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IWR/CDO co-crystallized zeolite molecular sieve synthesis method

A zeolite molecular sieve and co-crystallization technology, applied in molecular sieve and alkali exchange compounds, chemical instruments and methods, inorganic chemistry and other directions, to achieve the effects of strong operability, low price and wide synthesis range

Active Publication Date: 2019-04-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a synthetic method for IWR / CDO co-crystal zeolite molecular sieve in order to solve the problem of no IWR / CDO co-crystallization zeolite molecular sieve in the prior art

Method used

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  • IWR/CDO co-crystallized zeolite molecular sieve synthesis method
  • IWR/CDO co-crystallized zeolite molecular sieve synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve 2.1g of germanium oxide in 10.8g of 45wt% choline hydroxide aqueous solution, add 18.7g of tetraethylorthosilicate (TEOS) and 0.41g of aluminum isopropoxide, after the hydrolysis is complete, stir the container open overnight to volatilize ethanol , propanol and part of water until the reaction mixture reaches the final molar composition.

[0020] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 150°C for crystallization for 168 hours. After the reaction, the solid obtained by filtering, washing, drying and calcining is IWR / CDO co-crystal molecular sieve, wherein the proportion of IWR molecular sieve is 65%. The XRD pattern of the sample is as figure 1 As shown, the scanning electron microscope pictures are shown as figure 2 shown.

Embodiment 2

[0022] Dissolve 5.2g of germanium oxide in 13.5g of 45wt% choline hydroxide aqueous solution, add 20.8g of tetraethylorthosilicate (TEOS), after the hydrolysis is complete, open the container and stir overnight to volatilize ethanol and part of the water until the reaction mixture to reach the final molar composition.

[0023] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 170° C. for 72 hours for crystallization. The solid obtained after the reaction is filtered, washed, dried and calcined is an IWR / CDO co-crystal molecular sieve, wherein the proportion of the IWR molecular sieve is 5%.

Embodiment 3

[0025] Dissolve 5.2g germanium oxide in 13.5g 45wt% choline hydroxide aqueous solution, add 20.8g tetraethyl orthosilicate (TEOS) and 0.6g HBeta molecular sieve (SiO 2 / Al 2 o 3 =25), after the hydrolysis was complete, the container was opened and stirred overnight to volatilize ethanol and part of the water until the reaction mixture reached the final molar composition.

[0026] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 160°C for crystallization for 120 hours. After the reaction, the solid obtained by filtering, washing with distilled water, drying and calcining is IWR / CDO co-crystal molecular sieve, wherein the proportion of IWR molecular sieve is 77%.

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Abstract

The invention relates to an IWR / CDO co-crystallized zeolite molecular sieve synthesis method, wherein a mixture is subjected to hydrothermal crystallization for 30-300 h at a temperature of 100-200 DEG C according to a ratio of an organic templating agent choline hydroxide to YO2 to X2O3 to H2O of 0.15-0.95:1:0-0.08:2-28 to obtain a porous IWR / CDO co-crystallized zeolite molecular sieve material,wherein Y is at least a skeleton tetravalent element, and X is at least a trivalent skeleton element. According to the present invention, the IWR / CDO co-crystallized zeolite molecular sieve is synthesized with the inexpensive organic templating agent, the relative ratio of the two molecular sieves is adjusted within a range of 1-99%, and the synthesis method is simple and easy to perform, and is suitable for promotion.

Description

technical field [0001] The present invention relates to a synthesis method of zeolite molecular sieve, more precisely relates to a synthesis method of IWR / CDO co-crystal zeolite molecular sieve. technical background [0002] Zeolite molecular sieves are crystalline porous silicate materials that are widely used as adsorbents, ion exchangers, and industrial catalysts. At present, there are 235 molecular sieve topologies approved by the International Molecular Sieve Association. [0003] IWR molecular sieve has a channel structure of 12×12×10-membered rings, straight channels of 12-membered rings along the c-axis direction, zig-zag channels of 12-membered rings along the a-axis direction, and straight channels of 10-membered rings along the b-axis direction. The organic template for preparing IWR molecular sieves is generally hexamethylene hydroxide bis(trimethylammonium) cation (US7344696B). [0004] The CDO molecular sieve has a channel structure of 8×8 membered rings, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72C01P2004/03
Inventor 付文华杨为民袁志庆王振东滕加伟陶伟川
Owner CHINA PETROLEUM & CHEM CORP
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