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公开(公告)号：US5654371A
公开(公告)日：1997-08-05
申请号：US460308
申请日：1995-06-02
IPC分类号： C08C19/44 , C08F4/08 , C08F4/46 , C08F4/48 , C08F12/04 , C08F12/06 , C08F36/04 , C08F279/02 , C08F8/00
摘要： A process for the preparation of hydrocarbon solutions of monofunctional ether initiators of the following general structure:M--Q.sub.n --Z--OA(R.sup.1 R.sup.2 R.sup.3) (II)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 alkenylsubstituted aromatic hydrocarbons; Z is defined as a branched or straight chain hydrocarbon tether or connecting group which contains 3-25 carbon atoms, optionally containing aryl or substituted aryl groups; 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, aryl or substituted aryl groups, and n is an integer from 1 to 5. monofunctional ethers produced by the process, use of the initiators in a polymerization process and polymers produced by the polymerization process.
摘要翻译： 一种制备以下一般结构的单官能醚引发剂的烃溶液的方法：M-Qn-Z-OA（R1R2R3）（Ⅱ）其中M定义为碱金属，选自锂，钠和 钾，Q是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饱和或不饱和烃基; Z定义为含有3-25个碳原子的支链或直链烃系链或连接基团，任选含有芳基或取代的芳基; 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，烷基，取代的烷基，芳基或取代的芳基，n是1至5的整数。 聚合过程中引发剂的使用以及通过聚合方法制备的聚合物。
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公开(公告)号：US5605872A
公开(公告)日：1997-02-25
申请号：US459585
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：MQnZN（A（R1R2R3））2金属，选自锂，钠和钾，Q是衍生的饱和或不饱和烃基 通过并入选自共轭二烯烃和烯基取代的芳族烃的化合物; 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：US5565526A
公开(公告)日：1996-10-15
申请号：US436780
申请日：1995-05-08
IPC分类号： C08C19/44 , C08F4/08 , C08F4/46 , C08F4/48 , C08F12/04 , C08F12/06 , C08F36/04 , C08F279/02 , C07F1/02
摘要： A process for the preparation of hydrocarbon solutions of monofunctional ether initiators of the following general structure:M--Q.sub.n --Z--OA(R.sup.1 R.sup.2 R.sup.3) (II)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 alkenylsubstituted aromatic hydrocarbons; Z is defined as a branched or straight chain hydrocarbon tether or connecting group which contains 3-25 carbon atoms, optionally containing aryl or substituted aryl groups; 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, aryl or substituted aryl groups, and n is an integer from 1 to 5. monofunctional ethers produced by the process, use of the initiators in a polymerization process and polymers produced by the polymerization process.
摘要翻译： 一种制备以下一般结构的单官能醚引发剂的烃溶液的方法：M-Qn-Z-OA（R1R2R3）（Ⅱ）其中M定义为碱金属，选自锂，钠和 钾，Q是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饱和或不饱和烃基; Z定义为含有3-25个碳原子的支链或直链烃系链或连接基团，任选含有芳基或取代的芳基; 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，烷基，取代的烷基，芳基或取代的芳基，n是1至5的整数。 聚合过程中引发剂的使用以及通过聚合方法制备的聚合物。
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公开(公告)号：US5527753A
公开(公告)日：1996-06-18
申请号：US354998
申请日：1994-12-13
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：MQnZN（A（R1R2R3））2金属，选自锂，钠和钾，Q是衍生的饱和或不饱和烃基 通过并入选自共轭二烯烃和烯基取代的芳族烃的化合物; 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：US06194617B1
公开(公告)日：2001-02-27
申请号：US08762071
申请日：1996-12-09
IPC分类号： C07C330
摘要： 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.
摘要翻译： 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。
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公开(公告)号：US5276219A
公开(公告)日：1994-01-04
申请号：US973116
申请日：1992-11-06
CPC分类号： C07C29/70
摘要： A process for producing clear, colorless solutions of branched lithium alkoxides containing 3 to 12 carbon atoms, in a polar reaction solvent, comprising reacting a dispersion of lithium metal having a particle size less than 300 microns with a minimum of 5 mole percent excess over stoichiometric of a branched alkyl alcohol containing 4 to 12 carbon atoms, in a polar reaction solvent as the reaction medium, at a temperature between 50.degree. C. and the boiling point of the solvent in an inert atmosphere.
摘要翻译： 一种在极性反应溶剂中生产含有3至12个碳原子的支链烷氧基化物的透明无色溶液的方法，包括将粒度小于300微米的锂金属分散体与超过化学计量比的至少5摩尔％过量反应 的在极性反应溶剂中作为反应介质的含有4至12个碳原子的支链烷基醇在惰性气氛中在50摄氏度和溶剂的沸点之间。
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7.发明授权Contaminant free organometallic amide compositions and processes for making same 失效污染物游离有机金属酰胺组合物及其制备方法
公开(公告)号：US6060617A
公开(公告)日：2000-05-09
申请号：US670348
申请日：1996-06-25
申请人： Randy W. Hall , Bobby J. McElroy , James A. Schwindeman , Conrad W. Kamienski , Terry L. Rathman , Robert C. Morrison
发明人： Randy W. Hall , Bobby J. McElroy , James A. Schwindeman , Conrad W. Kamienski , Terry L. Rathman , Robert C. Morrison
IPC分类号： C07C211/65 , C07F7/10
CPC分类号： C07F7/10 , C07C211/65
摘要： Organometallic amide compositions and processes for preparing the same, for example, by: reacting an alkali metal, alkali metal hydride, or alkali metal amide with a substituted amine in the absence of an electron carrier; reacting an alkali metal with a substituted amine in the presence of an electron carrier in a hydrocarbon solvent; distilling a composition which includes an alkali metal amide and a reduced electron carrier to recover the alkali metal amide; reacting an alkali metal with a substituted amine in the presence of an alkyl halide; and reacting a substituted amine capable of reacting with an alkali metal to form a hydrocarbon insoluble alkali metal amide with an alkali metal in the presence of a substituted amine capable of reacting with an alkali metal to form a hydrocarbon soluble alkali metal amide.
摘要翻译： 有机金属酰胺组合物及其制备方法，例如：在不存在电子载体的情况下使碱金属，碱金属氢化物或碱金属氨化物与取代的胺反应; 在电子载体存在下在烃溶剂中使碱金属与取代的胺反应; 蒸馏包含碱金属氨化物和还原电子载体以回收碱金属胺的组合物; 在烷基卤存在下使碱金属与取代的胺反应; 并使能够与碱金属反应的取代的胺与能够与碱金属反应形成烃溶性碱金属氨化物的取代胺存在下与碱金属形成不溶于烃的碱金属胺。
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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：US5583269A
公开(公告)日：1996-12-10
申请号：US437268
申请日：1995-05-08
摘要： 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.
摘要翻译： 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。
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