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Synthesis method of IM-5 molecular sieve

A synthesis method and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite and the like

Active Publication Date: 2014-04-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The object of the present invention is to solve the problem of improving the crystallinity of IM-5 molecular sieve, and a kind of synthetic method of IM-5 molecular sieve is provided

Method used

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  • Synthesis method of IM-5 molecular sieve
  • Synthesis method of IM-5 molecular sieve
  • Synthesis method of IM-5 molecular sieve

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preparation example Construction

[0027] The present invention provides a kind of synthetic method of IM-5 molecular sieve, it is characterized in that, the method comprises:

[0028] (1) Under stirring conditions, the mixed solution containing the aluminum source is contacted with the silicon source to form a colloid, and the mixed solution containing the aluminum source is an aqueous solution containing an inorganic base, a mineralizer, an aluminum source and a templating agent;

[0029] (2) Under crystallization reaction conditions, the colloid is subjected to hydrothermal crystallization;

[0030] The feed intake of described inorganic base, described mineralizer, described aluminum source, described templating agent, described silicon source and water makes the composition of described colloid be in moles: SiO 2 :Al 2 o 3 :M 2 O:MX:SDA:H 2 O=10: (0.1-1): (1-10): (0.1-5): (0.1-4): (50-500); the silicon source is SiO 2 In terms of the aluminum source as Al 2 o 3 In terms of, the inorganic base is in ...

preparation example 1

[0057] IM was synthesized according to the method disclosed in the literature (Synthesis, characterization, and catalytic properties of zeolites IM-5 and NU-88; Synthesis, characterization, and catalytic properties of zeolites IM-5 and NU-88. Journal of Catalysis2003:215 151~170). -5 molecular sieves.

[0058] Mix 10.19g of 1,5-bis(N-methylpyrrolidine)pentane aqueous solution with 2.92g of NaOH, 1.1g of Al(NO 3 ) 3 9H 2 O is dissolved in an appropriate amount of deionized water, mixed evenly, and 6.19g of white carbon black is added under stirring conditions to make a milky white colloid, and the molar composition of the reaction mixture is: SiO 2 :Al 2 o 3 : Na 2 O: R: H 2 O=10:0.167:3.65:1.5:400 (where R is 1,5-bis(N-methylpyrrolidine)pentane). The obtained mixture was stirred at room temperature for 24 hours, and the obtained colloid was transferred to a 50 mL polytetrafluoroethylene-lined crystallization kettle, and rotated and crystallized at 160° C. for 14 days wi...

Embodiment 1

[0061] This example is used to illustrate the synthesis method of the IM-5 molecular sieve of the present invention.

[0062] 0.67gAlCl 3 , 4.53g NaOH, 1.71g NaCl, and 22.68g SDA were dissolved in an appropriate amount of deionized water, and mixed evenly. Under stirring conditions, 40g of silica sol was slowly added dropwise to form a milky white colloid, and continued to stir for 2h. The molar composition of the colloid is: SiO 2 :Al 2 o 3 : Na 2 O:NaCl:SDA:H 2 O=10:0.25:2.83:1:1.67:400.

[0063] Transfer the prepared colloid to a 100mL polytetrafluoroethylene-lined autoclave, rotate and crystallize at 175°C for 10 days, stop the crystallization reaction, wash and filter the product, and dry it overnight at 80°C to obtain molecular sieves Original powder A1.

[0064] The XRD measurement results of the molecular sieve powder A1 were compared with the XRD spectrum of the IM-5 molecular sieve published in the document "Determining the Pore Structure of IM-5 Molecular Sie...

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Abstract

The invention provides a synthesis method of an IM-5 molecular sieve. The method comprises the steps of: (1) under a stirring condition, contacting an aluminum source-containing mixed solution with a silicon source to make a colloid, with the aluminum source-containing mixed solution being an aqueous solution containing inorganic alkali, a mineralizer, an aluminum source and a template agent; and (2) under crystallization reaction conditions, subjecting the colloid to hydrothermal crystallization. According to the composition of the colloid, the mole ratio of the inorganic alkali, the mineralizer, the aluminum source, the template agent, the silicon source and water satisfies the following formula: SiO2:Al2O3:M2O:MX:SDA:H2O=10:(0.1-1):(1-10):(0.1-5):(0.1-4):(50-500). The silicon source is SiO2, the aluminum source is Al2O3, the inorganic alkali is M2O, MX is the mineralizer, and SDA is the template agent. The mineralizer is a metal halide able to regulate the molecular sieve crystal growth. The method can be used for preparing the IM-5 molecular sieve with enhanced crystallinity.

Description

technical field [0001] The invention relates to a synthesis method of IM-5 molecular sieve. Background technique [0002] The development of the petrochemical industry and the fine chemical industry, as well as the increasingly stringent requirements for sustainable development and environmentally friendly production, have led to an increasing demand for new catalytic materials. [0003] In 1997, French Petroleum Company (IFP) successfully synthesized IM-5 molecular sieve (WO98 / 17581A1, CN1234012A). The molecular sieve has a two-dimensional ten-membered ring channel system and limited short channels in the third dimension. The channel system is very similar to the ZSM-5 molecular sieve and has good shape selectivity. At the same time, IM-5 molecular sieve has good thermal stability and hydrothermal stability, excellent catalytic performance, and has a wide range of applications in catalytic reactions. For example, IM-5 molecular sieve loaded with hydrogenation / dehydrogenati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 陈俊文张超王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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