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Method for preparing dichlorohydrin and reaction device

A technology of dichloropropanol and a reaction device is applied in the field of a method for preparing dichloropropanol and a reaction device, and can solve the problems of serious environmental pollution, increased reaction process, difficult waste water treatment, etc., and achieves high reaction efficiency, improved reaction efficiency, The effect of improving industrial production efficiency

Active Publication Date: 2010-07-14
江苏德纳化学股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the organic nitrile compound catalyst needs to be processed with 30% HCl before use, the reaction process has been increased; secondly, the catalyzer after the HCl treatment contains highly toxic CN in the raffinate after the reaction. - , serious environmental pollution, difficult wastewater treatment
At the same time, these catalysts will still be converted into carboxylic acid catalysts when they encounter acid, so the above-mentioned defects of carboxylic acid catalysts still exist.

Method used

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  • Method for preparing dichlorohydrin and reaction device
  • Method for preparing dichlorohydrin and reaction device
  • Method for preparing dichlorohydrin and reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: see figure 1 , 2 , feed 93% glycerin in the head tank E1 into the reaction kettle E3, and at the same time feed the acetic acid catalyst accounting for 5% of the glycerin substance, heat to 65°C, and continuously feed HCl gas from the steel cylinder E2 to E3, and the speed of HCl feeding is It is advisable not to escape. After reacting for 1.5 hours, the material was introduced into the reaction kettle E4 to continue chlorination, the reaction temperature was controlled at 90° C., and HCl was continued to react for 1 hour.

[0029] The material after the primary reaction is introduced into the spray reaction tower E8 equipped with corrugated mesh packing, the temperature inside the tower is controlled at 110°C, HCl is continuously introduced from E7 to the bottom of the spray reaction tower E8, and the pressure at the outlet of the HCl gas is adjusted to 0.3~ 0.4MPa, the glycerin is completely reacted, and the reaction ends when no distillate flows out o...

Embodiment 2

[0032] Embodiment 2: basically with embodiment 1, just reduced a reactor E4, glycerin concentration 95%, catalyzer is the propionic acid that accounts for the amount of glycerin substance 5%, is heated to 70 ℃, continues reaction 2 hours. The top of the spraying reaction tower can obtain 99.3% dichloropropanol, the conversion rate of glycerol is 100% in the reaction process, and the yield of dichloropropanol is 96.2%.

Embodiment 3

[0033] Embodiment 3: see figure 1 , 2 93% of the glycerol in the head tank E1 is passed into the reactor E3, and simultaneously the acetic acid catalyst accounting for 5% of the glycerin substance amount and the p-toluenesulfonic acid catalyst of 3% of the glycerol substance amount are passed into, heated to 65° C., and automatically Steel cylinder E2 continuously feeds HCl gas into E3, and the amount of HCl that is fed in should not escape. After reacting for 1 hour, the materials were introduced into the reaction kettle E4 to continue chlorination, the reaction temperature was controlled at 90° C., and HCl was continued to react for 1 hour.

[0034] The material after the primary reaction is introduced into the spray reaction tower E8 equipped with corrugated mesh packing, the temperature inside the tower is controlled at 110°C, HCl is continuously introduced from E7 to the bottom of the spray reaction tower E8, and the pressure at the outlet of the HCl gas is adjusted to 0...

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Abstract

The invention relates to improvement on a method for preparing dichlorohydrin by chlorinating glycerin and a reaction device. The chlorinating reaction is the series reaction of a reaction kettle and a sprinkling reaction tower which is filled with filler. The sprinkling reaction tower is sequentially provided with a placing filter zone, a hollow built-in sprinkling device zone and a placing filter zone from top to bottom. After viscosity decrease by kettle type preaction, the sprinkling reaction is carried out, the reaction contact is sufficient, the reaction time is long, the reaction efficiency is greatly enhanced, the conversion rate of the glycerin achieves 100%, and the reaction time is short and only needs 6-8 hours. The dichlorohydrin yield can be enhanced to more than 96%, and the yield can be enhanced to more than 99.0% by adding kreatine and strong acid mixing catalyst. The invention has the advantages of simple process flow, convenient reaction operation and high reaction efficiency.

Description

technical field [0001] The present invention relates to the improvement of the preparation method and reaction device for the preparation of epichlorohydrin intermediate dichloropropanol by chlorination of glycerin, especially relates to a kind of dichloropropanol with high reaction efficiency and dichloropropanol yield and short reaction time Alcohol preparation method and reaction device. Background technique [0002] Epichlorohydrin, also known as epichlorohydrin, is an important organic chemical raw material and fine chemical with a wide range of uses. For example, it is an important raw material for the preparation of epoxy resin, synthetic elastomer, and paper sizing agent. Traditional synthesis methods include propylene high-temperature chlorination method and propylene acetate method, and later developed a glycerin method to prepare epichlorohydrin. The reaction process is as follows: [0003] [0004] The reaction process is divided into two steps, (1) formula; ...

Claims

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Application Information

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IPC IPC(8): C07C29/62C07C31/36B01J10/00
Inventor 秦旭东杨建伟张学君蒋大智段启伟
Owner 江苏德纳化学股份有限公司
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