A microporous quartz formulation and method of making the same

Abstract

The application relates to the technical field of microporous quartz, and discloses a microporous quartz formula and a preparation method thereof, which comprises the following components by weight: modified bentonite 10-20 parts, kaolin 10-15 parts, a binder 6-8 parts, sodium fluorosilicate 10-12 parts, quartz powder 20-25 parts, SiO2 60-80 parts, Al2O3 1-3 parts, TiO2 2-4 parts, BaO 1-2 parts, MnO 0.2-0.4 parts, MgO 1.2-2.5 parts and K2O 0.5-1.5 parts; the preparation method of the microporous quartz formula is as follows: the raw materials are stirred and mixed according to the proportion, are stirred for 3-5 hours at 110-120 DEG C, and then initial materials in a molten state are obtained; then, the initial materials in the molten state are added into a microporous quartz model, and the preparation is completed; the microporous quartz formula has good effects of fire resistance, wear resistance and antibiosis.

Description

Technical Field

[0001] This invention relates to the field of microporous quartz technology, specifically to a microporous quartz formulation and its preparation method. Background Technology

[0002] Quartz is one of the major rock-forming minerals, generally referring to low-temperature quartz, which is the most widely distributed mineral in the quartz group. In a broader sense, quartz also includes high-temperature quartz and coesite, etc. Its main component is SiO2, which is colorless and transparent. It often contains a small amount of impurities, which can turn it into translucent or opaque crystals. It is hard in texture and is a mineral resource with very stable physical and chemical properties. Its crystals belong to the trigonal crystal system and are oxide minerals. It is also a raw material for quartz refractory materials and ferrosilicon. Summary of the Invention

[0003] (a) Technical problems to be solved

[0004] To address the shortcomings of existing technologies, this invention provides a microporous quartz formulation and its preparation method, which exhibits good flame retardant, wear-resistant, and antibacterial effects.

[0005] (II) Technical Solution

[0006] To achieve the above objectives, the present invention provides the following technical solution: a microporous quartz formulation comprising the following weight components: 10-20 parts modified bentonite, 10-15 parts kaolin, 6-8 parts binder, 10-12 parts sodium fluorosilicate, and 20-25 parts quartz powder.

[0007] Preferably, the modified bentonite is prepared by:

[0008] (1) Add bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolving, add epichlorohydrin and sulfuric acid with a mass concentration of 40-60% to react. React at 50-80℃ for 14-20h. After the reaction is completed, distill under reduced pressure, filter, wash and dry to obtain epoxy bentonite.

[0009] (2) Add epoxy bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolution, add 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst to carry out ring-opening reaction. React at 60-80℃ for 4-6h. After the reaction, filter the solvent and wash with ethanol and distilled water to obtain intermediate product A.

[0010] (3) Add intermediate product A to toluene solvent and stir for 2-4 hours. Then add carboxylated imidazole and react at 40-60℃ for 6-8 hours. After the reaction, filter the solvent, filter, wash and dry to obtain modified bentonite.

[0011] Preferably, the mass ratio of bentonite to epichlorohydrin in (1) is 1.3-1.6:1.

[0012] Preferably, the mass ratio of epoxy bentonite, 3-hydroxyphenylphosphopropionic acid, and triethylamine catalyst in (2) is 2.1-2.5:1:0.02-0.05.

[0013] Preferably, the mass ratio of intermediate product A to carboxylated imidazole in (3) is 1.1-1.3:1.

[0014] Preferably, the preparation method of the carboxylated imidazole in (3) is as follows: 2,3-diaminobenzoic acid and methylbenzoyl chloride are added to a reactor, stirred evenly, and then triethanolamine catalyst is added. The reaction is carried out at 0-4℃ for 3-5 hours. After the reaction, the mixture is distilled under reduced pressure, filtered, washed and dried to obtain carboxylated imidazole.

[0015] Preferably, the mass ratio of the 2,3-diaminobenzoic acid, methylbenzoyl chloride, and triethanolamine catalyst is 2.1-2.5:1:0.01-0.03.

[0016] Preferably, the adhesive is any one of silicone sealant, acrylic sealant, or epoxy resin sealant.

[0017] Preferably, the preparation method of the microporous quartz formula includes the following steps: mixing modified bentonite, kaolin, binder, sodium fluorosilicate, quartz powder, SiO2, Al2O3, TiO2, BaO, MnO, MgO, and K2O according to the specified ratio, stirring at 110-120℃ for 3-5 hours to obtain a molten initial material, and then adding the molten initial material into a microporous quartz mold.

