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Regeneration method of titanium silicalite molecular sieve catalyst

A titanium-silicon molecular sieve and catalyst technology, which is applied in the field of titanium-silicon molecular sieve catalyst regeneration, can solve problems such as an effective regeneration method for a titanium-silicon molecular sieve Ti-MWW catalyst, etc., and achieve the effects of simple and easy operation and easy process control.

Inactive Publication Date: 2009-12-16
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] There is no report on the effective regeneration method of Ti-MWW catalyst of Ti-Si molecular sieve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The deactivated Ti-MWW molecular sieves come from deactivated catalysts run in the ammoximation reaction of butanone.

[0028] In the first step, the Ti-MWW molecular sieve of deactivation: the weight ratio=1:30 of acidic compound solution, the concentration of acidic compound solution is 0.5mol / l, and acidic compound is nitric acid; In the second step, the first step makes The reaction mixture was reacted at 100°C for 2 hours; in the third step, the Ti-MWW molecular sieve treated with acid: the weight ratio=1:10 of the basic compound solution, wherein the concentration of the basic compound solution was 3mol / l, and the basic The compound is piperidine; in the fourth step, the reaction mixture obtained in the third step is hydrothermally treated at 170° C. for 24 hours under its own pressure to obtain an alkali-treated Ti-MWW molecular sieve, which is then filtered, washed, dried and roasted to obtain Regenerated Ti-MWW molecular sieves.

Embodiment 2

[0030] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0031] In the first step, the Ti-MWW molecular sieve of inactivation: the weight ratio=1:50 of acidic compound solution, the concentration of acidic compound solution is 0.1mol / l, and acidic compound is sulfuric acid; In the second step, the first step makes The reaction mixture was reacted at 80°C for 1 hour; in the third step, the acid-treated Ti-MWW molecular sieve: the weight ratio of the basic compound solution=1:20, wherein the concentration of the basic compound solution was 0.5mol / l; Among the four steps, the reaction mixture obtained in the third step is hydrothermally treated at 120° C. under its own pressure. A regenerated Ti-MWW molecular sieve was obtained.

Embodiment 3

[0033] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0034] In the first step, the Ti-MWW molecular sieve of deactivation: the weight ratio=1:10 of acidic compound solution, the concentration of acidic compound solution is 2.0mol / l, and acidic compound is hydrochloric acid; In the second step, the first step makes The reaction mixture was reacted at 35°C for 8 hours; in the third step, the acid-treated Ti-MWW molecular sieve: the weight ratio of the basic compound solution=1:5, wherein the concentration of the basic compound solution was 5mol / l; the fourth In the first step, the reaction mixture prepared in the third step was hydrothermally treated at 180°C for 12 hours under its own pressure. A regenerated Ti-MWW molecular sieve was obtained.

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Abstract

The invention discloses a regeneration method of titanium silicalite molecular sieve catalyst, and the deactivated titanium silicalite molecular sieve is Ti-MWW molecular sieve which is from the epoxidation reaction of alkene and the ammonia oximation reaction of ketone. The method comprises the following steps: carrying out an acid compound solution treatment and an alkaline compound solution treatment on the deactivated titanium silicalite molecular sieve, then filtering, washing, drying and baking the Ti-MWW molecular sieve, thus obtaining the regenerative titanium silicalite molecular sieve. The invention has the advantages of simple operation, and easy-controlled process and the regenerative titanium silicalite molecular sieve catalytic activity can restore to the level of a fresh agent.

Description

technical field [0001] The invention relates to the technical field of inorganic chemical synthesis, in particular to a regeneration method of a titanium-silicon molecular sieve catalyst. 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. Using titanium silicate molecular sieve as catalyst and dilute H 2 o 2 It is a mild reaction system formed by an oxidant. It exhibits high activity and selectivity in organic oxidation reactions such as olefin epoxidation, aromatic hydrocarbon hydroxylation, ketone ammonia oximation, alkane oxidation, and alcohol oxidation. The by-product is only water. The environmentally friendly green chemical process has attracted widespread attention. At present, the titanium-silicon molecular sieves that have been industrialized and have wide applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/90B01J29/89B01J38/64B01J38/60
Inventor 刘月明杨俊霞赵松方向青吴鹏何鸣元
Owner EAST CHINA NORMAL UNIV
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