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Novel disposal method for fluorine-containing acylfluoride analog compound

A treatment method and technology of amine compounds, applied in organic chemistry, preparation of carboxylic acid halides, etc., can solve the problems of workers’ health, surrounding environmental pollution, difficulty in recrystallization and purification, poor post-processing adaptability, etc., and achieve environmental protection problem, easy handling, and stable performance

Active Publication Date: 2007-09-19
SANMING HEXAFLUO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Another major defect of the prior art is that a large amount of reaction heat is released during hydrolysis, which also makes higher requirements on the heat exchange capacity of the treatment equipment. If the heat exchange capacity is insufficient, acid waste gas containing hydrogen fluoride will be generated, which will affect the operation. health of workers and pollution of the surrounding environment
[0006] Another major defect of the prior art is that fluorine-containing carboxylic acids or their salts have poor adaptability to further post-treatment, which is embodied in the fact that fluorine-containing carboxylic acids have a high boiling point and are difficult to distill and purify. There is little difference in the solubility of the salt, and it is difficult to recrystallize and purify

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The present invention processes a fluorine-containing acyl fluoride compound (perfluorooctanoyl fluoride) by the following method:

[0036] 1. In a reactor with a stirrer, add 32 kg of methanol, and slowly add 79 kg of pyridine under stirring to mix the two evenly to obtain a mixture of methanol and pyridine;

[0037] 2. Transfer the mixture of methanol and pyridine obtained above into a closed reactor with stirrer. At room temperature of 0°C, start stirring, and slowly add 400 kg of perfluorooctanoyl fluoride to the mixture of methanol and pyridine in a dropwise manner, and continue stirring for 2 hours after the addition is complete;

[0038] 3. the reaction product obtained above is transferred to a tower still of a rectifying tower with a theoretical plate number of 60, rectifying, and obtains 395 kilograms of perfluorooctanoic acid methyl esters (about 96% yield), and reclaims 115 in the tower still The kilogram mixture, mainly the complex of pyridine and hydrogen...

Embodiment 2

[0040] The present invention processes a fluorine-containing acyl fluoride compound (trifluoroacetyl fluoride) by the following method:

[0041] 1. In a reaction kettle with a stirrer, add 32 kilograms of methyl alcohol, under stirring, slowly add 185 kilograms of tri-n-propylamine, make the two mix uniformly, obtain the mixture of methanol and tri-n-propylamine;

[0042] 2. The mixture of methanol and tri-n-propylamine obtained above is transferred to the raw material tank of a closed tube reaction system with a magnetic pump and a Venturi tube. At room temperature of 30°C, start the magnetic pump to circulate the mixture of methanol and tri-n-propylamine in the tubular reaction system, then open the valve of the acyl fluoride feed pipe, and slowly add 110 kg of trifluoroacetyl fluoride to the tubular reaction system In a mixture of methanol and tri-n-propylamine. Continue to circulate for 1 hour after adding;

[0043] 3. the reaction product obtained above is transferred t...

Embodiment 3

[0045] The present invention processes the mixture of two fluorine-containing acyl fluoride compounds (trifluoroacetyl fluoride and fluorophosgene) by the following method:

[0046] 1. In a reaction kettle with a stirrer, add 58 kg of propylene alcohol, and slowly add 31 kg of methylamine under stirring, so that the two are evenly mixed to obtain a mixture of propylene alcohol and methylamine;

[0047] 2. The mixture of propylene alcohol and methylamine obtained above is transferred to the raw material tank of a closed tower reaction system with magnetic pump and heater, and the moment saddle ring packing of PVDF is filled in the tower reactor. Start the magnetic pump to circulate the mixture of allyl alcohol and methylamine in the tower reaction system at 60°C. Then open the valve of the acyl fluoride feed pipe, and slowly add 90 kg of a 1:1 (molar ratio) mixture of trifluoroacetyl fluoride and fluorophosgene into the tower reaction system. Continue to circulate for 1 hour a...

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Abstract

The new acyl fluoride compound treating process includes the following steps: 1. mixing one kind of alcohol compound and one kind of amine compound in advance; 2. adding the acyl fluoride into the mixing of alcohol compound and amine compound for reaction; and 3. rectifying the reaction products in rectifying tower to obtain purified ester compound of corresponding fluorine containing carboxylic acid while recovering complex of hydrogen fluoride and amine compound. The treating process makes produced hydrogen fluoride become complex with less corrosion and the complex is one kind of chemical reagent with wide application. The ester compound has simple post-treatment. In addition, the present invention has relatively relaxed requirement in the treating apparatus and no environmental pollution problem.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and relates to a new treatment method for some fluorine-containing acyl fluoride compounds which are intermediate products in the production process of organic fluorine chemicals. Background technique [0002] In the manufacturing process of organic fluorine chemicals, some fluorine-containing acyl fluoride compounds are often produced as intermediates in the process. For example, perfluorooctanoyl fluoride is first produced when electrolytic fluorination is used to prepare perfluorooctanoic acid, and trifluorooctanoyl fluoride is first produced when electrolytic fluorination is used to prepare trifluorooctanoyl fluoride. When acetic acid is used, trifluoroacetyl fluoride is first produced. When perfluoropropoxy vinyl ether is prepared, perfluoropropoxypropionyl fluoride is first synthesized. When perfluoropropylene oxide is synthesized, trifluoroacetyl fluoride and fluorophosgene are produced. (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/14C07C69/02C07C69/34C07C69/52C07C53/46C07C53/48C07C53/50C07C55/40
Inventor 曹伟吕涛张威朱吉洪
Owner SANMING HEXAFLUO CHEM CO LTD