CN102414369A - 用于纸强度和工艺的磺基聚酯 - Google Patents

用于纸强度和工艺的磺基聚酯 Download PDF

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CN102414369A
CN102414369A CN201080018994XA CN201080018994A CN102414369A CN 102414369 A CN102414369 A CN 102414369A CN 201080018994X A CN201080018994X A CN 201080018994XA CN 201080018994 A CN201080018994 A CN 201080018994A CN 102414369 A CN102414369 A CN 102414369A
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paper
acid
paper product
repulpable
sulfonic polyester
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CN102414369B (zh
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R·K·古普塔
D·W·克洛西维奇
M·G·米切尔
N·L·米切尔
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Eastman Chemical Co
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/10—Coatings without pigments
    • D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
    • D21H19/24—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H19/28—Polyesters
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/58—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/18—Reinforcing agents
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/18—Reinforcing agents
    • D21H21/20—Wet strength agents

Abstract

磺基聚酯热塑性树脂在造纸工艺和纸产品(包括纸板)中提供优点。在造纸过程期间，通过加入磺基聚酯热塑性树脂和阳离子强度添加剂，实现纸产品的湿强度和干强度的改进。在纸产品中使用磺基聚酯热塑性树脂还显著增强纸的再制浆能力。

Description

用于纸强度和工艺的磺基聚酯
发明领域
本发明提供了一种改进纤维素纸的湿强度同时增强再制浆能力的方法。
发明背景
在纸产品(包括纸板)的制造时通常加入湿强度树脂。在不存在湿强度树脂时，纸在被水润湿之后通常仅保持其强度的3％-5％。然而，使用湿强度树脂制备的纸在润湿时通常保持其强度的至少10％-50％。湿强度可用于种类繁多的纸应用，这些应用中的一些实例为纸巾、牛奶和果汁硬纸盒、纸袋和波纹容器的衬板。
如在Handbook for Pulp and Paper Technologists(纸浆与纸技术手册)，Gary A.Smook，Angus Wilde Publications，1992(通过引用结合到本文中)中所述的：“纸在传统上定义为在细筛上由纤维的水悬浮液形成的粘结的片材。当前的纸产品通常遵守该定义，只是大多数产品还含有非纤维添加剂。现在利用干形成方法来制造少数专用纸产品。纸浆(pulp)为用于造纸的纤维状原料。纸浆纤维通常为植物来源，但是动物、矿物或合成的纤维可用于专门的应用。纸和纸板的区别基于产品厚度。名义上，超过0.3mm厚度的所有片材分类为纸板；但是足够多的例外使得该区别变得有些模糊。”
