A composite material for regenerating photoresist stripping waste liquid and a preparation method thereof
By using modified activated carbon and POSS-based reinforced components in the photoresist stripping waste liquid regeneration process, the problems of cumbersome and high cost in the prior art are solved, and efficient oil-water separation and impurity removal are achieved.
Patent Information
- Application Number
- CN202311114826.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-31
- Publication Date
- 2025-08-01
- Estimated Expiration
- 2043-08-31
AI Technical Summary
The regeneration steps of existing photoresist stripping waste liquid are cumbersome and expensive.
The fabric is impregnated with a mixed liquid composed of modified activated carbon and POSS-based reinforcement components, tetrahydrofuran, polydimethylsilane and curing agent, to form a superhydrophobic film, which is used for photoresist stripping waste liquid regeneration, and achieve oil-water separation and adsorption of impurities.
The photoresist stripping waste liquid regeneration process is simplified, energy consumption and treatment costs are reduced, and moisture, gel sludge and metal ion impurities are effectively removed.
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of stripping waste liquid treatment, and particularly relates to a composite material for regenerating photoresist stripping waste liquid and a preparation method thereof. Background Art
[0002] Wet electronic chemicals are one of the indispensable basic chemical materials in the production processes of liquid crystal panels, semiconductor chips, etc. According to different composition components and application processes, process chemicals can be divided into general wet electronic chemicals and functional wet electronic chemicals.
[0003] Among them, functional wet electronic chemicals refer to formulated or compounded chemicals that achieve special functions and meet the special process requirements in manufacturing through compounding means, mainly including stripping liquids, etching liquids, etc.
[0004] Currently, positive photoresists are mainly used in the liquid crystal panel and semiconductor industries, and the corresponding photoresist stripping liquids are mainly alkaline stripping liquids. Alkaline stripping liquids can be roughly divided into solvent-based and water-based stripping liquids, among which solvent stripping liquids are more widely used.
[0005] The main components of solvent-based photoresist stripping liquids are organic amine compounds, high-boiling organic solvents such as alcohol ethers, corrosion inhibitors, and additives, etc. Such stripping liquids can effectively strip photoresists, and basically have no corrosion on the substrate and metal wiring. At the same time, they have the advantages of low toxicity and easy refining and regeneration.
[0006] In recent years, panel manufacturers such as BOE, Visionox, and CSOT have, in order to improve the competitiveness of the prices of liquid crystal panels and further reduce the costs of various production links of the panels, required their stripping liquid suppliers to recycle and mix-process the used waste photoresist stripping liquid, and then reuse it. It is expected that the price of the recycled glass liquid will be 20% lower than that of the new glass liquid, and it is basically the same as the new liquid in terms of performance.
[0007] As disclosed in Chinese Patent CN108840495A, a method for purifying stripping waste liquid is provided. The stripping waste liquid is filtered and separated by a hollow fiber membrane filter to obtain a primary filtrate without particulate impurities and photoresist, and a concentrated liquid containing particulate impurities and photoresist. The primary filtrate is preheated by a preheater. The preheated primary filtrate is subjected to water separation treatment by a dehydration tower, and the separated water vapor is discharged from the top of the tower and condensed to form high-purity water. The pumped dehydration filtrate is subjected to adsorption treatment by an adsorption tower. The adsorption filtrate is heated and evaporated by an evaporator to form a material vapor. The material vapor is refined by a rectification tower to obtain the purified stripping liquid. Although this patent first uses a hollow fiber membrane filter to filter and separate the glass waste liquid, effectively removing the colloidal sludge, i.e., the particulate impurities, it forms a high-concentration concentrated waste liquid that requires secondary treatment, and subsequent steps such as water separation by a dehydration tower are needed, which has the defects of cumbersome process and high treatment cost. Summary of the Invention
[0008] The purpose of the present invention is to provide a composite material for regenerating photoresist stripping waste liquid and a preparation method thereof, so as to solve the problems of cumbersome steps and high cost in the existing regeneration treatment of photoresist stripping waste liquid.
