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Modification method for titanium silicate molecular sieve

A titanium-silicon molecular sieve and modification technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., to achieve the effects of superior catalytic activity stability, improved diffusion performance, and reduction of non-framework titanium

Active Publication Date: 2015-07-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the modification of titanium-silicon molecular sieves with an alkaline solution containing an organic chelating agent has not been reported in the existing open literature.

Method used

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  • Modification method for titanium silicate molecular sieve
  • Modification method for titanium silicate molecular sieve
  • Modification method for titanium silicate molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Take the TS-1 molecular sieve obtained in Comparative Example 1 and mix it evenly according to molecular sieve (g): alkali solution of organic chelating agent (mL) = 1:10, put it into a stainless steel sealed reaction kettle, treat it at 170°C for 96h, and then Methods Filtration, washing and drying to obtain modified titanium silicon molecular sieves. Wherein organic chelating agent is cyclohexanediaminetetraacetic acid, concentration is 0.04mol / L; Alkaline solution is ammoniacal liquor and tetrapropyl ammonium hydroxide mixed alkali solution, and ammoniacal liquor concentration is 0.5mol / L, and tetrapropylammonium hydroxide concentration is 0.06mol / L;

Embodiment 2

[0041] Take the titanium-silicon molecular sieve obtained in Comparative Example 2 and mix it evenly according to molecular sieve (g): alkali solution of organic chelating agent (mL) = 1:10, put it into a stainless steel sealed reaction kettle, treat it at 170°C for 48h, and then follow the conventional method Filter, wash and dry to obtain a modified titanium-silicon molecular sieve. Wherein the organic chelating agent is hydroxyethyl ethylenediamine triacetic acid, the concentration is 0.24mol / L; the alkali solution is the mixed alkali solution of ammonia water and tetrapropyl ammonium hydroxide, the concentration of ammonia water is 3.25mol / L, tetrapropyl ammonium hydroxide The concentration is 0.18mol / L;

Embodiment 3

[0043] Take the titanium-silicon molecular sieve obtained in Comparative Example 1 and mix it evenly according to molecular sieve (g): alkali solution of organic chelating agent (mL) = 1:5, put it into a stainless steel sealed reaction kettle, treat it at 150°C for 96h, and then follow the conventional method Filter, wash and dry to obtain a modified titanium-silicon molecular sieve. Wherein organic chelating agent is ethylenediaminetetraacetic acid, and concentration is 0.25mol / L; Alkaline solution is the mixed alkali solution of ammoniacal liquor and tetrapropyl ammonium hydroxide, and ammoniacal liquor concentration is 1.15mol / L, and tetrapropylammonium hydroxide concentration is 0.06mol / L;

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Abstract

The invention provides a modification method for a titanium silicate molecular sieve. The method comprises the steps of: evenly mixing an organic chelating agent-containing alkali solution and a titanium silicate molecular sieve according to a certain ratio, reacting in an airtight reaction kettle, filtering, washing, drying and calcinating the product to obtain the TS-1 molecular sieve which is modified with the organic chelating agent-containing alkali solution. By adopting the method, non-skeleton titanium can be reduced, even removed in the process of modifying the titanium silicate molecular sieve, so that the catalytic oxidation activity of the modified titanium silicate molecular sieve can be improved, especially, superior catalytic activity stability can be shown in reaction of olefin epoxidation, phenol hydroxylation, ketone ammoximation, alcohol oxidization and the like.

Description

technical field [0001] The invention belongs to the technical field of petrochemical catalysts, and more specifically relates to a method for modifying titanium-silicon molecular sieves with an alkaline solution containing an organic chelating agent. Background technique [0002] In 1981, Tarramasso et al first publicly reported (GB2071071, US4410501) the synthesis of titanium silicon molecular sieve (TS-1) with MFI structure. TS-1 has the shape-selective effect and stability of ZSM-5 molecular sieve, and at the same time transition metal titanium enters the molecular sieve framework to make it have excellent selective catalytic oxidation performance. , TS-1 molecular sieve in dilute H 2 o 2 In the mild reaction system of the oxidant, it has excellent catalytic performance, and shows high activity and selectivity in reactions such as olefin epoxidation, ammoximation of aromatic hydrocarbon hydroxylated ketones, alcohol oxidation and alkane oxidation, and the by-products O...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B01J29/89C07D303/04C07D301/12
Inventor 王祥生宋万仓
Owner DALIAN UNIV OF TECH
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