Regeneration method of deactivated titanium-silicon catalyst, regenerated catalyst and application thereof

A titanium-silicon catalyst, a technology for regenerating catalysts, applied in the direction of catalyst regeneration/reactivation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of complex regeneration methods, long regeneration process, difficult recovery of titanium-silicon catalyst activity, etc. The effect of less loss and generation of wastewater, short regeneration process, and easy industrial scale-up

Active Publication Date: 2019-03-15
SHANGHAI NOVEL CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The first object of the present invention is to provide a regeneration method for deactivated titanium-silicon molecular sieves, through a special regeneration process to solve the problems in the prior art that the activity of the deactivated titanium-silicon catalyst is difficult to recover, the regeneration method is complicated, and the regeneration process is long. , to rationally utilize waste titanium silicon catalyst

Method used

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  • Regeneration method of deactivated titanium-silicon catalyst, regenerated catalyst and application thereof
  • Regeneration method of deactivated titanium-silicon catalyst, regenerated catalyst and application thereof
  • Regeneration method of deactivated titanium-silicon catalyst, regenerated catalyst and application thereof

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Embodiment 1

[0054] Embodiment 1, the preparation of regenerated catalyst

[0055] The regeneration method of the deactivated titanium-silicon catalyst of the present embodiment may further comprise the steps:

[0056] (1) Take by weighing 14.5g dehydrated alcohol, 15g 30% hydrogen peroxide, 6.0g mass concentration be 25% TPAOH aqueous solution and 2.0g TBOT to join in the container of 250ml successively, then weigh 12.5g water and add in the container, stir until After TBOT is completely dissolved, the regeneration mixture R is obtained 1 , then weigh 10g of deactivated titanium-silicon catalyst wet material and add it to the regeneration mixture R 1 In, stir evenly, pour into the colloid mill and grind for 5h, the rotating speed is 3500rpm, and the uniform material M 1 .

[0057] (2) Transfer the homogeneous material in step (1) to a 100ml crystallization kettle, and conduct hydrothermal crystallization at a temperature of 170° C. for 15 hours to obtain a crystallized product;

[005...

Embodiment 2

[0062] Embodiment 2, the preparation of regeneration catalyst

[0063] The regeneration method of the deactivated titanium-silicon catalyst of the present embodiment, other conditions are all the same as embodiment 1, the difference is that the grinding time of the colloid treatment mill is 1h, and the regenerated catalyst S is obtained. 2 .

[0064] For regenerated catalyst S 2 Carry out XRD detection, the result is as follows figure 1 shown.

Embodiment 3

[0065] Embodiment 3, the preparation of regeneration catalyst

[0066] The regeneration method of the deactivated titanium-silicon catalyst of the present embodiment may further comprise the steps:

[0067] (1) Take by weighing 4.8g of absolute ethanol, 17.2g of 30% hydrogen peroxide, 7.5g of 25% TPAOH aqueous solution and 2.5g of TBOT in a 250ml container, then weigh 18.0g of water and add to the container, stir After TBOT is completely dissolved, the regeneration mixture R is obtained 3 , then weigh 10g of deactivated titanium-silicon catalyst wet material and add it to the regeneration mixture R 3 In, stir evenly, pour into the colloid mill and grind for 10h, the rotating speed is 3500rpm, and the uniform material M 3 .

[0068] (2) Transfer the homogeneous material in step (1) to a 100ml crystallization kettle, and conduct hydrothermal crystallization at a temperature of 170° C. for 15 hours to obtain a crystallized product;

[0069] (3) The crystallized product of ste...

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Abstract

The invention discloses a regeneration method of a deactivated titanium-silicon catalyst. The method comprises the following steps: (1) mixing a deactivated titanium-silicon catalyst wet material withregenerated mixed liquid, and grinding the mixture by adopting a colloid mill to obtain a uniform material; (2) performing hydrothermal crystallization on the uniform material obtained in the step (1) to obtain a crystallized product; and (3) filtering, washing and calcining the crystallized product obtained in the step (2) to obtain a regenerated catalyst, wherein the mass ratio of the deactivated titanium-silicon catalyst wet material to the regenerated mixed liquid is 1:(1-10). The obtained regenerated catalyst, prepared with the regeneration method of the deactivated titanium-silicon catalyst provided by the invention, has the advantages that the activity is recovered to a fresh agent level, the single-path life is obviously prolonged when the catalyst is used for cyclohexanone ammoximation reaction, only once washing is required during the entire regeneration process, the loss of the catalyst and the generated wastewater are less, the regeneration process is short, the regeneration cost is low, and industrial amplification is easy.

Description

technical field [0001] The invention belongs to the field of fine chemical catalysts, and in particular relates to a method for regenerating a deactivated titanium-silicon catalyst, a prepared regenerated catalyst and an application thereof. Background technique [0002] Since the first report by Taramasso et al. in 1983, TS-1 molecular sieve has been widely concerned by researchers at home and abroad because of the introduction of transition metal heteroatom Ti, which makes it have different catalytic activity from ordinary molecular sieves. TS-1 molecular sieve is an isomorphic substitution derivative obtained by partially substituting Si with Ti in all-silicon molecular sieve. It has the same MFI framework structure as ZSM-5, and the framework titanium is the active center of TS-1 participating in the selective catalytic oxidation reaction. . [0003] In recent years, the "green catalytic oxidation system" composed of TS-1 molecular sieve and hydrogen peroxide solution n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J29/90B01J38/02B01J38/64B01J38/06B01J38/48C07C251/42C07C249/04
CPCC07C249/04B01J29/89B01J29/90B01J38/02B01J38/06B01J38/48B01J38/64C07C2601/14Y02P20/584
Inventor 薛招腾夏娟夏建超文怀有谈赟
Owner SHANGHAI NOVEL CHEM TECH
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