Composite ceramic vermiculite insulation board and preparation method thereof
By mixing and sintering components such as vermiculite, modified bentonite, and ceramic powder through a preparation method, the problems of insufficient thermal insulation, impact resistance, and antibacterial properties of composite ceramic vermiculite insulation materials are solved, and excellent thermal insulation and antibacterial effects are achieved at high temperatures.
Patent Information
- Application Number
- CN202311166057.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-11
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2043-09-11
AI Technical Summary
Existing composite ceramic vermiculite insulation materials have deficiencies in thermal insulation performance, impact resistance and antibacterial performance.
A composite ceramic vermiculite insulation board is prepared by mixing components such as vermiculite, modified bentonite, ceramic powder, silicon phosphate, fiber and water glass in proportion, stirring, molding and sintering. The interlayer exchange between modified bentonite and vermiculite is used to increase the interlayer spacing, and the synergistic effect of quaternary ammonium salt and carboxylated phenformin is combined to improve the flame retardant, heat insulation and antibacterial properties of the material.
The composite ceramic vermiculite insulation board has excellent thermal insulation, impact resistance and antibacterial properties at high temperatures, and significantly improved the stability and mechanical properties of the material.
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Figure CN117185774B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of building materials, in particular to a composite ceramic vermiculite insulation board and a preparation method thereof. Background Art
[0002] Vermiculite is a layered, magnesium-containing hydroaluminosilicate secondary metamorphic mineral with a monoclinic crystal structure. It is typically derived from the weathering or hydrothermal alteration of minerals such as biotite, phlogopite, and chlorite. Vermiculite has the characteristic of expanding when heated. This expanded form is called expanded vermiculite. Expanded vermiculite has a layered, porous structure and boasts advantages such as low bulk density, non-toxicity, high temperature resistance, low thermal conductivity, low flammability, sound insulation, and chemical stability. It is an ideal fire-resistant and thermally insulating material. Expanded vermiculite can be mixed with inorganic binders such as cement to create lightweight concrete insulation. It can also be used as a flame retardant in combination with organic materials such as phenolic resin for building wall insulation.
[0003] The document "Preparation and Application of Flame-Retardant and Heat-Insulating Vermiculite Hydrosol Finishing Agent" uses cetyltrimethylammonium bromide as an intercalating agent to intercalate vermiculite ore to prepare organic pillared vermiculite; the organic pillared vermiculite is reacted with a variety of dispersants, and the organic pillared vermiculite is treated by secondary sand milling and high-pressure micro-jet homogenization to prepare vermiculite hydrosol, which is applied to the flame retardancy and heat insulation of textiles. The present invention prepares a new type of modified bentonite, which is mixed with vermiculite, ceramic powder, silicon phosphate, fiber, water glass, and dispersant to obtain a composite ceramic vermiculite insulation board with excellent thermal insulation performance. Summary of the Invention
[0004] (1) Technical problems solved
[0005] In view of the deficiencies of the prior art, the present invention provides a composite ceramic vermiculite insulation board and a preparation method thereof, which has excellent thermal insulation performance, impact resistance, antibacterial performance, and flame retardant performance.
[0006] (2) Technical solution
[0007] To achieve the above-mentioned object, the present invention provides the following technical solution: a composite ceramic vermiculite insulation board, characterized in that it comprises the following components by weight: 100 parts of vermiculite, 20-30 parts of modified bentonite, 30-50 parts of ceramic powder, 15-25 parts of silicon phosphate, 10-12 parts of fiber, 1-5 parts of water glass, and 1-2 parts of dispersant.
[0008] Preferably, the ceramic powder is any one or more of silicon nitride, magnesium nitride, silicon carbide, magnesium oxide, and aluminum oxide.
[0009] Preferably, the fiber is any one or more of carbon fiber, glass fiber, polyester fiber, bamboo fiber, and metal fiber.
[0010] Preferably, the dispersant is any one or more of poly(2-acrylamide-2-methyl-1-propanesulfonic acid), N,N'-methylenebisacrylamide, diacetoneacrylamide, and 4,4'-methylenebis(phenylisocyanate).
[0011] Preferably, the preparation method of the composite ceramic vermiculite insulation board is as follows: vermiculite, modified bentonite, ceramic powder, silicon phosphate, fiber, water glass, and dispersant are added to a blender in a required proportion and stirred for 1-3 hours to obtain a mixture, which is then poured into a mold and pressed into a green body using a molding device, and finally placed in a sintering furnace for sintering at a temperature of 1000-1200° C. for a sintering time of 4-6 hours, naturally cooled to room temperature, cured for 4-6 days, and demolded and trimmed to obtain a composite ceramic vermiculite insulation board.
