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Preparation method of titanium oxide carrying hydrophobic silicon dioxide composite film

A silicon dioxide and hydrophobic technology, applied in the field of composite membranes, can solve the problems of incompatibility and low permeation rate, and achieve the effects of low cost, increased permeation rate, and improved water vapor stability

Inactive Publication Date: 2019-09-06
XI'AN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To this end, many researchers at home and abroad are committed to improving the SiO 2 The study of membrane hydrophobicity, but often can not take into account the H 2 Permeation rate and H 2 / CO 2 Two indicators of separation efficiency, membranes with good gas selectivity tend to have lower permeation rates

Method used

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  • Preparation method of titanium oxide carrying hydrophobic silicon dioxide composite film
  • Preparation method of titanium oxide carrying hydrophobic silicon dioxide composite film

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A kind of TiO 2 Loaded hydrophobic SiO 2 The preparation method of composite film is specifically implemented according to the following steps:

[0045] Step 1, take the following components respectively by mass percentage:

[0046] (1) Orthoethyl silicate (TEOS): Methyltriethoxysilane (MTES): Water: HNO 3 (Concentration is 0.8mol / L)=1:0.80:7.7:7.2:0.086.

[0047] (2) Butyl titanate (TBOT): absolute ethanol (EtOH): water: HNO 3 (Concentration is 1.8mol / L)=1:50:4:0.2.

[0048] Step 2. Add ethyl orthosilicate, methyltriethoxysilane, and absolute ethanol weighed in step 1 (1) into a container placed in an ice-water bath, stir for 40 minutes, and mix them uniformly to obtain a mixed Solution 1, the water and HNO weighed in step 1(1) 3 Mix to obtain diluted HNO 3 solution, mix solution 1 with diluted HNO 3 Mix the solutions to obtain a mixed solution 2, heat the mixed solution 2 to 50°C while stirring, reflux for 2 hours with a condenser tube, and naturally cool to roo...

Embodiment 2

[0055] A kind of TiO 2 Loaded hydrophobic SiO 2 The preparation method of composite film is specifically implemented according to the following steps:

[0056] Step 1, take the following components respectively by molar ratio:

[0057] (1) Orthoethyl silicate (TEOS): dimethyldiethoxysilane (TMEO): absolute ethanol (EtOH): water: HNO 3 (Concentration is 0.9mol / L)=1:0.9:8.5:8.6:0.090.

[0058] (2) Butyl titanate (TBOT): absolute ethanol (EtOH): water: HNO 3 (Concentration is 2.0mol / L)=1:55:3.3:0.23.

[0059] Step 2. Add ethyl orthosilicate, dimethyldiethoxysilane, and absolute ethanol weighed in step 1 (1) into a container placed in an ice-water bath, stir for 45 minutes, and mix evenly to obtain Mix solution 1, the water and HNO weighed in step 1(1) 3 Mix to obtain diluted HNO 3 solution, mix solution 1 with diluted HNO 3 The solutions were mixed to obtain a mixed solution 2, and the mixed solution 2 was heated to 55°C while stirring, refluxed with a condenser for 2.5h,...

Embodiment 3

[0066] A kind of TiO 2 Loaded hydrophobic SiO 2 The preparation method of composite film is specifically implemented according to the following steps:

[0067] Step 1, take the following components respectively by molar ratio:

[0068] (1) Orthoethyl silicate (TEOS): trimethylethoxysilane (DMDES): absolute ethanol (EtOH): water: HNO 3 (Concentration is 1.0mol / L)=1:1.0:11.0:9.5:0.095.

[0069] (2) Butyl titanate (TBOT): absolute ethanol (EtOH): water: HNO 3 (Concentration is 2.2mol / L)=1:60:3.5:0.25.

[0070] Step 2. Add ethyl orthosilicate, trimethylethoxysilane, and absolute ethanol weighed in step 1 (1) into a container placed in an ice-water bath, stir for 50 minutes, and mix them uniformly to obtain a mixed Solution 1, the water and HNO weighed in step 1(1) 3 Mix to obtain diluted HNO 3 solution, mix solution 1 with diluted HNO 3 The solutions were mixed to obtain a mixed solution 2, and the mixed solution 2 was heated to 60°C while stirring, refluxed with a condens...

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Abstract

The invention discloses a preparation method of a titanium oxide carrying hydrophobic silicon dioxide composite film. Ethyl orthosilicate, a hydrophobic modifying agent and absolute ethyl alcohol aremixed in an ice-water bath and then are mixed with a diluted HNO3 solution, and the mixture is heated, condensed and then cooled to room temperature to obtain methylated modified SiO2 sol; butyl titanate and absolute ethyl alcohol are mixed and then are mixed with a diluted HNO3 solution, and the mixture is heated, condensed and then cooled to room temperature to obtain TiO2 sol; the SiO2 sol andthe TiO2 sol are mixed to obtain original TiO2-SiO2 sol, the original TiO2-SiO2 sol is diluted, porous ceramic serves as a support, an impregnation method is adopted to coat the surface of the supportwith diluted TiO2-SiO2 sol, and after drying at room temperature, the titanium oxide carrying hydrophobic silicon dioxide composite film is obtained through calcining. By adopting the preparation method, on the basis of improving the water vapor stability of a normal SiO2 composite film, the permeation rate of H2 and an H2 / CO2 separation factor are increased, and the cost is saved.

Description

technical field [0001] The invention belongs to the technical field of composite membranes and relates to a TiO 2 Loaded hydrophobic SiO 2 Preparation method of composite membrane. Background technique [0002] Coal gasification hydrogen production is currently proposed internationally to reduce the greenhouse gas CO 2 An effective method of emission, the hydrogen production process of coal gasification needs to convert CO 2 Separated and then transported to a designated location for storage, while the separated H 2 It is a kind of clean energy with great development prospects, therefore, from the mixed gas (H 2 +CO 2 ) is an important and key link to obtain high-purity hydrogen. [0003] Membrane separation technology is to purify H 2 effective method. In recent years, for H 2 The research on inorganic membranes for separation mainly focuses on palladium (Pd) and its alloy membranes, non-palladium alloy membranes, zeolite membranes, molecular sieve carbon membranes...

Claims

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Application Information

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IPC IPC(8): B01D67/00B01D69/10B01D69/12B01D71/02C01B3/50
CPCB01D67/0039B01D69/10B01D69/12B01D71/024C01B3/503C01B2203/0405
Inventor 杨靖贾德宝
Owner XI'AN POLYTECHNIC UNIVERSITY