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1. 发明授权

US09777115B2 Xylylenediamine composition and method for producing polyamide resin 有权
公开(公告)号：US09777115B2
公开(公告)日：2017-10-03
申请号：US15032031
申请日：2014-10-29
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Takashi Nakamura , Hajime Yamada , Tatsuya Tochihara , Katsumi Shinohara , Jun Mitadera , Takashi Yamamoto
IPC分类号： C08G69/26 , C08G69/28 , C08G69/30
CPC分类号： C08G69/265 , C08G69/26 , C08G69/28 , C08G69/30 , C08K5/0083 , C08K5/17 , C08K5/3432 , C08L77/06
摘要： Provided are [1] a xylylenediamine composition containing xylylenediamine and a pyridine compound (A) having at least one substituent including an amino group, wherein the content of the pyridine compound (A) is 0.001 to 0.1 parts by mass based on 100 parts by mass of the xylylenediamine; and [2] a method for producing a polyamide resin including the steps of introducing a pyridine compound (A) having at least one substituent including an amino group, a diamine including xylylenediamine (but excluding a diamine corresponding to the above-mentioned pyridine compound (A)), and a dicarboxylic acid into a reaction system and performing a polycondensation reaction, wherein the amount of the pyridine compound (A) to be introduced is 0.001 to 0.1 parts by mass based on 100 parts by mass of xylylenediamine.

2. 发明授权

US09637594B2 Xylylene diamine composition, and method for producing polyamide resin 有权
公开(公告)号：US09637594B2
公开(公告)日：2017-05-02
申请号：US15032020
申请日：2014-10-29
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Tatsuya Tochihara , Katsumi Shinohara , Takashi Nakamura , Hajime Yamada , Jun Mitadera , Takashi Yamamoto
IPC分类号： C08G69/26 , C08G69/28 , C08G59/50 , C08G69/30
CPC分类号： C08G69/28 , C08G59/50 , C08G59/5033 , C08G69/26 , C08G69/265 , C08G69/30 , C08K5/0083 , C08K5/17 , C08K5/18 , C08L77/06
摘要： Provided are [1] a xylylenediamine composition containing xylylenediamine and a compound represented by the following general formula (1), wherein the content of the compound represented by the general formula (1) is 0.001 to 0.1 parts by mass based on 100 parts by mass of the xylylenediamine; and a method for producing a polyamide resin including the steps of introducing a compound represented by the following general formula (1), a diamine including xylylenediamine (but excluding the compound represented by the general formula (1)), and a dicarboxylic acid into a reaction system and performing a polycondensation reaction, wherein the amount of the compound represented by the general formula (1) to be introduced is 0.001 to 0.1 parts by mass based on 100 parts by mass of the xylylenediamine, where, in the general formula (1), n and m each independently represent an integer of 0 to 6, excluding the case where n and m are both 1.

3. 发明授权

US10227451B2 Method for producing polyamide 有权
公开(公告)号：US10227451B2
公开(公告)日：2019-03-12
申请号：US15310654
申请日：2015-05-08
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Tatsuya Tochihara , Katsumi Shinohara , Kuniaki Muneyasu
IPC分类号： C08G69/28 , C08K3/32
摘要： A method for producing a polyamide, comprising performing melt polycondensation of a diamine component comprising xylylenediamine in an amount of 70 mol % or more and a dicarboxylic acid component comprising a linear aliphatic dicarboxylic acid having 6 to 18 carbon atoms in an amount of 70 mol % or more in the presence of a phosphorus atom-containing compound (A), wherein the decomposition temperature of the phosphorus atom-containing compound (A) is not lower than the melting point of the polyamide, and an aqueous solution of the phosphorus atom-containing compound (A) and the diamine component are added to the dicarboxylic acid component being in a molten state to perform the melt polycondensation.

4. 发明授权

US09783638B2 Xylylenediamine composition and method for producing polyamide resin 有权
公开(公告)号：US09783638B2
公开(公告)日：2017-10-10
申请号：US15032029
申请日：2014-10-29
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Tatsuya Tochihara , Katsumi Shinohara , Takashi Nakamura , Hajime Yamada , Jun Mitadera , Takashi Yamamoto
IPC分类号： C08G69/26 , C08G69/06 , C08L77/06 , C08G69/28 , C08G59/50 , C08L79/02
CPC分类号： C08G69/06 , C08G59/50 , C08G59/5033 , C08G69/26 , C08G69/265 , C08G69/28 , C08K5/0083 , C08K5/01 , C08L77/06 , C08L79/02
摘要： Provided are [1] a xylylenediamine composition containing xylylenediamine and 1,2-ditolylethane wherein the content of 1,2-ditolylethane is 0.001 to 0.02 parts by mass based on 100 parts by mass of the xylylenediamine; and [2] a method for producing a polyamide resin including the steps of introducing a diamine containing xylylenediamine, a dicarboxylic acid, and 1,2-ditolylethane into a reaction system and performing polycondensation reaction, wherein the amount of the 1,2-ditolylethane to be introduced is 0.001 to 0.02 parts by mass based on 100 parts by mass of the xylylenediamine.

