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公开(公告)号：US06274638B1
公开(公告)日：2001-08-14
申请号：US09712557
申请日：2000-11-14
IPC分类号： C08J928
摘要： This invention is targeted at providing a method for producing a porous cross-linked polymer material excelling in absorption properties and mechanical strength in a short period of time. In the production of a porous cross-linked polymer material from an HIPE, the method of this invention is characterized by comprising a step of polymerizing the HIPE till the bromine value thereof falls to not more than 25% of the value existing prior to the polymerization and a subsequent step of after curing the porous cross-linked polymer material by means of an active energy ray or a temperature higher than the polymerization temperature.
摘要翻译： 本发明的目的在于提供一种制造在短时间内具有优异的吸收性能和机械强度的多孔交联聚合物材料的方法。 在从HIPE生产多孔交联聚合物材料时，本发明的方法的特征在于包括使HIPE聚合直到其溴值下降到聚合之前存在的值的25％以下的步骤 以及随后通过活性能量射线或高于聚合温度的温度固化多孔交联聚合物材料的步骤。
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公开(公告)号：US06395792B1
公开(公告)日：2002-05-28
申请号：US09689350
申请日：2000-10-12
申请人： Kinya Nagasuna , Hirotama Fujimaru , Kenji Kadonaga , Kozo Nogi , Katsuhiko Sakamoto , Masazumi Sasabe , Kenji Minami
发明人： Kinya Nagasuna , Hirotama Fujimaru , Kenji Kadonaga , Kozo Nogi , Katsuhiko Sakamoto , Masazumi Sasabe , Kenji Minami
IPC分类号： C08J928
CPC分类号： C08J9/283 , C08F2/32 , C08J2201/028
摘要： An object of this invention is to provide a method for the production of a porous cross-linked polymer, which permits the polymerization (curing) of a water in oil type high internal phase emulsion (HIPE) in such an exceptionally brief time as not more than 30 minutes, preferably not more than 10 minutes without impairing the stability of the HIPE. The object of this invention mentioned above can be accomplished by a method for the production of a porous cross-linked polymer which comprises steps of mixing an oil phase containing a polymerizing monomer, a cross-linking monomer, and a surfactant as essential components with a water phase containing water as an essential component thereby obtaining a water in oil type high internal phase emulsion and heating said emulsion to a prescribed curing temperature thereby polymerizing the emulsion, wherein said emulsion is formed in a thickness of not more than 50 mm and the temperature-increasing rate of the emulsion is not less than 5° C./minute.
摘要翻译： 本发明的目的是提供一种生产多孔交联聚合物的方法，其允许在非常短的时间内将油包水型高内相乳液（HIPE）中的聚合（固化）不再多 超过30分钟，优选不超过10分钟，而不损害HIPE的稳定性。 上述本发明的目的可以通过生产多孔交联聚合物的方法来实现，该方法包括以下步骤：将含有聚合单体的油相，交联单体和表面活性剂作为必需组分混合， 水相作为必要成分，由此获得油包水型高内相乳液，并将所述乳液加热到规定的固化温度，从而使乳液聚合，其中所述乳液的形成厚度不大于50mm，温度 - 乳液的增加速度不低于5℃/分钟。
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公开(公告)号：US06822010B2
公开(公告)日：2004-11-23
申请号：US10474950
申请日：2003-10-14
IPC分类号： C08J928
CPC分类号： C08J9/28 , C08F2/32 , C08J2201/028
摘要： A method for producing a porous material excelling in stability of preservation is produced. A method for the production of a porous material comprising a step for obtaining a porous polymer by polymerizing an HIPE containing a polymerizable monomer is disclosed, which method comprises a step for adding a compound capable of reacting with a polymerization initiator and/or a compound capable of reacting with an unsaturated double bond to said emulsion, said porous polymer and/or said porous material having a conversion of not less than 70%. According to this invention, it is made possible to produce a porous material excelling in stability in storage and to decrease the polymerization initiator and the residual monomer very simply.
