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Method for preparation of 2, 4-dinitrophenoxyethanol

A technology of dinitrophenoxyethanol and dinitrochlorobenzene is applied in the field of preparation of 2.4-dinitrophenoxyethanol, can solve problems such as waste of ethylene glycol raw materials, achieve cost saving, reduce waste generation, high yield effect

Inactive Publication Date: 2017-02-15
CHONGQING BEISHENG PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a simple and safe preparation method of 2,4-dinitrophenoxyethanol, while solving the problem of waste of unreacted ethylene glycol raw materials in the process

Method used

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Examples

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Effect test

Embodiment 1

[0025] In a 2000L reactor, 2000kg of ethylene glycol was pumped into the reactor. After the temperature was raised to 75°C, 160kg of 2.4-dinitrochlorobenzene melted in advance was pumped by vacuum. After holding for 0.5h, open the manhole, add 60kg of sodium hydroxide solid, and control the temperature to 90℃. After 2 hours of reaction, samples were taken for HPLC detection, after the reaction was completed. Add to ice water to cool down to below 5-10°C and centrifuge to obtain condensate, which is centrifuged three times, each time not less than 2 hours, and washed with ice water. Weigh after centrifugation. The product is obtained by drying. After the mother liquor is distilled under reduced pressure to remove water, the remaining liquid can be used for ethylene glycol reuse. The purity is over 98.5%, and the yield is over 95%.

Embodiment 2

[0027] In a 2000L reactor, 2000kg of ethylene glycol was pumped into the reactor. After the temperature was raised to 80°C, 160kg of 2.4-dinitrochlorobenzene melted in advance was pumped by vacuum. After holding for 0.5h, open the manhole, add 126kg sodium bicarbonate, and control the temperature to 80℃. After 2 hours of reaction, samples were taken for HPLC detection, after the reaction was completed. Add to ice water to cool down to below 5-10°C and centrifuge to obtain condensate, which is centrifuged three times, each time not less than 2 hours, and washed with ice water. Weigh after centrifugation. The product is obtained by drying. After the mother liquor is distilled under reduced pressure to remove water, the remaining liquid can be used for ethylene glycol reuse. The purity is over 98.5%, and the yield is over 95%.

Embodiment 3

[0029] In a 2000L reactor, 2000kg of ethylene glycol was pumped into the reactor, and after the temperature was raised to 78°C, 160kg of 2.4-dinitrochlorobenzene melted in advance was pumped by vacuum. After holding for 0.5h, open the manhole, add 80kg sodium carbonate, and control the temperature to 85℃. After 2 hours of reaction, samples were taken for HPLC detection, after the reaction was completed. Add to ice water to cool down to below 5-10°C and centrifuge to obtain condensate, which is centrifuged three times, each time not less than 2 hours, and washed with ice water. Weigh after centrifugation. The product is obtained by drying. After the mother liquor is distilled under reduced pressure to remove water, the remaining liquid can be used for ethylene glycol reuse. The purity is over 98.5%, and the yield is over 95%.

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Abstract

The invention relates to a method for preparation of 2, 4-dinitrophenoxyethanol. The method is a simple and safe process and solves the unreacted ethylene glycol raw material waste problem. The method comprises pumping ethylene glycol in vacuum into a reactor, carrying out stirring heating to 75-80 DEG C, then pumping pre-molten 2,4-dinitrochlorobenzene in vacuum into the reactor, carrying out mixing, keeping the constant temperature for 0.5h, adding an inorganic base into the mixture, controlling the reaction temperature to 80-90 DEG C, after the reaction is finished, cooling the reaction system to less than or equal to 10 DEG C, and carrying out centrifugal filtration to obtain filter cake as a product. The method is simple and the 2, 4-dinitrophenol has less impurities and a high yield. The method can recover and recycle the unreacted ethylene glycol so that a cost is greatly reduced in large-scale production, wastes are reduced, clean production is realized and the ecological environment is protected.

Description

Technical field [0001] The invention relates to a preparation method of a hair dye intermediate, in particular to a preparation method of 2.4-dinitrophenoxyethanol. Background technique [0002] 2,4-Dinitrophenoxyethanol is an important hair dye intermediate. The product is non-toxic or pharmaceutical intermediate. It is widely used in real life. [0003] However, the existing methods for preparing 2,4-dinitrophenoxyethanol are less publicly reported, and the prior art produces more 2,4-dinitrophenols when preparing 2,4-dinitrophenoxyethanol. Great harm to the environment. In addition, the waste of organic solvents is relatively large, and the processing cost is relatively high. Summary of the invention [0004] The purpose of the present invention is to provide a simple and safe method for preparing 2,4-dinitrophenoxyethanol, and simultaneously solve the problem of waste of unreacted ethylene glycol raw materials in the process. [0005] In order to achieve the above object, the ...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/34
CPCC07C201/12
Inventor 潘先文董小峰吉澍
Owner CHONGQING BEISHENG PHARMA TECH CO LTD
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