5. 发明授权

US09562144B2 Xylylenediamine composition, and method for producing polyamide resin 有权
标题翻译：苯二胺组合物，聚酰胺树脂的制造方法
公开(公告)号：US09562144B2
公开(公告)日：2017-02-07
申请号：US14648006
申请日：2014-04-09
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Tatsuya Tochihara , Katsumi Shinohara , Takashi Nakamura , Hajime Yamada , Jun Mitadera
IPC分类号： C08K5/17 , C08G69/30 , C08G59/50 , C08G69/28 , C08G69/26 , C08L77/06
CPC分类号： C08K5/17 , C08G59/50 , C08G59/5033 , C08G69/265 , C08G69/28 , C08G69/30 , C08L77/06
摘要： Provided are a xylylenediamine composition containing xylylenediamine and bis(methylbenzyl)amine, a content of the bis(methylbenzyl)amine being 0.0005 to 0.1 parts by mass based on 100 parts by mass of the xylylenediamine; and a method for producing a polyamide resin including the steps of introducing a diamine containing xylylenediamine, a dicarboxylic acid, and bis(methylbenzyl)amine in an amount of 0.0005 to 0.1 parts by mass based on 100 parts by mass of the xylylenediamine into a reaction system and performing a polycondensation reaction.
摘要翻译：本发明提供含有苯二甲胺和双（甲基苄基）胺的苯二甲胺类组合物，相对于100质量份的苯二甲胺，双（甲基苄基）胺的含量为0.0005〜0.1质量份; 和聚酰胺树脂的制造方法，包括以相对于100质量份的苯二甲胺为基准的0.0005〜0.1质量份的二胺的二甲苯二胺，二羧酸和双（甲基苄基）胺的引入反应的工序，并进行缩聚反应。

6. 发明申请

US20150291736A1 METHOD FOR PRODUCING POLYAMIDE 审中-公开
标题翻译：生产聚酰胺的方法
公开(公告)号：US20150291736A1
公开(公告)日：2015-10-15
申请号：US14440407
申请日：2013-10-22
申请人： MITSUBISHI GAS CHEMICAL COMPANY, INC.
发明人： Kuniaki Muneyasu , Yuya Kimura , Katsumi Shinohara , Tatsuya Tochihara , Hideyuki Kurose
IPC分类号： C08G69/26
CPC分类号： C08G69/26 , C08G69/265 , C08G69/28
摘要： The invention is a method for producing a polyamide having a melting point of 255° C. or higher through polycondensation of a mixed xylylenediamine containing paraxylylenediamine as a diamine component and a dicarboxylic acid component in a batch reactor, wherein when the diamine component is dropwise added to the dicarboxylic acid component kept in a melt state by heating it to a temperature not lower than a melting point thereof under a pressure of 0.1 MPaG or more with keeping the melt state of a reaction mixture, a temperature of the reaction mixture is maintained at 255° C. or lower until a molar ratio (diamine component/dicarboxylic acid component) of the reaction mixture reaches 0.8, and the temperature of the reaction mixture at the end of the dropwise addition is controlled to be not lower than the melting point of the polyamide. The method enables production of a polyamide having an improved hue and being advantageous with respect to quality.
摘要翻译：本发明是通过在间歇式反应器中使作为二胺成分的含对苯二甲胺的混合苯二甲胺与二羧酸成分进行缩聚而制造熔点为255℃以上的聚酰胺的方法，其中，当二胺成分滴加时通过在保持反应混合物的熔融状态的同时将其在0.1MPaG以上的压力下加热至不低于其熔点的温度而保持在熔融状态的二羧酸成分，反应混合物的温度保持在 255℃以下，直到反应混合物的摩尔比（二胺成分/二羧酸成分）达到0.8，滴加结束后的反应混合物的温度控制在不低于聚酰胺。该方法能够生产具有改善的色调并且在质量方面是有利的聚酰胺。

