Resin material for filtration and preparation method thereof

Abstract

The invention discloses a resin material for filtering and a preparation method thereof, and belongs to the technical field of filtering materials. The resin material for filtration comprises the following raw material components in parts by weight: 10-20 parts by mass of epoxy resin, 3-8 parts by mass of a curing agent, 0.1-3 parts by mass of a curing reaction accelerator, 1-10 parts by mass of a modified filler, 30-70 parts by mass of a modified hard particle material, 20-50 parts by mass of water, 0.1-3 parts by mass of a soluble inorganic salt and 0.1-3 parts by mass of a surface active diluent. The prepared resin material for filtration is higher in breaking strength, and cavities and palm holes caused by bubbles are avoided.

Description

Technical Field

[0001] The invention relates to a resin material for filtering and a preparation method thereof. Background Art

[0002] In modern industry, filter resin materials are widely used in many fields, including but not limited to water treatment, air filtration, chemical industry and ceramic manufacturing. Among them, in the ceramic manufacturing process, the filter layer resin material, as a part of the mold, has a vital impact on the quality and production efficiency of the final product. At present, the known filter layer resin material is made by mixing and stirring ingredients such as epoxy compounds, curing agents, fillers and water, and then moisturizing and curing. After curing, this material will form a porous structure to allow liquid or gas to pass through while retaining particulate matter. In order to improve the flexibility and strength of the material, plasticizers are sometimes added.

[0003] However, there are several significant problems in the existing filter layer resin material preparation method:

[0004] 1. The flexural strength of traditional filter layer resin materials is usually lower than 15Mpa (test equipment: flexural testing machine), which means they are prone to breakage when subjected to pressure, especially in the ceramic grouting process. When faced with a mud alternating pressure of up to 1.5Mpa, the filter layer resin material may fail quickly due to poor flexural strength, resulting in a shortened mold life.

[0005] 2. Bubble cavities and brown eyes will be generated during the casting process of the filter layer. These problems not only affect the quality of the filter layer, but also for ceramic products, the defects on the surface of the filter layer will be directly reflected on the finished product, causing uneven surface, thus affecting product quality.

[0006] Therefore, in order to solve the above problems, it is necessary to develop a resin material for filtration and a preparation method thereof. Summary of the invention

[0007] The purpose of the present invention is to provide a resin material for filtration and a preparation method thereof, so as to solve the technical problems mentioned in the above background technology.

[0008] The technical solution for achieving the purpose of the present invention is:

[0009] The first aspect of the present invention provides a resin material for filtration. The raw material components include, by weight, 10 to 20 parts by weight of epoxy resin, 3 to 8 parts by weight of curing agent, 0.1 to 3 parts by weight of curing reaction accelerator, 1 to 10 parts by weight of modified filler, 30 to 70 parts by weight of modified hard particulate material, 20 to 50 parts by weight of water, 0.1 to 3 parts by weight of soluble inorganic salt, and 0.1 to 3 parts by weight of surfactant diluent.

[0010] Furthermore, the epoxy resin includes bisphenol A type and bisphenol F type epoxy resins, such as CYD-115, CYD-127, CYD-128, CYDF-180 produced by Yueyang Petrochemical, and E44, E42, E815, E828, and E827 epoxy resins produced by Shell.

[0011] Furthermore, the curing agent includes polyamine, polyamide, polycyclic aliphatic amine or aromatic amine curing agent, such as ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, 6-hydroxyethyldiamine.

[0012] Furthermore, the curing reaction accelerator includes BDMA (benzyl dimethylamine), DMP-10 (dimethylaminomethylphenol), DMP-30 (2,4,6-tris(dimethylaminomethylene)phenol), 2MZ (2-methylimidazole), 2E4MZ (2-ethyl-4-methylimidazole), and 2E4MZ-CN (2-ethyl-4-methylimidazole-carboxyl).

[0013] Furthermore, the surfactant diluent may be phenyl glycidyl ether, butyl glycidyl ether, or 2-ethylhexyl glycidyl ether.

[0014] Furthermore, the pH value of the water is between 6 and 8.

[0015] Further, the soluble inorganic salts include sodium hydroxide, calcium hydroxide, sodium chloride, calcium chloride, magnesium chloride, zinc sulfate, aluminum sulfate, copper sulfate, and magnesium sulfate.

[0016] Furthermore, the modified filler is obtained by pre-modifying zeolite with vinyltrichlorosilane and then modifying the pre-modified zeolite with 4-mercaptophenylboric acid.

