Method for preparing fluorine-containing sodium alkyl alcohol

A technology of fluorine-containing alkyl alcohol and alkyl alcohol, which is applied in the field of preparation of sodium fluorine-containing alkyl alkoxide solution, can solve the problems of more energy consumption and cost increase, and achieve the effect of increasing post-processing steps and saving production costs

Inactive Publication Date: 2009-10-28
山东中氟化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, although it is known that sodium fluorine-containing alcohols can be prepared by reacting metal sodium and fluorine-containing alkyl alcohols, the existing methods all need to use solvents, and the separation of solvents and fluorine-containing alkyl alcohols will consume more More energy, so that the cost is greatly increased

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2376g (18mol) of tetrafluoropropanol into a 2L four-necked flask, protect it with nitrogen, and stir mechanically (rotating speed 500r / min), and the treated sodium metal (peeled, cut into about 5×5×5mm Particles) were added to the flask, sodium metal was added in 10 batches, each time adding 9.2g (total 4mol). Wait until the sodium metal has completely disappeared before adding the next batch. The reaction temperature is 70-80°C, and the sodium metal is consumed after 23 hours of reaction. The theoretical solution concentration is about 25% by calculation; the measured value is 24.2%.

Embodiment 2

[0021] Add 2376g (18mol) of tetrafluoropropanol into a 2L four-necked flask, protect it with nitrogen, and stir it mechanically (rotating speed 500r / min). The processed sodium metal (peeled, cut into pieces with a size of about 5×5×5mm) Particles) were added to the flask, and sodium metal was added in 10 batches, adding 9.2 g each time, (a total of 4 mol). Wait until the sodium metal has completely disappeared before adding the next batch. The reaction temperature is 80-90°C, and the sodium metal is completely consumed after 15.5 hours of reaction. The theoretical solution concentration is about 25% by calculation; the measured value is 24.0%.

Embodiment 3

[0023] Add 2376g (18mol) of tetrafluoropropanol into a 2L four-necked flask, protect it with nitrogen, and stir it mechanically (rotating speed 500r / min). The processed sodium metal (peeled, cut into pieces with a size of about 5×5×5mm) Particles) were added to the flask, and sodium metal was added in 10 batches, adding 9.2 g each time, (a total of 4 mol). Wait until the sodium metal has completely disappeared before adding the next batch. The reaction temperature is 90-100°C, and the sodium metal is consumed after 7 hours of reaction. The theoretical solution concentration is about 25% by calculation; the measured value is 23.5%.

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Abstract

The invention relates to a method for preparing fluorine-containing sodium alkyl alcohol. The method mainly comprises the following steps that: under conditions of an inert gas atmosphere and quick stirring, crushed metal sodium particles are added into an excessive solution of fluorine-containing alkyl alcohol in batch for reaction at a temperature of between 20 portions and 110 DEG C to generate the solution of fluorine-containing alkyl alcohol, which contains sodium alcoholate; and after reaction, the concentration of the solution is detected by the alkalinity measuring method. The method has the advantages that: the excessive solution of fluorine-containing alkyl alcohol can be used as a solvent, so that other solvents are not necessarily added; and the post-treatment procedures of the separation of the added solvent and the solution of fluorine-containing sodium alkyl alcohol are also avoided, so that the production cost is saved.

Description

technical field [0001] The invention relates to a preparation method of sodium fluorine-containing alkyl alkoxide, in particular to a preparation method of sodium fluorine-containing alkyl alkoxide solution. Background technique [0002] Sodium fluorine-containing alkyl alkoxide solution is an important, commonly used chemical in synthetic reactions and manufacturing processes that require strong organic fluorine-containing bases. There are many methods for preparing sodium alkoxide by alkalinization with sodium or sodium compounds. For example, U.S. Patent 3702833 proposes to reflux heating fluorine-containing alcohol and metal sodium in tetrahydrofuran. Depending on the amount of alcohol used, this reaction can be carried out to various degrees. By generating sodium fluoride and observing that the alkalinity of the medium is lower than expected value, indicating that degradation has occurred. US Patent No. 4,357,458 proposes to carry out sodium alkalization with sodium h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/38C07C31/30C07C29/70
Inventor 肖玉岭张立亭
Owner 山东中氟化工科技有限公司
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