A method for increasing the yield of fluorine-containing alkyl ethanol

A fluorine-containing alkyl ethyl and alkyl ethanol technology is applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., to achieve the effects of short reaction time, reduced production cost and simple process

Inactive Publication Date: 2011-12-14
山东中氟化工科技有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of high cost and low yield in the above prior art, the present invention provides a more economical, higher yield production containing Fluoroalkylethanol method

Method used

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  • A method for increasing the yield of fluorine-containing alkyl ethanol

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preparation example Construction

[0022] Preparation of perfluoroalkylethyl iodide:

[0023] Add 4000g of perfluorohexyl iodide, 500g of sodium hydrosulfate, 200g of sodium bicarbonate, and 25g of sodium carbonate into a 10L stainless steel pressure-resistant reactor. Vacuumize and replace with high-purity nitrogen for 3 times. Add 1500ml of pure water and 3000ml of acetonitrile under negative pressure. Start stirring, heat up to 60°C, and continuously add ethylene. After 6 hours, the ethylene pressure in the kettle stopped dropping, and the reaction material was released, and the organic phase was separated to obtain 4880 g, with a theoretical purity of 87%.

[0024] The same method was used to prepare perfluorooctylethyl iodide with a theoretical purity of 82%.

Embodiment 1

[0026] In a 500ml four-necked flask, add 800g of prepared perfluorohexylethyl iodide, configure a water separator, a condenser, and a negative pressure device on the upper part, raise the temperature to 70-80°C, and control the negative pressure at -0.6-0.8MPa, And constantly put the raw materials brought out back into the kettle. After continuing for 4 hours, there is no longer obvious water to evaporate, and the operation is stopped, and the remaining 695g of the kettle material.

[0027] Add 600g of 20% fuming sulfuric acid in a 2L glass bottle, stir, then add 78.5g of perfluorohexylethyl iodide prepared within 1.5 hours, continue to insulate and stir for 60 minutes after adding to obtain a reaction solution; In a 2000ml flask cooled by a water bath, add 20g of sodium sulfite and 750ml of pure water, stir to dissolve. Slowly pour the black reaction solution into it, replace the heating mantle, start heating to reflux, and keep reflux for 1 hour; stop heating, replace the w...

Embodiment 2

[0031] According to the method, operation steps and process conditions of Example 1, perfluorooctyl ethyl iodide was used to prepare perfluorooctyl ethanol, and the raw materials and usage amounts listed in Table 1 were fed.

[0032] Table 1 Raw Material Feeding Table

[0033] Feeding raw material name Amount added A Perfluorooctylethyl iodide 170g B 25% oleum 750g C Na 2 SO 3 40g D Deionized water 1500ml

[0034] Finally, 115 g of perfluorooctyl ethanol was prepared with a yield of 83.7%.

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Abstract

The invention relates to the field of fluorine-containing alkyl ethanol, and provides a method for improving a fluorine-containing alkyl alcohol yield. The method comprises the following steps of removing a polar solvent and water from fluorine-containing alkyl ethyl iodide through a negative pressure water separator at a temperature of 70 to 80 DEG C under negative pressure of -0.6 to -0.8 MPa, wherein fluorine-containing alkyl ethyl iodide is produced by a solvent method, adding the fluorine-containing alkyl ethyl iodide obtained by the previous step into fuming sulphuric acid in 1.5 hours at a temperature of 90 to 100 DEG C, carrying out insulation stir for one hour, wherein a content ratio of fluorine-containing alkyl ethyl iodide to sulfur trioxide in fuming sulphuric acid is 1: (1.1to 1.6) and the content of sulfur trioxide in fuming sulphuric acid is in a range of 20 to 25%, adding the mixture obtained by the previous step into a sodium sulfite aqueous solution, wherein an amount of water is 1.25 to 2 times an amount of fuming sulphuric acid and an amount of sodium sulfite is 25.5 to 23.5% of that of fluorine-containing alkyl ethyl iodide, keeping backflow for 1 hour, and carrying out distillation and vacuum rectification to obtain fluorine-containing alkyl alcohol. The method has the characteristics of high yield, low cost, short reaction time and simple process. The method is suitable for industrialized production and iodine produced in reaction processes can be recovered and recycled.

Description

technical field [0001] The invention relates to the technical field of fluorine-containing alkyl ethanol, in particular to a method for increasing the yield of fluorine-containing alkyl ethanol. Background technique [0002] Fluorine-containing alkyl alcohol is a very important fluorine-containing chemical intermediate. It can prepare a series of surfactants, lubricants, and hydrophobic and oleophobic agents, which play a very important role in papermaking, leather industry, pharmaceutical synthesis and organic chemistry. [0003] The synthesis method for fluorine-containing alkyl ethanol is usually the hydrolysis of fluorine-containing alkyl ethyl iodide. Existing synthetic method has two kinds, and a kind of is oleum method such as publication number is the British patent of GB 994607, and this is the common method of industrial preparation fluorine-containing alkyl alcohol; A kind of is sodium nitrite method such as notification number is The Chinese patent of CN11465...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/124C07C31/38
Inventor 何日兴肖玉岭张立亭魏菁晶
Owner 山东中氟化工科技有限公司
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