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    • 1. 发明授权
    • Aryllithium products and processes
    • 芳基锂产品和工艺
    • US5626798A
    • 1997-05-06
    • US587813
    • 1996-01-05
    • James A. SchwindemanDouglas E. SuttonRobert C. MorrisonSonia S. Stryker
    • James A. SchwindemanDouglas E. SuttonRobert C. MorrisonSonia S. Stryker
    • C07F1/02
    • C07F1/02
    • An improved process for producing high purity solutions of aryllithium compounds comprising reacting a particulate alkali metal having a particle size in the range of 10 to 300 microns, with an aryl halide in a normally liquid etheral solvent of the formula ROR.sup.1, wherein R and R.sup.1 are selected from the group of alkyl radicals containing from 3 to 6 carbon atoms, in the presence of a Lewis base compound selected from compounds of the formula: R.sup.2 AR.sup.3 (R.sup.4).sub.z and ##STR1## wherein A is selected from oxygen, nitrogen, phosphorus or sulfur; R.sup.2, R.sup.3, and R.sup.4 are selected from alkyl radicals containing from 1 to 6 carbon atoms; R.sup.5 and R.sup.6 are independently selected from hydrogen or alkyl radicals containing one to six carbon atoms; y is an integer from 4 to 6; but when A is oxygen or sulfur, z is zero; and when A is nitrogen or phosphorus, z is one, and provided there is a mole ratio of ether to aryl halide of at least 1.3 to 1 and a mole ratio of Lewis base to aryl halide of from 0.01 to 0.50; and products of the process.
    • 一种用于生产芳族锂化合物的高纯度溶液的改进方法,包括使粒度在10-300微米范围内的颗粒状碱金属与式ROR1的通常液体的醚类溶剂中的芳基卤反应,其中R和R 1是 在选自下列化合物的路易斯碱化合物存在下,选自含有3至6个碳原子的烷基基团:R2AR3(R4)z和其中A选自氧,氮,磷或 硫; R2,R3和R4选自含有1至6个碳原子的烷基; R 5和R 6独立地选自氢或含有1至6个碳原子的烷基; y为4〜6的整数; 但当A为氧或硫时,z为零; 当A为氮或磷时,z为1,并且其醚与芳基卤的摩尔比至少为1.3:1,路易斯碱与芳基卤的摩尔比为0.01至0.50; 和产品的过程。
    • 7. 发明授权
    • Lithium tertiary alkoxides
    • 锂叔醇盐
    • US06194617B1
    • 2001-02-27
    • US08762071
    • 1996-12-09
    • Robert C. MorrisonConrad W. KamienskiJames A. Schwindeman
    • Robert C. MorrisonConrad W. KamienskiJames A. Schwindeman
    • C07C330
    • C07C31/30C07C29/70
    • A process for quickly preparing easily separable solutions of lithium tertiary-alkoxides. Comprising the steps of reacting lithium metal in bulk solid form, containing less than 0.1% by weight of sodium, with a tertiary alcohol in mole ratios of metal to alcohol ranging from 2 to 1 to 10 to 1 in a solvent selected from ethereal or hydrocarbon solvents under an inert atmosphere at elevated temperature for 1 to 10 hours, cooling the product and separating the product solution from the unreacted lithium metal in the reactor, and optionally adding solvent and sufficient lithium metal and alcohol to said unreacted metal in said reactor to maintain said mole ratio of lithium metal to alcohol, and continuing the reaction, thereby to form further lithium tert-alkoxide, and repeating said steps a number of times.
    • 一种用于快速制备易于分离的叔醇锂溶液的方法。 包括将含有小于0.1重量%钠的块状固体形式的锂金属与选自醚或烃的溶剂中的金属与醇的摩尔比范围为2至1至10比1的叔醇反应的步骤 溶剂在惰性气氛下在升高的温度下搅拌1至10小时,冷却产物并将产物溶液与反应器中的未反应的锂金属分离,并且任选地向所述反应器中的所述未反应金属加入溶剂和足够的锂金属和醇以维持 锂金属与醇的摩尔比,并继续反应,从而形成另外的叔 - 醇氧化物,并重复所述步骤多次。
    • 10. 发明授权
    • Organoalkali compounds and their preparation
    • 有机碱化合物及其制备方法
    • US5976403A
    • 1999-11-02
    • US65782
    • 1998-04-23
    • B. Troy DoverConrad W. KamienskiRobert C. MorrisonR. Thomas Currin, Jr.James A. Schwindeman
    • B. Troy DoverConrad W. KamienskiRobert C. MorrisonR. Thomas Currin, Jr.James A. Schwindeman
    • B01J13/00B22F1/00B22F9/06C01D7/00C01D15/08C09K3/00C07C31/30C07F1/02C07F1/04
    • C01D7/00B01J13/0086B22F1/0088B22F9/06C01D15/08Y10S516/926Y10S516/928Y10T428/2991
    • A process for producing dispersions of atmospherically stable, coated alkali metal particles and atmospherically stable, coated alkali metal powders by agitating a mixture of molten alkali metal in a hydrocarbon oil at dispersion speeds, optionally in the presence of a dispersing agent, contacting the molten alkali metal-hydrocarbon oil dispersion, above or below the surface of the dispersion, with up to 3 weight percent anhydrous carbon dioxide while agitating the dispersion for at least 1 minute. The dispersion in oil can be used directly in chemical reactions. The bulk of the oil can be removed from the dispersions to produce oil wet particles, the oil wet particles car be washed with a low boiling hydrocarbon to produce hydrocarbon wet particles which can be dried to produce atmospherically stable powders of coated metal particles. The dispersed particles in oil, the oil wet particles, the hydrocarbon wet particles and the atmospherically stable powders can each be used in chemical reactions. After washing and drying, the process produces lithium powders having a surface coating composition containing 0.1-0.3 atom percent lithium, 0.3-0.4 atom percent carbon, and 0.3-0.5 atom percent oxygen. The products of the invention may be used to synthesize organometallic compounds, esp. n-butyl lithium and sec-butyl lithium, having low color and low soluble inorganic chloride levels.
    • 通过搅拌熔融碱金属在烃油中的分散速度的混合物,任选地在分散剂存在下,使熔融碱接触,制备大气稳定的涂覆的碱金属颗粒和大气稳定的包覆的碱金属粉末的分散体的方法 在分散体表面上方或下方的金属 - 烃油分散体与最多3重量%的无水二氧化碳同时搅拌分散体至少1分钟。 油中的分散体可以直接用于化学反应。 大部分油可以从分散体中除去以产生油湿颗粒,用低沸点烃洗涤油湿颗粒汽车以产生烃湿颗粒,其可以被干燥以产生大气稳定的涂覆金属颗粒的粉末。 油中的分散颗粒,油湿颗粒,烃湿颗粒和气氛稳定的粉末均可用于化学反应。 洗涤和干燥后,该方法产生具有表面涂层组合物的锂粉末,其中含有0.1-0.3%原子百分比的锂,0.3-0.4%的碳和0.3-0.5%的氧。 本发明的产品可用于合成有机金属化合物, 正丁基锂和仲丁基锂,颜色低,可溶性无机氯化物水平低。