A method for preparing an adsorption pad for mask processing

Abstract

The application discloses a preparation method of an adsorption pad for mask plate processing, which is sequentially arranged from top to bottom by release paper, double-sided adhesive tape, a PET film, double-sided adhesive tape, modified polyurethane porous material and modified polyurethane protective film; the modified polyurethane porous material and the modified polyurethane protective film are both prepared by a mold through modified polyurethane; the modified polyurethane is used to replace the polyurethane porous material and the polyurethane protective film of the existing adsorption pad, so that the adsorption pad simultaneously has wear resistance, high-temperature resistance and antibacterial property, bacteria adhesion is avoided, and the quality during the processing of the adsorption pad is affected.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of adsorption pads, and particularly relates to a preparation method of an adsorption pad for mask plate processing. BACKGROUND

[0002] Chinese Patent No. CN113025222A discloses an adsorption pad for precision polishing of an electronic display screen, which is provided with, from top to bottom, a release paper, double-sided adhesive tape, a PET film, double-sided adhesive tape, a polyurethane porous material and a polyurethane protective film; the application also discloses a preparation method of the adsorption pad for precision polishing of the electronic display screen: first, the PET film is pasted on the top of the polyurethane porous material through double-sided adhesive tape, and then the release paper is pasted on the top of the PET film through double-sided adhesive tape to obtain a composite board; second, the composite board is placed in a roller-type hot press, and the bottom of the composite board is subjected to hot pressing at a pressure of 0.3-0.5 MPa; the hot-pressed composite board is placed in a heating device and heated for 10-15 s at a temperature of 100-115 DEG C; the polyurethane protective film is heated at the same temperature, and the polyurethane protective film is hot-pressed to the bottom of the composite board to obtain a semi-finished product, which is processed, cut and packaged.

[0003] In the prior art, the adsorption pad has the problems of short service life and short service cycle due to the poor high-temperature resistance and wear resistance of the polyurethane material, high production cost, and bacterial adhesion during use, which affects product processing. SUMMARY

[0004] The purpose of the application is to solve the problems in the background art, and a preparation method of an adsorption pad for mask plate processing is provided.

[0005] The purpose of the application can be achieved by the following technical solutions.

[0006] A preparation method of an adsorption pad for mask plate processing, which is obtained by sequentially arranging a release paper, double-sided adhesive tape, a PET film, double-sided adhesive tape, a modified polyurethane porous material and a modified polyurethane protective film from top to bottom; the modified polyurethane porous material and the modified polyurethane protective film are both prepared from modified polyurethane through a mold;

[0007] The preparation process of the modified polyurethane comprises the following steps:

[0008] Step 1: polytetrahydrofuran diol is placed in a reaction container, heated to 50 DEG C under stirring and nitrogen protection, toluene-2, 4-diisocyanate is added dropwise, a promoter dibutyltin dilaurate is added, and a 1, 2, 4-benzene tricarboxylic anhydride solution with a mass fraction of 8% in N, N-dimethylformamide is added to react for 3, to obtain a polyurethane oligomer;

[0009] Step 2: 1-hydroxymethyl-5,5-dimethylhydantin with a mass fraction of 10% is added dropwise to cyanuric chloride acetone solution with a mass fraction of 5%, and the reaction is carried out for 2h; the system is heated to 40℃, and methylsilanetriol is added to the system, and the reaction is carried out for 3h; an intermediate 1 is obtained;

[0010] Step 3: the polyurethane oligomer is added to the intermediate 1, and after stirring at 100℃ for 2h, a modified polyurethane oligomer is obtained;

[0011] Step 4: the modified polyurethane oligomer is continuously stirred and cooled to 35-45℃, and an active compound is added, and the system is cooled to room temperature, and a polymerization inhibitor and a free radical initiator are added, and the stirring is continuously carried out for 15-30min, and a modified polyurethane is obtained.

