Central Glass Company, Limited

Other

Toyo Tanso Co., Ltd.

Applied Science Research Institute

Watanabe Applied Science Research Institute

Yasushi Kita

Akira Sakanoue

Shiro Moroi

Nobuatsu Watanabe

Masayuki Kawaguchi

Koji Nozaki

Minoru Aramaki

Yoshinori Kubota

Hisaji Nakano

Shirou Moroi

Shoichi Tsujioka

Kiyotaka Miura

Natsuya Nishimura

Yoshiyuki Kobayashi

Hiromi Kawamoto

Hiroaki Sakaguchi

Tamio Nakamura

Nobuyuki Tokunaga

Naoki Okada

Hiromi Sugimoto

Masahiro Tainaka

Shigenori Sakai

Kenji Fujii

Kayoko Yamamoto

Seigo Okamura

Shoji Okabayashi

Hishagi Nakano

Hishaji Nakano

The present invention relates to a method for producing a fluoroalkylsulfonic acid anhydride represented by a general formula of (C.sub.n F.sub.2n+1 SO.sub.2).sub.2 O where n is an integer ranging from 1 to 8. This method includes a step of (a) reacting diphosphorus pentoxide with a fluoroalkylsulfonic acid represented by a general formula of C.sub.n F.sub.2n+1 SO.sub.3 H where n is an integer ranging from 1 to 8, in a fluorine-containing solvent, thereby to form the fluoroalkylsulfonic acid anhydride in the fluorine-containing solvent. A fluoroalkylsulfonic acid anhydride produced by this method is high in purity and yield.

Method for producing high-purity fluoroalkylsulfonic acid anhydride

The invention relates to a method of preparing a sulfonimide, a first salt thereof, or a second salt thereof. The method includes the step of: (a) reacting one or two sulfonyl fluorides with nonhydrous ammonia and an amine component which is one of a tertiary amine and a heterocyclic amine, so as to prepare the first salt. Alternatively, the method includes the step of: (a) reacting the sulfonyl fluoride with the amine component and a sulfonamide, so as to prepare the first salt. The method further optionally includes, after the step (a), the step of: (b) reacting, in an aqueous solution, the first salt with a metal compound, so as to prepare the second salt. The method still further optionally includes, after the step (a), the step of: (c) reacting the first salt with a strong acid so as to prepare the sulfonimide. Alternatively, the method further optionally includes, after the step (b), the step of: (d) reacting the second salt with a strong acid so as to prepare the sulfonimide. The sulfonimide, the first salt or the second salt is easily economically prepared in an industrial scale production with high purity and high yield.

Method of preparing sulfonimide or its salt

An upconversion laser material includes a micro-sphere which is doped with an ion of a rare earth element and made of one selected from the group consisting of crystals and glasses. Thus, the micro-sphere achieves the light confinement therein and serves as a resonator. Therefore, the Q-value of the resonator becomes large. With this, it is possible to obtain the upconversion laser oscillation at room temperature.

Upconversion laser material

The invention relates to water-repellent composite grains. Each composite grain includes: a first grain; and a low molecular weight polytetrafluoroethylene (PTFE) covering the first grain. The first grain is higher than the PTFE in mechanical strength. With this, the composite grains are improved in mechanical strength. A water-repellent article is produced by anchoring the composite grains to a substrate through an adhesive layer formed on the substrate. The composite grains are partly exposed on the adhesive layer and partly submerged in the adhesive layer. With this, the water-repellent article is made minutely rough. The water-repellent article is improved in mechanical strength and water repellency.