由于工业上日益着重开发基于回收的或再循环的纤维素的纸产品，越来越关注的是开发容易可再制浆的纸。当纸和纸板废料含有湿强度树脂时，不经过专门的化学处理，纸和纸板废料难以在含水系统中再制浆。
通常通过改变再制浆条件，实现改进含有湿强度树脂的纸的再制浆能力。然而，用于湿强度纸的许多常规的再制浆工艺导致形成在环境上不期望的含氯降解产物、涉及强氧化剂或进展缓慢。
需要制造纸产品的改进的方法，所述纸产品容易可再制浆，而不显著降低纸的湿强度和干强度性质。
发明概述
本发明涉及可再制浆的纸产品，所述纸产品包含：造纸纤维；阳离子强度添加剂；和磺基聚酯热塑性树脂。
本发明还涉及改进纸的湿强度的方法，所述方法包括在造纸过程期间向纸中加入阳离子强度添加剂；和磺基聚酯热塑性树脂。
本发明涉及纸产品，所述纸产品包含：造纸纤维；阳离子强度添加剂；和磺基聚酯热塑性树脂。
本发明涉及改进纤维素纸的湿强度的方法，所述方法包括在造纸过程期间向造纸纤维中加入阳离子强度添加剂和磺基聚酯热塑性树脂。
发明详述
参考本发明的以下详细说明和所包括的实例，可以更容易地理解本发明。
在公开和描述本发明的物质组成和方法之前，应理解的是，除非另外说明，否则本发明不局限于具体的合成方法或特定的制剂，因此，可不同于公开的内容。还应理解的是，使用的术语仅用于描述具体实施方案的目的，而不是意欲限制本发明的范围。
除非上下文明确另外说明，否则单数形式“一个”、“一”和“该”包括复数指示物。
任选的或任选是指随后描述的事件或情况可能发生或者可能不发生。该描述包括事件或情况发生的情况以及它们不发生的情况。
除非另外说明，否则在说明书和权利要求书中使用的表示成分、性质的量(比如分子量、反应条件等)的所有数字应理解为在所有情况下被术语“约”修饰。本文中的范围可表示为从约一个具体的值和/或到约另一个具体的值。当表示这样的范围时，应理解的是，另一个实施方案为从一个具体的值和/或到其他具体的值，以及在所述范围内的所有组合。相应地，除非说明相反的情况，否则在以下说明书和所附权利要求书中所述的数值参数为近似值，其可根据本发明要寻求得到的期望的性质而改变。至少，每一个数值参数应至少根据所报道的有效数字的数值以及应用普通的四舍五入技术而解释。另外，在本公开和权利要求书中陈述的范围意欲包括具体的整个范围而不仅仅是端点。例如，陈述为0-10的范围意欲公开0和10之间的所有的整数(比如，例如1、2、3、4等)、0和10之间的所有的分数(例如1.5、2.3、4.57、6.1113等)以及端点0和10。
在整个申请中，当参考专利或出版物时，这些参考文献所公开的全部内容意欲通过引用结合到本申请中，以便更充分地描述本发明所属领域的状态。
在本发明的上下文中使用的一些相关的技术术语应如下所示进行理解(除非在整个说明书中具体说明了另外的情况)。
本文使用的“造纸纤维”包括所有已知的纤维素纤维或包含纤维素纤维的纤维混合物。适用于制造本发明的纤维网的纤维包括任何天然或合成的纤维素纤维，包括但不限于：非木质纤维，比如棉或棉衍生物、蕉麻、槿麻、萨拜草(sabai grass)、亚麻、西班牙草、稻草、黄麻、甘蔗渣、马利筋属丝绵纤维和菠萝叶纤维；和木质纤维，比如由落叶和针叶树得到的那些，包括软木纤维，比如北方和南方软木牛皮纸纤维；硬木纤维，比如桉树、槭树、桦树和白杨。木质纤维可以高收率或低收率形式制备，并且可采用任何已知的方法制浆，包括牛皮纸、亚硫酸盐、磨木、热机械纸浆(TMP)、化学热机械纸浆(CTMP)和漂白的化学热机械纸浆(BCTMP)、高收率制浆方法和其他已知的制浆方法。可使用高白度纸浆，包括化学漂白的纸浆，并且还可使用未漂白的或半漂白的纸浆。再循环的纤维包括在本发明的范围内。可使用任何已知的制浆和漂白方法。还可使用由有机溶剂制浆方法制备的纤维。合适的造纸纤维还可包括再循环的纤维、原始纤维或它们的混合物。
