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Preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-propylene oxide

A technology of tetrafluoropropoxy and propylene oxide, which is applied in the field of ether preparation, can solve the problems of low yield, high preparation cost, and long reaction time, and achieve high product yield, low production cost, and short reaction time Effect

Inactive Publication Date: 2012-07-25
UNIV OF SHANGHAI FOR SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, because the reaction temperature of the system is higher and the alkalinity is larger, it is difficult to avoid the hydrolysis of tetrafluoropropanol, so the reaction process is used to prepare 3-(2,2,3,3-tetrafluoropropoxy)-1 , the yield of 2-propylene oxide is low. In addition, potassium hydroxide is not easily soluble in the oil phase and is difficult to disperse in the reaction system. Therefore, the reaction time is longer
Other synthesis processes are all similar to the above, therefore, there are low yields of monomer products, long reaction times, complicated post-processing, high preparation costs, which limit the preparation of fluorine-containing polyurethanes.

Method used

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  • Preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-propylene oxide
  • Preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-propylene oxide
  • Preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-propylene oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0022] In a container with water separator, dropping funnel and stirring device, add 200g (2.16mol) 1,2-epoxychlorohydrin (1,2-epoxychlorohydrin:tetrafluoropropanol is 4.8:1) And 60mL cyclohexane, stirred at 350rap / min, heated to cyclohexane reflux. Then, add dropwise 65g and 60g (0.45mol) of tetrafluoropropanol with a mass fraction of 40% potassium hydroxide aqueous solution respectively in the reaction system, remove water while reacting, after the potassium hydroxide aqueous solution and tetrafluoropropanol are added, React until no water comes out, and end the reaction. After cooling and filtering to remove potassium chloride, heat the mother liquor to 65°C under normal pressure to remove the cyclohexane in the reaction liquid. When no cyclohexane distills out, cool down to 30°C and use vacuum distillation instead. Adjust the pressure so that the temperature of the distillation system is controlled at 65°C, recover excess 1,2-epichlorohydrin, then collect the fraction at ...

Embodiment 2

[0026] In a container with water separator, dropping funnel and stirring device, add 292g (3.15mol) 1,2-epoxychlorohydrin (1,2-epoxychlorohydrin:tetrafluoropropanol is 7:1) And 60mL cyclohexane, stirred at 400rap / min, heated to cyclohexane reflux. Then, add dropwise 65g and 60g (0.45mol) of tetrafluoropropanol with a mass fraction of 40% potassium hydroxide aqueous solution respectively in the reaction system, remove water while reacting, after the potassium hydroxide aqueous solution and tetrafluoropropanol are added, React until no water comes out, and end the reaction. After cooling and filtering to remove potassium chloride, heat the mother liquor to 65°C under normal pressure to remove the cyclohexane in the reaction liquid. When no cyclohexane distills out, cool down to 30°C and use vacuum distillation instead. Adjust the pressure so that the temperature of the distillation system is controlled at 65°C, recover excess 1,2-epichlorohydrin, then collect the fraction at 12...

Embodiment 3

[0028]In a container with water separator, dropping funnel and stirring device, add 50g (0.54mol) 1,2-epoxychlorohydrin (1,2-epoxychlorohydrin:tetrafluoropropanol is 1.2:1) And 60mL cyclohexane, stirred at 350rap / min, heated to cyclohexane reflux. Then, add dropwise 65g and 60g (0.45mol) of tetrafluoropropanol with a mass fraction of 40% potassium hydroxide aqueous solution to the reaction system, remove water while reacting, after the potassium hydroxide aqueous solution and tetrafluoropropanol are added, React until no water comes out, and end the reaction. After cooling and filtering to remove potassium chloride, heat the mother liquor to 65°C under normal pressure to remove the cyclohexane in the reaction liquid. When no cyclohexane distills out, cool down to 30°C and use vacuum distillation instead. Adjust the pressure so that the temperature of the distillation system is controlled at 65°C, recover excess 1,2-epichlorohydrin, then collect the fraction at 120-130°C / 250-3...

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Abstract

The invention discloses a preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-propylene oxide. The method comprises the following steps: adding 1,2-epoxy chloropropane and cyclohexane into a container with a water separator, a dropping funnel and a stirring device, stirring, and heating until the cyclohexane flows back; respectively adding potassium hydroxide water solution and 2,2,3,3-tetrafluoropropanol; removing water while reacting; after the reaction ends up, filtering out potassium chloride, heating the mother liquor, heating to remove the cyclohexane, and collecting fraction under120-130 DEG C / 250-300 Pa; and distilling the fraction under reduced pressure, and collecting the fraction under 125-127 DEG C / 250-300 Pa, thereby obtaining the 3-(2,2,3,3-tetrafluoropropoxy)-1,2-propylene oxide. The preparation method has the advantages of shorter reaction time, higher product yield, low production cost and the like.

Description

technical field [0001] The present invention relates to the preparation method of ether, more specifically the preparation method of 3-(2,2,3,3-tetrafluoropropoxy)-1,2-epoxypropane. Background technique [0002] 3-(2,2,3,3-tetrafluoropropoxy)-1,2-propylene oxide is an important monomer for the preparation of fluorine-containing polyurethane. Fluorine-containing polyurethane refers to the 2 In addition to groups, there are also fluorine-containing high polymers containing many carbamate groups. This kind of fluorine-containing high polymer not only has the general characteristics of polyurethane elastomers: high strength, high elasticity, high wear resistance, excellent low-temperature performance and bonding performance; it also has the heat resistance and corrosion resistance of fluorine-containing high polymers , Chemical resistance, solvent resistance, oil resistance, low pollution and other excellent properties. Because fluorine-containing polyurethane has the above ad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/22C07D301/00
Inventor 王霞李颖李丽华金东元宋卫李玲玲
Owner UNIV OF SHANGHAI FOR SCI & TECH
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