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1. 发明专利

JPH0684316B2 失效
公开(公告)号：JPH0684316B2
公开(公告)日：1994-10-26
申请号：JP32822589
申请日：1989-12-20
申请人： TOKUYAMA SODA KK
发明人： OKADA NAOYA , YOSHINAGA MASAKI , ASADA KOJI
IPC分类号： A61K9/107 , C07B39/00 , C07B63/00 , C07C17/02 , C07C17/10 , C07C17/42 , C07C19/08 , C07C23/36 , C07C209/74 , C07C209/90 , C07C211/15

2. 发明专利

JPH0236155A METHOD FOR TREATING FLUORINATED PRODUCT 失效
公开(公告)号：JPH0236155A
公开(公告)日：1990-02-06
申请号：JP18370488
申请日：1988-07-25
申请人： TOKUYAMA SODA KK
发明人： OKADA NAOYA , YOSHINAGA MASAKI , ITONAGA KAZUMASA , TAKI TOMOYASU
IPC分类号： C07C209/84 , C07C67/00 , C07C209/00 , C07C209/74 , C07C209/90 , C07C211/15
摘要： PURPOSE:To obtain perfluorotrialkylamine reduced in generation of hydrogen fluoride by subjecting a fluorinated product containing perfluorotrialkylamine obtained by fluorination of trialkylamine to heat treatment at a specific temperature. CONSTITUTION:A fluorinated product containing perfluorotrialkylamine obtained by fluorinating trialkylamine using a well-known method is subjected to heat treatment in the temperature range expressed by the formula 14N+30

3. 发明专利

JPH06184014A PURIFICATION OF FLUORINE-BASED INERT LIQUID 失效
公开(公告)号：JPH06184014A
公开(公告)日：1994-07-05
申请号：JP34009392
申请日：1992-12-21
申请人： TOKUYAMA SODA KK
发明人： YOSHINAGA MASAKI , OKADA NAOYA
IPC分类号： C07B63/00 , C07C17/38 , C07C17/389 , C07C19/08 , C07C41/36 , C07C43/12 , C07C209/84 , C07C211/15
摘要： PURPOSE:To provide a more effective method for removing hydrogen fluoride contained in a fluorine-based inert liquid. CONSTITUTION:In this method for purification of a fluorine-based inert liquid, the fluorine-based inert liquid containing hydrogen fluoride is characteristically brought into contact with allophane (an amorphous clay mineral composed of a hydrous aluminum silicate).

4. 发明专利

JPH06146043A PRODUCTION OF PERFLUORO COMPOUND 失效
公开(公告)号：JPH06146043A
公开(公告)日：1994-05-27
申请号：JP29295192
申请日：1992-10-30
申请人： TOKUYAMA SODA KK
发明人： NISHIMURA MASAKATSU , OKADA NAOYA , HIRAI YASUHIKO , YOSHINAGA MASAKI
IPC分类号： C25B3/08 , C25B15/08
摘要： PURPOSE:To produce the perfluoro compd. as an electrically insulating liquid having excellent thermal stability and safety by continuously electrolytically fluorinating specific amine and hydrofluoric anhydride while circulating both in an electrolytic cell. CONSTITUTION:The electrolytic cell and a circulating cell are connected by a pipe to form a closed circuit. While the amine expressed by formula 1 (where A is a phenyl group or cyclohexyl group which may be substd. with fluorine atom; R , R are usually 1 to 3C alkyl groups of the same kind or different kinds) and the generally commercially available hydrofluoric anhydride are circulated in this closed circuit, both are continuously electrolytically fluorinated in the electrolytic cell having anode made of Ni and cathode made of Ni or Fe or stainless steel, by which the liquid perfluoro compd. consisting of a mixture composed of 75 to 95wt.% perfluoro(N,N-dialkyl cyclohexyl amine) and the balance perfluoro(N,N-dialkyl hexyl amine) and having the excellent thermal stability even at a high temp. of 250 deg.C and the good electrical insulating characteristic is produced.

