CN116814206A - Epoxy sealant for flexible display screen and preparation method thereof - Google Patents

Epoxy sealant for flexible display screen and preparation method thereof Download PDF

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Publication number
CN116814206A
CN116814206A CN202310783641.8A CN202310783641A CN116814206A CN 116814206 A CN116814206 A CN 116814206A CN 202310783641 A CN202310783641 A CN 202310783641A CN 116814206 A CN116814206 A CN 116814206A
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epoxy
hydrotalcite
flexible display
biochar
intercalated
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CN116814206B (en
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廖仲亮
兰婷婷
侯艳
刘远文
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Shenzhen Future New Material Industry Co ltd
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Shenzhen Future New Material Industry Co ltd
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Abstract

The invention discloses an epoxy sealant for a flexible display screen and a preparation method thereof, wherein a carboxymethyl cellulose solution and a mixed salt solution are blended, then hydrothermal reaction is carried out to obtain carboxymethyl cellulose intercalated hydrotalcite, then calcination is carried out to obtain biochar intercalated hydrotalcite, the obtained biochar has a certain adsorption effect on oxygen, and meanwhile, the biochar is intercalated in a hydrotalcite structure, so that the hydrotalcite structure is more compact and can play a role in blocking oxygen to a certain extent; according to the invention, the epoxy silane coupling agent is used for modifying the biochar intercalated hydrotalcite, epoxy groups are introduced into the surface of the biochar intercalated hydrotalcite, then the epoxy groups react with amino groups, octadecylamine is grafted on the hydrotalcite, the octadecylamine has a longer hydrophobic alkyl long-chain structure, and the octadecylamine is introduced into the epoxy sealant, so that the water absorption rate of the epoxy sealant can be effectively reduced.

