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Preparation method of fluorocarbon polyether compound

A technology for polyether compounds and fluorides, applied in the field of preparation of fluorocarbon polyether compounds, can solve the problems of increased cost, high price of antimony pentafluoride, poor conversion effect, etc., and achieves excellent high temperature stability and low cost Effect

Active Publication Date: 2013-07-17
太仓中化环保化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing method is to fluorinate the by-product with equivalent or excess antimony pentafluoride to the fluorine-containing polyether containing hydrogen atoms, but the conversion effect is not very good, and antimony pentafluoride is expensive , used in large quantities, greatly increasing the cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 0.05mol C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF(CF 3 )COOH (average weight-average molecular weight 3000) and 0.005mol of antimony trifluoride dried at 200°C for 2 hours were added to a 250ml Monel alloy autoclave, vacuum-nitrogen replaced three times, and then fluorine gas containing 0.1mol of fluorine gas was added / Nitrogen (volume ratio 40 / 60) mixed gas, start stirring, heat up to 160°C within 15 minutes and react for 6 hours, then vent the autoclave, filter to remove metal fluorides, distill off low boiling point components, and the residue weighs 142.6g. Infrared detection showed that the fluorocarbon polyether carboxylic acid was completely converted into the product C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF 2 CF 3 , yield 95.1%.

Embodiment 2

[0020] 0.05mol C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF(CF 3 )COOH (average weight-average molecular weight 3000) and 0.02mol of antimony trifluoride dried at 200°C for 2 hours were added to a 250ml Monel alloy autoclave, vacuum-nitrogen replaced three times, and then fluorine gas containing 0.2mol of fluorine gas / Nitrogen (volume ratio 40 / 60) mixed gas, start stirring, heat up to 120°C within 10 minutes and react for 10 hours, vent the autoclave, filter to remove metal fluorides, distill off low boiling point components, the residue weighs 139.2g, Infrared detection showed that the fluorocarbon polyether carboxylic acid was completely converted into the product C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF 2 CF 3 , yield 92.8%.

Embodiment 3

[0022] 0.05mol C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF(CF 3 )COOH (average weight-average molecular weight 3000) and 0.006mol of silver fluoride dried at 200°C for 2 hours were added to a 250ml Monel alloy autoclave, vacuum-nitrogen replaced three times, and then fluorine / nitrogen containing 0.2mol of fluorine was added (Volume ratio 30 / 70) Mixed gas, heat up while stirring, heat up to 200°C within 20 minutes, react for 6 hours, empty the autoclave, filter to remove metal fluorides, distill off low boiling point components, and the residue weighs 143.1g , Infrared detection showed that the fluorocarbon polyether carboxylic acid was completely converted into the product C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF 2 CF 3 , yield 95.4%.

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Abstract

The invention relates to a preparation method of fluorocarbon polyether compound, which comprises the following steps that: fluorocarbon polyether carboxylic acid and metal fluoride are added into a reaction kettle, after vacuum and nitrogen replacement, excess fluorine or excess mixed gas of fluorine and inert gases are introduced into the reaction kettle, then the temperature is raised to 80-260 DEG C, after the reaction is finished, the metal fluoride is filtered and the unreacted fluorine and a small quantity of low-boiling-point impurities are removed by distillation, so that the fluorocarbon polyether compound is obtained, wherein the metal fluoride is selected from one or more of antimony trifluoride, silver fluoride and cobalt fluoride, and the feed mole ratio of the fluorocarbon polyether carboxylic acid to the metal fluoride to the fluorine is 1.0: (0.005-1): (1.1-5). Through the adoption of the preparation method, the final product can be obtained through a simple one-step reaction, no fluorocarbon polyether with hydrogen atoms is detected in the final product, and the product has excellent high-temperature stability. Compared with the prior art, on the condition that the obtained products have same high-temperature stability, the preparation method provided by the invention is simpler and is much lower in cost.

Description

technical field [0001] The invention relates to a preparation method of a fluorocarbon polyether compound. Background technique [0002] Fluorocarbon polyether is a polymer whose molecular chain only contains three elements of C, F and O. It has excellent physical, chemical and electrical insulation properties, such as high temperature thermal oxidation stability, good viscosity Electricity, low surface tension, low pour point, low volatility, chemical inertness, biological inertness, etc. Fluorocarbon polyether products can be used in many fields, such as aerospace industry, magnetic media industry, nuclear industry, oxygen industry, machinery industry, electronics industry, automobile industry, chemical industry, high temperature and high load machinery, etc. If the molecular structure of the fluorocarbon polyether contains hydrogen atoms, the stability of the product will be greatly reduced, especially the stability of the fluorocarbon polyether containing the 2-position...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/00
Inventor 吴俊浩
Owner 太仓中化环保化工有限公司
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