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Preparation method of perfluoroalkyl ethyl alcohol

A technology of perfluoroalkyl ethyl alcohol and perfluoroalkyl iodoethane, which is applied in the field of preparation of perfluoroalkyl ethyl alcohol and can solve problems such as difficult reaction control

Inactive Publication Date: 2010-10-20
SHANGHAI 3F NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And excessive oleum is beneficial to increase the yield of perfluoroalkyl ethyl alcohol, but the consequence of excessive oleum is that the waste acid treatment after the reaction has become an issue that has to be considered in industrialization
In addition, the existing mixing of fuming sulfuric acid (such as the reaction method of perfluoroalkyl iodide and fuming sulfuric acid disclosed in U.S. Patent No. 3,283,012) is prone to foaming, which makes the reaction control more difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 100g of perfluoroalkyliodoethane was added dropwise to 300g of 25% oleum at 65°C, and then heated to 100°C for 2 hours of reaction. Only a small amount of foam was generated during the heating process. Then add 500 ml of deionized water dropwise in the ice-salt bath to dilute. with 5% Na 2 SO 3 The solution is decolorized, and then the reaction product is precipitated and separated, and the precipitated product is moved into a reaction flask with a water separator and a reflux condenser, and 1L of deionized water is added and heated to boiling, and two-phase separation occurs in the reactor as the temperature rises , After reflux for 1 hour, the oil layer was collected in the separator, the yield was 87%, and the system was colorless.

Embodiment 2

[0047] 100g of perfluoroalkyliodoethane was added dropwise to 300g of 25% oleum at 70°C, and then heated to 100°C for 2 hours of reaction. Only a small amount of foam was produced during the heating process. Then add 500 ml of deionized water dropwise in the ice-salt bath to dilute. with 5% Na 2 SO 3 The solution is decolorized, and then the reaction product is precipitated and separated, and the precipitated product is moved into a reaction flask with a water separator and a reflux condenser, and 1L of deionized water is added and heated to boiling, and two-phase separation occurs in the reactor as the temperature rises , After reflux for 1 hour, the oil layer was collected in the separator, the yield was 89%, and the system was colorless.

Embodiment 3

[0049] 100g of perfluoroalkyl iodoethane was added dropwise to 200g of 25% oleum at 65°C, and then the temperature was raised to 100°C for 2 hours of reaction. Only a small amount of foam was produced during the heating process. Then add 500 ml of deionized water dropwise in the ice-salt bath to dilute. with 5% Na 2 SO 3 The solution is decolorized, and then the reaction product is precipitated and separated, and the precipitated product is moved into a reaction flask with a water separator and a reflux condenser, and 1L of deionized water is added and heated to boiling, and two-phase separation occurs in the reactor as the temperature rises , and then refluxed for 1 hour, the oil layer was collected in the separator, the yield was 56%, and the decomposition of unreacted perfluoroalkylethyl iodide caused the system to turn red.

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Abstract

The invention discloses a method for preparing perfluoroalkyl ethyl alcohol with perfluoroalkyl ethyl iodide, which comprises the following steps: (a) fuming sulphuric acid and the perfluoroalkyl ethyl iodide are mixed at 55-75DEG C, thus obtaining premixed reactants; (b) the premixed reactants are heated to 130DEG C at most to ensure the fuming sulphuric acid to react with the premixed reactants of the perfluoroalkyl ethyl iodide, thus forming sulfate; and (c) hydrolysis is carried out and the perfluoroalkyl ethyl alcohol is separated.

Description

technical field [0001] The present invention relates to a method for preparing perfluoroalkyl ethyl alcohol from perfluoroalkyl iodoethane. The preparation of perfluoroalkyl ethyl alcohol by the method of the invention has the advantage of high yield. Background technique [0002] The practical value of fluorine-containing alcohols with a long carbon chain structure depends on the unique hydrophobic and oil-repellent properties of the perfluoro or polyfluoroalkyl chains contained in them. Carbon polymers have been widely used. [0003] The long carbon fluorine-containing chain structure can be obtained by electrolytic fluorination, tetrafluoroethylene-methanol telomerization and alkyl iodide-tetrafluoroethylene telomerization. Among them, the alkyl iodide-tetrafluoroethylene telomerization method has become the preferred method for preparing perfluoro long-carbon linear structures. [0004] Since the iodine atom is directly connected to the strong electron-withdrawing gro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/38C07C29/12
Inventor 冯东东粟小理胡根祥顾文怡
Owner SHANGHAI 3F NEW MATERIAL
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