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High-purity chlorohydrins and preparation method thereof

A chloroethanol and high-purity technology, applied in the field of preparing high-purity chloroethanol, can solve the problems of serious pollution, high cost of purification process, large energy consumption, etc., and achieve the effects of high yield, low pollution and simple post-processing

Inactive Publication Date: 2014-03-19
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the hypochlorous acid method, this process has the advantages of simple process, stable product quality, and high product purity, but the purification process of reaction raw material HCl gas is expensive, consumes a lot of energy, and causes serious pollution.

Method used

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  • High-purity chlorohydrins and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 125 grams of 1,4-dichloro-2-butene (1mol) and 200 milliliters of methanol into a 500-mL four-necked flask, mechanically stir at -25°C, and adjust the oxygen flow to carry out the ozonation reaction, followed by gas chromatography React, raw material disappears in about 3 hours, and reaction finishes and stops ozonation. Use nitrogen gas to drive away the ozone in the reaction bottle, keep the inner temperature at about -10°C, add dropwise to 150 ml of methanol solution containing 40.0 g of sodium borohydride (1.05 mol), and continue stirring for 1 hour after the addition. After the reaction is complete, usually The solvent was recovered under pressure, and the fraction at 128-129°C was collected by atmospheric distillation to obtain 136.8 g of a colorless transparent liquid with a gas phase content of 99.4% and a yield of 84.5%.

[0023] Product structure confirmation:

[0024] 1 HNMR (δppm, 400MHz, CDCl 3 ):3.60-3.74(m,2H,-CH 2 Cl);3.82-3.96(m,2H,-CH* 2 OH); 2...

Embodiment 2

[0027] Add 125 grams of 1,4-dichloro-2-butene (1mol) and 200 milliliters of ethanol into a 500-mL four-necked flask, stir mechanically at -10°C, and carry out ozonation reaction after adjusting the oxygen flow, followed by gas chromatography React, raw material disappears in about 3 hours, and reaction finishes and stops ozonation. Pass nitrogen to drive away the ozone in the reaction bottle, keep the inner temperature around 0°C, add dropwise to 150 ml ethanol solution containing 66.0 g potassium borohydride (1.2 mol), continue to stir and react for 1.5 hours after the addition, the reaction is completed, and the normal pressure The solvent was recovered, and the fraction at 128-129°C was collected by atmospheric distillation to obtain 140.3 g of a colorless transparent liquid with a gas phase content of 99.7% and a yield of 86.9%. Product nuclear magnetic spectrum is identical with embodiment 1.

Embodiment 3

[0029] Add 125 grams of 1,4-dichloro-2-butene (1mol) and 200 milliliters of isopropanol into a 500-mL four-neck flask, mechanically stir at 5°C, and adjust the oxygen flow to carry out the ozonation reaction. Gas chromatography Following the reaction, the raw materials disappeared in about 3 hours, and the ozonation was stopped at the end of the reaction. Pass nitrogen to drive off the ozone in the reaction bottle, keep the inner temperature at about 10°C, add dropwise to 150 ml of ethanol solution containing 50.0 g of potassium borohydride (0.91 mol), continue to stir and react for 2 hours after the addition, the reaction is completed, and the normal pressure The solvent was recovered, and the fraction at 128-129°C was collected by atmospheric distillation to obtain 138.7 g of a colorless transparent liquid with a gas phase content of 99.5% and a yield of 85.7%. Product nuclear magnetic spectrum is identical with embodiment 1.

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Abstract

The invention relates to the field of synthesis of chemical raw materials, and discloses a method for preparing high-purity chlorohydrins. The preparation method comprises the following steps: a, mixing a raw material 1, 4-dichloro-2-butene and an ozonization reaction solvent; agitating; charging ozone to perform ozonization reaction; tracking the reaction through gas chromatography; and stopping the ozonization reaction until raw materials disappear; and b, charging nitrogen to remove the ozone from a reaction flask; adding a reducing agent to reduce at -10-30 DEG C; agitating; recovering the solvent under a normal pressure condition; and distilling and collecting fractions under normal pressure to obtain the high-purity chlorohydrins. The preparation method is simple and convenient in process route, small in pollution, high in yield, fast in reaction speed, and simple in post-treatment; the chlorohydrins have the purity exceeding 99%, and thus the industrial value is relatively high.

Description

technical field [0001] The invention relates to the field of synthesis of chemical raw materials, in particular to a method for preparing high-purity chloroethanol. Background technique [0002] Chlorohydrin is an important organic solvent and chemical raw material. High-purity chloroethanol is widely used in industries such as chemical industry, medicine, pesticide, rubber and dyestuff. Meifen, Weifukang and Yantongxin, propranolol and procaine are used as raw materials for 1059 insecticide, chlordane (1068) insecticide and demeton in the pesticide industry. At present, there are mainly two methods for the industrial preparation of chloroethanol: the hypochlorous acid method and the hydrochloric acid method. The hypochlorous acid method is to pass ethylene and chlorine into water at the same time, chlorine and water react to form hypochlorous acid, and hypochlorous acid and ethylene are added to form chlorohydrin. The initial content of the chloroethanol aqueous solution ...

Claims

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Application Information

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IPC IPC(8): C07C31/36C07C29/14
CPCC07C29/132C07D301/03C07D303/08C07C31/36
Inventor 吴春雷
Owner SHAOXING UNIVERSITY
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