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Preparation method of beta molecular sieve

A beta molecular sieve and crystal seed technology, applied in the field of catalytic chemistry, can solve the problems of low product yield, high system water content, large amount of template agent, etc., achieve high thermal efficiency, improve yield and crystallinity, and shorten synthesis time. Effect

Inactive Publication Date: 2019-08-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adding templates to synthesize β molecular sieves is still the mainstream technology, but conventional hydrothermal synthesis has the problems of large amount of templates, high water content in the system, and low product yield.

Method used

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  • Preparation method of beta molecular sieve
  • Preparation method of beta molecular sieve
  • Preparation method of beta molecular sieve

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preparation example Construction

[0043] The present invention provides a kind of preparation method of β molecular sieve, and this preparation method comprises:

[0044] (1) Synthesis of initial gel: mix silicon source, aluminum source, template agent, alkaline metal source, water, and β molecular sieve seed crystals, stir evenly, and synthesize initial gel; silicon source is SiO 2 In terms of aluminum source as Al 2 o 3 In terms of templating agent TEA + In terms of alkaline metal sources as Na 2 In terms of O, the molar ratio of raw materials for synthesizing the initial gel is: SiO 2 / Al 2 o 3 =25~150, TEA + / SiO 2 =0.07~0.23, Na 2 O / SiO 2 =0.03~0.12,H 2 O / SiO 2 =3.0~11.5, preferably: SiO 2 / Al 2 o 3 =30~120:1, TEA + / SiO 2 =0.07~0.15:1, Na 2 O / SiO 2 =0.05~0.12:1, H 2 O / SiO 2 =3.0~7.5:1; β molecular sieve seed crystal silicon aluminum ratio SiO 2 / Al 2 o 3 =20~100, the amount added is SiO in the silicon source by mass 2 0.5% to 10% of the mass, mixed evenly to get the initial gel; ...

Embodiment 1

[0064] Add 11.00 g of deionized water and 13.00 g of tetraethylammonium hydroxide solution into a container in a water bath at 70° C., and stir evenly. Add 0.31g sodium hydroxide, add 1.85g sodium metaaluminate, stir to dissolve. Add 15.00g of coarse-porous silica gel and stir evenly. Add 0.30 g of β molecular sieve seed crystals and stir evenly to obtain an initial gel. Microwave heating crystallization reaction was carried out on the initial gel, and the temperature was controlled at 160°C for 15 hours. After the reaction is finished, the product is washed and dried, and characterized by X-ray diffraction. The crystallinity of the product is shown in Table 1. SEM and BET analysis were carried out, and the results are shown in Table 2.

Embodiment 2

[0066] Add 11.00 g of deionized water and 13.00 g of tetraethylammonium hydroxide solution into a container in a water bath at 70° C., and stir evenly. Add 0.31g sodium hydroxide, add 1.85g sodium metaaluminate, stir to dissolve. Add 15.00g of coarse-porous silica gel and stir evenly. Add 0.30 g of β molecular sieve seed crystals and stir evenly to obtain an initial gel. Microwave heating crystallization reaction was carried out on the initial gel, and the temperature was controlled at 120°C for 25h. After the reaction is finished, the product is washed and dried, and characterized by X-ray diffraction. The crystallinity of the product is shown in Table 1.

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Abstract

The invention discloses a preparation method of a beta molecular sieve. The preparation method comprises the steps of: 1. synthesis of initial gel: mixing a silicon source, an aluminum source, a template agent, an alkaline metal source, water and a beta molecular sieve seed crystal evenly to synthesize an initial gel, wherein the silicon source is calculated in terms of SiO2, the aluminum source is calculated in terms of Al2O3, the template agent is calculated in terms of TEA<+>, the alkaline metal source is calculated in terms of Na2O, and the raw materials for synthesizing the initial gel are in the following mole ratios that: SiO2 / Al2O3=25-150:1, TEA<+> / SiO2=0.07-0.23:1, Na2O / SiO2=0.03-0.12:1, and H2O / SiO2=3.0-11.5:1, the beta molecular sieve seed crystal has a Si-Al ratio of SiO2 / Al2O3=20-100:1, and in terms of mass, the adding amount is 0%-10% of the mass of SiO2; and 2. microwave heating crystallization reaction: conducting microwave heating treatment on the initial gel preparedby step 1, controlling the heating temperature at 120DEG C-180DEG C and the heating time at 4-25h, thus obtaining a beta molecular sieve product. The method provided by the invention can synthesize the beta molecular sieve with high crystallinity and abundant pore structures by only one step, and compared with the conventional hydrothermal synthesis method, the method provided by the invention cangreatly shorten the synthesis time of the beta molecular sieve, the grain size of the molecular sieve is smaller, and the pore channels are smoother.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, and in particular relates to a synthesis method of beta molecular sieves. Background technique [0002] β molecular sieve is a patented product USP3308069 researched and developed by Mobil Petroleum Company of the United States in 1967. The earlier reports that β molecular sieves have excellent catalytic performance are the follow-up patents EP0159846 and EP0159847 developed by Mobil Corporation for β molecular sieves, which disclose that β molecular sieves have excellent activity for hydrocarbon cracking and isomerization. Since the 1990s, with the understanding of the crystal structure of β molecular sieve, the research on the synthesis and catalytic performance of β molecular sieve has been carried out rapidly. Excellent catalytic performance in numerous catalytic reactions in petroleum refining and petrochemical processes such as wax and photocatalysis. Because it is the only hi...

Claims

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Application Information

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IPC IPC(8): C01B39/04B82Y40/00
CPCB82Y40/00C01B39/04C01P2002/72C01P2004/03C01P2004/64C01P2006/12C01P2006/14
Inventor 崔岩王晓化沈宜泓李梦晨喻昊庞新梅李发永
Owner PETROCHINA CO LTD
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