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Method for preparing high-performance titanium and silicon molecular sieve

A titanium-silicon molecular sieve, high-performance technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of poor product catalytic performance and high production costs

Active Publication Date: 2012-08-01
SHANGHAI NOVEL CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is the problem of high production cost and poor catalytic performance of the product in the prior art, and a method for synthesizing titanium-silicon molecular sieves with low water ratio and ammonium fluoride-assisted crystallization is provided

Method used

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  • Method for preparing high-performance titanium and silicon molecular sieve
  • Method for preparing high-performance titanium and silicon molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Weigh 15g of tetrapropylammonium bromide (TPABr content> 99 wt %), dissolved in 25g water, added 2.4g hydrogen peroxide solution (H 2 O 2 The content is 27wt%), 4g tetrabutyl titanate (TBOT, TiO 2 Content> 23 wt %), using concentrated ammonia (NH 3 The content is 25wt%) adjust the pH to 11, stir until it is clear, and then add 36g silica sol (SiO 2 The content is 31.4wt%), add water to form a molar ratio of 1 SiO 2 : 0.06 TiO 2 : 0.30 TPA + : 0.24 H 2 O 2 : 25H 2 The crystallization mother liquor of O was mixed well and transferred to a stainless steel crystallization kettle lined with polytetrafluoroethylene. It was dynamically crystallized at 170°C for 48 hours. The product was filtered, washed, and dried at 120°C for 6 hours, and then at 550°C. It is calcined for 4 hours to remove the template to obtain the original powder C of the titanium silicate molecular sieve.

Embodiment 2

[0024] Weigh 5g of tetrapropylammonium bromide (TPABr content> 99 wt %), dissolved in 15g water, added 2.4g hydrogen peroxide solution (H 2 O 2 The content is 27wt%), 4g tetrabutyl titanate (TBOT, TiO 2 Content> 23 wt %), using concentrated ammonia (NH 3 The content is 25wt%) adjust the pH to 12, stir until clear, and then add 36g silica sol (SiO 2 The content is 31.4wt%), add water to form a molar ratio of 1 SiO 2 : 0.06 TiO 2 : 0.10 TPA + : 0.24 H 2 O 2 : 25H 2 The crystallization mother liquor of O was mixed well and transferred to a stainless steel crystallization kettle lined with polytetrafluoroethylene. It was dynamically crystallized at 170°C for 48 hours. The product was filtered, washed, and dried at 120°C for 6 hours, and then at 550°C. It is calcined for 4 hours to remove the template agent to obtain the original powder D of titanium silicate molecular sieve.

Embodiment 3

[0026] Weigh 5g of tetrapropylammonium bromide (TPABr content> 99 wt %) and 1.4g ammonium fluoride (NH 4 F content> 99wt%), dissolved in 15g water, added 2.4g hydrogen peroxide solution (H 2 O 2 The content is 27wt%), 4g tetrabutyl titanate (TBOT, TiO 2 Content> 23 wt %), using concentrated ammonia (NH 3 The content is 25wt%) adjust the pH to 12, stir until clear, and then add 36g silica sol (SiO 2 The content is 31.4wt%), add water to form a molar ratio of 1 SiO 2 : 0.06 TiO 2 : 0.10 TPA + : 0.20 F - : 0.24 H 2 O 2 : 25H 2 The crystallization mother liquor of O was mixed well and transferred to a stainless steel crystallization kettle lined with polytetrafluoroethylene. It was dynamically crystallized at 170°C for 48 hours. The product was filtered, washed, and dried at 120°C for 6 hours, and then at 550°C. It is calcined for 4 hours to remove the template agent to obtain the original titanium silicate powder E.

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Abstract

The invention relates to a method for preparing a high-performance titanium and silicon molecular sieve. The method comprises the following steps of: 1) uniformly mixing tetrapropylammonium bromide, ammonium fluoride, water and a hydrogen peroxide solution to obtain a clarified solution A; 2) under the condition of stirring, adding a titanium source into the solution A, adjusting the pH to be 10 to 13 by using ammonia water, and ageing until a light yellow clarified solution B is formed; 3) adding a silicon source into the solution B, and uniformly mixing to obtain crystallized mother liquor C; and 4) crystallizing the crystallized mother liquor C at the temperature of between 130 and 190 DEG C and self-generated pressure for 10 to 100 hours, and separating to obtain the solid titanium and silicon molecular sieve product. According to the method, the problems of high production cost and low catalysis performance of the titanium molecular sieve in the prior art are well solved; and the method for assisting in synthesizing the titanium and silicon molecular sieve by using low-water-ratio ammonium fluoride can be applied to industrial production of the titanium and silicon molecular sieve.

Description

Technical field [0001] The present invention involves a preparation method for a high -performance titanium silicon molecule sieve, which is the field of inorganic material synthesis. [0002] Background technique [0003] In 1983, the US patent US4410501 first reported the successful synthesis of titanium silicon molecules TS-1.Similar to the current widely used ZSM-5 molecular sieve, this material also has a MFI topology structure. Its channel structure can accommodate the entry of most branches and single-ring organic objects, combined with its efficient catalytic hydrogen peroxide characteristics.Molecular sieves are widely used in many fields such as petrochemical and fine chemicals, and the future market development potential is huge. [0004] The classic synthetic path of the TS-1 molecular sieve is mixed crystallization of orthopedic silica ethyl, titanium titanate, tetraxide ammonium oxide, and appropriate amount of water.Tetrabal-based ammonium oxide is expensive and la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89
Inventor 夏建超夏娟文怀有谈赟
Owner SHANGHAI NOVEL CHEM TECH
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