[0012] As a further scheme of the present application: the amount ratio of polytetrahydrofuran diol, toluene-2,4-diisocyanate, dibutyltin dilaurate and 1,2,4-benzene tricarboxylic anhydride is controlled to be 1mol:2-2.4mol:0.06-0.08mol:1-1.2mol.

[0013] As a further scheme of the present application: the amount ratio of cyanuric chloride, 1-hydroxymethyl-5,5-dimethylhydantin and methylsilanetriol is controlled to be 1mol:2-2.5mol:0.5mol.

[0014] As a further scheme of the present application: the amount ratio of the polyurethane oligomer and the intermediate 1 is controlled to be 1mol:2-2.4mol.

[0015] As a further scheme of the present application: the active compound is one of N,N'-bisacryloyl-2,2-ethylenediamine, N,N'-bisacryloyl-1,6-hexanediamine and N,N'-bisacryloylpiperazine.

[0016] As a further scheme of the present application: the polymerization inhibitor is one of tert-butyl pyrocatechol and p-phenol monobutyl ether.

[0017] As a further scheme of the present application: the free radical initiator is di-tert-butyl peroxide and / or di-tert-amyl peroxide.

[0018] The present application has the following beneficial effects:

[0019] The present application uses polytetrahydrofuran dihydric alcohol, toluene-2,4-diisocyanate and 1,2,4-benzene tricarboxylic anhydride as raw materials to synthesize a carboxyl-terminated polyurethane oligomer; uses cyanuric chloride and 1-hydroxymethyl-5,5-dimethylhydantoin as raw materials to prepare a halamine antibacterial agent, then one chlorine atom in the halamine antibacterial agent reacts with two hydroxyl groups in methylsilane triol to obtain an antibacterial agent containing a Si-O bond; the carboxyl-terminated polyurethane oligomer reacts with the hydroxyl group of the intermediate 1 to obtain a modified polyurethane, and the halamine antibacterial agent containing silicon and hydroxyl groups is connected to the polyurethane oligomer, so that the polyurethane can effectively improve the wear resistance and high temperature resistance of the polyurethane due to the Si-O bond, and the halamine antibacterial agent can effectively improve the antibacterial performance of the polyurethane.

[0020] The modified polyurethane described above replaces the polyurethane porous material and the polyurethane protective film of the existing adsorption pad, so that the adsorption pad simultaneously has wear resistance, high temperature resistance and antibacterial performance, and avoids bacterial adhesion to affect the quality of the adsorption pad during processing. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0022] Embodiment 1

[0023] The present application is a preparation method of an adsorption pad for mask processing, which is provided with, from top to bottom, a release paper, double-sided adhesive tape, a PET film, double-sided adhesive tape, a modified polyurethane porous material and a modified polyurethane protective film; wherein the modified polyurethane porous material and the modified polyurethane protective film are both prepared by the modified polyurethane through a mold;

[0024] The adsorption pad is made by the following steps:

[0025] Firstly, the PET film is pasted on the top of the modified polyurethane porous material through the double-sided adhesive tape, and then the release paper is pasted on the top of the PET film through the double-sided adhesive tape to obtain a composite board.

[0026] Secondly, the composite board is placed in a roller type hot press, and the bottom of the composite board is hot pressed at a pressure of 0.3-0.5 MPa; the hot-pressed composite board is heated in a heating device for 10-15 s at a temperature of 100-115 DEG C; the modified polyurethane protective film is heated at the same temperature, and the modified polyurethane protective film is hot pressed to the bottom of the composite board to obtain the adsorption pad.

