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Method for rapid synthesis of titanium silicate molecular sieve

A titanium-silicon molecular sieve, fast technology, applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of long synthesis crystallization time, reduce production cost, shorten crystallization time, etc., achieve easy separation, low raw material cost, molecular crystal large grain effect

Inactive Publication Date: 2015-04-22
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problems of high cost and long crystallization time in the prior art, the present invention provides a new method for rapidly synthesizing titanium-silicon molecular sieves under microwave radiation conditions. Using the method provided by the present invention, due to the use of inorganic titanium-silicon raw materials and A small amount of template agent reduces the production cost, greatly shortens the crystallization time, and can be synthesized quickly, overcoming the disadvantage of the long crystallization time of titanium-silicon molecular sieve synthesis

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  • Method for rapid synthesis of titanium silicate molecular sieve
  • Method for rapid synthesis of titanium silicate molecular sieve
  • Method for rapid synthesis of titanium silicate molecular sieve

Examples

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Embodiment example 1

[0038]Use silica sol, titanium sulfate, and tetrapropylammonium hydroxide as templates, add ammonia water to adjust the alkalinity, and deionized water at a ratio of 1:0.013-0.035:0.025-0.2:25-45:15-35, wherein Si / TPA + =0.08 and different order of addition to mix glue, use ammonia water (NH 3 ) to adjust the alkalinity of the glue, add seed crystals, and stir continuously. After stirring for 1-5 hours, the gel solution is transferred to a microwave-specific polytetrafluoroethylene autoclave (30ml / 100ml), and the microwave power is adjusted. 400W-1600W, the crystallization temperature is 160-180°C, crystallize for 2-30h, then take it out to cool, filter, wash with distilled water several times until the filtrate is neutral, and then dry (> 12 hours), 550°C Roast at high temperature for 5-10 hours to obtain titanium silicon molecular sieve TS-1 raw powder. Mix the TS-1 raw powder obtained above with ammonia solution, adjust the pH to 8-13, keep the temperature at 130-190°C, an...

Embodiment example 2

[0042] Use silica sol, titanium sulfate, and tetrapropylammonium hydroxide as templates, add ammonia water to adjust the alkalinity, and deionized water at a ratio of 1:0.013-0.035:0.025-0.2:25-45:15-35, wherein Si / TPA + =0.08 and different order of addition to mix glue, use ammonia water (NH 3 ) to adjust the alkalinity of the glue, add seed crystals, and stir continuously. After stirring for 1-5 hours, the gel solution is transferred to a microwave-specific polytetrafluoroethylene autoclave (30ml / 100ml), and the microwave power is adjusted. 400W-1600W, the crystallization temperature is 160-180°C, crystallize for 2-30h, then take it out to cool, filter, wash with distilled water several times until the filtrate is neutral, and then dry (> 12 hours), 550°C Roast at high temperature for 5-10 hours to obtain titanium silicon molecular sieve TS-1 raw powder. Then mix the original powder with ammonia solution, adjust the pH to 8-13, keep the temperature at 130-190°C under microw...

Embodiment example 3

[0044] The steps are the same as the implementation case 1, changing Si / TPA + The ratio is 0.12.

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Abstract

The invention relates to a method for rapid synthesis of a titanium silicate molecular sieve and is characterized in that cheap inorganic raw materials are employed to synthesize the titanium silicate molecular sieve rapidly through microwave radiation hydro-thermal synthesis. The method of the invention can synthesize a titanium silicate molecular sieve TS-1 with excellent catalysis performance in a short time, and the prepared TS-1 has large particle and is easily separated after the catalytic reaction. The invention solves insufficiencies of high cost and long crystallization time in a prior art.

Description

technical field [0001] The invention relates to a method for rapidly synthesizing a titanium-silicon molecular sieve. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the 1980s. Titanium was successfully introduced into the molecular sieve framework, making molecular sieve resorption and separation, and acid-catalyzed reaction into the field of catalytic oxidation, which greatly expanded the application field of molecular sieves. After years of research, TS-1 with MFI topology, TS-2 with MEL structure and a new type of Ti-MWW molecular sieve have been synthesized. In particular, TS-1 exhibits excellent catalytic performance in a series of oxidation reactions using H2O2 as an oxygen source. The reaction conditions are mild, the process is simple and safe, and there is no secondary pollution. , Cyclohexanone ammoxidation and other reactions are widely used. [0003] The traditional synthesis method of mol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 周继承郑香兰王蒙谌敏飞
Owner XIANGTAN UNIV