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Method for recycling 2-chloro-4-(4-chlorophenoxy) acetophenone residue

A technology of chlorophenoxy and acetophenone, applied in the field of recovery and utilization of 2-chloro-4-acetophenone residues

Pending Publication Date: 2022-01-21
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the invention provides a kind of recycling method of 2-chloro-4-(4-chlorophenoxy) acetophenone residue, to solve 2-chloro-4-(4-chlorophenoxy) phenylethyl ketone The problem of ketone residue recycling, the present invention will 2-chloro-4-(4-chlorophenoxy) acetophenone residue in the presence of a strong base, under a certain pressure, 2-chloro-4-(4- Chlorophenoxy) acetophenone and isomers are converted into raw material 3,4'-dichlorodiphenyl ether, which can be used in the synthesis of 2-chloro-4-(4-chlorophenoxy) acetophenone to achieve Reuse of solid waste is economical and environmentally friendly; the conversion of 2-chloro-4-(4-chlorophenoxy)acetophenone and isomers is as follows:

Method used

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  • Method for recycling 2-chloro-4-(4-chlorophenoxy) acetophenone residue

Examples

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Effect test

Embodiment 1

[0023] A kind of recycling method of 2-chloro-4-(4-chlorophenoxy) acetophenone residue

[0024] The recycling method of 2-chloro-4-(4-chlorophenoxy) acetophenone residue, comprises the following steps:

[0025] (1) put residue 530g, water 300g, 30wt% liquid caustic soda 250g in 2000ml autoclave, replace 3 times with nitrogen, feed nitrogen to fill pressure to 0.5MPa, then heat up to 80 ℃, pressure rise to 0.55MPa, here Under the pressure and temperature, at the time of holding the temperature for 8 hours, sampling and analysis, the content of 2-chloro-4-(4-chlorophenoxy) acetophenone and isomers is less than 3%;

[0026] (2) cooling the system temperature to 30° C., layering to obtain an organic layer and an aqueous layer;

[0027] (3) the aqueous layer is extracted with 100 g of toluene, and then the toluene layer is separated; after the toluene layer is combined with the organic layer of step (2), washed once with 50 g of water, after phase separation, toluene is recovered ...

Embodiment 2

[0031] A kind of recycling method of 2-chloro-4-(4-chlorophenoxy) acetophenone residue

[0032] The recycling method of 2-chloro-4-(4-chlorophenoxy) acetophenone residue, comprises the following steps:

[0033] (1) put residue 530g, water 300g, 30wt% liquid caustic soda 300g in a 2000ml autoclave, replace it with nitrogen 3 times, feed nitrogen to fill the pressure to 0.5MPa, then heat up to 100°C, the pressure rises to 0.6MPa, here Under pressure and temperature, keep the temperature for 6 hours, take a sample for analysis, the content of 2-chloro-4-(4-chlorophenoxy) acetophenone and isomers is less than 1%;

[0034] (2) cooling the system temperature to 30° C., layering to obtain an organic layer and an aqueous layer;

[0035] (3) the aqueous layer is extracted with 100 g of toluene, and then the toluene layer is separated; after the toluene layer is combined with the organic layer of step (2), washed with 50 g of water, after phase separation, toluene is recovered under re...

Embodiment 3

[0039] A kind of recycling method of 2-chloro-4-(4-chlorophenoxy) acetophenone residue

[0040] The recycling method of 2-chloro-4-(4-chlorophenoxy) acetophenone residue, comprises the following steps:

[0041] (1) put residue 580g, water 350g, 35wt% liquid caustic soda 300g in a 2000ml autoclave, replace with nitrogen 3 times, feed nitrogen to fill the pressure to 0.6MPa, then heat up to 90 ° C, the pressure rises to 0.5MPa, here Under pressure and temperature, keep warm for 7 hours, take samples for analysis;

[0042] (2) cooling the system temperature to 30° C., layering to obtain an organic layer and an aqueous layer;

[0043] (3) the water layer is extracted with 100g toluene, and then the toluene layer is separated; after the toluene layer is combined with the organic layer of step (2), washed with 65g of water, after the phase separation, the toluene is recovered under reduced pressure to no flow, and under high vacuum Evaporate to obtain 3,4'-dichlorodiphenyl ether. ...

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Abstract

The invention discloses a method for recycling 2-chloro-4-(4-chlorophenoxy) acetophenone residue, which comprises the following steps of mixing a certain amount of residue, water and caustic soda liquid, and carrying out heat preservation treatment under a certain pressure, and then layering, extracting a water phase, combining organic phases, washing with water, splitting phases, recycling under reduced pressure, and steaming out under high vacuum to obtain the 3, 4'-dichlorodiphenyl ether. According to the method, the 2-chloro-4-(4-chlorophenoxy) acetophenone and the isomer are converted into the raw material 3, 4'-dichlorodiphenyl ether which can be used for synthesizing the 2-chloro-4-(4-chlorophenoxy) acetophenone, solid waste recycling is achieved, and the method is economical and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of waste residue treatment technology, in particular to a method for recycling 2-chloro-4-(4-chlorophenoxy) acetophenone residues. Background technique [0002] Difenoconazole, also known as oxadiazole, is an ultra-efficient, broad-spectrum, systemic triazole fungicide, which can strongly inhibit the spore formation of plant pathogens, and in the process of disease control, It shows the three major effects of prevention, treatment and eradication, and is widely used in various crops such as grain, cotton, fruits and vegetables. 2-Chloro-4-(4-chlorophenoxy)acetophenone is the key intermediate for the effective synthesis of the agricultural insecticide oxidazole, and the core of the synthesis of oxidazole. [0003] At present, there are many synthetic methods for 2-chloro-4-(4-chlorophenoxy) acetophenone, mainly using 3,4'-dichlorodiphenyl ether and acylating reagent acetic anhydride or acetyl chloride for ac...

Claims

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Application Information

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IPC IPC(8): C07C41/18C07C41/34C07C41/38C07C41/42C07C43/29C07C45/00C07C49/84
CPCC07C41/18C07C41/34C07C41/38C07C41/42C07C45/00C07C43/29C07C49/84
Inventor 赵振东潘光飞王进祁康旭徐瑶曾挺
Owner 浙江禾本科技股份有限公司
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