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Titanium silicalite molecular sieve and preparation and application thereof

A technology of titanium-silicon molecular sieve and silicon source, which is applied in the direction of molecular sieve compounds, molecular sieve catalysts, molecular sieve characteristic silicates, etc., can solve the problems of cost increase and synthesis cost increase, and achieve the reduction of the burden of alcohol removal, low price and rich synthesis The effect of raw materials

Active Publication Date: 2018-11-13
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

The introduction of alcohol increases the cost of subsequent alcohol removal and increases the synthesis cost. Therefore, it is very important to find a new way to introduce titanium source and avoid the addition of alcohol complexing agent.

Method used

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  • Titanium silicalite molecular sieve and preparation and application thereof
  • Titanium silicalite molecular sieve and preparation and application thereof
  • Titanium silicalite molecular sieve and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 46.2g of tetraethyl orthosilicate to the beaker and stir, then add 44g of 25wt% TPAOH aqueous solution and 38g of water, and hydrolyze at 30°C for 2h to obtain a silicon source hydrolysis mixture; add it to 0.52g of metatitanic acid, stirring conditions Then add 3.0g 30wt% H 2 o 2 aqueous solution and 10g of 25wt% TPAOH aqueous solution, and then stirred for 30min to obtain the titanium source hydrolysis mixture; the titanium source and the silicon source hydrolysis mixture were mixed, and alcohol was removed at 80°C for 1.5h, 50.2g of water was added and stirred for 30min, and the obtained The transparent glue was put into a crystallization kettle for crystallization, and crystallized at 170°C for 36 hours. After washing and drying, the obtained crystallized product was calcined at 540°C for 6 hours to obtain TS-1, which was designated as TS-1-B.

[0026] figure 1 It is the infrared absorption spectrum of TS-1-B, in the infrared spectrum at 960cm -1 The infrared...

Embodiment 2

[0029] Repeat the process in Example 1, just change the silicon source into silica sol, silica gel or fumed silica (white carbon black), keep the amount of the substance of silicon dioxide constant, after crystallization, through washing, drying, roasting Then get TS-1.

Embodiment 3

[0031] Repeat the process in Example 1, but change metatitanic acid to orthotitanic acid, keep the amount of titanium dioxide unchanged, after crystallization, obtain TS-1 after washing, drying and roasting, denoted as TS-1- c.

[0032] image 3 It is a scanning electron micrograph of TS-1-C, and it can be seen that the grain size of TS-1 is 100-200nm.

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Abstract

The invention provides a method for preparing a titanium silicalite molecular sieve TS-1. Solid metatitanic acid and photodegredation are used as a titanium source for performing synthesis of the TS-1. An alcohol substance does not need to be added in a process of introducing the new titanium source, a certain load is relieved for follow-up alcohol-removing steps, and the metatitanic acid and photodegredation are cheap in price, synthesis cost can be reduced. Catalytic performance of the TS-1 catalyst prepared by using the metatitanic acid and photodegredation as the titanium source is equivalent to that of the TS-1 prepared by a traditional method.

Description

technical field [0001] The invention relates to a titanium silicon molecular sieve and its preparation and application. technical background [0002] Titanium-silicon molecular sieves were first synthesized by Taramasso et al. in 1983. This molecular sieve has excellent catalytic performance in low-temperature selective oxidation, and has been one of the research hotspots of green chemistry for many years. Titanium silicate molecular sieves have been successfully used to catalyze propylene and H 2 o 2 Epoxidation to produce propylene oxide, and used in the ammoximation reaction of cyclohexanone, exhibits good catalytic oxidation activity, high product selectivity, and mild reaction conditions. [0003] The catalytic activity of titanium-silicon molecular sieve TS-1 is closely related to its preparation method, and the catalytic performance mainly depends on whether TS-1 has the characteristics of small crystal grains and high content of titanium in the four-coordinated fra...

Claims

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Application Information

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IPC IPC(8): C01B37/00B01J29/89B01J37/08C07D303/04C07D301/12C07C249/04C07C251/44
CPCB01J29/89B01J37/0009C01B37/005C01P2002/72C01P2002/82C01P2004/03C01P2004/62C07C249/04C07D301/12C07D303/04C07C251/44Y02P20/52
Inventor 黄家辉吕强
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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