Hydrogen peroxide-based etching solution for liquid crystal panel and preparation method thereof
By using copper corrosion inhibitors and chelating agents with specific components in the copper etching solution for LCD panels, a film structure that blocks the contact of the etching solution is formed, which solves the problem of reduced etching efficiency in the prior art, achieves a balance between high etching rate and corrosion inhibition rate, and improves the yield of high-quality LCD panels.
Patent Information
- Application Number
- CN202510200101.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-24
- Publication Date
- 2026-03-17
- Estimated Expiration
- 2045-02-24
AI Technical Summary
In the process of using existing LCD panel copper etching solutions, although metal corrosion inhibitors are added to improve the corrosion inhibition rate, the synthesized metal film layer will hinder the etching efficiency of the etching solution, resulting in a reduction in etching efficiency.
A hydrogen peroxide-based etching solution composed of hydrogen peroxide, hydrochloric acid, copper corrosion inhibitor, and chelating agent in a specific ratio is used. The copper corrosion inhibitor reacts with allyloxy polyoxyethylene ether in intermediate II of the copper corrosion inhibitor to form a copper corrosion inhibitor with aliphatic chains and multiple active adsorption centers, forming a film structure that blocks the contact of the etching solution. At the same time, the chelating agent has a high degree of compatibility with the etching solution components, ensuring the stability and efficiency of the etching process.
A balance between high etching rate and corrosion inhibition rate is achieved, reducing the generation of defective pits and scratches on the glass surface and improving the yield of high-quality LCD panels.
Smart Images

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Abstract
Description
Technical Field
[0001] This invention belongs to the field of etching solution technology, specifically relating to a hydrogen peroxide aqueous etching solution for liquid crystal panels and its preparation method. Background Technology
[0002] LCD panels are widely used in mobile phones, tablets, automotive displays, and other technological fields. The manufacturing process of LCD panels involves etching, which generates etching waste liquid. Among copper etching solutions, hydrogen peroxide-based copper etching solutions are currently the most widely used. Compared to other copper etching solutions such as ferric chloride systems, hydrogen peroxide-based copper etching solutions have advantages such as not introducing other metal ions into the copper layer surface, producing a more compatible and environmentally friendly product, achieving a high etching rate, and having a longer service life.
[0003] During the etching process, the concentration of the etching solution decreases over time. When the etching rate fails to meet process requirements, the etching solution needs to be replaced, resulting in waste solution. Adding an appropriate amount of slow-release agent to the etching solution helps reduce excessive corrosion of the metal caused by excessively high etching solution concentration in the early stages of etching and the problem of insufficient etching requirements due to reduced concentration in the later stages of etching, thereby avoiding excessive consumption of the etching solution.
[0004] Patent application CN104611702A discloses an etching solution for copper-molybdenum films in liquid crystal panels. This etching solution includes hydrogen peroxide, ammonia, a pH adjuster, a chelating agent, a metal corrosion inhibitor, and water. The metal inhibitor is specifically an organic hypophosphite. The organic hypophosphite decomposes to form an organic phosphate, which can deposit with the etched metal ions on the metal surface, especially in water, to form a film, thus acting as a cathodic corrosion inhibitor. However, the high binding efficiency of the organic phosphate with copper ions reduces the etching efficiency of the solution after deposition. Therefore, how to maintain a high etching rate while also achieving excellent corrosion inhibition is a pressing technical problem.
[0005] To address this technical deficiency, a solution is proposed. Summary of the Invention
[0006] The purpose of this invention is to provide a method for preparing a hydrogen peroxide-based etching solution for liquid crystal panels, which solves the technical problem in the prior art where a certain amount of metal slow-release agent is added to the etching solution to improve its etching rate and deposit a film; however, the synthesized metal film layer will hinder the etching efficiency of the etching solution.
[0007] The objective of this invention can be achieved through the following technical solutions:
[0008] A hydrogen peroxide-based etching solution for liquid crystal panels, comprising, by weight, 30-35 parts hydrogen peroxide solution, 25-35 parts hydrochloric acid solution, 5-10 parts copper corrosion inhibitor and 3-5 parts chelating agent.