[0009] The purpose of the present invention can be achieved by the following technical solutions:
[0010] A preparation method of a composite material for regenerating photoresist stripping waste liquid includes the following steps:
[0011] Put the modified activated carbon and POSS-based reinforcing component into tetrahydrofuran, stir, then add polydimethylsilane and a curing agent, and perform ultrasonic treatment for 30 min to obtain a mixed solution. Immerse the fabric in the mixed solution, perform ultrasonic treatment for 30 - 60 min, take it out, and cure it in an oven at 50 - 70 °C for 1 - 2 h to obtain the composite material for regenerating photoresist stripping waste liquid.
[0012] Further, the dosage ratio of the modified activated carbon, POSS-based reinforcing component, tetrahydrofuran, polydimethylsilane, and curing agent in the mixed solution is 0.5 g: 2 g: 20 - 40 mL: 8 mL: 0.76 - 0.8 g, and the curing agent is Sylgard 184 silicone rubber curing agent.
[0013] Further, the fabric is a pure cotton plain woven fabric, the warp and weft yarn linear densities are 17 and 18 tex respectively, the warp and weft densities are 536 and 230 per (10 cm) respectively, and the areal density is 120 g / m 2 .
[0014] Further, the modified activated carbon is prepared through the following steps:
[0015] Step A1: Ultrasonically mix activated carbon, absolute ethanol, and deionized water evenly to obtain suspension a. Stir absolute ethanol, ammonia water, tetraethyl orthosilicate, and deionized water at room temperature for 15 min to obtain mixture b. Add suspension a to mixture b, stir at room temperature for 4 h, then let it stand for 24 h. After that, dry it in an oven at 80 °C, and grind to obtain hybrid particles;
[0016] Step A2: Stir and mix the hybrid particles, absolute ethanol, and octadecylamine for 1 - 2 h. Then add the hydrolyzate of dodecyltrimethoxysilane and react at 50 - 60 °C for 2 - 4 h. Filter, wash the filter cake, and dry it to obtain modified activated carbon.
[0017] First, using activated carbon as the carrier and tetraethyl orthosilicate as the silicon source, activated carbon - supported silica hybrid particles were prepared by the solution - sol method. Then, through the hydrogen - bond interaction between the surface hydroxyl groups of the hybrid particles and octadecylamine, octadecylamine was introduced onto the surface of the hybrid particles to improve the hydrophobicity of the hybrid particles and introduce active amino groups. After that, the hydrophobicity of the hybrid particles was further improved by the coupling modification with dodecyltrimethoxysilane.
[0018] Furthermore, in step A1, the volume ratio of suspension a to mixture b is 1:4. Suspension a is composed of activated carbon, absolute ethanol, and deionized water according to the dosage ratio of 0.1 g:3 mL:2 mL. Mixture b is composed of absolute ethanol, ammonia water, tetraethyl orthosilicate, and deionized water according to the volume ratio of 10:1.5:10:10. The mass fraction of ammonia water is 28%, and the average particle size of the activated carbon is 200 mesh.
[0019] Furthermore, in step A2, the dosage ratio of the hybrid particles, absolute ethanol, octadecylamine, and the hydrolyzate of dodecyltrimethoxysilane is 10 g:100 mL:2.5 - 3.4 g:20 - 40 mL. The hydrolyzate of dodecyltrimethoxysilane is composed of dodecyltrimethoxysilane, absolute ethanol, and deionized water according to the dosage ratio of 1.5 - 2.4 g:30 - 35 mL:5 - 10 mL.
