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Regeneration method of titanium-silicon molecular sieve

A titanium-silicon molecular sieve and regeneration solution technology, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve environmental protection and economic constraints, high material consumption and energy consumption, and cumbersome and complicated operation processes. Achieve the effect of saving raw materials, increasing yield and reducing pollution

Active Publication Date: 2015-02-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the operation process of this method is cumbersome and complicated, and repeated filtration and washing produce a large amount of industrial wastewater containing acid and ammonia nitrogen, which has high material consumption and energy consumption, and is limited in environmental protection and economy.

Method used

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  • Regeneration method of titanium-silicon molecular sieve

Examples

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Comparison scheme
Effect test

Embodiment 1

[0032] This example illustrates the method for regenerating titanium-silicon molecular sieves provided by the present invention.

[0033] Mix the measured amount of amorphous silica gel with tetrapropylammonium hydroxide, add distilled water, stir at room temperature for 1.5h after mixing, add butyl titanate and stir for 0.5h, then stir at 75°C for 3h to obtain a regeneration solution. Its composition is silicon (mol): titanium (mol): organic base (mol): water (mol) = 0.05: 0.001: 0.15: 20 (where silicon and titanium are SiO 2 and TiO 2 In terms of organic bases in NH 3 meter), the obtained regeneration solution was mixed with a certain amount of filtered mother liquor (from Comparative Example 1, the same below), wherein the mass ratio of the regeneration solution to the filtered mother liquor was 100:15. Take 12g of inactivated TS-1 molecular sieve B-1 and mix with 60g of the above mixture, and then react in a sealed autoclave at 175°C for 52h. The obtained product was fi...

Embodiment 2

[0035] This example illustrates the method for regenerating titanium-silicon molecular sieves provided by the present invention.

[0036] Mix the measured ethyl silicate, ethyl titanate and tetraethylammonium hydroxide, add distilled water, stir at room temperature for 1.0h after mixing, and then stir at 65°C for 3h to obtain a regeneration solution, which consists of silicon (mol ): titanium (mol): organic base (mol): water (mol) = 0.01: 0.0005: 0.2: 35 (where silicon and titanium are SiO 2 and TiO 2 In terms of organic bases in NH 3 Calculate), mix the obtained regeneration solution with a certain amount of filtered mother liquor, wherein the mass ratio of the regeneration solution to the filtered mother liquor is 100:5. Take 12g of inactivated TS-1 molecular sieve B-1 and mix with 80g of the above mixture, and then react in a sealed autoclave at 160°C for 72h. The obtained product was filtered, washed, dried at 135°C for 120min, and then calcined at 500°C for 6h to obtai...

Embodiment 3

[0038] This example illustrates the method for regenerating titanium-silicon molecular sieves provided by the present invention.

[0039] Mix measured ethyl silicate and ethyl titanate with tetraethylammonium hydroxide and ethanolamine, add distilled water, stir at room temperature for 1.0h after mixing, and then stir at 75°C for 3h to obtain a regeneration solution, which consists of silicon (mol): titanium (mol): tetraethylammonium hydroxide (mol): ethanolamine (mol): water (mol) = 0.1: 0.01: 0.08: 0.05: 20 (where silicon and titanium are SiO 2 and TiO 2 In terms of organic bases in NH 3 The obtained regeneration solution is mixed with a certain amount of filtered mother liquor, wherein the mass ratio of the regeneration solution to the filtered mother liquor is 100:150. Take 12g of inactivated TS-1 molecular sieve B-1 and mix with 100g of the above mixture, and then react in a sealed autoclave at 140°C for 12h. The resulting product was filtered, washed, dried at 100°C f...

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Abstract

The invention relates to a regeneration method of a titanium-silicon molecular sieve. The method is characterized by: mixing a regeneration liquid with a filtered stock of a titanium-silicon molecular sieve synthesis process to obtain a mixed solution, contacting the mixed solution with a deactivated titanium-silicon molecular sieve, putting them in a closed reaction kettle to undergo a hydrothermal treatment, and recovering the regenerated titanium-silicon molecular sieve. The titanium-silicon molecular sieve regenerated by the method has activity equal to that of a fresh agent. The method is green and efficient, and has a high yield.

Description

technical field [0001] The invention relates to a method for regenerating titanium-silicon molecular sieves. 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 Ti-MWW 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, oxidation of cyclohexanone, and oxidation of alcohols. They are used as redox molecular sieves The catalyst has a good application prospect. [0003] Italy Taramasso etc. first disclose the preparation method of TS-1 molecular sieve (GB2071071A, US4410501), this method is to prepare a kind of reaction mixture containing silicon source, titanium source, organic base and / or basic oxide earlier, this reaction ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/90B01J29/89
Inventor 史春风朱斌林民
Owner CHINA PETROLEUM & CHEM CORP
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