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Preparation method of hierarchical porous titanium silicalite molecular sieves

A titanium-silicon molecular sieve and channel technology, applied in molecular sieve compounds, molecular sieve catalysts, molecular sieve characteristic silicates, etc., can solve the problems of PVA being unable to play a template role, phase separation, weakening of the precursor solution, etc., and achieve excellent catalytic effect.

Inactive Publication Date: 2017-02-08
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystallization temperature of MCM-41 is below 100°C. At this temperature, PVA is relatively stable. However, compared with MCM-41, the crystallization temperature of TS-1 is higher (>140°C). In TS-1 At a certain crystallization temperature, PVA will undergo rapid dehydration and carbonization, and the carbonization of PVA and the precursor solution will be greatly weakened, resulting in severe phase separation, and finally PVA will not be able to play the role of template.

Method used

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  • Preparation method of hierarchical porous titanium silicalite molecular sieves
  • Preparation method of hierarchical porous titanium silicalite molecular sieves
  • Preparation method of hierarchical porous titanium silicalite molecular sieves

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Experimental program
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Effect test

Embodiment 1

[0030] Under the condition of continuous stirring, 23.4g tetrapropylammonium hydroxide (20wt%) was slowly added in 15.0g tetraethyl orthosilicate, after tetraethyl orthosilicate was completely hydrolyzed, a colorless and transparent solution A was obtained; then , the mixed solution B of 0.72g titanium source and 2.4g isopropanol is slowly added in solution A to obtain colorless and transparent solution C; ) after being fully mixed, the solution was transferred to a hydrothermal reaction kettle, first crystallized at 90° C. for 24 hours, and then heated to 160° C. for 24 hours. After the obtained product was centrifuged and washed, it was dried at 110°C overnight, and finally the obtained solid was calcined at 550°C for 6 hours to finally obtain the multi-level channel TS-1.

Embodiment 2

[0032] Under the condition of continuous stirring, 23.4g tetrapropylammonium hydroxide (20wt%) was slowly added in 15.0g tetraethyl orthosilicate, after tetraethyl orthosilicate was completely hydrolyzed, a colorless and transparent solution A was obtained; then , the mixed solution B of 0.72g titanium source and 2.4g isopropanol was slowly added to solution A to obtain a colorless and transparent solution C; after solution C was removed from alcohol at 80°C for 2h, it was mixed with PVA solution of the same quality (10.0wt%) ) after being fully mixed, the solution was transferred to a hydrothermal reaction kettle, first crystallized at 90° C. for 24 hours, and then heated to 160° C. for 24 hours. After the obtained product was centrifuged and washed, it was dried at 110°C overnight, and finally the obtained solid was calcined at 550°C for 6 hours to finally obtain the multi-level channel TS-1.

Embodiment 3

[0034] Under the condition of continuous stirring, 23.4g tetrapropylammonium hydroxide (20wt%) was slowly added in 15.0g tetraethyl orthosilicate, after tetraethyl orthosilicate was completely hydrolyzed, a colorless and transparent solution A was obtained; then , the mixed solution B of 0.72g titanium source and 2.4g isopropanol was slowly added to solution A to obtain a colorless and transparent solution C; after solution C was removed from alcohol at 80°C for 2h, it was mixed with PVA solution of the same quality (15.0wt%) ) after being fully mixed, the solution was transferred to a hydrothermal reaction kettle, first crystallized at 90° C. for 24 hours, and then heated to 160° C. for 24 hours. After the obtained product was centrifuged and washed, it was dried at 110°C overnight, and finally the obtained solid was calcined at 550°C for 6 hours to finally obtain the multi-level channel TS-1.

[0035] figure 1 It is the XRD spectrum of the titanium-silicon molecular sieve T...

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Abstract

The invention relates to a preparation method of hierarchical porous titanium silicalite molecular sieves. The preparation method comprises the following steps: slowly adding a template into a silicon source under the condition of continuous stirring, and obtaining a colorless transparent solution after the silicon source is completely hydrolyzed; slowly adding a mixed solution of a titanium source and isopropanol into the above solution, removing alcohol, fully mixing with an aqueous solution of polyvinyl alcohol, carrying out hydrothermal crystallization, centrifuging, washing, drying, and roasting to obtain the hierarchical porous titanium silicalite molecular sieves. In comparison with the prior art, the prepared titanium silicalite molecular sieves have rich mesoporous channels, which are interconnected. The product has an excellent catalytic effect in the aspect of macromolecular catalytic oxidation, especially in the aspect of oxidation of dibenzothiophenes and 4,6-dimethyl dibenzothiophenes.

Description

technical field [0001] The invention relates to a preparation method of a molecular sieve, in particular to a preparation method of a multi-level porous titanium-silicon molecular sieve. Background technique [0002] Titanium silicate molecular sieve TS-1 was first synthesized in 1983 (USP 4410501), and has been widely used in phenol hydroxylation, olefin epoxidation, ammonia epoxidation, alkane oxidation, etc. due to its excellent catalytic oxidation performance. With TS-1 as a catalyst, the catalytic reaction uses environmentally friendly H 2 o 2 As an oxidizing agent, the reaction conditions are mild, and the reaction by-product is mainly water. [0003] The active centers of titanium-silicon molecular sieves mainly exist in its abundant micropore channels (0.55nm). However, the smaller pore size is not conducive to the diffusion of reactant and product molecules in its channels, and molecules with a kinetic diameter larger than the channel diameter cannot The contact ...

Claims

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Application Information

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IPC IPC(8): C01B37/00B01J29/03
CPCB01J29/0308C01B37/005C01P2002/72C01P2002/82C01P2004/04
Inventor 郭益平杜起段华南李华陈玉洁刘河洲
Owner SHANGHAI JIAO TONG UNIV
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