An adsorption pad for electronic display screen and its preparation process

By adding specific flame retardant antioxidants to the porous polyurethane adsorption film, the problem of adsorbing pads being easily flammable and oxidized under high temperature environments is solved, and its service life and performance are significantly improved.

CN116285754BActive Publication Date: 2025-05-09ANHUI HECHEN NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202310415472.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-04-18
Publication Date
2025-05-09
Estimated Expiration
2043-04-18

AI Technical Summary

Technical Problem

The adsorption pads for the production of existing electronic display screens are prone to combust during the polishing process and are prone to oxidation under long-term high-temperature environments, resulting in a shorter service life.

Method used

The flame retardant and antioxidant properties of the adsorbent film are improved by adding flame retardant and antioxidant agents synthesized from raw materials such as iminodiethyl diacetate, tetra-dimethylaminopyridine and diphenylphosphinyl chloride to the porous polyurethane adsorption film.

Benefits of technology

It significantly improves the flame retardant and oxidation resistance of the adsorbent pad, extends its service life, and reduces the risk of combustion and oxidation.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses an adsorption pad for an electronic display screen, comprising a dustproof film, a porous polyurethane adsorption film, a polyurethane adhesive, a double-sided adhesive layer and a release paper arranged in sequence from an adsorption end to a fixed end; the porous polyurethane adsorption film: diphenylphosphinyl chloride and diethyl iminodiacetate are subjected to nucleophilic substitution to obtain an intermediate 1, and the obtained intermediate 1 is reacted with ethylenediamine to obtain an intermediate 2; β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionyl chloride is used as a raw material, and an amidation condensation reaction is carried out with two amine groups on the intermediate 2 to obtain a flame retardant antioxidant; the obtained flame retardant antioxidant is added to a polyurethane material preparation process; the obtained polyurethane material is subjected to a film-forming process to obtain a porous polyurethane adsorption film, and the flame retardant antioxidant obtained by the invention is added to the polyurethane material preparation process, so that the prepared porous polyurethane adsorption film has good anti-oxidation and flame retardant properties.
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Description

Technical Field

[0001] The invention relates to the technical field of adsorption pads, and in particular to an adsorption pad for an electronic display screen and a preparation process thereof. Background Art

[0002] Chinese patent number CN113150712A is an adsorption pad for electronic display production and its preparation process, wherein the adsorption pad is provided with a dustproof film, a porous polyurethane adsorption film, a polyurethane adhesive, a base fabric layer, a double-sided adhesive layer, and a release paper in sequence from the adsorption end to the fixed end; the adsorption pad is prepared by the following steps: step one, preparing a base fabric, and corona treating the base fabric to roughen the surface, step two, coating a polyurethane adhesive on the surface of the roughened base fabric, gluing the porous polyurethane adsorption film and drying and curing to obtain a base pad, step three: ripening the base pad, step four: pasting double-sided adhesive on the surface of the ripened base pad, pasting release paper on the outside of the double-sided adhesive, and rolling up to obtain an adsorption pad roll, step five: cutting the adsorption pad roll according to specification requirements to obtain an adsorption pad for electronic display production;

[0003] In the prior art, the adsorption pad is in a high temperature environment during the polishing process, which may cause the adsorption pad to be at risk of burning. In addition, the adsorption pad may be easily oxidized during a long period of time at high temperature, which greatly threatens the service life of the adsorption pad. Summary of the invention

[0004] The purpose of the present invention is to solve the above-mentioned background technical problems and to provide an adsorption pad for electronic display screen and its preparation process.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] An adsorption pad for an electronic display screen, comprising a dustproof film, a porous polyurethane adsorption film, a polyurethane adhesive, a double-sided adhesive layer, and a release paper arranged in sequence from an adsorption end to a fixed end;

[0007] The porous polyurethane adsorption membrane is prepared by the following steps:

[0008] Step 1: Add diethyl iminodiacetate and 4-dimethylaminopyridine to chloroform and mix, add triethylamine under nitrogen protection to obtain solution A, and then add diphenylphosphine chloride to chloroform and mix to obtain solution B;

[0009] At room temperature, solution B is added dropwise to solution A. After the addition is complete, the temperature is raised to 75°C and the reaction time is 2-18 hours to obtain intermediate 1;