[0017] Furthermore, the modified hard particle material is obtained by modifying the hard particle material with a mixed silane coupling agent.

[0018] Furthermore, the mixed silane coupling agent is obtained by mixing silane coupling agent KH560 and dimethylsilanediol.

[0019] The second aspect of the present invention provides a method for preparing the resin material for filtration as described in the first aspect, comprising the following preparation steps:

[0020] (1) Prepare the following raw materials in parts by weight: 10 to 20 parts by weight of epoxy resin, 3 to 8 parts by weight of curing agent, 0.1 to 3 parts by weight of curing reaction accelerator, 1 to 10 parts by weight of modified filler, 30 to 70 parts by weight of modified hard particulate material, 20 to 50 parts by weight of water, 0.1 to 3 parts by weight of soluble inorganic salt, and 0.1 to 3 parts by weight of surfactant diluent.

[0021] (2) mixing the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1) and stirring the mixture thoroughly to obtain a premix;

[0022] (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir thoroughly for 13 to 17 minutes to obtain a mixed slurry;

[0023] (4) Inject the mixed slurry of step (3) into the master mold, seal the grouting port after injection, and harden it at 30-60°C for 20-72h, then heat it to 78-82°C for 7-9h, cool it to 30-60°C, clean it with pressurized water for 15-25min, clean it with pressurized air for 15-25min, and then harden it again for 7-9h. Furthermore, the preparation steps of the modified filler are as follows: 4 to 6 parts by mass of zeolite and 70 to 90 parts by mass of a hydrochloric acid solution with a concentration of 2 mol / L are heated to reflux for 4 to 6 minutes, cooled to room temperature, filtered, washed with water until neutral, dried in an oven at 75 to 85°C overnight to obtain an activated zeolite, and under nitrogen protection, the activated zeolite is added to 45 to 55 parts by mass of dry toluene, stirred evenly, and then 3.2 to 3.4 parts by mass of vinyltrichlorosilane is added dropwise, heated to reflux at 45 to 55°C for 23 to 25 hours, filtered after the reaction is completed, washed with toluene, acetone, water, and methanol, and dried. The mixture was dried in an oven at 55 to 65° C. overnight, then added to 35 to 45 parts by weight of anhydrous methanol, stirred and dispersed evenly, then 8 to 9 parts by weight of an anhydrous methanol solution of 4-mercaptophenylboric acid with a 5% content of 4-mercaptophenylboric acid was added, and the mixture was stirred and dispersed evenly, 4 to 5 parts by weight of an anhydrous methanol solution of 2,2-azobisisobutyronitrile with a 2% content of 2,2-azobisisobutyronitrile was added, and the mixture was stirred and dispersed evenly, the temperature was raised to 60 to 70° C., heated under reflux for 46 to 50 hours, the reaction system was cooled to room temperature, and then filtered, washed with water and methanol in turn, dried in an oven at 75 to 85° C. overnight to obtain a modified filler.

[0024] Furthermore, the zeolite particle size is below 10 μm, accounting for 40-80%.

[0025] Furthermore, the preparation method of the modified hard particulate material is as follows: 0.5 to 1.2 parts by mass of hard particulate material is added to 20 parts by mass of toluene, ultrasonically dispersed at room temperature for 30 minutes, then 0.09 to 0.11 parts by mass of mixed silane coupling agent is added, and ultrasonication is continued for 3 to 4 minutes, and then stirred at 85 to 95°C for 5.5 to 6.5 hours, and then centrifuged at room temperature and 12000r / min to obtain a modified hard particulate material.

[0026] Furthermore, the mass ratio of the silane coupling agent KH560 to dimethylsilanediol in the mixed silane coupling agent is 1:2-4.

[0027] Furthermore, the hard particulate material is silicon oxide powder with a particle size of less than 10 μm accounting for 20 to 70%.

[0028] By adopting the above technical solution, the present invention has the following beneficial effects:

[0029] The resin material for filtration of the present invention comprises, by weight, raw material components including 10 to 20 parts by weight of epoxy resin, 3 to 8 parts by weight of curing agent, 0.1 to 3 parts by weight of curing reaction accelerator, 1 to 10 parts by weight of modified filler, 30 to 70 parts by weight of modified hard particle material, 20 to 50 parts by weight of water, 0.1 to 3 parts by weight of soluble inorganic salt, and 0.1 to 3 parts by weight of surfactant diluent; wherein the modified filler is obtained by pre-modifying zeolite with vinyltrichlorosilane and then modifying the pre-modified zeolite with 4-mercaptophenylboric acid; the modified hard particle material is obtained by modifying the hard particle material with a mixed silane coupling agent; and the mixed silane coupling agent is obtained by mixing silane coupling agent KH560 and dimethylsilanediol.

