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Regeneration method for waste TS-1 titanium silicate molecular sieve

A technology of titanium-silicon molecular sieve, TS-1, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as environmental hazards, poor crystallization effect, and limited effect of titanium-silicon molecular sieves. Environmental pollution problems, the effect of reducing production costs

Active Publication Date: 2015-06-10
JIANGSU SANJILI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main function of the above regeneration is to clear the pores of the titanium-silicon molecular sieve, which has a limited effect on the scrapped titanium-silicon molecular sieve that loses titanium in the active center
And when direct heat treatment removes the organic pollutants that block the pores, it will cause harm to the environment
Patents CN 102309983 A and CN102188994A respectively disclose the method of supplementing titanium source through crystallization reaction, the reaction is carried out under normal pressure or autogenous hydrothermal pressure, the crystallization effect is poor, and non-skeleton titanium species will exist on the surface of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Add scrapped TS-1 titanium-silicon molecular sieve to 50% ethanol aqueous solution by volume, and ultrasonically clean it at 100W for 1 hour;

[0026] 2. Add the TS-1 titanium-silicon molecular sieve ethanol aqueous solution after ultrasonication to the membrane filtration device, and add deionized water according to the ratio of TS-1 titanium-silicon molecular sieve ethanol aqueous solution to deionized water volume ratio of 1:100, and the operating pressure is 0.1 MPa, filter and wash at room temperature for 2 hours, put the obtained TS-1 titanium-silicon molecular sieve into a drying oven at 80°C for 12 hours, and then crush it to 150 mesh;

[0027] 3. Mix tetrabutyl titanate, isopropanol, tetrapropylammonium hydroxide and water at a molar ratio of 1:30:3:500, and hydrolyze at 30°C for 2 hours to obtain titanium sol;

[0028] 4. Add the pulverized TS-1 titanium-silicon molecular sieve into the titanium sol, and after negative pressure suction for 30 minutes, filte...

Embodiment 2

[0032] 1. Add the scrapped TS-1 titanium silicon molecular sieve to 60% ethanol aqueous solution by volume, and ultrasonically clean it at 100W for 1h;

[0033] 2. Add the TS-1 titanium-silicon molecular sieve ethanol aqueous solution after ultrasonication to the membrane filtration device, and add deionized water according to the ratio of TS-1 titanium-silicon molecular sieve ethanol aqueous solution to deionized water volume ratio of 1:200, and the operating pressure is 0.2 MPa, filter and wash at room temperature for 1 hour, put the obtained TS-1 titanium silicon molecular sieve in a drying oven at 100°C for 12 hours, and then crush it to 200 mesh;

[0034] 3. Mix tetrabutyl titanate, isopropanol, tetrapropylammonium hydroxide and water at a molar ratio of 1:40:5:600, and hydrolyze at 50°C for 1 hour to obtain titanium sol;

[0035] 4. Add the pulverized TS-1 titanium-silicon molecular sieve into the titanium sol, and after negative pressure suction for 40 minutes, filter t...

Embodiment 3

[0039] 1. Add the scrapped TS-1 titanium silicon molecular sieve to 50% ethanol aqueous solution by volume, and ultrasonically clean it at 150W for 2 hours;

[0040] 2. Add the TS-1 titanium-silicon molecular sieve ethanol aqueous solution after ultrasonication to the membrane filtration device, and add deionized water according to the ratio of TS-1 titanium-silicon molecular sieve ethanol aqueous solution to deionized water volume ratio of 1:100, and the operating pressure is 0.3 MPa, filter and wash at room temperature for 1 hour, put the obtained TS-1 titanium silicon molecular sieve in a drying oven at 80°C for 10 hours, and then crush it to 150 mesh;

[0041] 3. Mix tetrabutyl titanate, isopropanol, tetrapropylammonium hydroxide and water at a molar ratio of 1:50:2:400, and hydrolyze at 40°C for 2 hours to obtain titanium sol;

[0042] 4. Add the pulverized TS-1 titanium-silicon molecular sieve into the titanium sol, and after negative pressure suction for 60 minutes, fil...

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Abstract

The invention discloses a regeneration method for a waste TS-1 titanium silicate molecular sieve. The regeneration method for the waste TS-1 titanium silicate molecular sieve includes that removing tar and the like organic pollutant which block holes through ultrasonic cleaning and membrane filtering; complementing the titanium loss of the TS-1 titanium silicate molecular sieve through a sol heat treatment method and high-pressure crystallization; washing through hydrochloric acid, and removing the extra-framework titanium from the surface of the titanium-complemented titanium silicate molecular sieve to enable the activity of the waste TS-1 titanium silicate molecular sieve to arrive at the fresh level. The regeneration method for the waste TS-1 titanium silicate molecular sieve is low in cost, the titanium element loss of the TS-1 titanium silicate molecular sieve framework is better complemented to realize the original activity, and moreover, the environment pollution due to the organic pollutant roasting in the regeneration process can be effectively reduced.

Description

technical field [0001] The invention relates to the field of petrochemical catalysts, in particular to a regeneration method for scrapped TS-1 titanium-silicon molecular sieves. Background technique [0002] Since Taramasso et al. first reported it in 1983, TS-1 titanium silicate molecular sieve has attracted widespread attention due to its excellent catalytic oxidation performance. In reactions such as olefin epoxidation, aromatic hydrocarbon hydroxylation, phenol hydroxylation, ketone ammonia oximation, alkane oxidation, etc., TS-1 titanium silicon molecular sieve as a catalyst shows excellent catalytic activity and selectivity, so TS-1 titanium silicon molecular sieve Known as a milestone in molecular sieve catalysis in the 1980s. [0003] The highly active TS-1 titanium-silicon molecular sieve disclosed in patent CN101327934B was successfully used in the production of catechol and hydroquinone by hydroxylation of phenol, but it was found that the activity of the molecul...

Claims

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Application Information

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IPC IPC(8): B01J29/90
Inventor 杨世刚刘德标徐传春
Owner JIANGSU SANJILI CHEM
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