Difluoroethanol synthesis process

A technology for difluoroethanol and synthesis process, which is applied in the field of synthesis technology of difluoroethanol, can solve problems such as difficulty in recycling, and achieve the effects of few steps, good process economy and simple process

Inactive Publication Date: 2018-05-25
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problem of the above method is that most of the reactions go through 2 to 3 steps, and the product purity and yield are only 96.3% and 87% at the highest. In addition, the reaction produces a large amount of metal salt mixture, which is difficult to recycle.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 860.9g of γ-butyrolactone and 149.6g of potassium hydroxide into the dry reaction kettle, then introduce 201g of 2,2-difluoro-1-chloroethane through the liquid phase port, then rapidly raise the temperature to 180°C, and react for 4h . The resulting reaction solution was filtered, distilled, and then dried through 4A molecular sieves to obtain the difluoroethanol product with a purity of 99.93% and a yield of 92.3%.

[0015] After the reaction solution was filtered, the solid was stirred with 1000 mL of anhydrous methanol at room temperature for 2 h, filtered, and dried to obtain potassium chloride; the filtrate was evaporated to dryness under reduced pressure to obtain potassium acetate. After drying, 94.4 g of potassium hydroxybutyrate was obtained, with a recovery rate of 96.1%.

Embodiment 2

[0017] Add 858.9g of γ-butyrolactone and 130.9g of potassium hydroxide into the dry reaction kettle, then introduce 200g of 2,2-difluoro-1-chloroethane through the liquid phase port, then rapidly raise the temperature to 200°C, and react for 6h . The resulting reaction solution was filtered, distilled, and then dried over anhydrous magnesium sulfate and 4A molecular sieve to obtain the difluoroethanol product with a purity of 99.91% and a yield of 92.7%.

[0018] After the reaction solution was filtered, the solid was stirred with 800 mL of anhydrous methanol at room temperature for 2 h, filtered, and dried to obtain potassium chloride; the filtrate was evaporated to dryness under reduced pressure to obtain potassium acetate. After drying, 48.0 g of potassium hydroxybutyrate was obtained with a recovery rate of 94.5%.

Embodiment 3

[0020] Add 1377.4g of γ-butyrolactone and 137.0g of potassium hydroxide into the dry reaction kettle, and then pass 199g of 2,2-difluoro-1-chloroethane through the liquid phase port, and then rapidly rise to 160°C, and react 8h. The resulting reaction solution was filtered, distilled, and then dried over anhydrous copper sulfate and 4A molecular sieve to obtain the difluoroethanol product with a purity of 99.90% and a yield of 92.1%.

[0021] After the reaction solution was filtered, the solid was stirred with 1000 mL of absolute ethanol at 35°C for 2 hours, filtered, and dried to obtain potassium chloride; the filtrate was evaporated to dryness under reduced pressure to obtain potassium acetate. After drying, 67.0 g of potassium hydroxybutyrate was obtained, with a recovery rate of 97.1%.

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PUM

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Abstract

The invention relates to a difluoroethanol synthesis process. The difluoroethanol synthesis process comprises the following steps: firstly adding gamma-butyrolactone and an alkali metal hydroxide intoa reactor, introducing 2,2-difluoro-1-halothane, rapidly heating to the reaction temperature, processing a feed liquid through a centrifugal machine after the reaction is finished, rectifying an obtained clear liquid in a separation tower to obtain difluoroethanol; centrifuging, enabling a solid to enter a washing kettle, washing with methyl alcohol or ethanol, processing a washing liquid throughthe centrifugal machine, drying an obtained solid through a drier to obtain potassium chloride, conducting vacuum distillation on the centrifuged clear liquid in a distilling kettle, recycling methylalcohol or ethanol, obtaining a solid of potassium hydroxybutyrate after distilling, drying through the drier, and returning to a reaction system to continue to react. By adopting the process, the operation is simple, the economic efficiency is relatively high, and the process is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of fluorine-containing fine chemicals, and in particular relates to a synthesis process of difluoroethanol. Background technique [0002] As an important aliphatic fluorine-containing fine chemical, difluoroethanol is widely used in the fields of herbicides, insecticides, pharmaceutical intermediates, fluoropolymers, optical cleaning agents, anesthetics, and heating pump working fluids. [0003] There are many synthetic methods of difluoroethanol reported at present, but relatively speaking, with cheap chlorofluorocarbon 2,2-difluoro-1-haloethane as raw material synthesis of difluoroethanol, with small investment, low cost, The method has the advantages of simple method and high safety. WO2009040367 discloses a three-step method for synthesizing difluoroethanol. First use vinylidene fluoride and HBr to react under ultraviolet light to generate 2,2-difluoro-1-bromoethane; then add carboxylate and generate fluorine-co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/124C07C29/80C07C31/38
CPCC07C29/124C07C29/80C07C31/38
Inventor 吕剑王为强杨建明张前惠丰袁俊李亚妮梅苏宁余秦伟赵锋伟
Owner XIAN MODERN CHEM RES INST
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