[0027] The modified polyurethane preparation process comprises the following steps:

[0028] Step 1: Put polytetrahydrofuran diol into a reaction container, stir and heat to 50 DEG C under nitrogen protection, drop toluene-2, 4-diisocyanate, and then add a promoter dibutyltin dilaurate;

[0029] The toluene-2, 4-diisocyanate content in the reaction system is determined every 15 min by selecting di-n-butylamine titration until the toluene-2, 4-diisocyanate content reaches the theoretical value;

[0030] Add 8% (mass fraction) 1, 2, 4-benzene tricarboxylic anhydride N, N-dimethylformamide solution, heat to 100 DEG C, and continuously react for 3 h to obtain a polyurethane oligomer;

[0031] The amount ratio of polytetrahydrofuran diol, toluene-2, 4-diisocyanate, dibutyltin dilaurate and 1, 2, 4-benzene tricarboxylic anhydride is 1 mol:2 mol:0.06 mol:1 mol;

[0032] Step 2: Drop 10% (mass fraction) 1-hydroxymethyl-5, 5-dimethyl hydantoin into 5% (mass fraction) trichloro cyanogen propyl ketone solution, control the system pH to be between 7-8 during the drop process, adjust with 10% (mass fraction) Na2CO3 solution, and continuously react for 2 h after the drop is completed;

[0033] Heat the system to 40 DEG C, add methylsilane triol into the system, control the system pH to be between 7-8, adjust with 10% (mass fraction) Na2CO3 solution, and continuously react for 3 h after the drop is completed; wash with deionized water and dry to obtain intermediate 1;

[0034] The amount ratio of trichloro cyanogen, 1-hydroxymethyl-5, 5-dimethyl hydantoin and methylsilane triol is 1 mol:2 mol:0.5 mol;

[0035] Step 3: Add the polyurethane oligomer into intermediate 1, continuously stir and react for 2 h at 100 DEG C to obtain a modified polyurethane oligomer;

[0036] The amount ratio of the polyurethane oligomer and intermediate 1 is 1 mol:2 mol;

[0037] Step 4: Continue to stir the modified polyurethane oligomer to cool to 35-45 DEG C, add an active compound, cool to room temperature, add a polymerization inhibitor and a free radical initiator, and then continue to stir for 15-30 min to obtain a modified polyurethane;

[0038] The active compound is one of N,N'-bisacryloyl-2,2-ethylenediamine, N,N'-bisacryloyl-1,6-hexanediamine, and N,N'-bisacryloylpiperazine, the polymerization inhibitor is one of tert-butyl catechol and p-phenol monobutyl ether, and the free radical initiator is di-t-butyl peroxide and / or di-t-amyl peroxide.

[0039] Example 2

[0040] The difference from the above-mentioned example 1 is that:

[0041] The modified polyurethane preparation process comprises the following steps:

[0042] Step 1: Put polytetrahydrofuran diol into a reaction container, stir and heat to 50℃ under nitrogen protection, drop toluene-2,4-diisocyanate, and then add a promoter dibutyltin dilaurate;

[0043] Select di-n-butylamine titration method to determine the content of toluene-2,4-diisocyanate in the reaction system every 15 min until the content of toluene-2,4-diisocyanate reaches the theoretical value;

[0044] Add 8% mass fraction of 1,2,4-benzene tricarboxylic anhydride in N,N-dimethylformamide solution, heat to 100℃, and continue to react for 3h to obtain polyurethane oligomer;

[0045] The amount ratio of polytetrahydrofuran diol, toluene-2,4-diisocyanate, dibutyltin dilaurate and 1,2,4-benzene tricarboxylic anhydride is 1 mol:2.2 mol:0.07 mol:1.1 mol;

[0046] Step 2: Drop 10% mass fraction of 1-hydroxymethyl-5,5-dimethylhydantoin into 5% mass fraction of trichloro cyanogen propyl ketone solution, control the pH of the system to be between 7-8 during the dropping process, adjust with 10% mass fraction of Na2CO3 solution, continue to react for 2h after the dropping is completed;

[0047] Heat the system to 40℃, add methylsilanetriol into the system, control the pH of the system to be between 7-8, adjust with 10% mass fraction of Na2CO3 solution, continue to react for 3h after the dropping is completed, wash with deionized water and dry to obtain intermediate 1;