摘要翻译： 制造出具有良好的保存稳定性的多孔材料的制造方法。 公开了一种生产多孔材料的方法，其包括通过聚合含有可聚合单体的HIPE获得多孔聚合物的步骤，该方法包括添加能够与聚合引发剂和/或化合物反应的化合物的步骤 与所述乳液的不饱和双键反应，所述多孔聚合物和/或所述多孔材料具有不小于70％的转化率。 根据本发明，可以制备出具有良好的储存稳定性的多孔材料，并且非常简单地降低聚合引发剂和残留单体。
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公开(公告)号：US06797735B2
公开(公告)日：2004-09-28
申请号：US10332219
申请日：2003-01-03
申请人： Kinya Nagasuna , Kenji Kadonaga , Hirotama Fujimaru , Kozo Nogi , Kenji Minami
发明人： Kinya Nagasuna , Kenji Kadonaga , Hirotama Fujimaru , Kozo Nogi , Kenji Minami
IPC分类号： C08J928
CPC分类号： C08J9/28 , C08F2/32 , C08J2201/028 , C08J2201/0504 , C08J2333/06
摘要： A method of production is provided which is capable of efficiently producing in a very short period of time a porous polymer possessing a uniform foam structure and truly excelling in absorption properties and physical properties. It is a method for the production of a porous polymer, characterized by comprising (a) an emulsifying step for forming a water-in-oil type high internal phase emulsion (HIPE) by mixing and stirring an oil phase containing a polymerizing monomer component and a surfactant as essential components, (b) a shaping step for shaping the HIPE in a specific form, and (c) a polymerizing step for polymerizing the shaped HIPE and controlling the temperatures of the emulsion at the component steps (a)-(c) so that they may not produce a change exceeding 10° C. or controlling all the component steps so that they may proceed at temperatures of not lower than 80° C.
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公开(公告)号：US06630519B2
公开(公告)日：2003-10-07
申请号：US10168847
申请日：2002-09-27
IPC分类号： C08J912
CPC分类号： C08F2/32
摘要： This invention concerns a method for the production of a porous polymer from a water-in-oil type high internal phase emulsion (HIPE). By using an oil-soluble polymerization initiator as the polymerization initiator, the method for producing a porous polymer with outstanding characteristics in a very short period even when the porous polymer is produced from an HIPE exhibiting a viscosity of not more than 500 mPa second at the emulsion formation temperature or when the porous polymer to be produced possesses a number-average pore diameter of not less than 80 &mgr;m is provided.
摘要翻译： 本发明涉及从油包水型高内相乳液（HIPE）生产多孔聚合物的方法。 通过使用油溶性聚合引发剂作为聚合引发剂，即使在多孔性聚合物由HIPE生产时，在非常短的时间内也具有突出特性的多孔性聚合物的制造方法， 乳液形成温度或当要生产的多孔聚合物具有不小于80μm的数均孔径时。
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公开(公告)号：US06187872B1
公开(公告)日：2001-02-13
申请号：US09051313
申请日：1998-04-06
申请人： Toru Yanase , Kazuki Kimura , Shin-ichi Fujino , Kinya Nagasuna , Kunihiko Ishizaki , Hirotama Fujimaru , Nobuyuki Harada
发明人： Toru Yanase , Kazuki Kimura , Shin-ichi Fujino , Kinya Nagasuna , Kunihiko Ishizaki , Hirotama Fujimaru , Nobuyuki Harada
IPC分类号： C08F812
CPC分类号： A61L15/60 , B01J20/26 , C08F8/00 , C08F8/44 , C08F2800/20 , C08F2810/20 , C08F220/06
摘要： A hydrogel polymer obtained by polymerizing a monomer component including acrylic acid (salt) is post-neutralized so that each of polymer particles derived from a polymer produced by neutralizing the hydrogel polymer has an allowable neutralization ratio. The polymer as obtained by neutralizing the hydrogel polymer is reacted with a crosslinking agent reactive to a functional group of the polymer. The allowable neutralization ratio, for example, is a neutralization ratio which is not lower, by not less than 20 mole percent, or more than, at least 55 mole percent, than an average neutralization ratio of a mass of the polymer particles, and the post-neutralization is carried out so that a number of polymer particles having a non-allowable neutralization ratio outside the allowable neutralization range is not more than 10 in 200 polymer particles, thus obtaining a water-absorbent agent having high absorbency under no applied pressure and high pressure wherein the amount of water soluble component is lower compared with the conventional water-absorbent agent and a change in pH of a swollen gel is small.