[0012] Preferably, the preparation method of the modified bentonite is:
[0013] (1) dispersing bentonite in ethanol, adding 10-20 parts by weight of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and dispersing for 20-40 minutes, heating to 60-100° C., reacting for a period of time, cooling, filtering, washing and drying to obtain amino bentonite;
[0014] (2) adding 8-10 parts by weight of amino bentonite to an ethanol solvent, heating the mixture in a water bath at 70-100° C., and adding 12-15 parts by weight of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise thereto at a constant pressure, reacting for 5-8 hours, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite;
[0015] (3) 10-12 parts by weight of carboxylated phenformin is dissolved in N,N-dimethylformamide solvent, 6-8 parts by weight of quaternary ammonium salt grafted bentonite and 1-2 parts by weight of catalyst are added thereto, and the mixture is reacted at 100-150° C. for 10-15 hours. After the reaction is completed, the mixture is transferred to anhydrous ethanol for precipitation for 3-6 hours, filtered, washed, and vacuum dried to obtain modified bentonite.
[0016] Preferably, the preparation method of the carboxylated phenformin in (3) is as follows: 12-16 parts by weight of carboxylated phenformin and 16-20 parts by weight of succinic anhydride are added to an N,N-dimethylformamide solvent, reacted at 50-80° C. for 2-3 hours, amidation reaction is carried out, filtered, washed with anhydrous ethanol, and dried to obtain the carboxylated phenformin.
[0017] Preferably, the catalyst in (3) is pyridine or hexamethyltriamine.
[0018] (3) Beneficial technical effects
[0019] The composite ceramic vermiculite heat insulation board is obtained by adding vermiculite, modified bentonite, ceramic powder, silicon phosphate, fiber, water glass and dispersant into a blender, stirring and evenly mixing to obtain a mixed material, pouring the mixed material into a mold, pressing the mixed material into a green body by using a molding device, and finally sintering the green body in a sintering furnace, naturally cooling the green body, curing, demoulding and finishing the green body.
[0020] Bentonite is grafted with 2,3-epoxypropyl hexadecyl quaternary ammonium salt, and cations between 2,3-epoxypropyl hexadecyl quaternary ammonium salt and vermiculite are exchanged. After intercalation of 2,3-epoxypropyl hexadecyl quaternary ammonium salt, the interlayer spacing of vermiculite increases, the pillaring effect is obvious, and the stability of the vermiculite system is greatly improved.
[0021] Quaternary ammonium salt is grafted onto bentonite and carboxylated phenformin is grafted onto the substrate. Carboxylated phenformin plays a curing role and cooperates with 2,3-epoxypropyl hexadecyl quaternary ammonium salt to provide flame retardant, heat insulating and antibacterial properties to the composite ceramic vermiculite insulation board. Silicon phosphate and fiber provide excellent mechanical properties to the composite ceramic vermiculite insulation board. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 This is the reaction formula for carboxylation of phenformin.
[0023] Figure 2 It is the reaction formula of modified bentonite. DETAILED DESCRIPTION
[0024] Example 1
[0025] (1) Disperse 15 g of bentonite in ethanol, add 10 g of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and disperse for 20 min, heat to 60° C., react for a period of time, cool, filter, wash and dry to obtain amino bentonite;
[0026] (2) adding 8 g of amino-bentonite to an ethanol solvent, heating the mixture in a water bath at 70° C., and adding 12 g of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise thereto at a constant pressure, reacting for 5 h, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite;
[0027] (3) adding 12-16 g of carboxylated phenformin and 16 g of succinic anhydride to an N,N-dimethylformamide solvent, reacting at 50-80° C. for 2-3 h to perform an amidation reaction, filtering, washing with anhydrous ethanol, and drying to obtain the carboxylated phenformin;
[0028] (4) 10 g of carboxylated phenformin was dissolved in N,N-dimethylformamide solvent, and 6 g of quaternary ammonium salt-grafted bentonite, 0.1 g of catalyst pyridine, and dihexamethylenetetramine were added thereto. The mixture was reacted at 100° C. for 10 h. After the reaction, the mixture was transferred to anhydrous ethanol for precipitation for 3 h, filtered, washed, and vacuum-dried to obtain modified bentonite.
