High-content 2-methyl allyl chloride preparation method

A methallyl chloride, high-content technology, applied in separation methods, halogenated hydrocarbon preparation, chemical instruments and methods, etc., can solve the problems of high energy consumption, large investment, complex separation process, etc., to simplify the separation process , reducing energy consumption and equipment investment, the effect of reducing the number of theoretical boards

Active Publication Date: 2018-06-15
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the separation process of this method is complicated

Method used

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  • High-content 2-methyl allyl chloride preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] in such as figure 1 The middle part of the first rectification tower (theoretical plate total number is 20) of the shown three-tower continuous rectification device continuously adds chlorination reaction liquid (mass content is: 2-methallyl chloride is 89.6%, chlorine 2.3% tert-butane, 1.3% isobutenyl chloride, 5.6% 1,2-dichloro-tert-butane, 1.2% 3,3'-dichloroisobutene), adjust the reflux ratio to 50, and use the total feed from the top of the tower The ratio of amount 2.3% obtains the chloro-tert-butane that content is more than 99%; A mixture of 1,2-dichloro-tert-butane and 3,3'-dichloroisobutene (82:18 in mass ratio), 1,2-dichloro-tert-butane and 3,3'-dichloroisobutene is added to the middle and upper part The mixture and the mass ratio of the feed are controlled at 2:1, and the reflux ratio at the top of the tower is controlled at 230, and the content is obtained from the top of the tower with the ratio of 1.3% of the first tower feed amount and is the isobutenyl ...

Embodiment 2

[0027] in such as figure 1 The middle part of the first rectifying tower (theoretical plate total number is 20) of the shown three-tower continuous rectifying device continuously adds the chlorination reaction solution (mass content is: 2-methallyl chloride is 88.7%, chlorine 2.1% tert-butane, 1.5% isobutenyl chloride, 6.0% 1,2-dichloro-tert-butane, 1.5% 3,3'-dichloroisobutene), adjust the reflux ratio to 56, and use the total feed from the top of the tower The ratio of amount 2.1% obtains the tert-butyl chloride that content is more than 99%; A mixture of 1,2-dichloro-tert-butane and 3,3'-dichloroisobutene (80:20 in mass ratio), 1,2-dichloro-tert-butane and 3,3'-dichloroisobutene is added to the middle and upper part The mixture and the mass ratio of feed are controlled at 3:1, and the reflux ratio at the top of the tower is controlled at 180, and the content is obtained from the top of the tower with the ratio of 1.5% of the first tower feed amount and is the isobutenyl chl...

Embodiment 3

[0029] in such as figure 1The middle part of the first rectification tower (theoretical plate total number is 20) of the shown three-tower continuous rectification device continuously adds chlorination reaction liquid (mass content is: 2-methallyl chloride is 85.2%, chlorine isobutane 3.2%, isobutenyl chloride 3.6%, 1,2-dichloro-tert-butane 6.1%, 3,3'-dichloroisobutene 1.9%), adjust the reflux ratio to 37, and use the total feed from the top of the tower The ratio of amount 3.2% obtains the tert-butyl chloride that content is more than 99%; A mixture of 1,2-dichloro-tert-butane and 3,3'-dichloroisobutene (80:20 in mass ratio), 1,2-dichloro-tert-butane and 3,3'-dichloroisobutene is added to the middle and upper part The mixture and the mass ratio of feed are controlled at 1:1, and the reflux ratio at the top of the tower is controlled at 110, and the content is obtained from the top of the tower with the ratio of 3.6% of the first tower feed amount as isobutenyl chloride that ...

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Abstract

The invention relates to a high-content 2-methyl allyl chloride preparation method. A chlorination reaction solution obtained through the reaction of isobutene and chlorine is taken as the raw material, the high-content 2-methyl allyl chloride is obtained through continuous rectifying of an isobutyl chloride separation tower, an isobutylene chloride separation tower and a 2-methyl allyl chloride separation tower, wherein the separation of isobutylene chloride uses a extractive distillation method. The preparation method has the advantages that the number of needed rectifying towers is small, the content of the obtained 2-methyl allyl chloride is high, and the energy consumption is low.

Description

technical field [0001] The invention relates to the separation process of organic matter, belongs to the field of fine organic chemical industry, and in particular relates to a preparation method of high-content 2-methallyl chloride. Background technique [0002] 2-Methallyl chloride is an important organic synthesis intermediate, which is widely used in the fields of medicine, pesticide, fragrance monomer, polymer material and so on. [0003] 2-Methallyl chloride is usually obtained by gas-phase chlorination of isobutylene with chlorine. For example, DE3402446, CN1030407, CN1288119, CN101182279, and CN202044960 all adopt isobutylene gas-phase chlorination to prepare 2-methallyl chloride. [0004] Various side reactions will occur during the chlorination reaction. In addition to the main product 2-methallyl chloride, the reaction product usually contains a certain amount of chloro-tert-butane, isobutenyl chloride, 1,2-di Chlorobutane, 3,3'-dichloroisobutene and other by-pr...

Claims

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Application Information

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IPC IPC(8): C07C17/38C07C17/386C07C17/383C07C21/067B01D3/00B01D3/14
CPCB01D3/002B01D3/143B01D3/146C07C17/38C07C17/383C07C17/386C07C21/067C07C17/10
Inventor 尹红陈志荣王伟松马夏坤马振祥王月芬万庆梅钱建芳董楠
Owner ZHEJIANG UNIV
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