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Method for preparing titanium-silicon molecular sieve

A molecular sieve and organic titanium technology, which is applied in the field of inorganic chemical synthesis, can solve the problems of not distinguishing the concentration of organic base template agent, high dosage of organic base template agent, long hydrothermal crystallization time, etc., so as to shorten the hydrothermal crystallization time, The effect of reducing the production cost and shortening the hydrothermal crystallization time

Inactive Publication Date: 2006-01-04
EAST CHINA NORMAL UNIV
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Problems solved by technology

Therefore, in the existing technology of synthesizing TS-1 molecular sieves with organic silicon sources, due to the high water content of the synthesis system, there is no distinction between the concentration of the organic base template agent in the process of hydrolysis and gelation and hydrothermal crystallization, so a high organic base template is used. The amount of template agent is used to achieve the purpose of high organic base template concentration, resulting in the disadvantages of high amount of organic base template agent, long hydrothermal crystallization time, low production efficiency and high production cost

Method used

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  • Method for preparing titanium-silicon molecular sieve
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  • Method for preparing titanium-silicon molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Organic silicon source and organic titanium source are TEOS and TBOT respectively

[0037] Preparation of the first step reaction mixture solution

[0038] Molar ratio of SiO in silicon source 2 : Organic base template: TiO in titanium source 2 :H 2 O: isopropanol is 1: 0.17: 0.04: 16.5: 5.0, prepare reaction mixture solution, wherein the concentration of TPAOH is 10.4%;

[0039] The third step alcohol concentration

[0040] The concentration of TPAOH in the reaction mixture sol clear liquid is 20.5%;

[0041] The fourth step hydrothermal crystallization

[0042] Static hydrothermal crystallization at 170°C for 2 days to obtain TS-1 molecular sieve, numbered SSH-1, and the solid content of the product mixture in the synthesis system was 153.8 g / l.

[0043] The XRD spectrum and IR spectrum of TS-1 molecular sieve are shown in the attached figure 1 and 2 .

Embodiment 2

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

[0046] Preparation of the first step reaction mixture solution

[0047] Molar ratio of SiO in silicon source 2 : Organic base template: TiO in titanium source 2 :H 2 O: isopropanol is 1: 0.17: 0.04: 16.5: 0, prepare reaction mixture solution;

[0048] The fourth step hydrothermal crystallization

[0049] TS-1 molecular sieve was obtained, coded as SSH-2, and the solid content of the product mixture in the synthesis system was 155 g / l.

[0050] XRD spectrum of TS-1 molecular sieve and figure 1 Similarly, the IR spectrum with figure 2 similar.

Embodiment 3～7

[0052] Implementation process first step, second step and third step are the same as embodiment 2;

[0053] The fourth step hydrothermal crystallization

[0054] The hydrothermal crystallization conditions are respectively: Example 3 is 150 ℃ hydrothermal crystallization for 3 days, embodiment 4, 5, 6 is 170 ℃ hydrothermal crystallization for 4 hours, 1 day, 2 days and embodiment 7 is 200 ℃ hydrothermal crystallization for 1 day to obtain TS-1 molecular sieves, respectively numbered SSH-3, SSH-4, SSH-5, SSH-6, SSH-7, and the solid content of the product mixture in the synthesis system is between 150 and 160g / l.

[0055] XRD spectrum of TS-1 molecular sieve and figure 1 Similarly, the IR spectrum with figure 2 similar.

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Abstract

The invention is a kind of manufacturing method for TS-1 molecular sift using organic silicon, organic titanium, organic template agent, water and and isopropanol are raw materials. The TS-1 molecular sift is produced through producing of reaction mix solvent, dydrolyse, condense, and water heat crystallizing. The character is: the organic alkali template agent TPAOH thickness are 3~15% and 15~35% in dydrolyse and crystallizing period. The producing efficiency high, the cost is low. The TS-1 molecular sift has a high catalyst and oxidizing activity.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve, that is, a TS-1 molecular sieve, and belongs to the technical field of inorganic chemical synthesis. Background technique [0002] TS-1 molecular sieve is a heteroatom molecular sieve developed in the early 1980s. Since the TS-1 molecular sieve introduces the transition metal titanium atoms with variable valence characteristics into the molecular sieve framework, it forms the oxidation-reduction (Redox) catalysis and endows the shape-selective function, so it has excellent directional catalytic oxidation performance and can be used as a new generation of choice. Novel catalysts for green chemistry of oxidation. At present, they have shown good industrial application prospects in the fields of oxidation of saturated alkanes, epoxidation of alkenes, oxidation of alcohols, ammoxidation of cyclohexanone, and hydroxylation of aromatic hydrocarbons. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C01B39/08C01B37/06
Inventor 刘月明沈刚林民张海娇杨建国曹平建朱观华李国繁单永奎何鸣元
Owner EAST CHINA NORMAL UNIV
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