Process for producing fluoroalkanol

A technology of fluorine-containing alkanols and manufacturing methods, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., and can solve problems such as difficulty in controlling the addition number of tetrafluoroethylene, low concentration, and low yield

Inactive Publication Date: 2003-11-05
ASAHI GLASS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the method of (1), it is difficult to control the addition number of tetrafluoroethylene, so even if one wants to obtain only the target object with a high useful addition number of 1 to 4, the molecular weight distribution of the product is also wide, and there is a high yield. low problem
In the method of (2), there are few products with a tetrafluoroethylene addition number of 1 to 2, and there is a problem that compounds with a tetrafluoroethylene addition number of 3 or more are mainly produced.
(3) have the long problem of necessary solid acid removal agent and reaction time in the method
However, in the method (4), there is the problem that the concentration of the obtained telomer is as low as about 10%, the average degree of polymerization is as high as 32, but the yield of the addition number is 1 to 4 is extremely low.

Method used

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  • Process for producing fluoroalkanol

Examples

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Effect test

Embodiment 1

[0054] Manufacture of 2,2,3,3-tetrafluoro-1-propanol

[0055] according to figure 1 The reaction was carried out as described in the flowchart. That is to say, with a 1-meter 3 A reaction kettle made of corrosion-resistant nickel-based alloy (Hastelloy) was used as a reactor, and 341 kg (432 L) of methanol was added therein, and the inner temperature was heated to 125°C. While maintaining this temperature, supply tetrafluoroethylene to the reactor so that the pressure is 0.9 MPa. In the initial stage of the reaction, use a metering pump to mix 5.5 kilograms of di-tert-butyl peroxide and 44 kilograms of methanol in the mixing tank. The mixed solution was continuously supplied at 25 L / hour for 0.5 hours, and then continuously supplied at 4.2 L / hour for 9 hours to perform a reaction.

[0056] Then, while continuously supplying tetrafluoroethylene so that the pressure in the reactor is 0.9 MPa, the solution mixed in the mixing tank at a ratio of 12 kg of di-tert-butyl peroxide ...

Embodiment 2

[0059] Manufacture of 2,2,3,4,4,4-perfluoro-1-butanol

[0060] according to figure 1 The reaction was carried out as described in the flowchart. That is to say, with a 1-meter 3 A reaction kettle made of corrosion-resistant nickel-based alloy (Hastelloy) was used as a reactor, and 170 kg (212 L) of methanol was added therein, and the inner temperature was heated to 130° C. In the initial stage of reaction, 2.8 kilograms of di-tert-butyl peroxide and 22 kilograms of methanol in the mixing tank were mixed with a metering pump to form a solution that was continuously supplied to the reactor for 0.25 hours at 25L / hour, and then continuously supplied at 4.2L / hour for 4 hours. react. At the same time, 20 kg of hexafluoropropane was continuously supplied to the reactor at a rate of 3 L / hour by a metering pump. Then, use a metering pump to mix 12 kg of di-tert-butyl peroxide with 315 kg of methanol to form a solution that is continuously supplied to the reactor at 28 L / hour, and s...

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Abstract

The present invention provides a method for producing fluorinated alkanols that can be industrially easily implemented with high selectivity. CHR1R2OH, free radical initiator and CF2=CFRf react at 105-135°C while supplying continuously, and discharge the generated H-(CFRfCF2)n-CR1R2-OH continuously. Wherein R1 and R2 are a hydrogen atom or an alkyl group with 1 to 3 carbon atoms, Rf is a fluorine atom or a polyfluoroalkyl group with 1 to 4 carbon atoms, and n is an integer of 1 to 4.

Description

technical field [0001] The present invention relates to a method for producing fluorine-containing alkanols. Background technique [0002] Fluorine-containing alkanols are useful as intermediates of water and oil repellents, surfactants, and photochromic materials (JP-A-54-154707, etc.). Since this compound is also insoluble in plastic substrates such as polycarbonate, it is also useful as a solvent for optical recording materials and pigments (JP-A-4-8585 and JP-A-5-258346). [0003] Conventionally, fluorine-containing alkanols have been produced by, for example, adding tetrafluoroethylene to methanol. Known methods include: (1) a method in which methanol, tetrafluoroethylene, and a radical initiator are charged together for heating ( No. USP2559628 specification), (2) methyl alcohol, tetrafluoroethylene and free radical initiator are dropped into reaction tower together and carry out the method for continuous reaction (USP 3022356 number specification), (3) methyl alcohol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/44C07C29/64C07C31/38
CPCC07C29/44C07C31/38
Inventor 藤间俊彦和田明宏
Owner ASAHI GLASS CO LTD
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