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Method for synthesizing dichloroether ether and 2-chloroethoxyethanol

A technology of chloroethoxyethanol and synthesis method, which is applied in chemical instruments and methods, ether preparation, ether separation/purification, etc., and can solve the problems of poor controllability of synthesis of 2-chloroethoxyethanol, difficult control of sulfuric acid, and flammability Explosive and other problems, to achieve the effect of safe and controllable synthesis, simple and controllable reaction, and low cost

Inactive Publication Date: 2019-05-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The oxirane that adopts when preparing 2-chloroethoxyethanol is a kind of poisonous carcinogen, and is inflammable and explosive, and sulfuric acid is difficult to control during the process of reaction, all above causes 2-chloroethoxyethanol The synthetic controllability of the compound is poor, and it has a high potential safety hazard

Method used

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  • Method for synthesizing dichloroether ether and 2-chloroethoxyethanol
  • Method for synthesizing dichloroether ether and 2-chloroethoxyethanol
  • Method for synthesizing dichloroether ether and 2-chloroethoxyethanol

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[0034] The embodiment of the present invention provides a synthetic method of dichloroethyl ether and 2-chloroethoxyethanol, the method comprising: adding diethylene glycol and a catalyst in a two-necked flask with a molar ratio of 0.8-1.5:0.3, and making the two-necked flask The two bottlenecks of flask 1 are respectively connected with separatory funnel and condenser tube;

[0035] Use a separatory funnel to drop the mixed acid into the double-necked flask, and react at 130°C-170°C. During the reaction, use a condenser to collect the condensate;

[0036] The condensate is distilled to obtain dichloroethyl ether;

[0037] The remaining liquid in the two-necked flask is suction filtered to obtain 2-chloroethoxyethanol;

[0038] The mixed acid includes: concentrated hydrochloric acid and concentrated sulfuric acid with a mass ratio of 25-35:1.

[0039] The method provided by the embodiment of the present invention can simultaneously generate dichloroethyl ether and 2-chloroet...

Embodiment 1

[0062] In this embodiment, the attached figure 1 Described synthesis device carries out the synthesis of dichloroethyl ether and 2-chloroethoxyethanol, and the steps are as follows:

[0063] Take 106g of diethylene glycol and 40.8g of zinc chloride and add them respectively to the first two-necked flask 1, and take 480ml of mixed acid and add them to the separatory funnel 2, and drop them into the first two-necked flask 1 at a rate of 20 drops / min. During this process, the reaction was carried out at 160° C. for 7 h under stirring conditions. The distilled liquid is condensed and recovered by the first condensing pipe 3 to obtain a light yellow transparent condensate. Wherein, the mixed acid is concentrated hydrochloric acid and concentrated sulfuric acid with a mass ratio of 30:1.

[0064] Get 1ml reaction liquid from the first two-necked flask 1, detect the content of 2-chloroethoxyethanol with gas chromatography, the measurement result shows: the selectivity of 2-chloroet...

Embodiment 2

[0067] In this embodiment, the attached figure 1 Described synthesis device carries out the synthesis of dichloroethyl ether and 2-chloroethoxyethanol, and the steps are as follows:

[0068] Take 106g of diethylene glycol and 40.8g of zinc chloride and add them respectively to the first two-necked flask 1, get 480ml of mixed acid and add them to the separatory funnel 2, and drop them into the first two-necked flask 1 at a rate of 15 drops / min. During this process, the reaction was carried out at 160° C. for 10 h under stirring conditions. The distilled liquid is condensed and recovered by the first condensing pipe 3 to obtain a light yellow transparent condensate. Wherein, the mixed acid is concentrated hydrochloric acid and concentrated sulfuric acid with a mass ratio of 29:1.

[0069] Get 1ml of reaction liquid from the first two-necked flask 1, detect the content of 2-chloroethoxyethanol with gas chromatography, the measurement result shows: the selectivity of 2-chloroeth...

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Abstract

The invention discloses a method for synthesizing dichloroether and 2-chloroethoxyethanol, and belongs to the field of organic synthesis. The method comprises the steps: adding diethylene glycol and acatalyst at a molar ratio of (0.8-1.5):0.3 into a two-necked flask, and connecting the two bottle mouths of the two-necked flask to a separating funnel and a condenser pipe separately; adding mixed acids dropwise to the two-necked flask by using the separating funnel, performing a reaction at 130-170 DEG C, collecting a condensate by using the condenser pipe during the reaction, performing distillation on the condensate so as to obtain dichloroether, and performing suction filtration on the remaining liquid in the two-necked flask so as to obtain 2-chloroethoxyethanol, wherein the mixed acidsinclude concentrated hydrochloric acid and concentrated sulfuric acid at a mass ratio of (25-35):1. Through the synthesis method, not only can dichloroether and 2-chloroethoxyethanol be synthesized simultaneously, but also the method can have a simple and controllable reaction, mild reaction conditions and safe and easily available raw materials, so that synthesis of the two is safer and more controllable, and the cost is lower.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing dichloroethyl ether and 2-chloroethoxyethanol. Background technique [0002] Both dichloroethyl ether and 2-chloroethoxyethanol are important organic products. Among them, dichloroethyl ether can be used as a solvent for fats, oils, waxes, rubber, tar, asphalt, resins, ethyl cellulose, etc. Insecticide; also used in organic synthesis and paint preparation; also used in the intermediate of organic product synthesis, and is an important raw material for the manufacture of fine chemical products. 2-Chloroethoxyethanol is an intermediate of hydroxyzine hydrochloride (Aetara), quetiapine and cetirizine for mental illness. Therefore, it is necessary to provide a synthetic method of dichloroethyl ether and 2-chloroethoxyethanol. [0003] In the prior art, ethylene oxide and 2-chloroethanol are usually reacted in the presence of sulfuric acid to synthesize 2-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/22C07C41/34C07C41/42C07C43/12C07C43/13
Inventor 杨超越易铧常宏岗何金龙熊钢陈庆梅黄韵弘屈珊珊
Owner PETROCHINA CO LTD
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