[0010] Step 2: After mixing intermediate 1 with tetrahydrofuran, ethylenediamine is added dropwise, and after the addition, the temperature is raised to 65°C and the reaction time is 3-4h to obtain intermediate 2;

[0011] Step 3: Mix β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride with chloroform to obtain solution C; add intermediate 2 and triethylamine to chloroform to obtain solution D;

[0012] At a temperature of 15°C and under nitrogen protection, solution D was added dropwise to solution C, the temperature was raised to 45°C, and the reaction was carried out at a constant temperature for 12 hours. After post-treatment, a flame retardant antioxidant was obtained;

[0013] Step 4: adding the obtained flame retardant antioxidant to the polyurethane material preparation process;

[0014] Step 5: The obtained polyurethane material is subjected to a film-forming process to prepare a porous polyurethane adsorption film.

[0015] As a further solution of the present invention: the dosage ratio of diethyl iminodiacetate, diphenylphosphinyl chloride, dimethylaminopyridine, triethylamine and chloroform is controlled to be 1 mol: 1-1.5 mol: 0.06-0.08 mol: 1-1.2 mol: 2-3L;.

[0016] As a further solution of the present invention: the dosage ratio of intermediate 1, ethylenediamine and tetrahydrofuran is controlled to be 1 mol:1-2 mol:1-2L.

[0017] As a further solution of the present invention: the dosage ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride, intermediate 2, triethylamine and chloroform is controlled to be 2-2.4 mol: 1 mol: 1-1.2 mol: 1-3L.

[0018] As a further solution of the present invention: the mass of the flame retardant antioxidant accounts for 5-8% of the mass of the reaction system of the polyurethane material.

[0019] As a further scheme of the present invention: in step 4, the polyether polyol is dehydrated and then stirred evenly, isophorone diisocyanate and polydimethylsiloxane are added to the system respectively, and then the temperature is raised to 80-90°C for prepolymerization, then the temperature is lowered to 80°C for chain extension reaction, 10% by mass of 1,4-butanediol solution containing flame retardant antioxidant is added, the temperature is kept for reaction for 2-3h, then the temperature is lowered to 40°C, triethylamine is added for neutralization reaction; finally, the temperature is lowered to room temperature, deionized water is added and emulsified with high-speed stirring, and a polyurethane material with flame retardancy and antioxidant properties is obtained.

[0020] A preparation process of an adsorption pad for an electronic display screen, characterized in that it comprises the following steps:

[0021] Step 1: prepare the base fabric, roughen both sides of the base fabric through a corona treatment device, and make the roughened base fabric into a roll for standby use;

[0022] Step 2: applying a polyurethane adhesive on the upper surface of the roughened base fabric, pasting a porous polyurethane adsorption film on the upper surface of the base fabric coated with the polyurethane adhesive, curing the film after pasting, cooling the film to room temperature, and using a laminating device to cover a dustproof film on the upper surface of the porous polyurethane adsorption film to obtain a base pad;

[0023] Step 3: placing the base mat obtained in step 2 in a curing chamber for 20-30 hours to obtain a cured base mat;

[0024] Step 4: Paste double-sided tape on the side of the matured base pad away from the dust-proof film, and paste release paper on the outside of the double-sided tape to obtain an adsorption pad for the production of an electronic display screen.

[0025] Beneficial effects of the present invention:

[0026] The present invention uses diphenylphosphine chloride and diethyl iminodiacetate for nucleophilic substitution, triethylamine as an acid-binding agent to promote the forward reaction, and chloroform as a solvent to obtain an intermediate 1 with flame retardant properties, and the obtained intermediate 1 is reacted with ethylenediamine to obtain a phosphorus-nitrogen synergistic flame retardant intermediate 2 with excellent flame retardant properties;

[0027] β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionyl chloride is used as a raw material to undergo an amidation condensation reaction with two amine groups on the intermediate 2 to obtain a flame retardant antioxidant having a molecular structure containing hindered phenol units, which not only has excellent flame retardant properties, but also has excellent antioxidant properties;

[0028] The obtained flame retardant antioxidant is added into the preparation process of polyurethane material, so that the prepared porous polyurethane adsorption film has good anti-oxidation and flame retardant properties, thereby improving the performance of the adsorption film and effectively increasing the service life of the adsorption pad. DETAILED DESCRIPTION