[0048] The amount ratio of trichloro cyanogen, 1-hydroxymethyl-5,5-dimethylhydantoin and methylsilanetriol is 1 mol:2.3 mol:0.5 mol;

[0049] Step 3: The polyurethane oligomer is added to the intermediate 1, and after stirring at 100℃ for 2h, a modified polyurethane oligomer is obtained;

[0050] The amount ratio of the polyurethane oligomer to the intermediate 1 is controlled to be 1 mol:2.2 mol;

[0051] Step 4: The modified polyurethane oligomer is continuously stirred and cooled to 35-45℃, and then an active compound is added. After cooling to room temperature, a polymerization inhibitor and a free radical initiator are added, and the stirring is continued for 15-30 min, to obtain a modified polyurethane;

[0052] The active compound is one of N,N'-bisacryloyl-2,2-ethylenediamine, N,N'-bisacryloyl-1,6-hexanediamine, and N,N'-bisacryloylpiperazine. The polymerization inhibitor is one of tert-butyl pyrocatechol and p-phenol monobutyl ether. The free radical initiator is di-t-butyl peroxide and / or di-t-amyl peroxide.

[0053] Example 3

[0054] The difference from the above example 1 is that:

[0055] The preparation process of the modified polyurethane includes the following steps:

[0056] Step 1: The polytetrahydrofuran diol is placed in a reaction container, and under nitrogen protection, it is stirred and heated to 50℃. Toluene-2,4-diisocyanate is added dropwise, and then a promoter dibutyltin dilaurate is added;

[0057] The di-n-butylamine titration method is selected to determine the content of toluene-2,4-diisocyanate in the reaction system every 15 min until the content of toluene-2,4-diisocyanate reaches the theoretical value;

[0058] An 8% mass fraction of 1,2,4-benzene tricarboxylic anhydride in N,N-dimethylformamide is added, and the temperature is raised to 100℃. The reaction is continued for 3h to obtain a polyurethane oligomer;

[0059] The amount ratio of the polytetrahydrofuran diol, toluene-2,4-diisocyanate, dibutyltin dilaurate, and 1,2,4-benzene tricarboxylic anhydride is controlled to be 1 mol:2.4 mol:0.08 mol:1.2 mol;

[0060] Step 2: A 10% mass fraction of 1-hydroxymethyl-5,5-dimethylhydantoin is added dropwise to a 5% mass fraction of trichloroacetonitrile solution. The pH of the system is controlled to be between 7 and 8 during the dropwise addition process, and a 10% mass fraction of Na2CO3 solution is used for adjustment. After the dropwise addition is completed, the reaction is continued for 2h;

[0061] The system is warmed to 40 DEG C, methylsilanetriol is added into the system, the pH of the system is controlled to be between 7-8, and the pH is adjusted by using a 10% Na2CO3 solution, after the dropwise addition is completed, the reaction is continued for 3h; the intermediate 1 is obtained by washing with deionized water and drying;

[0062] The amount ratio of cyanuric chloride, 1-hydroxymethyl-5,5-dimethylhydantoin and methylsilanetriol is controlled to be 1mol:2.5mol:0.5mol;

[0063] Step 3: the polyurethane oligomer is added into the intermediate 1, after the reaction is continued for 2h under the condition of continuous stirring at 100 DEG C, the modified polyurethane oligomer is obtained;

[0064] The amount ratio of the polyurethane oligomer and the intermediate 1 is controlled to be 1mol:2.4mol;

[0065] Step 4: the modified polyurethane oligomer is continuously stirred and cooled to 35-45 DEG C, the active compound is added, the temperature is cooled to room temperature, the polymerization inhibitor and the free radical initiator are added, and the stirring is continued for 15-30min, and the modified polyurethane is obtained;

[0066] The active compound is one of N,N'-bisacryloyl-2,2-ethylenediamine, N,N'-bisacryloyl-1,6-hexanediamine and N,N'-bisacryloylpiperazine, the polymerization inhibitor is one of tert-butyl o-dihydroxybenzene and p-phenol monobutyl ether, and the free radical initiator is di-tert-butyl peroxide and / or di-tert-amyl peroxide.