[0030] Firstly, the zeolite is pre-modified with vinyltrichlorosilane, and then the pre-modified zeolite is modified with 4-mercaptophenylboric acid. Vinyltrichlorosilane is grafted onto the surface of the activated zeolite through chlorosilane, and the mercapto group on the 4-mercaptophenylboric acid undergoes a click reaction with the vinyl group, and hydrophilic phenylboric acid is introduced onto the surface of the zeolite, which can effectively improve the dispersibility of the zeolite in the premix, thereby increasing the dispersibility of the zeolite in the filtration resin material; secondly, the hard particle material can be treated with a mixed silane coupling agent to increase the dispersibility of the hard particle material in the resin base material, and effectively avoid the influence of the agglomeration of the zeolite and the hard particle material on the mechanical properties of the filtration resin material.

[0031] Secondly, 10 to 20 parts by weight of epoxy resin, 3 to 8 parts by weight of curing agent, 0.1 to 3 parts by weight of curing reaction accelerator, 1 to 10 parts by weight of modified filler, 30 to 70 parts by weight of modified hard particulate material, 20 to 50 parts by weight of water, 0.1 to 3 parts by weight of soluble inorganic salt, and 0.1 to 3 parts by weight of surfactant diluent are mixed to obtain a mixed slurry, which is then heated to 78 to 82° C. after grouting and hardening. At this time, the silane coupling agent on the modified hard particulate material is hydrolyzed and condensed and reacts with the boric acid on the adjacent modified hard particulate material. The epoxy-containing polydimethylsilane and polysiloxane block copolymers are formed by the hard particle materials, which effectively improve the compatibility of the zeolite, hard particle materials and the base material interface, and effectively avoid the appearance of bubbles at the junction of the two phases. The presence of polydimethylsilane chain segments can quickly eliminate the bubbles generated in the preparation process of the filtration resin material and avoid the formation of cavities and brown eyes. At the same time, the rigid group benzene ring contained in the polysiloxane chain segments can improve the strength of the filtration resin material, among which the Si-OBO flexible chain segments can improve the toughness of the filtration resin material. DETAILED DESCRIPTION

[0032] In order to better understand the above technical solution, the above technical solution will be described in detail below in conjunction with specific implementation methods.

[0033] The following embodiments are only used to more clearly illustrate the technical solutions of the present invention, and are not intended to limit the protection scope of the present invention.

[0034] (Example 1)

[0035] A method for preparing a resin material for filtration comprises the following preparation steps:

[0036] (1) Prepare the following raw materials in parts by weight: 10 parts by weight of bisphenol A epoxy resin, 3 parts by weight of curing agent diethylenetriamine, 0.1 parts by weight of curing reaction accelerator 2E4MZ, 1 part by weight of modified filler, 30 parts by weight of modified hard particulate material, 20 parts by weight of water, 0.1 parts by weight of soluble inorganic salt sodium chloride, and 0.1 parts by weight of surfactant diluent phenyl glycidyl ether.

[0037] (2) mixing the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1) and stirring the mixture thoroughly to obtain a premix;

[0038] (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir thoroughly for 13 minutes to obtain a mixed slurry;

[0039] (4) Inject the mixed slurry of step (3) into the master mold, seal the grouting port after injection, and harden it at 30°C for 20 hours, then heat it to 78°C and keep it for 7 hours, cool it to 30°C, clean it with pressurized water for 15 minutes, clean it with pressurized air for 15 minutes, and then harden it again for 7 hours.

