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Titanium silicalite molecular sieve synthesizing method

A technology of titanium-silicon molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., and can solve the problem of low activity of titanium-silicon molecular sieve

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the preparation method of titanium silicon molecular sieve disclosed by Thangaraj et al. (Zeolites, 1992, Vol.12 pages 943-950), in order to balance the hydrolysis speed of organosilicon and titanium, isopropanol is introduced in the hydrolysis process of titanium, but this method The activity of the obtained titanium silicate molecular sieve is not high

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  • Titanium silicalite molecular sieve synthesizing method
  • Titanium silicalite molecular sieve synthesizing method
  • Titanium silicalite molecular sieve synthesizing method

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Embodiment approach

[0037] The synthetic method of titanium silicon molecular sieve provided by the present invention, a kind of preferred embodiment, comprises the following steps:

[0038] (1) Mix template agent, titanium source, organosilicon source, water, polyhydric alcohol and optional inorganic ammonium source to hydrolyze the titanium source and organosilicon source, and remove the produced monohydric alcohol from the mixture, i.e. hydrolyze Alcohol, and then add peroxide; Said hydrolysis of alcohol, usually at 0~150 ℃, such as 0~100 ℃, such as 50~95 ℃, the resulting mixture is stirred for at least 10 minutes, wherein the stirring time of stirring is 10 minutes~ 50 hours; where the inorganic ammonium source (as NH 4 + Calculated): Titanium source (as TiO 2 The molar ratio of meter) is 0~5:1;

[0039] (2) Aging the product obtained in step (1), the aging is to leave the product obtained in step (1) at room temperature to 50°C for 1 to 60 hours, such as 2 to 50 hours or 3 to 30 hours, fu...

Embodiment 1

[0089] Mix 21.5g tetraethyl silicate, 1.11g glycerin and 6.50g tetrapropylammonium hydroxide aqueous solution (25.05% by weight), add 59.8g deionized water and mix evenly; then hydrolyze at 60°C for 1.0h to obtain silicic acid Hydrolyzate of tetraethyl ester. Then, under the action of vigorous stirring, a solution consisting of 1.1 g of tetrabutyl titanate and 5.0 g of isopropanol was slowly dropped into the above hydrolyzate, and the mixture was stirred at 75°C for 3 hours to obtain a clear and transparent colloid , adding 0.88g concentration of 30% by weight hydrogen peroxide. Then move the colloid into a closed stainless steel reaction kettle, and crystallize at a constant temperature at 170° C. for 3 days to obtain TS-1 molecular sieve. Its XRD analysis spectrum is as figure 1 As shown, it has an MFI structure.

Embodiment 2

[0095] (1) 15g concentration is the tetrapropyl ammonium hydroxide aqueous solution of 25.05% by weight, 2.04g tetrabutyl titanate, 8.5g tetraethyl silicate, 4.97g glycerol, 2.1g concentration is the ammoniacal liquor of 20% by weight and 35.6 Add g water into a 500ml beaker in turn, put it into a magnetic stirrer with heating and stirring functions, mix evenly, and heat at 80°C for 4 hours, and replenish the evaporated water at any time to obtain a colorless transparent hydrolyzate. Alcohol content is no more than 10ppm (mass), then add 1.2g of hydrogen peroxide with a concentration of 30% by weight, and stir evenly;

[0096] (2) aging the product obtained in step (1) at room temperature for 12 hours to obtain an aging product;

[0097] (3) Add 9.6g of white carbon black powder to the above aging product under stirring, and stir for 1 hour after adding, forming a "viscous body". After 2 days, the TS-1 sample was obtained. The obtained TS-1 sample was filtered, washed, dried ...

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Abstract

The invention discloses a titanium silicalite molecular sieve synthesizing method which comprises the following steps: forming a crystallization mixture from a titanium source, a template agent, water, polyhydric alcohols, peroxide, a silicon source and an optional inorganic ammonium source, crystallizing, and recycling the titanium silicalite molecular sieve, wherein the silicon source refers to an organic silicon source and / or a solid silicon source. According to the method, the activity of the synthesized titanium silicalite molecular sieve can be improved, and the grain size is reduced.

Description

technical field [0001] The invention relates to a titanium silicon molecular sieve and a synthesis method thereof. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, MCM-22 with MWW structure and TS-48 with larger pore structure have been synthesized. Among them, TS-1 was first developed and synthesized by Italian EniChem Company. It is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. TS-1 It not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. Using this titanium-silicon molecular sieve as a catalyst can catalyze various types of organic oxidation reactions, such as epo...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 林民夏长久朱斌彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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