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    • 5. 发明授权
    • Method for preparation of graphite fluoride by contact reaction between
carbon and fluorine gas
    • 通过碳氟与氟气接触反应制备氟化石墨的方法
    • US4438086A
    • 1984-03-20
    • US413889
    • 1982-09-01
    • Minoru AramakiYasushi KitaHishagi NakanoShiro Moroi
    • Minoru AramakiYasushi KitaHishagi NakanoShiro Moroi
    • C01B31/04B01J8/02C01B31/00C01B9/08C01B31/30
    • B01J8/02C01B31/005B01J2208/00194B01J2208/00407B01J2208/0053B01J2208/00548B01J2219/182
    • 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.
    • 一种用于在约200-550℃之间的诸如石墨或石油焦炭等碳材料与氟气之间的非均相接触反应来制备(CF)n或(C2F)n等氟化石墨的方法和装置。 将小颗粒或粉末颗粒的形式保持在具有多个开口的保持器中,以便在保持器中形成碳材料层,该碳材料层放置在反应器中,以使得气体通道围绕保持器。 通过加热,氟气被强制地通过气体通道,而不会搅动保持器中的碳材料。 保持器的开口被成形和布置成使得氟气渗透通过保持器中的碳材料层。 例如,保持器是由丝网或穿孔金属板或由丝网制成的输送带制成的开放式箱体。 该方法对于防止由于反应碳材料层内的反应热的积累和/或对氟化碳的机械冲击或振动而导致的形成的氟化石墨的自发分解是有效的。
    • 7. 发明授权
    • Method of refining rare gas fluoride excimer laser gas
    • 精炼稀有气体氟化物准分子激光气体的方法
    • US4964137A
    • 1990-10-16
    • US466930
    • 1990-01-18
    • Minoru AramakiShinsuke NakagawaHisaji NakanoHiroshi IchimuraMasahiro Tainaka
    • Minoru AramakiShinsuke NakagawaHisaji NakanoHiroshi IchimuraMasahiro Tainaka
    • H01S3/097H01S3/036H01S3/223H01S3/225
    • H01S3/036H01S3/225
    • A laser gas used in a rare gas fluoride excimer laser is efficiently refined with little loss of the principal rare gas such as Ar, Kr or Xe by sequential contact of the laser gas first with a reactive metal, e.g. Si or Fe, for conversion of the fluorine source gas such as F.sub.2 or NF.sub.3 to a metal fluoride, then with a solid alkaline compound, e.g. Ca(OH).sub.2, for conversion of gaseous fluorides to solid metal fluorides, next with zeolite which is adsorbent of most of the remaining impurities and finally with an alkaline metal, e.g. Ca or Na, for decomposition of CF.sub.4 to form a solid metal fluoride and carbon. CF.sub.4 is formed during operation of the excimer laser by reaction of fluorine with a fluororesin used as electrical insulator in the laser apparatus, and accumulation of CF.sub.4 in the laser gas caused significal lowering of the laser output power.
    • 在稀有气体氟化物准分子激光器中使用的激光气体通过先将激光气体与活性金属例如反应性金属顺序接触而有效地精制而不损失诸如Ar,Kr或Xe的主要稀有气体。 Si或Fe,用于将氟源气体如F2或NF3转化为金属氟化物,然后用固体碱性化合物,例如, Ca(OH)2,用于将气态氟化物转化为固体金属氟化物,接下来是沸石,其是大部分剩余杂质的吸附剂,最后是碱金属,例如碱金属。 Ca或Na,用于分解CF4以形成固体金属氟化物和碳。 在激光装置中通过氟与用作电绝缘体的氟树脂反应而在准分子激光器的操作期间形成CF4,并且CF4在激光气体中的积聚导致激光输出功率的显着降低。
    • 9. 发明授权
    • Method for producing fluorine
    • 生产氟的方法
    • US4312718A
    • 1982-01-26
    • US161593
    • 1980-06-20
    • Nobuatsu WatanabeMinoru AramakiYasushi Kita
    • Nobuatsu WatanabeMinoru AramakiYasushi Kita
    • C04B35/52C04B35/532C25B1/24C25B11/12
    • C25B1/245C04B35/532C25B11/12
    • The use of an isotropic carbon block having an anisotropy of not more than 1.2 in terms of an anisotropic ratio of specific resistance as an anode in the production of fluorine by the electrolysis of an electrolyte comprising a mixed molten salt system of potassium fluoride and hydrogen fluoride has been found to be extremely useful for attaining increase in critical current density so that occurrence of the unfavorable anode effect can be effectively prevented. With such an isotropic carbon block anode, even if the anode effect occurs, the electrolysis can be stably continued again by lowering the potential of the electrode. Further, the incorporation of a fluoride into the isotropic carbon block anode and/or the addition of a fluoride into the electrolyte is effective for further increasing critical current density.
