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A kind of preparation method of SSZ-13 molecular sieve catalyst

A molecular sieve and catalyst technology, applied in the field of molecular sieve, can solve the problems of long preparation time of SSZ-13, and achieve the effect of high yield, simple and fast operation

Active Publication Date: 2021-07-20
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In 1985, the preparation method of SSZ-13 molecular sieve was first disclosed in U.S. Patent No. 4,544,538, and the template agent was N,N,N-trimethyl-1-adamantylamine cation; in 2006, Zones patent No.60 / 826,882 Disclosed in the combined use of benzyl quaternary ammonium ions and N,N,N-trimethyl-1-adamantylamine cations to prepare SSZ-13 molecular sieves; in 2006, Miller in the invention patent No.60 / 882,010 Among them, SSZ-13 was successfully prepared by using benzyl trimethyl quaternary ammonium ion instead of the traditional template; in 2013, Chen Biaohua of Beijing University of Chemical Technology and others mentioned in the patent with the announcement number CN103601211B that choline chloride was used as the structure Directing agent, successfully prepared SSZ-13 molecular sieve; the problem of long preparation time of SSZ-13 by the above method has not been solved

Method used

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  • A kind of preparation method of SSZ-13 molecular sieve catalyst
  • A kind of preparation method of SSZ-13 molecular sieve catalyst
  • A kind of preparation method of SSZ-13 molecular sieve catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Weigh 0.31g of sodium hydroxide and 23.10g of deionized water, mix well, stir at room temperature for 30min, add 2.57g of N,N,N-trimethyl-1-adamantyl ammonium hydroxide dropwise, stir for 30min, add 4.04g of ZSM -5 molecular sieve (SiO 2 / Al 2 o 3 =38), stirred at 25°C for 30min, and aged for 1h.

[0027] The solution obtained above was transferred to a reaction kettle, heated to 160°C for crystallization, and crystallized for 4 hours. The obtained product was washed, filtered and dried; the dried sample was fully calcined at 450°C for 5 hours to obtain the SSZ-13 sample.

[0028] figure 1 The XRD information of the obtained SSZ-13 molecular sieve is given.

[0029] The XRD pattern shows that it is SSZ-13 molecular sieve, no miscellaneous crystals appear, and it has good crystallinity.

Embodiment 2

[0031] Weigh 0.28g of sodium hydroxide and 23.10g of deionized water, mix well, stir at room temperature for 30min, add dropwise an appropriate amount of N,N,N-trimethyl-1-adamantyl ammonium hydroxide 2.07g, stir at room temperature for 30min, add 2g ZSM-5 molecular sieve (SiO 2 / Al 2 o 3 =80), stirred at 25°C for 30min, and aged for 4h.

[0032] Transfer the solution obtained above to a reaction kettle, raise the temperature to 140°C for crystallization, and crystallize for 16 hours. The obtained product is washed, filtered and dried; the dried sample is fully calcined at 500°C for 6 hours to obtain SSZ-13 molecular sieve.

[0033] figure 2 The XRD information of the obtained SSZ-13 molecular sieve is given.

[0034] The XRD pattern shows that it is SSZ-13 molecular sieve, no miscellaneous crystals appear, and it has good crystallinity.

Embodiment 3

[0036] Weigh 0.31g of potassium hydroxide and 18.96g of deionized water, mix well, stir at room temperature for 30min, add dropwise an appropriate amount of N,N,N-trimethyl-1-adamantyl ammonium hydroxide 4.57g, stir at room temperature for 30min, add 2.69 g ZSM-5 molecular sieve (SiO 2 / Al 2 o 3 =200), stirred at 25°C for 30min, and aged for 8h.

[0037] The solution obtained above was transferred to a reaction kettle, heated to 200°C for crystallization, and crystallized for 48 hours. The obtained product was washed, filtered, and dried; the dried sample was fully calcined at 550°C for 4 hours to obtain SSZ-13 molecular sieve.

[0038] image 3 Given the obtained SSZ-13 molecular sieve XRD information, Figure 4 The SEM image of the sample is given, showing the crystal morphology and size of SSZ-13 molecular sieve.

[0039] The XRD pattern shows that it is SSZ-13 molecular sieve with no miscellaneous crystals and high crystallinity. The scanning electron microscope shows...

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Abstract

The invention belongs to the field of molecular sieves, and specifically relates to a preparation method of a SSZ-13 molecular sieve catalyst, which uses ZSM-5 molecular sieve as a raw material, completes crystal conversion under the guidance of a template agent, and directly converts ZSM-5 molecular sieve into SSZ by means of crystal transformation ‑13 molecular sieve; this method is simple to operate, greatly improves the yield of SSZ‑13, the amount of template agent is less, the preparation time is short, and large-scale industrial production can be realized; at the same time, the synthesized SSZ‑13 molecular sieve has good crystallinity and high yield High, small crystal size and other characteristics.

Description

technical field [0001] The invention belongs to the field of molecular sieves, and in particular relates to a preparation method of an SSZ-13 molecular sieve catalyst. Background technique [0002] Molecular sieves have the characteristics of well-organized pore structure, large specific surface area, surface protonic acid centers and cation exchange properties; molecular sieves have attracted extensive attention from the industry because of their industrial value. [0003] According to the report of the International Zeolite Association (IZA), SSZ-13 zeolite has a CHA topology, mainly including basic units such as 4-, 6-, and 8-membered rings, and these basic units are cross-linked into a three-dimensional network structure. The network structure has uniform pores, and the largest ring in the CHA structure is an eight-membered ring with a diameter of 0.38nm. Therefore, only compounds with a molecular diameter of less than 0.38 nm are allowed to enter the cage, and macromol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/80B01J29/70B01J29/40
CPCB01J29/40B01J29/7015B01J29/80
Inventor 王广建李强邴连成韩德志王芳
Owner QINGDAO UNIV OF SCI & TECH