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Gas solid phase preparation method of high performance titanium silicon zeolite

A titanium silicalite, gas-solid phase technology, applied in crystalline aluminosilicate zeolite, chemical instruments and methods, molecular sieve compounds, etc., can solve problems such as poor hydroxylation performance of phenol, and achieve excellent catalytic performance and mild catalytic reaction conditions. , the preparation method is simple

Inactive Publication Date: 2005-08-10
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

However, although the titanium-silicon molecular sieve prepared by this method has good propylene epoxidation performance, its phenol hydroxylation performance is poor. [1]

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Synthesis of boron-containing zeolites

[0015] 143.8 grams of tetrapropylammonium bromide (TPABr) are added in the there-necked flask that 150ml 30% (wt) silica sol is housed, add appropriate amount of water and stir until fully dissolved, then adjust the stirring speed (do not make the colloid agglomerate into pieces) While adding sodium hydroxide aqueous solution (21.6 grams of sodium hydroxide dissolved in 150 ml of water), stir until the colloid is uniform. Slowly add boric acid aqueous solution (22.3 grams of boric acid dissolved in 600 ml of water) under stirring, after adding, continue to stir for 60 minutes. The glue solution was put into a polytetrafluoroethylene-lined stainless steel reactor, and crystallized at 165°C for 3 days. That is, the boron-containing molecular sieve A is obtained.

Embodiment 2

[0017] Synthesis of boron-containing zeolites

[0018] After the glue solution was put into the reactor, it was first crystallized at 80° C. for 2 hours, and other conditions were the same as in Example 1 to obtain boron-containing molecular sieve B.

Embodiment 3

[0020] Synthesis of boron-containing zeolites

[0021] After the glue solution was put into the reactor, it was first crystallized at 80° C. for 5 hours, and other conditions were the same as in Example 1 to obtain boron-containing molecular sieve C.

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Abstract

A process for preparing high-performance TiSi zeolite by gas-solid method includes properly treating the B-contained molecular sieve for removing B from skeleton to obtain high-Si molecular sieve with a lot of hydroxy pits, and gas-solid reaction with TiCl4 to obtain TiSi molecular sieve with high catalytic oxidizing performance.

Description

technical field [0001] The invention belongs to the technical field of preparation of titanium silicalite. Background technique [0002] In 1983, US Patent No. 4,410,501 reported the synthesis of titanium silicalite, and its unique catalytic oxidation performance has attracted great attention. However, because the template agent tetrapropylammonium hydroxide is expensive, the cost of TS-1 is very high, which limits its industrial application. Therefore, people have been looking for a cheap way to synthesize titanium silicalite catalysts. Using relatively cheap tetrapropylammonium bromide as template agent and ammonia water and hexamethylenediamine as alkali source, titanium silicalite with high crystallinity can be obtained. However, the titanium silicalite obtained by this type of method generally has relatively large crystallites. Moreover, the conditions for hydrothermal synthesis of TS-1 are harsh and the reproducibility is poor, and it is difficult to avoid the gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C01B37/00C01B39/08
Inventor 郭新闻刘民王祥生
Owner DALIAN UNIV OF TECH
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