[0018] Preferably, the micropore size of the microporous quartz formulation is 1-500 micrometers.

[0019] (III) Beneficial Technical Effects

[0020] This invention involves reacting bentonite and epichlorohydrin to obtain epoxy bentonite, then reacting it with 3-hydroxyphenylphosphopropionic acid in the presence of a catalyst to obtain intermediate product A. Carboxylated imidazole is then introduced for esterification to obtain modified bentonite. Modified bentonite, kaolin, epoxy resin, sodium fluorosilicate, and quartz powder are mixed according to a specified ratio to obtain a molten initial material. This molten initial material is then added to a microporous quartz mold to obtain microporous quartz.

[0021] The microporous quartz of this invention contains a phosphorus-based flame retardant of 3-hydroxyphenylphosphonopropionic acid and an imidazole-based antibacterial agent. The two work synergistically to achieve flame retardant and antibacterial effects. At the same time, this invention has low production cost, simple operation process and high production efficiency. Detailed Implementation

[0022] Example 1

[0023] (1) Add bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolving, add epichlorohydrin and sulfuric acid with a mass concentration of 40% to react. The mass ratio of bentonite to epichlorohydrin is 1.3:1. React at 50°C for 14 hours. After the reaction is completed, distill under reduced pressure, filter, wash and dry to obtain epoxy bentonite.

[0024] (2) Epoxy bentonite was added to N,N-dimethylformamide solvent for dissolution. After dissolution, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst were added to carry out ring-opening reaction. The mass ratio of epoxy bentonite, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst was 2.1:1:0.02. The reaction was carried out at 60℃ for 4 hours. After the reaction, the solvent was filtered and the product was washed with ethanol and distilled water to obtain intermediate product A.

[0025] (3) 2,3-Diaminobenzoic acid and methylbenzoyl chloride were added to the reactor and stirred evenly. Then, triethanolamine catalyst was added. The mass ratio of 2,3-diaminobenzoic acid, methylbenzoyl chloride and triethanolamine catalyst was 2.1:1:0.01. The reaction was carried out at 0℃ for 3h. After the reaction, the mixture was distilled under reduced pressure, filtered, washed and dried to obtain carboxylated imidazole.

[0026] (4) Add intermediate product A to toluene solvent and stir for 2 hours. Then add carboxylated imidazole, wherein the mass ratio of intermediate product A to carboxylated imidazole is 1.1:1. React at 40°C for 6 hours. After the reaction, filter the solvent, filter, wash and dry to obtain modified bentonite.

[0027] (5) Mix 10 parts by weight of modified bentonite, 10 parts by weight of kaolin, 6 parts by weight of epoxy resin, 10 parts by weight of sodium fluorosilicate, 20 parts by weight of quartz powder, 60 parts by weight of SiO2, 1 part by weight of Al2O3, 2 parts by weight of TiO2, 1 part by weight of BaO, 0.2 parts by weight of MnO, 1.2 parts by weight of MgO, and 0.5 parts by weight of K2O according to the specified ratio. Stir at 110℃ for 3 hours to obtain a molten initial material. Then add the molten initial material into a microporous quartz mold.

[0028] Example 2

[0029] (1) Add bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolving, add epichlorohydrin and sulfuric acid with a mass concentration of 60% to react. The mass ratio of bentonite to epichlorohydrin is 1.6:1. React at 80℃ for 20h. After the reaction is completed, distill under reduced pressure, filter, wash and dry to obtain epoxy bentonite.

[0030] (2) Epoxy bentonite was added to N,N-dimethylformamide solvent for dissolution. After dissolution, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst were added to carry out ring-opening reaction. The mass ratio of epoxy bentonite, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst was 2.5:1:0.05. The reaction was carried out at 80℃ for 6 hours. After the reaction, the solvent was filtered and the product was washed with ethanol and distilled water to obtain intermediate product A.

[0031] (3) 2,3-Diaminobenzoic acid and methylbenzoyl chloride were added to the reactor and stirred evenly. Then, triethanolamine catalyst was added. The mass ratio of 2,3-diaminobenzoic acid, methylbenzoyl chloride and triethanolamine catalyst was 2.5:1:0.03. The reaction was carried out at 4°C for 5 hours. After the reaction, the mixture was distilled under reduced pressure, filtered, washed and dried to obtain carboxylated imidazole.