[0029] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Example 1

[0031] The present invention is an adsorption pad for an electronic display screen, comprising a dustproof film, a porous polyurethane adsorption film, a polyurethane adhesive, a double-sided adhesive layer, and a release paper arranged in sequence from an adsorption end to a fixed end;

[0032] The preparation process of the adsorption pad for producing electronic display screens comprises the following steps:

[0033] Step 1: prepare the base fabric, roughen both sides of the base fabric through a corona treatment device, and make the roughened base fabric into a roll for standby use;

[0034] Step 2: applying a polyurethane adhesive on the upper surface of the roughened base fabric, pasting a porous polyurethane adsorption film on the upper surface of the base fabric coated with the polyurethane adhesive, curing the film after pasting, cooling the film to room temperature, and using a laminating device to cover a dustproof film on the upper surface of the porous polyurethane adsorption film to obtain a base pad;

[0035] Step 3: placing the base mat obtained in step 2 in a curing chamber for 20-30 hours to obtain a cured base mat;

[0036] Step 4: Paste a double-sided tape on the side of the matured base pad away from the dustproof film, and paste a release paper on the outside of the double-sided tape to obtain an adsorption pad for the production of an electronic display screen;

[0037] Wherein, the porous polyurethane adsorption membrane is prepared by the following steps:

[0038] Step 1: Add diethyl iminodiacetate and 4-dimethylaminopyridine to chloroform and mix, add triethylamine under nitrogen protection to obtain solution A, and then add diphenylphosphine chloride to chloroform and mix to obtain solution B;

[0039] At room temperature, solution B is added dropwise to solution A, and the adding time is controlled within 10-30 min. After the adding is completed, the temperature is raised to 75° C., and the reaction time is 2-18 h. After post-treatment, intermediate 1 is obtained;

[0040] The dosage ratio of diethyl iminodiacetate, diphenylphosphine chloride, dimethylaminopyridine, triethylamine and chloroform is controlled to be 1 mol: 1 mol: 0.06 mol: 1 mol: 2 L; the volume of chloroform in solution A is 1 L, and the volume of chloroform in solution B is 1 L;

[0041] The post-treatment steps are: washing with NaOH solution, dilute HCl, and saturated saline solution, drying with anhydrous NaSO4, filtering, and rotary evaporation to obtain a light yellow oil. After standing for a period of time, crystals precipitate, filter, and wash the crystals with a small amount of ethyl acetate until they turn white.

[0042] Step 2: After mixing the intermediate 1 obtained in step 1 with tetrahydrofuran, ethylenediamine is added dropwise, and the addition time is controlled to be 8-15 min. After the addition, the temperature is raised to 65° C., and the reaction time is 3-4 h. After post-treatment, the intermediate 2 is obtained;

[0043] Wherein, the dosage ratio of intermediate 1, ethylenediamine and tetrahydrofuran is controlled to be 1 mol:1 mol:1L;

[0044] The post-treatment steps are as follows: after the reaction solution is cooled to room temperature, the solvent and most of the ethylenediamine are removed by rotary evaporation, and then the residual ethylenediamine is removed by recrystallization;

[0045] Step 3: Mix β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride with chloroform to obtain solution C; add intermediate 2 and triethylamine to chloroform to obtain solution D;

[0046] At a temperature of 15°C and under nitrogen protection, solution D was added dropwise to solution C, the temperature was raised to 45°C, and the reaction was carried out at a constant temperature for 12 hours. After post-treatment, a flame retardant antioxidant was obtained;

[0047] Wherein, the dosage ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride, intermediate 2, triethylamine and chloroform is controlled to be 2 mol:1 mol:1 mol:1 L;

[0048] The volume of chloroform in solution C is 1 L, and the volume of chloroform in solution D is 1 L;

[0049] The post-treatment steps are: removing the solvent and the acid-binding agent by distillation under reduced pressure to obtain a light yellow solid; dissolving the solid with dichloromethane, first washing the solution with a NaHCO3 aqueous solution for 3 times, then washing the organic phase with 35 mL of a hydrochloric acid solution for 3 times, and finally washing the organic phase with a saturated saline solution for 2 times, drying the obtained organic phase with anhydrous MgSO4 overnight, removing the solvent by distillation under reduced pressure, washing the obtained solid with a 1:1 ethanol and NaOH solution for 3 times, and finally washing with a large amount of distilled water until the filtrate is neutral, and drying to obtain a flame retardant antioxidant;

