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Method for synthesizing TS-1 molecular screen

A synthesis method and technology of molecular sieves, applied in the direction of molecular sieve compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve problems such as unstable performance, poor repeatability, and large difference in TS-1 quality, and achieve catalytic oxidation activity and selectivity improvement , reduce the cost of synthesis, reduce the effect of dosage

Active Publication Date: 2008-06-04
CHINA PETROLEUM & CHEM CORP
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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 TS-1 molecular screen
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  • Method for synthesizing TS-1 molecular screen

Examples

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Embodiment 1

[0041] First mix the tetraethyl orthosilicate and tetrabutyl titanate uniformly, then add them to the aqueous solution of tetrapropylammonium hydroxide and stir and mix uniformly. Among them, tetraethyl orthosilicate, tetrabutyl titanate, tetrapropyl The molar ratio of ammonium hydroxide to water is 1:0.04:0.1:15, and hydrolysis is carried out under normal pressure and 40°C under ultrasonic stirring for 2 hours to obtain a titanium and silicon hydrolysis solution. Put the titanium and silicon hydrolyzate into a stainless steel sealed reactor, crystallize it at 170°C and autogenous pressure for 24 hours, filter the resulting crystallized product, wash it with water, and dry it at 110°C for 120 minutes, and then heat it at 550°C. It is calcined at a temperature of ℃ for 3 hours to obtain TS-1 molecular sieve. The yield is about 92%. Its XRD phase diagram is as follows figure 1 As shown in (B), it is similar to the comparative example; the Fourier infrared spectrum is as shown in fi...

Embodiment 2

[0043] Mix tetraethyl orthosilicate and tetrabutyl titanate uniformly and add them to the aqueous solution of tetrapropylammonium hydroxide by ultrasonic stirring and mix uniformly to obtain a hydrolysis solution of titanium and silicon. Among them, tetraethyl orthosilicate and tetrabutyl titanate The molar ratio of ester, tetrapropylammonium hydroxide and water is 1:0.1:0.15:75. Put the titanium and silicon hydrolysate into a stainless steel sealed reactor, and crystallize it at a temperature of 150°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 90%. Its XRD phase diagram is as follows figure 1 As shown in (C), it is similar to the comparative example; the Fourier infrared spectrum is shown as figure 2 As shown in (c), similar to the comparative example, the infrared spectrum is at 960 cm -1 There i...

Embodiment 3

[0045] Mix tetraethylorthosilicate and tetrabutyl titanate uniformly, then add them to the aqueous solution of tetrapropylammonium hydroxide and triethanolamine, and stir and mix uniformly to obtain titanium and silicon hydrolysis solution. Among them, tetraethylorthosilicate, titanium The molar ratio of tetrabutyl phosphate, tetrapropylammonium hydroxide, triethanolamine and water is 1:0.05:0.15:0.15:35. Put this titanium and silicon hydrolyzate into a stainless steel sealed reactor, and set it at a temperature of 170℃ and The crystallized product was crystallized under autogenous pressure for 48 hours, and 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 the product. The yield is about 89%. X-ray diffraction (XRD) and infrared spectroscopy (IR) characterization proved that the obtained sample is TS-1 molecular sieve, and its ultraviolet-visible spectrum has a strong absorption band...

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Abstract

A synthetic method of TS-1 molecular sieve is characterized in that: first mixing silicon source with titanium source, then mixing thereof with organo-alkali compound solution; under the ultrasonic agitation, the hydrolytic solution of silicon and titanium is acquired; then hydrothermally crystallizing the mixture in a reaction vessel and recycling to get TS-1 molecular sieve. 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 (TS-1) with an MFI structure. Background technique [0002] Titanium silicate molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, there have been synthesized TS-1 with MFI-type structure, TS-2 with MEL-type structure, and TS-48 with larger pore structure. Among them, TS-1 molecular sieve is a new type of titanium silicate molecular sieve with excellent catalytic and 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 the oxidant in the oxidation reaction of organics, it avoids the problem of compl...

Claims

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Application Information

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Patent Type & Authority Applications(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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