[0020] Furthermore, the POSS - based reinforcing component is prepared through the following steps:
[0021] Step B1: Add octa - amino POSS, 3,4 - dihydroxybenzaldehyde, and THF into a reaction kettle, stir, and then add glacial acetic acid. Under an argon atmosphere, heat and reflux for 72 h. Then remove THF and glacial acetic acid by vacuum distillation to obtain the POSS - based Schiff base compound;
[0022] Step B2: Add the POSS-based Schiff base compound, potassium hydroxide, and absolute ethanol into a reaction kettle. After stirring, add epichlorohydrin. Under a nitrogen atmosphere, react at 70 °C for 4 h and then cool to room temperature. Dropwise add an aqueous solution of 40 wt% potassium hydroxide. After the dropwise addition is completed, raise the temperature to 60 °C and stir and react for 6 h. Then cool to room temperature, filter to remove the inorganic salts in the reaction system, and rotary evaporate the obtained filtrate to obtain the POSS-based reinforcing component.
[0023] Using octaamino POSS and 3,4-dihydroxybenzaldehyde as substrates, through the condensation reaction between amino groups and aldehyde groups, a POSS-based Schiff base compound with a cage-like polyhedral oligomeric silsesquioxane structure, Schiff base groups, and phenolic hydroxyl groups is obtained. Then, the POSS-based Schiff base compound reacts with epichlorohydrin to undergo an HCl elimination reaction to obtain the POSS-based reinforcing component.
[0024] Further, in step B1, the dosage ratio of octaamino POSS, 3,4-dihydroxybenzaldehyde, THF, and glacial acetic acid is 0.01 mol: 0.08 mol: 350 - 500 mL: 2 - 3 mL. Octaamino POSS is octaamino cage-like polyhedral oligomeric silsesquioxane, purchased from Hybrid Plastics Company in the United States, and its product number is AM0285.
[0025] Further, in step B2, the dosage ratio of the POSS-based Schiff base compound, potassium hydroxide, absolute ethanol, epichlorohydrin, and the aqueous potassium hydroxide solution is 4.8 - 5.2 g: 0.5 g: 100 - 150 mL: 9.2 - 10.4 g: 8.4 g.
[0026] Further, a composite material for regenerating photoresist stripping waste liquid is prepared by the above preparation method.
[0027] Advantages of the present invention:
[0028] 1. The present invention provides a composite material for regenerating photoresist stripping waste liquid and a preparation method thereof. It is obtained by impregnating and drying a fabric in a mixed solution composed of modified activated carbon, POSS-based reinforcing component, tetrahydrofuran, polydimethylsilane, and a curing agent. The modified activated carbon, POSS-based reinforcing component, and polydimethylsilane crosslink and react to form a superhydrophobic film on the fabric surface, endowing the composite material with excellent superhydrophobic and high adsorption characteristics. Installing it on a separation device and applying it in the process of regenerating photoresist stripping waste liquid, firstly, it realizes oil-water separation, reduces the water content in the photoresist stripping waste liquid, eliminates the water separation and other links in the traditional process, saves energy, and reduces costs. Secondly, it uses the characteristic of a relatively low pore structure of its own to filter and remove macromolecular impurities such as colloidal sludge in the photoresist stripping waste liquid. Thirdly, it uses the activated carbon, cage-like polyhedral oligomeric silsesquioxane structure, Schiff base structure, etc. in the matrix to adsorb metal ions and reduce the metal ion impurities in the photoresist stripping waste liquid.
[0029] 2. The present invention introduces modified activated carbon into the composite material. Actually, it is activated carbon modified by octadecylamine and dodecyltrimethoxysilane loaded with silica particles, belonging to organic-inorganic particulate composite particles. The surface contains many alkyl long chains, having good hydrophobic characteristics, and contains active amino groups, which can crosslink with the epoxy groups of the POSS-based reinforcing group to form a rough surface with a micron structure on the fabric surface. Combining with the low surface energy characteristics of polydimethylsilane, a superhydrophobic effect is formed on the fabric surface. Combining with the high adsorption characteristics of activated carbon itself, the composite material is given good adsorption performance.