摘要翻译： 通过使包含丙烯酸（盐）的单体组分聚合而获得的水凝胶聚合物被后中和，使得通过中和水凝胶聚合物产生的聚合物衍生的各聚合物颗粒具有允许的中和比。 通过中和水凝胶聚合物获得的聚合物与与聚合物的官能团反应的交联剂反应。 例如，容许的中和比例是中和比，其比不到聚合物颗粒的质量的平均中和比不低于20摩尔％，或至多55摩尔％，而且 进行中和后，使得在200个聚合物粒子中，许多中和比例不超过允许中和比例的聚合物颗粒数不超过10个，从而获得在无施加压力下具有高吸收性的吸水剂， 其中水溶性成分的量与常规吸水剂相比较低，并且溶胀凝胶的pH变化很小。
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公开(公告)号：US5981070A
公开(公告)日：1999-11-09
申请号：US793712
申请日：1997-03-03
CPC分类号： C08F8/00 , A61L15/60 , C08J3/245 , C08J9/08 , C08J9/102 , C08J9/36 , C08J2207/12 , C08J2300/14 , C08J2333/02 , Y10S521/905 , Y10T428/2991 , Y10T428/2998
摘要： A manufacturing method of water-absorbent agent powders of the present invention is a method of a reducing an amount of a residue of an epoxy crosslinking agent remaining therein by adding a nucleophilic reagent in a form of powder to surface region crosslinked water-absorbent resin powders having a carboxyl group under an applied heat in which the residue of the crosslinking agent remains. Since the method permits an amount of the residue of the crosslinking agent to be reduced by adding a nucleophilic reagent to the heated water-absorbent resin powders, the water-absorbent agent powders exhibiting well-balanced properties which are mutually negatively correlated from one another, i.e., high absorbency under pressure, a reduced amount of a residue of the epoxy crosslinking agent and a high absorbing rate compared with the conventional surface region crosslinked water-absorbent resin powders can be achieved. Such water-absorbent agent powders are suitably used in sanitary materials such as disposable diaper, sanitary napkins, etc.
摘要翻译： PCT No.PCT / JP96 / 01863 Sec。 371日期1997年3月3日 102（e）1997年3月3日PCT PCT 1996年7月5日PCT公布。 出版物WO97 / 03114 日本1997年1月30日本发明的吸水剂粉末的制造方法是通过将表面区域交联的粉末状的亲核试剂添加到其中而残留的环氧交联剂的残渣量减少的方法 具有羧基的吸水性树脂粉末，其中保留了交联剂的残余物。 由于该方法允许通过向加热的吸水性树脂粉末中添加亲核试剂来减少交联剂的残留量，所以表现出彼此相互负相关的良好平衡性能的吸水剂粉末， 即，与传统的表面区域交联的吸水性树脂粉末相比，可以实现在压力下的高吸收性，环氧交联剂残留量的减少和吸收率高的优点。 这种吸水剂粉末适用于一次性尿布，卫生巾等卫生材料。
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8.发明授权
公开(公告)号：US5610208A
公开(公告)日：1997-03-11
申请号：US388838
申请日：1995-02-15
申请人： Yorimichi Dairoku , Kinya Nagasuna , Yoshihiko Masuda , Nobuyuki Harada , Yoshihiro Motono , Kunihiko Ishizaki
发明人： Yorimichi Dairoku , Kinya Nagasuna , Yoshihiko Masuda , Nobuyuki Harada , Yoshihiro Motono , Kunihiko Ishizaki
CPC分类号： C08J3/245 , A61L15/24 , A61L15/60 , C08F220/06 , C08J2300/14
摘要： A method for the production of a water-absorbent agent comprises mixing an absorbent resin containing a carboxyl group with an additive soluble in the aqueous solution of at least one member selected from the group consisting of inorganic acids, organic acids, and polyamino acids and a cross-linking agent capable of reacting with the carboxyl group. A water-absorbent agent obtained by adding from 0.005 to 8 parts by weight of an epoxy compound to 100 parts by weight of a water-absorbent resin, exhibiting an absorption capacity without load of at least 45 (g/g), an absorption capacity under load of 20 g/cm.sup.2 of not less than 30 (ml/g) and having a residue amount of an epoxy compound of not more than 2 ppm. A water-absorbent composition comprises a polyamino acid (salt) and a water-absorbent resin containing a carboxyl group.
