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Synthetic method of siliceous molecular sieve

A synthesis method and technology of silicon molecular sieve, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of high energy consumption and poor economy, and achieve the effects of reducing energy consumption, reducing the production of finished products, and improving the production capacity of a single kettle

Inactive Publication Date: 2012-06-27
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems in the prior art, the present invention provides a method for preparing silicon-containing molecular sieves, which solves the problems of high energy consumption and poor economic efficiency of molecular sieve products per unit weight in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 160L of tetraethylammonium hydroxide aqueous solution with a mass fraction of 25% into the reactor, add tetraethylammonium hydroxide to the reactor under stirring conditions, so that the mol ratio of tetraethylammonium hydroxide to the silicon source is 1:32. Stirring was stopped after feeding, and the precursor solution sol was changed to a gel state after aging for 6 hours at room temperature. Raise the temperature to 100°C and crystallize for 80h. After cooling down to room temperature, it was washed by membrane filtration until the filtrate was neutral, dried at 100°C for 10 hours, and calcined at 500°C for 8 hours to obtain 321kg of S-1 molecular sieve.

[0028] After a certain post-treatment, the obtained S-1 was applied to the gas-phase Beckmann rearrangement of cyclohexanone oxime to produce caprolactam at a reaction temperature of 330°C, a reaction pressure of 0.1MPa, and a weight space velocity of 1h -1 Under the conditions, when the weight ratio of ammo...

Embodiment 2

[0030] Put 140L of 35% tetrapropylammonium hydroxide aqueous solution into the reactor by mass fraction, add 25% silica sol in the reactor under stirring condition, make the mol ratio of tetrapropylammonium hydroxide and silicon source be 1:24. Stirring was stopped after feeding, aged at room temperature for 2 hours, heated to 140°C, and crystallized for 72 hours. After cooling down to room temperature, it was washed by membrane filtration until the filtrate was neutral, dried at 120°C for 8 hours, and calcined at 650°C for 6 hours to obtain 278kg of S-1 molecular sieve.

[0031] After a certain post-treatment, the obtained S-1 was applied to the gas-phase Beckmann rearrangement of cyclohexanone oxime to produce caprolactam. The reaction temperature was 350°C, the reaction pressure was 0.1MPa, and the weight space velocity was 2h. -1 Under the conditions, when the weight ratio of ammonia, water, cyclohexanone oxime and methanol is 0.006:0.5:30:70, after 400 hours of reaction,...

Embodiment 3

[0033] Put 150L of tetrapropylammonium hydroxide aqueous solution with a mass fraction of 20% into the reaction kettle, add ethyl orthosilicate into the reaction kettle under stirring conditions, stir for 1 hour, and then add the isopropanol solution of butyl titanate Add it into the reaction kettle so that the molar ratio of tetrapropylammonium hydroxide, titanium source and silicon source is 1:1:24. Stirring was stopped after feeding, aged at room temperature for 10 hours, heated to 170°C, and crystallized for 120 hours. After cooling down to room temperature, it was washed by membrane filtration until the filtrate was neutral, dried at 120°C for 6 hours, and calcined at 600°C for 6 hours to obtain 202kg of TS-1 molecular sieve.

[0034] After a certain post-treatment, the obtained TS-1 is applied to the reaction of cyclohexanone ammoximation to cyclohexanone oxime, and reacted in a batch reactor at a reaction temperature of 75°C and a reaction pressure of 0.3MPa Under the ...

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Abstract

The invention provides a preparation method of a siliceous molecular sieve, in particular to a gelatin crystallization method. The siliceous molecular sieve is synthesized under the condition of a high-concentration organic base template; a silicon source and the high-concentration organic base template, or the silicon source, a titanium source and the high-concentration organic base template are mixed in a certain proportion to prepare the precursor lyosol of the molecular sieve; the lyosol is aged for 1 to 10 h at ambient temperature, so as to obtain precursor lyogel; and the lyogel is put into a high-pressure crystallization kettle to be crystallized for 3 to 7 d at the temperature of 200 DEG C, and then is washed, dried and roasted, so as to obtain the S-1or TS-1 molecular sieve. Through the adoption of the method, the concentration of the template is increased, and a precursor liquid is crystallized in a gel state, so as to improve the productivity of the single kettle and reduce the production cost. S-1 and TS-1 molecular sieve catalysts prepared by using the method are respectively applied to the cyclohexanone-oxime gas phase reaction for preparing caprolactam and the cyclohexanone ammoximation reaction for preparing cyclohexanone oxime, and both achieve better catalytic effects. Therefore, the preparation method has an industrial application value.

Description

technical field [0001] The invention relates to a method for preparing silicon-containing molecular sieves, belonging to the technical field of molecular sieve preparation. Background technique [0002] Silicon-containing molecular sieves S-1 and TS-1 are catalytic materials with MFI topology, which are widely used in the petrochemical industry. S-1 molecular sieves are mainly used in Beckmann gas phase rearrangement reactions; TS-1 molecular sieves are mainly used in in rare H 2 o 2 Participate in reactions such as olefin epoxidation, cyclohexanone ammoximation, aromatic hydrocarbon hydroxylation and other reactions. Especially in the green caprolactam production process, cyclohexanone ammoximation to cyclohexanone oxime and cyclohexanone oxime vapor-phase Beckmann rearrangement to caprolactam use TS-1 and S-1 molecular sieve catalysts respectively. The catalyst has been industrially applied. [0003] Patent CN102120589A discloses a preparation method of S-1 all-silicon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 袁海鹏王绍伟刘文张媛王元平宋辉梁莹史文涛钱震王志文孙世谦曹振岩王海国张蒙袁学民王志远刘俊生张舜光
Owner CHINA TIANCHEN ENG
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