Method for preparing TS-1 molecular sieve

A molecular sieve, TS-1 technology, applied in molecular sieve compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of long synthesis time, waste, environmental pollution, etc., to improve synthesis efficiency, reduce preparation costs, and improve efficiency. Effect

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AI Technical Summary

Problems solved by technology

[0012] In the existing technology for preparing titanium-silicon molecular sieves (such as GB2,071,071A, USP4,410,501, and Zeolites, 1992, Vol.12:943), it is necessary to heat and remove alcohol during the early synthesis, so that the early synthesis time is relatively long
At the same time, the utilization rate of organosilicon is about 75-95%, and the utilization rate of template agent is about 50-95%. In this way, 5-25% of organosilicon and 5-50% of template agent are left in the synthetic waste liquid and are not obtained. If it is used as sewage, it will not only cause a lot of waste, but also pollute the environment.

Method used

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  • Method for preparing TS-1 molecular sieve
  • Method for preparing TS-1 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Mix tetraethyl orthosilicate and tetrabutyl titanate evenly, and then add the mixed solution to the aqueous solution of tetrapropyl ammonium hydroxide and mix evenly, wherein tetraethyl orthosilicate, tetrabutyl titanate, tetrapropyl The molar ratio of basic ammonium hydroxide to water is 1:0.035:0.25:85, hydrolyzed at normal pressure and 40° C. for 2 hours to obtain titanium and silicon hydrolysis solution.

[0068] Add cetyltrimethylammonium bromide to the obtained titanium and silicon hydrolyzate, mix the hydrolysis solution of titanium and silicon with the ratio of 25:1 by weight of cetyltrimethylammonium bromide, and quickly There is agglomeration of solid particles.

[0069] Filter out the solid particles and put them into a stainless steel sealed reaction vessel, crystallize at 170°C under autogenous pressure for 24 hours, filter the resulting crystallized product, wash with water, and dry at 110°C for 120 minutes, then in 550°C Calcined at ℃ for 3 hours to obta...

Embodiment 2

[0072] A proper amount of tetraethyl orthosilicate and tetraethyl titanate were added successively to the remaining filtrate in Example 1 at a molar ratio of 1:0.1, and solid particles agglomerated quickly. Filter out the solid particles and put them into a sealed stainless steel reaction vessel, crystallize at 170°C under autogenous pressure for 24 hours, filter the obtained crystallized product, wash with water, and dry at 110°C for 120 minutes, then in 550°C Calcined at ℃ for 3 hours to obtain TS-1 molecular sieve.

[0073] The XRD crystal phase diagram is as shown in Figure 1 (C), and the relative crystallinity is 96.4%; -1 The characteristic absorption peak that all-silicon molecular sieves do not have appears nearby, indicating that titanium has entered the molecular sieve framework.

Embodiment 3

[0075] An appropriate amount of tetrabutyl orthosilicate and tetraethyl titanate were added successively to the remaining filtrate in Example 2 at a molar ratio of 0.25:1, and solid particles agglomerated quickly. Filter out the solid particles and put them into a stainless steel sealed reaction kettle, stir and pre-crystallize at a temperature of 110°C and autogenous pressure for 2.5 hours, then raise the temperature to 170°C, continue to stir and crystallize for 24 hours, and the obtained crystallized product Filter, wash with water, dry at 110°C for 120 minutes, and then bake at 550°C for 3 hours to obtain TS-1 molecular sieve.

[0076] The XRD crystal phase diagram is as shown in Figure 1 (D), and the relative crystallinity is 96.1%; -1 The characteristic absorption peak that all-silicon molecular sieves do not have appears nearby, indicating that titanium has entered the molecular sieve framework.

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Abstract

The TS-1 molecular sieve preparing process features that surfactant is added into the mother liquid for synthesizing the molecular sieve, so that most of the silicon source and titanium source after hydrolysis agglomerate into solid grains. After the solid grains are filtered out and crystallized, the filtrate containing small amount of residual silicon source and titanium source is used as the alkali source for hydrolyzing the newly added silicon source and titanium source for synthesizing the next batch of molecular sieve. The process has greatly reduced environmental pollution, lowered preparation cost and raised synthesizing efficiency and benefit.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve, and more specifically relates to a preparation method of 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. This type of molecular sieve has excellent selective oxidation performance and high catalytic activity for many organic oxidation reactions, such as epoxidation of olefins, hydroxylation of aromatic hydrocarbons, oximation of cyclohexanone, and oxidation of alcohols. -ox) type molecular sieve catalysts have good application prospects. [0003] TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B37/00
Inventor 林民史春风龙军朱斌舒兴田汪燮卿汝迎春
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