Check patentability & draft patents in minutes with Patsnap Eureka AI!

Preparation method of dichloroalkane

A technology of dichloroalkanes and diols, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc. The formation of products, the effect of reducing the generation of side reactions

Active Publication Date: 2021-02-09
山东嘉成医药科技有限公司
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing preparation method of chlorinated alkanes, affected by the reaction process, chlorinated ether by-products are easily produced, and a large amount of sewage is produced after the reaction, causing environmental pollution ; In addition, the existing preparation method, the reaction time is longer, greatly limits its application in industry

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

[0026] Embodiment 1 The preparation method of 1,6-dichlorohexane, the steps are as follows:

[0027] Into the 1000ml reaction bottle with oil-water separator and condensing tube, add 400 grams of water, 5 grams of ammonium chloride, and 500 grams of 1,6-hexanediol in turn, stir and heat up to 50 ° C; start HCL gas, when the reaction When the clear and transparent reaction solution in the bottle turns milky white, continue to pass HCL gas, raise the temperature of the reaction solution to 110°C, and start reflux and liquid separation; as the reflux reaction progresses, there is stratification in the oil-water separator, and the reflux reaction 3 Hours, the molar ratio of 1,6-hexanediol to HCL gas is 1:2.5; the lower aqueous phase is refluxed into the reaction flask, and the upper oil layer is separated and collected from 1,6-dichlorohexane. The purity detected by HPLC was 99.6%, and the yield was 96% based on 1,6-dichlorohexane.

Embodiment 2

[0028] Embodiment 2 The preparation method of 1,3-dichloropropane, the steps are as follows:

[0029] Into the 1000ml reaction bottle with oil-water separator and condenser tube, add 400 grams of water, 5 grams of ammonium chloride, and 322 grams of 1,3-propanediol in sequence, stir and heat up to 60 ° C; start HCL gas, when the reaction bottle When the clear and transparent reaction solution turns milky white, continue to pass HCL gas, raise the temperature of the reaction solution to 107°C, and start reflux and liquid separation; as the reflux reaction progresses, there is stratification in the oil-water separator, and the reflux reaction lasts for 3 hours. The molar ratio of 1,3-propanediol and HCL gas is 1:3; the lower aqueous phase is refluxed into the reaction flask, and the upper oil layer is separated and collected from 1,3-dichloropropane. The purity detected by HPLC was 99.7%, and the yield based on 1,3-dichloropropane was 97.2%.

Embodiment 3

[0030] Embodiment 3 The preparation method of 1,4-dichlorobutane, the steps are as follows:

[0031] Into the 1000ml reaction flask with oil-water separator and condensing tube, add 400 grams of water, 5 grams of ammonium chloride, and 322 grams of 1,4-butanediol in turn, stir and heat up to 56 ° C; start HCL gas, when the reaction When the clear and transparent reaction solution in the bottle turns milky white, continue to pass HCL gas, raise the temperature of the reaction solution to 105°C, and start reflux and liquid separation; as the reflux reaction progresses, there is stratification in the oil-water separator, and the reflux reaction 3 Hours, the molar ratio of 1,4-butanediol and HCL gas is 1:2.6; the lower aqueous phase is refluxed into the reaction flask, and the upper oil layer is separated and collected from 1,4-dichlorobutane. The purity detected by HPLC was 99.5%, and the yield based on 1,4-dichlorobutane was 97%.

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 preparation method of dichloroalkane, which comprises the following steps: mixing diol, a catalyst and a solvent, stirring and heating the components, introducing HCl gas into the mixture, and carrying out reflux reaction for 3-5 hours; and after the reaction is finished, treating the reaction solution to obtain dichloroalkane. According to the preparation method providedby the invention, the catalyst ammonium chloride is added, so that the reaction speed is obviously increased, and side reactions are reduced. In the invention, a large amount of solvent water is added in the reaction process, so that on one hand, the formation of monochloro ether by-products can be effectively inhibited, a water phase can be directly and repeatedly used, and basically no sewage is discharged; besides, by using the oil-water separator, the dichloroalkane product can be effectively separated, the product purity is high, and the yield is high.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to a method for preparing dichloroalkane. Background technique [0002] Dichloroalkanes are an important class of organic chemical intermediates, which play an important role in medicine, pesticides and other aspects. The use of hydrogen chloride gas to prepare dichloroalkanes not only solves the problem of hydrogen chloride utilization, but also obtains valuable chemical products. intermediate. [0003] In the existing preparation method of chlorinated alkanes, affected by the reaction process, chlorinated ether by-products are likely to be produced, and a large amount of sewage is produced after the reaction, causing environmental pollution; in addition, the existing preparation method has a long reaction time and greatly limit its industrial application. At present, in order to meet the needs of industrial production, it is necessary to explore more effective and p...

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 Applications(China)
IPC IPC(8): C07C17/16C07C19/01
CPCC07C17/16C07C19/01
Inventor 王平生赵士杰梁志红刘志强刘宏林
Owner 山东嘉成医药科技有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com