[0009] The copper corrosion inhibitor is obtained by reacting intermediate II with allyloxy polyoxyethylene ether. Intermediate II is obtained by reacting intermediate I with 3-aminomethylthiophene. Intermediate I is obtained by reacting 5-chloro-2-methylbenzoic acid with propargylamine.
[0010] Furthermore, the preparation method of the copper corrosion inhibitor includes the following steps:
[0011] A1. p-Toluenesulfonic acid hydrate is heated at 100-105℃ until completely dissolved to obtain a catalyst liquid; the catalyst liquid, ethanol, 5-chloro-2-methylbenzoic acid and propargylamine are mixed to obtain a mixture; the mixture is heated at 60-70℃ for 40-48h, and after post-processing, intermediate product I is obtained.
[0012] Using p-toluenesulfonic acid hydrate as a catalyst and ethanol as a solvent, 5-chloro-2-methylbenzoic acid and propargylamine undergo a nucleophilic substitution reaction to give intermediate I. The structural formula of the reaction is as follows:
[0013]
[0014] A2. The catalyst liquid, ethanol, intermediate product I and 3-aminomethylthiophene are mixed to obtain the reactant; the reactant is refluxed at 20-40℃ for 24h to obtain the product; the product is then processed to obtain intermediate II.
[0015] The intermediate product undergoes an addition reaction with 3-aminomethylthiophene to give intermediate II.
[0016]
[0017] A3. Add ammonium persulfate to intermediate II, then heat to 60-80℃, and then add allyloxy polyoxyethylene ether to intermediate II in 2-5 portions. After the addition is complete, heat to 100-120℃ and keep the reaction at this temperature for 5-6 hours to obtain copper corrosion inhibitor.
[0018] Intermediate II contains carbon-carbon unsaturated double bonds. After the addition of an initiator, an addition polymerization reaction of the unsaturated double bonds occurs, thus preparing a copper corrosion inhibitor.
[0019] Further, in step A, the ratio of catalyst liquid, ethanol, 5-chloro-2-methylbenzoic acid, and propargylamine is 3-4.5g:250mL:1.7-3.42g:0.53-1.06g; in step A1, the post-processing steps include: allowing the mixture to stand and cool to room temperature, then filtering to obtain the reactants; adding NaOH solution dropwise to the reactants to adjust the pH of the reactants to neutral; then washing the reactants with saturated NaCl solution and drying with anhydrous sodium sulfate to obtain intermediate product I.
[0020] Further, in step A2, the ratio of catalyst liquid, ethanol, intermediate product and 3-aminomethylthiophene is 5-0g:300mL:2.06-4.2g:1.13-2.26g; in step A2, the post-processing steps include: allowing the product to stand and cool to room temperature, filtering, to obtain the product; the product is washed with deionized water and dried with anhydrous sodium sulfate to obtain intermediate II.
[0021] Furthermore, in step A3, the weight ratio of intermediate II, ammonium persulfate, and allyloxy polyoxyethylene ether is 50-60:2-3:20-30.
[0022] Furthermore, the preparation method of the chelating agent includes the following steps:
[0023] B1, ethyl acetate, benzoyl chloride and potassium thiocyanate were mixed to obtain the reactants;
[0024] B2. The reactants are reacted at 60-70℃ for 2-3 hours, then filtered to remove the generated potassium chloride; the filtrate is cooled until crystals precipitate, then filtered and recrystallized to obtain the solid product chelating agent.
[0025] Benzoyl chloride has high reactivity and can undergo a nucleophilic substitution reaction with potassium thiocyanate to obtain the chelating agent prepared in this invention.
[0026] Furthermore, in step B1, the ratio of ethyl acetate, benzoyl chloride, and potassium thiocyanate is 50 mL: 7-3.4 g: 0.09-0.8 g.
