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Hydrothermal regenerating method of titanium silicon molecular sieve

A titanium-silicon molecular sieve, hydrothermal technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst regeneration/reactivation, etc., can solve the problems of high material consumption and energy consumption, environmental protection and economic limitations, complicated and complicated operation process, etc. To achieve the effect of improving product yield

Active Publication Date: 2012-01-11
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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  • Hydrothermal regenerating method of titanium silicon molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Mix measured amorphous silica gel with tetrapropylammonium hydroxide, add distilled water, stir at room temperature for 1.5 hours after mixing, then add butyl titanate and stir for 0.5 hours, then stir at 75°C for 3 hours to obtain a regeneration solution , its composition is silicon (mol): titanium (mol): organic base (mol): water (mol) = 0.05: 0.001: 0.15: 20 (wherein silicon and titanium are SiO 2 and TiO 2 count). Take 12 grams of deactivated TS-1 molecular sieve B-1 and mix with 60 grams of regeneration solution, and then react in a sealed autoclave at 175° C. for 52 hours.

[0034] The resulting product was filtered, washed, dried at 180°C for 120 minutes, and then calcined at 650°C for 2 hours to obtain hydrothermally regenerated molecular sieve A.

Embodiment 2

[0036] Mix measured amounts of ethyl silicate, ethyl titanate and tetraethylammonium hydroxide, add distilled water, stir at room temperature for 1.0 hour after mixing, and then stir at 65°C for 3 hours to obtain a regeneration solution, which consists of silicon ( mole): titanium (mole): organic base (mole): water (mole) = 0.01: 0.0005: 0.2: 35 (where silicon and titanium are SiO 2 and TiO 2 count). Take 12 grams of deactivated TS-1 molecular sieve B-2 regenerated by roasting and mix with 65 grams of regeneration solution, and then react in a sealed autoclave at 160° C. for 72 hours.

[0037] The resulting product was filtered, washed, dried at 135°C for 120 minutes, and then calcined at 500°C for 6 hours to obtain hydrothermally regenerated molecular sieve B.

Embodiment 3

[0039] Mix measured ethyl silicate, ethyl titanate, tetraethylammonium hydroxide, and ethanolamine, add distilled water, stir at room temperature for 1.0 hour after mixing, and then stir at 75°C for 3 hours to obtain a regeneration solution, which consists of Silicon (mol): titanium (mol): tetraethylammonium hydroxide (mol): ethanolamine (mol): water (mol) = 0.1 (mol): 0.01 (mol): 0.08 (mol): 0.05: 20 (mol ). Take 10 grams of deactivated molecular sieve S-1 and mix them evenly with 55 grams of regeneration solution, and then react in a sealed autoclave at 140°C for 72 hours.

[0040] The resulting product was filtered, washed, dried at 100°C for 300 minutes, and then calcined at 580°C for 4 hours to obtain regenerated TS-1 molecular sieve C.

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Abstract

The invention relates to a hydrothermal regenerating method of a titanium silicon molecular sieve, which is characterized by comprising the following steps of: mixing regenerating liquid containing organic base, silicon and titanium with an inactivated titanium silicon molecular sieve; then treating for 2-144 hours under the self generated pressure in a sealed container; and filtering, washing, drying and roasting the obtained material to obtain a regenerated titanium silicon molecular sieve. The activity of the titanium silicon molecular sieve regenerated by the method is equal to the activity of a fresh agent, and the yield is high.

Description

technical field [0001] The invention relates to a hydrothermal regeneration method of a titanium-silicon molecular sieve. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, and Ti-MWW with larger pore structure have been synthesized. 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] In 1981, Italian Marco Taramasso et al first disclosed the preparation method of TS-1 molecular sieve (GB2071071A, USP4,410,501), the method is to prepare a silicon source, titanium source, organic base (RN + ) and / or basic oxides (Me n / 2 O) the reaction mi...

Claims

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Application Information

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IPC IPC(8): B01J29/90B01J29/89B01J38/64B01J38/02
Inventor 龙立华林民舒兴田朱斌史春风慕旭宏罗一斌邹飞艳夏长久汝迎春
Owner CHINA PETROLEUM & CHEM CORP