component B is a modified alicyclic amine curing agent; the catalyst is one or more than two of 2,4, 6-tri (dimethylamino methyl) phenol, triethanolamine and trimethyl amino methyl phenol.
8. The packaging adhesive for the mini LED screen according to claim 7, wherein the modified alicyclic amine curing agent is one or more of R-2265, R-2266, R-2269 and R-3301.
9. A method for preparing the packaging adhesive of the mini LED screen of any one of claims 1 to 8 is characterized by comprising the following steps:
(1) uniformly mixing the organic silicon modified epoxy resin, the antioxidant and the defoaming agent to obtain a component A, and uniformly mixing the curing agent and the catalyst to obtain a component B;
(2) and uniformly mixing the component A and the component B, and then standing at room temperature to obtain the cured mini LED screen packaging adhesive.
10. The method of claim 9, wherein: the standing time in the step (2) is 2-6 h.
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