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公开(公告)号：US08298446B2
公开(公告)日：2012-10-30
申请号：US12682451
申请日：2008-09-12
CPC分类号： C08F2/18 , C08F14/22 , H01M4/621 , H01M4/623 , H01M10/052 , Y02P20/544
摘要： A method for producing a vinylidene fluoride based polymer powder having a high molecular weight and excellent solubility in an organic solvent, which is useful as an electrode binder for nonaqueous cells, is provided. Methods for producing an NMP solution and an electrode mixture are also provided.A vinylidene fluoride based polymer powder produced by supercritical suspension polymerization in an aqueous dispersion medium wherein a volume of pores having a pore diameter of 0.03 μm to 1.0 μm, as measured by a mercury porosimeter, is 77 vol % to 93 vol % of a total pore volume and an inherent viscosity is 2.0 dl/g or greater is obtained.
摘要翻译： 本发明提供了可用作非水电池用电极粘合剂的有机溶剂中具有高分子量和溶解性优异的偏二氟乙烯类聚合物粉末的制造方法。 还提供了制备NMP溶液和电极混合物的方法。 通过在水分散介质中通过超临界悬浮聚合制造的偏二氟乙烯基聚合物粉末，其中通过水银孔率计测量的孔径为0.03μm至1.0μm的孔的体积为总共的77vol％至93vol％ 孔体积和特性粘度为2.0dl / g以上。
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公开(公告)号：US20100270509A1
公开(公告)日：2010-10-28
申请号：US12682451
申请日：2008-09-12
CPC分类号： C08F2/18 , C08F14/22 , H01M4/621 , H01M4/623 , H01M10/052 , Y02P20/544
摘要： A method for producing a vinylidene fluoride based polymer powder having a high molecular weight and excellent solubility in an organic solvent, which is useful as an electrode binder for nonaqueous cells, is provided. Methods for producing an NMP solution and an electrode mixture are also provided.A vinylidene fluoride based polymer powder produced by supercritical suspension polymerization in an aqueous dispersion medium wherein a volume of pores having a pore diameter of 0.03 μm to 1.0 μm, as measured by a mercury porosimeter, is 77 vol % to 93 vol % of a total pore volume and an inherent viscosity is 2.0 dl/g or greater is obtained.
摘要翻译： 本发明提供了可用作非水电池用电极粘合剂的有机溶剂中具有高分子量和溶解性优异的偏二氟乙烯类聚合物粉末的制造方法。 还提供了制备NMP溶液和电极混合物的方法。 通过在水分散介质中通过超临界悬浮聚合制备的偏二氟乙烯基聚合物粉末，其中通过水银孔率计测量的孔径为0.03μm至1.0μm的孔的体积为总共的77vol％至93vol％ 孔体积和特性粘度为2.0dl / g以上。
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公开(公告)号：US5744576A
公开(公告)日：1998-04-28
申请号：US888599
申请日：1997-07-07
CPC分类号： C08G75/0254
摘要： In a process for producing poly(phenylene sulfide), in which an alkali metal sulfide is reacted with a dihalo-aromatic compound in an organic amide solvent, the reaction is conducted through the following Steps 1 and 2, thereby efficiently providing granular, high-molecular weight poly(phenylene sulfide) having excellent whiteness in a short period of time and at a high yield. Step 1: a step comprising reacting the alkali metal sulfide with the dihalo-aromatic compound within a temperature range of 170.degree.-270.degree. C. in the organic amide solvent containing water in a proportion of 0.5-2.0 moles per mole of the alkali metal sulfide charged while raising the reaction temperature at an average heating rate of 0.1.degree.-1.degree. C./min in at least a temperature range of from 220.degree. C. to 240.degree. C., so as to give a conversion of the dihalo-aromatic compound of 70-98 mol %, thereby forming a: prepolymer of poly(phenylene sulfide); and Step 2: a step comprising adding water to the reaction system at a temperature of at least 235.degree. C. in such a manner that water is present in a proportion of 2.1-10 moles per mole of the alkali metal sulfide charged, and continuing the reaction for 0.5-10 hours within a temperature range of 245.degree.-290.degree. C., thereby converting the prepolymer to high-molecular weight poly(phenylene sulfide).
