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Continuous production process of p-xylylene dichloride and device

A technology for the production of p-dichlorobenzyl, which is applied in the field of organic chemical synthesis, can solve the problems of low product yield, high production cost, and discontinuous production, and achieve simple device structure, low cost, and good physical and chemical properties. Effect

Active Publication Date: 2016-02-24
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a continuous production process for dichlorobenzyl, which solves the problems of discontinuous production, low product yield and high production cost in the existing process, and has the advantages of simple process flow, short production cycle and high product purity. The characteristics of; the present invention simultaneously provides the device of its use

Method used

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  • Continuous production process of p-xylylene dichloride and device
  • Continuous production process of p-xylylene dichloride and device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The device used in this example is figure 1 As shown, feed tank 1 is connected with three-stage chlorination still 3, secondary chlorination still 5, first-level chlorination still 7, separation tank 8 and rectifying tower 12 successively, and first-level chlorination still 7 and secondary chlorine Between the chlorination stills 5, between the secondary chlorination stills 5 and the third-level chlorination stills 3, all are connected in parallel; the feed tank 1 is connected with the third-level chlorination stills 3 through the feed valve 2, and the third-level chlorination stills 3 The bottom is connected to the secondary chlorination kettle 5 through the secondary reflux pump 4, the bottom of the secondary chlorination kettle 5 is connected to the primary chlorination kettle 7 through the primary reflux pump 6, and the bottom of the separation tank 8 is connected to the rectifying tank 8 through the feed pump 9. The towers 12 are connected, the top of the primary c...

Embodiment 2

[0034] The device used in this embodiment is as in Example 1, except that between the feed tank 1 and the three-stage chlorination kettle 3, between the three-stage chlorination kettle 3 and the secondary chlorination kettle 5, the secondary chlorination The potential difference between the kettle 5 and the primary chlorination kettle 7, and between the primary chlorination kettle 7 and the separation tank 8 is 2m.

[0035] The specific operation is as follows:

[0036] (1) p-Xylene and 1-dodecyl-3-methylimidazolium chloride salt are joined in the feed tank 1, wherein 1-dodecyl-3-methylimidazolium chloride salt is 5% of the p-xylene quality ‰, and then the feed valve 2 at the bottom of the feed tank 1 flows into the three-stage chlorination kettle 3, the second-stage chlorination kettle 5 and the first-stage chlorination kettle 7 in order. Port 13 to feed, then open the chlorine feed valve 10 on the top of the primary chlorination kettle 7, the material in the primary chlorin...

Embodiment 3

[0041] The device used in this embodiment is as in Example 1, except that between the feed tank 1 and the three-stage chlorination kettle 3, between the three-stage chlorination kettle 3 and the secondary chlorination kettle 5, the secondary chlorination The potential difference between the kettle 5 and the primary chlorination kettle 7, and between the primary chlorination kettle 7 and the separation tank 8 is 3m.

[0042] The specific operation is as follows:

[0043] (1) P-xylene and 1-butyl-2,3-methylimidazolium chloride are added to feed tank 1, wherein 1-butyl-2,3-methylimidazolium chloride is the quality of p-xylene 1‰, and then the feed valve 2 at the bottom of the feed tank 1 flows into the uniform material into the three-stage chlorination kettle 3, the secondary chlorination kettle 5 and the first-level chlorination kettle 7 respectively, and the reaction kettles at all levels Feed through the overflow port 13, then open the chlorine feed valve 10 on the top of the...

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Abstract

The invention relates to a continuous production process of p-xylylene dichloride and a device, and belongs to the technical field of organic chemical synthesis. The device provided by the invention comprises a feed tank, wherein the feed tank is successively connected with a third order chloride kettle, a second order chloride kettle, a first order chloride kettle, a knockout drum and a rectifying tower; the first order chloride kettle is connected with the second order chloride kettle in parallel, and the second order chloride kettle is connected with the third order chloride kettle in parallel; the continuous production process comprises the steps of mixing paraxylene and an ionic liquid catalyst, then introducing chlorine to the mixture under the irradiation of an LED (light-emitting diode) light source, obtaining p-xylylene dichloride reaction liquid after the third order chlorine reaction, cooling and separating the p-xylylene dichloride reaction liquid, performing vacuum distillation, then collecting cut fraction to obtain the p-xylylene dichloride. The continuous production process of the p-xylylene dichloride solves the problem in the existing process that the production is discontinuous, the product yield is low and the production cost is high, has the characteristics of simple technological process, short production cycle and high product purity, and the device is simple in structure and is liable to operate.

Description

technical field [0001] The invention relates to a continuous production process and device for p-dichlorobenzyl, belonging to the technical field of organic chemical synthesis. Background technique [0002] p-Dichlorobenzyl is an important chemical raw material, its appearance is white flaky crystal, as an intermediate of organic synthesis, it is mainly used in the manufacture of p-xylylenedimethanol, p-xylylene dimethyl ether, terephthalaldehyde and other dyes. Can be used as pharmaceutical intermediates. CN104230653A discloses chlorination with p-xylene at 80°C, when the p-dichlorobenzyl content in the sample reaches 35wt%, stop passing chlorine, then obtain p-dichlorobenzyl by performing flash distillation and rectification, the process is in When the conversion rate of benzyl dichloride reaches 35%, flash distillation and vacuum distillation are carried out, which has problems such as low product conversion rate and high cost. Contents of the invention [0003] The p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C22/04C07C17/14C07C17/383C07C17/38
CPCC07C17/14C07C17/38C07C17/383C07C22/04
Inventor 薛居强王荣海张清新张泰铭毕义霞谢圣斌
Owner SHANDONG KAISHENG NEW MATERIALS
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