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Preparation method of CoP-coated Co2P nanosheet catalyst for synthesizing amylamine from valeronitrile

A technology of nanosheets and catalysts, applied in the field of preparation of CoP@Co2P nanosheet catalysts for the synthesis of pentylamine from valeronitrile, which can solve the problems of high pressure, many by-products, and low product yields, so as to reduce the reaction temperature and improve hydrogenation Activity, the effect of good catalytic activity

Pending Publication Date: 2022-05-27
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of CoP@Co that pentylamine is synthesized from valeronitrile 2 The preparation method of P nanosheet catalyst, in order to solve above-mentioned adopting valeronitrile method to prepare pentylamine in the process that needs high pressure, product yield is lower and by-product is more problem

Method used

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  • Preparation method of CoP-coated Co2P nanosheet catalyst for synthesizing amylamine from valeronitrile
  • Preparation method of CoP-coated Co2P nanosheet catalyst for synthesizing amylamine from valeronitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The process of preparing catalysts

[0027] Weigh 5g of cobalt acetate, dissolve it in 150g of ethanol, and then add 0.01mol / L of ammonia 10g dropwise, stir and transfer to the hydrothermal synthesis kettle, 140 °C water heat 4.5h, filter drying to obtain Co 3 O 4 。 Take 1 g of the Co prepared above 3 O 4, with 5g LiCl and 3g sodium hypophosphite placed in a mortar grinding, and then transferred to the quartz boat, placed in a tube furnace, roasted at 250 ° C for 4.0h, and then washed and dried to obtain CoP@Co 2 P nanosheet catalyst, closed preservation.

[0028] Hydrogenation reaction process

[0029] Take the above prepared catalyst 0.1g in a round bottom flask, through the nitrogen for replacement, and then 1.0 g of pentylenitrile and 0.8 g of aminoborane solution into the round bottom flask, stirring, heating to 70 °C reaction, after the end of the reaction to remove the catalyst to obtain the target product penylamine.

[0030] The conversion rate of pentylene nitrile...

Embodiment 2

[0032] The process of preparing catalysts

[0033] Weigh 5g cobalt acetate, dissolve it in 225g ethanol, and then add a certain 0.05mol / L ammonia 5g dropwise, stir and transfer to the hydrothermal synthesis kettle, 160 °C water heat 2.5h, filter drying to obtain Co 3 O 4 。 Take 1 g of the Co prepared above 3 O 4 With 1gLiCl and 2g sodium hypophosphite placed in a mortar grinding, then transferred to a quartz boat, placed in a tubular furnace, roasted at 400 ° C for 2.0h, and then washed and dried to obtain CoP@Co 2 P nanosheet catalyst, closed preservation.

[0034] Hydrogenation reaction process

[0035] Take the above prepared catalyst 0.1g in a round bottom flask, through the nitrogen for displacement, and then 1.4 g of pentylenitrile and 1.5 g of aminoborane solution into the round bottom flask, stirring, heating to 90 °C reaction, after the end of the reaction to remove the catalyst to obtain the target product penylamine.

[0036]The conversion rate of pentylene nitrile was ...

Embodiment 3

[0038] The process of preparing catalysts

[0039] Weigh 5g cobalt acetate, dissolve it in 175g ethanol, and then add a certain 0.04mol / L ammonia water 6g dropwise, stir and transfer to the hydrothermal synthesis kettle, 150 °C water heat 3.5h, filter drying to obtain Co 3 O 4 。 Take 1 g of the Co prepared above 3 O 4 With 3gLiCl and 2.5g sodium hypophosphite placed in a mortar grinding, then transferred to a quartz boat, placed in a tubular furnace, roasted at 300 ° C for 3.0h, and then washed and dried to obtain CoP@Co 2 P nanosheet catalyst, closed preservation.

[0040] Hydrogenation reaction process

[0041] Take the above prepared catalyst 0.1g in a round bottom flask, through the nitrogen for replacement, and then 1.2 g of pentylenitrile and 1.3 g of aminoborane solution into the round bottom flask, stirring, heating to 80 °C reaction, after the end of the reaction to remove the catalyst to obtain the target product penylamine.

[0042] The conversion rate of pentylene nitr...

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Abstract

The invention discloses a preparation method of a CoP-Co2P nanosheet catalyst for synthesizing amylamine from valeronitrile, which comprises the following steps: dissolving a cobalt source in ethanol, dropwise adding ammonia water, stirring, transferring into a synthesis kettle, carrying out hydrothermal treatment, filtering and drying to obtain Co3O4; the preparation method comprises the following steps: grinding Co3O4, LiCl and a phosphorus source in a mortar, transferring into a quartz boat, roasting in a tubular furnace, washing with water, and drying to obtain the CoP-coated Co2P nanosheet catalyst. According to the preparation method of the CoP-Co2P nanosheet catalyst for synthesizing the pentylamine from the valeronitrile, the CoP-Co2P nanosheet is used as the catalyst, ammonia borane in-situ released hydrogen is used as a hydrogen source, the selectivity of the target product pentylamine can reach 97% or above, the byproducts of dipentylamine and tripentylamine are both 3% or below, the reaction temperature can be remarkably reduced, and the yield of the catalyst is increased. The high-selectivity synthesis of the pentylamine under a mild condition is realized.

Description

Technical field [0001] The present invention relates to the field of fine chemical technology, in particular to a CoP@Co for the synthesis of pentylene amines from a kind of pentylonitrile 2 Preparation method of P nanosheet catalyst. Background [0002] Pentylamine is an important chemical raw material and product, but also a high-value pharmaceutical synthesis intermediate, mainly used in the production of organic synthesis, medicine, emulsifiers, antioxidants, rubber vulcanizing agents. With the development of modern industry, the synthesis method of pentylamine is becoming more and more perfect, and the current industrial applications mainly include valeraldehyde method, caprolamide method, di-n-pentyl boron chloride method, and valeritrile method. Among them, the selectivity of the valeraldehyde method is about 48%, the selectivity of the caprolamide method is about 81%, the selectivity of the di-n-n-pentyl boron chloride method is about 93%, and the selectivity of the penty...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J35/02B01J37/10B01J37/08C07C211/07C07C209/48B01J35/00
CPCB01J27/1853B01J37/10B01J37/08C07C209/48B01J35/40C07C211/07Y02P20/584
Inventor 梁雨李贵曹云钟朱宁静万超吴胜华许立信何孝军
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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