[0040] The preparation steps of the modified filler are as follows: 4 parts by mass of zeolite and 70 parts by mass of hydrochloric acid solution with a concentration of 2 mol / L are heated to reflux for 4 minutes, cooled to room temperature, filtered, washed with water until neutral, dried in an oven at 75°C overnight to obtain activated zeolite, and under nitrogen protection, the activated zeolite is added to 4 parts by mass of dry toluene, stirred evenly, and then 3.2 parts by mass of vinyltrichlorosilane is added dropwise, heated to reflux for 23 hours at 45°C, filtered after the reaction is completed, washed with toluene, acetone, water, and methanol, dried in an oven at 55°C, and then dried in an oven at 55°C. The mixture was dried overnight in a vacuum evaporator, then added to 35 parts by weight of anhydrous methanol, stirred and dispersed evenly, then 8 parts by weight of an anhydrous methanol solution of 4-mercaptophenylboric acid with a 5% content of 4-mercaptophenylboric acid was added, and stirring and dispersing was continued evenly, 4 parts by weight of an anhydrous methanol solution of 2,2-azobisisobutyronitrile with a 2% content of 2,2-azobisisobutyronitrile was added, and stirring and dispersing was continued evenly, the temperature was raised to 60°C, and heated to reflux for 46 hours. The reaction system was cooled to room temperature, then filtered, washed with water and methanol in turn, dried in an oven at 75°C overnight to obtain a modified filler.

[0041] The zeolite particle size is less than 10 μm, accounting for 50%.

[0042] The preparation method of the modified hard particle material is as follows: 0.5 parts by mass of hard particle material is added to 20 parts by mass of toluene, ultrasonically dispersed at room temperature for 30 minutes, then 0.09 parts by mass of mixed silane coupling agent is added, ultrasonication is continued for 3 minutes, then stirred and reacted at 85°C for 5.5 hours, and then centrifuged at room temperature and 12000r / min to obtain the modified hard particle material.

[0043] The mass ratio of silane coupling agent KH560 to dimethylsilanediol in the mixed silane coupling agent is 1:2. The hard particle material is silicon oxide powder with a particle size of less than 10 μm accounting for 50%.

[0044] (Example 2)

[0045] A method for preparing a resin material for filtration comprises the following preparation steps:

[0046] (1) Prepare the following raw materials in parts by weight: 15 parts by weight of bisphenol A epoxy resin, 6 parts by weight of curing agent diethylenetriamine, 1.5 parts by weight of curing reaction accelerator 2E4MZ, 6 parts by weight of modified filler, 50 parts by weight of modified hard particulate material, 35 parts by weight of water, 1.5 parts by weight of soluble inorganic salt sodium chloride, and 1.5 parts by weight of surfactant diluent phenyl glycidyl ether.

[0047] (2) mixing the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1) and stirring the mixture thoroughly to obtain a premix;

[0048] (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir for 15 minutes to obtain a mixed slurry;

[0049] (4) Inject the mixed slurry of step (3) into the master mold, seal the grouting port after injection, and harden it at 45°C for 40 hours, then heat it to 80°C for 8 hours, cool it to 45°C, clean it with pressurized water for 20 minutes, clean it with pressurized air for 20 minutes, and then harden it again for 8 hours.

[0050] The preparation steps of the modified filler are as follows: 5 parts by mass of zeolite and 80 parts by mass of a hydrochloric acid solution with a concentration of 2 mol / L are heated to reflux for 5 minutes, cooled to room temperature, filtered, washed with water until neutral, dried in an oven at 80°C overnight to obtain an activated zeolite, and under nitrogen protection, the activated zeolite is added to 50 parts by mass of dry toluene, stirred evenly, and then 3.3 parts by mass of vinyltrichlorosilane is added dropwise, heated to reflux at 50°C for 24 hours, filtered after the reaction is completed, washed with toluene, acetone, water, and methanol, and dried in an oven at 60°C. The mixture was dried overnight, then added to 40 parts by mass of anhydrous methanol, stirred and dispersed evenly, then 8.5 parts by mass of anhydrous methanol solution of 4-mercaptophenylboric acid with a 5% content of 4-mercaptophenylboric acid was added, and stirring was continued to disperse evenly, 4.5 parts by mass of anhydrous methanol solution of 2,2-azobisisobutyronitrile with a 2% content of 2,2-azobisisobutyronitrile was added, and stirring was continued to disperse evenly, the temperature was raised to 65°C, heated to reflux for 48 hours, the reaction system was cooled to room temperature, and then filtered, washed with water and methanol in turn, dried in an oven at 80°C overnight to obtain a modified filler.

[0051] The zeolite particle size is less than 10 μm, accounting for 50%.

[0052] The preparation method of the modified hard particle material is as follows: 0.8 parts by mass of hard particle material is added to 20 parts by mass of toluene, ultrasonically dispersed at room temperature for 30 minutes, then 0.1 parts by mass of mixed silane coupling agent is added, and ultrasonication is continued for 3 minutes, then stirred and reacted at 90°C for 6 hours, and then centrifuged at room temperature and 12000r / min to obtain the modified hard particle material.