    • 使用通过电解电解生产氟的电阻率的各向异性比不大于1.2的各向同性碳块,其包含氟化钾和氟化氢的混合熔融盐体系 已经发现对于获得临界电流密度的增加是非常有用的,从而可以有效地防止出现不利的阳极效应。 使用这种各向同性的碳块阳极,即使发生阳极效应,也可以通过降低电极的电位来再次稳定地进行电解。 此外,将氟化物并入各向同性碳嵌段阳极和/或向电解质中添加氟化物对于进一步提高临界电流密度是有效的。
    • 10. 发明授权
    • Process of preparing fluorocarbon carboxylic or sulfonic acid from its
fluoride
    • 从其氟化物制备氟碳羧酸或磺酸的方法
    • US4927962A
    • 1990-05-22
    • US237072
    • 1988-08-29
    • Minoru AramakiHiroaki SakaguchiTamio Nakamura
    • Minoru AramakiHiroaki SakaguchiTamio Nakamura
    • C07C51/04C07C51/58C07C303/00
    • C25B3/08C07C303/02C07C303/32C07C51/04C07C51/58
    • A fluorocarbon carboxylic acid Rf(COOH).sub.m (Rf is C.sub.1 -C.sub.10 perfluoroalkyl group, m is 1 or 2) is prepared by the steps of hydrolyzing Rf(COF).sub.m with water to obtain an acidic solution, neutralizing the acidic solution with aqueous solution of KOH to form Rf(COOK).sub.m, precipitating and separating Rf(COOK).sub.m from the solution and converting Rf(COOK).sub.m into Rf(COOH).sub.m by acid decomposition. The content of free fluorine can extremely be reduced by treating Rf(COOK).sub.m with sulfuric acid and silica. The mother liquor is recycled after removing KF by treatment with a metal hydroxide and replenishing with KOH. In preparing a fluorocarbon sulfonic acid RfSO.sub.3 H (Rf is C.sub.1 -C.sub.3 perfluoroalkyl group) in substantially the same way, RfSO.sub.3 K is formed in aqueous solution of KOH by bringing gaseous RfSO.sub.2 F into contact with the KOH solution under normal pressure, while controlling the feed rate of RfSO.sub.2 F per unit area of gas-liquid contact at a sufficiently low level.
    • 氟化碳羧酸Rf(COOH)m(Rf为C1-C10全氟烷基,m为1或2)通过以下步骤制备:用水水解Rf(COF)m,得到酸性溶液,用水溶液中和酸性溶液 KOH溶液形成Rf(COOK)m,沉淀并从溶液中分离Rf(COOK)m,并通过酸分解将Rf(COOK)m转化为Rf(COOH)m。 通过用硫酸和二氧化硅处理Rf(COOK)m可以极大地降低游离氟的含量。 通过用金属氢氧化物处理除去KF后再加入母液并用KOH补充。 在以相同的方式制备氟碳磺酸RfSO 3 H(Rf为C 1 -C 3全氟烷基)时,通过在常压下使气态RfSO 2 F与KOH溶液接触,在KOH的水溶液中形成RfSO 3 K,同时控制 每单位面积的气 - 液接触的RfSO 2 F足够低。