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Catalyst for synthesizing N, N-diethyl propargylamine and preparation method thereof

A technology of diethylpropargylamine and catalyst is applied in the field of catalyst for synthesizing N,N-diethylpropargylamine and its preparation field, and can solve the problem of reducing the yield and purity of N,N-diethylpropargylamine , The copper salt catalyst is not easy to recover, the catalyst is rapidly deactivated, etc., to reduce the probability of side reactions, shorten the reaction time, and improve the selectivity.

Active Publication Date: 2020-04-28
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the production scale-up process, it was found that the copper salt catalyst had poor selectivity and low activity, and a large number of side reactions occurred in the production process, in which the by-product polyacetylene could rapidly deactivate the catalyst, resulting in N,N-diethylpropyne Amine yield and purity are reduced; in addition, copper salt catalysts are not easy to recycle and can only be treated in waste water pools, which will also cause heavy metal pollution to a certain extent

Method used

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  • Catalyst for synthesizing N, N-diethyl propargylamine and preparation method thereof

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preparation example Construction

[0017] The present invention also provides a method for preparing a catalyst for synthesizing N,N-diethylpropynylamine, comprising the following steps: after dissolving the mixture of copper salt, bismuth salt and cerium salt, a metal salt solution is obtained, and the The coarse-porous microsphere silica gel after calcining and expanding the pores is aged and adsorbed in the metal salt solution, and then calcined and activated to obtain the finished product.

[0018] As a preferred embodiment of the present invention, the mass of the coarse-porous microsphere silica gel is 1 to 8 times the mass of the mixture of copper salt, bismuth salt and cerium salt; the metal salt solution uses deionized water as a solvent, and the deionized The quality of water is 5 to 20 times that of the mixture of copper salt, bismuth salt and cerium salt; by optimizing the amount of coarse-pore microsphere silica gel and metal salt solution, the catalytic efficiency of the catalyst can be improved an...

Embodiment 1

[0024] Example 1 of the present invention provides a catalyst for synthesizing N,N-diethylpropynylamine, in which the molar ratio of copper salt, bismuth salt and cerium salt is 1:0.0253:0.0324.

[0025] The catalyst is prepared as follows:

[0026] (1) Add 250g of deionized water to a 500ml single-necked flask, add 20g of copper sulfate, 1g of bismuth chloride and 1g of cerium chloride to the single-necked flask in turn under stirring at room temperature, then raise the temperature to 60°C, heat and dissolve for 2 to 4 hours, to obtain a metal salt solution;

[0027] (2) After calcining 100 g of coarse-pore microsphere silica gel in a muffle furnace at 400 ° C for 4 hours, cool to room temperature, then add the calcined and expanded coarse-pore microsphere silica gel into the well-insulated metal salt solution, and age chemical adsorption for 30h;

[0028] (3) Dry the coarse-porous microsphere silica gel aged in step (2) to remove water, and then calcinate and activate it i...

Embodiment 2

[0031] Example 2 of the present invention provides a catalyst for synthesizing N,N-diethylpropynylamine, in which the molar ratio of copper salt, bismuth salt and cerium salt is 1:0.0223:0.0206.

[0032] The catalyst is prepared as follows:

[0033] (1) Add 300 g of deionized water to a 500 ml single-necked flask, add 30 g of copper chloride, 2 g of bismuth nitrate and 2 g of cerium nitrate to the single-necked flask successively under stirring at room temperature, then raise the temperature to 60° C., heat and dissolve for 2 to 4 hours, and obtain Metal salt solution;

[0034] (2) After calcination of 120 g of coarse-pore microsphere silica gel in a muffle furnace at 400 ° C for 6 hours, cool to room temperature, then add the calcined and expanded coarse-pore microsphere silica gel into the well-insulated metal salt solution, and age chemical adsorption for 24h;

[0035] (3) Dry the coarse-porous microsphere silica gel aged in step (2) to remove water, and then calcinate an...

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Abstract

The invention discloses a catalyst for synthesizing N, N-diethyl propargylamine, which takes coarse-pore microsphere silica gel as a carrier and is loaded with a mixture of copper salt, bismuth salt and cerium salt. According to the catalyst provided by the invention, the coarse-pore microsphere silica gel is used as the carrier, the specific surface area of the catalyst is increased and is dozensof times or even hundreds of times that of a conventional catalyst, the catalyst can be in full contact with reaction raw materials, the reaction rate is increased, the reaction time is shortened, the probability of side reactions is reduced, and meanwhile, the use amount of the catalyst is greatly reduced; and the catalyst takes a mixture of copper salt, bismuth salt and cerium salt as an activecomponent, and the copper salt, bismuth salt and cerium salt have a synergistic effect, so that the side reaction in the process of synthesizing N, N-diethylpropargylamine can be effectively inhibited, the reaction selectivity is improved, and the yield and purity of N, N-diethylpropargylamine are improved. The invention also provides a preparation method of the catalyst.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for synthesizing N,N-diethylpropynylamine and a preparation method thereof. Background technique [0002] N,N-Diethylpropargylamine is a nickel plating additive with excellent performance, which has excellent brightening and leveling effects, and is widely used in nickel plating and alloy electroplating industries. Its CAS number is 4079-68-9 and its molecular formula is C 7 h 13 N, the molecular weight is 111.20. [0003] At present, the industrialized production method of N,N-diethylpropynylamine mainly uses formaldehyde, diethylamine and acetylene (or formaldehyde, propynyl chloride and acetylene) as raw materials, copper salt as a catalyst, and reacts in an organic solvent or water system to form N,N-Diethylpropynylamine. The method has the advantages of easy acquisition of raw materials, low cost, short production cycle, large output, little poll...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/843C07C209/00C07C211/23
CPCB01J23/8437B01J23/002C07C209/00B01J2523/00C07C211/23B01J2523/17B01J2523/3712B01J2523/54
Inventor 冯庆诚付远波杨威黄开伟宋文华
Owner 湖北吉和昌化工科技有限公司
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