[0053] The mass ratio of silane coupling agent KH560 to dimethylsilanediol in the mixed silane coupling agent is 1:3. The hard particle material is silicon oxide powder with a particle size of less than 10 μm accounting for 50%.

[0054] (Example 3)

[0055] A method for preparing a resin material for filtration comprises the following preparation steps:

[0056] (1) Prepare the following raw materials in parts by weight: 20 parts by weight of bisphenol A epoxy resin, 8 parts by weight of curing agent diethylenetriamine, 3 parts by weight of curing reaction accelerator 2E4MZ, 10 parts by weight of modified filler, 70 parts by weight of modified hard particulate material, 50 parts by weight of water, 3 parts by weight of soluble inorganic salt sodium chloride, and 3 parts by weight of surfactant diluent phenyl glycidyl ether.

[0057] (2) mixing the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1) and stirring the mixture thoroughly to obtain a premix;

[0058] (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir thoroughly for 17 minutes to obtain a mixed slurry;

[0059] (4) Inject the mixed slurry of step (3) into the master mold, seal the grouting port after injection, place it in a 60°C environment to harden for 72 hours, then heat it to 82°C and keep it for 9 hours, cool it to 60°C, clean it with pressurized water for 25 minutes, clean it with pressurized air for 25 minutes, and then harden it again for 9 hours.

[0060] The preparation steps of the modified filler are as follows: 6 parts by mass of zeolite and 90 parts by mass of hydrochloric acid solution with a concentration of 2 mol / L are heated to reflux for 6 minutes, cooled to room temperature, filtered, washed with water until neutral, dried in an oven at 85°C overnight to obtain activated zeolite, and under nitrogen protection, the activated zeolite is added to 55 parts by mass of dry toluene, stirred evenly, and then 3.4 parts by mass of vinyltrichlorosilane is added dropwise, heated to reflux for 25 hours at 55°C, filtered after the reaction is completed, washed with toluene, acetone, water, and methanol, dried in an oven at 65°C, and then the zeolite is dried. The mixture was dried in an oven overnight, then added to 45 parts by mass of anhydrous methanol, stirred and dispersed evenly, then 9 parts by mass of an anhydrous methanol solution of 4-mercaptophenylboric acid with a 5% content of 4-mercaptophenylboric acid was added, and stirring and dispersing was continued, and 5 parts by mass of an anhydrous methanol solution of 2,2-azobisisobutyronitrile with a 2% content of 2,2-azobisisobutyronitrile was added, and stirring and dispersing was continued, the temperature was raised to 70°C, and heated to reflux for 50 hours. The reaction system was cooled to room temperature, then filtered, washed with water and methanol in turn, dried in an oven at 85°C overnight to obtain a modified filler.

[0061] The zeolite particle size is less than 10 μm, accounting for 50%.

[0062] The preparation method of the modified hard particle material is as follows: 1.2 parts by mass of hard particle material is added to 20 parts by mass of toluene, ultrasonically dispersed at room temperature for 30 minutes, then 0.11 parts by mass of mixed silane coupling agent is added, and ultrasonication is continued for 4 minutes, then stirred and reacted at 95°C for 6.5 hours, and then centrifuged at room temperature and 12000r / min to obtain the modified hard particle material.

[0063] The mass ratio of silane coupling agent KH560 to dimethylsilanediol in the mixed silane coupling agent is 1:4. The hard particle material is silicon oxide powder with a particle size of less than 10 μm accounting for 50%.

[0064] (Comparative Example 1)

[0065] A method for preparing a resin material for filtration comprises the following preparation steps:

[0066] (1) Prepare the following raw materials in parts by weight: 15 parts by weight of bisphenol A epoxy resin, 6 parts by weight of curing agent diethylenetriamine, 1.5 parts by weight of curing reaction accelerator 2E4MZ, 6 parts by weight of zeolite, 50 parts by weight of modified hard particulate material, 35 parts by weight of water, 1.5 parts by weight of soluble inorganic salt sodium chloride, and 1.5 parts by weight of surfactant diluent phenyl glycidyl ether.

