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English to Japanese: Process for making galantamine（extraction） General field: Law/Patents Detailed field: Patents
Source text - English In step (2) it is preferred that the coupling of activated B13X is allowed to react with A12 in a solvent in the presence of a base. It should be noted that the base does not have to be used, when the blocking group in compound of Formula I is not halogen, such as bromo. The solvent is typically an organic solvent which is preferably selected from methylene chloride (CH2Cl2), methanol (MeOH), ethanol (EtOH), isopropanol (IPA), methylisobutyl ketone (MIBK), toluene, tetrahydrofuran (THF), diethyl ether, diglyme, and methyl t-butyl ether (MTBE), and mixtures thereof. The mixture of methylene chloride (CH2Cl2) and methanol (MeOH) is a preferred solvent system. Typically, the base is an alkali hydroxide.
Alternatively, the base can be a tertiary amine base. The coupling can also be carried out in a two phase system with an organic solvent and an aqueous base of alkali hydroxide or alkali carbonate. It is more preferred to carry out the reaction in a mixture of methylene chloride (CH2Cl2) and methanol (MeOH) with sodium hydroxide as the base. The reaction is typically carried out at a temperature of about 0-500C. When the mixture of methylene chloride and methanol is used as solvent, and sodium hydroxide is used as a base, the preferred reaction temperature is about 0 to 50C.
2-(4-hydroxyphenyl) ethanol is converted to the corresponding 2-(4-hydroxyphenyl)ethyl chloride or bromide on reacting with concentrated aqueous hydrochloric acid or hydrobromic acid, respectively. Amination of the 2-(4-hydroxyphenyl)ethyl chloride or bromide is effectively conducted with a large excess of aqueous methylamine solution or an organic solution of methylamine. Organic solvents inert to amination can be used for the reaction. The preferred organic solvent is a low boiling alcohol solvent such as methanol (MeOH), ethanol (EtOH), isopropanol (IPA), n-butanol, and sec-butanol.
Translation - Japanese 工程（２）では、溶媒中、塩基存在下で活性化したＢ１３ＸのカップリングをＡ１２と反応させるのが好ましい。化学式Ｉの化合物中の保護基が臭素などのハロゲンでない場合は、塩基を使用する必要がないことに留意されたい。溶媒は典型的には有機溶媒であり、好ましくは塩化メチレン（ＣＨ２Ｃｌ２）、メタノール（ＭｅＯＨ）、エタノール（ＥｔＯＨ）、イロプロパノール（ＩＰＡ）、メチルイソブチルケトン（ＭＩＢＫ）、トルエン、テトラヒドロフラン（ＴＨＦ）、ジエチルエーテル、ジグリム、及びメチル－ｔ－ブチルエーテル、並びにこれらの混合物から選択される。塩化メチレン（ＣＨ２Ｃｌ２）とメタノール（ＭｅＯＨ）との混合物が好ましい溶媒系である。一般的に、塩基はアルカリ水酸化物である。
Translation - English FIELD OF THE INVENTION
The invention relates to composite carbon fibers. More particularly, the present invention relates to composite carbon fiber which is easily dispersed over matrix such as resins without leaving aggregates thereon, and excels in imparting low resistance property thereto, and wherein the multi-walled carbon nanotube is homogeneously dispersed within graphitized carbon nanofiber and in proximity to the surface of the graphitized carbon nanofiber.
BACKGROUND OF THE INVENTION
The methods of manufacturing multi-walled carbon nanotube include chemical vapor deposition in which hydrocarbon and other materials are thermally decomposed on catalyst metal and formed to multi-walled carbon nanotube, and physical vapor deposition in which graphite is sublimated by arc, laser or the like and then formed to multi-walled carbon nanotube in cooling process.
Chemical vapor deposition method is suitable for mass synthesis of multi-walled carbon nanotube since it is relatively easy to increase the size of reactor. Chemical vapor deposition method may be broadly classified into two methods. One is floating catalyst method, in which catalyst metal compound and co-catalyst such as sulfur are dissolved in hydrocarbons such as benzene and resulting solution is provided by a carrier gas of hydrogen to a reaction field which has been heated to 1000 °C or higher and catalyst is produced and multi-walled carbon nanotube is grown in the reaction field. Another one is supported catalyst method in which previously prepared supported catalyst (i.e. a carrier bearing catalyst metals or precursors thereon) is charged to reaction field which has been heated in the range of 500 °C to 700°C, then mixed gas of hydrocarbon such as ethylene and hydrogen or nitrogen is provided thereto for reaction.
In one embodiment of the present invention, composite carbon fiber can be obtained from, for example, the following method. First multi-walled carbon nanotube and graphitized carbon nanofiber are added and mixed in pure water to provide a mixed solution. The mixed solution is then pumped into pulverization nozzle of high pressure dispersion device to provide a paste. Strong shearing force is generated by turbulent flow of the mixed solution passing through the pulverization nozzle at an ultra-high speed, and the multi-walled carbon nanotube aggregate is decomposed by the shearing force and then uniformly mixed with the graphitized carbon nanofiber. The solid concentration in the mixed solution (i.e. the concentration of the multi-walled carbon nanotube and the graphitized carbon nanofiber) is preferably 5% or less by mass. If the solid concentration is more than 5% by mass, the efficient pulverization of multi-walled carbon nanotube aggregate tends to be prevented, since the viscosity of the mixed solution increases. It is preferred not to use dispersing agent since it is difficult to remove it from the composite carbon fiber once it has been added to the mixed solution.
Examples of high pressure dispersion device include Nanovater® manufactured by Yoshida kikai co., ltd., Star Burst® manufactured by Sugino machine ltd., and Nono Maker™ manufactured by Advanced Nano Technology Co., Ltd., etc. Injection pressure to the nozzle is preferably in the range of 100 MPa to 250 MPa. The number of times the mixed solution is injected to and passed through the nozzle is preferably 5 times or less. The number of times of injection and passing is more than 5 times, the multi-walled carbon nanotube and the graphitized carbon nanofiber tend to be short and re-aggregated.
The resulting slurry is then dried and powdered. Drying methods include spray-drying, freeze drying, drum drying, flash drying, hot air drying, vacuum drying, or the like. Drying temperature shall be set appropriately depending upon the type of drier. Drying is performed preferably until water content of the slurry measured by Karl Fischer method is 0.5% or less by mass. After drying, the dried body is preferably crushed as needed. Preferred crushing methods are the methods using pulverizer utilizing impact force of hammer or the like, jet mill utilizing the collision of crushed objects, or the like.
1. Composite carbon fiber comprising multi-walled carbon nanotube having fiber diameter of 5nm to 30nm and graphitized carbon nanofiber having fiber diameter of 50nm to 300nm, wherein the multi-walled carbon nanotube is homogeneously dispersed within the graphitized carbon nanofiber and in proximity to the surface of the graphitized carbon nanofiber.
2. The composite carbon fiber according to claim 1, wherein the specific resistance of the composite carbon fiber at compressed density of 0.8g/cm3 is lower than the specific resistance of the multi-walled carbon nanotube alone at compressed density of 0.8g/cm3 and the specific resistance of the multi-walled carbon nanofiber alone at compressed density of 0.8g/cm3.
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Keywords: Japanese, English patent, patents, chemical, chemistry, medical, translation