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Preparation method of titanium-silicate molecular sieve having large particle size

A technology of titanium-silicon molecular sieve and large particle size, which is applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., and can solve the problems of separation and recovery of difficult products of small particle size titanium-silicon molecular sieves, etc. Achieve the effects of simple operation, easy process control, and short crystallization time

Active Publication Date: 2015-04-08
ZHEJIANG JINHUA NEW MATERIALS
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  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide the preparation method of large particle size titanium silicon molecular sieve, the present invention has overcome the deficiency of prior art, and the prepared titanium silicon molecular sieve can solve the problem that small particle size titanium silicon molecular sieve is difficult to produce in industry Separation and Recycling Issues

Method used

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  • Preparation method of titanium-silicate molecular sieve having large particle size
  • Preparation method of titanium-silicate molecular sieve having large particle size
  • Preparation method of titanium-silicate molecular sieve having large particle size

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preparation example Construction

[0034] The invention provides a preparation method of a large-diameter titanium-silicon molecular sieve, which is characterized in that it comprises the following preparation process:

[0035] (1) Preparation of the mixed solution:

[0036] At room temperature, slowly add the organic template aqueous solution to the inorganic silicon source. After the addition, stir for 0.5-2 hours to obtain the initial mixed solution; then add the inorganic titanium source to the initial mixed solution. After the addition, fully stir for 0.5-2 hours. 5h to obtain a mixed solution; the molar ratio of inorganic silicon source, inorganic titanium source, organic template and water in the mixed solution is 1:(0.013~0.025):(0.025~0.2):(30~60), wherein the inorganic silicon source SiO 2 In terms of inorganic titanium source as TiO 2 Wherein, the preferred molar ratio of inorganic silicon source, inorganic titanium source, organic templating agent and water in the mixed solution is 1: (0.015~0.02)...

preparation example 1

[0047] Slowly add tetrapropyl ammonium hydroxide aqueous solution to 12.1g silica sol (SiO 2 content is 30%), after stirring for 30 minutes, slowly add titanium trichloride solution, and stir for 1 hour to obtain a mixed solution. Wherein the molar ratio of silica sol, titanium trichloride, tetrapropylammonium hydroxide and water in the mixed solution is 1:0.018:0.1:40.

Embodiment 1

[0051] At a mixing temperature of 60°C, first slowly add tetrapropylammonium hydroxide aqueous solution to 6.8g of tetraethyl silicate, stir well for 1 hour to obtain component A; then add isopropanol to tetraethyl titanate After mixing evenly, component B is obtained; slowly add component B to component A, and after fully stirring for 30 minutes, the preparation solution is obtained. In the preparation solution, tetraethyl silicate, tetraethyl titanate, tetrapropyl The molar ratio of ammonium hydroxide, isopropanol and water is 1:0.02:0.2:1.0:30.

[0052] The preparation solution was added into a sealed reaction kettle, and the preparation solution was hydrothermally crystallized at a crystallization temperature of 170°C and a crystallization time of 4 days; then the preparation solution was filtered to obtain the first filter cake, and the first filter cake was washed to Neutral, and vacuum-dry the first filter cake at 120°C for 10 hours to obtain a crystalline material;

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Abstract

The invention discloses a preparation method of a titanium-silicate molecular sieve having large particle size and belongs to the technical field of inorganic chemical synthesis. The preparation method comprises the following steps of synthesizing a crystalline material; introducing the crystalline material into a mixed solution comprising an inorganic silicon source, an inorganic titanium source, an organic template agent and water, controlling pH by virtue of an alkaline source, carrying out hydrothermal crystallization, filtering, washing, drying and calcining to obtain the titanium-silicate molecular sieve. By the preparation method, the deficiencies of the prior art are overcome and by the prepared titanium-silicate molecular sieve, the problem that titanium-silicate molecular sieve having small particle size is difficult to be separated from the product and recovered in the industry can be well solved. The titanium-silicate molecular sieve prepared by the preparation method, which is disclosed by the invention has the advantages that the average particle size is greater than 5mu m or more, the crystallization time is short, the product is high in purity, the method has good repeatability, the operation is simple and feasible and the process is easy to control.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve, in particular to a preparation method of a large-diameter titanium-silicon molecular sieve. Background technique [0002] Titanium-silicon molecular sieve is the introduction of transition metal titanium atoms into the molecular sieve framework with a certain topology to form a porous crystalline material with catalytic oxidation activity. Titanium-silicon molecular sieves can be used to catalyze various organic oxidation reactions, such as olefin epoxidation, alkane partial oxidation, alcohol oxidation, phenol hydroxylation, cyclic ketone ammoxidation, etc. As an oxidant, hydrogen oxide has high reaction selectivity, relatively simple process, and has incomparable advantages of energy saving, economy, and environmental friendliness compared with traditional oxidation systems, and is considered to be a typical representative of environmentally friendly catalysts. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
CPCC01B39/085
Inventor 马利勇李宏峰周强林晓云
Owner ZHEJIANG JINHUA NEW MATERIALS
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