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The preparation method of stf zeolite molecular sieve

A zeolite molecular sieve and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of increasing the preparation cost of STF molecular sieve, complex organic template structure, limited availability, etc., to facilitate promotion, enhance structure orientation, and operability strong effect

Active Publication Date: 2021-11-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The organic templates in the above methods are complex in structure and expensive, which greatly increases the preparation cost of STF molecular sieves, thereby limiting their usability in industrial processes.

Method used

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  • The preparation method of stf zeolite molecular sieve
  • The preparation method of stf zeolite molecular sieve
  • The preparation method of stf zeolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 41.6g tetraethyl orthosilicate (TEOS) was slowly added dropwise into 76.8g 1,1,2,6-TMPOH aqueous solution (20wt%), stirred at room temperature, and after the hydrolysis was complete, the container was opened and stirred overnight to volatilize ethanol and Part of the water, add 7.5g hydrofluoric acid (40wt%), continue to volatilize part of the water after stirring, until the reaction mixture reaches the following molar composition:

[0025] 0.5(1,1,2,6-TMPOH):SiO 2 :0.75HF:7.5H 2 o

[0026] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 150°C for crystallization for 168 hours. The solid obtained after the reaction is filtered, washed, dried and calcined is STF molecular sieve. The XRD pattern of the sample is as figure 1 As shown, the scanning electron microscope photo is shown as figure 2 shown.

Embodiment 2

[0028] Slowly add 34.7g tetraethyl orthosilicate (TEOS) dropwise into 115g 1,1,2,6-TMPOH aqueous solution (20wt%), stir at room temperature, after the hydrolysis is complete, open the container and stir overnight to volatilize ethanol and some Water, add 30g ammonium fluoride solution (37wt%), continue to volatilize part of water after stirring, until reaction mixture reaches following molar composition:

[0029] 0.9(1,1,2,6-TMPOH):SiO 2 :1.8NH 4 F:18H 2 o

[0030] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 160°C for crystallization for 144 hours. The solid obtained after the reaction is filtered, washed, dried and calcined is STF molecular sieve.

Embodiment 3

[0032] Slowly add 27.7g tetraethyl orthosilicate (TEOS) dropwise into 154g 1,1,2,6-TMPOH aqueous solution (20wt%), stir at room temperature, after the hydrolysis is complete, stir the container open overnight to volatilize ethanol and some Water, add 10g hydrofluoric acid (40wt%) and 13.34g ammonium fluoride solution (37wt%), continue to volatilize part of water after stirring, until the reaction mixture reaches the following molar composition:

[0033] 1.5(1,1,2,6-TMPOH):SiO 2 :1.5HF:1NH 4 F:30H 2 o

[0034] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 175°C for crystallization for 96 hours. The solid obtained after the reaction is filtered, washed, dried and calcined is STF molecular sieve.

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Abstract

The invention relates to a preparation method of an STF zeolite molecular sieve, which mainly solves the problem that the organic template used for synthesizing the STF molecular sieve is too complex in the prior art. The present invention comprises the step of obtaining molecular sieves by contacting tetravalent framework element Y source, framework heteroatom element X source, organic template R, fluorine source and water under crystallization conditions; and optionally, roasting the The step of the molecular sieve that obtains; The molar ratio F of described fluorine source and organic template agent ‑ / R is greater than 1; the organic template R is a TMP containing tetramethylpiperidinium cation + A quaternary ammonium salt or a quaternary ammonium base to obtain a porous crystalline STF zeolite molecular sieve. The invention uses an organic template agent with a simple structure; the synthesis range is wide, the operation is simple and easy, and the promotion is convenient.

Description

technical field [0001] The invention relates to a method for synthesizing zeolite molecular sieves, more precisely, to a method for synthesizing STF zeolite molecular sieves. [0002] technical background [0003] Zeolite molecular sieves are crystalline porous silicate materials that are widely used as adsorbents, ion exchangers, and industrial catalysts. At present, there are 235 molecular sieve topologies approved by the International Molecular Sieve Association. [0004] STF molecular sieve has a one-dimensional 10-membered ring channel structure, and the channel direction is [001]. The earliest molecular sieve with STF topology is SSZ-35. Chevron disclosed in U.S. Patent US 5316753 the use of various conformationally restricted azapolycyclic ring systems as templates to prepare SSZ-35, including 3,3-dimethyl-3-azonium-7- Methyl-7-aza-bicyclononane, N-ethyl-N-methyl-9-azoniumbicyclo[3.3.1]nonane and 1,3,3,8,8-pentamethyl-3 - Azonia bicyclo[3.2.1]octane. The company a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/03
Inventor 付文华袁志庆王振东滕加伟张铁柱
Owner CHINA PETROLEUM & CHEM CORP