Synthesis of titanium-silica molecular sieve

A synthesis method and molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problem of large amount of organic base template agent tetrapropylammonium hydroxide, complicated operation process, poor repeatability, etc. problems, to achieve the effect of easy control of the synthesis process, good repeatability and low cost

Inactive Publication Date: 2005-02-02
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When synthesizing TS-1 molecular sieve by organic synthesis, because at least one of the silicon source and the titanium source is an organic raw material, there is a hydrolysis process, and the hydrolysis process is not easy to control, so the operation process is complicated and the repeatability is poor; at the same time, the organic base template Agent tetrapropyl ammonium hydroxide (TPAOH) consumption is also large, therefore, the cost is higher when organic synthesis method synthesizes TS-1 molecular sieve

Method used

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  • Synthesis of titanium-silica molecular sieve
  • Synthesis of titanium-silica molecular sieve
  • Synthesis of titanium-silica molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Step 1 Solid silica and Ti(SO 4 ) 2 Preparation of the mixture

[0034] Molar ratio of SiO in solid silica gel 2 :Ti(SO 4 ) 2 TiO in 2 1:0.04, prepare the mixture, and bake at 400°C for 24 hours;

[0035] Preparation of the second step reaction mixture

[0036] SiO in the mixture prepared in the previous step by molar ratio 2 +TiO 2 :TPAOH:H 2O is 1:0.2:10, preparing the reaction mixture;

[0037] The third step hydrothermal crystallization

[0038] Hydrothermal crystallization at 170°C for 4 days to obtain TS-1 molecular sieve.

[0039] The XRD spectrum and IR spectrum of TS-1 molecular sieve are shown in figure 1 and 2 .

Embodiment 2

[0041] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0042] Step 1 Solid silica and Ti(SO 4 ) 2 Preparation of the mixture

[0043] Calcined at 150°C for 48 hours.

[0044] XRD spectrum of TS-1 molecular sieve and figure 1 Similarly, the IR spectrum with figure 2 similar.

Embodiment 3

[0046] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0047] Step 1 Solid silica and Ti(SO 4 ) 2 Preparation of the mixture

[0048] Calcined at 600°C for 18 hours.

[0049] XRD spectrum of TS-1 molecular sieve and figure 1 Similarly, the IR spectrum with figure 2 similar.

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Abstract

The present invention is the synthesis process of Ti-Si molecular sieve, TS-1 molecular sieve, and belongs to the field of inorganic chemical synthesis. The materials, including solid silica gel, Ti(SO4)2, organic alkali template and water, are prepared into TS-1 molecular sieve via a three-step reaction process, including the preparation of solid silica gel and Ti(SO4)2 mixture, the preparation of reaction mixture and hydrothermal crystallization, and routine filtering, washing, drying and roasting. Inside the solid silica gel and Ti(SO4)2 mixture, Ti(SO4)2 is single-layer dispersed in the surface of solid silica gel. The process has the advantages of cheap materials, no need of hydrolysis, less consumption of organic template agent, easy-to-control process, high repeatability, high yield and low cost.

Description

technical field [0001] The invention relates to a synthesis 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 an oxidation-reduction (Redox) catalysis and endows a 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. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C01B39/08
Inventor 刘月明张海娇杨建国何鸣元
Owner EAST CHINA NORMAL UNIV
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