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Preparation method and application of a silica-zirconia composite sol with controllable particle size

A technology of silica and composite sol, which is applied in the field of preparation of silica-zirconia composite sol, which can solve the problems of poor hydrothermal stability of sol film and difficulty in controlling the particle size of sol

Active Publication Date: 2017-06-06
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For existing SiO 2 Due to the poor hydrothermal stability of the sol film and the defect that the particle size of the sol is difficult to control in the preparation process, the present invention provides a relatively simple and economical method for preparing a silica-zirconia composite sol with controllable particle size. A zirconium alkoxide reagent was introduced into the oxysilane to prepare a composite sol, which was fired into a film by hot coating method under high temperature conditions. Due to the introduction of the zirconium alkoxide reagent, the film showed good hydrothermal stability

Method used

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  • Preparation method and application of a silica-zirconia composite sol with controllable particle size
  • Preparation method and application of a silica-zirconia composite sol with controllable particle size
  • Preparation method and application of a silica-zirconia composite sol with controllable particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) 5.0g tetramethoxysilane (Si(OCH 3 ) 4 ), 64.50g of absolute ethanol were mixed and stirred for 10min, then 3.6g of deionized water, 32.249g of CH 3 CH 2 OH, 37% concentrated hydrochloric acid solution containing 0.1823g HCl, continue to stir for 30 minutes, so that the mixed solution is partially hydrolyzed and polymerized;

[0023] (2) Continue to add 73.71g of CH to the mixed system obtained in step (1) 3 CH 2 OH, 11.51g of zirconium ethoxide (Zr(OC 2 h 5 ) 4 ), 0.36g of H 2 0. Contain 37% concentrated hydrochloric acid solution of 0.182gHCl, continue to stir for 10h, at this moment, the hydrolysis-polymerization reaction takes place further in the mixed solution;

[0024] (3) Add 36.86g of CH 3 CH 2 OH, 0.72g of H 2 O, the 37% concentrated hydrochloric acid solution that contains 0.182gHCl joins in the mixed solution that step (2) obtains, and stirs 30min;

[0025] (4) Add 37% concentrated hydrochloric acid solution containing 4.01gHCl to the system o...

Embodiment 2

[0028] (1) 6.67g of tetraethoxysilane (Si(OC 2 h 5 ) 4 ), 69.105g of absolute ethanol were mixed and stirred for 10min, and then 4.14g of deionized water and 36.87g of CH 3 CH 2 OH, 37% concentrated hydrochloric acid solution containing 0.219g HCl, continue to stir for 30 minutes, so that the mixed solution is partially hydrolyzed and polymerized;

[0029] (2) Continue to add 78.32g of CH to the mixed system obtained in step (1) 3 CH 2 OH, 15.35g of zirconium n-butoxide (ZrO 4 C 16 h 36 ), 0.414g of H 2 0. Contain 37% concentrated hydrochloric acid solution of 0.219gHCl, continue to stir for 10h, at this moment, the hydrolysis-polymerization reaction takes place further in the mixed solution;

[0030] (3) Add 39.16g of CH 3 CH2 OH, 0.81g of H 2 O, the 37% concentrated hydrochloric acid solution that contains 0.219gHCl joins in the mixed solution that step (2) obtains, and stirs 30min;

[0031] (4) Add 37% concentrated hydrochloric acid solution containing 4.38gHCl ...

Embodiment 3

[0034] (1) 8.33g of tetra-n-butoxysilane (Si(OC 4 h 9 ) 4 ), 73.71g of absolute ethanol were mixed and stirred for 10min, and then 4.5g of deionized water and 41.46g of CH 3 CH 2 OH, 37% concentrated hydrochloric acid solution containing 0.255g HCl, continue to stir for 30min, so that the mixed solution is partially hydrolyzed and polymerized;

[0035] (2) Continue to add 82.93g of CH to the mixed system obtained in step (1) 3 CH 2 OH, 15.35g of zirconium tert-butoxide (ZrO 4 C 16 h 36 ), 0.45g of H 2 0. Contain 37% concentrated hydrochloric acid solution of 0.255gHCl, continue to stir for 10h, at this moment, the hydrolysis-polymerization reaction takes place further in the mixed solution;

[0036] (3) Add 41.46g of CH 3 CH 2 OH, 0.9g of H 2 O, the 37% concentrated hydrochloric acid solution that contains 0.255gHCl joins in the mixed solution that step (2) obtains, and stirs 30min;

[0037] (4) Add 37% concentrated hydrochloric acid solution that contains 4.74gHC...

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Abstract

The invention belongs to the field of inorganic membrane material preparation, and especially relates to a preparation method and an application of a silica-zirconia composite sol. The preparation method comprises the following steps: introducing a zirconium alkoxide reagent to alkoxy silane, and discontinuously supplementing water to a system in the heating boiling soil preparation process to make the volume of the obtained solution unchanged in order to prepare the composite sol. The particle size of the composite sol is controllable, and the average particle size of the sol is about 100nm; and the sol is sintered under high temperature conditions through adopting a heat coating process to form a membrane, and introduction of the zirconium alkoxide reagent makes the membrane have good hydrothermal stability.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic membrane materials, and in particular relates to a preparation method and application of a silica-zirconia composite sol. Background technique [0002] In recent years, membrane separation technology has been at the forefront of separation technology. Due to the characteristics of energy saving, high efficiency, environmental protection, easy control, and simple operation, it has developed rapidly in the past 20 years. As an important membrane material, inorganic membrane has many excellent properties, and its application fields are becoming more and more extensive. [0003] SiO 2 Membrane, as an important inorganic membrane material, has a very broad application prospect, but it is difficult to control the particle size of the prepared sol and the poor hydrothermal stability of the prepared membrane limits its further application. Contents of the invention [0004] For existing SiO 2...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/85
Inventor 徐荣郭猛钟璟张琪
Owner CHANGZHOU UNIV