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: 2004-04-14
EAST CHINA NORMAL UNIVERSITY
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  • Description
  • Claims
  • Application Information

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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 crystallizati

Method used

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Examples

Experimental program
Comparison scheme
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Example Embodiment

[0035] Example 1

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

[0037] The first step is the preparation of the 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, the reaction mixture solution is prepared, wherein the concentration of TPAOH is 10.4%;

[0039] The third step is to catch the alcohol concentration

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

[0041] Step 4 Hydrothermal crystallization

[0042] After static hydrothermal crystallization at 170°C for 2 days, TS-1 molecular sieve, numbered SSH-1, was obtained. The solid content of the product mixture of the synthesis system was 153.8g / l.

[0043] The XRD and IR spectra of TS-1 molecular sieve are attached respectively figure 1 with 2 .

Example Embodiment

[0044] Example 2

[0045] The implementation process is the same as in Example 1 except for the following differences:

[0046] The first step is the preparation of the 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, and the reaction mixture solution is prepared;

[0048] Step 4 Hydrothermal crystallization

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

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

Example

[0051] Examples 3-7

[0052] The first, second, and third steps of the implementation process are the same as in Example 2;

[0053] Step 4 Hydrothermal crystallization

[0054] The hydrothermal crystallization conditions were as follows: Example 3 was 150°C hydrothermal crystallization for 3 days, Examples 4, 5, and 6 were 170°C hydrothermal crystallization for 4 hours, 1 day, and 2 days, and Example 7 was 200 After 1 day of hydrothermal crystallization at ℃, TS-1 molecular sieves were obtained, which were numbered SSH-3, SSH-4, SSH-5, SSH-6, SSH-7, and the solid content of the product mixture of the synthetic system was 150~160g / l.

[0055] The XRD spectrum of TS-1 molecular sieve and figure 1 Similarly, the IR spectrum is similar to 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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IPC IPC(8): B01J29/89C01B37/06C01B39/08
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 UNIVERSITY
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