[0029] (5) Add vermiculite, modified bentonite, ceramic powder magnesium nitride, silicon phosphate, carbon fiber, water glass, and dispersant poly (2-acrylamide-2-methyl-1-propanesulfonic acid) into a blender according to the required proportion and stir for 1 hour to obtain a mixture. Pour the mixture into a mold and press it into a green body using a molding device. Finally, place the mixture in a sintering furnace and sinter at a sintering temperature of 1000 ° C for 4 hours. Cool the mixture naturally to room temperature, maintain for 4 days, and then demould and trim to obtain a composite ceramic vermiculite insulation board.
[0030] Example 2
[0031] (1) Dispersing 20 g of bentonite in ethanol, adding 20 g of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and dispersing for 40 min, heating to 100° C., reacting for a period of time, cooling, filtering, washing and drying to obtain amino bentonite;
[0032] (2) adding 10 g of amino-modified bentonite to an ethanol solvent, heating the mixture in a water bath at 100° C., and adding 15 g of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise at a constant pressure, reacting for 8 h, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite;
[0033] (3) adding 16 g of carboxylated phenformin and 20 g of succinic anhydride to N,N-dimethylformamide solvent, reacting at 80° C. for 3 h to perform amidation reaction, filtering, washing with anhydrous ethanol, and drying to obtain carboxylated phenformin;
[0034] (4) 12 g of carboxylated phenformin was dissolved in N,N-dimethylformamide solvent, and 8 g of quaternary ammonium salt-grafted bentonite, 0.2 g of catalyst pyridine, and dihexamethylenetriamine were added thereto. The mixture was reacted at 150° C. for 15 h. After the reaction was completed, the mixture was transferred to anhydrous ethanol for precipitation for 6 h, filtered, washed, and vacuum-dried to obtain modified bentonite;
[0035] (5) Add vermiculite, modified bentonite, ceramic powder magnesium oxide, silicon phosphate, polyester fiber, water glass, and dispersant diacetone acrylamide into a blender in the required proportion and stir for 3 hours to obtain a mixture. Pour the mixture into a mold and press it into a green body using a molding device. Finally, place the mixture in a sintering furnace and sinter at a sintering temperature of 1200°C for 6 hours. Cool the mixture naturally to room temperature, maintain for 6 days, and then demould and trim to obtain a composite ceramic vermiculite insulation board.
[0036] Example 3
[0037] (1) Disperse 17.5 g of bentonite in ethanol, add 15 g of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and disperse for 30 min, heat to 80° C., react for a period of time, cool, filter, wash and dry to obtain amino bentonite;
[0038] (2) adding 9 g of amino-bentonite to an ethanol solvent, heating the mixture in a water bath at 85° C., and adding 13.5 g of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise at a constant pressure, reacting for 6.5 h, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite;
[0039] (3) adding 14 g of carboxylated phenformin and 18 g of succinic anhydride to N,N-dimethylformamide solvent, reacting at 65° C. for 2.5 h to carry out amidation reaction, filtering, washing with anhydrous ethanol, and drying to obtain carboxylated phenformin;
[0040] (4) 11 g of carboxylated phenformin was dissolved in N,N-dimethylformamide solvent, and 7 g of quaternary ammonium salt-grafted bentonite, 0.15 g of catalyst pyridine, and dihexamethylenetriamine were added thereto. The mixture was reacted at 125° C. for 12.5 h. After the reaction was completed, the mixture was transferred to anhydrous ethanol for precipitation for 4.5 h, filtered, washed, and vacuum-dried to obtain modified bentonite;
[0041] (5) Add vermiculite, modified bentonite, ceramic powder alumina, silicon phosphate, metal fiber, water glass, and dispersant N,N'-methylenebisacrylamide into a blender in the required proportion and stir for 2 h. Mix the mixture evenly to obtain a mixture, pour it into a mold and use a molding device to press it into a green body. Finally, put it into a sintering furnace for sintering at a temperature of 1100 ° C and a sintering time of 5 h. Cool it naturally to room temperature, maintain it for 5 days, and then demold and trim it to obtain a composite ceramic vermiculite insulation board.
