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Treatment method of deactivated titanium-silicon molecular sieve

A titanium-silicon molecular sieve and processing method technology, applied in molecular sieve catalysts, chemical instruments and methods, chemical/physical processes, etc., to achieve the effects of saving raw materials, reducing material consumption, and restoring relative crystallinity

Active Publication Date: 2014-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there is no report on using this filtered waste liquid to treat the deactivated titanium-silicon molecular sieve

Method used

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  • Treatment method of deactivated titanium-silicon molecular sieve

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Effect test

Embodiment 1

[0041] Mix measured tetrapropyl silicate, tetraethyl titanate and tetramethylammonium hydroxide, add distilled water, mix well, stir at room temperature for 1.0h for hydrolysis, and then stir at 75°C for 3h to obtain reclaimed rubber. Its molar composition is silicon: titanium: organic base: water = 1: 0.02: 0.75: 20 (silicon and titanium are represented by SiO 2 and TiO 2 In terms of organic bases in NH 3 , the same below), then mixed the reclaimed rubber and the filtered mother liquor according to the mass ratio of 100:10 to obtain a mixed solution; then mixed the inactivated molecular sieve sample S-1 with the above mixed solution according to the mass ratio of 100:40, Put it into a 50mL polytetrafluoroethylene liner and place it in a 100mL polytetrafluoroethylene liner, and react in a sealed autoclave at 145°C for 60h. The obtained molecular sieve regenerated by steam treatment was dried at 180° C. for 120 minutes, and then calcined at 580° C. for 5 hours to obtain the r...

Embodiment 2

[0043] Mix the metered Z-type silica gel with tetrapropylammonium hydroxide, add distilled water, mix well, stir at room temperature for 1.0h, then add butyl titanate and stir for 0.5h, then stir at 65°C for 6h to obtain reclaimed rubber. Its molar composition is silicon: titanium: organic base: water = 1: 0.025: 0.8: 20, then the reclaimed rubber and the filtered mother liquor are mixed according to the mass ratio of 100: 50 to obtain a mixed solution; then the roasted molecular sieve sample B -1 Mix with the above mixed solution at a mass ratio of 100:50, put it into a 50mL polytetrafluoroethylene liner and place it in a 100mL polytetrafluoroethylene liner, and then react in a sealed autoclave at 175°C for 48h . The obtained product was dried at 135° C. for 180 minutes, and then calcined at 500° C. for 6 hours to obtain regenerated TS-1 molecular sieve B.

Embodiment 3

[0045] Mix measured tetraethyl orthosilicate, tetraethyl titanate, tetraethylammonium hydroxide and n-butylamine, add distilled water, mix well, stir at room temperature for 1.0h for hydrolysis, and then stir at 70°C for 4h, Obtain the reclaimed rubber, its molar composition is silicon: titanium:: tetraethylammonium hydroxide: n-butylamine: water=1: 0.02: 0.35: 0.3: 25, then the reclaimed rubber and the filtered mother liquor are 100: 40 according to the mass ratio The proportion of mixing to get a mixed solution; then the inactivated molecular sieve sample S-2 and the above mixed solution were mixed according to the mass ratio of 100:20, it was packed into 50mL polytetrafluoroethylene liner and placed in 100mL polytetrafluoroethylene Lined with ethylene, and then reacted at 160°C for 65h in a sealed autoclave. The obtained product was dried at 100° C. for 300 minutes, and then calcined at 650° C. for 4 hours to obtain regenerated TS-1 molecular sieve C.

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Abstract

The invention relates to a treatment method of a deactivated titanium-silicon molecular sieve. The method includes: mixing a reclaimed rubber with a filtrated stock obtained in a titanium silicon molecular sieve synthesis process to obtain a mixed solution, then contacting the mixed solution with a deactivated titanium-silicon molecular sieve and placing them in a sealed reaction kettle, conducting a treatment for at least 2h at a temperature of 120-200DEG C, and then drying and roasting the product under normal temperature and pressure to obtain a regenerated titanium silicon molecular sieve. Specifically, the reclaimed rubber contains a silicon source, a titanium source and organic alkali, the reaction kettle contains a water amount able to form saturated steam under the reaction conditions, and the weight ratio of the water to the deactivated titanium-silicon molecular sieve is less than 1.2. Meanwhile, the treating amount of the deactivated titanium-silicon molecular sieve is at least 10g / L reaction kettle volume. After treatment by the method, the titanium-silicon molecular sieve has equal activity to a fresh agent. The regeneration process has low material consumption and high yield, and is green and efficient.

Description

technical field [0001] The invention relates to a method for treating inactivated 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] TS-1 is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing the transition metal element titanium into the molecular sieve framework with ZSM-5 structure. It not only has the cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/90B01J29/89B01J38/66B01J38/48B01J38/52C07C37/60
CPCY02P20/584
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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