[0027] As another aspect of the present invention, a method for preparing a hydrogen peroxide-based etching solution for liquid crystal panels includes the following steps: adding 35-40%wt of hydrogen peroxide solution, 37-40%wt of hydrochloric acid solution, copper corrosion inhibitor and chelating agent to a high-density polyethylene tank, stirring at room temperature for 30-60 min, and then letting stand for 30 min to obtain a hydrogen peroxide-based etching solution for liquid crystal panels.
[0028] The present invention has the following beneficial effects:
[0029] 1. The etching solution used in this invention is a hydrogen peroxide-based etching solution (comprising a certain mass concentration of hydrogen peroxide and a certain mass concentration of hydrochloric acid solution). A certain amount of auxiliary agents, chelating agents, and copper corrosion inhibitors are added to the etching solution to improve its stability and etching efficiency. 5-Chloro-2-methylbenzoic acid and propargylamine react to obtain intermediate I; intermediate I further undergoes a nucleophilic substitution reaction with 3-aminomethylthiophene to obtain intermediate II; the unsaturated double bonds in intermediate II are used to graft allyloxy polyoxyethylene ether, thereby obtaining a copper corrosion inhibitor with aliphatic chains and multiple active adsorption centers. Amino groups and unsaturated double bonds connect the various components of the copper corrosion inhibitor, resulting in a molecular chain that combines rigidity and flexibility. The aforementioned copper corrosion inhibitor can combine with copper atoms on the surface to form a film structure that blocks contact with the etching solution. This film structure does not react with the etching solution, thus forming a localized protection to prevent further etching. In addition, the prepared copper etching solution can ensure a large contact area when adsorbed onto the carbon steel surface, and its flexibility allows for a greater engagement angle with the imperfectly smooth surface of the liquid crystal panel, resulting in a high etching rate and slow release rate for the liquid crystal panel.
[0030] 2. A small amount of chelating agent is added to the hydrogen peroxide-based etching solution used in this invention. Potassium thiocyanate itself has a certain chelating effect; by grafting potassium thiocyanate with benzoyl chloride, the compatibility between the prepared chelating agent and the components in the hydrogen peroxide-based etching solution is improved. The components in the etching solution prepared by this invention work synergistically, making the entire etching process stable, effective, and controllable. Furthermore, it effectively inhibits the formation of undesirable pits, bumps, and scratches on the glass surface during the etching process, thereby significantly improving the yield of superior products. Detailed Implementation
[0031] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0032] The allyloxy polyoxyethylene ether used in Examples 1-3 of this invention was purchased from Maclean Reagents, CAS No. 27274-3-3, catalog No. A874998-25g, with a molecular weight of 2400.
[0033] Example 1
[0034] This embodiment provides a method for preparing a copper corrosion inhibitor for a hydrogen peroxide-based etching solution used in liquid crystal panels, comprising the following steps:
[0035] A1. Add 3g of p-toluenesulfonic acid hydrate to a sealed tube and heat at 100℃ until completely dissolved to obtain a catalyst liquid. Add 3g of the catalyst liquid to a 500mL three-necked flask, then add 250mL of ethanol, 1.7g of 5-chloro-2-methylbenzoic acid, and 0.53g of propargylamine to the three-necked flask, mix well, and obtain a mixture.
[0036] A2. The three-necked flask was transferred to a water bath and heated at 60°C for 40 hours. The flask was then allowed to cool to room temperature and filtered to obtain the reactants. 0.1 mol / L NaOH solution was added dropwise to the reactants to adjust the pH to neutral. The reactants were then washed with saturated NaCl solution and dried with anhydrous sodium sulfate to obtain intermediate product I.
[0037] A3. Add 5g of catalyst liquid and 300mL of ethanol to a sealed tube, then add 2.06g of intermediate product I and 1.13g of 3-aminomethylthiophene to obtain the reactants. React the reactants at 20℃ for 24h to obtain the product. Allow the product to stand and cool to room temperature, then filter to obtain the product; wash the product with deionized water and dry it with anhydrous sodium sulfate to obtain a solid, which is the prepared intermediate II.