[0030] 3. The present invention introduces a POSS-based reinforcing component into the composite material. Its intramolecular porous pore structure and a large number of cage-shaped Si-O-Si structures can interact with organic pollutants and inorganic heavy metal ions, thereby realizing the adsorption of organic pollutants and inorganic heavy metal ions. And it contains a Schiff base structure, and the Schiff base structure has a good coordination effect on metal ions, which can further enhance the removal of metal ions in the photoresist stripping waste liquid by the composite material. Detailed implementation manners
[0031] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.
[0032] Example 1
[0033] A kind of modified activated carbon is made through the following steps:
[0034] Step A1: Ultrasonically mix 0.1 kg of activated carbon (average particle size 200 mesh), 3 L of absolute ethanol and 2 L of deionized water evenly to obtain suspension a. Stir 10 L of absolute ethanol, 1.5 L of ammonia water (28 wt%), 10 L of tetraethyl orthosilicate and 10 L of deionized water at room temperature for 15 min to obtain mixture b. According to the volume ratio of suspension a to mixture b being 1:4, add suspension a into mixture b, stir at room temperature for 4 h, then let it stand for 24 h, and then dry it in an oven at 80 °C, and grind it to obtain hybrid particles;
[0035] Step A2: Stir and mix 10 g of hybrid particles, 100 mL of absolute ethanol and 2.5 g of octadecylamine for 1 h, then add 20 mL of the hydrolysis solution of dodecyltrimethoxysilane, react at 50 °C for 2 h, filter, wash and dry the filter cake to obtain modified activated carbon. The hydrolysis solution of dodecyltrimethoxysilane is composed of dodecyltrimethoxysilane, absolute ethanol and deionized water according to the dosage ratio of 1.5 g:30 mL:5 mL.
[0036] Example 2
[0037] A modified activated carbon is prepared by the following steps:
[0038] Step A1: 0.1 kg of activated carbon (average particle size 200 mesh), 3 L of absolute ethanol and 2 L of deionized water are ultrasonically mixed evenly to obtain suspension a. 10 L of absolute ethanol, 1.5 L of ammonia water (28 wt%), 10 L of tetraethyl orthosilicate and 10 L of deionized water are stirred at room temperature for 15 min to obtain mixture b. According to the volume ratio of suspension a to mixture b being 1:4, suspension a is added to mixture b, stirred at room temperature for 4 h, then left to stand for 24 h, and then dried in an oven at 80 °C, and ground to obtain hybrid particles;
[0039] Step A2: 10 g of hybrid particles, 100 mL of absolute ethanol and 3.4 g of octadecylamine are stirred and mixed for 2 h, then 40 mL of the hydrolysis solution of dodecyltrimethoxysilane is added, and the reaction is carried out at 60 °C for 4 h, filtered, and the filter cake is washed and dried to obtain the modified activated carbon. The hydrolysis solution of dodecyltrimethoxysilane is composed of dodecyltrimethoxysilane, absolute ethanol and deionized water according to the dosage ratio of 2.4 g:35 mL:10 mL.
[0040] Comparative Example 1
[0041] In Step A2 of Example 1, the hybrid particles are replaced with activated carbon with an average particle size of 200 mesh, and the other raw materials and preparation process are the same as in Example 1.
[0042] Example 3
[0043] A POSS-based reinforcing component is prepared by the following steps:
[0044] Step B1: 0.01 mol of octaamino POSS, 0.08 mol of 3,4-dihydroxybenzaldehyde and 350 mL of THF are added to a reaction kettle, stirred, and 2 mL of glacial acetic acid is added. Under an argon atmosphere, the reaction is heated under reflux for 72 h, and then THF and glacial acetic acid are removed by reduced pressure distillation to obtain a POSS-based Schiff base compound. Octaamino POSS is the same as in Example 3;
[0045] Step B2: 4.8 g of the POSS-based Schiff base compound, 0.5 g of potassium hydroxide and 100 mL of absolute ethanol are added to a reaction kettle, stirred, and 9.2 g of epichlorohydrin is added. Under a nitrogen atmosphere, the reaction is carried out at 70 °C for 4 h and then cooled to room temperature. 8.4 g of a 40 wt% potassium hydroxide aqueous solution is added dropwise. After the dropwise addition is completed, the temperature is raised to 60 °C and stirred for 6 h, and then cooled to room temperature. The inorganic salts in the reaction system are removed by filtration, and the obtained filtrate is rotary evaporated to obtain the POSS-based reinforcing component.
