Device and method for synthesizing carbonyl fluoride

A technology for synthesizing carbon and carbonyl fluoride, which is applied in the fields of fluorine chemical industry and electronic industrial gas, can solve the problems of difficult industrialization and separation, and achieve the effects of mild reaction process, increased yield and purity

Inactive Publication Date: 2016-11-16
天津长芦新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to overcome the disadvantages of the prior art or not easy to separate, or not easy to industrialize, to provide a method and device for synthesizing carbonyl fluoride

Method used

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  • Device and method for synthesizing carbonyl fluoride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1, with 60g perfluoroalkyl iodide mixture (TI-n), 75% is TI-10 (perfluorodecyl iodide), 16% is TI-12 (perfluorododecyl iodide), and the rest For TI-8 (perfluorooctyl iodide), TI-14 and (perfluorotetradecyl iodide) other trace impurities, add it to a 100ml three-necked reaction flask, and one of the ports of the reaction flask is used to communicate with the air inlet Bottle (in this embodiment is oxygen cylinder) connection, the port in the middle is used for placing thermometer, and another port is used for connecting with heating reaction tube 4, and heating reaction tube is the stainless steel ring that is 5m in length and 6mm in inner diameter in this embodiment. Spiral tube, wherein, the helical part of the spiral tube is placed in the tube furnace 5, and the straight tube part is wound with a heating belt 9 for heating to prevent perfluoroalkyl iodide condensation from blocking the pipeline.

[0033] Heat the TI-n to 150°C to make it gasify, then blow in O...

Embodiment 2

[0034] Example 2, 60g of perfluorododecyl iodide is heated to 150°C to vaporize it, then high-purity oxygen is blown in at a gas velocity of 300ml / min, the temperature of the tube furnace is 350°C, and the reaction is until the inlet pipe touches Less than TI-n liquid level. Infrared testing of a sample taken from the opening of the product collection bottle showed COF 2 The characteristic peak, the liquid in the tail gas treatment bottle is analyzed by gas chromatography to show that dimethyl carbonate is generated, which further proves that there is COF 2 Generated with a yield of 92% and a purity of 99%.

Embodiment 3

[0035] Embodiment 3, 60g perfluorooctyl iodide is heated to 150 ℃ to make it vaporize, then be the O2 / N2 mixed gas of 60% oxygen concentration with the gas velocity of 300ml / min blowing in afterwards, the temperature of tube furnace is 550 °C, react until the inlet pipe does not touch the TI-n liquid level. Infrared test shows that there is a characteristic peak of COF2, and a characteristic peak of C=C in addition, indicating that the reaction temperature is too high to produce tetrafluoroethylene, and the liquid in the tail gas treatment bottle is analyzed by gas chromatography to show that dimethyl carbonate is generated, which further proves that there is COF2 was generated with a yield of 55% and a purity of 62%.

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Abstract

The invention belongs to the fields of fluorine chemical engineering and electronic industrial gases, and particularly relates to a method and a device for synthesizing carbonyl fluoride. The method comprises the following steps of using perfluoroalkyl iodide as a raw material, and making the perfluoroalkyl iodide be in an oxygen atmosphere to obtain the carbonyl fluoride in a heating condition. The heating condition is that the heating temperature is 250 DEG C to 650 DEG C; the concentration of oxygen is 20 to 100 percent; the speed at which the oxygen is introduced is 100ml/min to 500ml/min. According to the method and the device for synthesizing the carbonyl fluoride, the perfluoroalkyl iodide is adopted as a reactant; a brand-new method is provided for producing the carbonyl fluoride; the use of strong-corrosion and high-toxicity gases of fluorine, phosgene and the like is avoided; the use of such a greenhouse gas of trifluoromethane is also avoided; a reaction process is relatively mild; a too high temperature is not needed; further, risks of explosions do not exist; crucially, gas-phase by-products of carbon dioxide or hydrogen fluoride and the like are not generated in a reaction product; the obtaining of high-purity carbonyl fluoride is facilitated.

Description

technical field [0001] The invention belongs to the fields of fluorine chemical industry and electronic industrial gas, and specifically relates to a method and a device for synthesizing carbonyl fluoride. Background technique [0002] Carbonyl fluoride (COF2) is widely used as cleaning gas and etching gas in the semiconductor manufacturing process. Due to its very low global warming potential (GWP), it has gradually replaced perfluorocarbons (PFCs) and trifluorinated Conventional cleaning and etching gases such as nitrogen (NF3), and the application of carbonyl fluoride in the field of liquid crystal manufacturing have also been reported. [0003] At present, according to the classification of the reaction raw materials, the synthesis methods of carbonyl fluoride are mainly divided into four types. [0004] 1: Carbon monoxide or carbon dioxide react with fluorine or silver difluoride [0005] Japanese Patent Laid-Open No. 11-116216, Japanese Patent Laid-Open No. 2003-2677...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00
CPCC01P2006/80
Inventor 王博张志君徐雅硕
Owner 天津长芦新材料研究院有限公司
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