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Preparation method of integrated TS-1 catalyst for chloro propylene epoxidation

A monolithic, catalyst-based technology, applied in catalyst activation/preparation, physical/chemical process catalysts, molecular sieve catalysts, etc., can solve problems such as catalyst deactivation, reaction conversion rate decline, etc., to achieve simple preparation methods and devices, and catalyst loss Less, more stable effect

Inactive Publication Date: 2006-09-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst is easily deactivated, and the reaction needs to be carried out under the condition of excess hydrogen peroxide, and the reaction conversion rate also decreases

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The commercially available cordierite carrier, the specification is φ18×50mm, and the channel is composed of 90 regular triangles with a side length of 1mm, and its specific surface area is 10.54m 2 / g, after calcination at 550°C for 8 hours, cool down to room temperature naturally, and store in a desiccator for future use. According to ethyl orthosilicate: tetrapropyl ammonium hydroxide (40% aqueous solution): the ratio of the molar ratio of water is 1: 0.15: 30 will tetrapropyl ammonium hydroxide (TPAOH) and deionized water were added to a stirred flask and stirred for 30 minutes. According to tetrabutyl titanate: isopropanol molar ratio of 4:11, tetrabutyl titanate (TBOT) isopropanol solution was dropped into the flask drop by drop so that the molar ratio of TBOT / TEOS was 0.04. Stir at 80°C for 3 hours. Then, add an appropriate amount of deionized water to make H 2 The O / TEOS molar ratio was 100, and the synthetic solution was obtained after stirring. Add the car...

Embodiment 2

[0017] The commercially available cordierite carrier, the specification is φ18×50mm, the cross-section is composed of 90 regular triangles with a side length of 1mm, and its specific surface area is 10.54m 2 / g, after calcination at 550°C for 8 hours, cool down to room temperature naturally, and store in a desiccator for future use. 5 g of ethyl orthosilicate, 1.83 g of tetrapropylammonium hydroxide (40% in water) and 13 ml of deionized water were added to the stirred flask and stirred for 30 minutes. Dissolve 0.33 g of tetrabutyl titanate into 4.5 ml of isopropanol solution, and drop it into the flask drop by drop, and stir at 80° C. for 3 hours after all the drops are completed. Then, 29 mL of deionized water was added and stirred to obtain a synthetic solution. Add the carrier and synthesis liquid into a stainless steel crystallization kettle with polytetrafluoroethylene lining, and make the synthesis liquid immerse the carrier. After sealing the crystallization kettle, p...

Embodiment 3

[0019] Embodiment 3 (comparative example)

[0020] Put 14.0g TS-1 molecular sieve powder (commercially available), 3.5g white carbon black (industrial product), 0.71g kale powder (industrial product) and 17.8g alkaline silica sol (industrial product) into a mortar and grind After 30 minutes, 8 g of distilled water was added dropwise while grinding. The agglomerated mixture was extruded with an extruder to obtain a bar-shaped TS-1 catalyst with a diameter of 0.2 mm and a length of 2 mm. After the obtained catalyst was dried at 110°C for 24 hours, it was placed in a muffle furnace and calcined at 550°C for 12 hours to obtain a strip-shaped TS-1 catalyst product.

[0021] The strip-type TS-1 catalyst prepared above is used to catalyze the epoxidation reaction of chloropropene and hydrogen peroxide. The reaction device is a stainless steel fixed bed reactor, and constant temperature water is passed through the jacket of the reactor to control the reaction temperature. Fill 20mL ...

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PUM

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Abstract

An integral catalyst TS-1 used for epoxidizing chloropropene to obtain epoxy chloropropane is prepared through calcining the multi-channel cylindrical porous ceramic in fuffle furnace, natural cooling, adding it to the synthetic liquid prepared from tert-butyl titanate, ethyl silicate, deionized water, ammonium tetrapropyl hydroxide and isopropanol, crystallizing reaction in crystallizer, and activating.

Description

technical field [0001] The invention relates to a preparation method of a monolithic TS-1 catalyst for the epoxidation of propene chloride, which belongs to the preparation technology of a loaded TS-1 catalyst. Background technique [0002] Titanium silicate molecular sieve (TS-1) catalyzed epoxidation of allyl chloride and dilute hydrogen peroxide aqueous solution is a new environmentally friendly method for the preparation of epichlorohydrin. Patent CN03121153.4 (2003.03.28) describes this method: put chloropropene, hydrogen peroxide, solvent and titanium-silicon molecular sieve catalyst fine particles into the reactor for reaction, solvent and unreacted chloropropene directly return to the Reactor, after the slurry in the reactor is filtered, the obtained clear liquid is separated to obtain epichlorohydrin products. In this method, the separation of the reaction material and the fine particles of the titanium-silicon molecular sieve catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/00B01J29/89C01B39/08C07D301/12C07D303/08
Inventor 周颖王莅张香文范双双米镇涛
Owner TIANJIN UNIV
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