[0032] (4) Add intermediate product A to toluene solvent and stir for 4 hours. Then add carboxylated imidazole, wherein the mass ratio of intermediate product A to carboxylated imidazole is 1.3:1. React at 60°C for 8 hours. After the reaction, filter the solvent, filter, wash and dry to obtain modified bentonite.

[0033] (5) Mix 20 parts by weight of modified bentonite, 15 parts by weight of kaolin, 8 parts by weight of acrylic adhesive, 12 parts by weight of sodium fluorosilicate, 25 parts by weight of quartz powder, 80 parts by weight of SiO2, 3 parts by weight of Al2O3, 4 parts by weight of TiO2, 0.4 parts by weight of BaO2, 2.5 parts by weight of MnO, 2.5 parts by weight of MgO, and 1.5 parts by weight of K2O according to the specified ratio. Stir at 120℃ for 5 hours to obtain the initial material in the molten state. Then add the initial material in the molten state into the microporous quartz mold.

[0034] Example 3

[0035] (1) Add bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolving, add epichlorohydrin and sulfuric acid with a mass concentration of 50% to react. The mass ratio of bentonite to epichlorohydrin is 1.45:1. React at 65℃ for 17h. After the reaction is completed, distill under reduced pressure, filter, wash and dry to obtain epoxy bentonite.

[0036] (2) Epoxy bentonite was added to N,N-dimethylformamide solvent for dissolution. After dissolution, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst were added to carry out ring-opening reaction. The mass ratio of epoxy bentonite, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst was 2.3:1:0.035. The reaction was carried out at 70℃ for 5 h. After the reaction, the solvent was filtered and the product was washed with ethanol and distilled water to obtain intermediate product A.

[0037] (3) 2,3-Diaminobenzoic acid and methylbenzoyl chloride were added to the reactor and stirred evenly. Then, triethanolamine catalyst was added. The mass ratio of 2,3-diaminobenzoic acid, methylbenzoyl chloride and triethanolamine catalyst was 2.3:1:0.02. The reaction was carried out at 2℃ for 4 hours. After the reaction, the mixture was distilled under reduced pressure, filtered, washed and dried to obtain carboxylated imidazole.

[0038] (4) Add intermediate product A to toluene solvent and stir for 3 hours. Then add carboxylated imidazole, wherein the mass ratio of intermediate product A to carboxylated imidazole is 1.2:1. React at 50°C for 7 hours. After the reaction, filter the solvent, filter, wash and dry to obtain modified bentonite.

[0039] (5) Mix 15 parts by weight of modified bentonite, 12.5 parts by weight of kaolin, 7 parts by weight of silicone sealant, 11 parts by weight of sodium fluorosilicate, 22.5 parts by weight of quartz powder, 70 parts by weight of SiO2, 2 parts by weight of Al2O3, 3 parts by weight of TiO2, 1.5 parts by weight of BaO, 0.3 parts by weight of MnO, 1.85 parts by weight of MgO, and 1.0 parts by weight of K2O according to the specified ratio. Stir at 115℃ for 4 hours to obtain the initial material in the molten state. Then add the initial material in the molten state into the microporous quartz mold.

[0040] Example 4

[0041] (1) Add bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolving, add epichlorohydrin and sulfuric acid with a mass concentration of 60% to react. The mass ratio of bentonite to epichlorohydrin is 1.6:1. React at 80℃ for 20h. After the reaction is completed, distill under reduced pressure, filter, wash and dry to obtain epoxy bentonite.

[0042] (2) Epoxy bentonite was added to N,N-dimethylformamide solvent for dissolution. After dissolution, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst were added to carry out ring-opening reaction. The mass ratio of epoxy bentonite, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst was 2.5:1:0.05. The reaction was carried out at 80℃ for 6 hours. After the reaction, the solvent was filtered and the product was washed with ethanol and distilled water to obtain intermediate product A.

[0043] (3) 2,3-Diaminobenzoic acid and methylbenzoyl chloride were added to the reactor and stirred evenly. Then, triethanolamine catalyst was added. The mass ratio of 2,3-diaminobenzoic acid, methylbenzoyl chloride and triethanolamine catalyst was 2.5:1:0.03. The reaction was carried out at 4°C for 5 hours. After the reaction, the mixture was distilled under reduced pressure, filtered, washed and dried to obtain carboxylated imidazole.

