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Method for preparing epoxy chloropropane by cyclizing dichloropropanol in microreactor

An epichlorohydrin and microreactor technology, applied in the chemical industry, organic chemistry, sustainable manufacturing/processing, etc., can solve the problems of reduced reaction yield, high local alkali concentration, intensified hydrolysis reaction, etc. High yield, high selectivity, and the effect of increasing effective concentration

Active Publication Date: 2012-07-25
JIANGSU ANPON ELECTROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to ensure that the reaction of 2,3-dichloropropanol is complete, more lye (generally adopt milk of lime, the difference between the molar weight of hydroxide radical contained in it and the molar weight needed to neutralize hydrogen chloride is About 1.2 times of the molar weight of dichloropropanol) and longer residence time, at the same time, the inhomogeneous mixing of materials will cause local alkali concentration to be higher and the residence time will cause the hydrolysis reaction to intensify, the reaction yield will reduce, and the COD in the wastewater will higher value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Carry out experiment according to this method, preparation solution A, containing dichloropropanol concentration is 2wt.%, hydrogen chloride concentration is 0, preparation solution B, containing sodium hydroxide concentration is 2wt.%, both flows are respectively 20ml / min and 6.2 ml / min, the ratio of the molar ratio (hydroxide / (dichloropropanol+hydrogen chloride)) to 1 is passed into the membrane dispersion micro-reactor, the temperature of the reaction system is 90°C, the two-phase fluid in the reaction equipment The dwell time is 10s. The product was analyzed, and the conversion rate of the reaction reached 98%, and the selectivity reached 99.4%.

Embodiment 2

[0018] Carry out experiment according to this method, preparation solution A, containing dichloropropanol concentration is 5wt.%, hydrogen chloride concentration is 1.4wt.%, preparation solution B, containing sodium hydroxide concentration is 10wt.%, both flows are respectively 20ml / min and 7.4ml / min, the molar ratio (hydroxide / (dichloropropanol+hydrogen chloride)) is 1.2 into the membrane dispersion microreactor, the temperature of the reaction system is 70 ° C, the two-phase fluid is reacting The dwell time in the device is 100s. The product was analyzed, and the conversion rate of the reaction reached 99%, and the selectivity reached 98.3%.

Embodiment 3

[0020] Carry out experiment according to this method, preparation solution A, containing dichloropropanol concentration is 10wt.%, hydrogen chloride concentration is 2.8wt.%, preparation solution B, containing sodium hydroxide concentration is 5wt.%, both flows are respectively 20ml / min and 24.6ml / min, with the ratio of molar ratio (hydroxide / (dichloropropanol+hydrogen chloride)) being 1, it is passed into the micro-sieve reactor, the temperature of the reaction system is 40°C, and the two-phase fluid is in the reaction equipment The dwell time in is 600s. The product was analyzed, and the conversion rate of the reaction reached 98%, and the selectivity reached 96.3%.

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Abstract

The invention discloses a method for preparing epoxy chloropropane by cyclizing dichloropropanol in a microreactor, belonging to the technical field of chemical reaction engineering. The method comprises the following steps: quickly mixing a dichloropropanol water solution with a sodium hydroxide water solution in the microreactor; controlling the temperature of the cyclization reaction to be 40-100 DEG C; finishing reaction in a delay tube; and finally separating in a rectifying tower to obtain epoxy chloropropane. According to the method, the reaction material solutions are quickly mixed in the microreactor, so that the cyclization reaction is fully finished while side reactions caused by non-uniformly mixing are prevented and the usage amount of alkali liquor is guaranteed to be closer to the theoretical value. Compared with the traditional cyclization tower and the reactive distillation coupling technology, the method for preparing epoxy chloropropane by cyclizing dichloropropanol in the microreactor has the advantages of short material retention time, high conversion rate, high selectivity and the like, so that the production cost can be saved, the material consumption can be reduced and the byproduct amount can be decreased.

Description

technical field [0001] The invention belongs to the technical field of chemical reaction engineering, and particularly relates to a method for preparing epichlorohydrin by cyclization of dichloropropanol in a microreactor. More specifically, the invention relates to the efficient realization of two A method for preparing epichlorohydrin by cyclization of chloropropanol. Background technique [0002] Epichlorohydrin is an important organic chemical product with a wide range of uses, mainly used in the production of epoxy resin, chlorohydrin rubber, etc. At present, the main methods of producing epichlorohydrin at home and abroad are propylene high-temperature chlorination method and propylene acetate method. Wherein more than 90% of epichlorohydrin is produced by high-temperature chlorination of propylene. With the development of the biodiesel industry, a large amount of bioglycerol is produced by-product, the price of glycerol has fallen and the demand for epichlorohydrin ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/26
CPCY02P20/10
Inventor 吕阳成张吉松王凯骆广生姜育田
Owner JIANGSU ANPON ELECTROCHEM
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