Description

Epoxy sealant for flexible display screen and preparation method thereof
Technical Field
The invention relates to the technical field of epoxy sealants, in particular to an epoxy sealant for a flexible display screen and a preparation method thereof.
Background
At present, more and more electronic devices with display functions are widely applied to daily life and work of people, bring great convenience to daily life and work of people, and become an indispensable important tool for people at present. The main components of the electronic device for realizing the display function are a display screen, which can be a flexible display screen capable of being bent and a rigid display screen not capable of being bent according to bending characteristics.
The flexible display screen is applied to the fields of black-and-white display screens, various mobile phones, notebook computers, station display boards and the like in daily life, and along with the continuous development of technology, the sensitivity degree of a display luminescent material to water vapor and oxygen is higher and higher, so that the development of a sealant with low water absorption rate, high oxygen barrier rate and better adhesion to flexible materials is very critical and necessary.
The Chinese patent document CN201510481688.4 discloses a room temperature curing ultralow temperature epoxy sealant and a preparation method thereof, wherein the epoxy sealant comprises 40-60 parts of polyurethane modified bisphenol S type glycidyl ether epoxy resin, 40-60 parts of 680 epoxy resin, 20-33 parts of alicyclic amine curing agent and 10-30 parts of T-31 curing agent, and the prepared epoxy sealant has good low temperature bonding and sealing performance, but has higher water absorption rate and still needs to be further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the epoxy sealant for the flexible display screen and the preparation method thereof, and the prepared epoxy sealant has the characteristics of low water absorption rate and high oxygen barrier rate.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the epoxy sealant for the flexible display screen comprises the following raw materials in parts by weight: 40-50 parts of epoxy resin, 20-30 parts of polyether amine, 10-20 parts of hydrotalcite composite material, 0.1-1 part of dispersing agent and 0.1-1 part of curing accelerator.
Preferably, the preparation method of the hydrotalcite composite material comprises the following steps:
(1) Dissolving magnesium nitrate, aluminum nitrate and urea in water to prepare a mixed salt solution, adding a carboxymethyl cellulose solution into the mixed salt solution under the stirring condition, transferring the mixed salt solution into a reaction kettle for hydrothermal reaction, centrifuging and freeze-drying after the reaction is completed to obtain carboxymethyl cellulose intercalated hydrotalcite;
(2) Calcining the carboxymethyl cellulose intercalated hydrotalcite in a nitrogen atmosphere to obtain biochar intercalated hydrotalcite;
(3) Dispersing biochar intercalated hydrotalcite in ethanol water solution, adding epoxy silane coupling agent into the solution, stirring the mixture for reaction, centrifuging, washing and drying the mixture to obtain epoxy modified hydrotalcite material;
(4) Dispersing epoxy modified hydrotalcite material in ethanol solvent, adding octadecylamine, heating and stirring to react, filtering, washing and drying to obtain hydrotalcite composite material.
Preferably, in the step (1), the mass ratio of the magnesium nitrate to the aluminum nitrate to the urea to the carboxymethyl cellulose solution is 4-6:2-3:3-4:40-50, and the mass fraction of the carboxymethyl cellulose solution is 5-10%.
Preferably, in the step (1), the temperature of the hydrothermal reaction is 100-120 ℃, and the time of the hydrothermal reaction is 12-18 hours.
Preferably, in the step (2), the calcination temperature is 400-500 ℃ and the calcination time is 1-2h.
Preferably, in the step (3), the mass ratio of the biochar intercalated hydrotalcite to the ethanol aqueous solution to the epoxy silane coupling agent is 4-8:100:1-2.
Preferably, in the step (3), the mass fraction of the ethanol aqueous solution is 60-80%.
Preferably, in the step (4), the mass ratio of the epoxy group modified hydrotalcite material to the octadecylamine is 10-15:4-6.
Preferably, in the step (4), the reaction temperature is 60-70 ℃ and the reaction time is 4-8h.
The invention also provides a preparation method of the epoxy sealant, which comprises the following steps: uniformly stirring and mixing epoxy resin, polyether amine, hydrotalcite composite material, a dispersing agent and a curing agent, then rolling into paste on a grinder, and then vacuum defoaming to obtain the epoxy sealant.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the carboxymethyl cellulose solution and the mixed salt solution are blended, then hydrothermal reaction is carried out to obtain carboxymethyl cellulose intercalated hydrotalcite, and then calcination is carried out to obtain the biochar intercalated hydrotalcite, wherein the obtained biochar has a certain adsorption effect on oxygen, and meanwhile, the biochar is intercalated in a hydrotalcite structure, so that the hydrotalcite structure is more compact, and the effect of blocking oxygen can be achieved to a certain extent.