[0050] Step 4: Dehydrate the polyether polyol, stir evenly, add isophorone diisocyanate and polydimethylsiloxane into the system respectively, then heat to 80-90°C for prepolymerization, then cool to 80°C for chain extension, add 10% by mass of 1,4-butanediol solution containing flame retardant and antioxidant, keep warm for 2-3h, then cool to 40°C, add triethylamine for neutralization; finally cool to room temperature, add deionized water and stir at high speed for emulsification, and obtain a polyurethane material with flame retardancy and antioxidant properties;

[0051] The mass of the flame retardant antioxidant accounts for 5% of the mass of the reaction system of the polyurethane material;

[0052] Step 5: The obtained polyurethane material is subjected to a film-forming process to prepare a porous polyurethane adsorption film.

[0053] Example 2

[0054] The difference from the above-mentioned embodiment 1 is that:

[0055] The dosage ratio of diethyl iminodiacetate, diphenylphosphine chloride, dimethylaminopyridine, triethylamine and chloroform is controlled to be 1 mol:1.2 mol:0.07 mol:1.1 mol:2.5 L; the volume of chloroform in solution A is 1.2 L, and the volume of chloroform in solution B is 1.2 L;

[0056] The dosage ratio of intermediate 1, ethylenediamine and tetrahydrofuran is controlled to be 1 mol:1.5 mol:1.1 L;

[0057] The dosage ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride, intermediate 2, triethylamine and chloroform was controlled to be 2.2 mol: 1 mol: 1.1 mol: 2 L;

[0058] The volume of chloroform in solution C is 1.2 L, and the volume of chloroform in solution D is 1.2 L;

[0059] The mass of the flame retardant antioxidant accounts for 7% of the mass of the reaction system of the polyurethane material.

[0060] Example 3

[0061] The difference from the above embodiment 1 is that:

[0062] The dosage ratio of diethyl iminodiacetate, diphenylphosphine chloride, dimethylaminopyridine, triethylamine and chloroform is controlled to be 1 mol:1.5 mol:0.08 mol:1.2 mol:3 L; the volume of chloroform in solution A is 1.5 L, and the volume of chloroform in solution B is 1.5 L;

[0063] The dosage ratio of intermediate 1, ethylenediamine and tetrahydrofuran is controlled to be 1 mol: 2 mol: 2 L;

[0064] The dosage ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride, intermediate 2, triethylamine and chloroform was controlled to be 2.4 mol: 1 mol: 1.2 mol: 3 L;

[0065] The volume of chloroform in solution C is 1.5 L, and the volume of chloroform in solution D is 1.5 L;

[0066] The mass of the flame retardant antioxidant accounts for 8% of the mass of the reaction system of the polyurethane material.

[0067] Comparative Example 1

[0068] Comparative Example 1 is a porous polyurethane adsorption film in an adsorption pad of Chinese Patent No. CN113150712A;

[0069] Performance test: The porous polyurethane adsorption membranes of Examples 1-3 and Comparative Example 1 were tested, and the test results are shown in the following table;

[0070] Limiting oxygen index test: using the YG (B) oxygen index tester produced by Wenzhou Darong, according to GB / T-"Textile Combustion Performance Test Oxygen Index Method", the size of the sample to be tested is 80mm*80mm;

[0071] Antioxidation test: The sample size is 80mm*80mm, and the temperature is raised to 200℃ at an oxygen concentration of 99.5%, an oxygen flow rate of 50mL / min, and a heating rate of 20℃ / min. According to the national standard GB / T 19466.6-2009, the oxidation induction time under isothermal conditions is measured;

[0072]

[0073] From the data recorded in the above table, it can be seen that the porous polyurethane adsorption film obtained by the present invention has good flame retardant and antioxidant properties.

