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Method for producing 4-chloro-3-hydroxyl-1-butene

A production method and a hydroxyl technology, which are applied in the field of producing 4-chloro-3-hydroxy-1-butene, can solve the problems of unsuitability for chemical production, difficult operation, large equipment, etc., so as to improve the utilization rate of equipment and simplify the operation. , The effect of solving the sedimentation problem

Inactive Publication Date: 2009-06-17
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In RICHARDG.KADESCH VOL68, it was introduced that 1,3-butadiene and carbon dioxide were passed into 3.5% calcium hypochlorite solution at a ratio of 6:1. If the concentration is too low, the equipment will be too large; in addition, if the flow rate ratio of 1,3 butadiene and carbon dioxide is strictly controlled at 6:1, it is actually not easy to operate, and a large amount of calcium carbonate precipitation produced in the reaction process will also cause raw materials A large amount of waste of 1,3-butadiene, so this method is not suitable for chemical production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 700 grams of 50% sodium hypochlorite aqueous solution to a 1000 ml reaction flask, control the temperature between 0 and 3°C, add 300 grams of 15% hydrochloric acid dropwise to make it acidic, and then pass 1,3- For butadiene, keep the reaction temperature between 0 and 3°C. After 1 hour, use starch potassium iodide test paper to detect the end of the reaction. It is found that the system has no bottom, and the aqueous solution is extracted with ether (6000 ml, extracted in six times), and the ether is combined. solution, and ether was recovered to obtain 221 g of solid 4-chloro-3-hydroxy-1-butene. Yield 48.7%.

Embodiment 2

[0015] Add 700 grams of 50% sodium hypochlorite aqueous solution to a 1000 ml reaction flask, control the temperature between 0 and 3°C, add 150 grams of 30% hydrochloric acid dropwise to make it acidic, and then pass 1,3- For butadiene, keep the reaction temperature between 0 and 3°C. After 1 hour, use starch potassium iodide test paper to detect the end of the reaction. It is found that the system has no bottom, and the aqueous solution is extracted with ether (6000 ml, extracted in six times), and the ether is combined. solution, and the ether solution was recovered to obtain 207 g of 4-chloro-3-hydroxy-1-butene. Yield 45.6%.

Embodiment 3

[0017] Add 700 grams of 50% sodium hypochlorite aqueous solution to a 1000 ml reaction flask, control the temperature between 8 and 10°C, add 300 grams of 15% hydrochloric acid dropwise to make it acidic, and then pass 1,3- For butadiene, keep the reaction temperature between 8 and 10°C. After 1 hour, use starch potassium iodide test paper to detect the end of the reaction. It is found that the system has no bottom, and the aqueous solution is extracted with ether (6000 milliliters, divided into six extractions, that is, 1000 milliliters* 6), the ether solution was combined, and the ether solution was recovered to obtain 210 g of 4-chloro-3-hydroxyl-1-butene. Yield 46.35%.

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Abstract

The invention relates to a method for producing 4-chlorine-3-hydroxyl-1-butylene, which is to take 1,3-butadiene as a raw material, and perform addition reaction under the action of hypochlorous acid to obtain the 4-chlorine-3-hydroxyl-1-butylene, wherein the temperature of the addition reaction is between 10 DEG C below zero and 10 DEG C. The method prepares the target product by directly taking the hypochlorous acid as a catalyst and performing addition reaction on the 1,3-butadiene, and can completely avoid the precipitation phenomenon, reduce the equipment investment, improve the utilization rate of equipment, and simplify the operation.

Description

technical field [0001] The present invention relates to a process for the production of 4-chloro-3-hydroxy-1-butene. Background technique [0002] 4-Chloro-3-hydroxy-1-butene is an important organic chemical intermediate. In RICHARDG.KADESCH VOL68, it was introduced that 1,3-butadiene and carbon dioxide were passed into 3.5% calcium hypochlorite solution at a ratio of 6:1. If the concentration is too low, the equipment will be too large; in addition, if the flow rate ratio of 1,3 butadiene and carbon dioxide is strictly controlled at 6:1, it is actually not easy to operate, and a large amount of calcium carbonate precipitation produced in the reaction process will also cause raw materials A large amount of waste of 1,3-butadiene, so this method is not suitable for chemical production. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a production method of 4-chloro-3-hydroxyl-1-butene with low equipment investmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/42C07C29/66C07C29/64
Inventor 王小龙
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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