[0044] (4) Add intermediate product A to toluene solvent and stir for 4 hours. Then add carboxylated imidazole, wherein the mass ratio of intermediate product A to carboxylated imidazole is 1.3:1. React at 60°C for 8 hours. After the reaction, filter the solvent, filter, wash and dry to obtain modified bentonite.

[0045] (5) Mix 15 parts by weight of modified bentonite, 12.5 parts by weight of kaolin, 7 parts by weight of silicone sealant, 11 parts by weight of sodium fluorosilicate, 22.5 parts by weight of quartz powder, 70 parts by weight of SiO2, 2 parts by weight of Al2O3, 3 parts by weight of TiO2, 1.5 parts by weight of BaO, 0.3 parts by weight of MnO, 1.85 parts by weight of MgO, and 1.0 parts by weight of K2O according to the specified ratio. Stir at 115℃ for 4 hours to obtain the initial material in the molten state. Then add the initial material in the molten state into the microporous quartz mold.

[0046] Example 5

[0047] (1) Add bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolving, add epichlorohydrin and sulfuric acid with a mass concentration of 60% to react. The mass ratio of bentonite to epichlorohydrin is 1.6:1. React at 80℃ for 20h. After the reaction is completed, distill under reduced pressure, filter, wash and dry to obtain epoxy bentonite.

[0048] (2) Epoxy bentonite was added to N,N-dimethylformamide solvent for dissolution. After dissolution, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst were added to carry out ring-opening reaction. The mass ratio of epoxy bentonite, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst was 2.5:1:0.05. The reaction was carried out at 80℃ for 6 hours. After the reaction, the solvent was filtered and the product was washed with ethanol and distilled water to obtain intermediate product A.

[0049] (3) 2,3-Diaminobenzoic acid and methylbenzoyl chloride were added to the reactor and stirred evenly. Then, triethanolamine catalyst was added. The mass ratio of 2,3-diaminobenzoic acid, methylbenzoyl chloride and triethanolamine catalyst was 2.3:1:0.02. The reaction was carried out at 2℃ for 4 hours. After the reaction, the mixture was distilled under reduced pressure, filtered, washed and dried to obtain carboxylated imidazole.

[0050] (4) Add intermediate product A to toluene solvent and stir for 3 hours. Then add carboxylated imidazole, wherein the mass ratio of intermediate product A to carboxylated imidazole is 1.2:1. React at 50°C for 7 hours. After the reaction, filter the solvent, filter, wash and dry to obtain modified bentonite.

[0051] (5) Mix 10 parts by weight of modified bentonite, 10 parts by weight of kaolin, 6 parts by weight of epoxy resin, 10 parts by weight of sodium fluorosilicate, 20 parts by weight of quartz powder, 60 parts by weight of SiO2, 1 part by weight of Al2O3, 2 parts by weight of TiO2, 1 part by weight of BaO, 0.2 parts by weight of MnO, 1.2 parts by weight of MgO, and 0.5 parts by weight of K2O according to the specified ratio. Stir at 110℃ for 3 hours to obtain a molten initial material. Then add the molten initial material into a microporous quartz mold.

[0052] Example 6

[0053] (1) Add bentonite to N,N-dimethylformamide solvent to dissolve it. After dissolving, add epichlorohydrin and sulfuric acid with a mass concentration of 50% to react. The mass ratio of bentonite to epichlorohydrin is 1.45:1. React at 65℃ for 17h. After the reaction is completed, distill under reduced pressure, filter, wash and dry to obtain epoxy bentonite.

[0054] (2) Epoxy bentonite was added to N,N-dimethylformamide solvent for dissolution. After dissolution, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst were added to carry out ring-opening reaction. The mass ratio of epoxy bentonite, 3-hydroxyphenylphosphonopropionic acid and triethylamine catalyst was 2.3:1:0.035. The reaction was carried out at 70℃ for 5 h. After the reaction, the solvent was filtered and the product was washed with ethanol and distilled water to obtain intermediate product A.

[0055] (3) 2,3-Diaminobenzoic acid and methylbenzoyl chloride were added to the reactor and stirred evenly. Then, triethanolamine catalyst was added. The mass ratio of 2,3-diaminobenzoic acid, methylbenzoyl chloride and triethanolamine catalyst was 2.1:1:0.01. The reaction was carried out at 0℃ for 3h. After the reaction, the mixture was distilled under reduced pressure, filtered, washed and dried to obtain carboxylated imidazole.