Water-repellent composite grains, method for producing same, and

Metal containing compounds having a graphite-like layer structure are derived from poly(amino-s-triazine), [A], which has a layer structure and is represented by (C.sub.3 N.sub.3).sub.2 N.sub.x H.sub.y, where 2.ltoreq.x.ltoreq.4, and 0.ltoreq.y.ltoreq.8. Reaction of [A] with a transition metal M at 400.degree.-1000.degree. C. gives a compound represented by C.sub.a NH.sub.b M.sub.c, where 0.6.ltoreq.a.ltoreq.20.0, 0.ltoreq.b.ltoreq.1.0, and 0.001.ltoreq.c.ltoreq.0.5. This compound exhibits magnetism. Reaction of [A] with a halide of a transition metal or aluminum at 200.degree.-500.degree. C. gives C.sub.6 N.sub.p H.sub.q M.sub.r X.sub.s, where M is a transition metal or Al, X is a halogen, 8.ltoreq.p.ltoreq.10, 0.ltoreq.q.ltoreq.10, 0.6.ltoreq.r.ltoreq.1.5, and 0.ltoreq.s.ltoreq.1. When M is a transition metal the compound exhibits paramagnetism. When X is Al, heating of a powder of the compound at 800.degree.-950.degree. C. provides an AlN powder coated with an amorphous organic substance composed of C, N and H and, hence, protected against oxidation. The same coated AlN powder is obtained also by reacting a powder of [A] with an aluminum halide at 800.degree.-950.degree. C. By heating the coated AlN powder at a temperature above 1000.degree. C. the amophous organic coating sublimates and decomposes to leave a pure AlN powder which is suitable for sintering.

Metal containing derivatives of aminotriazine polymer and method of

Crystallization of a fluoride glass article is suppressed by treating the surface(s) of the fluoride glass article with a solution of a fluorine-containing alkali metal compound or a fluorine-containing ammonium compound such as, e.g., LiPF.sub.6, NaBF.sub.4 or NH.sub.4 BF.sub.4, in a nonaqueous solvent such as, e.g., ethanol, N,N-dimethylformamide or acetonitrile. The treatment can be made at room temperature.

Method for suppressing crystallization of fluoride glass articles by

The invention provides a lithium secondary battery using hydric boron carbonitride which is a layered compound represented by BC.sub.x N.sub.y H.sub.z, where 0.5.ltoreq.x.ltoreq.12, 0.7.ltoreq.y.ltoreq.1.5, and 0.01.ltoreq.z.ltoreq.3, as the active material of the negative electrode. This compound is obtained by a CVD process. The electrolyte is a solution of a lithium salt in an organic solvent. The material of the positive electrode is an oxide such as MnO.sub.2 or V.sub.2 O.sub.5, a sulfide such as MoS.sub.2 or TiS.sub.2 or a conductive organic polymer such as polyaniline. In this secondary battery Li is smoothly intercalated in and released from the hydric boron carbonitride of the negative electrode, and the energy density with respect to the active material of the negative electrode is sufficiently high. This battery bears a fairly large number of charge-discharge cycles. Also it is possible to use hydric boron carbonitride as the active material of the positive electrode of a lithium secondary battery in combination with negative electrode of metallic Li or hydric boron carbonitride with intercalation of a larger amount of Li.

Lithium secondary battery using hydric boron carbonitride as electrode

A polymeric compound, named poly(amino-s-triazine), which has a layer structure with a structural unit represented by (C.sub.3 N.sub.3).sub.2 N.sub.x H.sub.y, where 2.ltoreq.x.ltoreq.4 and 0.ltoreq.y.ltoreq.8, is obtained by reaction of cyanuric trichloride with ammonia or melamine. This compound is stable in the air up to about 400.degree. C. and exhibits fluorescence by excitation at wavelength of 365 nm. When the above reaction is carried out at a temperature ranging from room tempertaure to about 400.degree. C. the product is an oligomeric compound (C.sub.3 N.sub.3).sub.a (NH).sub.b (NH.sub.2).sub.c Cl.sub.d, where 2.ltoreq.a.ltoreq.10, 1.ltoreq.b.ltoreq.10, 0.ltoreq.c.ltoreq.11 and 1.ltoreq.d.ltoreq.12, and poly(amino-s-triazine) is obtained by heating the oligomeric compound at 400.degree.-600.degree. C. in an inactive gas. The oligomeric compound too exhibits fluorescence and is higher in fluorescence intensity. An alkali metal ion can be introduced into poly(amino-s-triazine) by treatment with an alkali metal hydroxide solution, or hydroxyl group can be introduced by treatment with a mineral acid. In either case the modified polymer is very higher in fluorescence intensity and narrower in the width of flurorescence peak.

Aminotriazine polymers and method of preparing same

The invention relates to a chemical vapor deposition (CVD) method for forming tungsten carbide, W.sub.3 C, by subjecting a gas mixture of tungsten hexafluoride, hydrogen and an aromatic hydrocarbon, e.g. benzene, to vapor phase reaction at an elevated temperature. The reaction temperature can be lowered to the extent of 250.degree. C. and the reaction can be carried out even at normal pressure, not necessarily under reduced pressure, by proportioning tungsten hexafluoride, hydrogen and the hydrocarbon such that in the gas mixture the atomic ratio of C to W falls in the range from 2 to 10 while the atomic ratio of H to C is not lower than 3. By this method a W.sub.3 C film excellent in glossiness can be deposited on various metal parts without adversely affecting the metal parts by the elevated temperature.

