Synthetic method of Beta molecular sieve with low silica-alumina ratio

A kind of technology of low silicon-aluminum ratio, synthesis method

Active Publication Date: 2020-06-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, there are still some problems in the reported synthesis methods of Beta molecular sieves: high cost, cumbersome preparation process, low preparation reproducibility, low product yield, etc., which limit its industrial production to a certain extent.

Method used

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  • Synthetic method of Beta molecular sieve with low silica-alumina ratio
  • Synthetic method of Beta molecular sieve with low silica-alumina ratio
  • Synthetic method of Beta molecular sieve with low silica-alumina ratio

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Experimental program
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Embodiment 1

[0065] Weigh 0.08 g of sodium metaaluminate and 6.48 g of 25% tetraethylammonium hydroxide solution, mix well, add 6.6 g of 40% silica sol solution, and then stir evenly. Transfer the mixed solution into a polytetrafluoroethylene-lined stainless steel reaction kettle, raise the temperature to 160°C and keep it for 1 day, cool to room temperature and take it out, then add 0.05g of sodium metaaluminate and 3.9g of water to it, stir well and put The mixed solution was then transferred into a polytetrafluoroethylene-lined stainless steel reaction kettle, heated to 160°C for 2 days, cooled to room temperature, washed with deionized water for 3 times, dried in an oven at 120°C, and roasted at 550°C for 12 hours , to prepare Beta molecular sieves. Its XRD spectrum is attached Figure 4 ; NH 3 -TPD diagram attached Figure 5 . The Si / Al and acid content characterization results of the obtained Beta molecular sieves are summarized in Table 1.

Embodiment 2

[0067] Weigh 0.08g of sodium metaaluminate and 7g of 25% tetraethylammonium hydroxide solution, mix well, add 6.6g of 40% silica sol solution, and then stir evenly. Transfer the mixed solution into a polytetrafluoroethylene-lined stainless steel reaction kettle, raise the temperature to 170°C and keep it for 1 day. After cooling to room temperature, add 0.12g of sodium metaaluminate and 3.9g of water to it, stir well, and put The mixed solution was then transferred into a polytetrafluoroethylene-lined stainless steel reaction kettle, heated to 170°C for 2 days, cooled to room temperature, washed with deionized water for 3 times, dried in an oven at 120°C, and roasted at 550°C for 12 hours , to prepare Beta molecular sieves. The Si / Al and acid content characterization results of the obtained Beta molecular sieves are summarized in Table 1.

Embodiment 3

[0069] Weigh 0.08 g of sodium metaaluminate and 7.5 g of 25% tetraethylammonium hydroxide solution, mix well, add 6.6 g of 40% silica sol solution, and then stir evenly. Transfer the mixed solution into a polytetrafluoroethylene-lined stainless steel reaction kettle, raise the temperature to 170°C and keep it for 1 day, then cool to room temperature, then add 0.32g of sodium metaaluminate and 3.9g of water to it, stir the mixed solution evenly Move it into a polytetrafluoroethylene-lined stainless steel reaction kettle, raise the temperature to 170°C and keep it for 2 days, then cool it to room temperature, wash it with deionized water for 3 times, dry it in an oven at 120°C, and roast it at 550°C for 12 hours to obtain Beta molecular sieve. The Si / Al and acid content characterization results of the obtained Beta molecular sieves are summarized in Table 1.

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Abstract

The invention discloses a synthesis method of a Beta molecular sieve with a low silica-alumina ratio. The method comprises the following steps: 1) crystallizing a mixture A containing a silicon source, an aluminum source, a template agent R and water at 80-300 DEG C for 5-72 hours to obtain a mixture B, wherein the template agent R is at least one selected from organic amines; 2) adding an aluminum source and water into the mixture B to obtain a mixture C; and 3) crystallizing the mixture C at 80-300 DEG C for 5-72 hours, separating, and roasting at 500-800 DEG C for 5-36 hours to obtain the Beta molecular sieve with low silica-alumina ratio.

Description

technical field [0001] The application relates to a method for synthesizing Beta molecular sieves with a low silicon-aluminum ratio, and belongs to the field of molecular sieve synthesis. Background technique [0002] Beta molecular sieve is a molecular sieve with a three-dimensional structure and a twelve-membered ring cross structure. It is widely used in alkane isomerization due to its large specific surface area, unique mechanism and good hydrothermal stability. NH 3 It is an important industrial molecular sieve catalyst in petroleum refining and fine chemical catalytic reactions such as oxidative degradation, VOC oxidation, and aromatic hydrocarbon alkylation. [0003] Huang et al. (Huang Gang, Ji Peng, Xu Hao, et a1. Microporous and Mesoporous Materials, 2017, 248:30-39.) used lamellar H-type hydrosilica as a silicon source, through 170℃ high temperature hydrothermal crystallization Within 0-24 hours, a hierarchically porous Beta molecular sieve was rapidly prepared. ...

Claims

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Application Information

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IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72
Inventor田志坚王帅旗王从新吕广王苹王小平
OwnerDALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI