Preparation and application of 2,2,3,3-tetrafluoropropanol_Industrial additives

Background and overview^[1]

2,2,3,3-tetrafluoropropanol, commonly known as tetrafluoropropanol, CAS number 76-37-9 , is an important chemical raw material for the preparation of fluorine-containing acrylic resin and some fluorine-containing resins, and is also an important organic intermediate.

Preparation^[1]

Combine methanol and peroxydicarbonate Isopropyl is preformed into a solution and stored in a storage tank, and tetrafluoroethylene is stored in another storage tank. Set the flow rate ratio of the metering pump to diisopropyl peroxydicarbonate: methanol: tetrafluoroethylene as 38g: 95g. : 370g, pass the materials into the straight channel preheating module respectively, preheat diisopropyl peroxydicarbonate and methanol at 20°C for 10s, preheat tetrafluoroethylene at 70°C for 60s, methanol and peroxydicarbonate The mixed solution of diisopropyl ester is pumped into the heart-shaped mixing module of the micromixer with a metering pump for mixing. The mixed materials then enter the heart-shaped reaction module, mixed with tetrafluoroethylene, and then polymerized at 40°C for 30 seconds. The reaction product Flow into the distillation reaction kettle, and after distillation, collect the fractions with boiling points between 109 and 110°C to obtain 466g of 2,2,3,3-tetrafluoropropanol. Calculate the yield of 2,2,3,3-tetrafluoropropanol. 95%.

Application^[2-3]

1. CN201510235681.4 reports a 2,2,3,3-tetrafluoropropyl-2 , The preparation method of 2,3,3,4,4,4-heptafluorobutyl ether includes the following steps: under the action of alkali solution, perfluorobutylsulfonyl fluoride and 2,2,3,3-tetrafluorobutyl ether Propanol reaction, after the reaction is completed, filter to remove insoluble salts, the reaction product is allowed to stand and separated, the organic phase is separated, and washed with water 2-3 times to obtain the intermediate product 2,2,3,3-tetrafluoropropylperfluorobutan sulfonate; in an organic solvent, under the action of a catalyst, the intermediate product 2,2,3,3-tetrafluoropropyl perfluorobutane sulfonate and 2,2,3,3,4,4,4 – Reaction of heptafluorobutanol to obtain a crude product; the crude product is distilled under normal pressure to obtain. The method of the invention has the characteristics of mild conditions, normal pressure reaction, simple operation, convenient post-processing, easy product separation and purification, high yield, and is suitable for industrial production.

2. CN201010234364.8 discloses a preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-epoxypropane. That is, add 1,2-epoxychloropropane and cyclohexane to a container with a water separator, a dropping funnel and a stirring device, stir and heat until cyclohexane refluxes, and then add potassium hydroxide aqueous solution and 2, 2,3,3-Tetrafluoropropanol, remove water while reacting. After the reaction, filter out the potassium chloride and heat the mother liquor to remove cyclohexane. Then, collect the fraction at 120~130℃/250~300Pa. The fraction is then rectified under reduced pressure, and the fraction at 125~127℃/250~300Pa is collected to obtain 3-(2,2,3,3-tetrafluoropropoxy)-1,2-epoxypropane. The preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-epoxypropane of the present invention has the advantages of short reaction time, high product yield, and low production cost. .

References

[1] [Chinese invention, Chinese invention authorization] CN201611031873.4 A preparation method of 2,2,3,3?tetrafluoropropanol [public] /A preparation method of 2,2,3,3-tetrafluoropropanol [Authorized]

[2] CN201510235681.4 A kind of 2,2,3,3-tetrafluoropropyl-2 , Preparation method of 2,3,3,4,4,4-heptafluorobutyl ether

[3] CN201010234364.8 A kind of 3-(2,2,3,3-tetrafluoropropyl ether Preparation method of oxy)-1,2-epoxypropane