Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of recovery catalyst from synthesis n,n-dicyanoethyl arylamine mother liquor and its method for catalytic synthesis of ethyl chloride

A technology of dicyanoethyl arylamine mother liquor and dicyanoethyl aryl amine, applied in chemical instruments and methods, physical/chemical process catalysts, chemical recovery, etc., to save resources, increase economic income, and improve raw material utilization Effect

Active Publication Date: 2019-11-01
湖南天童环保有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the patent CN1342645A is used to synthesize N,N-dicyanoethyl arylamine, it contains high concentration of AlCl 3 -ZnCl 2 Whether the mother liquor can be used to catalyze the synthesis of ethyl chloride after being treated to recover the catalyst has not been reported.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] N,N-dicyanoethyl-m-toluidine filtered mother liquor source: to 10M 3 Add 2800kg of acrylonitrile, 10kg of hydroquinone, anhydrous AlCl 3 400kg, ZnCl 2 200kg, keep warm at 60~65℃ for 1h. Then add m-toluidine 2000kg in 3 times, react at reflux temperature for 24h. After the reaction is completed, acrylonitrile is recovered by distillation. Then add 600kg of water into the kettle, keep it warm at 75-80°C for 1 hour, press it into a dilution barrel filled with 1200kg of 80°C water and 200kg of 10% hydrochloric acid solution, cool to 25°C under stirring for crystallization, finally press into the filter box, pump Filter, must filter mother liquor 2302kg.

[0026] The catalyst is recovered from the mother liquor of synthesizing N,N-dicyanoethyl-m-toluidine and its method for catalytically synthesizing ethyl chloride comprises the following steps:

[0027] (1) Place the above-mentioned 2302kg filtered mother liquor in a still, heat it to 75°C, continue to distill to 85°...

Embodiment 2

[0035] The source of the filtered mother liquor of N,N-dicyanoethyl-m-toluidine: the same process as in Example 1 to obtain 2318 kg of the filtered mother liquor.

[0036] The catalyst is recovered from the mother liquor of synthesizing N,N-dicyanoethyl-m-toluidine and its method for catalytically synthesizing ethyl chloride comprises the following steps:

[0037] (1) Put the above-mentioned 2318kg of filtered mother liquor in a distillation pot, heat it to 75°C, and then distill it to 85°C under nitrogen bubbling to stop, condense and recover the residual acrylonitrile; then, stop feeding the nitrogen, and continue heating the above-mentioned mother liquor Distill at 85-100°C for 3.5 hours, condense and recover residual m-toluidine;

[0038] (2) Cool the mother liquor after the above treatment to 10°C, filter and separate the residual N-cyanoethyl-m-toluidine and N,N-dicyanoethyl-m-toluidine to obtain filtrate A, and press the filtrate A into the still , heated to 60°C, adde...

Embodiment 3

[0044] N,N-dicyanoethylaniline filtered mother liquor source: to 10M 3 Add 3000kg of acrylonitrile, 10kg of hydroquinone, anhydrous AlCl to the reaction kettle 3 350kg, ZnCl 2 180kg, keep warm at 60~65℃ for 1h. Then add 1860kg of aniline in 3 times, and react at reflux temperature for 20h. After the reaction is completed, acrylonitrile is recovered by distillation. Then add 700kg of water into the kettle, keep it warm at 75-80°C for 1 hour, press into the dilution tank containing 1200kg of 75°C water, add 160kg of 10% hydrochloric acid solution, cool to 15°C under stirring for crystallization, and finally press into and filter box, suction filtration to obtain 2296kg of filtered mother liquor.

[0045] The method for recovering catalyst and its method for catalytically synthesizing ethyl chloride from the mother liquor of synthesizing N,N-dicyanoethylaniline comprises the following steps:

[0046] (1) Put the above-mentioned 2296kg of filtered mother liquor in a distill...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for recovering a catalyst from synthesized N,N-dicyan-ethyl arylamine mother liquor and synthesizing chloroethane by means of catalyzed synthesis of the catalyst. The method comprises the following steps: firstly, carrying out distillation recovery on acrylonitrile under the condition of nitrogen bubbling; stopping the replenishment of nitrogen, and then recovering arylamine by means of distillation; cooling, filtering and separating N-cyanoethyl arylamine and the N,N-dicyan-ethyl arylamine so as to obtain filtrate A; heating the filtrate A up to 40-80 DEG C, adding activated carbon, stirring, and filtering to obtain filtrate B; carrying out evaporation and concentration on the filtrate B under the condition of heating until the solution density is 1.16-1.32g / cm<3>, and then adding hydrogen chloride gas to obtain an AlCl3 / ZnCl2 / HCL concentrated solution; conveying the AlCl3 / ZnCl2 / HCL concentrated solution into a reaction kettle containing ethyl alcohol, supplementing AlCl3 and / or ZnCl2, adding the hydrogen chloride gas, and carrying out catalyzed synthesis at the temperature of 80-130 DEG C to obtain the chloroethane. The method realizes effective combination of an N,N-dicyan-ethyl arylamine catalyzed synthesis technology and a chloroethane catalyzed synthesis technology, and completes the continuous application of two catalytic reactions by one catalytic system, thus realizing green catalysis and saving the resources.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine chemicals, and in particular relates to a method for recovering a catalyst from a mother liquor for synthesizing N,N-dicyanoethyl arylamine and using it for catalytically synthesizing ethyl chloride. Background technique [0002] Ethyl chloride is an important chemical, mainly used as a raw material for tetraethyl lead, ethyl cellulose and ethyl carbazole dyes, and also used as aerosol, refrigerant, local anesthetic, insecticide, ethyl Base agent, olefin polymerization solvent, gasoline anti-vibration agent, etc. It is also used as a catalyst for polypropylene. [0003] CN1342645A discloses a kind of preparation method of N,N-dicyanoethyl arylamine, the synthetic N,N-dicyanoethyl aniline and N,N-dicyanoethyl m-toluidine intermediate can be used to produce disperse yellow 163 , Disperse Orange 44, Disperse Orange 45 and other disperse dyes. Due to the advantages of simple equipment, con...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/16C07C19/043B01J27/32
CPCB01J27/32C07C17/16C07C19/043Y02P20/584
Inventor 赵莹赵起余泽华刘伟袁遥黄慧坚马强
Owner 湖南天童环保有限公司