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Method and device used for preparing dichloropropanol through micro channel chlorination reaction

A microchannel reactor, dichloropropanol technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, introduction of halogen preparation, etc., can solve the problem of long reaction time, high reaction temperature, low yield, etc. problems, to achieve the effect of reducing difficulty, reducing operating costs, and improving reaction efficiency

Pending Publication Date: 2018-11-02
山东民基新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process is relatively mature, but there are still many problems in reaction time, reaction temperature, catalyst dosage and yield, such as long reaction time, high reaction temperature, large catalyst dosage, low yield, etc.

Method used

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  • Method and device used for preparing dichloropropanol through micro channel chlorination reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 500kg of glycerin with a purity of 95wt.% to the mixer by the glycerin delivery pump, and at the same time release 3.02kg of adipic acid from the catalyst silo, and add it to the mixer, stir and mix for 10 minutes at room temperature to form a mixed solution;

[0032] After mixing the mixture with 433.5kg hydrogen chloride gas in the pipeline before the pre-reaction tank, it enters the inner wall with solid acid catalyst SO4 2- / ZrO 2 -Pr 2 O 3 The pre-reaction is carried out in the pre-reaction tank; the pre-reaction tank is controlled under normal pressure, the temperature is 65℃, and the reaction residence time is 15s; the solid acid catalyst SO4 on the inner wall of the pre-reaction tank 2- / ZrO 2 -Pr 2 O 3 The thickness of the coating is 6.5 mm.

[0033] Then enter the inner wall of the microchannel with solid acid catalyst SO4 2- / ZrO 2 -Pr 2 O 3 In the microchannel reactor, the dichloropropanol reaction solution is obtained by the chlorination reaction; the microcha...

Embodiment 2

[0037] 500kg of glycerol with a purity of 95wt.% is added to the mixer by the glycerin delivery pump, and 3.56kg of adipic acid is discharged from the catalyst silo, and then added to the mixer, stirred and mixed for 10 minutes at room temperature to form a mixed liquid;

[0038] After mixing the mixture with 380.6kg hydrogen chloride gas in the pipeline before the pre-reaction tank, it enters the inner wall with solid acid catalyst SO4 2- / ZrO 2 -Pr 2 O 3 The pre-reaction is carried out in the pre-reaction tank; the pre-reaction tank is controlled under normal pressure, the temperature is 75℃, and the reaction residence time is 60s; the solid acid catalyst SO4 on the inner wall of the pre-reaction tank 2- / ZrO 2 -Pr 2 O 3 The thickness of the coating is 5mm.

[0039] Then enter the inner wall of the microchannel with solid acid catalyst SO4 2- / ZrO 2 -Pr 2 O 3 In the microchannel reactor, the dichloropropanol reaction liquid is obtained by the chlorination reaction; the microchannel...

Embodiment 3

[0043] 500kg of glycerin with a purity of 95wt.% is added to the mixer by the glycerin delivery pump, and 2.46kg of adipic acid is discharged from the catalyst silo, and then added to the mixer, stirred and mixed for 12 minutes at room temperature to form a mixed solution;

[0044] After mixing the mixed liquid with 561.7kg of hydrogen chloride gas in the pipeline before the pre-reaction tank, it enters the inner wall with a solid acid catalyst SO4 2- / ZrO 2 -Pr 2 O 3 The pre-reaction is carried out in the pre-reaction tank; the pre-reaction tank is controlled under normal pressure, the temperature is 70℃, and the reaction residence time is 100s; the solid acid catalyst SO4 on the inner wall of the pre-reaction tank 2- / ZrO 2 -Pr 2 O 3 The thickness of the coating is 6mm.

[0045] Then enter the inner wall of the microchannel with a solid acid catalyst SO4 2- / ZrO 2 -Pr 2 O 3 In the microchannel reactor, the dichloropropanol reaction solution is obtained by the chlorination reaction;...

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Abstract

The invention belongs to the field of dichloropropanol, and more specifically relates to a method and a device used for preparing dichloropropanol through micro channel chlorination reaction. The method comprises following steps: glycerin, and adipic acid are uniformly mixed so as to obtain a mixed solution, the mixed solution is mixed with hydrogen chloride in a pipeline before entering into a pre-reaction tank, and an obtained mixed material is introduced into the pre-reaction tank for pre-reaction, wherein the internal wall of the pre-reaction tank is attached with a solid acid catalyst; anobtained product is introduced into a micro channel reactor for chlorination reaction, wherein the internal wall of the micro channel reactor is provided with the solid acid catalyst; an obtained reaction product is introduced into a normal pressure tower for normal pressure distillation, the fractions collected from the top of the normal pressure tower are low-boiling-point substances, and are subjected to layering and water washing so as to obtain dichloropropanol; and the fractions collected from the bottom of the normal pressure tower are introduced into a pressure reduction tower for distillation so as to obtain dichloropropanol. According to the method, solid super strong acid SO4<2-> / ZrO2-Pr2O3 is attached onto the internal wall of the pre-reaction tank and the micro channel internal wall of the micro channel reactor, so that reaction efficiency is increased, the subsequent processing difficulty is reduced, and operation cost is reduced.

Description

Technical field [0001] The invention relates to dichloropropanol, in particular to a method and a device for preparing dichloropropanol by microchannel chlorination reaction. Background technique [0002] Dichloropropanol is an important chemical intermediate. As an important raw material for the preparation of epichlorohydrin, the demand continues to increase; common methods for preparing dichloropropanol include propylene chlorination, glycerol chlorination and allyl alcohol As the price of crude oil in the international market continues to rise and the pressure on environmental protection is increasing, the glycerol chlorination method has become the main process for producing dichloropropanol. [0003] Chinese patent CN105566253A discloses a process for synthesizing epichlorohydrin by glycerol method, which includes two units of glycerol chlorination reaction and dichloropropanol saponification reaction. The steps of the glycerol chlorination reaction unit are as follows: adip...

Claims

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Application Information

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IPC IPC(8): C07C29/62C07C31/36B01J8/00B01J8/02B01J19/00
CPCB01J8/008B01J8/02B01J19/0093C07C29/62B01J2219/00835B01J2208/00814C07C31/36
Inventor 韦兵张海朋李建军王建芹杨中原祝新涛张瑞扈世琳李萍林苗苗
Owner 山东民基新材料科技有限公司
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