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Preparation method of beta molecular sieve

A technology of β molecular sieve and crystal seed, which is applied in the field of catalytic chemistry, can solve the problems of stable reaction system, difficult control of reaction conditions, and difficult control of reaction conditions, so as to improve yield and crystallinity, shorten synthesis time, Realize the effect of rapid crystal growth

Active Publication Date: 2019-08-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since no organic template is added to the system, it is difficult to maintain the stability of the reaction system only by the structure-guiding effect of the seed crystals. As a result, the phase region of the synthesized β molecular sieve is very narrow, and it is difficult to control the actual reaction conditions, and it is easy to generate miscellaneous crystals
[0006] To sum up, conventional hydrothermal synthesis of β molecular sieves generally uses organic templates, and the production time is relatively long, especially due to the large amount of templates used, resulting in very high production costs, and the molecular sieve products need to be roasted to release templates in the later stage. , will cause damage to the product structure, and the removed template agent will also seriously pollute the environment
Now there is a technology for synthesizing β molecular sieves without adding additional organic templates. However, due to the conventional hydrothermal synthesis method, it is difficult to maintain the stability of the reaction system only by the structure-guiding effect of the seed crystals. As a result, the phase region of the synthesized β molecular sieves is very narrow. It is more difficult to control the actual reaction conditions, and it is easier to produce miscellaneous crystals

Method used

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

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preparation example Construction

[0043] A kind of preparation method of β molecular sieve provided by the present invention, this preparation method comprises:

[0044] (1) Synthesis of initial gel: mix silicon source, aluminum source, alkaline metal source, and water, stir evenly, and synthesize initial gel; silicon source is SiO 2 In terms of aluminum source as Al 2 o 3 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 =30~150,Na 2 O / SiO 2 =0.03~0.35,H 2 O / SiO 2 =3.0~50.0; preferably: SiO 2 / Al 2 o 3 =30~95:1, Na 2 O / SiO 2 =0.07~0.30:1,H 2 O / SiO 2 =3.5~22:1;

[0045] (2) Microwave treatment of the initial gel: add β molecular sieve seed crystals to the initial gel prepared in step (1), the 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 3% to 25% of the effective mass, mixed evenly and then heated by microwave at a temperature ...

Embodiment 1

[0064] Add 28.43 g of deionized water and 0.42 g of sodium hydroxide into a container in a water bath at 70° C., and stir to dissolve. Add 1.65g of sodium metaaluminate and stir to dissolve. Add 15.00g of coarse-porous silica gel and stir evenly. Add 1.80 g of β molecular sieve seed crystals and stir evenly to obtain an initial gel. Microwave treatment was performed on the initial gel at a controlled temperature of 120°C for 4 hours to obtain a crystallized precursor gel. Then microwave heating was carried out to carry out the crystallization reaction, the temperature was controlled at 170° C., and the reaction time was 10 h. After the reaction was completed, the product was 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 28.43 g of deionized water and 0.42 g of sodium hydroxide into a container in a water bath at 70° C., and stir to dissolve. Add 1.65g of sodium metaaluminate and stir to dissolve. Add 15.00g of coarse-porous silica gel and stir evenly. Add 0.75 g of β molecular sieve seed crystals and stir evenly to obtain an initial gel. Microwave treatment was performed on the initial gel at a controlled temperature of 120°C for 4 hours to obtain a crystallized precursor gel. Then microwave heating was carried out to carry out the crystallization reaction, the temperature was controlled at 170° C., and the reaction time was 10 h. After the reaction was completed, the product was 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 method comprises the following steps: step 1, synthesizing initial gel: mixing a silicon source, an aluminum source, an alkaline metal source and water, and performing uniform stirring to synthesize the initial gel, wherein based on SiO2 of the silicon source, Al2O3 of the aluminum source, and Na2O of the alkaline metal source, molar ratios of raw materials for synthesizing the initial gel are as follows: SiO2 / Al2O3=(30-150):1, Na2O / SiO2=(0.03-0.35):1, and H2O / SiO2=(3.0-50.0):1; step 2, performing microwave treatment on the initial gel: adding a beta molecular sieve seed crystal into the initial gel prepared in the step 1, wherein a ratio of silicon to aluminum in the seed crystal is as follows: SiO2 / Al2O3=(20-100):1, and the adding amount is 3%-25% by mass of SiO2, performing uniform mixing, and performing microwave heating treatment to obtain crystallized precursor gel; and step 3, performing a crystallization reaction: performing a crystallization reaction on the crystallized precursor gel obtained in the step 2 by microwave heating to obtain the beta molecular sieve product, wherein the reaction temperature is 140-180 DEG C, and the reaction time is 4-20 h. According to the method provided by the invention, the molecular sieve obtained by the method has a smaller particle size, a rich pore structureand a relatively-smooth channel, thereby facilitating promoting catalytic cracking and isomerization.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B82Y40/00
CPCB82Y40/00C01B39/02C01P2002/72C01P2004/03C01P2004/64C01P2006/12C01P2006/14
Inventor 崔岩王晓化沈宜泓李梦晨于宏悦庞新梅李发永
Owner PETROCHINA CO LTD
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