Method for sintering of porous ceramic support and in-situ hydrothermal synthesis of molecular sieve membrane by molecular sieve

A porous ceramic, in-situ hydrothermal technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc. The effect of less waste, good separation selectivity and permeability, and easy operation

Active Publication Date: 2018-06-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to avoid the disadvantages of high price and inefficiency in the synthesis of nano-crystal seeds, and to overcome the instability and non-repeatability of the existing crystal-coating technology, and to provide a preparation process that does not change the original porous ceramic support. Simple doping of molecular sieves in ingredients and efficient in situ hydrothermal synthesis for the preparation of dense molecular sieve membranes on the surface of porous ceramic supports

Method used

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  • Method for sintering of porous ceramic support and in-situ hydrothermal synthesis of molecular sieve membrane by molecular sieve
  • Method for sintering of porous ceramic support and in-situ hydrothermal synthesis of molecular sieve membrane by molecular sieve
  • Method for sintering of porous ceramic support and in-situ hydrothermal synthesis of molecular sieve membrane by molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Preparation of porous alumina hollow fiber support containing NaA molecular sieve conversion

[0041] Step A. Configure the alumina hollow fiber spinning solution containing NaA molecular sieve

[0042] According to the composition mass ratio NMP:PES:(Al 2 o 3 +NaA):PVP=40.2:8.5:50.8:0.5 to prepare hollow fiber spinning solution, wherein NaA:(Al 2 o 3 +NaA) was 10% by mass. The mixing step is: add PES into NMP, stir for 2 hours to fully dissolve, then add NaA molecular sieve and stir for 12 hours. Added NaA molecular sieves such as figure 1 As shown, it has a typical cubic shape. Then, under continuous stirring, the Al 2 o 3 The powder is added in batches and the PVP is added at the end. The obtained white hollow fiber spinning solution still needs to be continuously stirred for more than 2 days.

[0043] Step B. Spinning to obtain the hollow fiber precursor and sintering at high temperature

[0044] Under the action of nitrogen, the spinning solution is...

Embodiment 2

[0048] (1) Preparation of porous alumina hollow fiber support containing NaA molecular sieve conversion

[0049] Step A. Configure the alumina hollow fiber spinning solution containing NaA molecular sieve

[0050] According to the composition mass ratio NMP:PES:(Al 2 o 3 +NaA):PVP=40.2:8.5:50.8:0.5 to prepare hollow fiber spinning solution, wherein NaA:(Al 2 o 3 +NaA) was 20% by mass. The mixing step is: add PES into NMP, stir for 2 hours to fully dissolve, then add NaA molecular sieve powder and stir for 12 hours. Then, under continuous stirring, the Al 2 o 3 The powder is added in batches and the PVP is added last. The obtained white hollow fiber spinning solution still needs to be continuously stirred for more than 2 days.

[0051] Step B. Spinning to obtain the hollow fiber precursor and sintering at high temperature

[0052] Under the action of nitrogen, the spinning solution is extruded from the spinning head, firstly contacts the inner coagulation bath (water),...

Embodiment 3

[0056] (1) Preparation of porous alumina hollow fiber support containing NaA molecular sieve conversion

[0057] With embodiment 1.

[0058] (2) In situ hydrothermal synthesis of NaA molecular sieve membrane

[0059] According to molar ratio Na 2 O:SiO 2 :Al 2 o 3 :H 2O=41.9:4.4:1:833.3 Prepare the synthesis solution for synthesizing molecular sieve membranes. Weigh 4.34g of water glass (solid content 55%) and 19.15g of sodium hydroxide into 54.86g of deionized water, and stir at room temperature for 15 minutes to completely dissolve it; simultaneously weigh 1.20g of sodium aluminate and add to 36.20g of In deionized water, stir at room temperature for 15 minutes to dissolve completely. Then pour the sodium aluminate solution into the constantly stirring sodium silicate solution. After the end, the synthetic solution was continuously stirred at room temperature for 1 hour to complete the aging. The support was inserted into the synthesis solution, and after static in-s...

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Abstract

The invention discloses a method for sintering of a porous ceramic support and in-situ hydrothermal synthesis of a molecular sieve membrane by a molecular sieve. The method comprises adding an appropriate amount of molecular sieve powder into conventional porous ceramic support ingredients, carrying out molding, carrying out drying, carrying out sintering at a high temperature to obtain a porous ceramic support containing a molecular sieve conversion product, putting the ceramic support into a synthesis solution for preparing a molecular sieve film and carrying out in-situ hydrothermal synthesis to obtain a molecular sieve membrane. Compared with the molecular sieve membrane without the molecular sieve conversion product on the ceramic support, the molecular sieve membrane containing the molecular sieve conversion product is compacter and has better separation performances. The method is easy to operate, reduces a sintering temperature and is free of crystal coating and support post-treatment. The synthetic molecular sieve membrane is continuous and compact, has good separation performances and good repeatability, saves energy, is environmentally friendly and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a method for preparing a porous ceramic support body by adding molecular sieve sintering and in-situ hydrothermal synthesis of a molecular sieve membrane, in particular to a method for preparing a porous ceramic support body by adding molecular sieve powder to a conventional porous ceramic support body batching, through seedless coating A method for preparing molecular sieve membranes by in situ hydrothermal synthesis. Background technique [0002] Molecular sieve is a microporous inorganic crystal material formed with silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron as the basic skeleton. Molecular sieves have the following advantages as inorganic membrane materials: 1) Molecular sieves have regular pores and a single pore size distribution; and the pore size of molecular sieves is similar to the molecular size of many important industrial raw materials, and molecules can be separated by molecular sieving or shape-se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00B01D69/10
CPCB01D67/0044B01D69/105B01D71/028
Inventor 王正宝马楠柯王睿
Owner ZHEJIANG UNIV
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