(2) According to the invention, the epoxy silane coupling agent is used for modifying the biochar intercalated hydrotalcite, epoxy groups are introduced into the surface of the biochar intercalated hydrotalcite, then the epoxy groups react with amino groups, octadecylamine is grafted on the hydrotalcite, the octadecylamine has a longer hydrophobic alkyl long-chain structure, and the octadecylamine is introduced into the epoxy sealant, so that the water absorption rate of the epoxy sealant can be effectively reduced.
Detailed Description
The present invention will be described in further detail with reference to the following preferred examples, but the present invention is not limited to the following examples.
Unless otherwise specified, the chemical reagents involved in the present invention are all commercially available.
The epoxy resin used in the invention is bisphenol A type epoxy resin, the epoxy equivalent is 180-190, and the epoxy resin is purchased from Wan Qing chemical technology Co., ltd;
polyetheramines were purchased from Jinbang environmental protection technology Co., ltd., CAS number: 9046-10-0;
the model of the dispersant is BYK-130;
curing accelerators were purchased from wehai morning source molecular new materials, model: CYD-N2401;
the epoxy silane coupling agent is selected to be KH560.
Example 1
The preparation method of the epoxy sealant for the flexible display screen comprises the following steps:
uniformly stirring and mixing 40 parts of epoxy resin, 30 parts of polyether amine, 10 parts of hydrotalcite composite material, 0.5 part of dispersing agent and 0.5 part of curing agent, then rolling into paste on a grinding machine, and then vacuum defoaming for 30min to obtain epoxy sealant;
the preparation method of the hydrotalcite composite material comprises the following steps:
(1) Dissolving 4g of magnesium nitrate, 2g of aluminum nitrate and 3g of urea in 100g of water to prepare a mixed salt solution, adding 40g of 5wt% of carboxymethyl cellulose solution into the mixed salt solution under the condition of stirring, transferring the mixed salt solution into a reaction kettle, carrying out hydrothermal reaction for 18h at 100 ℃, centrifuging and freeze-drying after the reaction is finished to obtain carboxymethyl cellulose intercalated hydrotalcite;
(2) Calcining the carboxymethyl cellulose intercalated hydrotalcite in nitrogen atmosphere at 400 ℃ for 2 hours to obtain the biochar intercalated hydrotalcite;
(3) Dispersing 4g of biochar intercalated hydrotalcite in 100g of 60wt% ethanol water solution, then adding 1g of KH560 into the solution, stirring the mixture for 2h for reaction, and obtaining an epoxy modified hydrotalcite material through centrifugation, washing and drying;
(4) Dispersing 10g of epoxy modified hydrotalcite material in 200mL of ethanol solvent, adding 4g of octadecylamine, heating and stirring at 60 ℃ for reaction for 8 hours, and filtering, washing and drying after the reaction is completed to obtain the hydrotalcite composite material.
Example 2
The preparation method of the epoxy sealant for the flexible display screen comprises the following steps:
uniformly stirring and mixing 50 parts of epoxy resin, 25 parts of polyether amine, 20 parts of hydrotalcite composite material, 0.1 part of dispersing agent and 1 part of curing agent, then rolling into paste on a grinding machine, and then vacuum defoaming for 30min to obtain epoxy sealant;
the preparation method of the hydrotalcite composite material comprises the following steps:
(1) Dissolving 6g of magnesium nitrate, 3g of aluminum nitrate and 4g of urea in 100g of water to prepare a mixed salt solution, adding 40g of 10wt% of carboxymethyl cellulose solution into the mixed salt solution under the condition of stirring, transferring the mixed salt solution into a reaction kettle, carrying out hydrothermal reaction for 12 hours at 120 ℃, and centrifuging and freeze-drying after the reaction is finished to obtain carboxymethyl cellulose intercalated hydrotalcite;
(2) Calcining the carboxymethyl cellulose intercalated hydrotalcite in nitrogen atmosphere at 500 ℃ for 1h to obtain the biochar intercalated hydrotalcite;
(3) Dispersing 8g of biochar intercalated hydrotalcite in 100g of 60wt% ethanol water solution, then adding 2g of KH560 into the solution, stirring the mixture for 2h for reaction, and obtaining an epoxy modified hydrotalcite material through centrifugation, washing and drying;
(4) Dispersing 15g of epoxy modified hydrotalcite material in 200mL of ethanol solvent, adding 6g of octadecylamine, heating and stirring at 70 ℃ for reaction for 4 hours, and filtering, washing and drying after the reaction is completed to obtain the hydrotalcite composite material.
Example 3
The preparation method of the epoxy sealant for the flexible display screen comprises the following steps:
uniformly stirring and mixing 45 parts of epoxy resin, 20 parts of polyether amine, 15 parts of hydrotalcite composite material, 0.6 part of dispersing agent and 0.8 part of curing agent, then rolling into paste on a grinding machine, and then vacuum defoaming for 30min to obtain epoxy sealant;
the preparation method of the hydrotalcite composite material comprises the following steps:
(1) Dissolving 5g of magnesium nitrate, 2g of aluminum nitrate and 4g of urea in 100g of water to prepare a mixed salt solution, adding 50g of 8wt% carboxymethyl cellulose solution into the mixed salt solution under the condition of stirring, transferring the mixed salt solution into a reaction kettle, carrying out hydrothermal reaction for 18h at 100 ℃, centrifuging and freeze-drying after the reaction is finished to obtain carboxymethyl cellulose intercalated hydrotalcite;
(2) Calcining the carboxymethyl cellulose intercalated hydrotalcite in nitrogen atmosphere at the calcining temperature of 450 ℃ for 2 hours to obtain the biochar intercalated hydrotalcite;
(3) Dispersing 6g of biochar intercalated hydrotalcite in 100g of 80wt% ethanol water solution, then adding 1.5g of KH560 into the solution, stirring the mixture for 2h for reaction, and obtaining an epoxy modified hydrotalcite material through centrifugation, washing and drying;
(4) Dispersing 12g of epoxy modified hydrotalcite material in 200mL of ethanol solvent, adding 5g of octadecylamine, heating and stirring at 65 ℃ for reaction for 6h, and filtering, washing and drying after the reaction is completed to obtain the hydrotalcite composite material.
Comparative example 1
The preparation method of the epoxy sealant for the flexible display screen comprises the following steps:
uniformly stirring and mixing 45 parts of epoxy resin, 20 parts of polyether amine, 15 parts of hydrotalcite material, 0.6 part of dispersing agent and 0.8 part of curing agent, then rolling into paste on a grinding machine, and then vacuum defoaming for 30min to obtain epoxy sealant;
the preparation method of the hydrotalcite material comprises the following steps:
5g of magnesium nitrate, 2g of aluminum nitrate and 4g of urea are dissolved in 100g of water to prepare mixed salt solution, then the mixed salt solution is transferred into a reaction kettle, hydrothermal reaction is carried out for 18h at 100 ℃, and after the reaction is finished, the hydrotalcite material is obtained through centrifugation and freeze drying.
Comparative example 2
The preparation method of the epoxy sealant for the flexible display screen comprises the following steps:
uniformly stirring and mixing 45 parts of epoxy resin, 20 parts of polyether amine, 15 parts of hydrotalcite composite material, 0.6 part of dispersing agent and 0.8 part of curing agent, then rolling into paste on a grinding machine, and then vacuum defoaming for 30min to obtain epoxy sealant;
the preparation method of the hydrotalcite composite material comprises the following steps:
(1) Dissolving 5g of magnesium nitrate, 2g of aluminum nitrate and 4g of urea in 100g of water to prepare a mixed salt solution, adding 50g of 8wt% carboxymethyl cellulose solution into the mixed salt solution under the condition of stirring, transferring the mixed salt solution into a reaction kettle, carrying out hydrothermal reaction for 18h at 100 ℃, centrifuging and freeze-drying after the reaction is finished to obtain carboxymethyl cellulose intercalated hydrotalcite;
(2) Calcining the carboxymethyl cellulose intercalated hydrotalcite in nitrogen atmosphere at the calcining temperature of 450 ℃ for 2 hours to obtain the biochar intercalated hydrotalcite;
(3) Dispersing 6g of biochar intercalated hydrotalcite in 100g of 80wt% ethanol water solution, then adding 1.5g of KH560 into the solution, stirring the mixture for 2h for reaction, and obtaining the hydrotalcite composite material through centrifugation, washing and drying.
The epoxy sealants prepared in examples 1-3 and comparative examples 1-2 were subjected to performance testing as follows:
water absorption test: the method comprises the steps of performing a test by referring to a test method of water absorption of standard ASTM D570-05 plastic, curing an adhesive to prepare a sample with the thickness of 76.2mm multiplied by 25.4mm multiplied by 3.2mm, testing the water absorption after soaking the sample in water at 23 ℃ for 24 hours, and calculating the water absorption according to a formula in the standard;
oxygen transmission rate test: the epoxy sealants prepared in examples 1 to 3 and comparative examples 1 to 2 were flat-pressed into a film having a thickness of 400. Mu.m, and then tested by an oxygen permeation rate meter under the conditions of 23℃and 50% RH, and the test results are shown in the following table:
water absorption (%) oxygen transmission (cc/m 2. 24 h)
Finally, it should be noted that: the above examples are not intended to limit the present invention in any way. Modifications and improvements will readily occur to those skilled in the art upon the basis of the present invention. Accordingly, any modification or improvement made without departing from the spirit of the invention is within the scope of the invention as claimed.