[0074] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. An adsorption pad for an electronic display screen, characterized in that: The device comprises a dustproof film, a porous polyurethane adsorption film, a polyurethane adhesive, a double-sided adhesive layer, and a release paper arranged in sequence from the adsorption end to the fixed end; The porous polyurethane adsorption membrane is prepared by the following steps: Step 1: Add diethyl iminodiacetate and 4-dimethylaminopyridine to chloroform and mix, add triethylamine under nitrogen protection to obtain solution A, and then add diphenylphosphine chloride to chloroform and mix to obtain solution B; At room temperature, solution B is added dropwise to solution A. After the addition is complete, the temperature is raised to 75°C and the reaction time is 2-18 hours to obtain intermediate 1; Step 2: After mixing intermediate 1 with tetrahydrofuran, ethylenediamine is added dropwise, and after the addition, the temperature is raised to 65°C and the reaction time is 3-4h to obtain intermediate 2; Step 3: Mix β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride with chloroform to obtain solution C; add intermediate 2 and triethylamine to chloroform to obtain solution D; At a temperature of 15°C and under nitrogen protection, solution D was added dropwise to solution C, the temperature was raised to 45°C, and the reaction was carried out at a constant temperature for 12 hours, and a flame retardant antioxidant was obtained after post-treatment; Step 4: Adding flame retardant antioxidant to the polyurethane material preparation process; Step 5: preparing a porous polyurethane adsorption film by subjecting the obtained polyurethane material to a film-forming process; Among them, the mass of the flame retardant antioxidant accounts for 5-8% of the mass of the reaction system of the polyurethane material; the usage ratio of diethyl iminodiacetate and diphenylphosphine chloride is 1 mol: 1-1.5 mol; the usage ratio of intermediate 1 and ethylenediamine is 1 mol: 1-2 mol; the usage ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride and intermediate 2 is 2-2.4 mol: 1 mol.

2. The adsorption pad for an electronic display screen according to claim 1, characterized in that: The usage ratio of diethyl iminodiacetate, diphenylphosphine chloride, dimethylaminopyridine, triethylamine and chloroform is 1 mol: 1-1.5 mol: 0.06-0.08 mol: 1-1.2 mol: 2-3 L.

3. The adsorption pad for an electronic display screen according to claim 1, characterized in that: The usage ratio of intermediate 1, ethylenediamine and tetrahydrofuran is 1 mol: 1-2 mol: 1-2 L.

4. The adsorption pad for an electronic display screen according to claim 1, characterized in that: The usage ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride, intermediate 2, triethylamine and chloroform is 2-2.4 mol: 1 mol: 1-1.2 mol: 1-3 L.

5. The adsorption pad for an electronic display screen according to claim 1, characterized in that: In step 4, the polyether polyol is dehydrated and then stirred evenly, isophorone diisocyanate and polydimethylsiloxane are added to the system respectively, and then the temperature is raised to 80-90°C for prepolymerization reaction, and then the temperature is lowered to 80°C for chain extension reaction, and a 10% by mass fraction of 1,4-butanediol solution containing a flame retardant antioxidant is added, and the reaction is kept warm for 2-3 hours, and then the temperature is lowered to 40°C, and triethylamine is added for neutralization reaction; finally, the temperature is lowered to room temperature, and deionized water is added and emulsified with high-speed stirring to obtain a polyurethane material with flame retardancy and antioxidant properties.

6. A process for preparing an adsorption pad for an electronic display screen as claimed in any one of claims 1 to 5, characterized in that: The following steps are involved: Step 1: prepare the base fabric, roughen both sides of the base fabric through a corona treatment device, and make the roughened base fabric into a roll for standby use; Step 2: applying a polyurethane adhesive on the upper surface of the roughened base fabric, pasting a porous polyurethane adsorption film on the upper surface of the base fabric coated with the polyurethane adhesive, curing the film after pasting, cooling the film to room temperature, and using a laminating device to cover a dustproof film on the upper surface of the porous polyurethane adsorption film to obtain a base pad; Step 3: placing the base mat obtained in step 2 in a curing chamber for 20-30 hours to obtain a cured base mat; Step 4: Paste double-sided tape on the side of the matured base pad away from the dust-proof film, and paste release paper on the outside of the double-sided tape to obtain an adsorption pad for the production of an electronic display screen.

Citation Information

Patent Citations

  • Adsorption pad for production of electronic display screen, and preparation process thereof

    CN113150712A

  • Method for synthesizing dendritic phenolic antioxidant

    CN101704948A

  • Water-borne polyurethane hydrophilic chain extender and preparation method thereof

    CN104211890A