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Method for synthesizing halogenated alkanes

A synthesis method and technology of halogenated alkanes, which are applied in the fields of halogen addition preparation, organic chemistry, etc., can solve the problems of no strong oil resistance, solvent resistance, weather resistance, high and low temperature resistance, unsatisfactory, small bond energy, etc. The raw materials are easily available, the operation is simple, and the reaction process is stable.

Active Publication Date: 2013-07-31
JINZHOU DPF TH CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the small carbon-hydrogen bond energy of hydrocarbon alkane containing dibromine and diiodide, it does not have strong oil resistance, solvent resistance, weather resistance, high and low temperature resistance, etc., so its application is limited and cannot meet the rapid development of industry. Require

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 500g of bromine, 260g of tetrafluoroethyltetrafluoropropyl ether, and 5g of antimony pentafluoride in a 1L high-pressure reactor equipped with stirring, electric heating, thermocouple, cooling coil, and pressure display instrument after evacuating and replacing oxygen. Use tetrafluoroethylene to prepare a pressure of 0.1Mpa, heat the material in the reactor to 150°C, use tetrafluoroethylene to increase the pressure to 0.8Mpa and reduce the pressure to 0.7Mpa for supplementary pressure, and measure and consume 350g of tetrafluoroethylene after 3 hours of reaction. After the reaction material was cooled to 35°C, the unreacted bromine was recovered, and 771 g of the product was obtained after rectification under reduced pressure, with a yield of 95%. The purity of the product was analyzed by liquid chromatography to be 99.6%. The obtained compound was confirmed by infrared spectroscopy to have Br(CF 2 -CF 2 ) Structure of Br.

Embodiment 2

[0014] Add 400g of bromine, 200g of tetrafluoroethyl tetrafluoropropyl ether, and 4g of antimony pentafluoride in the 1L high-pressure reactor equipped with stirring, electric heating, thermocouple, cooling coil, and pressure display instrument to evacuate and replace the oxygen. , use tetrafluoroethylene to prepare the pressure to 0.6Mpa, heat the material in the reactor to 200°C, use tetrafluoroethylene to increase the pressure to 1.6Mpa and reduce the pressure to 1.5Mpa for supplementary pressure, and measure and consume 480g of tetrafluoroethylene after 5 hours of reaction After cooling the reaction material to 40°C, the unreacted bromine was recovered, and 655g of the product obtained after separation by vacuum distillation, the yield was 91%, and the purity was 99.5% by liquid chromatography analysis. The obtained compound was confirmed by infrared spectroscopy to have Br(CF 2 -CF 2 ) The structure of 2Br.

Embodiment 3

[0016] After the 1L high-pressure reactor equipped with stirring, electric heating, thermocouple, cooling coil, and pressure display instrument was evacuated to replace oxygen, 100g of iodine, 300g of dimethylaniline, 5g of antimony pentafluoride, and tetrafluoroethylene were added. Prepare the pressure to 0.1Mpa, heat the material in the reaction kettle to 230°C, pressurize it to 1.8Mpa with tetrafluoroethylene, wait for the pressure to drop to 1.6Mpa, and add it. After 8 hours of reaction, measure and consume 300g of tetrafluoroethylene. After cooling to 30°C, the unreacted bromine was recovered, and 316 g of the product was obtained after vacuum distillation and separation, with a yield of 94.8%, and a product purity of 99.6% by liquid chromatography analysis. The obtained compound was determined to have I(CF 2 -CF 2 ) The structure of 6I.

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PUM

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Abstract

The invention discloses a method for synthesizing halogenated alkanes, which comprises the following steps of: adding 20 to 30 weight parts of solvent and 0.3 to 0.8 weight part of catalyst into 10 to 60 weight parts of halogens and 26 to 48 weight parts of fluorine-containing olefins, which serve as major ingredients, wherein the halogens may be a bromine simple substance or an iodine simple substance, the solvent is dimethylaniline or tetrafluoroethyl tetrafluoropropyl ether, and the catalyst is antimony pentafluoride; and reserving the pressure to between 0.05 and 0.6 MPa by using the olefins, heating to the temperature of between 150 and 230 DEG C, and reacting under the pressure of between 0.7 and 1.8 MPa for 3 to 8 hours, cooling to the temperature of between 30 and 40 DEG C, recovering unreacted raw materials, and rectifying under the reduced pressure to obtain a target product. In the method, the raw materials are readily available, and by-products are not generated; the process can be controlled, and the integral reaction process is stable and is easy and convenient to operate, so the method has the special advantage on a reaction process, and the product obtained finally has the purity of up to over 99.5 percent and yield of up to over 91 percent and can be used as the raw materials of fluorine-containing materials which are used for synthesizing fluororubber resistant to the temperature of between -50 and 260 DEG C and have stable chemical performance.

Description

technical field [0001] The invention relates to a method for synthesizing halogenated alkanes. Background technique [0002] Alkanes containing dibromine and diiodide have active agent groups that can react and can retain a bromine and iodine group at the same time, so they are widely used in technical fields such as special fluororubbers, fluorine-containing medicines, and fluorine-containing intermediates. Due to the small carbon-hydrogen bond energy of hydrocarbon alkane containing dibromine and diiodide, it does not have strong oil resistance, solvent resistance, weather resistance, high and low temperature resistance, etc., so its application is limited and cannot meet the rapid development of industry. Require. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for synthesizing halogenated alkanes with strong oil resistance, solvent resistance, weather resistance and high and low temperature resistan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/04C07C19/14C07C19/16
Inventor 魏潇杨碧祥孙百开
Owner JINZHOU DPF TH CHEM CO LTD
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