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Method for preparing 1-bromo-2-iodotetrafluoroethane

A technology of iodotetrafluoroethane and tetrafluoroethylene is applied in the field of manufacturing fluorine-containing alkyl iodides, can solve the problems of restricted application, high price, etc., and achieves low price, high product selectivity, easy separation and purification. Effect

Active Publication Date: 2013-02-27
CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, only a few companies at home and abroad can provide 1-bromo-2-iodotetrafluoroethane with a purity of about 97%, and the price is very high, which seriously restricts its application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0027] The preparation method involved in the present invention can also be like this:

[0028] Add quantitative solid iodine bromide to the reaction system, seal the reaction system and replace it with an inert gas to make the system a dry and oxygen-free system, and add quantitative fluorine-containing halogenated alkane or hydrogen-containing fluorine-containing halogenated alkane solvent under vacuum conditions; The temperature of the system rises to 50-80°C, preferably 70-80°C, and then 0.1-2.0MPa tetrafluoroethylene gas, preferably 0.5-1.0MPa tetrafluoroethylene gas, is introduced to keep the reaction temperature at 70-80°C until the end of the reaction; After reaching room temperature, replace the unreacted tetrafluoroethylene gas with nitrogen, distill off the reaction product, and rectify to obtain the finished product of 1-bromo-2-iodotetrafluoroethane.

Embodiment 1

[0036] Add 2.0kg of solid iodine into a 5L fluorine-lined stainless steel reactor, close the reaction system and replace it with high-purity nitrogen after vacuuming to make the system dry and anaerobic, and add 1.26kg of liquid bromine and 2LCFCl under vacuum conditions 2 CFCl 2Solvent; raise the temperature of the reaction system to 40°C, stir and react for 2 hours; raise the temperature of the reaction system to 50°C and continuously feed 0.2MPa tetrafluoroethylene gas, and keep the reaction temperature at 70-75°C until the end of the reaction; the temperature drops to After room temperature, the unreacted tetrafluoroethylene gas was replaced with nitrogen, the liquid phase reaction product was distilled off, and rectified to obtain 1.73 kg of 1-bromo-2-iodotetrafluoroethane product with a purity of 95.6%. Based on the actual collected products, the yield of 1-bromo-2-iodotetrafluoroethane was 34.24%, and the selectivity was 69.4%.

Embodiment 2

[0038] Add 2.0kg of solid iodine into a 5L fluorine-lined stainless steel reactor, close the reaction system and vacuumize it, and replace it with high-purity nitrogen to make the system dry and anaerobic. Add 1.26kg of liquid bromine and 2LCF under vacuum 2 ClCCl 3 Solvent; raise the temperature of the reaction system to 80°C, stir and react for 3 hours; raise the temperature of the reaction system to 55°C and continuously feed 0.8MPa tetrafluoroethylene gas, and keep the reaction temperature at 70-75°C until the end of the reaction; the temperature drops to After room temperature, the unreacted tetrafluoroethylene gas was replaced with nitrogen, the liquid phase reaction product was distilled off, and rectified to obtain 1.91 kg of 1-bromo-2-iodotetrafluoroethane product with a purity of 95.5%. Based on the actual collected products, the yield of 1-bromo-2-iodotetrafluoroethane was 37.76%, and the selectivity was 71.2%.

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Abstract

The invention discloses a method for preparing 1-bromo-2-iodotetrafluoroethane. In the method, under the existence of organic solvent or absence of solvent, tetrafluoroethylene and iodine bromide are subjected to gas-liquid phase reaction under the initial reaction temperature of 50 DEG C to 80 DEG C and the tetrafluoroethylene gas pressure of 0.1MPa to 2.0MPa, so that the 1-bromo-2-iodotetrafluoroethane is produced, and the organic solvent is C2-C4 fluorine-containing halogenated hydrocarbon or C2-C4 hydrogen fluorin-containing halogenated hydrocarbon, the boiling point of which is higher than the boiling point of the 1-bromo-2-iodotetrafluoroethane. The product selectivity of the method is high, and the product is easy to separate and purify. The purity is about 97 percent, and the price is relatively low.

Description

technical field [0001] The invention relates to a method for preparing fluorine-containing alkyl iodides, in particular to a method for preparing 1-bromo-2-iodotetrafluoroethane. Background technique [0002] Fluorine-containing alkyl iodides are an important class in the family of organic fluorides. They are intermediates for the synthesis of many organic fluorides. The widely used downstream fine chemicals can be obtained from fluorine-containing alkyl iodides through a series of substitution reactions. , and its downstream fluorine-containing alkyl compounds will also be endowed with excellent physical and chemical properties such as high thermal stability, high chemical stability, and high surface activity. [0003] Fluorine-containing alkyl iodides are also easy to undergo addition reactions with monomers such as tetrafluoroethylene, vinylidene fluoride, and hexafluoropropylene to form fluorine-containing alkyl iodide adducts. In the products, the iodine atom is no long...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/16C07C17/04
Inventor 王益王其明沈德新陈志刚龙湘犁钱刚
Owner CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS
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