[0046] Example 4
[0047] A POSS-based reinforcing component is prepared through the following steps:
[0048] Step B1: Add 0.01 mol of octaamino POSS, 0.08 mol of 3,4-dihydroxybenzaldehyde, and 500 mL of THF into a reaction kettle. After stirring, add 3 mL of glacial acetic acid. Under an argon atmosphere, heat and reflux for 72 h. Then, remove THF and glacial acetic acid by vacuum distillation to obtain a POSS-based Schiff base compound. The octaamino POSS is octaamino cage-like polyhedral oligomeric silsesquioxane, purchased from Hybrid Plastics Company in the United States, and its product number is AM0285;
[0049] Step B2: Add 5.2 g of the POSS-based Schiff base compound, 0.5 g of potassium hydroxide, and 150 mL of absolute ethanol into a reaction kettle. After stirring, add 10.4 g of epichlorohydrin. Under a nitrogen atmosphere, react at 70 °C for 4 h and then cool to room temperature. Dropwise add 8.4 g of 40 wt% potassium hydroxide aqueous solution. After the addition is complete, raise the temperature to 60 °C and stir for 6 h. Then, cool to room temperature, filter to remove the inorganic salts in the reaction system, and rotary evaporate the obtained filtrate to obtain the POSS-based reinforcing component.
[0050] Comparative Example 2
[0051] The octaamino cage-like polyhedral oligomeric silsesquioxane in this comparative example is purchased from Hybrid Plastics Company in the United States, and its product number is AM0285.
[0052] Example 5
[0053] A preparation method of a composite material for regenerating photoresist stripping waste liquid includes the following steps:
[0054] Put 0.5 kg of the modified activated carbon in Example 1 and 2 kg of the POSS-based reinforcing component in Example 3 into 20 L of tetrahydrofuran. After stirring, add 8 L of polydimethylsilane and 0.76 kg of a curing agent, and perform ultrasonic treatment for 30 min to obtain a mixed solution. Immerse the fabric in the mixed solution, perform ultrasonic treatment for 30 min, take it out, and cure it in an oven at 50 °C for 2 h to obtain the composite material for regenerating photoresist stripping waste liquid.
[0055] Among them, the curing agent is Sylgard 184 silicone rubber curing agent, and the fabric is pure cotton plain woven fabric. The warp and weft yarn linear densities are 17 and 18 tex respectively, the warp and weft densities are 536 and 230 per (10 cm) respectively, and the areal density is 120 g / m 2 .
[0056] Example 6
[0057] A preparation method of a composite material for regenerating photoresist stripping waste liquid includes the following steps:
[0058] Put 0.5 kg of the modified activated carbon of Example 1 and 2 kg of the POSS-based reinforcing component of Example 4 into 30 L of tetrahydrofuran. After stirring, add 8 L of polydimethylsilane and 0.76 kg of curing agent, and perform ultrasonic treatment for 30 min to obtain a mixed solution. Immerse the fabric in the mixed solution, perform ultrasonic treatment for 40 min, take it out, and cure it in an oven at 60 °C for 1.5 h to obtain a composite material for regenerating photoresist stripping waste liquid.
[0059] Among them, the curing agent is Sylgard 184 silicone rubber curing agent, and the fabric is a pure cotton plain woven fabric. The warp and weft yarn linear densities are 17 and 18 tex respectively, the warp and weft densities are 536 and 230 per (10 cm) respectively, and the areal density is 120 g / m 2 .