5. 发明专利

JPH0525671A ELECTROLYTICALLY FLUORINATING METHOD 失效
公开(公告)号：JPH0525671A
公开(公告)日：1993-02-02
申请号：JP18128491
申请日：1991-07-22
申请人： TOKUYAMA SODA KK
发明人： NISHIMURA MASAKATSU , OKADA NAOYA , HIRAI YASUHIKO , SHIRAI MASAHIRO
IPC分类号： C25B3/08 , C25B15/02
摘要： PURPOSE:To improve the productivity of a desired fluorinated product by increasing an electrode area to increase an electrolytic current. CONSTITUTION:This method consists in executing the electrolytic fluorination of an org. compd. having a carbon-hydrogen bond in an electrolytic cell 1 by circulating an electrolytic bath liquid contg. the org. compd. having the carbon- hydrogen between this electrolytic cell 1 and a circulating cell 2. The electrolytic cell 1 installed with electrode groups 3, 3', 3'' is connected in series and the electrolytic fluorination is executed by maintaining the temp. difference in the flow direction of the electrolytic bath liquid in the respective electrode groups 3, 3', 3'' at

6. 发明专利

JPH04352747A STABILIZATION OF FLUORINATED PRODUCT 失效
公开(公告)号：JPH04352747A
公开(公告)日：1992-12-07
申请号：JP12171891
申请日：1991-05-28
申请人： TOKUYAMA SODA KK
发明人： YOSHINAGA MASAKI , OKADA NAOYA
IPC分类号： C07C209/90 , C07C211/15 , C07C211/17
摘要： PURPOSE:To suppress rise in concentration, by heating or long-term preservation, of hydrogen fluoride, dissolved in a fluorinated product containing a perfluoro- tert-amine and to stabilize the fluorinated product. CONSTITUTION:A fluorinated product containing a perfluoro-tert-amine obtained by fluorinating preferably a 4-27C, more preferably 5-18C tertiary amine containing carbon-hydrogen bonds in molecule, especially a compound shown by the formula R4N(R5)R6 (R4 is CH3; R5 and R6 are aliphatic or aromatic hydrocarbon group, R5 is 1-5C hydrocarbon, R6 is 3-15C hydrocarbon, especially R4=R5=CH3 and R6 is 3-8C above-mentioned hydrocarbon group) is brought into contact with water in the presence of preferably 0.1-20wt.%, especially 0.5-10wt.%, based on the fluorinated product, of metal zinc to give the fluorinated product having concentration of hydrogen fluoride not rising by heating and long-term preservation. Stabilizing effects of the fluorinated product can be further increased by adding an acid, a base or a salt as an additive to water.

7. 发明专利

JPH03190826A METHOD FOR TREATING FLUORINATED PRODUCT 失效
公开(公告)号：JPH03190826A
公开(公告)日：1991-08-20
申请号：JP32822589
申请日：1989-12-20
申请人： TOKUYAMA SODA KK
发明人： OKADA NAOYA , YOSHINAGA MASAKI , ASADA KOJI
IPC分类号： A61K9/107 , C07B39/00 , C07B63/00 , C07C17/02 , C07C17/10 , C07C17/42 , C07C19/08 , C07C23/36 , C07C209/74 , C07C209/90 , C07C211/15
摘要： PURPOSE:To obtain a perfluoro-organic compound reduced in occurrence of HF even in the case of heating by irradiating a fluorinated product containing the perfluoro-organic compound having no bonding cleaved by ultraviolet ray irradiation with ultraviolet ray in absence of F2 gas. CONSTITUTION:A fluorinated product containing a perfluoro-organic compound having no bonding cleaved by ultraviolet ray irradiation (e.g. ether bond, thioether bond or bond of halogen other than F and carbon) is irradiated with an ultraviolet ray having 190-400nm wavelength in absence of F2 gas at 150 deg.C for 1-50hr to provide a fluorinated product from which HF is not generated by heating. The product is suitable as heat medium for vapor phase soldering, test medium of electronic component, artificial blood, etc., because the product hardly process HF.

