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A kind of preparation method of large particle size titanium silicon molecular sieve catalyst and its method for preparing cyclohexanone oxime

A technology of titanium-silicon molecular sieves and catalysts, which is applied in the direction of molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve problems such as catalyst separation difficulties, achieve reduced production costs and operational difficulties, uniform crystal grains, and crystallinity high effect

Active Publication Date: 2020-10-09
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the raw powder catalyst is used, the average particle diameter is usually between 0.1 and 2 microns, making it very difficult to separate the catalyst from the liquid reaction product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0022] The preparation method of a kind of large particle size titanium silicon molecular sieve catalyst of the present invention comprises the following steps:

[0023] 1) Synthesis of titanium silicon molecular sieve:

[0024] Molar ratio of SiO in inorganic silicon source 2 : TiO in inorganic titanium source 2 : organic template agent: alkali source: water = 1: 0.01~0.03: 0.02~0.2: 20~80: 30~70, at a temperature of 30~90°C, slowly add the inorganic silicon source into the aqueous solution of the organic template agent, After the feeding is completed, fully stir for 0.2 to 2 hours. After mixing evenly, slowly add the inorganic titanium source. After the feeding is completed, stir fully for 0.5 to 4 hours. The solution is hydrothermally crystallized at 120-200°C for 2-10 days, filtered, and the filter cake is washed with deionized water until the pH value is 8-9, and vacuum-dried at 120°C for 10-16 hours to obtain a titanium-silicon molecular sieve ;

[0025] 2) Acid trea...

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PUM

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Abstract

The invention discloses a preparation method of a large-particle-size titanium silicalite molecular sieve catalyst and a method for preparing cyclohexanone-oxime with the catalyst. An inorganic silicon source and an inorganic titanium source are used, tetrapropylammonium hydroxide or tetrapropylammonium bromide is used as a template agent, ammonia water or organic ammonium is used as an alkali source, preparation of a reaction mixed solution, hydrothermal crystallization, filtration, washing, drying, acid treatment and alkali treatment are performed, the final titanium silicalite molecular sieve is obtained through calcination, and cyclohexanone-oxime is prepared through cyclohexanone ammoxidation of the titanium silicalite molecular sieve. The prepared titanium silicalite molecular sievecatalyst has uniform particle size, has the advantage particle size larger than 10 micrometers, is easy to separate and recycle after reactions, can increase the recycle rate and has the advantages offew synthesis steps, low cost, operation simplicity, high product quality stability and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing a large-diameter titanium-silicon molecular sieve catalyst and a method for preparing cyclohexanone oxime. 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, and non-polluting low-concentration hydrogen peroxide can be used as the oxidant. The reaction selectivity is high, the process is relatively simple, and it has incomparable energy saving, economy and environmental friendliness compared with traditional oxidation systems. And other advantages, it is considered to be a typical representative of environment-friendly catalysts. The process of u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B01J29/89C07C249/04C07C251/44
CPCB01J29/89C01B39/085C01P2004/64C07C249/04C07C2601/14C07C251/44
Inventor 马利勇林晓云李宏峰汪宇轩
Owner JUHUA GROUP TECH CENT