Manufacturing method of 2,2-difluoroethanol
I. INTRODUCTION
2,2-difluoroethanol (DFE) is an important fluorine-containing organic compound, which is widely used in the fields of pharmaceuticals, pesticides, liquid crystal materials and so on. Due to its unique physical and chemical properties, the manufacturing method of DFE has attracted much attention. In this paper, we will introduce an effective manufacturing method in anticipation of contributing to the development of the field of raw materials for chemical production.
II. MATERIALS AND METHODS
1. MATERIALS
Raw materials: chloroform, potassium fluoride, potassium hydroxide, ethylene glycol.
Reagents: anhydrous sodium sulfate, saturated saline, ethyl acetate.
2. Equipment
Reactor, stirrer, condenser, water separator, thermometer, pH meter.
3. Manufacturing method
(1) Add chloroform, potassium fluoride and potassium hydroxide into the reaction kettle according to a certain proportion, stir and heat up to a certain temperature, and then react for a period of time to produce 2,2-difluoroacetone.
(2) 2,2-difluoroacetone and ethylene glycol were added to the reaction kettle, heated to a certain temperature, and the pH was controlled, and the addition reaction was carried out to produce 2,2-difluoroethanol.
(3) After the reaction, the reaction solution was cooled to room temperature, washed with saturated brine, dried with anhydrous sodium sulfate, and filtered to obtain the crude product.
(4) The crude product was distilled and the product in the specified fractions was collected as pure 2,2-difluoroethanol.
III. RESULTS AND DISCUSSION
1. RESULTS
With the present method of fabrication, we have successfully synthesized 2,2-difluoroethanol with high purity and high yield.
Table 1 Yield and purity of 2,2-difluoroethanol
|Batch | Yield (%) | Purity (%) |
| --- | --- | --- |
| 1 | 85 | 98 |
| 2 | 88 | 99 |
| 3 | 90 | 99 |
2. Discussion
(1) The effect of the reaction temperature and time on the yield: in the experiments, we found that the reaction temperature and time had a greater influence on the yield. Appropriately increasing the reaction temperature can speed up the reaction rate and increase the yield. However, too high temperature may lead to the increase of side reaction and affect the purity of the product. At the same time, the reaction time also needs to be controlled appropriately to ensure that the reaction is carried out completely.
(2) The effect of raw material ratios on the yield: In the experiment, we tried different raw material ratios and found that the yield was higher when the molar ratio of chloroform, potassium fluoride and potassium hydroxide was 1:1.2:1.5. Meanwhile, the amount of ethylene glycol needs to be controlled appropriately to ensure the smooth progress of the addition reaction.
IV.CONCLUSION
In this paper, an effective method for the manufacture of 2,2-difluoroethanol was introduced, and by controlling the reaction conditions, a product with high purity and satisfactory yield can be obtained. The method is easy to operate, the raw materials are easy to obtain, and it has a good prospect for industrialization. It is hoped that this paper can play a role in promoting the development of the field of raw materials for the production of chemicals.
