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Preparation method of catalyst for synthesizing pyrrolidine from tetrahydrofuran by catalytic amination

A tetrahydropyrrole catalyst and tetrahydrofuran catalyzed amine technology are applied in the field of preparation of tetrahydropyrrole catalysts synthesized from tetrahydrofuran, which can solve the problems of high requirements, difficulties, and huge investment in reaction equipment and environment, and achieve high tetrahydropyrrole selectivity , low reaction catalytic temperature, simple preparation process

Inactive Publication Date: 2017-05-24
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The method for preparing tetrahydropyrrole in the literature has butanediol and ammonia as the gas-phase catalytic synthesis method [J.org.Chem, 1994,59 (14), 3998] of raw material, but this technique needs the reaction condition of high temperature and high pressure, to reaction There are high requirements for equipment and environment, and the initial investment in equipment is huge. There are certain difficulties in actual mass production, and potential safety problems are also prominent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Prepare a ferric nitrate solution with a concentration of 2.5mol / L, take 5g of alumina pellets and impregnate them in an equal volume, the loaded iron content is about 8% of the mass of the carrier, vibrate with ultrasonic wave for 30 minutes, let it stand for 12 hours, and then in Dry at 110°C for 10 hours.

[0017] (2) The catalyst obtained in step (1) was immersed in a 0.5 mol / L dilute sulfuric acid solution for 45 minutes, filtered, dried, and then put into a muffle furnace and calcined at 550°C for 5 hours to obtain the catalyst.

[0018] The prepared catalyst was subjected to tetrahydrofuran and ammonia as raw materials to prepare tetrahydropyrrole in a fixed bed reaction, and the obtained tetrahydropyrrole crude product was analyzed by gas chromatography to form a conversion rate of tetrahydrofuran of 72.1%, and the selectivity of tetrahydropyrrole was 87.7%. %.

Embodiment 2

[0020] (1) Prepare a ferrous sulfate solution with a concentration of 1.8mol / L, take 5g of alumina pellets and impregnate them in an equal volume, the loaded iron content is about 6% of the mass of the carrier, oscillate with ultrasonic waves for 45 minutes, let stand for 8 hours, and then Dry at 110°C for 12 hours.

[0021] (2) The catalyst obtained in step (1) was immersed in a 0.6 mol / L dilute sulfuric acid solution for 50 minutes, filtered, dried, and then baked in a muffle furnace at 550°C for 5 hours to obtain the catalyst.

[0022] The prepared catalyst was subjected to tetrahydrofuran and ammonia as a fixed bed reaction for preparing tetrahydropyrrole as a raw material, and the crude product of tetrahydropyrrole was analyzed by gas chromatography to obtain a conversion rate of 73.7% and a selectivity of tetrahydropyrrole of 86.5%. %.

Embodiment 3

[0024] (1) Prepare a ferrous chloride solution with a concentration of 1.7mol / L. After impregnating 6g of nano-alumina in equal volume, the loaded iron content is about 5% of the mass of the carrier, then oscillate with ultrasonic waves for 50 minutes, and let it stand for 12 hours , and then dried at 110°C for 12 hours.

[0025] (2) The catalyst obtained in step (1) was immersed in a 0.4 mol / L dilute sulfuric acid solution for 1 hour, filtered, dried, and then baked in a muffle furnace at 600°C for 4 hours to obtain the catalyst.

[0026] After the prepared catalyst was pressed into tablets, tetrahydrofuran and ammonia were used as a fixed-bed reaction to prepare tetrahydropyrrole as a raw material. The crude product of tetrahydropyrrole was analyzed by gas chromatography and the conversion rate of tetrahydrofuran was 74.3%. The selection of tetrahydropyrrole The rate is 84.8%.

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Abstract

The invention discloses a preparation method of a catalyst for synthesizing pyrrolidine from tetrahydrofuran by catalytic amination, belonging to the technical field of tetrahydrofuran synthesis. The preparation method comprises the following steps: (1) preparing a solution of iron nitrate or other iron salts (such as ferrous sulfate, ferrous chloride or the like) with a certain concentration, taking a certain amount of carrier, carrying out isometric impregnation, and drying at 110 DEG C; and (2) impregnating the dried catalyst in sulfuric acid, and roasting at 450-600 DEG C to obtain the catalyst. By researching the reaction mechanism for synthesizing pyrrolidine from tetrahydrofuran, the invention provides a preparation method of a pyrrolidine catalyst applicable to solid bed reactors. The catalyst is simple to prepare and low in cost. The catalyst has high mechanical strength, and does not corrode the equipment. The catalyst has the advantages of lower catalytic temperature and higher pyrrolidine selectivity; and the product can be easily separated.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for synthesizing tetrahydropyrrole from tetrahydrofuran, belonging to the technical field of tetrahydrofuran synthesis. Background technique [0002] Tetrahydropyrrole is a colorless to slightly yellow liquid with the properties of general amines, and has a wide range of uses in the fields of medicine, pesticides, daily chemicals, coatings, desulfurizers, additives, and zeolite template substances. [0003] The method for preparing tetrahydropyrrole in the literature has butanediol and ammonia as the gas-phase catalytic synthesis method [J.org.Chem, 1994,59 (14), 3998] of raw material, but this technique needs the reaction condition of high temperature and high pressure, to reaction There are high requirements for equipment and environment, and the initial investment in equipment is huge. There are certain difficulties in actual mass production, and potential safety problems are also promine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J29/46B01J37/02B01J37/34C07D295/023C07D295/027
CPCB01J23/745B01J29/46B01J37/0205B01J37/343C07D295/023C07D295/027
Inventor 何明阳查杰钱俊峰孙富安陈圣春陈群
Owner CHANGZHOU UNIV