[0060] Example 7
[0061] A preparation method of a composite material for regenerating photoresist stripping waste liquid, comprising the following steps:
[0062] Put 0.5 kg of the modified activated carbon of Example 2 and 2 kg of the POSS-based reinforcing component of Example 4 into 40 L of tetrahydrofuran. After stirring, add 8 L of polydimethylsilane and 0.8 kg of curing agent, and perform ultrasonic treatment for 30 min to obtain a mixed solution. Immerse the fabric in the mixed solution, perform ultrasonic treatment for 60 min, take it out, and cure it in an oven at 70 °C for 2 h to obtain a composite material for regenerating photoresist stripping waste liquid.
[0063] Among them, the curing agent is Sylgard 184 silicone rubber curing agent, and the fabric is a pure cotton plain woven fabric. The warp and weft yarn linear densities are 17 and 18 tex respectively, the warp and weft densities are 536 and 230 per (10 cm) respectively, and the areal density is 120 g / m 2 .
[0064] Comparative Example 3
[0065] Compared with Example 5, replace the modified activated carbon in Example 5 with the substance in Comparative Example 1, and the other raw materials and preparation process are the same as those in Example 5.
[0066] Comparative Example 4
[0067] Compared with Example 5, replace the modified activated carbon in Example 5 with the substance in Comparative Example 2, and the other raw materials and preparation process are the same as those in Example 5.
[0068] Test the composite materials obtained in Examples 5 - 7 and Comparative Examples 3 - 4, and the test items are as follows:
[0069] I. Hydrophobic property test: Use a contact angle measuring instrument to evaluate the wettability of the surface of each group of composite materials. The water droplet size is 4 μL, randomly select 6 different positions on the sample surface for testing, and take the average value as the test result;
[0070] II. Oil-water separation performance: Install each group of composite materials on the oil-water separation device. Pour a mixed solution of 5 mL of distilled water (dyed with methylene blue) and 20 mL of sunflower oil (dyed with Sudan IV) into the device. Calculate the oil-water separation efficiency based on the volume of the oil before and after separation and the separation time. The oil-water separation effect = V1 / V×100%, where V is the volume of the oil before separation and V1 is the volume of the oil after separation. Each sample is tested for cyclic separation 5 times;
[0071] III. Adsorption capacity: Conduct an adsorption experiment on metal ion pollutants "copper sulfate" for each group of composite materials. The entire adsorption process is carried out in a constant temperature shaker at a temperature of 25°C, a rotation speed of 120 r / min, and an adsorption duration of 4 h. Calculate the mass of pollutants in the solution per unit mass of the composite material when adsorption reaches equilibrium. The calculation formula is as follows:
[0072] q = (C0 - C1)V / W
[0073] q is the adsorption capacity, unit: mg / g; C0 and C1 are the initial and final concentrations of copper ions in the solution, unit: mg / L; V is the volume of the solution, unit: L; W is the mass of the composite material, unit: g;
[0074] The test results are shown in Table 1:
[0075] Table 1
[0076] Project Example 5 Example 6 Example 7 Comparative Example 3 Comparative Example 4 Contact Angle (°) 155.8 156.4 157.8 154.2 155.2 Separation Efficiency (%) 97.4 98.0 98.7 96.5 95.2 <![CDATA[Cu 2+ Adsorption capacity (mg / g)]]> 130 137 145 132 74
[0077] As can be seen from Table 1, compared with Comparative Example 3 and Comparative Example 4, the composite materials obtained in Example 5, Example 6, and Example 7 not only have good oil-water separation characteristics but also have excellent adsorption capacity, and have high application value in the regeneration of photoresist stripping waste liquid.
[0078] It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variation thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements but also includes other elements not expressly listed, or further includes elements inherent to such process, method, article or device.
