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Silicon dioxide composite film with disilane precursor as well as preparation method and application of silicon dioxide composite film

A technology of silicon dioxide and composite membrane, applied in the field of composite membrane, can solve the problems of low flux and poor hydrothermal stability of silicon dioxide membrane, and achieve the effects of easy batching, stable network structure and increased flux

Pending Publication Date: 2021-05-28
NANTONG ACETIC ACID CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The silicon dioxide membranes in the prior art are mostly used for gas separation and should not be used in the field of pervaporation because of their poor hydrothermal stability; a few silicon dioxide membranes used in the field of pervaporation have low flux

Method used

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  • Silicon dioxide composite film with disilane precursor as well as preparation method and application of silicon dioxide composite film
  • Silicon dioxide composite film with disilane precursor as well as preparation method and application of silicon dioxide composite film
  • Silicon dioxide composite film with disilane precursor as well as preparation method and application of silicon dioxide composite film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056]The preparation method is performed in step (1) to step (3), and each step is explained.

[0057]Step (1): Preparation of large, small particle sol and precursor sol

[0058]1) The preparation process of large and small particle sol is as follows:

[0059]Process (1-1): 3 g of orthosilicate was added to 110 g of ethanol solution, and 1 g of deionized water and 3 g of concentrated hydrochloric acid were oscillated at room temperature for 3 h after mixing.

[0060]Process (1-2): After the ethane hydrolysis is hydrolyzed, 6 g of ni-niol zirconium continues to oscillate 12h;

[0061]Process (1-3): The above solution was transferred into a three flask to add a large amount of deionized water to 500 mL and an appropriate amount of hydrochloric acid was added to 2 or less, boiled for 8 h, and the total volume of the solution was maintained at 500 mL;

[0062]Procedure (1-4): Cool until the reaction was completed to room temperature. The prepared adhesive sol was divided into two alcohols, and two alum...

Embodiment 2

[0080]In this example, the film tube was soaked in a hydrochloride prepared to PH = 2 (± 0.2), and the film tube was removed, and the diaphragm is taken out, and the test is removed, and the test is subjected to the acid solution. , Repeat operation until the end of the immersion is 15 days. The operating temperature of the permeable vaporization performance was maintained at 75 ° C, and the aqueous content of the isopropyl alcohol solution to be separated was 15% by weight.

[0081]Figure 4 Under the hydrochloric acid treatment of the double silane precursor, the hydrochloric acid solution of pH = 2, the effect of different treatment time on its permeation vaporization performance. As can be seen from the figure, the flux of the membrane tube has gradually stabilized the change in the decline as the acid immersion time, and finally stabilizes the water content, and the water content of the permeate is also a slow increase. trend. The prepared silica composite membrane can remain stabl...

Embodiment 3

[0083]In this example, the monosilane (Btese) silica composite film is prepared, and the silane silica composite film in Example 1 is subjected to permeability.

[0084]The preparation step (1) to step (3) of this Example 3 is only that the difference from the first embodiment is only that

[0085]1) Preparation process of precursor sol: Process (1-5): Add Btese to anhydrous ethanol and add mixed solution of nitric acid and deionized water therein, and quench the reaction after reaction in an ice bath. Mono-transparent Btese sol; process (1-5) each substance molar ratio is: Btese: EtoH: HNO3: H2O = 1: 10: 0.1: 6.

[0086]Others are all identical, no longer educated.

[0087]In this Example 3, 5 sets of silica composite film tubes were prepared under the same conditions, respectively, respectively, made of silane (Btese / MTES) and single silane (Btese) as the precursor substance by sol gel method.

[0088]Figure 5 The permeation vaporification properties of the silica composite film prepared by do...

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Abstract

The invention provides a silicon dioxide composite film taking disilane as a precursor substance. According to the invention, alpha-aluminum oxide is taken as a support body, and a bottom layer and a top layer sequentially coat the support body; the bottom layer is obtained by repeatedly the surface of the support body to coating and calcining of large and small aluminum oxide particle sol in sequence; and the top layer is prepared by mixing two silane precursors and an acid catalyst according to a ratio of 1: (0.1-0.5), generating precursor sol under an ice bath condition, and repeatedly subjecting the support body to coating and calcining of the precursor sol. The film has good hydrothermal stability. Compared with a silicon dioxide composite film prepared from a monosilane precursor, the composite film has higher permeation flux.

Description

Technical field[0001]The present invention relates to the field of composite membranes, and more particularly to a silica composite film, a preparation method thereof and an application thereof.Background technique[0002]Permeation vaporization is a green energy-saving membrane process for the separation of liquid molecular mixture, combining membrane permeation and evaporation, and is applied to selective separation of liquid molecular mixture. The current permeation vaporization plays an increasingly important role in various film technologies. However, in practice applications in common molecular sieve membranes, the non-acid resistance of molecular sieve membranes limits its development. The silica film is excellent in acid resistance, with high research value, has a broad application prospect.[0003]The prior art silicon dioxide film is mostly used in gas separation, and is not applied to the field of permeation vaporization because of poor water and thermal stability; a small am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00B01D69/12B01D69/10B01D69/02B01D61/36
CPCB01D71/027B01D71/025B01D67/0039B01D69/105B01D69/12B01D69/02B01D61/362B01D2325/22B01D2325/30
Inventor 庆九俞新南朱小刚刘芳周志辉
Owner NANTONG ACETIC ACID CHEM
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