[0038] A4. Select a 500mL enamel-lined reactor equipped with a stirrer, thermometer, condenser, and water separator. Add 50 parts by weight of intermediate II and 2 parts by weight of ammonium persulfate to the reactor, and then heat the reactor to 60℃ with stirring. Then add 20 parts by weight of allyloxy polyoxyethylene ether to the enamel-lined reactor in two portions, with an interval of 8 minutes between each addition. After the addition is complete, heat the reactor to 100℃ and keep it at this temperature for 5 hours to obtain the product, which is the prepared copper corrosion inhibitor.
[0039] Example 2
[0040] This embodiment provides a method for preparing a copper corrosion inhibitor for a hydrogen peroxide-based etching solution used in liquid crystal panels, comprising the following steps:
[0041] A1. Add 3.5g of p-toluenesulfonic acid hydrate to a sealed tube and heat at 102℃ until completely dissolved to obtain a catalyst liquid. Add 3.5g of the catalyst liquid to a 500mL three-necked flask, then add 250mL of ethanol, 2.56g of 5-chloro-2-methylbenzoic acid, and 0.80g of propargylamine to the three-necked flask, mix well, and obtain a mixture.
[0042] A2. The three-necked flask was transferred to a water bath and refluxed at 65°C for 44 hours. The flask was then allowed to cool to room temperature and filtered to obtain the reactants. 0.1 mol / L NaOH solution was added dropwise to the reactants to adjust the pH to neutral. The reactants were then washed with saturated NaCl solution and dried with anhydrous sodium sulfate to obtain intermediate product I.
[0043] A3. 8 g of catalyst liquid and 300 mL of ethanol were added to a sealed tube, followed by 3.09 g of intermediate product I and 1.70 g of 3-aminomethylthiophene, yielding the reactants. The reactants were refluxed at 50 °C for 24 h to obtain the product. The product was allowed to stand and cool to room temperature, then filtered to obtain the product. The product was washed successively with deionized water and dried over anhydrous sodium sulfate to obtain a solid, which is the prepared intermediate II.
[0044] A4. Select a 500mL enamel-lined reactor equipped with a stirrer, thermometer, condenser, and water separator. Add 55 parts by weight of intermediate II and 2.3 parts by weight of ammonium persulfate to the reactor, and then heat the reactor to 70°C with stirring. Add 25 parts by weight of allyloxy polyoxyethylene ether to the enamel-lined reactor in three portions, with an interval of 5 minutes between each addition. After the addition is complete, heat the reactor to 110°C and maintain the temperature at this temperature for 5.5 hours to obtain the product, which is the prepared copper corrosion inhibitor.
[0045] Example 3
[0046] This embodiment provides a method for preparing a copper corrosion inhibitor for a hydrogen peroxide-based etching solution used in liquid crystal panels, comprising the following steps:
[0047] A1. Add 4.5 g of p-toluenesulfonic acid hydrate to a sealed tube and heat at 105 °C until completely dissolved to obtain a catalyst liquid. Add 4.5 g of the catalyst liquid to a 500 mL three-necked flask, then add 250 mL of ethanol, 3.42 g of 5-chloro-2-methylbenzoic acid, and 1.06 g of propargylamine to the three-necked flask, mix well, and obtain a mixture.
[0048] A2. The three-necked flask was transferred to a water bath and heated at 70°C for 48 hours. The flask was then allowed to cool to room temperature and filtered to obtain the reactants. 0.1 mol / L NaOH solution was added dropwise to the reactants to adjust the pH to neutral. The mixture was then washed with saturated NaCl solution and dried over anhydrous sodium sulfate to obtain intermediate product I.
[0049] A3. 10 g of catalyst liquid and 300 mL of ethanol were added to a sealed tube, followed by 4.2 g of intermediate product I and 2.26 g of 3-aminomethylthiophene, yielding the reactants. The reactants were reacted at 40 °C for 24 h to obtain the product. The product was allowed to stand and cool to room temperature, then filtered to obtain the product. The product was washed successively with deionized water and dried over anhydrous sodium sulfate to obtain a solid, which is the prepared intermediate II.
