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Method for preparing mesoporous silica material by hydroxyethyl cellulose serving as template

A technology of hydroxyethyl cellulose and mesoporous silica, applied in the direction of silica, silicon oxide, etc., can solve the problem of increasing production costs, energy consumption and pollutant discharge, limiting the application of mesoporous silica materials, increasing Difficulty in the post-processing process, etc., to achieve the effects of high efficiency and non-toxicity in the preparation process, mild and controllable preparation conditions, and concentrated pore size distribution

Active Publication Date: 2019-04-05
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In CN1348920A, use inorganic silicon material as silicon source, colloidal particle and block copolymer as template, prepared mesoporous silica material in alcoholic solvent, but this reaction sol-gel process speed is slow, and solvent evaporates in large quantities Finally, the shrinkage rate of the material is very large, resulting in many cracks in the material, and the operation steps are cumbersome
[0004] In CN1605562A, the oil-soluble silicon source is used, and the emulsion formed by mixing an aqueous electrolyte solution, a nonionic surfactant and anionic surfactant as a template has prepared a mesoporous silica material, but the reaction is introduced while the electrolyte , also introduces a large number of impurities, which increases the difficulty of the post-processing process
Although the preparation conditions of this invention are relatively mild, the concentration of raw material silicate in the system is too low (mass concentration is not more than 10%), which will inevitably lead to excessive equipment volume during large-scale production, increasing production costs, energy consumption and pollutant emissions Wait
[0006] At present, the main silicon source for synthesizing mesoporous silicon materials is silicate, most of which is orthoethyl silicate (TEOS). The synthesis cost of this kind of silicon source is relatively high, which limits the industrial application of mesoporous silica materials.

Method used

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  • Method for preparing mesoporous silica material by hydroxyethyl cellulose serving as template
  • Method for preparing mesoporous silica material by hydroxyethyl cellulose serving as template
  • Method for preparing mesoporous silica material by hydroxyethyl cellulose serving as template

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Embodiment 1

[0027] A method for preparing a mesoporous silica material using hydroxyethyl cellulose as a template, specifically comprising the following steps:

[0028] 1) 10g (0.035mol) Na 2 SiO 3 9H 2 O was dissolved in 50mL of water, and stirred to make it reach a dissolution equilibrium to obtain an aqueous alkali metal silicate solution;

[0029] 2) Add 2g of hydroxyethyl cellulose (DS=3, MS=6, molar mass: 736.7g / mol) with a viscosity of 5000-6400mpa·s into 300mL of water, heat in an oil bath at 80°C and fully stir to dissolve to obtain hydroxyethyl cellulose Cellulose aqueous solution;

[0030] 3) Slowly add the aqueous alkali metal silicate solution obtained in the above step 1) into the reaction flask containing the aqueous solution of hydroxyethyl cellulose obtained in step 2), stir well until a clear and translucent solution is obtained, and use 15-20% H 2 SO 4 Adjust the pH value of the reaction system to 6 with the solution, let it stand for 24 hours to obtain the reactio...

Embodiment 2

[0034] A method for preparing a mesoporous silica material using hydroxyethyl cellulose as a template, specifically comprising the following steps:

[0035] 1) Add 5g Na 2 SiO 3 9H 2 O (0.018mol) was dissolved in 30mL of water, stirred to make it reach a dissolution equilibrium to obtain an aqueous alkali metal silicate solution;

[0036] 2) Add 1.5 g of hydroxyethyl cellulose with a viscosity of 3400 to 5000 mpa·s into 220 mL of water, heat in an oil bath at 80°C, stir and dissolve to obtain an aqueous solution of hydroxyethyl cellulose;

[0037]3) Slowly add the alkali metal silicate aqueous solution obtained above into the reaction flask equipped with the aqueous hydroxyethyl cellulose solution obtained in step 2), stir fully until a clear and translucent solution is obtained, and adjust the reaction system with 2mol / L HCl solution When the pH value reaches 6, let it stand still for 24 hours to obtain the reaction solution. Centrifuge the reaction solution after standing...

Embodiment 3

[0040] A method for preparing a mesoporous silica material using hydroxyethyl cellulose as a template, specifically comprising the following steps:

[0041] 1) Add 5g Na 2 SiO 3 9H 2 O (0.018mol) was dissolved in 30mL of water, stirred to make it reach a dissolution equilibrium to obtain an aqueous alkali metal silicate solution;

[0042] 2) Add 1.5 g of hydroxyethyl cellulose with a viscosity of 2600 to 3300 mpa s into 165 mL of water, heat in an oil bath at 80°C, stir and dissolve to obtain an aqueous solution of hydroxyethyl cellulose;

[0043] 3) Slowly add the aqueous alkali metal silicate solution obtained in the above step 1) into the reaction flask containing the aqueous solution of hydroxyethyl cellulose obtained in step 2), stir well until a clear and translucent solution is obtained, and use 15-20% H 2 SO 4 Adjust the pH value of the reaction system to 5 with the solution, let it stand for 24 hours to obtain the reaction solution, centrifuge the reaction solutio...

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Abstract

The invention relates to a method for preparing a mesoporous silica material by hydroxyethyl cellulose serving as a template. The method particularly includes the steps: 1) adding hydroxyethyl cellulose into water, heating, stirring and dissolving to obtain hydroxyethyl cellulose water solution, slowly adding alkali metal silicate water solution into the hydroxyethyl cellulose water solution to uniformly mixing mixture, sufficiently stirring the mixture until clear and bright solution is acquired, adjusting a pH (potential of hydrogen) of a reaction system to reach 5-6 by acid solution, and standing for 1-24 hours to obtain reaction liquid; 2) centrifuging the reaction liquid, drying and collecting to obtain a solid matter, and calcining the solid matter to obtain the mesoporous silica material. According to the method, a non-ionic surface active agent serves as a hydroxyethyl cellulose template agent to assemble mesoporous silica, unformed mesoporous silica material is synthesized byan unconventional acid hydrolysis process, and the raw materials are rich, renewable and good in biocompatibility, and the method is simple in synthetic process, mild and controllable in preparation condition and simple, efficient and nontoxic in preparation process.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and in particular relates to a method for synthesizing a mesoporous silica material through a sol-gel method by using inorganic silicate and cellulose nonionic surfactant. Background technique [0002] Mesoporous silicon material has a narrow pore size distribution range, adjustable size, stable skeleton, and regular and orderly structure. It is a good adsorbent carrier, especially its surface is easy to functionalize, and can be used to prepare mesoporous adsorbents with different surface properties. The introduction of specific functional objects makes mesoporous silicon materials a new material with different functionalities to meet the needs of different use environments. In addition, these materials are easy to separate from the mother liquor after adsorption. Through pickling, roasting or extraction and other processes, pollutants can be recycled and adsorbents can be regenerate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/14
CPCC01B33/14C01P2004/03C01P2006/14C01P2006/12C01P2006/17C01P2006/16
Inventor 吕仁亮张成夏婷李泽钦王存文罗晓刚陈苏芳覃远航汪铁林王为国
Owner WUHAN INSTITUTE OF TECHNOLOGY
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