8. 发明专利

JPH0230785A METHOD FOR ELECTROLYTIC FLUORINATION 失效
公开(公告)号：JPH0230785A
公开(公告)日：1990-02-01
申请号：JP10416088
申请日：1988-04-28
申请人： TOKUYAMA SODA KK
发明人： MURATA YASUO , OKADA NAOYA , HIRAI YASUHIKO , TAKI TOMOYASU
IPC分类号： C25B3/08
摘要： PURPOSE:To stably recover org. perfluorochemicals in high yield over a long period by circulating an electrolyte between an anode and a cathode for specified residence time to electrolytically fluorinate an org. compd. CONSTITUTION:The org. compds. such as hydrocarbons, amines, ethers, etc., are dissolved or dispersed in hydrogen fluoride to obtain an electrolyte. A current is applied between the anode and cathode in the electrolyte at about 0.1-6A/dm and about 4-9V cell voltage. As a result, the org. compd. is fluorinated to obtain an org. perfluorochemical. In the electrolytic fluorination method, the electrolyte is circulated so that the residence time of the electrolyte in the space between the anode and cathode per one cycle is controlled to 0.5-25sec. The distance between both electrodes is preferably controlled to about 0.5-5mm, and the linear velocity of the electrolyte to about >=1.5cm/sec. By this method, an org. perfluorochemical is obtained in high yield, the cell voltage is not increased, and stabilized electrolytic fluorination can be continued over a long period.

9. 发明专利

JPH05112496A METHOD FOR STABILIZING FLUORINATION PRODUCT 失效
公开(公告)号：JPH05112496A
公开(公告)日：1993-05-07
申请号：JP27407491
申请日：1991-10-22
申请人： TOKUYAMA SODA KK
发明人： YOSHINAGA MASAKI , OKADA NAOYA
IPC分类号： C07C209/82 , C07C209/90 , C07C211/15 , C07C211/17
摘要： PURPOSE:To suppress a rise in hydrogen fluoride concentration and stabilize the subject product useful as artificial blood, etc., by bringing a fluorination product containing a perfluoro-tertiary amine prepared by fluorinating a tertiary amine having C-H bond in the molecule into contact with active carbon. CONSTITUTION:A tertiary amine (e.g. N,N-dimethylaniline) having carbon- hydrogen bond in the molecule is electrolyzed in the presence of anhydrous hydrofluoric acid by using an electrolyzer made of nickel and having the cathode and anode made of nickel at 1.5A/dm current density and the produced fluorination product is intermittently taken from the bottom of the electrolyzer. The taken out product is refluxed in a mixture containing equal volumes of a 40wt.% aqueous solution of sodium hydroxide and diisobutylamine for 120hr while being heated. The resultant mixture is then distilled to afford a fluorination product containing a perfluoro-tertiary amine [e.g. perfluoro(N,N- dimethylcyclohexylamine]. The obtained fluorination product is subsequently brought into contact with active carbon, stirred at 80 deg.C for 8hr and then filtered to separate the active carbon. Thereby, the objective fluorination product is stabilized.

10. 发明专利

JPH04315959A STATIONARY PHASE FOR CHROMATOGRAPHY 失效
公开(公告)号：JPH04315959A
公开(公告)日：1992-11-06
申请号：JP8241691
申请日：1991-04-15
申请人： TOKUYAMA SODA KK
发明人： OKADA NAOYA , ITONAGA KAZUMASA
IPC分类号： B01J20/281 , B01J20/22 , G01N30/88
摘要： PURPOSE:To enable separation and analysis of structural isomers of a perfluoro compound by using as a stationary phase for chromatography the high boiling fraction of a fluorine compound of tertiary amine having hydrogen-carbon bonding. CONSTITUTION:A high boiling fraction of a fluororine compound whose boiling point at pressure P(mmHg) ms above an absolute temperature T(K) expressed by an equation of 1/T=-1.23X10 in(P)+2.58X10 , for example, a high boiling fraction whose boiling point at normal pressure is more than about 30 deg.C is carried on a carrier such as diatomite and is packed in a column and used as a stationary phase for chromatography, the fluorine compound being obtained through fluorination of tertiary amine having hydrogen-carbon bonding. A compound having the total carbon number of 2 to 30 and preferably 8 to 24 is desirable for the tertiary amine. The use of the stationary phase provides excellent separative power during the analysis of a perfluoro compound having structural isomers and a sharp peak with less tailing can be obtained even during the analysis of a hydrocarbon amine or a polar compound such as alcohol.

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