7. 发明授权

US10786928B2 Polyamide pellets, method for producing polyamide pellets, and method for producing polyamide molded article 有权
公开(公告)号：US10786928B2
公开(公告)日：2020-09-29
申请号：US15329793
申请日：2015-07-23
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Tatsuya Tochihara , Katsumi Shinohara , Kaname Sato , Tomonori Kato , Jun Mitadera
IPC分类号： B29C45/47 , B29B9/10 , C08G69/30 , C08J3/12 , B29B7/42 , B29B9/12 , C08G69/26 , B29C48/505 , B29B9/06 , B29C45/00 , B29K77/00 , B29K105/00
摘要： The polyamide pellet of the present invention includes a polyamide including diamine units and dicarboxylic acid units, 50% by mole or more of the diamine units being derived from m-xylylenediamine, wherein a spherulite density of a skin portion of the pellet is 40,000 to 250,000/mm2.

8. 发明申请

US20160304671A1 XYLYLENE DIAMINE COMPOSITION, AND METHOD FOR PRODUCING POLYAMIDE RESIN 有权
标题翻译： XYLYLENE DIAMINE COMPOSITION，以及生产聚酰胺树脂的方法
公开(公告)号：US20160304671A1
公开(公告)日：2016-10-20
申请号：US15032020
申请日：2014-10-29
申请人： MITSUBISHI GAS CHEMICAL COMPANY, INC.
发明人： Tatsuya Tochihara , Katsumi Shinohara , Takashi Nakamura , Hajime Yamada , Jun Mitadera , Takashi Yamamoto
IPC分类号： C08G69/28 , C08G69/30 , C08G59/50
CPC分类号： C08G69/28 , C08G59/50 , C08G59/5033 , C08G69/26 , C08G69/265 , C08G69/30 , C08K5/0083 , C08K5/17 , C08K5/18 , C08L77/06
摘要： Provided are [1] a xylylenediamine composition containing xylylenediamine and a compound represented by the following general formula (1), wherein the content of the compound represented by the general formula (1) is 0.001 to 0.1 parts by mass based on 100 parts by mass of the xylylenediamine; and a method for producing a polyamide resin including the steps of introducing a compound represented by the following general formula (1), a diamine including xylylenediamine (but excluding the compound represented by the general formula (1)), and a dicarboxylic acid into a reaction system and performing a polycondensation reaction, wherein the amount of the compound represented by the general formula (1) to be introduced is 0.001 to 0.1 parts by mass based on 100 parts by mass of the xylylenediamine, where, in the general formula (1), n and m each independently represent an integer of 0 to 6, excluding the case where n and m are both 1.
摘要翻译：提供[1]含有苯二甲胺的苯二甲胺类组合物和由以下通式（1）表示的化合物，其中由通式（1）表示的化合物的含量相对于100质量份为0.001〜0.1质量份的苯二甲胺; 和聚酰胺树脂的制造方法，其特征在于，将下述通式（1）表示的化合物，含有二甲苯二胺的二胺（但不包括通式（1）表示的化合物））和二羧酸引入到反应体系，进行缩聚反应，其中相对于100质量份的苯二甲胺，引入的通式（1）表示的化合物的量为0.001〜0.1质量份，其中，在通式（1）），n和m各自独立地表示0〜6的整数，不包括n和m均为1的情况。

