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Preparation method and application of alkaline titanium silicalite molecular sieve TS-1

A titanium silicon molecular sieve, TS-1 technology, applied in molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., to achieve the effect of high selectivity, simple operation and consumption saving

Active Publication Date: 2021-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] According to one aspect of the present application, a preparation method of basic titanium-silicon molecular sieve TS-1 is provided, which solves the problem that basic additives need to be used in the existing propylene epoxidation reaction process

Method used

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  • Preparation method and application of alkaline titanium silicalite molecular sieve TS-1
  • Preparation method and application of alkaline titanium silicalite molecular sieve TS-1
  • Preparation method and application of alkaline titanium silicalite molecular sieve TS-1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1: Preparation of amino-modified amorphous mesoporous titanium dioxide / silica spheres

[0055] Under the condition of stirring at 30-100°C, dissolve the structure directing agent I (R) in 60 mL of deionized water and ethanol solution, then add ammonia water to the solution to adjust the pH value of the solution, and then add an amino-free silicon source ( Component II), aminosilane coupling agent (component I) and titanium source, and continue stirring for 2-12 hours. After the product was filtered, washed, washed with water, and dried, the structure-directing agent I was removed by reflux in an acidic ethanol solution to obtain a white powder, which was designated as samples MTS-I~MTS-VI. The raw material types and proportions, reaction temperature and time of the prepared samples MTS-I~MTS-VI are shown in Table 1 respectively.

[0056] Table 1 Synthesis conditions and performance parameters of mesoporous titania / silicon

[0057]

[0058]

[0059] Sampl...

Embodiment 2

[0060] Embodiment 2: Preparation of samples TS-1-1~TS-1-8

[0061] Preparation of sample TS-1-1:

[0062] Firstly, tetrapropylammonium hydroxide (structure directing agent II) was added into deionized water, stirred and dissolved to obtain a mixed solution. A certain amount of the above solution was taken to impregnate the amino-modified amorphous titanium oxide / silicon spheres prepared in Example 1, and dried at room temperature for a period of time to obtain a solid mixture. The above solid mixture was transferred to the upper plate of the stainless steel autoclave, and water was added to the bottom of the autoclave. Seal the stainless steel reaction kettle, put it in an oven, and crystallize at 100-200°C for 12-100h. Cool quickly after the reaction, separate the solid product, wash with deionized water, dry at 110°C in the air atmosphere for 12 hours, stir and wash in ethanol solution for 6 hours, and then centrifuge and dry to obtain the basic TS-1 molecular sieve. The s...

Embodiment 3

[0070] Embodiment 3: Propylene epoxidation reaction evaluation

[0071] In the experiment, the TS-1 sample was synthesized by the traditional hydrothermal method, and the ratio of the synthetic gel was 1SiO 2 :0.25TPAOH:0.02TiO 2 :35H 2 O. Concrete gel preparation steps: first, add tetrapropylammonium hydroxide (TPAOH) to deionized water at room temperature and stir; after it is fully dissolved, slowly add a certain amount of ethyl orthosilicate and butyl titanate; After continuing to stir at room temperature for 24h, the raw material was transferred to a stainless steel synthesis kettle and crystallized at 150°C for 24h. The resulting solid product was centrifuged, washed, dried overnight at 110°C, and finally calcined at 550°C for 6 hours to remove the organic template, which was named conv-TS-1.

[0072] The prepared conv-TS-1 and the basic TS-1 molecular sieve prepared in Example 2 were evaluated for the epoxidation reaction of propylene, and the epoxidation reaction o...

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Abstract

The invention discloses a preparation method of an alkaline titanium silicalite molecular sieve TS-1. The preparation method comprises the following steps: 1) subjecting a silicon source and a titanium source to reacting in an alkaline system to obtain an amino-containing titanium dioxide / silicon composite material; 2) adding the amino-containing titanium dioxide / silicon composite material obtained in the step 1) into a solution containing a structure-directing agent II, and conducting drying to obtain an initial synthesis mixture; 3) carrying out a crystallization reaction on the initial synthesis mixture obtained in the step 2) by adopting a dry gel method; and 4) separating and roasting a reaction product obtained in the step 3) to obtain the alkaline titanium silicalite molecular sieve TS-1. According to the method, raw materials can be effectively utilized, and production cost is saved; and compared with the prior art, the method is simple and feasible, the prepared TS-1 molecular sieve crystal is high in crystallinity and contains an alkaline center and a framework titanium oxidation active center, and the content of framework titanium and the content of amino groups can be adjusted in a wide range.

Description

technical field [0001] The application relates to a preparation method and application of basic titanium-silicon molecular sieve TS-1, belonging to the technical field of catalyst synthesis. Background technique [0002] Propylene oxide is an important basic organic chemical raw material, the largest use is the production of polyether polyols, and then as a polyurethane raw material; followed by the production of widely used propylene glycol, propylene glycol ether, isopropanolamine, allyl alcohol, 1, 4-butanediol, etc., and propylene oxide can also be used in large quantities in the production of nonionic surfactants, oil field demulsifiers, pesticide emulsifiers and developers, etc. Propylene oxide derivatives are widely used in industry and people's daily life, such as automobile, construction, food, medicine and cosmetics industries, which are of great significance to improving the quality of human life. [0003] At present, the industrial production of propylene oxide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B39/04B01J29/89C07D301/12C07D303/04
CPCC01B39/085C01B39/04B01J29/89C07D301/12C07D303/04C01P2004/61C01P2004/62C01P2004/64C01P2004/03C01P2002/72B01J2229/36B01J2229/38
Inventor 张晓敏许磊陈磊赵晓炜
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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