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Synthesis method of titanium-containing molecular sieve

A synthesis method and molecular sieve technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve problems such as cyclic molecular amines that have not yet been seen, and achieve reduced production costs, less pollutant emissions, good repeatability

Inactive Publication Date: 2007-10-24
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the templates used in the synthesis are basically quaternary ammonium salts as the main template, and there has been no report on the use of cyclic molecular amines as the template in the synthesis.

Method used

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  • Synthesis method of titanium-containing molecular sieve
  • Synthesis method of titanium-containing molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Synthesis of the first step directing agent

[0031] SiO in molar ratio tetraethylsilicate 2 : Tetrapropylammonium hydroxide : TiO in tetrabutyl titanate 2 :H 2 O is 1:0.1:0.04:20, prepare a reaction mixture, conduct hydrolysis at 60°C to form a gel for 0.5 to 1 hour, then raise the temperature to 80°C, and chase the alcohol for 4 hours to prepare the directing agent;

[0032] Preparation of the second reaction mixture

[0033] The silicon source is silica gel, the titanium source is tetrabutyl titanate, the template agent is hexamethyleneimine, and the SiO in the silicon source is molar ratio 2 : Organic base template: TiO in titanium source 2 :H 2 O is 1:1:0.033:12 to prepare the mixture solution, add SiO in the silicon source 2 The directing agent that the last step of 3% of weight makes, forms reaction mixture;

[0034] The third step of hydrothermal crystallization

[0035] Hydrothermal crystallization at 170°C for 4 days to obtain TS-1 molecular sieve.

...

Embodiment 2

[0038] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0039] Synthesis of the first step directing agent

[0040] Molar ratio of SiO in silicon source 2 : Organic base template: TiO in titanium source 2 :H 2 O is 1:0.2:0.1:80;

[0041] Preparation of the second reaction mixture

[0042] The organic template is a mixture of hexamethyleneimine and piperidine, and the molar ratio of the two is 5:5.

[0043] The XRD spectrum of TS-1 molecular sieve is similar to Figure 1, and the IR spectrum is similar to Figure 2.

Embodiment 3

[0045] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0046] Preparation of the second reaction mixture

[0047] The organic template is piperidine, adding SiO based on silicon source 2 15% by weight of the directing agent prepared in the previous step to form a reaction mixture.

[0048] The XRD spectrum of TS-1 molecular sieve is similar to Figure 1, and the IR spectrum is similar to Figure 2.

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Abstract

The invention relates the method for synthesizing titanium molecular screen, belonging to inorganic chemical synthesized technique field. The method comprises the following steps: using silica gel or silicasol as silicon source, using organic titanium acid ester as titanium source, using hexamethylene diamine or piperidine or the mixture of them as organic form agent, synthesizing the guiding agent, preparing reaction liquid, carrying out thermal crystallization, then filtering, washing, drying, calcining, and getting the TS-1 molecular screen. The method has the advantages of low cost, good repeatability and low pollution emission.

Description

technical field [0001] The invention relates to a method for synthesizing a titanium-containing molecular sieve, specifically, a method for synthesizing a TS-1 molecular sieve, and belongs to the technical field of inorganic chemical synthesis. Background technique [0002] Since Taramasso et al. (US 4,410,501) first reported in 1983, TS-1 molecular sieve has attracted widespread attention due to its excellent catalytic oxidation performance. At present, using TS-1 molecular sieve as catalyst and dilute H 2 o 2 It is a mild reaction system of oxidant, which shows high activity and selectivity in organic oxidation reactions such as olefin epoxidation, aromatic hydrocarbon hydroxylation, ketone ammonia oximation, alkane oxidation and alcohol oxidation, and the by-product is only water environment Friendly green chemical process, so TS-1 molecular sieve is known as a milestone in molecular sieve catalysis in the 1980s. [0003] At present, the typical m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C01B39/08
Inventor 刘月明张海娇吴海虹吴鹏何鸣元
Owner EAST CHINA NORMAL UNIV
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