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A kind of preparation method of acetic acid dehydration ZSM-5 zeolite membrane

A technology of ZSM-5 and zeolite membrane, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., which can solve the problems of low separation selectivity and low acid-resistant flux of zeolite molecular sieve membrane , to achieve the effect of continuous and uniform film layer, stable performance of acetic acid dehydration and separation, and thin film layer

Active Publication Date: 2011-12-21
DALIAN UNIV OF TECH
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  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved in the present invention is to provide a nano-aggregate crystal seed on a macroporous carrier for the acid resistance of the zeolite molecular sieve membrane faced by the dehydration of the organic acid, the low flux of the membrane, and the low separation selectivity. f - Direct synthesis of ultra-thin, acid-resistant ZSM-5 zeolite membrane with excellent separation performance through membrane microstructure optimization under the condition of inorganic structure-directing agent

Method used

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  • A kind of preparation method of acetic acid dehydration ZSM-5 zeolite membrane
  • A kind of preparation method of acetic acid dehydration ZSM-5 zeolite membrane
  • A kind of preparation method of acetic acid dehydration ZSM-5 zeolite membrane

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Effect test

Embodiment 1

[0043] ①Carrier tube pretreatment: The surface of the carrier tube is polished with 600-mesh and 800-mesh waterproof sandpaper in turn until the surface of the carrier is smooth, and then ultrasonically shakes with acid and alkali respectively to remove the residues in the carrier pores, and wash with deionized water until neutral Afterwards, let it dry naturally, and finally dry it at a temperature of 150°C for later use.

[0044] ②Pre-seed crystal: introduce large seed crystal by hot dipping method, use figure 1 The structural unit shown is a zeolite molecular sieve group composed of ZSM-5 with a grain size of about 100nm, which is a large seed crystal, and α-Al 2 o 3 The two ends of the carrier tube are sealed with polytetrafluoroethylene plugs. This is to force the seed crystals to be introduced only to the outer surface of the carrier. During hot dipping, a pressure difference can be generated on the carrier surface; place the sealed carrier tube in an oven at 175°C for ...

Embodiment 2

[0053] The preparation method is the same as in Example 1, except that the Si / Al in the crystallization mother liquor is changed to 20, 30, and 40, which are respectively recorded as Z02, Z03, and Z04.

Embodiment 3

[0055] The preparation method is the same as in Example 1, but the synthesis time is changed to 24h and 72h, which are respectively recorded as Z05 and Z06.

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Abstract

The invention discloses a method for synthesizing zeolite socony mobil-5 (ZSM-5) zeolite membrane by dehydration by acetic acid, which comprises: directly introducing an ultrathin crystal seed layer onto a macroporous carrier by a two-step crystal process, regulating the Si to Al ratio of a crystallization mother solution by using F<-> as an inorganic structural guiding agent, and preparing a 5 to 6 micrometer thick ZSM-5 zeolite membrane, particularly a ZSM-5 zeolite membrane in which the Si to Al ratio is 10, by using a secondary growth process; therefore, the limit that the membrane can only be formed under a condition that the Si to Al ratio of the crystallization mother solution is more than 20 if an organic template agent is not used is break through, the hydrophilic property of themembrane is improved greatly, and the generation of microstructures which are not acid resistant with aluminum enriched surface and inter-crystal gap is avoided effectively. The membrane thus has high acetic acid dehydration and separation selectively and high acid resistance, the low-flux, low-selectivity and low-acid-resistance technical bottlenecks that zeolite membrane organic acid dehydration faces are broken through, and a firm foundation is laid for the industrial use of the zeolite membrane.

Description

technical field [0001] The invention belongs to the technical field of osmotic separation of inorganic materials, relates to the preparation method of zeolite membrane, especially relates to - It is a method for synthesizing ultra-thin, acid-resistant and excellent acetic acid dehydration ZSM-5 zeolite membrane by optimizing the microstructure of the membrane under the condition of inorganic structure-directing agent. Background technique [0002] Acetic acid is an extremely important organic chemical intermediate with hundreds of derivatives and widely used. Acetic acid is used in the chemical industry to produce chloroacetic acid, acetonitrile, butyl acetate, ethyl acetate, acetic anhydride, cellulose acetate, synthetic camphor and metal salts of acetic acid, such as sodium acetate, lead acetate, etc.; used in the dye industry to produce Disperse and vat dyes; used in the paint industry to produce polyvinyl acetate emulsion, latex paint, interior and exterior wall paint, ...

Claims

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Application Information

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IPC IPC(8): C01B39/38
Inventor 王金渠陈赞杨建华殷德宏杨丽君鲁金明张艳
Owner DALIAN UNIV OF TECH
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