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High yield rapid synthesis method of titanium-silicon molecular sieve TS-1

A titanium-silicon molecular sieve, TS-1 technology, applied in the direction of molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of large molecular sieve particles, low skeleton titanium content, large amount of templates, etc. Problems, to achieve the effect of short synthesis cycle, fast crystallization rate, and increase crystallization temperature

Active Publication Date: 2016-08-03
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] The purpose of the present invention is to solve the problems existing in the existing synthesis technology of titanium-silicon molecular sieve TS-1, such as low content of skeleton titanium, large amount of template agent, large amount of waste water, long synthesis cycle, low yield or large molecular sieve particles, etc.

Method used

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  • High yield rapid synthesis method of titanium-silicon molecular sieve TS-1
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  • High yield rapid synthesis method of titanium-silicon molecular sieve TS-1

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Effect test

Embodiment 1

[0054] Add 41.7g of methyl orthosilicate into a jacketed three-necked flask, sequentially add 3.4g of tetraethyl titanate and 15.3g of 40wt% tetrapropylammonium hydroxide solution, immerse the three-necked flask in a 40°C water bath, and hydrolyze for 2.5h . After removing the alcohol at 90°C for 1 hour, the hydrolyzed product was put into a crystallization kettle and crystallized at 230°C for 8 hours. After washing and drying the crystallized product, it was roasted at 540°C for 6 hours to obtain TS-1, which is numbered as TS-1-C.

[0055] TS-1 was synthesized according to the above-mentioned method, the 100mL crystallization tank was filled with 70%, and the mass of the synthesized TS-1 molecular sieve was 24.6g.

Embodiment 2

[0057] Add 31.3g of ethyl orthosilicate into a jacketed three-necked flask, sequentially add 2.6g of tetrabutyl titanate and 6.8g of 50wt% tetrapropylammonium hydroxide solution, and immerse the three-necked flask in a 50°C water bath for 1 hour of hydrolysis. After removing the alcohol at 90°C for 0.5h, the hydrolyzed product was put into a crystallization kettle, and crystallized at 240°C for 4h. After washing and drying the crystallized product, it was roasted at 540°C for 5h. The obtained TS-1 was numbered for TS-1-D.

[0058] figure 2 It is a scanning electron microscope photo of titanium silicon molecular sieve TS-1-D; it can be seen from the figure that the particle size of the synthesized TS-1-D sample is about 100nm.

[0059] TS-1 was synthesized according to the above method, the 100mL crystallization tank was filled with 70%, and the mass of TS-1 molecular sieve synthesized was 25.0g.

Embodiment 3

[0061] Add 20.6 g of tetrabutyl titanate and 7.5 g of 40 wt % tetrapropylammonium hydroxide solution in a jacketed three-necked flask, and then immerse the three-necked flask in a 50° C. water bath for 1 hour of hydrolysis. After removing the alcohol at 90°C for 1 hour, the hydrolyzed product was put into a crystallization kettle and crystallized at 250°C for 2 hours. After washing and drying the crystallized product, it was roasted at 540°C for 3 hours to obtain TS-1, which is numbered as TS-1-E.

[0062] image 3 It is the X-ray diffraction spectrum of titanium-silicon molecular sieve TS-1-E; it can be seen from the figure that the synthesized TS-1-E sample has characteristic diffraction peaks of typical MFI structures at 7.8, 8.8, 23.4, 23.9, and 24.4° , and the crystallinity of the sample is very high.

[0063] TS-1 was synthesized according to the above method, the 100mL crystallization tank was filled with 70%, and the mass of TS-1 molecular sieve synthesized was 24.9g...

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Abstract

The invention provides a high yield rapid synthesis method of a titanium-silicon molecular sieve TS-1. The synthesis method comprises the following steps: mixing raw materials namely a silicon source, a titanium source, tetrapropyl ammonium hydroxide and water according to a ratio of SiO2:TiO2:TPAOH:H2O of 1:(0.0501-0.099):(0.0501-0.1499):(0.101-4.999), wherein the silicon source is at least one of n-methyl silicate, n-ethyl silicate, silica sol, and white carbon black; the titanium source is at least one of tetraethyl titanate, tetrabutyl titanate, isopropyl titanate, titanium trichloride, and titanium tetrachloride; carrying out hydrolysis for 0-5 hours at a temperature of 30 to 60 DEG C, performing alcohol removal for 0 to 1 hour at a temperature of 90 DEG C, filling the hydrolysis product into a crystallization kettle, carrying out crystallization for 2 to 10 hours at a temperature of 210 to 250 DEG C; drying, and burning to obtain the titanium-silicon molecular sieve TS-1. The titanium-silicon molecular sieve TS-1 synthesized by the provided method has the advantages of high content of titanium in skeleton, little using amount of template, no generation of wastewater, and high crystallization speed. The particle size of obtained nano level titanium-silicon molecular sieve is about 100 nm. The titanium-silicon molecular sieve has an excellent catalytic performance on alkene epoxidation and aromatic hydrocarbon hydroxylation.

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis, in particular to a rapid synthesis method of titanium-silicon molecular sieve TS-1 with high catalytic oxidation activity. Background technique [0002] Since the synthesis of titanium-silicon molecular sieve TS-1 was first reported in US Patent US4410501 in 1983, its oxidation system with hydrogen peroxide has shown high activity for olefin epoxidation, aromatic hydrocarbon hydroxylation, and ketone ammoxidation. Moreover, the by-product is water, which belongs to an environmentally friendly process, so it has attracted widespread attention. [0003] The synthetic method of the titanium-silicon molecular sieve disclosed by U.S. Patent No. 4,410,501 adopts ethyl orthosilicate as a silicon source, tetraethyl titanate as a titanium source, and tetrapropylammonium hydroxide (TPAOH) as a template agent in a hydrothermal system. Among them, it is obtained by crystallization for 6 to 30 day...

Claims

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Application Information

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IPC IPC(8): C01B39/08
CPCC01B39/085C01P2002/72C01P2002/82C01P2004/03C01P2004/62C01P2004/64
Inventor 左轶郭新闻刘民
Owner DALIAN UNIV OF TECH
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