Method for preparing high-purity perfluoroisobutyronitrile

A technology of perfluoroisobutyronitrile and fluorine-containing olefins, which is applied to the purification/separation of carboxylic acid nitriles, organic chemistry, reagents, etc., can solve the problems of equipment and operator damage and injury, and achieve stable and reliable preparation process and high product quality. High yield, reasonable and simple process

Active Publication Date: 2019-12-03
泉州宇极新材料科技有限公司
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  • Claims
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Problems solved by technology

Chinese patent application "preparation method of perfluoronitrile" (CN108424375A) discloses the preparation of heptafluoroisobutyronitrile, which uses carbonyl fluoride and perfluoroalkene gas phase catalysis to obtain acid fluoride, and then amination and dehydration to obtain perfluoronitrile, the product Part of the fluorine-containing olefins present in the chemical is toxic and corrosive to a certain extent, if not removed, it will cause damage and injury to the equipment and operators
At present, there are few reports about the purification method for preparing high-purity perfluoroisobutyronitrile, so it is particularly important to provide a separation and purification method with simple process, high safety factor, high product yield and low operating cost.

Method used

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  • Method for preparing high-purity perfluoroisobutyronitrile
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  • Method for preparing high-purity perfluoroisobutyronitrile

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Embodiment 1

[0025] Pass 3 kg of crude perfluoroisobutyronitrile with a purity of 88% into a single-stage stainless steel adsorption tower at a rate of 0.2 L / min. The adsorption temperature is 25° C., the adsorption pressure is 0.1 MPa, the adsorbent is 5A molecular sieve, and the molecular sieve loading capacity is 10 kg. Collect the adsorbed perfluoroisobutyronitrile into the still of the rectification tower, a total of 2.7kg, adjust the rectification temperature to 10°C, and the pressure inside the tower to 0.03MPa. The flow rate of min is to discharge the former fraction. Use GC-PDHID gas chromatograph to analyze the purity of the fractions, and collect the fractions into the product gas storage tank after the purity is greater than 99.99%. The finished gas was filled into steel cylinders for storage by using a diaphragm compressor with a filling factor of 1.0, and finally 2.15 kg of purified product was obtained with a total yield of 81.6%.

Embodiment 2

[0027] Pass 3kg of crude perfluoroisobutyronitrile with a purity of 92% into a single-stage stainless steel adsorption tower at a rate of 0.5L / min, the adsorption temperature is 15°C, the adsorption pressure is 0.08MPa, the adsorbent is 10X molecular sieve, and the molecular sieve filling capacity is 8kg. Collect the adsorbed perfluoroisobutyronitrile into the still of the rectification tower, a total of 2.7kg, adjust the rectification temperature to 15°C, and the pressure inside the tower to 0.05MPa. The flow rate of min is to discharge the former fraction. Use GC-PDHID gas chromatograph to analyze the purity of the fractions, and collect the fractions into the product gas storage tank after the purity is greater than 99.99%. The finished product gas was filled into steel cylinders for storage by using a diaphragm compressor with a filling coefficient of 0.8, and finally 2.38 kg of purified product was obtained with a total yield of 86.1%.

Embodiment 3

[0029] Pass 3kg of crude perfluoroisobutyronitrile with a purity of 95% into a single-stage stainless steel adsorption tower at a rate of 1L / min, the adsorption temperature is 5°C, the adsorption pressure is 0.03MPa, the adsorbent is NaY molecular sieve, and the molecular sieve filling capacity is 5kg. Collect the adsorbed perfluoroisobutyronitrile into the still of the rectification tower, a total of 2.8kg, adjust the rectification temperature to 5°C, and the pressure inside the tower to 0.01MPa. The flow rate of min is to discharge the former fraction. Use GC-PDHID gas chromatograph to analyze the purity of the fractions, and collect the fractions into the product gas storage tank after the purity is greater than 99.99%. The finished product gas is filled into steel cylinders for storage by using a diaphragm compressor with a filling coefficient of 0.5, and finally 2.44 kg of purified product is obtained with a total yield of 85.6%.

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Abstract

The invention discloses a method for preparing high-purity perfluoroisobutyronitrile. The method comprises the steps that the raw material perfluoroisobutyronitrile passes through a single-stage adsorption tower at a certain flow rate under a certain temperature and pressure by using a mass flowmeter; and after most water and a small amount of acidic matter are adsorbed and removed, the raw material perfluoroisobutyronitrile enters a rectifying tower, then batch rectification is carried out at a low temperature, and impurities such as nitrogen, oxygen, carbon dioxide, carbon monoxide, halogenated alkane, halogenated olefin and fluorocarbon are removed by emptying the tower top, so that the high-purity perfluoroisobutyronitrile with the purity of more than 99.99% is obtained. The method isreasonable in process and simple to operate, and is an ideal technology for preparing the high-purity perfluoroisobutyronitrile.

Description

technical field [0001] The invention belongs to the technical field of refining and purifying fluorine-containing organic compounds, and in particular relates to a purification process of high-purity perfluoroisobutyronitrile. Background technique [0002] Perfluoroisobutyronitrile is an environmentally friendly insulating gas that can be used in electrical insulation switchgear. The mixed gas of perfluoroisobutyronitrile has excellent insulation and arc extinguishing properties, and is compatible with the materials in the switch. It has low toxicity, no flash point, meets health and safety requirements, has a wide temperature range, is environmentally friendly, and has ozone destruction potential. (ODP) is zero and Greenhouse Potential (GWP) is only SF 6 one-tenth of. [0003] Since the production process of perfluoroisobutyronitrile is relatively complicated, the crude product of perfluoroisobutyronitrile often contains various impurities. Chinese patent application "pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/34C07C255/10
CPCC07C253/34C07C255/10Y02P20/151
Inventor 董利庆飞要贾晓卿马晓迅
Owner 泉州宇极新材料科技有限公司
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