[0042] Example 4
[0043] (1) Disperse 15 g of bentonite in ethanol, add 10 g of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and disperse for 20 min, heat to 60° C., react for a period of time, cool, filter, wash and dry to obtain amino bentonite;
[0044] (2) adding 8 g of amino-bentonite to an ethanol solvent, heating the mixture in a water bath at 70° C., and adding 12 g of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise thereto at a constant pressure, reacting for 5 h, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite;
[0045] (3) adding 16 g of carboxylated phenformin and 20 g of succinic anhydride to N,N-dimethylformamide solvent, reacting at 80° C. for 3 h to perform amidation reaction, filtering, washing with anhydrous ethanol, and drying to obtain carboxylated phenformin;
[0046] (4) 12 g of carboxylated phenformin was dissolved in N,N-dimethylformamide solvent, and 8 g of quaternary ammonium salt-grafted bentonite, 0.2 g of catalyst pyridine, and dihexamethylenetriamine were added thereto. The mixture was reacted at 150° C. for 15 h. After the reaction was completed, the mixture was transferred to anhydrous ethanol for precipitation for 6 h, filtered, washed, and vacuum-dried to obtain modified bentonite;
[0047] (5) Add vermiculite, modified bentonite, ceramic powder alumina, silicon phosphate, metal fiber, water glass, and dispersant N,N'-methylenebisacrylamide into a blender in the required proportion and stir for 2 h. Mix the mixture evenly to obtain a mixture, pour it into a mold and use a molding device to press it into a green body. Finally, put it into a sintering furnace for sintering at a temperature of 1100 ° C and a sintering time of 5 h. Cool it naturally to room temperature, maintain it for 5 days, and then demold and trim it to obtain a composite ceramic vermiculite insulation board.
[0048] Example 5
[0049] (1) Dispersing 20 g of bentonite in ethanol, adding 20 g of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and dispersing for 40 min, heating to 100° C., reacting for a period of time, cooling, filtering, washing and drying to obtain amino bentonite;
[0050] (2) adding 10 g of amino-modified bentonite to an ethanol solvent, heating the mixture in a water bath at 100° C., and adding 15 g of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise at a constant pressure, reacting for 8 h, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite;
[0051] (3) adding 14 g of carboxylated phenformin and 18 g of succinic anhydride to N,N-dimethylformamide solvent, reacting at 65° C. for 2.5 h to carry out amidation reaction, filtering, washing with anhydrous ethanol, and drying to obtain carboxylated phenformin;
[0052] (4) 11 g of carboxylated phenformin was dissolved in N,N-dimethylformamide solvent, and 7 g of quaternary ammonium salt-grafted bentonite, 0.15 g of catalyst pyridine, and dihexamethylenetriamine were added thereto. The mixture was reacted at 125° C. for 12.5 h. After the reaction was completed, the mixture was transferred to anhydrous ethanol for precipitation for 4.5 h, filtered, washed, and vacuum-dried to obtain modified bentonite;
[0053] (5) Add vermiculite, modified bentonite, ceramic powder magnesium nitride, silicon phosphate, carbon fiber, water glass, and dispersant poly (2-acrylamide-2-methyl-1-propanesulfonic acid) into a blender according to the required proportion and stir for 1 hour to obtain a mixture. Pour the mixture into a mold and press it into a green body using a molding device. Finally, place the mixture in a sintering furnace and sinter at a sintering temperature of 1000 ° C for 4 hours. Cool the mixture naturally to room temperature, maintain for 4 days, and then demould and trim to obtain a composite ceramic vermiculite insulation board.
[0054] Comparative Example 1
[0055] (1) Disperse 15 g of bentonite in ethanol, add 10 g of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and disperse for 20 min, heat to 60° C., react for a period of time, cool, filter, wash and dry to obtain amino bentonite;
[0056] (2) adding 8 g of amino-bentonite to an ethanol solvent, heating the mixture in a water bath at 70° C., and adding 12 g of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise thereto at a constant pressure, reacting for 5 h, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite;
[0057] (3) Add vermiculite, quaternary ammonium salt grafted bentonite, ceramic powder magnesium oxide, silicon phosphate, polyester fiber, water glass, and dispersant diacetone acrylamide into a blender according to the required proportion and stir for 3 hours to obtain a mixture. Pour the mixture into a mold and press it into a green body using a molding device. Finally, place the mixture in a sintering furnace and sinter at a sintering temperature of 1200°C for 6 hours. Cool the mixture naturally to room temperature, maintain for 6 days, and then demould and trim to obtain a composite ceramic vermiculite insulation board.
