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Synthetic method with MWW structure si/b molecular sieve

A synthesis method and molecular sieve technology are applied in the direction of crystalline aluminosilicate zeolite, etc., which can solve the problems of highly toxic preparation and complexity of template agents, and achieve the effect of less template agent usage and avoiding environmental pollution.

Active Publication Date: 2014-10-15
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The technical problem to be solved by the present invention is the shortcoming of highly toxic template agent or complex preparation in the prior art, and a new synthesis method of Si / B molecular sieve with MWW structure is provided

Method used

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  • Synthetic method with MWW structure si/b molecular sieve

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Effect test

Embodiment 1

[0019] Dissolve 0.4 grams of sodium hydroxide in 37.8 grams of water, then add 3.6 grams of diethyldimethylammonium hydroxide (DEDMAOH), add 12.5 grams of boric acid under the condition of uniform stirring, add 22.5 grams of 40% boric acid after fully dissolving Silica sol, continue to stir for 1 hour, the molar ratio of gained reaction mother liquor is 0.67B 2 o 3 : SiO 2 :0.06OH - : 0.20DEDMAOH : 19.0H 2 O. Then put the mother liquor into a 100 ml high-pressure crystallization kettle, and conduct dynamic crystallization at 170° C. for 3 days, filter after cooling, wash, and dry to obtain a Si / B molecular sieve with a MWW structure. The XRD spectrum pattern of obtained molecular sieve is shown in figure 1 , XRD diffraction peaks with a typical MWW structure.

Embodiment 2

[0021] Dissolve 2.0 grams of sodium hydroxide in 35.0 grams of water, then add 4.5 grams of diethyldimethylammonium hydroxide, add 10.8 grams of boric acid under the condition of uniform stirring, add 25.0 grams of 30% silica sol after fully dissolving, Continue stirring for 1 hour, the molar ratio of the resulting reaction mother liquor is 0.70B 2 o 3 : SiO 2 : 0.40OH - : 0.30DEDMAOH : 23.0H 2 O. Then put the mother liquor into a 100 ml high-pressure crystallization kettle, and conduct dynamic crystallization at 170° C. for 3 days, filter after cooling, wash, and dry to obtain a Si / B molecular sieve with a MWW structure. The XRD spectrum pattern of obtained molecular sieve and figure 1 Similarly, it is a molecular sieve with a typical MWW structure.

Embodiment 3

[0023] Dissolve 0.5 gram of lithium hydroxide in 56.2 gram of water, then add 3.8 gram of diethyldimethylammonium hydroxide, add 13.2 gram of boric acid under the condition of uniform stirring, add 22.5 gram of ethyl orthosilicate after fully dissolving, Continue stirring for 1 hour, the molar ratio of the resulting reaction mother liquor is 0.98B 2 o 3 : SiO 2 : 0.19OH - : 0.30DEDMAOH : 28.9H 2 O. Then put the mother liquor into a 100 ml high-pressure crystallization kettle, and dynamically crystallize at 160° C. for 4 days. After cooling, filter, wash, and dry to obtain a Si / B molecular sieve with a MWW structure. The XRD spectrum pattern of obtained molecular sieve and figure 1 Similarly, it is a molecular sieve with a typical MWW structure.

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Abstract

The invention relates to a synthetic method of an MWW structured Si / B molecular sieve and mainly solves problems of severe toxicity of a template or complex preparation in the prior art. The synthetic method provided by the invention comprises the following steps: mixing a boron source, a silicon source, alkaline MOH, a template R and water, wherein the mol ratio of the mixture is B2O3:SiO2:OH-:R:H2O=(0.01-1.00):1:(0.02-0.30):(0.01-0.50):(5-50); carrying out hydrothermal crystallization on the above mixture at the temperature of 100-200 DEG C for 1-10 days; separating, washing and drying to obtain the MWW structured Si / B molecular sieve, wherein the template R is diethyldimethylammonium hydroxide. The technical scheme can be applied in industrial production of the MWW structured Si / B molecular sieve.

Description

technical field [0001] The invention relates to a synthesis method of Si / B molecular sieve with MWW structure. Background technique [0002] Molecular sieves are composed of silicon-oxygen tetrahedra and balanced cations. They have a highly ordered crystal structure and regular and uniform sub-nanometer pores. They have been widely used in various fields such as catalysis, adsorption and ion exchange. [0003] MWW molecular sieves are a class of molecular sieves with sinusoidal 10-membered ring network pore system, 12-membered ring cavity and supercage pore system structure (Science, 1994, 264: 1910). MCM-22 molecular sieve was first synthesized by Mobil in 1990 (USP4,954,325). In 1994, Leonowicz et al. determined the structure of MCM-22 through high-resolution electron microscopy and X-ray powder diffraction analysis. In 1997, the International Zeolite Association (IZA) The molecular sieve is officially named MCM-22 (Micro. Meso. Mater. 1998, 22, 551), which belongs to the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 张斌孙洪敏宦明耀沈震浩杨为民
Owner CHINA PETROLEUM & CHEM CORP
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