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Preparation method of perfluorinated alkyl ethyl bromide

A technology of perfluoroalkyl ethyl and hexadecyl triethyl ammonium bromide, applied in halogen substitution preparation, organic chemistry and other directions, can solve the problem of high reaction temperature and pressure, high reaction equipment requirements and complex preparation process and other problems, to achieve the effects of mild reaction conditions, good product purity, and safe and easy-to-obtain raw materials

Active Publication Date: 2014-03-05
灏怡(海南)投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production method of perfluoroalkyl ethyl bromide is: under the condition of high temperature and high pressure, it is prepared by the bromination reaction of elemental bromine and perfluoroalkyl ethyl iodide, but the method has the following problems: 1) the reaction temperature and The pressure is high, the reaction conditions are harsh, and the process safety is poor; 2) The raw material bromine used and the iodine bromide in the product are highly corrosive and toxic substances, which require high reaction equipment, which is not conducive to production operations and pollution The environment is severe; 3) The post-treatment process requires multiple steps such as iodine reduction, separation, neutralization, washing, and distillation, and the preparation process is complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 346g (1mole) of perfluorobutylethyl iodide, 231g of tetraethylammonium bromide (1.1mole) and 400mL of acetone to a 2L four-necked flask equipped with mechanical stirring, temperature measuring point, and reflux condenser, and heat to Reflux, react at 55°C~60°C for 3 hours, filter to remove the solid, and remove the solvent acetone by rotary evaporation (the evaporated acetone is recovered and reused, and can continue to be used as a solvent for the preparation of perfluorohexylethyl bromide), in the system Pressure -0.096MPa~-0.095MPa, heating temperature 80°C~85°C, carry out vacuum distillation and purification to obtain 326g of colorless and transparent liquid perfluorobutyl ethyl bromide, the purity of gas chromatography is 99.5%, and the yield is 99.2 %.

Embodiment 2

[0015] Add 446g (1mole) of perfluorohexyl iodide, 265g of benzyltrimethylammonium bromide (1.15mole) and 450mL of acetone into a 2L four-neck flask equipped with mechanical stirring, temperature measuring point, and reflux condenser, and heat to reflux , after reacting at 55°C~60°C for 4 hours, filter to remove the solid, and remove the solvent acetone from the liquid by rotary evaporation (the evaporated acetone is recovered and reused, and can continue to be used as a solvent for the preparation of perfluorohexylethyl bromide), at system pressure -0.097MPa~-0.096MPa, at a heating temperature of 85°C~90°C, carry out distillation and purification under reduced pressure to obtain 425g of perfluorohexylethyl bromide as a colorless and transparent liquid, with a purity of 99.3% and a yield of 98.9% by gas chromatography.

Embodiment 3

[0017] Add 546g (1mole) perfluorooctyl ethyl iodide and 354g dodecyltrimethylammonium bromide (1.15mole) and 500mL Acetone, heated to reflux, reacted at 55°C~60°C for 5 hours, filtered to remove the solid, and the liquid was removed by rotary evaporation to remove the solvent acetone (the evaporated acetone can be recovered and reused, and can continue to be used as a solvent for the preparation of perfluorohexylethyl bromide ), at a system pressure of -0.098MPa~-0.097MPa, and a heating temperature of 90°C~95°C, carry out distillation and purification under reduced pressure to obtain 524g of white solid perfluorooctylethyl bromide, the purity of which was detected by gas chromatography was 99.2%. The rate is 98.7%.

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Abstract

The invention discloses a preparation method of perfluorinated alkyl ethyl bromide. According to the preparation method, perfluorinated alkyl ethyl iodine and quaternary ammonium salt serve as reaction substrates, wherein the quaternary ammonium salt is one of tetraethylammonium bromide, benzyltrimethylammonium bromide, dodecyltrimethylammonium bromide and cetyltriethylammonium bromide, and acetone serves as a solvent. The preparation method comprises the following steps of: performing halogen substitution reaction on the materials for 3 to 5 hours under a heating backflow condition; filtering the materials to remove the solvent after the reaction; and performing reduced pressure distillation and purification on the materials to obtain the perfluorinated alkyl ethyl bromide. According to the preparation method, the raw materials are safe and easy to get, the production process is simple, the reaction conditions are mild, the needed temperature is low, and substances with strong corrosiveness and strong toxicity are prevented from being used and produced in the production process so as to ensure the safety and environment friendliness in the production.

Description

technical field [0001] The invention belongs to the field of perfluoro compounds, in particular to a preparation method of perfluoroalkyl ethyl bromide. Background technique [0002] Perfluoroalkyl ethyl bromide (also known as perfluoroalkyl ethyl bromide, the general formula is R f CH 2 CH 2 Br, where R f It is a straight-chain perfluoroalkyl group with a carbon number of 4~) is the basic raw material for the production of fluorine-containing surfactants, fabric finishing agents and other fluorine-containing fine chemicals, and is an important organic fluorine intermediate, widely used in chemistry, machinery , textile and paper industries, as well as ink coatings and fire protection. [0003] At present, the production method of perfluoroalkyl ethyl bromide is: under the condition of high temperature and high pressure, it is prepared by the bromination reaction of elemental bromine and perfluoroalkyl ethyl iodide, but the method has the following problems: 1) the react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/14C07C17/20
Inventor 魏奇谷峰魏潇
Owner 灏怡(海南)投资有限公司
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