9. 发明授权

US09359477B2 Production method for polyamide 有权
标题翻译：聚酰胺的生产方法
公开(公告)号：US09359477B2
公开(公告)日：2016-06-07
申请号：US14381182
申请日：2013-02-25
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Tatsuya Tochihara , Katsumi Shinohara
IPC分类号： C08G69/28 , C08L77/10 , C08G69/26 , B01J19/00 , B01J19/18 , B01F7/00 , C08L77/06 , B01F7/16
CPC分类号： C08G69/28 , B01F7/00266 , B01F7/00291 , B01F7/00441 , B01F7/00641 , B01F7/16 , B01J19/0066 , B01J19/18 , C08G69/26 , C08G69/265 , C08L77/06 , C08L77/10
摘要： The present invention is directed to a process for producing a polyamide, which process includes directly melt-polymerizing a diamine component including 70 mol % or more of p-xylylenediamine and a dicarboxylic acid component including 70 mol % or more of a C6 to C18 aliphatic dicarboxylic acid, in the absence of solvent in a batch-type reactor equipped with a stirring blade, the process including: (1) reacting the diamine component with the dicarboxylic acid component under a pressure condition of 0.2 to 0.5 MPa (Abs); (2) maintaining a vapor phase section of a reaction tank of the reactor at 200° C. or higher during reaction; (3) stirring the contents of the reaction tank, from the start of adding the diamine component until after completion of the addition and before the start of pressure falling, such that the stirring-related Froude number represented by a specific formula is adjusted to 0.0002 to 0.15; and (4) employing a stirring blade having no structural body in the horizontal direction or having a structural body in the horizontal direction, which body does not come into contact with the interface between the reaction mixture and the vapor phase section during stirring. In the polyamide production process, deposition of solid matter in the reaction tank vapor section and in a vapor pipe is suppressed, and incorporation into the product of unmelted solid matter originating from the deposits is reduced.
摘要翻译：本发明涉及一种聚酰胺的制造方法，该方法包括将包含70摩尔％以上的对苯二甲胺的二胺成分和包含70摩尔％以上的C6〜C18脂肪族的二羧酸成分直接熔融聚合在具有搅拌叶片的间歇式反应器中，在不存在溶剂的情况下，将二胺成分与二羧酸成分在0.2〜0.5MPa（Abs）的压力条件下反应，（2）在反应期间将反应器的反应槽的气相部分维持在200℃以上; （3）从加入二胺成分开始到添加完成，开始压力下降之前搅拌反应槽的内容物，将由特定式表示的与搅拌有关的弗劳德数调整为0.0002 至0.15; 和（4）在水平方向上使用没有结构体的搅拌叶片或在水平方向上具有结构体，在搅拌期间该主体不与反应混合物和气相部分之间的界面接触。在聚酰胺生产过程中，固体物质在反应罐蒸气部分和蒸气管中的沉积被抑制，并且引入到源自沉积物的未熔化的固体物质的产物中。

10. 发明申请

US20150073120A1 PRODUCTION METHOD FOR POLYAMIDE 有权
标题翻译：聚酰胺的生产方法
公开(公告)号：US20150073120A1
公开(公告)日：2015-03-12
申请号：US14381182
申请日：2013-02-25
申请人： Mitsubishi Gas Chemical Company, Inc.
发明人： Tatsuya Tochihara , Katsumi Shinohara
IPC分类号： C08G69/28
CPC分类号： C08G69/28 , B01F7/00266 , B01F7/00291 , B01F7/00441 , B01F7/00641 , B01F7/16 , B01J19/0066 , B01J19/18 , C08G69/26 , C08G69/265 , C08L77/06 , C08L77/10
摘要： The present invention is directed to a process for producing a polyamide, which process includes directly melt-polymerizing a diamine component including 70 mol % or more of p-xylylenediamine and a dicarboxylic acid component including 70 mol % or more of a C6 to C18 aliphatic dicarboxylic acid, in the absence of solvent in a batch-type reactor equipped with a stirring blade, the process including: (1) reacting the diamine component with the dicarboxylic acid component under a pressure condition of 0.2 to 0.5 MPa (Abs); (2) maintaining a vapor phase section of a reaction tank of the reactor at 200° C. or higher during reaction; (3) stirring the contents of the reaction tank, from the start of adding the diamine component until after completion of the addition and before the start of pressure falling, such that the stirring-related Froude number represented by a specific formula is adjusted to 0.0002 to 0.15; and (4) employing a stirring blade having no structural body in the horizontal direction or having a structural body in the horizontal direction, which body does not come into contact with the interface between the reaction mixture and the vapor phase section during stirring. In the polyamide production process, deposition of solid matter in the reaction tank vapor section and in a vapor pipe is suppressed, and incorporation into the product of unmelted solid matter originating from the deposits is reduced.
摘要翻译：本发明涉及一种聚酰胺的制造方法，该方法包括将包含70摩尔％以上的对苯二甲胺的二胺成分和包含70摩尔％以上的C6〜C18脂肪族的二羧酸成分直接熔融聚合在具有搅拌叶片的间歇式反应器中，在不存在溶剂的情况下，将二胺成分与二羧酸成分在0.2〜0.5MPa（Abs）的压力条件下反应，（2）在反应期间将反应器的反应槽的气相部分维持在200℃以上; （3）从加入二胺成分开始到添加完成，开始压力下降之前搅拌反应槽的内容物，将由特定式表示的与搅拌有关的弗劳德数调整为0.0002 至0.15; 和（4）在水平方向上使用没有结构体的搅拌叶片或在水平方向上具有结构体，在搅拌期间该主体不与反应混合物和气相部分之间的界面接触。在聚酰胺生产过程中，固体物质在反应罐蒸气部分和蒸气管中的沉积被抑制，并且引入到源自沉积物的未熔化的固体物质的产物中。

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