Preparation method of trans-1, 3-dichloropropene

A dichloropropene and reaction technology, which is applied in the field of preparation of trans-1,3-dichloropropene, can solve the problems of high separation difficulty, high energy consumption, low economic value, no mention, etc., and achieves easy industrial implementation, The effect of less discharge of three wastes and mild reaction conditions

Active Publication Date: 2021-06-04
JIANGSU YANGNONG CHEM GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The boiling point difference of cis / trans-1,3-dichloropropene is less than 7°C, which is separated by multi-stage rectification in industry, which is difficult to separate and consumes a lot of energy
[0005] CN1466559A discloses a low-colored trans-1,3-dichloropropene and its preparation method, which will contain cis-1,3-dichloropropene Composition of chloropropene, trans-1,3-dichloropropene and C6 compounds, by chlorination step and rectification step, removal of lower boiling cis-1,3-dichloropropene, rectification removal of higher boiling point The C6 chlorinated compound can obtain trans-1,3-dichloropropene with chromaticity ≤ 200. This method only conducts rectification and separation of mixed 1,3-dichloropropene, and there is no cis-transposition to generate trans-related process. , the separated cis is still mixed with mixed 1,3-dichloropropene and used as soil fumigant and insecticide, the economic value is low, and the problem that cis-1,3-dichloropropene has no suitable outlet has not been solved
This method provides a way to prepare cis-1,3-dichloropropene, but does not mention how to prepare trans-1,3-dichloropropene

Method used

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  • Preparation method of trans-1, 3-dichloropropene
  • Preparation method of trans-1, 3-dichloropropene

Examples

Experimental program
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Effect test

Embodiment 1

[0048] This embodiment provides a preparation method of trans-1,3-dichloropropene, the preparation method comprising the following steps:

[0049] (1) mixed reaction raw material (80.1wt% cis-1,3-dichloropropene and 17.8wt% trans-1,3-dichloropropene) and nano titanium dioxide as catalyst, the mass ratio of reaction raw material and catalyzer is 1:0.03, heat up to 30°C, and react for 3 hours under the condition of 20W, 310nm LED ultraviolet light to prepare trans-1,3-dichloropropene;

[0050] (2) The product containing trans-1,3-dichloropropene obtained after the reaction is separated by rectification, the vacuum degree of rectification separation is -0.070~-0.072MPa, and the temperature at the top of the tower is 64~65°C, The temperature at the bottom of the tower is 72-75°C, the reflux ratio is 3.2-3.5:1, and cis-1,3-dichloropropene and trans-1,3-dichloropropene are produced sequentially from the top of the tower.

Embodiment 2

[0052] This embodiment provides a preparation method of trans-1,3-dichloropropene, the preparation method comprising the following steps:

[0053] (1) Mixed reaction raw materials (55.6wt% cis-1,3-dichloropropene and 43.4wt% trans-1,3-dichloropropene) and nano-alumina as catalyst, the mass ratio of reaction raw materials to catalyst The ratio is 1:0.05, the temperature is raised to 50°C, and the reaction is carried out under the condition of 50W, 310nm LED light for 2 hours to prepare trans-1,3-dichloropropene;

[0054] (2) The product containing trans-1,3-dichloropropene obtained after the reaction is separated by rectification, the vacuum degree of rectification separation is -0.065~-0.070MPa, and the temperature at the top of the tower is 65~67°C, The temperature at the bottom of the tower is 75-77°C, the reflux ratio is 3-3.3:1, and the cis-1,3-dichloropropene and trans-1,3-dichloropropene are produced sequentially from the top of the tower.

Embodiment 3

[0056] This embodiment provides a preparation method of trans-1,3-dichloropropene, the preparation method comprising the following steps:

[0057] (1) mixed reaction raw material (95.6wt% cis-1,3-dichloropropene and 2.7wt% trans-1,3-dichloropropene) and cadmium sulfide as catalyst, the mass ratio of reaction raw material and catalyzer is 1:0.1, the temperature was raised to 75°C, and the reaction was carried out under natural light conditions for 1 hour to prepare trans-1,3-dichloropropene;

[0058] (2) The product containing trans-1,3-dichloropropene obtained after the reaction is separated by rectification, the vacuum degree of rectification separation is -0.070~-0.075MPa, and the temperature at the top of the tower is 66~68°C, The temperature at the bottom of the tower is 70-73°C, the reflux ratio is 4.3-5:1, and cis-1,3-dichloropropene and trans-1,3-dichloropropene are produced sequentially from the top of the tower.

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Abstract

The invention provides a preparation method of trans-1, 3-dichloropropene, the preparation method adopts a specific catalyst to convert cis-1, 3-dichloropropene into trans-1, 3-dichloropropene, only needs the catalyst and illumination, does not need to add other solvents and assistants, and has the advantages of mild reaction conditions, simple process and easy industrial implementation. Few byproducts are produced in the reaction process, the subsequent separation is simple, and the application prospect is wide.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of trans-1,3-dichloropropene. Background technique [0002] 1,3-dichloropropene has two configurations: trans-1,3-dichloropropene and cis-1,3-dichloropropene. The two cis-trans isomers have similar properties and are both flammable and colorless liquids , a strong irritant, with a smell similar to chloroform, insoluble in water, soluble in most organic solvents such as ethanol, ether, and benzene. Among them, trans-1,3-dichloropropene is mainly used as an intermediate in the synthesis of cyclohexenone herbicides and in the synthesis of antifungal medicine Terbinafine hydrochloride. The mixed 1,3-dichloropropene and cis-1,3-dichloropropene can be directly used as soil fumigant and soil insecticide, and can also be used to produce new insecticide raw materials. [0003] 1,3-Dichloropropene is a by-product in the production process of chloropropene. For...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/073C07C17/358C07C17/383
CPCC07C17/358C07C17/383C07B2200/09C07C21/073Y02P20/584
Inventor 王怡明徐林丁克鸿刘相李卞辰超赵慧张巍伟
Owner JIANGSU YANGNONG CHEM GROUP
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