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Synthesis method of 2-hydroxyl-3-chloropropyl-2'-chloroethyl ether, and application thereof

A technology of chloroethyl ether and chloropropyl, which is applied in the field of synthesis of 2-hydroxy-3-chloropropyl-2'-chloroethyl ether, can solve the problem of material elongation decrease and thermal air aging resistance change Poor problems, to achieve the effect of the best mechanical properties and fuel resistance

Active Publication Date: 2012-10-31
锦西化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

How to further improve the fuel resistance of polysulfide rubber is an important research topic. Experiments show that increasing the sulfur content of polysulfide rubber can improve oil resistance, but the elongation of the material decreases and the aging resistance to hot air becomes worse.

Method used

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  • Synthesis method of 2-hydroxyl-3-chloropropyl-2'-chloroethyl ether, and application thereof
  • Synthesis method of 2-hydroxyl-3-chloropropyl-2'-chloroethyl ether, and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Into a 1L three-neck flask with stirring, add 606g of 2-chloroethanol (industrial product, purity 99%) and 2g of tin tetrachloride pentahydrate (analytically pure, 99%) respectively, and heat up to 45°C. 173 g of epichlorohydrin (industrial product, purity: 99.9%) was slowly added dropwise over the course of 1 hour, and then reacted at 70° C. for 4 hours. Afterwards, rectification under reduced pressure was carried out, and fractions at 114°C to 117°C (1.33kPa) were collected to obtain 226g of 2-hydroxy-3-chloropropyl-2'-chloroethyl ether (chromatographic method, purity 98.1%).

Embodiment 2

[0025] In a 1L three-necked flask with stirring, 606 g of 2-chloroethanol (industrial product, purity 99%), boron trifluoride etherate complex (chemically pure, BF 3 46.8% to 47.8%) 0.74g, heated to 45°C, slowly added 173g of epichlorohydrin (industrial product, purity 99.9%) dropwise in 1 to 1.5 hours, and then maintained at 80°C for 5 hours. Afterwards, rectification under reduced pressure was carried out, and fractions at 114°C to 117°C (1.33kPa) were collected to obtain 251 g of 2-hydroxy-3-chloropropyl-2'-chloroethyl ether (chromatographic method, purity 98.3%).

Embodiment 3

[0027] In a 1L three-necked flask with stirring, 606 g of 2-chloroethanol (industrial product, purity 99%), boron trifluoride etherate complex (chemically pure, BF 3 46.8% to 47.8%) 1.5g, heated to 45°C, slowly added 173g of epichlorohydrin (industrial product, purity 99.9%) dropwise in 1 to 1.5 hours, and then maintained at 60°C for 4 hours. Afterwards, rectification under reduced pressure was carried out, and fractions at 114°C to 117°C (1.33kPa) were collected to obtain 259g of 2-hydroxy-3-chloropropyl-2'-chloroethyl ether (chromatographic method, purity 98.5%).

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Abstract

The invention provides a synthesis method of 2-hydroxyl-3-chloropropyl-2'-chloroethyl ether, and an application thereof. The method comprises the steps of: firstly, mixing 2-chlorohydrin and a catalyst, and heating up to be at 45 DEG C; maintaining the temperature of 45 DEG C, and slowly dripping epoxy chloropropane into the mixture within 1-1.5 hours; then, controlling the reaction temperature to be within the range of 45-80 DEG C and the reaction time to be within the range of 3-5 hours, wherein the molar ratio between the 2-chlorohydrin and the epoxy chloropropane is 1.5-5.0, and the mass fraction of the catalyst accounts 0.2-1.5% of that of the epoxy chloropropane; and finally, carrying out vacuum distillation on reaction liquid, and collecting fraction under 1.33kPa at 114-117 DEG C. The 2-hydroxyl-3-chloropropyl-2'-chloroethyl ether synthesized by using the method can be taken as a comonomer for preparing polysulfide rubber, and the prepared polysulfide rubber has relatively good mechanical property and fuel resistance.

Description

technical field [0001] The invention relates to the technical field of organic chemical production, in particular to a synthesis method and application of 2-hydroxy-3-chloropropyl-2'-chloroethyl ether. Background technique [0002] Polysulfide rubber is a kind of special synthetic rubber. Currently, liquid polysulfide rubber is widely used. In 1943, Thiokol Chemical Company of the United States was the first to produce it industrially. At present, only Germany, Japan, Russia, and China produce polysulfide rubber (American polysulfide rubber production enterprises have ceased production in 2001), all of which use dichloroethyl formal as the polysulfide rubber monomer. [0003] Polysulfide rubber is usually synthesized by the following process route. First, excess sodium disulfide and dichloroethyl formal monomer (according to the brand, add a certain amount of trichloropropane as a crosslinking agent) undergo polycondensation reaction to generate high molecular weight disulfi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/13C08G75/16
Inventor 王绍民赫平张全成宋琳珩
Owner 锦西化工研究院有限公司
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