Method of forming tungsten carbide by chemical vapor deposition

Graphite fluoride in the form of submicron particles is easily obtained at high yield by using, exclusively, acetylene black as the carbon material to be fluorinated with fluorine gas. Use of any other type of carbon black does not give comparable results. Graphite fluoride produced from acetylene black is superior in dispersibility.

Method of producing ultrafine particles of graphite fluoride

Using a positive active material in powder form such as a metal salt or graphite fluoride, an anode for use in an electric cell, and particularly suitable for use in an organic electrolyte cell, is produced by the steps of dispersing the active material, and a conductive material such as carbon powder where necessary, in a solution of an organic polymer used as binder in a suitable liquid, mixing the dispersion with another liquid in which the polymer is substantially insoluble so as to cause precipitation of the polymer in a state intimately mixed with the active material and the conductive material, separating the solid phase mixture from the liquid phase and drying it, and press-shaping the dried mixture into an anode body of a desired shape. By mixing the binder with the active material in this manner, it is possible to obtain an anode body sufficient in mechanical strength and high in electrochemical activity by using only a very small amount of binder.

Method of producing electric cell anode using powdery active material

A graphite fluoride can be produced safely and in high yield on a commercial production scale by a process comprising reacting a carbon material having an average size of 100.mu. to 10 mm with fluorine. Further, when the fluorination reaction is stopped before completion thereof and the graphite fluoride product is subjected to sifting with a sieve to separate a desired graphite fluoride from the raw carbon material remaining unreacted.

Process for producing a graphite fluoride

A method of preparing graphite fluoride such as (CF).sub.n or (C.sub.2 F).sub.n by heterogeneous contact reaction between a carbon material such as graphite or petroleum coke and fluorine gas at about 200.degree.-550.degree. C. In the gas phase of the reaction system, the total concentration of higher fluorocarbons having more than four carbon atoms formed by side reactions is controlled so as not to become above 3% by volume by, for example, condensation or catalytic decomposition of at least a portion of the higher fluorocarbons in the gas flowed out of the reaction chamber for recirculation. Such control is highly effective for prevention of rapid and violent decomposition of the graphite fluoride existing in the solid phase of the reaction system induced by sudden decomposition of the higher fluorocarbons in the reaction system to lower fluorocarbons.

Method of safely preparing graphite fluoride

A lubricant comprising a partially defluorinated graphite fluoride obtained by exposing a dispersion of raw material graphite fluoride to electromagnetic radiation, followed by the separation of the resulting partially degraded graphite fluoride. The partially defluorinated graphite fluoride is not only excellent in lubricating properties but also has excellent compatibilities with resins, greases and oils. The excellent compatibilities of the partially defluorinated graphite fluoride are effective in preventing the unfavorable deposition of the graphite fluoride in a liquid lubricant composition and advantageously lead to improvement in the moldability of any graphite fluoride-resin composition, thereby enabling the ultimate composition to exhibit excellent lubricating properties.

Lubricant comprising a partially defluorinated graphite fluoride

A method and apparatus for preparation of a graphite fluoride such as (CF).sub.n or (C.sub.2 F).sub.n by heterogeneous contact reaction between a carbon material such as graphite or petroleum coke and fluorine gas at about 200.degree.-550.degree. C. The carbon material in the form of small pieces such as granules or powder particles is kept in a holder having a number of openings so as to form a carbon material layer in the holder, which is placed in a reactor so as to leave gas passages around the holder. With heating, fluorine gas is forcibly passed through the gas passages without agitating the carbon material in the holder. The openings of the holder are shaped and arranged such that the fluorine gas permeates through the carbon material layer in the holder. For example, the holder is an open-type box made of either a wire screen or a perforated metal plate, or a conveyor belt made of a wire screen. This method is effective for prevention of spontaneous decomposition of the formed graphite fluoride attributed to accumulation of the heat of reaction within the reacting carbon material layer and/or mechanical shocks or vibrations to the fluorinated carbon.

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Ube, Japan

Yasushi Kita