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Process for Purifying Nitrogen-Fluoride

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Process for Purifying Nitrogen-Fluoride Europaisches Patentamt 19 European Patent Office Office europeen des brevets © Publication number: 0 345 354 B1 12 EUROPEAN PATENT SPECIFICATION @ Date of publication of patent specification © int. ci.5: F25J 1/00, F25J 3/02, 03.02.93 Bulletin 93/05 C01B 21/083 (2j) Application number: 88909616.0 (22) Date of filing : 04.11.88 (86) International application number : PCT/JP88/01120 @ International publication number : WO 89/04444 18.05.89 Gazette 89/11 (S) Process for purifying nitrogen-fluoride. @ Priority: 04.11.87 JP 277514/87 @ Inventor: HYAKUTAKE, Hiroyuki 1541-2-3-5, Yabe-cho Totsuka-ku Yokohama-shi @ Date of publication of application Kanagawa 244 (JP) 13.12.89 Bulletin 89/50 Inventor : HARADA, Isao 7-2, Sako-machi 5-chome Hikoshima Shimonoseki-shi Publication of the of the (45) grant patent : Yamaguchi 750 (JP) 03.02.93 Bulletin 93/05 Inventor: IWANAGA, Naruyuki 7-1, Sako-machi 5-chome @ Designated Contracting States : Hikoshima Shimonoseki-shi BE CH DE FR GB IT LI NL SE Yamaguchi 750 (JP) Inventor : NISHITSUJI, Toshihiko 9-6, Sako-machi 5-chome © References cited : Hikoshima Shimonoseki-shi FR-A- 2 165 930 Yamaguchi 750 (JP) US-A- 4 078 907 (74) Representative : Schiiler, Horst, Dr. (73) Proprietor : MITSUI TOATSU CHEMICALS, Inc. Patentanwalt, Kaiserstrasse 69 2-5 Kasumigaseki 3-chome W-6000 Frankfurt/Main 1 (DE) Chiyoda-Ku Tokyo 100 (JP) CO If) CO If) CO Note : Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been LU filed until the opposition fee has been paid (Art. 99(1) European patent convention). Jouve, 18, rue Saint-Denis, 75001 PARIS EP 0 345 354 B1 Description The present invention relates to a method for preparing purified liquid nitrogen-fluoride, in particular to a method of purifying NF3 formed in the production of NF3. 5 NF3 is a colorless gas having such physical properties that the boiling point is -129 °C, and the melting point is -208 °C. Since the activity of NF3 is suitably weak as a fluorine source in comparison with fluorine (F2), and the toxi- city thereof is low, conventionally NF3 was used as a fluorine source in adjusting fluoroolef ins, and was used as an oxidizing agent of high energy fuels. Also, in recent years, NF3 as a cleaning agent for CVD apparatuses 10 in the field of electronic materials as well as as a dry etching gas for very large-scale integrated circuits has become to be used. There are many processes for the production of NF3. As major processes thereof can be mentioned, for example, a molten salt electrolytic process using an ammonium acid fluoride (U.S. Patent No. 3,235,474), a process wherein an ammonium acid fluoride in a molten state is reacted with gaseous fluorine (Japanese Pa- rs tent Publication No. 8926/1980), and a process wherein an ammonium complex of a metal fluoride in the solid state is reacted with F2 in the elemental state (Japanese Patent Publication No. 21724/1987). In any of these processes, in the reaction step of producing NF3, it is required that an inert gas is introduced as a carrier gas into the reaction system in order to prevent explosion to improve the safety or in order to control the reaction suitably, and as this inert gas, inexpensive nitrogen (N2) gas is employed in most cases. Even in 20 the case wherein the reaction is carried out without making a particular introduction of a carrier gas from the outside, in any of the above processes, N2 gas is formed as a by-product, and remains mixed in the formed NF3 gas. Therefore, when NF3 produced in any of the above processes is to be used for various applications as men- tioned above, it is required to eliminate impurities such as N2 gas, nitrous oxide (N2)), and carbon dioxide (C02). 25 However, since generally N2 gas (N2 gas as a carrier gas, and N2 gas as a by-product) is contained in a con- siderable amount in the NF3 produced in any of the above processes, in order to eliminate the N2 gas, the so- called NF3 condensing step wherein the N2 gas is eliminated after the reaction step is joined to follow the re- action step. (Note that, in some cases, a purifying step of eliminating impurities other than N2gas such as N20 and C02 as mentioned above, and hydrogen fluoride (HF) that has remained unreacted or has been produced 30 as a by-product is also placed between the reaction step and the condensation step.) In this case, although there are various ways of condensing NF3, a process of liquefying NF3 is described in US Patent 4091 081 using a refrigerant is commonly