Synthesis method for 2,2'-dichloroethyl ether

A technology of dichloroethyl ether and diethylene glycol, applied in chemical instruments and methods, preparation of organic compounds, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of strict process conditions and large waste discharge , high cost of raw materials and other issues, to achieve the effect of high catalytic selectivity, low environmental pollution and low cost

Pending Publication Date: 2019-03-26
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the technical problems existing in the existing 2,2'-dichloroethyl ether synthesis methods, such as strict requirements on process conditions, high cost of raw materials, large discharge of wastes such as sulfur dioxide, and low yield, the present invention provides a low-cost, simple and convenient synthesis method Synthetic method of 2,2'-dichloroethyl ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 212g of diethylene glycol and 6.36g of catalyst (of which: 2.12g of glacial acetic acid, 4.24g of zinc chloride) ), start stirring and heat up to 75±2°C, continue to feed hydrogen chloride gas for 4 hours, and the molar ratio of hydrogen chloride gas to diethylene glycol is 2.2:1;

[0030] (2) After the introduction of hydrogen chloride gas is completed, the system continues to heat up to 95~98°C for 3 hours;

[0031] (3) At the end of the heat preservation, the temperature is lowered to 50±2°C, and the excess hydrogen chloride gas is distilled off under the pressure condition of -0.003~-0.002MPa and the tail gas is absorbed;

[0032] (4) Maintain the vacuum degree of the system at about 1.2KPa (about 9mmHg), carry out rectification under reduced pressure, and collect the fraction at 68~70°C at the top of the rectification tower to obtain 261.63g of 2,2'-dichloroethyl ether product.

[0033] Characterized by gas chromatograph GC: the gas chromatographic purity ...

Embodiment 2

[0035] (1) Add 212g of diethylene glycol and 6.36g of catalyst (of which: 2.12g of n-butyric acid, 4.24 g) When stirring and heating to 75±2°C, continue to feed hydrogen chloride gas for 5 hours, and the molar ratio of hydrogen chloride gas to diethylene glycol is 2.4:1;

[0036] (2) After the introduction of hydrogen chloride gas is completed, the system continues to heat up to 95~98°C for 4 hours;

[0037](3) At the end of the heat preservation, the temperature is lowered to 50±2°C, and the excess hydrogen chloride gas is distilled off under the pressure condition of -0.003~-0.002MPa and the tail gas is absorbed;

[0038] (4) Maintain the vacuum degree of the system at about 1.4KPa (about 11mmHg), carry out rectification under reduced pressure, and collect the fraction at 68~70°C at the top of the rectification tower to obtain 261.95g of 2,2'-dichloroethyl ether product.

[0039] Characterized by gas chromatograph GC: the gas chromatographic purity of 2,2'-dichloroethyl eth...

Embodiment 3

[0041] (1) Add 212g of diethylene glycol and 8.48g of catalyst (including: 2.83g of glacial acetic acid, 5.65g of aluminum chloride, ), start stirring and heat up to 75±2°C, continue to feed hydrogen chloride gas for 5 hours, and the molar ratio of hydrogen chloride gas to diethylene glycol is 2.4:1;

[0042] (2) After the introduction of hydrogen chloride gas is completed, the system continues to heat up to 95~98°C for 5 hours;

[0043] (3) At the end of the heat preservation, the temperature is lowered to 50±2°C, and the excess hydrogen chloride gas is distilled off under the pressure condition of -0.003~-0.002MPa and the tail gas is absorbed;

[0044] (4) Maintain the vacuum degree of the system at about 1.4KPa (about 11mmHg), carry out rectification under reduced pressure, and collect the fraction at 68~70°C at the top of the rectification tower to obtain 258.63g of 2,2'-dichloroethyl ether product.

[0045] Characterized by gas chromatograph GC: the gas chromatographic p...

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Abstract

The invention discloses a synthesis method for 2,2'-dichloroethyl ether. The method specifically comprises the following steps: introducing hydrogen chloride gas into a reaction kettle containing diethylene glycol and catalyst within a certain period of time at 70-80 DEG C; continuing to increase temperature to 95-98 DEG C and reacting for 3-5 hours; cooling and distilling under negative pressure,thereby removing redundant hydrogen chloride gas; collecting cut fraction under the temperature of tower top at 68-70 DEG C in the manner of decompression rectification, namely, collecting 2,2'-dichloroethyl ether. According to the invention, hydrogen chloride gas is taken as a chlorinating agent and diethylene glycol takes part in disubstituted chlorination reaction under the action of a composite catalyst composed of organic carboxylic acid-lewis acid, so as to compound 2,2'-dichloroethyl ether; the catalytic performance is excellent, the breakage of ether bond can be effectively preventedand the yield of products is high; the method has the advantages of easily acquired raw materials, simple synthetic process, less environmental pollution, low production cost and easiness in realizingindustrial production.

Description

technical field [0001] The invention relates to the field of organic intermediate synthesis, in particular to a method for preparing an oxygen-containing fungicide synthesis intermediate dichloroethyl ether. Background technique [0002] In the process of industrial circulating cooling water treatment, the method of adding a certain amount of bactericide is usually used to control the formation of microorganisms and the reproduction of bacteria and algae. According to the bactericidal mechanism, fungicides can be divided into oxidizing and non-oxidizing. Oxidizing fungicides include halogen-containing compounds, peroxides, etc.; non-oxidizing fungicides are mostly organic compounds. In actual production and application, oxidizing fungicides are more convenient and effective than non-oxidizing fungicides, but they are prone to problems such as microbial resistance and the impact of their residues and decomposition products on the environment. For a long period of time, quat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/22C07C43/12B01J31/26
CPCB01J27/125B01J27/138B01J31/04B01J31/26B01J35/0006C07C41/22C07C43/123
Inventor 陈树招程终发赵坤王燕平陆久田王宁宁齐晓婧
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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