[0067] Comparative Example 1

[0068] The adsorbing pad of Comparative Example 1 adopts the adsorbing pad disclosed in Example 1 of patent No. CN113025222A;

[0069] The adsorbing pads of Examples 1-3 and Comparative Examples are subjected to performance tests, and the test results are shown in the following table:

[0070]

[0071]

[0072] It can be known from the above table that the adsorbing pads prepared by Examples 1-3 of the present application have good wear resistance and high temperature resistance compared with the existing adsorbing pads.

[0073] The above describes one embodiment of the present application in detail, but the content described is only the preferred embodiment of the present application, and cannot be considered as limiting the implementation range of the present application. Any equivalent changes and improvements made according to the application scope of the present application should still belong to the patent coverage range of the present application.

Claims

1. A method for preparing an adsorption pad for mask plate processing, comprising: a release paper, a double-sided tape, a PET film, a double-sided tape, a modified polyurethane porous material, and a modified polyurethane protective film, arranged in order from top to bottom; characterized in that: The modified polyurethane porous material and the modified polyurethane protective film are both prepared by using the modified polyurethane through a mold; The modified polyurethane preparation process includes the following steps: Step 1: Place polytetrahydrofuran diol in a reaction vessel, stir and heat to 50°C under nitrogen protection, add toluene-2,4-diisocyanate dropwise, then add accelerator dibutyltin dilaurate to react, and then add 8% by mass fraction of 1,2,4-benzenetricarboxylic anhydride in N,N-dimethylformamide solution to react for 3 hours to obtain a polyurethane oligomer; Step 2: Add 10% by mass of 1-hydroxymethyl-5,5-dimethylhydantoin to 5% by mass of cyanuric chloride acetone solution, controlling the pH of the system to be maintained between 7 and 8, and react for 2 hours; heat the system to 40°C, add methylsilanetriol to the system, controlling the pH of the system to be maintained between 7 and 8, and react for 3 hours to obtain intermediate 1; Step 3: adding the polyurethane oligomer to the intermediate 1, and reacting at 100° C. with continuous stirring for 2 h to obtain a modified polyurethane oligomer; Step 4: Continue stirring the modified polyurethane oligomer and cool it to 35-45°C, add the active compound, cool it to room temperature, add the polymerization inhibitor and free radical initiator, and continue stirring for 15-30 minutes to obtain the modified polyurethane; The active compound is one of N,N'-bisacryloyl-2,2-ethylenediamine, N,N'-bisacryloyl-1,6-hexanediamine and N,N'-bisacryloylpiperazine.

2. The method for preparing an adsorption pad for mask processing according to claim 1, characterized in that: The dosage ratio of polytetrahydrofuran diol, toluene-2,4-diisocyanate, dibutyltin dilaurate and 1,2,4-benzenetricarboxylic anhydride is controlled to be 1 mol: 2-2.4 mol: 0.06-0.08 mol: 1-1.2 mol.

3. The method for preparing an adsorption pad for mask processing according to claim 1, characterized in that: The dosage ratio of cyanuric chloride, 1-hydroxymethyl-5,5-dimethylhydantoin and methylsilanetriol is controlled to be 1 mol:2-2.5 mol:0.5 mol.

4. The method for preparing an adsorption pad for mask processing according to claim 1, characterized in that: The usage ratio of the polyurethane oligomer to the intermediate 1 is controlled to be 1 mol:2-2.4 mol.

5. The method for preparing an adsorption pad for mask processing according to claim 1, characterized in that: The polymerization inhibitor is one of tert-butylcatechol and p-phenol monobutyl ether.

6. The method for preparing an adsorption pad for mask processing according to claim 1, characterized in that: The free radical initiator is di-tert-butyl peroxide and / or di-tert-amyl peroxide.

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