摘要翻译： 制造吸水剂的方法包括将含羧基的吸收性树脂与可溶于选自无机酸，有机酸和聚氨基酸中的至少一种的水溶液中的添加剂混合，以及 能够与羧基反应的交联剂。 通过将0.005〜8重量份的环氧化合物与100重量份的吸水性树脂相加而获得的吸水剂，其表现出无负载的吸收能力为至少45（g / g），吸收能力 负荷为20g / cm 2以下，不低于30（ml / g），残留量不超过2ppm的环氧化合物。 吸水性组合物包含聚氨基酸（盐）和含有羧基的吸水性树脂。
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公开(公告)号：US5532323A
公开(公告)日：1996-07-02
申请号：US26407
申请日：1993-03-04
申请人： Kazutaka Yano , Katsuhiro Kajikawa , Kinya Nagasuna , Yoshio Irie
发明人： Kazutaka Yano , Katsuhiro Kajikawa , Kinya Nagasuna , Yoshio Irie
IPC分类号： A61L15/60 , C08F220/04 , C08F8/14 , C08J3/24
CPC分类号： C08F220/04 , A61L15/60
摘要： An absorbent resin exhibiting a high absorption ratio, having only a small water-soluble component content, and have excellent gel stability to withstand the effect of aging is produced. The production of the absorbent resin comprises a step of polymerizing a water-soluble monoethylenically unsaturated monomer by using, in a proportion of 0.01-0.3 mol % based on the amount of the water-soluble monoethylenically unsaturated monomer, a cross-linking agent having at least one group of the following formula I: ##STR1## wherein R.sup.1 is an alkylene group of 2 to 4 carbon atoms interposed between two polymerizing unsaturated groups in the molecular unit thereof and then heat-treating the resin produced by the polymerization at a temperature in the range of from 160.degree. to 230.degree. C.
摘要翻译： 产生具有高吸收比，仅具有小的水溶性组分含量并且具有优异的凝胶稳定性以抵抗老化的效果的吸收性树脂。 吸收性树脂的制造包括以水溶性单烯属不饱和单体的量为基准，以水溶性单烯键式不饱和单体的量计，以0.01-0.3摩尔％的比例使用水溶性单烯属不饱和单体的交联剂 至少一组下列通式I：（CH2CH2OR1O）（I）其中R1是分子单元中两个聚合不饱和基团之间插入2至4个碳原子的亚烷基，然后热处理由聚合产生的树脂 温度范围为160〜230℃。
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公开(公告)号：US5478879A
公开(公告)日：1995-12-26
申请号：US822916
申请日：1992-01-21
CPC分类号： C08F2/10 , Y10S524/916
摘要： A method for the production of an absorbent resin, which method comprises mixing 100 parts by weight of (A) a hydrated gel of absorbent resin which is resulted from aqueous solution polymerization having a polymerization ratio in the range of from 60 to 99%, an average particle diameter in the range of from 0.1 to 200 mm, a water content in the range of from 30 to 90% by weight, and a temperature in the range of from 40.degree. to 110.degree. C., with from 1 to 50 parts by weight of (B) a substantially dry fine absorbent resin powder having an average particle diameter smaller than the average particle diameter assumed by said hydrated gel of absorbent resin (A) while in a dried state, then raising the polymerization ratio of said hydrated gel of absorbent resin (A) to a level higher than the polymerization ratio of said hydrated gel when being mixed.
摘要翻译： 一种制造吸收性树脂的方法，该方法包括将100重量份由（A）由聚合率为60-99％范围的水溶液聚合得到的吸水性树脂的水合凝胶， 平均粒径为0.1〜200mm，水含量为30〜90重量％，温度为40〜110℃，1〜50份 （B）在干燥状态下，平均粒径小于由吸水性树脂（A）的所述水合凝胶构成的平均粒径的基本上干燥的细小吸水树脂粉末，然后提高所述水合凝胶的聚合比例 的吸水性树脂（A）的混合比例高于所述水合凝胶的混合比。
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