[0079] Although embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A preparation method of a composite material for regenerating photoresist stripping waste liquid, characterized in that, It includes the following steps: First step: Stir and mix the hybrid particles, absolute ethanol, and octadecylamine for 1 - 2 h, then add the hydrolysis solution of dodecyltrimethoxysilane, react at 50 - 60 °C for 2 - 4 h, filter, wash and dry the filter cake to obtain modified activated carbon; Second step: Place the modified activated carbon and POSS - based reinforcing component in tetrahydrofuran, add polydimethylsilane and curing agent after stirring, ultrasonically treat for 30 min to obtain a mixed solution, immerse the fabric in the mixed solution, ultrasonically treat for 30 - 60 min and take it out, cure in an oven at 50 - 70 °C for 1 - 2 h to obtain the composite material for regenerating photoresist stripping waste liquid; The hybrid particles are prepared through the following steps: Ultrasonically mix activated carbon, absolute ethanol, and deionized water evenly to obtain suspension a, stir absolute ethanol, ammonia water, tetraethyl orthosilicate, and deionized water at room temperature for 15 min to obtain mixed solution b, add suspension a to mixed solution b, stir at room temperature for 4 h, then let it stand for 24 h, and then dry in an oven at 80 °C, grind to obtain hybrid particles; The POSS - based reinforcing component is prepared through the following steps: Step B1: Add octa - amino POSS, 3,4 - dihydroxybenzaldehyde, and THF to a reaction kettle, add glacial acetic acid after stirring, reflux and react in an argon atmosphere for 72 h to obtain POSS - based Schiff base compound; Step B2: Add the POSS - based Schiff base compound, potassium hydroxide, and absolute ethanol to a reaction kettle, add epichlorohydrin after stirring, react at 70 °C for 4 h in a nitrogen atmosphere and then cool to room temperature, dropwise add 40 wt% potassium hydroxide aqueous solution, after dropping, heat up to 60 °C and stir and react for 6 h to obtain the POSS - based reinforcing component.
2. The preparation method of a composite material for the regeneration of photoresist stripping waste liquid according to claim 1, wherein The dosage ratio of the hybrid particles, absolute ethanol, octadecylamine, and the hydrolysis solution of dodecyltrimethoxysilane is 10 g: 100 mL: 2.5 - 3.4 g: 20 - 40 mL, and the hydrolysis solution of dodecyltrimethoxysilane is composed of dodecyltrimethoxysilane, absolute ethanol, and deionized water according to the dosage ratio of 1.5 - 2.4 g: 30 - 35 mL: 5 - 10 mL.
3. The preparation method of a composite material for regenerating photoresist stripping waste liquid according to claim 1, characterized in that, The dosage ratio of the modified activated carbon, POSS - based reinforcing component, tetrahydrofuran, polydimethylsilane, and curing agent in the mixed solution is 0.5 g: 2 g: 20 - 40 mL: 8 mL: 0.76 - 0.8 g.
4. The preparation method of a composite material for regenerating photoresist stripping waste liquid according to claim 1, characterized in that, The volume ratio of suspension a and mixed solution b is 1:4, suspension a is composed of activated carbon, absolute ethanol, and deionized water according to the dosage ratio of 0.1 g: 3 mL: 2 mL, and mixed solution b is composed of absolute ethanol, ammonia water, tetraethyl orthosilicate, and deionized water according to the volume ratio of 10: 1.5: 10:
10.
5. The preparation method of a composite material for the regeneration of photoresist stripping waste liquid according to claim 1, characterized in that, In step B1, the dosage ratio of octa - amino POSS, 3,4 - dihydroxybenzaldehyde, THF, and glacial acetic acid is 0.01 mol: 0.08 mol: 350 - 500 mL: 2 - 3 mL, and octa - amino POSS is octa - amino cage - shaped polyhedral oligomeric silsesquioxane.
6. The preparation method of a composite material for the regeneration of photoresist stripping waste liquid according to claim 1, wherein, In step B2, the dosage ratio of the POSS - based Schiff base compound, potassium hydroxide, absolute ethanol, epichlorohydrin, and potassium hydroxide aqueous solution is 4.8 - 5.2 g: 0.5 g: 100 - 150 mL: 9.2 - 10.4 g: 8.4 g.
7. A composite material for the regeneration of photoresist stripping waste liquid, characterized in that, Prepared by the preparation method according to any one of claims 1-6.
Citation Information
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