[0067] (2) mixing the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1) and stirring the mixture thoroughly to obtain a premix;

[0068] (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir for 15 minutes to obtain a mixed slurry;

[0069] (4) Inject the mixed slurry of step (3) into the master mold, seal the grouting port after injection, and harden it at 45°C for 40 hours, then heat it to 80°C for 8 hours, cool it to 45°C, clean it with pressurized water for 20 minutes, clean it with pressurized air for 20 minutes, and then harden it again for 8 hours.

[0070] The zeolite particle size is less than 10 μm, accounting for 50%.

[0071] The preparation method of the modified hard particle material is as follows: 0.8 parts by mass of hard particle material is added to 20 parts by mass of toluene, ultrasonically dispersed at room temperature for 30 minutes, then 0.1 parts by mass of mixed silane coupling agent is added, and ultrasonication is continued for 3 minutes, then stirred and reacted at 90°C for 6 hours, and then centrifuged at room temperature and 12000r / min to obtain the modified hard particle material.

[0072] The mass ratio of silane coupling agent KH560 to dimethylsilanediol in the mixed silane coupling agent is 1:3. The hard particle material is silicon oxide powder with a particle size of less than 10 μm accounting for 50%.

[0073] (Comparative Example 2)

[0074] A method for preparing a resin material for filtration comprises the following preparation steps:

[0075] (1) Prepare the following raw materials in parts by weight: 15 parts by weight of bisphenol A epoxy resin, 6 parts by weight of curing agent diethylenetriamine, 1.5 parts by weight of curing reaction accelerator 2E4MZ, 6 parts by weight of modified filler, 50 parts by weight of hard particulate material, 35 parts by weight of water, 1.5 parts by weight of soluble inorganic salt sodium chloride, and 1.5 parts by weight of surfactant diluent phenyl glycidyl ether.

[0076] (2) mixing the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1) and stirring the mixture thoroughly to obtain a premix;

[0077] (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir for 15 minutes to obtain a mixed slurry;

[0078] (4) Inject the mixed slurry of step (3) into the master mold, seal the grouting port after injection, and harden it at 45°C for 40 hours, then heat it to 80°C for 8 hours, cool it to 45°C, clean it with pressurized water for 20 minutes, clean it with pressurized air for 20 minutes, and then harden it again for 8 hours.

[0079] The preparation steps of the modified filler are as follows: 5 parts by mass of zeolite and 80 parts by mass of a hydrochloric acid solution with a concentration of 2 mol / L are heated to reflux for 5 minutes, cooled to room temperature, filtered, washed with water until neutral, dried in an oven at 80°C overnight to obtain an activated zeolite, and under nitrogen protection, the activated zeolite is added to 50 parts by mass of dry toluene, stirred evenly, and then 3.3 parts by mass of vinyltrichlorosilane is added dropwise, heated to reflux at 50°C for 24 hours, filtered after the reaction is completed, washed with toluene, acetone, water, and methanol, and dried in an oven at 60°C. The mixture was dried overnight, then added to 40 parts by mass of anhydrous methanol, stirred and dispersed evenly, then 8.5 parts by mass of anhydrous methanol solution of 4-mercaptophenylboric acid with a 5% content of 4-mercaptophenylboric acid was added, and stirring was continued to disperse evenly, 4.5 parts by mass of anhydrous methanol solution of 2,2-azobisisobutyronitrile with a 2% content of 2,2-azobisisobutyronitrile was added, and stirring was continued to disperse evenly, the temperature was raised to 65°C, heated to reflux for 48 hours, the reaction system was cooled to room temperature, and then filtered, washed with water and methanol in turn, dried in an oven at 80°C overnight to obtain a modified filler.

[0080] The zeolite particle size is less than 10 μm, accounting for 50%.

[0081] The hard particle material is silicon oxide powder with a particle size of less than 10 μm accounting for 50%.

[0082] (Comparative Example 3)

[0083] A method for preparing a resin material for filtration comprises the following preparation steps:

[0084] (1) Prepare the following raw materials in parts by weight: 15 parts by weight of bisphenol A epoxy resin, 6 parts by weight of curing agent diethylenetriamine, 1.5 parts by weight of curing reaction accelerator 2E4MZ, 6 parts by weight of modified filler, 50 parts by weight of modified hard particulate material, 35 parts by weight of water, 1.5 parts by weight of soluble inorganic salt sodium chloride, and 1.5 parts by weight of surfactant diluent phenyl glycidyl ether.

