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    • 32. 发明授权
    • Aluminum nitride powder and a process for the preparation thereof
    • 氮化铝粉末及其制备方法
    • US4923691A
    • 1990-05-08
    • US364013
    • 1989-06-09
    • Dieter PetersGero HeymerChristian May
    • Dieter PetersGero HeymerChristian May
    • C01B21/072
    • C01B21/072C01P2002/60C01P2004/62C01P2006/12C01P2006/60
    • An aluminum nitride powder has a crystallite size of 40 to 150 nm, measured by powder diffractometry and evaluated by the method of Scherrer, a primary particle size of 0.1 to 0.5 .mu.m, a specific surface according to BET of 5 to 50 m.sup.2 /g and a degree of whiteness of more than 91%, measured using light of a 400 to 700 nm wavelength against barium sulfate analytical reagent as standard of whitness.To prepare this aluminum nitride powder, metallic aluminum and monoamminealuminum chloride [AlCl.sub.3 (NH.sub.3)] are first molten together in an inert gas atmosphere at temperatures above 125.degree. C. and allowed to react with one another with evolution of hydrogen. 8 to 20 g of ammonia are then introduced per hour per mol of monoamminealuminum chloride into the aluminum-containing monoamminealuminum chloride melt at temperatures between 250.degree. and 400.degree. C., aluminum nitride being precipitated as a solid until the conversion of the aluminum is complete. The temperature of the melt is finally raised to more than 400.degree. C.
    • 氮化铝粉末的微晶尺寸为40〜150nm,用粉末衍射法测定,用Scherrer法评价,一次粒径为0.1〜0.5μm,BET比表面积为5〜50m 2 / g 白度为91%以上,采用400〜700nm波长的光作为白度标准测定硫酸钡分析试剂。 为了制备这种氮化铝粉末,首先在惰性气体气氛中,在高于125℃的温度下将金属铝和一氯化铝[AlCl 3(NH 3)]熔融在一起,并使其彼此发生氢气反应。 然后在250-400℃的温度下将8至20g的氨每小时每摩尔氯化单铝酸铵引入含铝单胺氯化铝熔体中,将氮化铝作为固体沉淀直到铝的转化完全 。 熔体的温度最终升至400℃以上。
    • 33. 发明授权
    • Continuous process for complete removal or organic impurities from and
complete decolorization of prepurified wet-process phosphoric acid
    • 用于完全去除或有机杂质的连续方法和完全脱湿的湿法磷酸完全脱色
    • US4906445A
    • 1990-03-06
    • US311640
    • 1989-02-16
    • Gunther SchimmelGerhard BettermannGero HeymerFriedrich Kolkmann
    • Gunther SchimmelGerhard BettermannGero HeymerFriedrich Kolkmann
    • C01B25/234C01B25/235C01B25/46
    • C01B25/461C01B25/235
    • A continuous process is indicated for complete removal of organic impurities from and complete decolorization of pre-purified wet-process phosphoric acid which has been purified by an extractive method using an organic solvent, freed from residual hydrofluoric acid by steam stripping and treated with hydrogen peroxide at elevated temperature, which comprises mixing the pre-purified wet-process phosphoric acid and the hydrogen peroxide in a mixing zone at a temperature of from 100.degree. to 200.degree. C., preferably 140.degree. to 160.degree. C., and allowing them to react at this temperature for a further 1 to 4 hours, cooling to from 85.degree. to 90.degree. C. the pre-purified wet-process phosphoric acid treated in this way and pumping it at this temperature with exclusion of air firstly through an activated charcoal bed which has been prepared on the basis of peat and has been steam-activated and has a BET surface area of from 800 to 1000 m.sup.2 /g, and subsequently through a silicon carbide and/or graphite bed while maintaining a pumping rate of less than 0.5 m.sup.3 /h of wet-process phosphoric acid per m.sup.3 of activated charcoal bed.