摘要翻译： 在有机酰胺溶剂中使碱金属硫化物与二卤芳香族化合物反应的聚苯硫醚的制造方法中，通过以下的工序1和2进行反应， 分子量的聚（苯硫醚）在短时间内具有优异的白度并以高产率。 步骤1：包括使碱金属硫化物与二卤代芳族化合物在170-270℃的温度范围内反应，所述有机酰胺溶剂含有0.5-2.0摩尔/摩尔碱金属的比例的水 硫化物在220℃至240℃的至少220℃的温度范围内以0.1-1℃/分钟的平均加热速率升高反应温度，从而使二卤代 - 芳族化合物为70-98mol％，从而形成：聚苯硫醚的预聚物; 和步骤2：包括在至少235℃的温度下向反应体系中加入水的步骤，使得水以每摩尔所加入的碱金属硫化物为2.1-10摩尔的比例存在，并且继续 在245〜-290℃的温度范围内反应0.5-10小时，由此将预聚物转化为高分子量聚苯硫醚。
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公开(公告)号：US20090156780A1
公开(公告)日：2009-06-18
申请号：US12370201
申请日：2009-02-12
IPC分类号： C08G75/14
CPC分类号： C08G75/0259
摘要： A dehydration step is conducted by heating a mixture containing an organic amide solvent and a sulfur source including an alkali metal hydrosulfide, and a part of an overall charged amount of an alkali metal hydroxide as needed. The mixture remaining within the system after the dehydration step is mixed with a dihalo-aromatic compound, the resultant mixture is heated to conduct a polymerization reaction, and the alkali metal hydroxide is added to the mixture for polymerization reaction continuously or in portions to control the pH of the mixture for polymerization reaction within a range of from 7 to 12.5 from the beginning to the end of the polymerization reaction. The poly(arylene sulfide) according to the present invention has a nitrogen content of at most 800 ppm.
摘要翻译： 通过根据需要加热含有有机酰胺溶剂和包含碱金属氢硫化物的硫源的混合物和总量的碱金属氢氧化物的一部分来进行脱水步骤。 将脱水步骤后残留在体系内的混合物与二卤代芳族化合物混合，加热所得混合物进行聚合反应，并将碱金属氢氧化物连续地或部分加入到混合物中用于聚合反应，以控制 从聚合反应的开始到结束，聚合反应的混合物的pH在7至12.5的范围内。 本发明的聚（亚芳基硫醚）的氮含量为800ppm以下。
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5.发明授权Method of producing anode material for non-aqueous electrolyte secondary battery 有权制造非水电解质二次电池用负极材料的方法公开(公告)号：US08945445B2
公开(公告)日：2015-02-03
申请号：US13188008
申请日：2011-07-21
申请人： Hajime Komatsu , Kenjiro Hara , Michihisa Miyahara
发明人： Hajime Komatsu , Kenjiro Hara , Michihisa Miyahara
IPC分类号： B28B1/00 , H01M10/0525 , C04B35/528 , C04B35/626 , H01M4/587
CPC分类号： H01M10/0525 , C04B35/528 , C04B35/6269 , C04B2235/5427 , C04B2235/5436 , C04B2235/602 , C04B2235/663 , C04B2235/723 , C04B2235/95 , H01M4/587 , Y02E60/122 , Y02P70/54 , Y02T10/7011
摘要： Provided is a method of producing an anode material for a non-aqueous electrolyte secondary battery having battery characteristics equivalent to those of a conventional product by simpler production steps than those of a conventional method.A thermally-polymerized petroleum based or coal based pitch is cooled to the softening point or below so that the pitch is solidified to obtain a solidified pitch. The solidified pitch is ground to form a fine pitch powder having an average particle size (median size) of 60 μm or smaller. Then, the fine pitch powder is compression molded at a pressure of 20 to 100 MPa or 0.1 to 6 MN/m to form a porous compression molded pitch. The porous compression molded pitch is subjected to infusibilization treatment.
摘要翻译： 提供一种通过比常规方法更简单的制造步骤制造具有与常规产品相当的电池特性的非水电解质二次电池用负极材料的方法。 将热聚合的石油基或煤基沥青冷却至软化点或更低，使得沥青固化以获得固化沥青。 将固化沥青研磨成平均粒径（中值粒径）为60μm以下的细间距粉末。 然后，在20〜100MPa或0.1〜6MN / m 2的压力下对细间距粉末进行压缩成型，形成多孔压缩成型间距。 将多孔压缩成形间距进行不熔化处理。
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公开(公告)号：US20110253928A1
公开(公告)日：2011-10-20
申请号：US13141740
申请日：2009-12-14
IPC分类号： H01M4/88
CPC分类号： H01M4/587 , C01B32/05 , H01M4/0404 , H01M4/1393 , H01M10/052 , H01M2010/4292 , Y02E60/122 , Y02P70/54
摘要： There are provided a method of producing an anode material for a non-aqueous electrolyte secondary battery which is suitable for use in a high input/output current-type non-aqueous electrolyte secondary battery exemplified by a non-aqueous electrolyte secondary battery for a hybrid electric vehicle (HEV), has reduced irreversible capacity and superior charge-discharge efficiency, and an anode material obtained by the above production method.A method of producing an anode material for a non-aqueous electrolyte secondary battery from a petroleum-based pitch material, comprising a tar removal step in which an infusibilized pitch having an oxygen content of 5 to 20 wt % is heated to a temperature of 480° C. to 700° C. while flowing an inert gas at the space velocity of 0 to 120 (min−1).
