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: 2015-06-17
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 method for synthesizing IM-5 molecular sieve, which is characterized in that the method includes:

[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 template agent;

[0029] (2) Under the conditions of the crystallization reaction, hydrothermally crystallize the colloid;

[0030] The inorganic base, the mineralizer, the aluminum source, the template, the silicon source, and water are charged so that the composition of the colloid is 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 The aluminum source is Al 2 O 3 Calculated, the inorganic base is M 2 In terms of O, MX is the mineralizer, SDA is the template agent; the mineralizer is a metal ...

preparation example 1

[0057] According to the literature (Synthesis, characterization and catalytic properties of IM-5 and NU-88 molecular sieves; Synthesis, characterization, and catalytic properties of zeolites IM-5 and NU-88. Journal of Catalysis 2003:215 151~170) -5 molecular sieve.

[0058] Combine 10.19g 1,5-bis(N-methylpyrrolidine)pentane aqueous solution, 2.92g NaOH, 1.1g Al(NO 3 ) 3 ·9H 2 Dissolve O in an appropriate amount of deionized water, mix well, add 6.19g white carbon black under stirring conditions to make a milky white colloid, 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 resulting mixture was stirred at room temperature for 24 hours, and the prepared colloid was transferred to a 50 mL polytetrafluoroethylene lined crystallization kettle, and rotated at 160°C for 14 days after crystallization, and the rotation speed was 100 rpm. The crystallization reaction is stopped...

Embodiment 1

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

[0062] 0.67gAlCl 3 , 4.53g NaOH, 1.71g NaCl, and 22.68g SDA are dissolved in an appropriate amount of deionized water and mixed uniformly. Under stirring conditions, 40g silica sol is slowly added dropwise to form a milky white colloid, and stirring is continued 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. After rotating and crystallizing at 175℃ for 10 days, stop the crystallization reaction. After washing and filtering, the product is dried at 80℃ overnight to obtain molecular sieve. Original powder A1.

[0064] The XRD measurement results of the original molecular sieve powder A1 were compared with the XRD spectra of IM-5 molecular sieve published in the document "Determining the pore structure of IM-5 mol...

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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 Patents(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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