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Method for synthesizing titanium-silicon molecular screen

A technology of silicon source and titanium source, which is applied in the direction of molecular sieve compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of unstable performance, poor repeatability, and large difference in TS-1 quality, so as to speed up the synthesis speed and catalytic oxidation The effect of improving activity and selectivity and reducing dosage

Active Publication Date: 2013-03-06
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

In the existing technology for synthesizing titanium-silicon molecular sieves (such as Zeolites, 1992, Vol.12: 943), although the improved method can increase the content of titanium in the skeleton, it does not fundamentally solve the polymerization of titanium in the colloidal process This is the main reason why the quality of TS-1 synthesized by different laboratories using the same method varies greatly, and even the performance of different batches synthesized by the same operator is unstable and poor in repeatability

Method used

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  • Method for synthesizing titanium-silicon molecular screen
  • Method for synthesizing titanium-silicon molecular screen
  • Method for synthesizing titanium-silicon molecular screen

Examples

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Effect test

Embodiment 1

[0033] Add tetraethyl orthosilicate and tetrabutyl titanate successively into the aqueous solution of tetrapropyl ammonium hydroxide and mix them uniformly by ultrasonic stirring, among which tetraethyl orthosilicate, tetrabutyl titanate, tetrapropyl ammonium hydroxide The molar ratio with water is 1:0.04:0.05:25, hydrolyzed at normal pressure and 40° C. for 2 hours to obtain titanium and silicon hydrolysis solution. Put the titanium and silicon hydrolyzate into a sealed stainless steel reaction kettle, crystallize at 170°C and autogenous pressure for 24 hours, filter the resulting crystallized product, wash with water, and dry at 110°C for 120 minutes, then dry it at 550°C ℃ for 3 hours to obtain TS-1 molecular sieve. The yield is about 90%. Its XRD crystal phase diagram is as follows figure 1 Shown in (B), similar to comparative example; Fourier transform infrared spectrogram is as figure 2 As shown in (b), it is also similar to the comparative example, at 960cm -1 The ...

Embodiment 2

[0035] Add tetrabutyl titanate and tetraethyl orthosilicate successively to the aqueous solution of tetrapropyl ammonium hydroxide and ultrasonically stir and mix uniformly to obtain titanium and silicon hydrolysis solution, in which tetraethyl orthosilicate, tetrabutyl titanate, The molar ratio of tetrapropylammonium hydroxide and water is 1: 0.1: 0.15: 55. Put this titanium and silicon hydrolyzate into a stainless steel sealed reaction kettle, and crystallize it for 72 hours at a temperature of 150° C. and under autogenous pressure. The crystallized product was filtered, washed with water, dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain TS-1 molecular sieve. The yield is about 89%. Its XRD crystal phase diagram is as follows figure 1 Shown in (C), similar to comparative example; Fourier transform infrared spectrogram is as figure 2 Shown in (c), similar to the comparative example, in the infrared spectrum at 960cm -1 The infrared absorpti...

Embodiment 3

[0037] Add tetraethyl orthosilicate and tetrabutyl titanate to the aqueous solution of tetrapropylammonium hydroxide and triethanolamine respectively, and ultrasonically stir and mix evenly, then mix and ultrasonically stir for a period of time to obtain titanium and silicon hydrolysis solution, in which orthosilicic acid The molar ratio of tetraethyl ester, tetrabutyl titanate, tetrapropyl ammonium hydroxide, triethanolamine and water is 1: 0.2: 0.15: 0.15: 85, put the titanium and silicon hydrolyzate into a stainless steel sealed reaction kettle, and After crystallization at 130°C and autogenous pressure for 96 hours, the obtained crystallized product was filtered, washed with water, dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain TS-1 molecular sieve. The yield is about 88%, and it is proved by X-ray diffraction (XRD) and infrared spectrum (IR) that the obtained sample is TS-1 molecular sieve.

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Abstract

A method of synthesizing titanium silicate molecular sieve is to hydrothermally crystallize the hydrolytic solution of silicon and titanium in a closed reaction vessel and then recycle the product. The method is characterized in that the hydrolytic solution of silicon and titanium is gotten by any one of the following three methods: A. under ultrasonic agitation, silicon source is first hydrolyzed in organo-alkali compound solution and then the titanium source is hydrolyzed in the solution; B. under the ultrasonic agitation, titanium source is first hydrolyzed in organo-alkali compound solution and then the silicon source is hydrolyzed in the solution; C. under the ultrasonic agitation, silicon source and titanium source are respectively hydrolyzed in organo-alkali compound solution and then mixed together. The synthetic method can eliminate partial uneven concentration, leads the amount of TiO2 generated by self agglomeration after the hydrolysis of titanium source to be as little as possible and reduces the production of extra framework titanium. Compared with the prior art, the TS-1 molecular sieve synthesized by the method not only has better catalytic oxidation activity and selectivity but also has better stability of catalytic activity.

Description

technical field [0001] The invention relates to a method for synthesizing a titanium-silicon molecular sieve, more particularly to a method for synthesizing a titanium-silicon molecular sieve (TS-1) with an MFI structure. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. TS-1 with MFI structure, TS-2 with MEL structure, and TS-48 with larger pore structure have been synthesized so far. Among them, TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. Since TS-1 molecular sieve can use non-polluting low-concentration hydrogen peroxide as an oxidant in the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08C01B37/00B01J29/89
Inventor 林民史春风龙军朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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