摘要翻译： 提供了一种适用于高输入输出电流型非水电解质二次电池的非水电解质二次电池用负极材料的制造方法，其特征在于，以非水电解质二次电池 电动车辆（HEV）具有降低的不可逆容量和优异的充放电效率，以及通过上述制造方法得到的负极材料。 一种从石油基沥青材料制造非水电解质二次电池用负极材料的方法，其特征在于，将含有5〜20重量％氧含量的熔融沥青加热至480℃的焦油除去工序 同时以0〜120（min-1）的空速流动惰性气体。
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公开(公告)号：US07094867B2
公开(公告)日：2006-08-22
申请号：US10497525
申请日：2002-11-29
IPC分类号： C08F6/00
CPC分类号： C08G75/0281 , C08G75/0213 , C08G75/0254
摘要： A polymerizate slurry obtained through a reaction of an alkali sulfide source and an aromatic dihalide compound in an organic polar solvent and comprising polyarylene sulfide particles, a by-produced alkali metal salt and the polar organic solvent, is continuously contacted countercurrently with a washing liquid, thereby continuously and efficiently recovering washed polyarylene sulfide particles. Furthermore, the by-produced alkali metal salt is removed, and the polar organic solvent is recovered, efficiently.
摘要翻译： 通过碱金属硫化物源和芳族二卤化物在有机极性溶剂中反应并且包含聚芳硫醚颗粒，副产物碱金属盐和极性有机溶剂而获得的聚合物浆料与洗涤液体逆流地连续接触， 从而连续有效地回收洗涤的聚芳硫醚颗粒。 此外，除去副产的碱金属盐，有效地回收极性有机溶剂。
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公开(公告)号：US07767783B2
公开(公告)日：2010-08-03
申请号：US12370201
申请日：2009-02-12
CPC分类号： C08G75/0259
摘要： A dehydration step is conducted by heating a mixture containing an organic amide solvent and a sulfur source including an alkali metal hydrosulfide, and a part of an overall charged amount of an alkali metal hydroxide as needed. The mixture remaining within the system after the dehydration step is mixed with a dihalo-aromatic compound, the resultant mixture is heated to conduct a polymerization reaction, and the alkali metal hydroxide is added to the mixture for polymerization reaction continuously or in portions to control the pH of the mixture for polymerization reaction within a range of from 7 to 12.5 from the beginning to the end of the polymerization reaction. The poly(arylene sulfide) according to the present invention has a nitrogen content of at most 800 ppm.
摘要翻译： 通过根据需要加热包含有机酰胺溶剂和包含碱金属氢硫化物的硫源的混合物和总量的碱金属氢氧化物的一部分来进行脱水步骤。 将脱水步骤后残留在体系内的混合物与二卤代芳族化合物混合，加热所得混合物进行聚合反应，并将碱金属氢氧化物连续地或部分加入到混合物中用于聚合反应，以控制 从聚合反应的开始到结束，聚合反应的混合物的pH在7至12.5的范围内。 本发明的聚（亚芳基硫醚）的氮含量为800ppm以下。
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公开(公告)号：US07504476B2
公开(公告)日：2009-03-17
申请号：US10542543
申请日：2004-01-21
CPC分类号： C08G75/0259
摘要： A dehydration step is conducted by heating a mixture containing an organic amide solvent and a sulfur source including an alkali metal hydrosulfide, and a part of an overall charged amount of an alkali metal hydroxide as needed. The mixture remaining within the system after the dehydration step is mixed with a dihalo-aromatic compound, the resultant mixture is heated to conduct a polymerization reaction, and the alkali metal hydroxide is added to the mixture for polymerization reaction continuously or in portions to control the pH of the mixture for polymerization reaction within a range of from 7 to 12.5 from the beginning to the end of the polymerization reaction. The poly(arylene sulfide) according to the present invention has a nitrogen content of at most 800 ppm.
摘要翻译： 通过根据需要加热包含有机酰胺溶剂和包含碱金属氢硫化物的硫源的混合物和总量的碱金属氢氧化物的一部分来进行脱水步骤。 将脱水步骤后残留在体系内的混合物与二卤代芳族化合物混合，加热所得混合物进行聚合反应，并将碱金属氢氧化物连续地或部分加入到混合物中用于聚合反应，以控制 从聚合反应的开始到结束，聚合反应的混合物的pH在7至12.5的范围内。 本发明的聚（亚芳基硫醚）的氮含量为800ppm以下。
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公开(公告)号：US20050087215A1
公开(公告)日：2005-04-28
申请号：US10497525
申请日：2002-11-29
CPC分类号： C08G75/0281 , C08G75/0213 , C08G75/0254
摘要： A polymerizate slurry obtained through a reaction of an alkali sulfide source and an aromatic dihalide compound in an organic polar solvent and comprising polyarylene sulfide particles, a by-produced alkali metal salt and the polar organic solvent, is continuously contacted countercurrently with a washing liquid, thereby continuously and efficiently recovering washed polyarylene sulfide particles. Furthermore, the by-produced alkali metal salt is removed, and the polar organic solvent is recovered, efficiently.
摘要翻译： 通过碱金属硫化物源和芳族二卤化物在有机极性溶剂中反应并且包含聚芳硫醚颗粒，副产物碱金属盐和极性有机溶剂而获得的聚合物浆料与洗涤液体逆流地连续接触， 从而连续有效地回收洗涤的聚芳硫醚颗粒。 此外，除去副产的碱金属盐，有效地回收极性有机溶剂。
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