[0085] (2) mixing the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1) and stirring the mixture thoroughly to obtain a premix;

[0086] (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir for 15 minutes to obtain a mixed slurry;

[0087] (4) Inject the mixed slurry from step (3) into the master mold, seal the injection port after injection, and harden it at 45°C for 40 hours, then clean it with pressurized water for 20 minutes, clean it with pressurized air for 20 minutes, and then harden it again for 8 hours.

[0088] The preparation steps of the modified filler are as follows: 5 parts by mass of zeolite and 80 parts by mass of a hydrochloric acid solution with a concentration of 2 mol / L are heated to reflux for 5 minutes, cooled to room temperature, filtered, washed with water until neutral, dried in an oven at 80°C overnight to obtain an activated zeolite, and under nitrogen protection, the activated zeolite is added to 50 parts by mass of dry toluene, stirred evenly, and then 3.3 parts by mass of vinyltrichlorosilane is added dropwise, heated to reflux at 50°C for 24 hours, filtered after the reaction is completed, washed with toluene, acetone, water, and methanol, and dried in an oven at 60°C. The mixture was dried overnight, then added to 40 parts by mass of anhydrous methanol, stirred and dispersed evenly, then 8.5 parts by mass of anhydrous methanol solution of 4-mercaptophenylboric acid with a 5% content of 4-mercaptophenylboric acid was added, and stirring was continued to disperse evenly, 4.5 parts by mass of anhydrous methanol solution of 2,2-azobisisobutyronitrile with a 2% content of 2,2-azobisisobutyronitrile was added, and stirring was continued to disperse evenly, the temperature was raised to 65°C, heated to reflux for 48 hours, the reaction system was cooled to room temperature, and then filtered, washed with water and methanol in turn, dried in an oven at 80°C overnight to obtain a modified filler.

[0089] The zeolite particle size is less than 10 μm, accounting for 50%.

[0090] The preparation method of the modified hard particle material is as follows: 0.8 parts by mass of hard particle material is added to 20 parts by mass of toluene, ultrasonically dispersed at room temperature for 30 minutes, then 0.1 parts by mass of mixed silane coupling agent is added, and ultrasonication is continued for 3 minutes, then stirred and reacted at 90°C for 6 hours, and then centrifuged at room temperature and 12000r / min to obtain the modified hard particle material.

[0091] The mass ratio of silane coupling agent KH560 to dimethylsilanediol in the mixed silane coupling agent is 1:3. The hard particle material is silicon oxide powder with a particle size of less than 10 μm accounting for 50%.

[0092] Effect example:

[0093] Appearance performance: Observe the filter resin materials prepared in the examples and comparative examples with human eyes to see whether there are cavities and brown eyes.

[0094] Flexural strength: The filtration resin materials prepared in the embodiment and the comparative example with the same area and volume were tested for flexural strength using a flexural testing machine.

[0095] Table 1 below shows the performance test results of the filtration resin materials prepared in the examples and comparative examples:

[0096] Table 1

[0097]

[0098] As shown in Table 1 above, the filtration resin material prepared in the embodiment has higher flexural strength and no cavities and brown eyes caused by bubbles;

[0099] Comparative Example 1 Compared with Example 2, the zeolite in Comparative Example 1 was not modified, and the zeolite in the obtained filtration resin material was partially agglomerated, causing a small amount of cavities and brown eyes, resulting in poor flexural strength of the filtration resin material. Comparative Example 2 Compared with Example 2, the hard particulate material in Comparative Example 2 was not modified, and the hard particulate material in the obtained filtration resin material was agglomerated, forming cavities and brown eyes, resulting in poor flexural strength of the filtration resin material.

[0100] Comparative Example 3 is compared with Example 2. In Comparative Example 3, the temperature was not raised to 80° C. for 8 hours of heat preservation after hardening, and the epoxy-containing polydimethylsilane and polysiloxane block copolymer could not be formed in the obtained filtration resin material, and the flexural strength of the filtration resin material was poor.

[0101] The specific embodiments described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A resin material for filtration, characterized in that: In parts by weight, the raw material components include 10 to 20 parts by weight of epoxy resin, 3 to 8 parts by weight of curing agent, 0.1 to 3 parts by weight of curing reaction accelerator, 1 to 10 parts by weight of modified filler, 30 to 70 parts by weight of modified hard particulate material, 20 to 50 parts by weight of water, 0.1 to 3 parts by weight of soluble inorganic salt, and 0.1 to 3 parts by weight of surfactant diluent.

