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Preparation method of 2H-perfluoro (2-methylpentane)

A technology of methyl pentane and methyl, applied in the field of preparation of 2H-perfluoro, can solve the problems of harsh reaction conditions, large environmental pollution, low reaction yield and the like, and achieves the effects of mild conditions and low operating costs

Pending Publication Date: 2022-03-11
浙江诺亚氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the difficult problems of harsh reaction conditions, low reaction yield and large environmental pollution in the existing technology for preparing 2H-perfluoro(2-methylpentane), and provide a kind of 2H-perfluoro(2-methylpentane) 2-Methylpentane) Preparation method

Method used

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  • Preparation method of 2H-perfluoro (2-methylpentane)
  • Preparation method of 2H-perfluoro (2-methylpentane)
  • Preparation method of 2H-perfluoro (2-methylpentane)

Examples

Experimental program
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Effect test

Embodiment 1

[0021] A 1000 ml four-necked flask is connected with a condensing reflux tube, and 100 grams of perfluoro-2-methyl-2-pentene is added in the 1000 ml four-necked flask, then 500 grams of acetonitrile and 1 gram of trimethylamine are added in acetonitrile solution (trimethylamine mass concentration 10%), cool down to 0°C, and pass through ozone at a flow rate of 500 mL / min (the concentration of ozone is 80g / m 3 ), kept for 5 hours, and stopped feeding ozone. The temperature was raised to 20°C, stirred for 2 hours, and finally directly rectified, and the fraction at 66-70°C was collected to obtain 53 grams of 2H-perfluoro(2-methylpentane) product, with a mass yield of 53%. According to gas chromatography analysis, the purity content of 2H-perfluoro (2-methylpentane) product is 99.5%.

[0022] MS (300.95, 129.5, 168.95, 168.95, 113.0, 69.05);

[0023] 1 H-NMR (CDCl 3 ):δ (ppm) 4.0(s, 1H);

[0024] 19 F-NMR (CDCl 3 ): δ (ppm) –62.061, -80.461, -111.987, -125.543.

[0025] T...

Embodiment 2

[0027] A condensing reflux tube is connected to a 1500 ml four-necked flask, and 100 grams of perfluoro-2-methyl-2-pentene is added to the 1500 ml four-necked flask, followed by 1000 grams of hydrofluoroether HFE-347 and 1 gram of triethylamine, cooled to 20°C, and passed into ozone at a flow rate of 500mL / min (the concentration of ozone is 100g / m 3 ), keep it for 2 hours, and stop feeding ozone. The temperature was raised to 50°C, stirred for 8 hours, and finally directly rectified, and the fraction at 66-70°C was collected to obtain 65 grams of 2H-perfluoro(2-methylpentane), with a mass yield of 65%. According to gas chromatography analysis, the purity content of 2H-perfluoro (2-methylpentane) product is 99.0%.

Embodiment 3

[0029] A condensing reflux tube is connected to a 1000 ml four-necked flask, and 100 grams of perfluoro-2-methyl-2-pentene is added to the 1000 ml four-necked flask, followed by 800 grams of hydrofluoroether HFE-347 and 0.8 gram of triethylamine, cooled to 10°C, and passed into ozone at a flow rate of 500mL / min (the concentration of ozone is 100g / m 3 ), keep it for 3 hours, and stop feeding ozone. The temperature was raised to 30°C, stirred for 5 hours, and finally directly rectified, and the fraction at 66-70°C was collected to obtain 68 grams of 2H-perfluoro(2-methylpentane), with a mass yield of 68%. Gas chromatography analysis shows that the purity content of 2H-perfluoro (2-methylpentane) product is 99.1%.

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Abstract

The invention discloses a preparation method of 2H-perfluoro (2-methylpentane), which comprises the following steps: adding perfluoro-2-methyl-2-pentene into a solvent with the mass being 5-10 times that of the perfluoro-2-methyl-2-pentene, adding micromolecular organic amine, uniformly stirring to form a reaction solution, cooling to 0-20 DEG C, introducing ozone into the reaction solution, keeping for 2-5 hours, and stopping introducing the ozone; and heating to 20-50 DEG C, stirring to react for 2-8 hours, directly rectifying the reaction liquid, and collecting the fraction at 66-70 DEG C to obtain the 2H-perfluoro (2-methylpentane) product. The method disclosed by the invention has the technical advantages of mild reaction conditions, high reaction yield, small environmental pollution and the like.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of 2H-perfluoro(2-methylpentane). Background technique [0002] 2H-perfluoro(2-methylpentane), CAS No.: 30320-28-6, is a perfluorinated liquid compound with high stability at room temperature, transparent and colorless, with high dielectric constant, ideal chemical inertness, advanced Excellent electrical conductivity, and excellent system matching compatibility. It can be applied to various temperature-controlled heat dissipation systems, immersion phase liquid cooling of data center servers, cooling and cooling in various links of semiconductor manufacturing (such as wafer manufacturing cooling machines, etc.), high-speed train power supply inverters, lithium-ion powered vehicles Cooling and temperature control, nuclear power, UHV power grid and military radar system, cooling and heat dissipation of heat dissipation system for internal heating co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/00C07C19/08
CPCC07C17/00C07C19/08
Inventor 蒋成君张向阳单长领张悦
Owner 浙江诺亚氟化工有限公司