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公开(公告)号：US5976403A
公开(公告)日：1999-11-02
申请号：US65782
申请日：1998-04-23
申请人： B. Troy Dover , Conrad W. Kamienski , Robert C. Morrison , R. Thomas Currin, Jr. , James A. Schwindeman
发明人： B. Troy Dover , Conrad W. Kamienski , Robert C. Morrison , R. Thomas Currin, Jr. , James A. Schwindeman
IPC分类号： B01J13/00 , B22F1/00 , B22F9/06 , C01D7/00 , C01D15/08 , C09K3/00 , C07C31/30 , C07F1/02 , C07F1/04
CPC分类号： C01D7/00 , B01J13/0086 , B22F1/0088 , B22F9/06 , C01D15/08 , Y10S516/926 , Y10S516/928 , Y10T428/2991
摘要： 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.
摘要翻译： 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。
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公开(公告)号：US5776369A
公开(公告)日：1998-07-07
申请号：US639250
申请日：1996-04-22
申请人： B. Troy Dover , Conrad W. Kamienski , Robert C. Morrison , R. Thomas Currin, Jr. , James A. Schwindeman
发明人： B. Troy Dover , Conrad W. Kamienski , Robert C. Morrison , R. Thomas Currin, Jr. , James A. Schwindeman
CPC分类号： C01D7/00 , B01J13/0086 , B22F1/0088 , B22F9/06 , C01D15/08 , Y10S516/926 , Y10S516/928 , Y10T428/2991
摘要： 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 can be washed with a low boiling hydrocarbon to produce hydrocarbon wet particles which can be dried to produce atmospherically stable powders of coated metal particle 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 having low color and low soluble inorganic chloride levels.
摘要翻译： 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，油湿颗粒可以用低沸点烃洗涤以产生烃湿颗粒，其可以被干燥以产生包覆的金属颗粒的大气稳定的粉末分散的颗粒 在油中，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具有低颜色和低可溶性无机氯化物含量的有机金属化合物。
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公开(公告)号：US5523364A
公开(公告)日：1996-06-04
申请号：US458198
申请日：1995-06-02
申请人： John F. Engel , Conrad W. Kamienski , James A. Schwindeman , Randy W. Hall , Robert C. Morrison , B. Troy Dover
发明人： John F. Engel , Conrad W. Kamienski , James A. Schwindeman , Randy W. Hall , Robert C. Morrison , B. Troy Dover
摘要： A process for the preparation of hydrocarbon solutions of monofunctional amine initiators of the following general structures: ##STR1## wherein M is defined as an alkali metal, selected from the group consisting of lithium, sodium and potassium, Q is a saturated or unsaturated hydrocarbyl group derived by incorporation of a compound selected from the group consisting of conjugated diene hydrocarbons and alkenyl substituted aromatic hydrocarbons; Z is a hydrocarbon tether group which contains 3-25 carbon atoms; A is an element selected from Group IVa of the periodic table and R.sup.1, R.sup.2, and R.sup.3 are independently selected from hydrogen, alkyl, substituted alkyl, cycloalkyl, aryl or substituted aryl groups, m is an integer from 0 to 7, and n is an integer from 1 to 5, monofunctional amine initiators produced by the process, use of the initiators in a polymerization process and polymers produced by the polymerization process.
摘要翻译： 制备以下一般结构的单官能胺引发剂的烃溶液的方法：其中M定义为碱金属，其选自锂，钠和钾，Q是饱和或 通过引入选自共轭二烯烃和烯基取代的芳族烃的化合物衍生的不饱和烃基; Z是含有3-25个碳原子的烃系链基团; A是选自元素周期表IVa的元素，R1，R2和R3独立地选自氢，烷基，取代的烷基，环烷基，芳基或取代的芳基，m是0-7的整数，n是 1至5的整数，通过该方法制备的单官能胺引发剂，在聚合方法中使用引发剂和通过聚合方法制备的聚合物。
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公开(公告)号：US5550203A
公开(公告)日：1996-08-27
申请号：US460305
申请日：1995-06-02
申请人： John F. Engel , Conrad W. Kamienski , James A. Schwindeman , Randy W. Hall , Robert C. Morrison , B. Troy Dover
发明人： John F. Engel , Conrad W. Kamienski , James A. Schwindeman , Randy W. Hall , Robert C. Morrison , B. Troy Dover
摘要： A process for the preparation of hydrocarbon solutions of monofunctional amine initiators of the following general structures:M--Q.sub.n --Z--N(A(R.sup.1 R.sup.2 R.sup.3)).sub.2or ##STR1## wherein M is defined as an alkali metal, selected from the group consisting of lithium, sodium and potassium, Q is a saturated or unsaturated hydrocarbyl group derived by incorporation of a compound selected from the group consisting of conjugated diene hydrocarbons and alkenyl substituted aromatic hydrocarbons; Z is a hydrocarbon tether group which contains 3-25 carbon atoms; A is an element selected from Group IVa of the periodic table and R.sup.1, R.sup.2, and R.sup.3 are independently selected from hydrogen, substituted alkyl, cycloalkyl, aryl or substituted aryl groups, m is an integer from 0 to 7, and n is an integer from 1 to 5, monofunctional amine initiators produced by the process, use of the initiators in a polymerization process and polymers produced by the polymerization process.
