Method for synthesizing titanium silicalite molecular sieve

A titanium-silicon molecular sieve and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of complex synthesis process, increased cost, and reduced output of a single reactor, etc.

Inactive Publication Date: 2015-06-10
QUFU NORMAL UNIV
View PDF4 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. In the traditional process of synthesizing titanium-silicon molecular sieves, the amount of template tetrapropylammonium hydroxide used in the synthesis of molecular sieves is large, and the molar ratio of tetrapropylammonium hydroxide (TPAOH) to silicon oxide is above 0.35, and its synthesis cost accounts for the total More than 90% of the cost of consumables;
[0004] 2. The silicon and titanium raw materials used for synthesis are o

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Tetrabutyl titanate (0.01mol) was added dropwise to 25% TPAOH aqueous solution (TPAOH content 0.02mol), stirred at room temperature to form a clear solution, and then tetraethyl silicate (0.04mol) was added to the clear solution at 20°C Stir and hydrolyze for 3h, then remove the alcohol produced by hydrolysis at 40~60℃, and then make up the volatilized water to make the molar composition of TiO 2 :SiO 2 :TPAOH:H2O=0.25:1.0:0.35:20, then react in a polytetrafluoroethylene autoclave at 80~100℃ for 24 hours;

[0019] The mixture obtained above is mixed with solid silica gel (0.36mol), dried at 40°C to form a solid mixture, the molar composition of the solid mixture is TiO 2 :SiO 2 :TPAOH=0.0125:1.0:0.10, react the solid mixture at 180°C for 36h in a closed reaction kettle, take out the solid after cooling, dry it at 100°C for 12 hours, and then calcinate at 500-600°C to remove organics in an air atmosphere to obtain TS- 1 molecular sieve.

Embodiment 2

[0021] Add tetrabutyl titanate (0.01mol) dropwise to 25% TPAOH aqueous solution (TPAOH content 0.02mol), stir at room temperature to form a clear solution, then add silica sol (0.04mol) to the clear solution, stir and hydrolyze at 40℃ 1h, then remove the alcohol produced by hydrolysis at 60~80℃, and then make up the volatilized water to make the molar composition of TiO 2 :SiO 2 :TPAOH:H2O=0.05:1.0:0.35:20, then react in a polytetrafluoroethylene autoclave at 80~100℃ for 24 hours;

[0022] The mixture obtained above is mixed with white carbon black (0.36mol), dried at 40~80℃ to form a solid mixture, the molar composition of the solid mixture is TiO 2 :SiO 2 :TPAOH=0.05:1.0:0.025, react the solid mixture at 170°C for 96h in a closed reaction kettle, take out the solid after cooling, dry it at 100°C for 12 hours, and then calcinate at 500-600°C to remove organics in an air atmosphere to obtain TS- 1 molecular sieve.

Embodiment 3

[0024] Add tetrabutyl titanate (0.01mol) dropwise to 25% TPAOH aqueous solution (TPAOH content 0.02mol), stir at room temperature to form a clear solution, then add white carbon black (0.04mol) to the clear solution and stir at 30°C Hydrolyze for 2h, then remove the alcohol produced by hydrolysis at 50~70℃, and then make up the volatilized water to make the molar composition of TiO 2 :SiO 2 :TPAOH:H2O=0.25:1.0:0.25:20, then react in a polytetrafluoroethylene autoclave at 80~100℃ for 24 hours;

[0025] The mixture obtained above is mixed with white carbon black (0.36mol), dried at 40~80℃ to form a solid mixture, the molar composition of the solid mixture is TiO 2 :SiO 2 :TPAOH=0.025:1.0:0.05, the solid mixture is reacted at 180°C for 12h in a closed reaction kettle, and the solid is taken out after cooling, dried at 100°C for 12 hours, and then calcined at 500-600°C in an air atmosphere to remove organics to obtain TS- 1 molecular sieve.

[0026] The present invention first hydrolyz...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Specific surface areaaaaaaaaaaa
Login to view more

Abstract

The invention relates to a method for synthesizing a titanium silicalite molecular sieve, which comprises the following steps: mixing, stirring and hydrolyzing a titanium-containing compound, a TPAOH aqueous solution and a silicon raw material, and putting the obtained mixture into a high-pressure reaction kettle to heat for reacting; and mixing an obtained reaction mixture with solid silica gel, drying the obtained object so as to obtain a solid mixture, carrying out heating reaction on the solid mixture in an airtight reaction kettle, after the solid mixture is cooled, taking out and then roasting the solid mixture so as to remove organic matters, so that a TS-1 molecular sieve is obtained. In the technical scheme above, by reducing the application amount of a guiding agent tetrapropylammonium hydroxide (TPAOH), taking inorganic silicon oxide for replacing organosilicone as a raw material, and taking a solid-phase solvent-free crystallization method, the steps of filtering, washing and the like are omitted, thereby simplifying the synthesis operation of the TS-1 molecular sieve and reducing the synthetic cost.

Description

Technical field [0001] The invention relates to the field of molecular sieve synthesis, in particular to a method for synthesizing titanium silicon molecular sieve. Background technique [0002] Titanium silicate molecular sieve (TS-1) as a catalyst has the characteristics of mild reaction conditions, process safety, and good atomic economy in the catalytic reaction process. However, compared with other aluminosilicate zeolites, the synthesis process of TS-1 molecular sieve is complicated and the raw materials used are more expensive. It has the following disadvantages: [0003] 1. In the traditional synthesis process of titanium silicate molecular sieve, the template agent tetrapropylammonium hydroxide used in the synthesis of molecular sieve is used in a large amount, the molar ratio of tetrapropylammonium hydroxide (TPAOH) to silica is over 0.35, and its synthesis cost accounts for the total More than 90% of the cost of consumables; [0004] 2. The silicon and titanium raw mater...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C01B39/08
Inventor 岳明波王晓宁张建辉刘志秦丹
Owner QUFU NORMAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap