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Method for synthesizing titanium silicate molecular sieve employing organic quaternary ammonium salt template agent

A technology of titanium-silicon molecular sieve and organic quaternary ammonium salt, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc. It can solve the problems of low oxidation activity and no further improvement of the activity of titanium-silicon molecular sieves. , to achieve high oxidation activity, improve raw material utilization, and reduce synthesis costs

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

At present, the synthesis of titanium silicon molecular sieves with organic quaternary ammonium salts has the problem of low oxidation activity.
In addition, the prior art does not involve further improving the activity of titanium silicon molecular sieves

Method used

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  • Method for synthesizing titanium silicate molecular sieve employing organic quaternary ammonium salt template agent
  • Method for synthesizing titanium silicate molecular sieve employing organic quaternary ammonium salt template agent
  • Method for synthesizing titanium silicate molecular sieve employing organic quaternary ammonium salt template agent

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Experimental program
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Effect test

Embodiment approach

[0041] (4) Crystallize the titanium-silicon molecular sieve obtained in step (3) in an organic alkali solution, and then recover the titanium-silicon molecular sieve. The titanium-silicon molecular sieve obtained in this process has a hollow structure, which is called molecular sieve rearrangement in the present invention. Among them, titanium silicon molecular sieves (using SiO 2 The molar ratio of the base) to the organic base is 1:0.02~0.5, for example, 1:0.02~0.2; 2 The molar ratio of molecular sieve to water is 1:2~50, for example, 2~30, or 2~20, or 5~10; the crystallization temperature is 120~200°C, and the time is 0.5~8 days; the crystallization pressure For autogenous pressure, wherein said organic base is preferably an organic quaternary ammonium base. Preferably, the crystallization temperature in step (4) is 150-200° C., the crystallization time is 0.5-10 days or 1-6 days, and the molar ratio of molecular sieve to water is 1:2-30. The recovery method is an existi...

Embodiment 1

[0067] (1) 19.65g of tetrapropylammonium bromide (TPABr) aqueous solution with a concentration of 25.05% by weight, 2.04g of tetrabutyl titanate, 8.5g of tetraethyl silicate, 2.42g of ethylenediamine, and 2g of a concentration of 20% Add ammonia water and 35g water into a 500ml beaker in sequence, put them into a magnetic stirrer with heating and stirring functions, mix evenly, and stir at 80°C for 4 hours, replenish evaporated water at any time, and obtain a colorless transparent hydrolyzate .

[0068] (2) Aging the obtained hydrolyzed solution at room temperature (26° C.) for 12 hours to obtain an aging product;

[0069] (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 at 120°C for 24 hours, and roasted at 550°C for 6 hours to obtain the titanium silicon TS-1 molecular sieve product d...

Embodiment 2

[0072] (1) 15g concentration is 25.5% by weight of tetrapropylammonium bromide, 2.04g tetrabutyl titanate, 8.5g tetraethyl silicate, 0.55g ethylenediamine, 2g concentration is 20% by weight of ammonia and 120g Add water to a 500ml beaker in turn, put it into a magnetic stirrer with heating and stirring functions, mix evenly, and stir at 90°C for 1 hour, and replenish evaporated water at any time to obtain a colorless transparent alkaline hydrolyzate.

[0073] (2) standing the hydrolyzed solution at room temperature for 3 hours to obtain an aging product;

[0074] (3) Add 9.6g of white carbon black powder slowly under stirring, and stir for 1.5 hours after the addition to form a uniform "viscous body". Crystallize at constant temperature for 6 days, filter, wash, dry at 120°C for 24 hours, and roast at 550°C for 6 hours to obtain a TS-1 molecular sieve sample, which is denoted as TS-1F2, and its BET specific surface area is 428m 2 / g, the external area is 59m 2 / g, micropore ...

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Abstract

The invention discloses a method for synthesizing a titanium silicate molecular sieve employing an organic quaternary ammonium salt template agent. The synthesis method of the titanium silicate molecular sieve comprises the following steps: (1) mixing a titanium source, a template agent, an organosilicone source, an optional inorganic ammonium source and water, hydrolyzing to remove alcohol, aging, mixing the aged mixture with a solid silicon source, crystallizing in a closed reaction kettle, and recycling the titanium silicate molecular sieve. The titanium silicate molecular sieve grain obtained by the method is rich in silicon; the surface silicon-titanium ratio of the titanium silicate molecular sieve is higher than the bulk-phase silicon-titanium ratio; the titanium silicate molecular sieve disclosed by the invention has relatively high oxidative activity; and the invalid decomposition activity of side reaction hydrogen peroxide is obviously 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): C01B39/08B01J29/89
Inventor 夏长久朱斌林民彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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