还适于使用合成的纤维素纤维，包括其所有种类的人造丝和源自粘胶的其他纤维或化学改性的纤维素。可使用经化学处理的天然纤维素纤维，比如丝光处理的纸浆、化学变硬或交联的纤维、磺化纤维等。合适的合成聚合物纤维包括人造丝、聚烯烃纤维、聚酯纤维、聚酰胺纤维等。合适的合成聚合物纤维结构包括单组分、双组分和多组分纤维，比如芯-鞘型、海岛型(islands-in-the-sea)、并列型、橘瓣型(segmentedpie)等。
在本发明的一个实施方案中，造纸纤维包括木质纤维、软木牛皮纸浆、硬木牛皮纸浆、再循环的纤维、非木质纤维、合成聚合物纤维、玻璃纤维或它们的组合。在一个实施方案中，合成聚合物纤维的平均纤维直径小于5微米。在另一个实施方案中，合成聚合物纤维构成大于造纸纤维总量的50％或大于造纸纤维总量的70％。
为了在使用造纸纤维中得到良好的机械性质，可期望纤维相对未被破坏和大部分未精制或仅轻微精制。虽然可使用再循环的纤维，但是原始纤维由于它们的机械性质和缺少污染物也是可用的。可使用丝光处理的纤维、再生的纤维素纤维、由微生物生产的纤维素、人造丝和其他纤维素材料或纤维素衍生物。合适的造纸纤维还可包括再循环的纤维、原始纤维或它们的混合物。
本文使用的“高收率纸浆纤维”为通过提供约65％或更高的收率的制浆工艺生产的纸浆的那些造纸纤维，。收率为经加工的纤维所得到的量，用初始木材质量的百分比表示。高收率纸浆包括漂白的化学热机械纸浆(BCTMP)、化学热机械纸浆(CTMP)加压/加压热机械纸浆(PTMP)、热机械纸浆(TMP)、热机械化学纸浆(TMCP)、高收率亚硫酸盐纸浆和高收率牛皮纸浆，均含有具有高水平木素的纤维。特有的高收率纤维的木素含量可为约1％质量或更大。在一个实施方案中，在通过制浆和任选的漂白步骤制备之后，并且在形成为干捆或纤维网之前，合适的高收率纸浆纤维还可表征为包含相当完整的相对未被破坏的纤维、高打浆度(加拿大标准打浆度(CSF)为250或更大)和低细屑含量(小于25％，通过Britt jar测试)。在一个实施方案中，高收率纤维主要为软木，例如北方软木。
本文使用的术语“纤维素”是指包括具有纤维素作为主要组成的任何材料，并且具体包含约50％重量或更多的纤维素或纤维素衍生物。由此，该术语包括棉、典型的木浆、非木质纤维素纤维、纤维素乙酸盐、纤维素三乙酸盐、人造丝、粘胶纤维、热机械木浆、化学木浆、脱粘的化学木浆、由纤维素在NMMO中的溶液形成的莱塞尔(lyocell)纤维和其他纤维、马利筋属纤维或细菌纤维素。如果需要，可排他地使用未纺成的或由溶液再生的纤维，或者至少约80％的纤维网可不含纺成纤维或由纤维素溶液产生的纤维。
本发明的一方面涉及由造纸纤维的含水浆料生产纸产品(包括纸和纸板)。已发现，含有阳离子强度添加剂和磺基聚酯热塑性树脂的本发明的纸产品产生具有改进的或保持的湿强度和干强度同时具有显著增强的再制浆能力的纸产品。
本发明的一个实施方案涉及可再制浆的纸产品，所述纸产品包含：造纸纤维；阳离子强度添加剂；和热塑性磺基聚酯树脂。
本发明的另一个实施方案涉及纸产品，所述纸产品包含：造纸纤维；阳离子强度添加剂；和热塑性磺基聚酯树脂。本发明的纸产品提供增强再制浆能力。
除了增强的再制浆能力以外，本发明的纸产品还提供增强的片材强度，提高的机器速度和改进的保留。通过减少或消除某些湿部添加剂(包括干强度树脂、阳离子淀粉、助滤剂和助留剂和凝结剂)的使用，本发明还使得造纸者能简化湿部(wet end)。当本发明同时用作湿强度和干强度助剂时，纸产品的吸收性不下降。本发明对片材性能提供了以下改进：较低的基础重量、提高的再循环纤维利用、能在较高浓度下或以固体形式提供分散、延长的保存期限、降低的牛皮纸利用、立即固化、改进的印刷接收性、改进的表面强度、改进的片材加工性、改进的机器运行性、提高的生产、较高的片材灰含量和填料成本节约、改进的纤维回收、降低的白水固体和浊度、提高的湿强度添加剂的保留、降低的系统沉积，提供了高水平的受控的滤水、改进的形成、提高的机器速度、降低的干燥器能耗、由较少的添加剂引起的简化的和更干净的湿部、成本高效的添加剂方案和湿部化学效率增加。
常见的是向纸浆或造纸纤维的含水浆料中包括各种无机和有机材料以改进纸产品和造纸工艺。可在任何常规的造纸设备上进行制造本发明的纸产品的工艺。