[0056] (4) Add intermediate product A to toluene solvent and stir for 2 hours. Then add carboxylated imidazole, wherein the mass ratio of intermediate product A to carboxylated imidazole is 1.1:1. React at 40°C for 6 hours. After the reaction, filter the solvent, filter, wash and dry to obtain modified bentonite.

[0057] (5) Mix 20 parts by weight of modified bentonite, 15 parts by weight of kaolin, 8 parts by weight of acrylic adhesive, 12 parts by weight of sodium fluorosilicate, 25 parts by weight of quartz powder, 80 parts by weight of SiO2, 3 parts by weight of Al2O3, 4 parts by weight of TiO2, 0.4 parts by weight of BaO2, 2.5 parts by weight of MnO, 2.5 parts by weight of MgO, and 1.5 parts by weight of K2O according to the specified ratio. Stir at 120℃ for 5 hours to obtain the initial material in the molten state. Then add the initial material in the molten state into the microporous quartz mold.

[0058] Comparative Example 1

[0059] (1) Mix 15 parts by weight of kaolin, 8 parts by weight of acrylic glue, 12 parts by weight of sodium fluorosilicate and 25 parts by weight of quartz powder according to the ratio, stir at 120°C for 5 hours to obtain the initial material in the molten state, and then add the initial material in the molten state into the microporous quartz mold.

[0060] The microporous quartz formulations prepared in Examples 1-6 and Comparative Example 1 were subjected to antibacterial tests, and the test results are shown in Table 1.

[0061] Table 1: Antibacterial test.

[0062]

[0063]

[0064] As shown in Table 1, the microporous quartz of the present invention has good antibacterial properties.

[0065] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to the specific implementations described. Clearly, 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 microporous quartz characterized in that, It comprises the following weight components: modified bentonite 10-20 parts, kaolin 10-15 parts, binder 6-8 parts, sodium fluorosilicate 10-12 parts, quartz powder 20-25 parts, SiO2 60-80 parts, Al2O3 1-3 parts, TiO2 2-4 parts, BaO 1-2 parts, MnO 0.2-0.4 parts, MgO 1.2-2.5 parts, K2O 0.5-1.5 parts; The preparation method of the modified bentonite is: (1) adding bentonite into N,N-dimethylformamide solvent for dissolution, then adding epichlorohydrin and 40-60% mass concentration sulfuric acid for reaction at 50-80℃ for 14-20h, after the reaction, distillation under reduced pressure, filtration, washing and drying to obtain epoxy bentonite; (2) adding epoxy bentonite into N,N-dimethylformamide solvent for dissolution, then adding 3-hydroxyphenyl phosphonic acid and triethylamine catalyst for ring-opening reaction at 60-80℃ for 4-6h, after the reaction, filtering the solvent, washing with ethanol and distilled water to obtain intermediate product A; (3) adding intermediate product A into toluene solvent for stirring for 2-4h, then adding carboxylated imidazole for reaction at 40-60℃ for 6-8h, after the reaction, filtering the solvent, filtration, washing and drying to obtain modified bentonite; The mass ratio of bentonite and epichlorohydrin in (1) is 1.3-1.6:1; The mass ratio of epoxy bentonite, 3-hydroxyphenyl phosphonic acid and triethylamine catalyst in (2) is 2.1-2.5:1:0.02-0.05; The mass ratio of intermediate product A and carboxylated imidazole in (3) is 1.1-1.3:1; The preparation method of carboxylated imidazole in (3) is: adding 2,3-diaminobenzoic acid and methylbenzoyl chloride into a reactor, stirring uniformly, then adding triethanolamine catalyst, reacting at 0-4℃ for 3-5h, after the reaction, distillation under reduced pressure, filtration, washing and drying to obtain carboxylated imidazole.

2. The microporous quartz of claim 1, wherein, The mass ratio of 2,3-diaminobenzoic acid, methylbenzoyl chloride and triethanolamine catalyst is 2.1-2.5:1:0.01-0.

03.

3. The microcellular quartz of claim 1 wherein, The binder is any one of silicone glue, acrylic glue and epoxy resin glue.

4. A method of producing microporous quartz as claimed in any one of claims 1 to 3, characterised in that, The preparation method of the microporous quartz comprises the following steps: mixing modified bentonite, kaolin, binder, sodium fluorosilicate, quartz powder, SiO2, Al2O3, TiO2, BaO, MnO, MgO and K2O according to the proportion, stirring at 110-120℃ for 3-5h to obtain initial material in molten state, then adding the initial material in molten state into a microporous quartz model.

Images