Method for synthesizing molecular sieve

A molecular sieve and supergravity reactor technology, applied in the direction of molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as long aging time and reaction time, complicated molecular sieve synthesis process, cumbersome aging process, etc., to achieve aging Ultra-short crystallization time, good catalytic effect, and high single-pot efficiency

Pending Publication Date: 2020-05-08
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the method described in the above patents, the aging process is cumbersome, the crystallization process is basically static crystallization, the zeolite growth process is not stirred, the required aging time is 4h to 48h and the reaction time is long, and the synthesis process of preparing molecular sieves is relatively complicated.

Method used

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  • Method for synthesizing molecular sieve
  • Method for synthesizing molecular sieve
  • Method for synthesizing molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Synthesis method: After the flow rate of the supergravity metering pump is corrected, it is washed and used. Add 9g of tetrapropylammonium hydroxide and 0.09g of aluminum sulfate octadecahydrate to 15g of water, and add 6.7g of silica sol. Pass the above solution into the supergravity reactor, adjust the flow rate to 50ml / min, adjust the supergravity speed to 1500rpm, circulate into the supergravity reactor, and after the residence time is 8min, recover the solution to obtain the liquid to be crystallized. Then put it into a crystallization kettle, raise the temperature to 180°C, and crystallize under 150rpm stirring for 8h. After the reaction, cool to room temperature, wash and centrifuge with deionized water for 3 times, dry at 80°C for 12h, and roast to obtain the final product.

[0034] figure 1 It is the XRD spectrogram of the product obtained in Example 1, it can be seen that the product has the characteristic diffraction peak of ZSM-5, and has a higher crystalli...

Embodiment 2

[0036] Using the same conditions as in Example 1, changing the residence time to 15min, adjusting the high-gravity reactor flow to 60ml / min, to obtain the final product. According to the XRD characterization results of the sample, it can be seen that the product has ZSM-5 characteristic diffraction peaks, and the SEM photo shows that the sample is a uniform nano-ZSM-5 molecular sieve with a slightly increased particle size.

Embodiment 3

[0038] Using the same conditions as in Example 1, changing the residence time to 20min, adjusting the high-gravity reactor speed to 1600rpm, to obtain the final product. According to the XRD characterization results of the sample, it can be seen that the product has ZSM-5 characteristic diffraction peaks, and the SEM photo shows that the sample is a uniform nano-ZSM-5 molecular sieve with uniform particle size.

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Abstract

The invention belongs to the technical field of zeolite molecular sieve synthesis, and particularly relates to a method for synthesizing a molecular sieve under super-gravity within a super-short time. The method is mainly characterized in that cheap raw materials are aged into a gel in a super-gravity reactor, and stirring and hydrothermal crystallization are carried out in a crystallization process, and after the crystallization is finished, filtering, washing and drying are performed to obtain a uniformly distributed nano zeolite product. The method is low in synthesis cost, super-short inaging crystallization time, high in purity of the obtained zeolite, simple in operation process, high in single-kettle yield and capable of reducing mother liquor discharge. According to the invention, the sample XRD shows that the obtained product is good in crystallinity, the SEM shows that the nano zeolite is uniformly distributed, and the method can be used for industrial synthesis of molecular sieves.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, which belongs to the technical field of synthesizing zeolite molecular sieves, in particular to a synthesis method for synthesizing zeolite molecular sieves of different sizes in a super-gravity and ultra-short time. Background technique [0002] Due to the action of centrifugal force, the liquid is highly dispersed in the packing layer, the degree of turbulence is increased, the mixing is intensified, and the mass transfer efficiency is greatly improved. Compared with traditional equipment, the volume mass transfer coefficient of the high-gravity rotating bed can be increased by 1 to 2 orders of magnitude, so that the purpose of reducing the size of the equipment, reducing investment costs and shortening the crystallization time can be achieved. Conventional molecular sieve synthesis aging time needs 4-48h, and the cost is high. [0003] CN108217674A discloses a kind of supergravity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40C01B39/48
CPCC01B39/40C01B39/48C01P2002/72C01P2004/03
Inventor 滕加伟史静徐建军
Owner CHINA PETROLEUM & CHEM CORP
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