    • 指示完全除去有机杂质并完全脱色预纯化的湿法磷酸的连续方法,其通过萃取方法使用有机溶剂纯化,通过汽提除去残留的氢氟酸并用过氧化氢处理 在高温下,其包括在预先纯化的湿法磷酸和过氧化氢的混合区中在100至200℃,优选140至160℃的温度下混合,并使它们 在该温度下再反应1至4小时,冷却至85℃至90℃,预纯化的湿法磷酸以此方式处理并在该温度下泵送,首先通过活性炭排除空气 基于泥炭制备并已蒸汽活化并具有800至1000m2 / g的BET表面积的床,随后通过碳化硅和/或石墨b 同时保持每立方米活性炭床的湿法磷酸的泵送速率小于0.5m 3 / h。
    • 38. 发明授权
    • Process for making aqueous alkali metal phosphate solutions
    • 制备碱金属磷酸盐水溶液的方法
    • US4385041A
    • 1983-05-24
    • US326078
    • 1981-11-30
    • Klaus JoddenGero Heymer
    • Klaus JoddenGero Heymer
    • C01B25/30C01B15/16C01B25/26
    • C01B25/30
    • The invention relates to a process for making aqueous alkali metal phosphate solutions by subjecting aqueous alkali metal phosphite solutions to catalytic oxidation with oxygen or air. More particularly, oxygen or air in stoichiometric excess proportions is introduced into the aqueous alkali metal phosphite solution at about 30.degree. to 110.degree. C., at a pH-value of 0 to about 8, and in the presence of SiO.sub.2 or aluminum silicate containing at most 10 weight % Al.sub.2 O.sub.3, for as long as necessary to achieve conversion of the alkali metal phosphite to alkai metal phosphate. After completion of the oxidation, the aqueous solution is separated from the catalyst.
    • 本发明涉及通过使碱金属亚磷酸盐水溶液用氧气或空气进行催化氧化来制备碱金属磷酸盐水溶液的方法。 更具体地说,在约30℃至110℃,pH值为0至约8的条件下,在含碱金属亚磷酸盐水溶液中的化学计量过量的氧气或空气中,在含有 至多10重量%的Al 2 O 3,只要需要实现碱金属亚磷酸盐转化为磷酸金属。 氧化完成后,将水溶液与催化剂分离。
    • 39. 发明授权
    • Continuous production of organic phosphines
    • 连续生产有机膦
    • US4163760A
    • 1979-08-07
    • US872250
    • 1978-01-25
    • Georg ElsnerGero HeymerHans-Werner Stephan
    • Georg ElsnerGero HeymerHans-Werner Stephan
    • C07F9/50C07F9/6568C07F9/54
    • C07F9/5059C07F9/65683
    • Organic phosphines are produced by reacting an alkylene, cycloalkylene or aralkylene in the presence of a free radical-yielding catalyst. More specifically, a pressure reactor, which is provided in its interior with mixing elements, kept free from oxygen, and subdivided so as to comprise an upper cooling zone and a lower reaction zone, is continuously supplied from above with (a) a solution of the alkylene, cycloalkylene or aralkylene and the catalyst in an inert solvent, and (b) a stoichiometric excess of hydrogen phosphide, the said (a) and (b) reactants being supplied jointly with but separately from one another; the (a) and (b) reactants are mixed in the upper cooling zone of the reactor at about 0.degree. to 35.degree. C. and under a PH.sub.3 -pressure of about 80 to 300 bars; the resulting mixture, which travels downwardly in the reactor, is reacted in the lower reaction zone at about 90.degree. to 190.degree. C., the reactants being allowed to remain in the reactor for a period of time about 13 to 15 times longer than the half life period of the catalyst; the reaction mixture is removed through the bottom portion of the reactor and subjected to distillation so as to separate the organic phosphines.
    • 有机膦通过在产生自由基的催化剂存在下使亚烷基,亚环烷基或亚芳烷基反应来制备。 更具体地,在其内部设置有保持无氧的并且被分为包括上部冷却区和下部反应区的混合元件的压力反应器从上方连续地供给(a) 所述(a)和(b)反应物是由彼此共同供应的;(b)化学计量过量的磷酸氢盐,所述(a)和(b) (a)和(b)反应物在反应器的上部冷却区中在约0℃至35℃下混合,并在约80至300巴的PH3压力下混合; 在反应器中向下移动的所得混合物在下部反应区中在约90℃至190℃下反应,使反应物在反应器中保留约13至15倍的时间 催化剂的半衰期; 将反应混合物通过反应器的底部除去并进行蒸馏以分离有机膦。