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Preparation method and device of difluoroethanol

A technology of difluoroethanol and difluoroethane, which is applied in the field of preparation of difluoroethanol, can solve the problems of difficult treatment, long process route, and many solid wastes, and achieve mild reaction conditions, no pollution to the environment, and easy-to-obtain raw materials Effect

Inactive Publication Date: 2018-02-27
SHANDONG HUAAN NEW MATERIAL
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is an obvious defect in the technology disclosed in this patent: the solid waste generated is large and difficult to handle, so the cost of industrial production is relatively high
[0005] Other technical routes such as the reduction of difluoroacetic acid carboxylate to prepare difluoroethanol are economically unacceptable due to the long process route and high cost of raw materials

Method used

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  • Preparation method and device of difluoroethanol
  • Preparation method and device of difluoroethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of this difluoroethanol comprises the steps:

[0026] (1) Add 600g of solvent and 100g of potassium hydroxide in a 1.5L reactor to react under stirring, the reaction temperature is 140°C, and the reaction time is 0.5 hours;

[0027] (2) After the reaction in step (1) is completed, slowly add 300 g of 2-chloro-1,1-difluoroethane to the reactor at a flow rate of 100 mL / h, the reaction temperature is 200 ° C, the reaction time is 10 hours, and then the The product is sequentially sent to the rough steamer 4 and the rectification tower 7 for separation to obtain 2,2-difluoroethanol.

[0028] The reaction of step (1) and step (2) is carried out in an inert gas nitrogen, and the stirring speed is controlled at 600 rpm.

[0029] The water of 5%~10% potassium hydroxide weight is added in the reaction process of step (1) and step (2) or before reaction starts.

[0030] The solvent is γ-butyrolactone.

[0031] 2-Chloro-1,1-difluoroethane storage tank 1 a...

Embodiment 2

[0036] The difference between this example and Example 1 is: add 600g of solvent and 100g of potassium hydroxide to a 1.5L reactor, control the stirring speed at 600r / min, the temperature at 160°C, and react for 1.5h; Add 300 g of 2-chloro-1,1-difluoroethane, control the temperature at 250° C., and react for 10 hours. After the reaction is completed, difluoroethanol is separated and collected.

Embodiment 3

[0038] The difference between this example and Example 1 is: add 1000g of solvent, 100g of potassium hydroxide and 10g of water into a 1.5L reactor, control the stirring speed at 400r / min, the temperature at 130°C, and react for 1h; 300 g of 2-chloro-1,1-difluoroethane was injected at a flow rate of 2-chloro-1,1-difluoroethane, the temperature was controlled at 190° C., and the reaction was carried out for 8 hours. After the reaction was completed, difluoroethanol was separated and collected.

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Abstract

The invention relates to a preparation method and device of difluoroethanol. The preparation method of the difluoroethanol comprises the following steps: enabling a solvent to react with potassium hydroxide in a closed reaction kettle to generate an intermediate product; slowly introducing excess 2-chloro-1,1-difluoroethane into the reaction kettle; after reacting for a certain period of time, separating and purifying a product to obtain high-purity 2,2,-difluoroethanol. According to the preparation method provided by the invention, the difluoroethanol is prepared from 2-chloro-1,1-difluoroethane; the raw material, which is a byproduct of 1,-chloro-1,1-difluoroethane, is easily available and has low cost; the reaction conditions are mild, few byproducts are produced, and environmental pollution is avoided.

Description

technical field [0001] The invention relates to a preparation method and device of difluoroethanol. Background technique [0002] Difluoroethanol is mainly used in the synthesis of fluorine-containing medicines, pesticides and dyes. 2,2-Difluoroethanol is an important aliphatic fluorine-containing intermediate. It is a colorless liquid with an alcohol smell at room temperature. It is stable in nature and can be freely miscible with water and various organic solvents. Due to its unique physical and chemical properties and molecular structure, it has different properties from other alcohols and can participate in various organic chemical reactions, so it has broad prospects for development and utilization. [0003] At present, many patents and documents have reported the technology for preparing the difluoroethanol, such as the technology disclosed in Chinese Patent Application No. 2012800356104. The technology disclosed in this patent includes the following steps: step (i): ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/124C07C31/38
CPCC07C29/124C07C31/38
Inventor 王瑞英段琦明文勇孟翔徐甲超田勇王通
Owner SHANDONG HUAAN NEW MATERIAL
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