[0050] A4. Select a 500mL enamel-lined reactor equipped with a stirrer, thermometer, condenser, and water separator. Add 60 parts by weight of intermediate II and 3 parts by weight of ammonium persulfate to the reactor, and then heat the reactor to 80℃ with stirring. Then add 30 parts by weight of allyloxy polyoxyethylene ether to the enamel-lined reactor in 5 portions, with an interval of 10 minutes between each addition. After the addition is complete, heat the reactor to 120℃ and keep it at this temperature for 6 hours to obtain the product, which is the prepared copper corrosion inhibitor.
[0051] Example 4
[0052] This embodiment provides a method for preparing a chelating agent for a hydrogen peroxide-based etching solution for liquid crystal panels, comprising the following steps:
[0053] B1. Select a 100mL four-necked reaction flask equipped with a stirrer and a reflux condenser. Add 50mL of ethyl acetate and 1.4g of benzoyl chloride to the four-necked reaction flask, and then add 0.97g of potassium thiocyanate to obtain the reactants.
[0054] B2. The reactants were reacted at 60°C for 2 hours, then filtered to remove the generated potassium chloride, yielding a filtrate. The filtrate was cooled until crystals precipitated, then filtered again and recrystallized to obtain the solid product, a chelating agent.
[0055] Example 5
[0056] This embodiment provides a method for preparing a chelating agent for a hydrogen peroxide-based etching solution for liquid crystal panels, comprising the following steps:
[0057] B1. Select a 100mL four-necked reaction flask equipped with a stirrer and a reflux condenser. Add 50mL of ethyl acetate and 2.1g of benzoyl chloride to the four-necked reaction flask, and then add 1.45g of potassium thiocyanate to obtain the reactants.
[0058] B2. The reactants were reacted at 65°C for 2.2 hours, then filtered to remove the generated potassium chloride, yielding a filtrate. The filtrate was cooled until crystals precipitated, then filtered and recrystallized to obtain the solid product, a chelating agent.
[0059] Example 6
[0060] This embodiment provides a method for preparing a chelating agent for a hydrogen peroxide-based etching solution for liquid crystal panels, comprising the following steps:
[0061] B1. Select a 100mL four-necked reaction flask equipped with a stirrer and a reflux condenser. Add 50mL of ethyl acetate and 2.8g of benzoyl chloride to the four-necked reaction flask, and then add 1.96g of potassium thiocyanate to obtain the reactants.
[0062] B2. The reactants were reacted at 70°C for 3 hours, then filtered to remove the generated potassium chloride, yielding a filtrate. The filtrate was cooled until crystals precipitated, then filtered and recrystallized to obtain the solid product, a chelating agent.
[0063] Example 7
[0064] This embodiment provides a method for preparing a hydrogen peroxide-based etching solution for liquid crystal panels, including the following steps:
[0065] According to the weight percentage, 35 parts of 35%wt hydrogen peroxide solution, 35 parts of 37%wt hydrochloric acid solution, 5 parts of copper corrosion inhibitor prepared in Example 1 and 3 parts of chelating agent prepared in Example 4 were added to a high-density polyethylene bucket, stirred at 100 r / min for 30 min at room temperature, and then allowed to stand for 30 min to obtain copper etching solution.
[0066] Example 8
[0067] This embodiment provides a method for preparing a hydrogen peroxide-based etching solution for liquid crystal panels, including the following steps:
[0068] According to the weight percentage, 32 parts of 38%wt hydrogen peroxide solution, 30 parts of 38%wt hydrochloric acid solution, 8 parts of copper corrosion inhibitor prepared in Example 2 and 4 parts of chelating agent prepared in Example 5 were added to a high-density polyethylene bucket, stirred at 100 r / min for 50 min at room temperature, and then allowed to stand for 30 min to obtain copper etching solution.
