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A kind of preparation method of sodium fluorine-containing alkyl alkoxide

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: 2011-12-28
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 preparation method of sodium fluorine-containing alkyl alkoxide, which mainly includes the following steps: adding crushed metal sodium particles into excess fluorine-containing alkyl alcohol solution in batches under an inert gas atmosphere and rapid stirring, The reaction is carried out at 20-110°C to generate a fluorine-containing alkyl alcohol solution containing sodium alkoxide, and the concentration of the solution is determined by measuring the alkalinity after the reaction is completed. The beneficial effect of the present invention is: excessive fluorine-containing alkyl alcohol can play the role of solvent, so do not need to add any other solvent, also avoid adding solvent and increase the separation of solvent and fluorine-containing alkyl alkoxide sodium solution, after adding processing steps, saving production costs.

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 Patents(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