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Hydro-thermal synthesis method for TS-1 molecular sieve and obtained product

A hydrothermal synthesis, TS-1 technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems that are difficult to promote to industrial applications, increase production costs, etc., and achieve easy promotion, increase content, Effects with small magnification effects

Inactive Publication Date: 2016-05-25
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most methods for synthesizing multi-level structure TS-1 molecular sieves use organic additives such as mesoporous templates or organosilanes, which increases production costs and is difficult to promote to industrial applications.

Method used

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  • Hydro-thermal synthesis method for TS-1 molecular sieve and obtained product
  • Hydro-thermal synthesis method for TS-1 molecular sieve and obtained product
  • Hydro-thermal synthesis method for TS-1 molecular sieve and obtained product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1T

[0034] The synthesis of embodiment 1TS-1 molecular sieve

[0035] 1. Take 15 grams of ethyl orthosilicate (according to SiO 2 0.07mol) was added to 17 grams of tetrapropylammonium hydroxide (concentration is 25%, 0.02mol by TPAOH), stirred for 30 minutes to obtain the silicon source hydrolyzate, and 1.62 grams of butyl titanate (by TiO 2 0.00466mol) was added to 9.28 grams of isopropanol (0.155mol), stirred for 5 minutes, added to the above-mentioned silicon source hydrolyzate, stirred for 60 minutes, added 39.3 grams of water (2.18mol), stirred for 30 minutes, and the initial gel;

[0036] 2. Put the initial gel into the reactor and crystallize at 100 degrees Celsius for 7 hours, and cool to room temperature after crystallization;

[0037] 3. Take 15 grams of ethyl orthosilicate (according to SiO 2 0.07mol) was added to the product obtained in step 2, stirred for 30 minutes, heated and stirred in a water bath at 60 degrees Celsius for 150 minutes to remove isopropanol to o...

Embodiment 2

[0041] The synthesis of embodiment 2TS-1 molecular sieve

[0042] 1. Take 15 grams of ethyl orthosilicate (according to SiO 2 0.07mol) was added to 17 grams of tetrapropylammonium hydroxide (concentration is 25%, 0.02mol by TPAOH), stirred for 30 minutes to obtain the silicon source hydrolyzate, and 1.62 grams of butyl titanate (by TiO 2 0.00466mol) was added to 9.28 grams of isopropanol (0.155mol), stirred for 5 minutes, added to the above-mentioned silicon source hydrolyzate, stirred for 60 minutes, added 39.3 grams of water (2.18mol), stirred for 30 minutes, and the initial gel was prepared. glue;

[0043] 2. Put the initial gel into the reactor and crystallize at 100 degrees Celsius for 24 hours, and cool to room temperature after crystallization;

[0044] 3. Take 15 grams of ethyl orthosilicate (according to SiO 20.07mol) was added to the product obtained in step 2, stirred for 30 minutes, heated and stirred in a water bath at 60 degrees Celsius for 150 minutes to remo...

Embodiment 3

[0049] 1. Take 15 grams of ethyl orthosilicate (according to SiO 2 0.07mol) was added to 17 grams of tetrapropylammonium hydroxide (concentration is 25%, 0.02mol by TPAOH), stirred for 30 minutes to obtain silicon source hydrolyzate, and 1.62 grams of butyl titanate (by TiO 2 0.00466mol) was added to 9.28 grams of isopropanol (0.155mol), stirred for 5 minutes, added to the above-mentioned silicon source hydrolyzate, stirred for 60 minutes, added 39.3 grams of water (2.18mol), stirred for 30 minutes, and the initial gel was prepared. glue;

[0050] 2. Put the initial gel into the reactor and crystallize at 100 degrees Celsius for 24 hours, and cool to room temperature after crystallization;

[0051] 3. Take 15 grams of ethyl orthosilicate (according to SiO 2 0.07mol) was added to the product obtained in step 2, stirred for 30 minutes, heated and stirred in a water bath at 60 degrees Celsius for 150 minutes to remove alcohol, and 3.6 grams of ammonia water (concentration was 2...

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Abstract

The invention provides a hydro-thermal synthesis method for a TS-1 molecular sieve. The hydro-thermal synthesis method includes the steps that 1, a silicon source and a template agent are mixed to obtain silicon source hydrolysate, a titanium source and polyhydric alcohol are mixed to be added into the silicon source hydrolysate, and then water is added; 2, a product obtained through step1 is subjected to pre-crystallization for 5-24 hours; 3, a silicon source is added again and heated to 60 DEG C-90 DEG C, and then polyhydric alcohol is removed; 4, a product obtained through step3 is crystallized, after the crystallization reaction, a reaction mixture is subjected to solid-liquid separation, and a solid is taken to be dried and calcined. In the hydro-thermal synthesis method, after the silicon source and the titanium source are gelatinized, alcohol is not removed, namely, crystallization is performed for 5-24 hours at 90 DEG C-100 DEG C under the presence of alcohol, in this way, forming of non-framework titanium can be effectively reduced, and the content of framework titanium can be increased. In the process of constructing a multi-level structure in the TS-1 molecular sieve, no mesporous template agent, organosilane and other organic additives are needed, in the whole synthesis process, operation is easy, the cost is low, an expected amplification effect is small, and large-scale industrial production and popularization are easy.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to the preparation and application of a titanium-containing molecular sieve catalyst. Background technique [0002] TS-1 molecular sieve is a kind of microporous molecular sieve with MFI topology. The four-coordinate titanium isolated on its skeleton is a good active center for oxidation reaction. The regular pore structure endows it with good shape selectivity and stability. The green oxidation system composed of TS-1 molecular sieve and hydrogen peroxide is widely used in selective oxidation reactions such as olefin epoxidation, phenol hydroxylation, ketone ammoximation, and alkane oxidation. It has mild reaction conditions, high atom utilization, and is environmentally friendly. Pollution and other outstanding advantages, it overcomes the disadvantages of traditional organic oxidation reaction, such as large amount of waste liquid and slag, and serious environmental pollution...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J37/10C07C249/04C07C251/44
CPCB01J29/89B01J37/10C07C249/04C07C251/44
Inventor 曹鹏窦涛吴志杰张军亮顾洪歌王海玲
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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