[0069] Example 9
[0070] This embodiment provides a method for preparing a hydrogen peroxide-based etching solution for liquid crystal panels, including the following steps:
[0071] According to the weight percentage, 30 parts of 40%wt hydrogen peroxide solution, 25 parts of 40%wt hydrochloric acid solution, 10 parts of copper corrosion inhibitor prepared in Example 3 and 5 parts of chelating agent prepared in Example 6 were added to a high-density polyethylene bucket, stirred at 100 r / min for 60 min at room temperature, and then allowed to stand for 30 min to obtain copper etching solution.
[0072] Comparative Example 1
[0073] The difference between this comparative example and Example 9 is that step A4 is omitted in the preparation of the copper corrosion inhibitor, and intermediate II is used as the copper corrosion inhibitor.
[0074] Comparative Example 2
[0075] The difference between this comparative example and Example 9 is that, in the preparation of the copper corrosion inhibitor, step A3 is omitted, and intermediate product I is used as an equal mass substitute for intermediate II and allyloxy polyoxyethylene ether as the copper corrosion inhibitor.
[0076] Comparative Example 3
[0077] The difference between this comparative example and Example 9 is that potassium thiocyanate of the same molecular weight was used instead of the chelating agent.
[0078] Performance testing:
[0079] 1. Corrosion test of metallic copper
[0080] The amount of copper leached was determined using a metal corrosion leaching method. Copper was immersed in the hydrogen peroxide-based etching solutions for liquid crystal panels prepared in Examples 7-9 and Comparative Examples 1-3 for 10 minutes each. The copper content in the etching solutions was then determined using a spectrophotometer to verify the corrosion performance of the prepared etching solutions on copper.
[0081] 2. Sustained-release rate test
[0082] Hydrogen peroxide-based etching solution for liquid crystal panels was added to a round-mouthed bottle. Metallic copper was immersed in the hydrogen peroxide-based etching solution for liquid crystal panels prepared in Examples 7-9 and Comparative Examples 1-3, respectively. The round-mouthed bottle was then sealed with a polytetrafluoroethylene cap, and its slow-release rate η was then measured.
[0083] η=(Ⅰcorr-Ⅰ'corr) / Ⅰcorr
[0084] Wherein, Icorr is the corrosion current density of the metal in a solution without corrosion inhibitor; I'corr is the corrosion current density after adding the hydrogen peroxide aqueous etching solution for liquid crystal panels prepared in Examples 7-9. Specific test results are shown in Table 1:
[0085] Table 1. Test data for each test specimen
[0086]
[0087] As shown in Table 1, the hydrogen peroxide-based etching solutions for liquid crystal panels prepared in Examples 7-9 of this invention have high etching rates, as evidenced by the high amount of copper ions dissolved in the etching solutions during leaching of metallic copper in Examples 7-9. However, in Comparative Example 3, potassium thiocyanate of the same molecular weight was used instead of the chelating agent. Because the chelating agent has higher compatibility with other components of the etching solution, the chelation efficiency of the etching solution is higher. Therefore, compared to Examples 7-9, the etching efficiency of the etching solution prepared in Comparative Example 3 is lower, and the amount of copper ions dissolved is also lower.
[0088] In Comparative Example 1, intermediate II was used as the copper corrosion inhibitor. Compared to copper corrosion inhibitors with long chains, it did not form a film layer that blocked the contact of the etching solution, and its interlocking with the rough areas of the liquid crystal panel deteriorated, thus reducing the corrosion inhibition rate of the prepared etching solution. In Comparative Example 2, intermediate product I and allyloxy polyoxyethylene ether were blended as copper corrosion inhibitors during the preparation of the copper corrosion inhibitor. On the one hand, intermediate product I and allyloxy polyoxyethylene ether did not react, failing to form an organic monolithic copper corrosion inhibitor; on the other hand, compared to intermediate II formed by further reaction, intermediate product I had fewer adsorption active centers for copper ions. This resulted in a decrease in the corrosion inhibition rate.
[0089] The above description is merely an example and illustration of the structure of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the structure of the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.
