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Preparation method and application of silazane modified mesoporous molecular sieve/PDMS (polydimethylsiloxane) hybridized composite membrane

A mesoporous molecular sieve and hybrid composite technology, applied in the field of membrane separation, can solve the problem of less application of nitrogen silane, and achieve the effects of simple process, increased selectivity, and improved permeation flux

Active Publication Date: 2013-10-16
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the research, coupling agents such as siloxane and chlorosilane are often used to carry out alkylation and hydrophobic modification of molecular sieves, and nitrogen silane is rarely used.

Method used

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  • Preparation method and application of silazane modified mesoporous molecular sieve/PDMS (polydimethylsiloxane) hybridized composite membrane
  • Preparation method and application of silazane modified mesoporous molecular sieve/PDMS (polydimethylsiloxane) hybridized composite membrane
  • Preparation method and application of silazane modified mesoporous molecular sieve/PDMS (polydimethylsiloxane) hybridized composite membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Weigh a certain amount of mesoporous molecular sieve MCM-41 and lay it flat on a porcelain boat, place it in a muffle furnace, program the temperature to 200°C for 2h, keep it warm for 1h, cool down, and remove the moisture in the molecular sieve. Weigh 2.0 g of dehydrated mesoporous molecular sieves, disperse them in ethanol, and ultrasonicate for 30 minutes to fully disperse them. The suspension was poured into the reaction flask, nitrogen gas was introduced for 15-30min, and the air in the flask was discharged. Stir, heat, condense and reflux, and raise the temperature to 80°C. After stabilization, add 0.5g of 1,1,3,3-tetramethyldisilazane and react for 8h. After the reaction is completed, the suspension containing the modified molecular sieve is poured out, and the modified mesoporous molecular sieve is repeatedly washed with ethanol to remove the unreacted silane coupling agent. Dry in an oven at 50°C and grind.

[0025] (2) After cleaning the industrialized ...

Embodiment 2

[0034] (1) Weigh a certain amount of mesoporous molecular sieve MCM-41 and lay it flat on a porcelain boat, place it in a muffle furnace, program the temperature to 200°C for 2h, keep it warm for 1h, cool down, and remove the moisture in the molecular sieve. Weigh 2.0 g of dehydrated mesoporous molecular sieves, disperse them in n-heptane, and ultrasonicate for 30 minutes to fully disperse them. The suspension was poured into the reaction, nitrogen gas was introduced for 15-30min, and the air in the flask was discharged. Stir, heat, condense and reflux, and raise the temperature to 100°C. After stabilization, add 1.0g of 1,3-di-n-octyltetramethylsilazane and react for 10h. After the reaction is completed, the suspension containing the modified molecular sieve is poured out, and the modified mesoporous molecular sieve is repeatedly washed with n-heptane to remove the unreacted silane coupling agent. Dry in an oven at 50°C and grind.

[0035] (2) After cleaning the industriali...

Embodiment 3

[0041] (1) Weigh a certain amount of mesoporous molecular sieve SBA-15-1 and lay it flat on a porcelain boat, place it in a muffle furnace, program the temperature to 200°C for 2 hours, keep it warm for 1 hour, cool down, and remove the moisture in the molecular sieve. Weigh 2.0 g of dehydrated mesoporous molecular sieves, disperse them in ethanol, and ultrasonicate for 30 minutes to fully disperse them. The suspension was poured into the reaction flask, nitrogen gas was introduced for 15-30min, and the air in the flask was discharged. Stir, heat, condense and reflux, raise the temperature to 80°C, after stabilization, add 1.0g of 1,3-di-n-octyltetramethylsilazane, and react for 8h. After the reaction is completed, the suspension containing the modified molecular sieve is poured out, and the modified mesoporous molecular sieve is repeatedly washed with ethanol to remove the unreacted silane coupling agent. Dry in an oven at 50°C and grind.

[0042] (2) After cleaning the ind...

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Abstract

The invention relates to a preparation method and application of a silazane modified mesoporous molecular sieve / PDMS (polydimethylsiloxane) hybridized composite membrane and belongs to the technical field of membrane separation. The preparation method of the silazane modified mesoporous molecular sieve / PDMS hybridized composite membrane comprises the following steps of: carrying out hydrophobic modification on a mesoporous molecular sieve by adopting a silane coupling agent under the heating, condensation and refluxing conditions; cleaning an industrial polysulfone (PSF) basement membrane by adopting deionized water, then soaking the industrial polysulfone basement membrane in an ethanol / aqueous solution for a period of time, and baking for spare use; and doping the modified mesoporous molecular sieve into PDMS in certain proportion, and preparing the hybridized composite membrane on the basement membrane by adopting a coating or impregnating method. According to the preparation method of the silazane modified mesoporous molecular sieve / PDMS hybridized composite membrane, a regular pore structure of the mesoporous molecular sieve and the modifiable characteristic of pore canals are utilized, hydrophobic modification by virtue of silazane on the mesoporous molecular sieve is easy to realize, and adsorption of alcohol molecules on the surface of the membrane and mass transfer diffusion in the pore canals of the mesoporous molecular sieve can be facilitated, so that separation performance of the hybridized membrane is improved; and the preparation method of the silazane modified mesoporous molecular sieve / PDMS hybridized composite membrane is simple, the mesoporous molecular sieve and the basement membrane are cheap and easily available, and the silazane modified mesoporous molecular sieve / PDMS hybridized composite membrane has a broad prospect in industrial application.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, and in particular relates to the preparation and application of hydrophobically modified mesoporous molecular sieves and pervaporation preferential alcohol permeation hybrid membranes by using a nitrogen silane coupling agent. Background technique [0002] At present, organic / inorganic hybrid membranes have become one of the research hotspots in the field of pervaporation membrane separation due to the advantages of both organic and inorganic components. The introduction of inorganic particles into the organic network can effectively improve the shortcomings of organic polymer membranes such as low mechanical strength and poor solvent resistance, and the separation performance of the membrane can be further improved by hydrophobic modification of inorganic particles. At present, there are many researches on doping ZSM-5, Silicalite-1 and other microporous zeolite molecular sieves in P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/70B01D69/12B01D67/00
Inventor 纪树兰高静刘威刘吉达秦振平
Owner BEIJING UNIV OF TECH