Claims (10)

1. The epoxy sealant for the flexible display screen is characterized by comprising the following raw materials in parts by weight: 40-50 parts of epoxy resin, 20-30 parts of polyether amine, 10-20 parts of hydrotalcite composite material, 0.1-1 part of dispersing agent and 0.1-1 part of curing accelerator.
2. The epoxy sealant for a flexible display screen according to claim 1, wherein the hydrotalcite composite material is prepared by the following method:
(1) Dissolving magnesium nitrate, aluminum nitrate and urea in water to prepare a mixed salt solution, adding a carboxymethyl cellulose solution into the mixed salt solution under the stirring condition, transferring the mixed salt solution into a reaction kettle for hydrothermal reaction, centrifuging and freeze-drying after the reaction is completed to obtain carboxymethyl cellulose intercalated hydrotalcite;
(2) Calcining the carboxymethyl cellulose intercalated hydrotalcite in a nitrogen atmosphere to obtain biochar intercalated hydrotalcite;
(3) Dispersing biochar intercalated hydrotalcite in ethanol water solution, adding epoxy silane coupling agent into the solution, stirring the mixture for reaction, centrifuging, washing and drying the mixture to obtain epoxy modified hydrotalcite material;
(4) Dispersing epoxy modified hydrotalcite material in ethanol solvent, adding octadecylamine, heating and stirring to react, filtering, washing and drying to obtain hydrotalcite composite material.
3. The epoxy sealant for a flexible display screen according to claim 2, wherein in the step (1), the mass ratio of magnesium nitrate, aluminum nitrate, urea and carboxymethyl cellulose solution is 4-6:2-3:3-4:40-50, and the mass fraction of the carboxymethyl cellulose solution is 5-10%.
4. The epoxy sealer for a flexible display panel according to claim 2, wherein in the step (1), the temperature of the hydrothermal reaction is 100 to 120 ℃ and the time of the hydrothermal reaction is 12 to 18 hours.
5. The epoxy sealer for flexible display panel according to claim 2, wherein in the step (2), the calcination temperature is 400 to 500 ℃ and the calcination time is 1 to 2 hours.
6. The epoxy sealant for a flexible display screen according to claim 2, wherein in the step (3), the mass ratio of the biochar intercalated hydrotalcite, the ethanol aqueous solution and the epoxy silane coupling agent is 4-8:100:1-2.
7. The epoxy sealer for a flexible display panel according to claim 2, wherein in the step (3), the mass fraction of the aqueous ethanol solution is 60 to 80%.
8. The epoxy sealer for flexible display according to claim 2, wherein in the step (4), the mass ratio of the epoxy-based modified hydrotalcite material to octadecylamine is 10-15:4-6.
9. The epoxy sealer for flexible display according to claim 2, wherein in the step (4), the heating and stirring reaction temperature is 60 to 70 ℃ and the heating and stirring reaction time is 4 to 8 hours.
10. A method of preparing an epoxy sealant for flexible display screens as claimed in any one of claims 1 to 9, comprising the steps of: uniformly stirring and mixing epoxy resin, polyether amine, hydrotalcite composite material, a dispersing agent and a curing agent, then rolling into paste on a grinder, and then vacuum defoaming to obtain the epoxy sealant.
CN202310783641.8A 2023-06-29 2023-06-29 Epoxy sealant for flexible display screen and preparation method thereof Active CN116814206B (en)

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Publication number Priority date Publication date Assignee Title
CN104874365A (en) * 2015-05-27 2015-09-02 闫春燕 Carboxymethyl cellulose ion intercalated hydrotalcite-like composite material, and preparation method and application thereof
CN107670632A (en) * 2017-10-19 2018-02-09 北京化工大学 A kind of medium temperature carbon dioxide absorber and its preparation and application
CN107903827A (en) * 2017-11-10 2018-04-13 雷笑天 A kind of preparation method of high-adhesion high temperature resistant anchoring adhesive
CN109608745A (en) * 2018-12-29 2019-04-12 安徽天康(集团)股份有限公司 A kind of power cable
CN110327904A (en) * 2019-07-19 2019-10-15 四川正祥环保技术有限公司 A kind of wastewater treatment material and preparation method thereof removing lead waste water
CN112813678A (en) * 2020-12-31 2021-05-18 陕西科技大学 Self-cleaning hydrotalcite/fiber fabric composite material with wear-resisting and self-repairing functions and preparation method thereof
CN114634783A (en) * 2022-04-13 2022-06-17 广州慧能新材料科技有限公司 Halogen-free flame-retardant high-temperature-resistant epoxy resin sealant and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104874365A (en) * 2015-05-27 2015-09-02 闫春燕 Carboxymethyl cellulose ion intercalated hydrotalcite-like composite material, and preparation method and application thereof
CN107670632A (en) * 2017-10-19 2018-02-09 北京化工大学 A kind of medium temperature carbon dioxide absorber and its preparation and application
CN107903827A (en) * 2017-11-10 2018-04-13 雷笑天 A kind of preparation method of high-adhesion high temperature resistant anchoring adhesive
CN109608745A (en) * 2018-12-29 2019-04-12 安徽天康(集团)股份有限公司 A kind of power cable
CN110327904A (en) * 2019-07-19 2019-10-15 四川正祥环保技术有限公司 A kind of wastewater treatment material and preparation method thereof removing lead waste water
CN112813678A (en) * 2020-12-31 2021-05-18 陕西科技大学 Self-cleaning hydrotalcite/fiber fabric composite material with wear-resisting and self-repairing functions and preparation method thereof
CN114634783A (en) * 2022-04-13 2022-06-17 广州慧能新材料科技有限公司 Halogen-free flame-retardant high-temperature-resistant epoxy resin sealant and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
郑水林: "《粉体表面改性》", vol. 2, 中国建材工业出版社, pages: 228 *

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