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Method for preparing 2,2,3,3,3-pentafluoro-1-propanol

A technology of pentafluoropropanol and pentafluoropropionate, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of complex operation, difficult industrialization, and many synthesis steps, and meet the reaction conditions Mild, less synthetic steps, easy to obtain raw materials

Inactive Publication Date: 2019-03-29
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The existing methods for synthesizing 2,2,3,3,3-pentafluoropropanol are mainly addition method and catalytic hydrogenation method, both of which have many synthesis steps, complicated operation, expensive reagents, and low yield.
[0007] Japanese patent JP 06072925 reported that in liquid HF, TiF4 was used as a catalyst to obtain 2,2,3,3,3-pentafluoropropanol through the addition reaction of trioxane and tetrafluoropropene. The method used liquid HF, TiF 4 and other reagents, which are highly polluting, highly toxic, unfriendly to the environment, and have high safety risks; US4273947 reported that 2,2,3,3,3-pentafluoropropionic acid was used as a raw material in the presence of a Ru / C catalyst to undergo catalytic hydrogenation in one step Synthesis of 2,2,3,3,3-pentafluoropropanol, the raw material price of this method is high, it is difficult to industrialize, and it needs to react under the condition of hydrogen, which has a large safety risk; PTC2002026679 reported 2,2,3,3 , 3-pentafluoropropanamide is used as a raw material to synthesize 2,2,3,3,3-pentafluoropropanol in one step through catalytic hydrogenation in the presence of a Pd / C catalyst. This method has high raw material prices, is difficult to industrialize, and requires Reaction under hydrogen conditions, there is a greater safety risk

Method used

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Examples

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preparation example Construction

[0015] The catalyst in the present invention is M-KF / Al 2 O 3 The preparation methods include:

[0016] (1) Transfer 20g pseudo-boehmite into 200Ml EG to form a suspension;

[0017] (2) Under the water bath temperature of 60℃ and magnetic stirring, quickly add 20g potassium fluoride solution and 2g active metal M precursor solution to the suspension described in step (1), and continue stirring for 2h after the addition is complete Then it turns into a semi-solid wet gel;

[0018] (3) The wet gel described in step (2) is aged overnight in an air atmosphere and then transferred to an oven to dry at 110°C for 24 hours to obtain a white dry gel powder that is the M-KF / Al 2 O 3 catalyst.

Embodiment 1

[0020] Into the reactor containing 100g ethyl pentafluoropropionate, slowly add 5g 1% Pt-KF / Al 2 O 3 The catalyst, stirred vigorously, and heated to 50°C, reacted for 4 hours, and the result of gas chromatography analysis showed that the conversion rate was 99.3%, and the selectivity of 2,2,3,3,3-pentafluoropropanol was 90.5%

Embodiment 2~5

[0022] The method for preparing 2,2,3,3,3-pentafluoropropanol in Examples 2 to 5 is the same as in Example 1, except that the reaction time is changed. The reaction results are shown in Table 1.

[0023] Table 1

[0024]

[0025]

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Abstract

The invention discloses a method for preparing 2,2,3,3,3-pentafluoro-1-propanol. According to the method, pentafluoropropionate with a general formula of CF3CF2COOCnH(2n+1) is taken as a raw materialfor preparing 2,2,3,3,3-pentafluoro-1-propanol through a one-step process under the existence of a catalyst. M-KF / Al2O3 is served as the catalyst; catalytic active metal M is one or more of Pt, Au, Pd, Ag and Cu; mass percent of the catalytic active metal M in the catalyst is 0.1%-20%; the pentafluoropropionate with the general formula of CF3CF2COOCnH(2n+1) is composed of methyl pentafluoropropionate and ethyl pentafluoropropionate; in the invention, reaction temperature is at 40 DEG C-100 DEG C, reaction time is 1h-8h, and mass ratio of pentafluoropropionate to catalyst is at 1:(0.05-0.2); the method for preparing 2,2,3,3,3-pentafluoro-1-propanol provided by the invention has the advantages of few reaction step, simple operation, low-cost and easily acquired raw materials, high yield andmild reaction condition.

Description

Technical field [0001] The invention belongs to the field of fluorine chemicals and relates to a preparation method of 2,2,3,3,3-pentafluoropropanol. Background technique [0002] ODS cleaning agent (ODS is the abbreviation of "Ozone Depleting Substance", meaning "ozone depleting substance") is an important class of substances commonly used in human life and industry. It has the characteristics of low toxicity, non-combustibility, and chemical inertness, so it is widely used It is used as a refrigerant, foaming agent, aerosol, and cleaning agent for electronic components and precision parts. Its application range covers households and all walks of life, and it has become an indispensable product for modern life. [0003] However, ODS cleaning agent has a strong destructive effect on the ozone layer and will cause global temperature warming. According to the effective "Montreal Protocol on Substances that Deplete the Ozone Layer" and the "Overall ODS Phase-out Plan for China's Clea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/147C07C31/38
CPCC07C29/147C07C31/38
Inventor 唐晓博吕剑杨志曾纪珺韩升赵波亢建平郝志军李凤仙
Owner XIAN MODERN CHEM RES INST
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