[0090] In the description of this specification, the references to terms such as "an embodiment," "example," and "specific example" indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. The preferred embodiments of the present invention disclosed above are merely for the purpose of illustrating the invention. The preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Obviously, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims
1. A hydrogen peroxide-based etching solution for a liquid crystal panel, characterized by comprising: According to parts by weight, including 30-35 parts of hydrogen peroxide solution, 25-35 parts of hydrochloric acid solution, 5-10 parts of copper corrosion inhibitor and 3-5 parts of chelating agent; The preparation method of the copper corrosion inhibitor comprises the following steps: A1, p-toluenesulfonic acid hydrate is heated at 100-105 DEG C until completely dissolved to obtain a catalyst liquid; the catalyst liquid, ethanol, 5-chloro-2-methylbenzoic acid and propargylamine are uniformly mixed to obtain a mixture; the mixture is heated at 60-70 DEG C for 40-48 h, and after post-process treatment, an intermediate product I is obtained; A2, the catalyst liquid, ethanol, the intermediate product I and 3-aminomethyl thiophene are mixed to obtain a reactant; the reactant is reacted at 20-40 DEG C for 24 h to obtain a product; the product is treated by post-process to obtain an intermediate II; A3, ammonium persulfate is added to the intermediate II, and then heated to 60-80 DEG C; allyloxy polyoxyethylene ether is added to the intermediate II in 2-5 portions; after the addition is completed, the temperature is raised to 100-120 DEG C; and the reaction is maintained at this temperature for 5-6 h to obtain the copper corrosion inhibitor; The preparation method of the chelating agent comprises the following steps: B1, ethyl acetate, benzoyl chloride and potassium thiocyanate are blended to obtain a reactant; B2, the reactant is reacted at 60-70 DEG C for 2-3 h, and then filtered to remove the generated potassium chloride; the filtrate is cooled until crystals are precipitated; and after suction filtration and recrystallization, a solid product, the chelating agent, is obtained.
2. The hydrogen peroxide-based etching solution for a liquid crystal panel according to claim 1, characterized by comprising: In step A1, the amount ratio of the catalyst liquid, ethanol, 5-chloro-2-methylbenzoic acid and propargylamine is 3-4.5 g:250 mL:1.7-3.42 g:0.53-1.06 g; in step A1, the post-process treatment step comprises: standing and cooling to room temperature, and then filtering to obtain a reactant; NaOH solution is added dropwise to the reactant to adjust the pH value of the reactant to neutral; and then the reactant is washed with saturated NaCl solution and dried with anhydrous sodium sulfate to obtain the intermediate product I.
3. The hydrogen peroxide-based etching solution for a liquid crystal panel according to claim 1, characterized by comprising: In step A2, the amount ratio of the catalyst liquid, ethanol, the intermediate product I and 3-aminomethyl thiophene is 5-10 g:300 mL:2.06-4.2 g:1.13-2.26 g; in step A2, the post-process treatment step comprises: standing and cooling the product to room temperature, and then filtering to obtain a product; and the product is sequentially washed with deionized water and dried with anhydrous sodium sulfate to obtain the intermediate II.
4. The hydrogen peroxide-based etching solution for a liquid crystal panel according to claim 1, characterized by comprising: In step A3, the weight ratio of the intermediate II, ammonium persulfate and allyloxy polyoxyethylene ether is 50-60:2-3:20-30.
5. The hydrogen peroxide-based etching solution for a liquid crystal panel according to claim 1, characterized by comprising: In step B1, the amount ratio of ethyl acetate, benzoyl chloride and potassium thiocyanate is 50 mL:1.4-2.8 g:0.97-1.96 g.
6. A method for preparing the hydrogen peroxide-based etching solution for a liquid crystal panel according to any one of claims 1 to 5, characterized by, The following steps are included: 35-40%wt of hydrogen peroxide solution, 37-40%wt of hydrochloric acid solution, the copper corrosion inhibitor and the chelating agent are added into a high-density polyethylene barrel, stirred at room temperature for 30-60 min, and then stood for 30 min to obtain a liquid crystal panel hydrogen peroxide etching solution.
Citation Information
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