2. The resin material for filtration according to claim 1, characterized in that The modified filler is obtained by pre-modifying zeolite with vinyltrichlorosilane and then modifying the pre-modified zeolite with 4-mercaptophenylboric acid.

3. The resin material for filtration according to claim 1, characterized in that The modified hard particle material is obtained by modifying the hard particle material with a mixed silane coupling agent.

4. The resin material for filtration according to claim 3, characterized in that The mixed silane coupling agent is obtained by mixing silane coupling agent KH560 and dimethylsilanediol.

5. A method for preparing a resin material for filtration according to any one of claims 1 to 4, characterized in that: The method comprises the following preparation steps: (1) Prepare the following raw materials in parts by weight: 10-20 parts by weight of epoxy resin, 3-8 parts by weight of curing agent, 0.1-3 parts by weight of curing reaction accelerator, 1-10 parts by weight of modified filler, 30-70 parts by weight of modified hard particulate material, 20-50 parts by weight of water, 0.1-3 parts by weight of soluble inorganic salt, and 0.1-3 parts by weight of surfactant diluent.

6. (2) Mix the modified filler, modified hard particulate material, water, and soluble inorganic salt weighed in step (1), stir and mix thoroughly to obtain a premix; (3) adding the epoxy resin, curing agent, curing reaction accelerator, and surfactant diluent weighed in step (1) to the premix obtained in step (2), and continuing to stir thoroughly for 13 to 17 minutes to obtain a mixed slurry; (4) Inject the mixed slurry in step (3) into the master mold, seal the grouting port after injection, place it in an environment of 30-60°C for hardening for 20-72 hours, then heat it to 78-82°C for insulation reaction for 7-9 hours, cool it to 30-60°C, clean it with pressurized water for 15-25 minutes, clean it with pressurized air for 15-25 minutes, and then harden it again for 7-9 hours.

7. The method for preparing a resin material for filtration according to claim 5, characterized in that: The preparation steps of the modified filler are as follows: 4-6 parts by weight of zeolite and 70-90 parts by weight of a hydrochloric acid solution with a concentration of 2 mol / L are heated to reflux for 4-6 minutes, cooled to room temperature, filtered, washed with water until neutral, dried in an oven at 75-85°C overnight to obtain an activated zeolite, and under nitrogen protection, the activated zeolite is added to 45-55 parts by weight of dry toluene, stirred evenly, and then 3.2-3.4 parts by weight of vinyltrichlorosilane is added dropwise, heated to reflux at 45-55°C for 23-25 ​​hours, filtered after the reaction is completed, washed with toluene, acetone, water, and methanol, and dried at 55 ~65 ℃ oven for drying overnight, then added to 35~45 parts by weight of anhydrous methanol, stirred and dispersed evenly, then added 8~9 parts by weight of anhydrous methanol solution of 4-mercaptophenylboric acid with a 5% content of 4-mercaptophenylboric acid, continued to stir and disperse evenly, added 4~5 parts by weight of anhydrous methanol solution of 2,2-azobisisobutyronitrile with a 2% content of 2,2-azobisisobutyronitrile, continued to stir and disperse evenly, heated to 60~70 ℃, heated to reflux for 46~50h, the reaction system was cooled to room temperature, then filtered, washed with water and methanol in turn, dried in an oven at 75~85 ℃ overnight to obtain a modified filler.

8. The method for preparing a resin material for filtration according to claim 6, characterized in that: The zeolite particle size is below 10 μm, accounting for 40-80%.

9. The method for preparing a resin material for filtration according to claim 5, characterized in that: The preparation method of the modified hard particle material is as follows: 0.5-1.2 parts by mass of hard particle material is added to 20 parts by mass of toluene, ultrasonically dispersed at room temperature for 30 minutes, then 0.09-0.11 parts by mass of mixed silane coupling agent is added, and ultrasonication is continued for 3-4 minutes, then stirred and reacted at 85-95°C for 5.5-6.5 hours, and then centrifuged at room temperature and 12000r / min to obtain the modified hard particle material.

10. The method for preparing a resin material for filtration according to claim 8, characterized in that: The mass ratio of the silane coupling agent KH560 to dimethylsilanediol in the mixed silane coupling agent is 1:2-4.

11. The method for preparing a resin material for filtration according to claim 8, characterized in that: The hard particle material is silicon oxide powder with a particle size of less than 10 μm accounting for 20-70%.

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