摘要翻译： 制备以下一般结构的单官能胺引发剂的烃溶液的方法：选自锂，钠和钾的M-Qn-ZN（A（R1R2R3））2金属，Q是饱和或 通过引入选自共轭二烯烃和烯基取代的芳族烃的化合物衍生的不饱和烃基; Z是含有3-25个碳原子的烃系链基团; A是选自元素周期表Ⅳa的元素，R 1，R 2和R 3独立地选自氢，取代的烷基，环烷基，芳基或取代的芳基，m是0至7的整数，n是整数 1至5个，通过该方法制备的单官能胺引发剂，在聚合过程中使用引发剂和通过聚合方法制备的聚合物。
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公开(公告)号：US5523447A
公开(公告)日：1996-06-04
申请号：US477843
申请日：1995-06-07
CPC分类号： C07F1/02
摘要： A process for preparing easily separable solutions of organolithium compounds comprising the steps of reacting lithium metal, in the form of cast or extruded ingots or pieces cut therefrom, with an organo halide in mole ratios ranging from 3:1 to 20:1 in a solvent selected form a group of liquid hydrocarbons, alkyl ethers, and mixtures thereof under an inert atmosphere for one to ten hours with moderate stirring, cooling the resulting product, and separating the solution of the organolithium compound from the reacted lithium metal and by-product lithium chloride in the reactor.
摘要翻译： 一种用于制备容易分离的有机锂化合物溶液的方法，包括以下步骤：将以铸造或挤出的锭或其切割的碎片形式的锂金属与摩尔比为3:1至20:1的有机卤化物在溶剂 在惰性气氛下选择形成一组液体烃，烷基醚及其混合物，在适度搅拌下搅拌1至10小时，冷却所得产物，并将有机锂化合物的溶液与反应的锂金属和副产物锂 氯化物在反应器中。
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公开(公告)号：US5332533A
公开(公告)日：1994-07-26
申请号：US87582
申请日：1993-07-06
申请人： James A. Schwindeman , Robert C. Morrison , B. Troy Dover , John F. Engel , Conrad W. Kamienski , Randy W. Hall , Douglas E. Sutton
发明人： James A. Schwindeman , Robert C. Morrison , B. Troy Dover , John F. Engel , Conrad W. Kamienski , Randy W. Hall , Douglas E. Sutton
IPC分类号： C07F1/02
CPC分类号： C07F1/02
摘要： A high temperature process for producing alkyllithium compounds in high yields of at least 90% and high purity comprising reacting, in a liquid hydrocarbon solvent, an alkyl halide containing 3 to 16 carbon atoms and mixtures thereof with lithium metal particles of less than 300 microns in size at a temperature between 35.degree. and 125.degree. C. and recovering the alkyllithium compound.
摘要翻译： 用于以高产率生产烷基锂化合物的高温方法为至少90％和高纯度，包括在液体烃溶剂中将含有3至16个碳原子的烷基卤及其与小于300微米的锂金属颗粒的混合物反应 在35〜125℃的温度下回收烷基锂化合物。
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公开(公告)号：US5211887A
公开(公告)日：1993-05-18
申请号：US749245
申请日：1991-08-22
IPC分类号： C07F1/02
CPC分类号： C07F1/02
摘要： A process for the preparation of alkyllithium compounds including 2-alkyl-substituted alkyllithium compounds by reacting in a liquid organic solvent, in an inert atmosphere a C.sub.2 to C.sub.18 saturated, acyclic, primary alkyl halide including 2-alkyl-substituted alkyl halides with a dispersion of particulate lithium and sodium metals in which there is 5 to 50 mole percent sodium based on the lithium content at a temperature of 0.degree. to a temperature up to but not exceeding the decomposition temperature of the product.
摘要翻译： 包括2-烷基取代的烷基锂化合物在内的烷基锂化合物的制备方法，其在液体有机溶剂中，在惰性气氛中，C2至C18饱和无环的包含2-烷基取代的烷基卤化物的烷基卤化物与分散体 的锂和钠金属颗粒，其中基于锂含量为5至50摩尔％的钠，其温度为0℃至高于但不超过产物的分解温度。
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公开(公告)号：US5145600A
公开(公告)日：1992-09-08
申请号：US391811
申请日：1989-08-09
申请人： Conrad W. Kamienski , B. Troy Dover
发明人： Conrad W. Kamienski , B. Troy Dover
IPC分类号： C07F3/02
CPC分类号： C07F3/02
摘要： This invention concerns an improved process for preparing a hydrocarbon soluble dialkylmagnesium compound by reacting a dialkylmagnesium-magnesium chloride composition in an inert hydrocarbon solvent with a chemical selected from an alkali metal alkyl compound and an alkali metal trialkylmagnesiate compound and dialkylmagnesium compounds of the formulaMgR.sub.a R.sup.1.sub.b R.sup.2.sub.c R.sup.3.sub.d R.sup.4.sub.ewherein a+b+c+d=2, R is a 2-alkylsubstituted primary alkyl group and R.sup.1, R.sup.2, R.sup.3 and R.sup.4 are hydrocarbyl groups which may be the same or different.
摘要翻译： 本发明涉及通过使二烷基镁 - 氯化镁组合物在惰性烃溶剂中与选自碱金属烷基化合物和碱金属三烷基镁化合物的化学式和式MgRaR1bR2cR3dR4e的二烷基镁化合物反应来制备烃溶性二烷基镁化合物的改进方法，其中 a + b + c + d = 2，R是2-烷基取代的伯烷基，R 1，R 2，R 3和R 4是可以相同或不同的烃基。
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