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In-situ synthetic method for zeolite molecular sieve membrane

A technology for synthesizing zeolite and molecular sieve, applied in the field of membrane technology separation, can solve the problems of poor uniformity and low repetition rate, and achieve the effects of good stability and permeability, uniform distribution and thin membrane layer

Inactive Publication Date: 2018-06-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of poor uniformity and low repetition rate of acid-resistant zeolite molecular sieve membrane products in the prior art, the present invention provides an in-situ method for synthesizing acid-resistant zeolite molecular sieve membranes

Method used

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  • In-situ synthetic method for zeolite molecular sieve membrane
  • In-situ synthetic method for zeolite molecular sieve membrane
  • In-situ synthetic method for zeolite molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Dissolve 0.515g of aluminum sec-butoxide in 3.668g of 35wt.% tetraethylammonium hydroxide aqueous solution to form a colorless homogeneous solution 1, and dissolve 2.585g of 40wt.% silica sol in 3.668g of 35wt.% tetraethylammonium hydroxide Ammonium aqueous solution forms milky white solution 2, pour solution 2 into solution 1, stir for 3 hours until it is evenly mixed, put the light milky white sol in an oven at 95°C for aging for 18 hours, and obtain a colorless homogeneous charge density mismatch solution; weigh Dissolve 0.400g of tetramethylammonium chloride in 0.766g of deionized water, add it to the charge density mismatch solution and stir for 30min to obtain a synthetic solution; 2 o 3 Put it horizontally in the synthesis liquid, screw the reactor tightly; put the closed reactor in an oven at 150°C for 96 hours. After the reaction was completed, 10 mL of deionized water was used to ultrasonically wash and dry at 65°C. A zeolite molecular sieve membrane synthes...

Embodiment 2

[0049] 0.570g of aluminum sec-butoxide was dissolved in 7.794g of 35wt.% tetraethylammonium hydroxide aqueous solution to form a colorless homogeneous solution 1, and 3.858g of 40wt.% tetraethoxysilane was added to solution 1 under stirring conditions, Stir well until the mixture is complete to form a light milky white solution 2, which is aged in a water bath at 80°C for 24 hours to obtain a colorless homogeneous charge density mismatch solution; weigh 0.254g of tetramethylammonium chloride and dissolve it in 4.934g of deionized In water, after ultrasonication, it was added to the charge density mismatch solution, and stirred for 30 minutes to obtain a synthetic solution; the synthetic solution was transferred to a high-pressure reactor; the closed reactor was placed in an oven at 150°C for 96 hours. After the reaction was completed, the product was centrifuged to obtain a white solid product, which was ultrasonically washed with deionized water and centrifuged three times, an...

Embodiment 3

[0051] Dissolve 0.515g of aluminum sec-butoxide in 3.668g of 35wt.% tetraethylammonium hydroxide aqueous solution to form a colorless homogeneous solution 1, and dissolve 2.585g of 40wt.% silica sol in 3.668g of 35wt.% tetraethylammonium hydroxide Ammonium aqueous solution forms milky white solution 2, pour solution 2 into solution 1, stir for 3 hours until it is evenly mixed, put the light milky white sol in an oven at 95°C for aging for 18 hours, and obtain a colorless homogeneous charge density mismatch solution; weigh Dissolve 0.400g of tetramethylammonium chloride in 0.766g of deionized water, add it to the charge density mismatch solution and stir for 30min to obtain a synthetic solution; transfer the synthetic solution to a microwave reaction with a polytetrafluoroethylene liner In the kettle, at the same time, the α-Al 2 o 3 Put it horizontally in the synthesis solution, and tighten the reactor; put the closed reactor in an oven at 150°C for 10 hours. After the react...

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Abstract

An in-situ synthetic method for a zeolite molecular sieve membrane comprises the steps of: preparing a synthetic solution from a silicon source, an aluminum source and an organic template agent, placing a porous carrier in the synthetic solution, and synthesizing an acid-resistant zeolite molecular sieve membrane under hydrothermal conditions. The zeolite molecular sieve membrane prepared by the synthetic method of the invention has thin, continuous, dense and uniform distribution without obvious defects. The average thickness of the membrane is 100 nm-50 [mu]m, the silicon-aluminum ratio is relatively high (5-12), and the pore diameter is relatively small (0.36*0.44 nm). The zeolite molecular sieve membrane shows extremely good stability and permeation performance in organic acid solutions with various acidity, is applicable to a pervaporation process under acidic conditions, and exhibits excellent selective permeability on water molecules in organic / water mixtures, especially in acidic systems.

Description

technical field [0001] The invention belongs to the field of membrane technology separation, and in particular relates to a novel acid-resistant zeolite molecular sieve membrane for liquid mixture separation and a preparation method thereof. Background technique [0002] In recent years, with the rapid development of my country's economy, the society's demand for energy is increasing. my country's current energy system efficiency is 33%, which is about 10 percentage points lower than the international average level, so we must attach great importance to the issue of process energy conservation. The separation process is one of the important operating processes in industrial production, and it is widely used in chemical, pharmaceutical, food, biochemical and other industrial processes. At present, the separation process accounts for 40-60% of the energy consumption in the chemical industry process, so reducing the energy consumption of the separation process has received wid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01D61/36
CPCB01D61/362C01B39/04C01P2002/72C01P2004/03
Inventor 杨维慎姚瑞李砚硕班宇杰金花
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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