[0058] Comparative Example 2
[0059] Vermiculite, bentonite, ceramic powder alumina, silicon phosphate, metal fiber, water glass, and dispersant N,N'-methylenebisacrylamide are added to a blender in the required proportions and stirred for 2 hours to obtain a mixture. The mixture is then poured into a mold and pressed into a green body using a molding device. Finally, the green body is placed in a sintering furnace and sintered at a temperature of 1100°C for 5 hours. The green body is naturally cooled to room temperature, cured for 5 days, and demolded and trimmed to obtain a composite ceramic vermiculite insulation board.
[0060] The thermal conductivity of the composite ceramic vermiculite insulation board was tested by the flat plate method using a DRS-Ⅲ thermal conductivity tester with a test accuracy of ±5%, a test range of 0.010 W / m·k-2 W / m·k, and a maximum hot surface temperature of 1200°C. The test results are shown in Table 1.
[0061] Table 1
[0062]
[0063] As can be seen from Table 1, the thermal conductivity of the composite ceramic vermiculite insulation board of the present invention at 550°C, 750°C, and 950°C is lower in Examples 1-5 than in Comparative Examples 1-2, indicating good thermal insulation effect.
[0064] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to the specific embodiments described. Obviously, many modifications and variations are possible based on the content of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A composite ceramic vermiculite insulation board, characterized in that: The invention comprises the following components by weight: 100 parts of vermiculite, 20-30 parts of modified bentonite, 30-50 parts of ceramic powder, 15-25 parts of silicon phosphate, 10-12 parts of fiber, 1-5 parts of water glass and 1-2 parts of dispersant; The preparation method of the modified bentonite is: (1) dispersing bentonite in ethanol, adding 10-20 parts by weight of N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane and dispersing for 20-40 minutes, heating to 60-100° C., reacting for a period of time, cooling, filtering, washing and drying to obtain amino bentonite; (2) adding 8-10 parts by weight of amino bentonite to an ethanol solvent, heating the mixture in a water bath at 70-100° C., and adding 12-15 parts by weight of 2,3-epoxypropyl hexadecyl quaternary ammonium salt dropwise thereto at a constant pressure, reacting for 5-8 hours, washing with distilled water and anhydrous ethanol in sequence, filtering, concentrating, and drying to obtain quaternary ammonium salt-grafted bentonite; (3) dissolving 10-12 parts by weight of carboxylated phenformin in N,N-dimethylformamide solvent, adding 6-8 parts by weight of quaternary ammonium salt grafted bentonite and 1-2 parts by weight of catalyst thereto, reacting at 100-150° C. for 10-15 hours, and after the reaction is completed, transferring the mixture to anhydrous ethanol for precipitation for 3-6 hours, filtering, washing, and vacuum drying to obtain modified bentonite; The preparation method of the carboxylated phenformin in (3) is as follows: 12-16 parts by weight of phenformin and 16-20 parts by weight of succinic anhydride are added to an N,N-dimethylformamide solvent, reacted at 50-80° C. for 2-3 hours, amidation reaction is carried out, and the carboxylated phenformin is obtained by filtering, washing with anhydrous ethanol, and drying.
2. The composite ceramic vermiculite insulation board according to claim 1, characterized in that: The catalyst in (3) is pyridine and dihexamethylenetriamine.
3. The composite ceramic vermiculite insulation board according to claim 1, characterized in that: The ceramic powder is any one or more of silicon nitride, magnesium nitride, silicon carbide, magnesium oxide, and aluminum oxide.
4. The composite ceramic vermiculite insulation board according to claim 1, characterized in that: The fiber is any one or more of carbon fiber, glass fiber, polyester fiber, bamboo fiber, and metal fiber.
5. The composite ceramic vermiculite insulation board according to claim 1, characterized in that: The dispersant is any one or more of poly (2-acrylamide-2-methyl-1-propanesulfonic acid), N,N'-methylenebisacrylamide, diacetoneacrylamide, and 4,4'-methylenebis (phenyl isocyanate).
6. A method for preparing the composite ceramic vermiculite insulation board according to any one of claims 1 to 5, characterized in that: The preparation method of the composite ceramic vermiculite thermal insulation board comprises the following steps: adding vermiculite, modified bentonite, ceramic powder, silicon phosphate, fiber, water glass and dispersant in a required proportion into a blender, stirring for 1-3 hours, uniformly mixing to obtain a mixture, pouring the mixture into a mold, pressing the mixture into a green body using a molding device, and finally sintering the green body in a sintering furnace at a sintering temperature of 1000-1200° C. for 4-6 hours, naturally cooling the green body to room temperature, curing the green body for 4-6 days, and then demolding and trimming the green body to obtain the composite ceramic vermiculite thermal insulation board.
Citation Information
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