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Method for preparing silicon oxide-based aerogel ball with controllable particle size through continuous liquid phase polymerization

A technology based on liquid phase polymerization and wet gel balls, which is applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problems of cumbersome ball drop method, difficult quantitative production, time-consuming and labor-consuming, etc. Simple, easy to use, good effect

Pending Publication Date: 2022-04-29
NANJING UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent with the application number CN202010651923.9 discloses a method for preparing spherical SiO 2 A method for airgel materials, which uses water glass as a silicon source, and prepares spherical SiO by the ball drop method 2 Airgel materials, but the ball drop method has the defects of cumbersome process, time-consuming and labor-intensive, it is difficult to quantify production, and it is difficult to truly realize industrialization

Method used

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  • Method for preparing silicon oxide-based aerogel ball with controllable particle size through continuous liquid phase polymerization
  • Method for preparing silicon oxide-based aerogel ball with controllable particle size through continuous liquid phase polymerization
  • Method for preparing silicon oxide-based aerogel ball with controllable particle size through continuous liquid phase polymerization

Examples

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Effect test

example 1

[0028] At room temperature, dissolve 0.1 mol of methyltrimethoxysilane, 0.1 mol of o-phthalaldehyde, and 0.2 mol of silane coupling agent KH550 in 16 mol of methanol, mix well and add 8 mol of acetic acid aqueous solution with a concentration of 1 mmol / L Stirring was continued, and ultrasonication was performed at 50° C. for 60 minutes to carry out a prepolymerization reaction to obtain a silicon oxide-based reaction solution with a pH of 5. At 50°C, 10ml of urea solution was dispersed in 120ml of water-based silicone oil, and mixed evenly to obtain a coagulation bath with a pH of 8. At 70°C, under the condition of rotating speed of 10000rpm, the reaction solution was mixed with the coagulation bath, kept at 70°C for 30 minutes, separated and filtered, and washed with deionized water at 60°C for 8 minutes to obtain silica-based wet gel balls. After methanol replacement and spray drying, silicon oxide-based airgel spheres with controllable particle size are obtained. The avera...

example 2

[0033] At room temperature, dissolve 0.2mol of methyltriethoxysilane, 0.4mol of isophthalaldehyde, and 0.2mol of silane coupling agent KH560 in 16mol of ethanol, mix well and add 8mol of oxalic acid with a concentration of 2mmol / L The aqueous solution continued to stir, and was ultrasonicated at 60° C. for 50 minutes to carry out a prepolymerization reaction to obtain a silicon oxide-based reaction solution with a pH of 4. At 25°C, disperse 10ml of ammonia water in 100ml of methyl silicone oil, and mix evenly to obtain a coagulation bath with a pH of 10. At 80°C, the reaction solution was mixed with a coagulation bath at a rotational speed of 100 rpm, kept at 80°C for 20 minutes, separated and filtered, washed with deionized water at 70°C for 6 minutes to obtain silica-based wet gel balls. After replacing with n-hexane and drying under normal pressure, the silica-based airgel spheres with controllable particle size are obtained. The average particle size of silica-based airge...

example 3

[0035] At room temperature, dissolve 1 mol of trimethylmethoxysilane, 5 mol of terephthalaldehyde, and 5 mol of silane coupling agent KH570 in 20 mol of isopropanol, mix well and add 10 mol of carbonic acid aqueous solution with a concentration of 5 mmol / L Stirring was continued, followed by water heating at 100° C. for 10 minutes to carry out prepolymerization to obtain a silicon oxide-based reaction solution with a pH of 6. At 90°C, disperse 30ml of NaOH solution in 180ml of corn oil, and mix evenly to obtain a coagulation bath with a pH of 12. At 80°C, under the condition of rotating speed of 1000rpm, the reaction solution was mixed with the coagulation bath, kept at 80°C for 10 minutes, separated and filtered, and washed with deionized water at 70°C for 6 minutes to obtain silica-based wet gel balls. After ethanol replacement and vacuum drying, silica-based airgel spheres with controllable particle size were obtained. The average particle size of silica-based airgel balls...

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Abstract

The invention relates to a method for preparing a silicon oxide-based aerogel ball with a controllable particle size through continuous liquid phase polymerization. The preparation method comprises the following steps: adding a silicon source, aldehyde, a silane coupling agent and an organic / inorganic solvent serving as reaction solutions into an alkaline coagulating bath, preparing silicon oxide-based wet gel balls through a continuous liquid phase polymerization method and a sol-gel method, and carrying out solvent replacement and drying treatment to obtain the silicon oxide-based aerogel balls with controllable particle sizes. According to the method, the adopted procedures are simple, raw materials are easy to obtain, the obtained aerogel balls are controllable in particle size and excellent in performance, and continuous large-scale industrial production can be achieved. The prepared silicon oxide-based aerogel ball has typical application in filler with heat insulation, heat preservation, purification and adsorption functions.

Description

technical field [0001] The invention belongs to the field of preparation of new materials, and relates to a method for preparing silicon oxide-based airgel balls with controllable particle diameters through continuous liquid phase polymerization. Background technique [0002] Airgel is a nanoporous material with a three-dimensional nano-network structure. It has structural characteristics such as low density, high specific surface area, and high porosity, endowing it with excellent functions such as heat insulation, adsorption, catalysis, and drug loading, so it is widely used. It is used in the fields of aerospace military industry, building insulation, transportation, daily heat preservation and environmental purification. Current SiO 2 Although aerogels have been industrialized, commercialized and applied in engineering, there are still international problems that need to be solved urgently, such as high cost, poor mechanical properties (specifically manifested as high b...

Claims

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Application Information

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IPC IPC(8): C01B33/158
CPCC01B33/1585C01P2004/32C01P2004/61C01P2004/60C01P2006/11C01P2006/12C01P2006/32C01P2006/90C01P2006/17C01P2002/82
Inventor 赵志扬朱昆萌孔勇任建沈晓冬
Owner NANJING UNIV OF TECH