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Phosphorus-containing ZSM-5 molecular sieve membrane and preparation method thereof

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the requirements of harsh operation, difficult to control the microstructure of molecular sieve membrane, film-forming process-dependent performance and other problems, to achieve the effect of good uniform density

Active Publication Date: 2014-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the secondary growth method can reduce the nucleation process and improve the repeatability and orientation control ability of the synthesis of molecular sieve membranes, it first needs to obtain uniformly coated seeds on the surface of the support, and the operation requirements are relatively strict.
[0008] The in-situ hydrothermal synthesis method is widely used in the field of molecular sieve membrane synthesis, and the steps are simple, but it requires high synthesis conditions, and it is not easy to control the microstructure of the molecular sieve membrane, and the film formation process of this method largely depends on the surface of the support. performance

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  • Phosphorus-containing ZSM-5 molecular sieve membrane and preparation method thereof
  • Phosphorus-containing ZSM-5 molecular sieve membrane and preparation method thereof
  • Phosphorus-containing ZSM-5 molecular sieve membrane and preparation method thereof

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preparation example Construction

[0033] According to the preparation method of the phosphorus-containing ZSM-5 molecular sieve membrane of the present invention, wherein, the present invention has no special requirements on the step of uniformly mixing the aluminum source, silicon source, template agent and the phosphorus-containing buffer solution, Preferably, this step includes: (1) dissolving the aluminum source and the template agent in the phosphorus-containing buffer solution and stirring thoroughly to obtain a translucent emulsion. Wherein, there is no special requirement for the sequence of dissolving the aluminum source and the template agent in the phosphorus-containing buffer solution, and the aluminum source and the template agent can be dissolved in the phosphorus-containing buffer solution at the same time or in batches or respectively. (2) Dissolving the silicon source in the mixture obtained in step (1) to form a gel. The present invention has no special requirements on the way of adding the s...

Embodiment 1

[0044] In the there-necked flask, add 0.33 grams of aluminum sulfate octadecahydrate, 1.07 grams of tetrapropylammonium bromide, 1.06 grams of tetrapropylammonium hydroxide aqueous solution of 30% by weight, the buffer solution of diammonium hydrogen phosphate and ammoniacal liquor (PO 4 3- The concentration is 0.20mol / L, the buffer solution pH=10.2) 40.02g, fully stirred for 30 minutes, then slowly added dropwise 10.49g of tetraethyl silicate, and continued to stir for 2 hours to obtain a uniform gel. Put the pretreated aluminum oxide membrane tube porous support (porosity 60%, pore size 100nm-10μm) in a 100 ml stainless steel reaction tank, slowly inject the gel obtained above, so that the surface of the gel is fully immersed in the membrane tube The top of the porous support was sealed and statically crystallized at 130°C for 72 hours. The porous support body of the membrane tube was taken out, washed, dried, and baked at 550° C. for 6 hours to obtain a phosphorus-containi...

Embodiment 2

[0049] Add 0.33 grams of aluminum sulfate octadecahydrate, 0.7 grams of tetrapropylammonium bromide, and a buffer solution of diammonium hydrogen phosphate and ammonia water (PO 4 3- The concentration of the solution is 0.15mol / L, buffer solution pH=10.6) 34 grams, fully stirred for 30 minutes, then slowly added dropwise 10.4 grams of tetraethyl silicate, and continued to stir for 2 hours to obtain a uniform gel. Put the pretreated aluminum oxide membrane tube porous support (porosity 60%, pore size 100nm-10μm) in a 100 ml stainless steel reaction tank, slowly inject the gel obtained above, so that the surface of the gel is fully immersed in the membrane tube The top of the porous support was sealed and statically crystallized at 130°C for 72 hours. The porous support body of the membrane tube was taken out, washed, dried, and baked at 550° C. for 6 hours to obtain a phosphorus-containing ZSM-5 molecular sieve membrane. After crystallization, the pH of the supernatant in the...

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Abstract

The invention provides a phosphorus-containing ZSM-5 molecular sieve membrane and a preparation method thereof. The method comprises steps of uniformly mixing an aluminium source, a silicon source, a template and a phosphorus-containing buffer solution to obtain a uniform gel; and then carrying out hydrothermal crystallization on the gel on a porous support body under hydrothermal crystallization conditions to form the phosphorus-containing ZSM-5 molecular sieve membrane, wherein the phosphorus-containing buffer solution is a buffer solution with a pH value of 9.5-11.5 and containing ammonium phosphate salt and ammoniacal liquor. The invention also provides the phosphorus-containing ZSM-5 molecular sieve membrane prepared by the method. The preparation method of the phosphorus-containing ZSM-5 molecular sieve membrane provided by the invention can obtain uniform compact phosphorus-containing ZSM-5 molecular sieve membrane. The synthesized phosphorus-containing ZSM-5 molecular sieve membrane can be subjected to secondary crystallization to still obtain uniform compact phosphorus-containing ZSM-5 molecular sieve membrane.

Description

technical field [0001] The invention relates to a phosphorus-containing ZSM-5 molecular sieve membrane and a preparation method thereof. Background technique [0002] The supported molecular sieve membrane is a molecular sieve crystallized and grown on the surface of a porous carrier with a certain strength to form a dense and continuous film layer. The carriers used mainly include cellulose, porous metals, porous ceramics, porous metal oxides and the like. Supported molecular sieve membranes usually have good shape-selective separation and catalytic performance, high temperature resistance, strong chemical corrosion resistance and high mechanical strength, and have good application prospects in membrane separation and membrane reaction. [0003] ZSM-5 molecular sieve has a two-dimensional ten-membered ring channel and is an important catalyst or carrier in petrochemical industry. ZSM-5 molecular sieve membrane has the characteristics of high thermal stability, good acid r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40
Inventor 姜健准张明森柯丽杨菁梁中伟张伟
Owner CHINA PETROLEUM & CHEM CORP