used as the most effective process since impurities will not be introduced and the facilities are simple in comparison with other processes wherein compression by us- ing a compressor is effected. As the refrigerant for liquefying, use is made of a liquefied gas having a boiling 35 point lower than that of NF3 such as liquid nitrogen, liquid air, and liquid argon, and when, of these, liquid nitrogen is used, it is the most preferable because, for example, the condensation of NF3 becomes easy, N2 is an inert substance, therefore the use thereof is safe, and N2 is inexpensive. However, in the case wherein NF3 is produced by using apparatus including the production steps as men- tioned above, when the NF3 formed in the condensation step is cooled and liquefied by using liquid nitrogen 40 as a refrigerant, because N2 gas that is a carrier gas and N2 gas that has been formed as a by-product are also partly liquefied together with NF3, the pressure in the condensation step is decreased, and the pressure in the whole reaction system is also decreased. Since the formation reaction of NF3 is carried out continuously, such a state makes quite difficult the control of the reaction in the reaction step, and safety problems arise, making impossible the reaction to be continued 45 for a long period of time. This is described using the molten salt electrolytic process as an example as follows. For example, in the case wherein, in order to produce NF3, a molten salt electrolysis is carried out in an NH4F/HF system using, as raw material, acid ammonium fluoride or ammonium fluoride and hydrogen fluoride or a KF/NH4F/HF system that is formed by adding as a raw material, acid potassium fluoride or potassium fluoride to the NH4F/HF sys- 50 tern, NF3 gas is released from the anode of the electrolytic cell while H2 gas is released from the cathode. If the NF3 gas and the H2 gas are mixed, they will explode, and therefore, in order to avoid the mixing, as shown in Fig. 3, the electrolytic cell is provided with a partition 13 for separating the anode 14 and the cathode 15 in such a manner that the partition 13 is fixed to a lid plate 16 with a suitable distance between it and the bottom plate of the electrolytic cell, so that the electrolytic cell is formed with an anode chamber 18 and a cath- 55 ode chamber 1 9 (the partition is positioned in such a way that the electrolyte can move freely between the anode chamber and the cathode chamber at the bottom part of the electrolytic cell.) to prevent the NF3 gas and the H2 gas from mixing. In order to prevent the partition at the time of the electrolysis from having a bipolarization phenomenon, the partition is made of afluorocarbon resin or has the surfaces coated with afluorocarbon resin. 2 EP 0 345 354 B1 As the f luorocarbon resin used for the partition in the present invention, any of generally known ones can be suitably used such as polytetraf luoroethylene, polychlorotrif luoroethylene, polyvinyl idene fluoride, polyvinyl fluoride, tetrafluoroethylene/hexafluoropropylene copolymer, tetrafluoroethylene/ethylene copolymer, tetra- fluoroethylene/perfluoroalkylvinyl ether copolymer, and chlorotrifluoroethylene/ethylene copolymer. 5 The NF3 gas and the H2 gas released respectively from the anode chamber and the cathode chamber of the electrolytic cell are led to the outside of the system, and then the NF3 gas is led to the next step, that is, the condensation step while the H2 gas is utilized as a by-product or is burnt and then released into the atmos- phere. Therefore it is impossible to keep the pressure in the anode chamber and the pressure in the cathode chamber at the same level all the time, resulting in a pressure difference. As a result, the level of the electrolyte 10 in the anode chamber becomes different from the level of the electrolyte in the cathode chamber. As the pressure difference becomes great, the difference in the level of the electrolyte surface becomes greater between the anode chamber and the cathode chamber, and when this difference exceeds a certain limit, either the NF3 gas or the H2 gas passes below the partition, and then mixes with the other gas thereby leading in the end to formation of a gas within the explosion limit. In order to obviate this, an inert gas is intro- 15 duced as a carrier gas into the anode chamber and the cathode chamber of the electrolytic cell respectively in suitable amounts to control the difference. Thus, the term "carrier gas" means a gas that is fed into the re- action tank for the purpose of improving the safety and controlling the reaction.
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