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Ti-Si molecular sieve and synthesis method thereof

A titanium-silicon molecular sieve and molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problems that do not involve further improving the activity of titanium-silicon molecular sieves, and it is difficult to increase the solid content of the synthesized and crystallized products of molecular sieves. , low content of active ingredients of molecular sieve, etc., to achieve the effect of improving the utilization rate of raw materials, reducing the synthesis cost and reducing the activity

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

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Problems solved by technology

Organic silicon sources such as organosilicon ester TEOS are relatively expensive, and the content of active ingredients forming molecular sieves is also low. It is difficult to increase the solid content of molecular sieve crystallization products, and a large amount of ethanol is volatilized during the production of molecular sieves, and these ethanols are difficult to collect. Reuse
In order to reduce costs, researchers have studied the use of inorganic silicon sources to replace part or all of the organic silicon sources. However, the activity of titanium-silicon molecular sieves synthesized using inorganic silicon sources (solid silicon sources) is lower than that of titanium-silicon molecular sieves synthesized entirely using organic silicon sources.
In addition, the prior art does not involve further improving the activity of titanium silicon molecular sieves

Method used

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  • Ti-Si molecular sieve and synthesis method thereof
  • Ti-Si molecular sieve and synthesis method thereof
  • Ti-Si molecular sieve and synthesis method thereof

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Embodiment approach

[0031] In one embodiment, the template agent includes an organic base, including an organic quaternary ammonium compound, and the molar ratio of the organic base introduced into the template agent to the silicon source is not less than 0.05:1, for example, 0.05-0.45; 1, the The organic base is an organic quaternary ammonium base and / or an organic amine; the molar ratio of the organic quaternary ammonium compound to the silicon source is not less than 0.05:1, such as 0.05 to 0.45:1, and the organic quaternary ammonium compound is an organic quaternary ammonium compound. Ammonium bases and / or organic quaternary ammonium salts.

Embodiment approach

[0032] A kind of implementation method, described template agent, comprises organic quaternary ammonium base, can be organic quaternary ammonium base or the mixture that comprises organic quaternary ammonium base, for example described template agent is the mixture of organic quaternary ammonium base and organic amine, A mixture of an organic quaternary ammonium base and an organic quaternary ammonium salt, or a mixture of an organic quaternary ammonium base, an organic quaternary ammonium salt and an organic amine. Preferably, the molar ratio of organic quaternary ammonium base to organic ammonium is 1:0 to 10, such as 1:0 to 8, and the molar ratio of organic quaternary ammonium base to organic quaternary ammonium salt is 1:0 to 10, such as 1:0 to 8. The molar ratio of the organic quaternary ammonium base to the total silicon source is 0.05-0.45:1, for example 0.05-0.3:1, for example 0.05-0.2:1.

[0033] The method for synthesizing a titanium-silicon molecular sieve provided...

Embodiment 1

[0066] (1) 15g of tetrapropylammonium hydroxide (TPAOH) aqueous solution with a concentration of 25.05% by weight, 2.04g of tetrabutyl titanate, 8.5g of tetraethyl silicate, 2g of ammonia water with a concentration of 20% by weight and 38g of water in sequence Add it into a 500ml beaker, put it into a magnetic stirrer with heating and stirring functions, mix evenly, and stir at 80°C for 4 hours, replenish the evaporated water at any time, and obtain a colorless transparent hydrolyzate;

[0067] (2) Aging the obtained hydrolyzate at room temperature (26°C) for 12 hours to obtain an aging product;

[0068] (3) Add 9.6g of white carbon black powder to the above aging product under stirring, and stir for 1 hour after adding to form 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 described in the prese...

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Abstract

The invention provides a Ti-Si molecular sieve and a synthesis method thereof. The crystal surface of the Ti-Si molecular sieve is rich in Si, and the surface Ti-Si ratio of the Ti-Si molecular sieve is higher than the bulk-phase Ti-Si ratio of the Ti-Si molecular sieve. The synthesis method of the Ti-Si molecular sieve comprises the steps as follows: mixing a Ti source, a template agent, an organic Si source, an inorganic Si source and water, removing alcohol by hydrolysis, aging, mixing an aged product with a solid Si source, performing crystallization in an airtight reaction kettle, and recycling the Ti-Si molecular sieve. The Ti-Si molecular sieve provided by the invention has higher oxidative activity, and the activity in non-effective decomposition of hydrogen peroxide in side reaction 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
CPCB01J29/89C01B39/08C01P2002/72C01P2004/04C01P2006/12
Inventor 夏长久林民朱斌彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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