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Method for synthesizing tetrahydropyrrole by continuous catalytic amination of tetrahydrofuran

A technology for continuously catalyzing amines and tetrahydropyrroles with tetrahydrofuran, which is applied in the field of catalysis to achieve the effects of mild reaction conditions, high activity, and long life at high temperature

Inactive Publication Date: 2021-03-19
SINOPEC CHANGCHENG ENERGY CHEM NINGXIA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the continuous catalytic amination of tetrahydrofuran to prepare tetrahydropyrrole is still a blank

Method used

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  • Method for synthesizing tetrahydropyrrole by continuous catalytic amination of tetrahydrofuran
  • Method for synthesizing tetrahydropyrrole by continuous catalytic amination of tetrahydrofuran

Examples

Experimental program
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Embodiment 1

[0018] This example provides a method for preparing tetrahydropyrrole by continuous catalytic amination of tetrahydrofuran. A catalyst is placed in the middle section of the HZSM-5 (Si / Al=50) catalyst reactor, and the upper section and the lower section are filled with quartz sand respectively. Reaction raw material tetrahydrofuran (liquid hourly space velocity is 0.4 / h -1 ) enters the upper end of the reactor through a peristaltic pump for high-temperature gasification, fully mixes with ammonia gas (the molar ratio of ammonia gas and tetrahydrofuran is 7:1), and then enters the reactor for reaction. The reaction product is collected in a gas-liquid separator after being condensed, and the product is collected at intervals for gas chromatographic analysis.

Embodiment 2

[0020] This example provides a method for preparing tetrahydropyrrole by continuous catalytic amination of tetrahydrofuran. A catalyst is placed in the middle section of the HZSM-5 (Si / Al=80) catalyst reactor, and the upper section and the lower section are filled with quartz sand respectively. Reaction raw material tetrahydrofuran (liquid hourly space velocity is 0.4 / h -1 ) enters the upper end of the reactor through a peristaltic pump for high-temperature gasification, fully mixes with ammonia gas (the molar ratio of ammonia gas and tetrahydrofuran is 7:1), and then enters the reactor for reaction. The reaction product is collected in a gas-liquid separator after being condensed, and the product is collected at intervals for gas chromatographic analysis.

Embodiment 3

[0022] This example provides a method for preparing tetrahydropyrrole by continuous catalytic amination of tetrahydrofuran. A catalyst is placed in the middle section of the HZSM-5 (Si / Al=120) catalyst reactor, and the upper section and the lower section are filled with quartz sand respectively. Reaction raw material tetrahydrofuran (liquid hourly space velocity is 0.4 / h -1 ) enters the upper end of the reactor through a peristaltic pump for high-temperature gasification, fully mixes with ammonia gas (the molar ratio of ammonia gas and tetrahydrofuran is 7:1), and then enters the reactor for reaction. The reaction product is collected in a gas-liquid separator after being condensed, and the product is collected at intervals for gas chromatographic analysis.

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Abstract

A preparation method for preparing tetrahydropyrrole through continuous catalytic amination of tetrahydrofuran is carried out on a continuous fixed bed reactor, the reactor is composed of a stainlesssteel pipe with the size of [phi] 14*600 mm, and the reactor is placed in a tubular resistance furnace; placing a catalyst in the middle section of the reactor, and filling the upper section and the lower section with quartz sand; a reaction raw material tetrahydrofuran enters the upper end of a reactor through a peristaltic pump to be gasified at high temperature, is fully mixed with ammonia gasand then enters the reactor to react, a reaction product is condensed and then collected in a gas-liquid separator, and the product is collected at set intervals for gas chromatographic analysis. According to the method, tetrahydropyrrole is prepared through continuous catalytic amination of tetrahydrofuran, raw materials are easy to obtain, and reaction conditions are mild; in addition, the catalyst is higher in activity and long in high-temperature-resistant service life compared with aluminum oxide or a catalyst taking aluminum oxide as a carrier to load a metal component; therefore, the preparation method is simple and convenient for industrial production.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a method for preparing tetrahydropyrrole through continuous catalytic amination of tetrahydrofuran. Background technique [0002] Tetrahydropyrrole has a wide range of uses in medicine, pesticides, and fine chemicals. At present, the synthesis of tetrahydropyrrole by catalytic amination of tetrahydrofuran and ammonia has the advantages of easy availability of raw materials, mild reaction conditions, more research on catalysts, high atom utilization and less pollution. [0003] From the perspective of the reaction mechanism, the preparation of tetrahydropyrrole from tetrahydrofuran is an acid-catalyzed reaction. Most of the relevant research uses solid acid catalysts. Early scholars conducted a series of studies on alumina or metal components loaded on it as a carrier. Later, with the rise of zeolite catalysts, a large number of scholars applied various molecular si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/023C07D295/027B01J29/40
CPCC07D295/023C07D295/027B01J29/40
Inventor 唐元唐宇虹丁陶薛慧燕郎永福郭会军
Owner SINOPEC CHANGCHENG ENERGY CHEM NINGXIA CO LTD