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Preparation method for mesoporous silica material

A technology of mesoporous silica and alkali metal silicate, applied in the direction of silica, silica, etc., can solve the problems of energy consumption, pollutant discharge, uneven distribution, long production cycle, etc., and shorten the preparation time , reduce production costs, and improve the effect of industrialization value

Active Publication Date: 2014-02-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methods listed above have more or less deficiencies, such as: large particle size and uneven distribution, complicated process, harsh preparation conditions, long production cycle, etc. Among them, although CN1618736A adopts a relatively mild preparation Conditions, but the concentration of raw material silicate in the system is too low (mass concentration is not more than 10%), large-scale production will inevitably lead to excessive equipment volume, increase production costs, energy consumption and pollutant emissions, etc.

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  • Preparation method for mesoporous silica material
  • Preparation method for mesoporous silica material

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preparation example Construction

[0011] First, the present invention provides a method for preparing a mesoporous silica material, wherein the method includes: (1) contacting an aqueous solution of an alkali metal silicate with a weakly acidic cation exchange resin under hydrolysis conditions to obtain a silica sol; (2) In the presence of a template agent, the obtained silica sol is subjected to microwave irradiation to produce mesoporous silica raw powder; (3) The product obtained by microwave irradiation is subjected to solid-liquid separation to remove the obtained mesoporous silica Templating agent in raw powder.

[0012] In the method of the present invention, the weakly acidic cation exchange resin can exchange metal cations such as alkali metal cations in the ionic state in the aqueous solution for H by contacting with an aqueous solution of an alkali metal silicate. + .

[0013] In the method of the present invention, theoretically as long as the amount of the weakly acidic cation exchange resin can ...

Embodiment 1

[0035] (1) Dissolve 260g of sodium silicate with a modulus of 3.6 in 140g of deionized water at 90°C to obtain an aqueous solution of sodium silicate. Under stirring, add 200g of weakly acidic cation exchange resin to the aqueous solution of sodium silicate in 16 times D113 (manufactured by Tianjin Nanda Resin Technology Co., Ltd., with a total exchange capacity of 10mmol / g), add the weakly acidic cation exchange resin for the last time and then continue to stir for 5 minutes (at this time, it is 80 minutes before adding the weakly acidic cation exchange resin), The weakly acidic cation exchange resin is removed by filtration to obtain a silica sol, and the particle diameter of the colloidal particles in the silica sol measured by a laser particle size analyzer is 15-20 nm.

[0036] (2) Add 13g of cetyltrimethylammonium bromide to the silica sol obtained in step (1) under stirring, and put the mixture into a microwave oven. Set the power of the microwave oven to 250W and the ti...

Embodiment 2

[0040] (1) Dissolve 200g of sodium silicate with a modulus of 3.4 in 240g of deionized water at 75°C to obtain an aqueous solution of sodium silicate. Under stirring, add 210g of weakly acidic cation exchange resin to the aqueous solution of sodium silicate for 10 times D114 (manufactured by Tianjin Nanda Resin Technology Co., Ltd., with a total exchange capacity of 8mmol / g), add the weakly acidic cation exchange resin for the last time and then continue to stir for 10 minutes (at this time, it is 70 minutes before adding the weakly acidic cation exchange resin), The weakly acidic cation exchange resin is removed by filtration to obtain a silica sol, and the particle diameter of the colloidal particles in the silica sol measured by a laser particle size analyzer is 15-25 nm.

[0041] (2) Under stirring, add 5g of P123 to the silica sol obtained in step (1), and put the mixture into a microwave oven at the same time, set the power of the microwave oven to 400W and the time to 0....

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Abstract

The invention provides a preparation method for a mesoporous silica material. The method comprises the following steps: (1) contacting an aqueous solution of an alkali metal silicate with a weakly acidic cation-exchange resin under a hydrolysis condition so as to obtain a silica sol; (2) in the presence of a template, subjecting the obtained silica sol to microwave irradiation so as to produce raw mesoporous silica powder; and (3) subjecting a product obtained in microwave irradiation to solid-liquid separation so as to remove the template in the obtained raw mesoporous silica powder. The method provided by the invention has high preparation efficiency and a good industrialization value. The mesoporous silica material prepared by using the method has a uniform particle size.

Description

technical field [0001] The invention relates to a method for preparing a mesoporous silicon dioxide material with high preparation efficiency. Background technique [0002] Nano-sized silica materials have been widely used in industrial production as important fillers and additives in the fields of oil recovery, rubber, plastics, medicine, cosmetics and coatings, and can play the role of reinforcement, thickening and anti-aging . The size distribution of nanometer-sized silica materials has a great influence on material applications. [0003] At present, the methods for synthesizing silica materials are mainly: after hydrolysis and condensation of alkali metal silicates or silicates under acidic or alkaline conditions, with or without the presence of surfactants (and templates in some cases) , obtained by drying and roasting. For example: (1) ZL95102373.X discloses that silicate is hydrolyzed and condensed at pH 3-4 in the presence of hexadecylamine at 80-90°C for 8-12 ho...

Claims

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Application Information

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IPC IPC(8): C01B33/18
Inventor 张杰杜昕李传清徐林解希铭于国柱姜科段海东刘冬梅苗玉红
Owner CHINA PETROLEUM & CHEM CORP
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