总的来说，本发明的工艺包括提供造纸纤维的浆料，向纸浆造纸纤维的浆料中加入本发明的各组分，在成形织物上沉积含有本发明的各组分的纸浆造纸纤维的浆料，以及干燥浆料以形成纸网。
在本发明的一个实施方案中，待由根据本发明处理的造纸纤维形成的纤维状网可湿法成网，比如可使用已知的造纸技术来形成纤维网，其中将稀释的含水纤维浆料在移动的金属丝网上布置，以滤出纤维并形成纸网，随后通过多个单元的组合进行脱水，所述单元包括抽吸箱、湿压机、干燥器单元等。毛细脱水也可适用于从纤维网中除去水。
根据本发明，可使用任何常规的干燥方法或干燥器。一般而言，干燥操作可包括转鼓干燥、彻底干燥、蒸汽干燥比如过热蒸汽干燥、置换脱水、杨克式(yankee)干燥、红外干燥、微波干燥、射频干燥；和脉冲干燥。
通过泡沫形成工艺还可形成潮湿的纤维状网，其中在脱水之前将经处理的纤维夹带或悬浮于泡沫中，或者，其中在脱水或干燥之前将泡沫施用于纸网。
纤维状网通常为无规的多种造纸纤维，其可任选与粘合剂接合在一起。可使用本文定义的任何造纸纤维或它们的混合物，比如来自牛皮纸或亚硫酸盐化学制浆工艺的漂白的纤维。还可使用再循环的纤维，就像棉短绒或含棉的造纸纤维。可使用高收率和低收率纤维二者。在一个实施方案中，纤维可主要为硬木，比如至少50％硬木或约60％硬木或更多或约80％硬木或更多或基本上100％硬木。在另一个实施方案中，纤维网主要为软木，比如至少约50％软木或至少约80％软木或约100％软木。在另一个实施方案中，纤维网主要为合成聚合物纤维，比如至少约50％合成聚合物纤维或至少约80％合成聚合物纤维或约100％合成聚合物纤维。
本发明的纤维状网可由单层或多层形成。还可形成分层的纤维网，其中至少一层包含软木纤维，而另一层包含硬木或其他纤维类型。通过本领域已知的任何方式产生的分层的结构在本发明的范围内。在多层的情况下，各层通常安置为并列或为面对面的关系，并且全部或一部分层可与邻接的层粘合。纸网还可由多个单独的纸网形成，其中各单独的纸网可由单层或多层形成。
本发明的一个实施方案提供了一种改进纤维素纸的湿强度的方法，所述方法包括在造纸过程期间向纸中加入阳离子强度添加剂；和磺基聚酯热塑性树脂。
制造本发明的纸产品或可再制浆的纸产品的工艺包括多个步骤。一个步骤包括形成造纸纤维或纸浆的含水浆料，其可通过常规的方式进行，即，已知的机械、化学和半化学等制浆工艺。另一个步骤包括向造纸纤维或纸浆的含水浆料中加入阳离子强度添加剂和热塑性磺基聚酯树脂。可在任何时间点进行该步骤，在片材形成之前，或者可在片材形成之后由槽式施胶器或施胶压机施用，或者由喷淋器向干燥的或部分干燥的片材施用。再一个步骤包括将含有阳离子热固性树脂的造纸或纸浆纤维的含水浆料形成片材和干燥。可通过任何常规的方式实现该步骤。
在一个实施方案中，将包含阳离子强度添加剂和热塑性磺基聚酯树脂的本发明的各组分分别加入到纸浆浆料，但是根据纤维网期望的强度特性，可将阳离子强度添加剂或热塑性磺基聚酯树脂的任一在另一个之前加入到浆料中。
在造纸过程期间，可通过各种方法掺入阳离子强度添加剂，包括加在纸浆纤维浆料中或在纸浆挤压时掺入。在本发明的一个实施方案中，在磺基聚酯热塑性树脂之前将阳离子强度添加剂加入到浆料中。不希望束缚于任何理论，阳离子强度添加剂与带阴离子电荷的纤维素纸浆纤维键合，产生带正电荷的纸浆纤维。随后，将带阴离子电荷的磺基聚酯热塑性树脂施用于纸浆纤维，产生离子键。可通过各种方法(包括喷涂)施用磺基聚酯树脂。
在另一个实施方案中，本发明的工艺包括提供纸浆或造纸纤维的浆料，序贯将本发明的各组分加入到纸浆或造纸纤维的含水浆料中，在形成织物上沉积含有本发明的各组分的纸浆或造纸纤维的浆料，以及干燥浆料以形成纸网。这些组分还可在形成之后趁湿在纤维网上喷涂、印刷或涂布，或者在形成之前加入到造纸机器的湿部中。
根据本发明，可将包含阳离子强度添加剂和热塑性磺基聚酯树脂的各组分按需以约1∶5-约5∶1的比率加入到浆料中。
在过程期间可调节浆料的pH。例如，在一个实施方案中，可将浆料的pH调节至酸性pH，比如约6或更低。然而，在另一个实施方案中，可将pH调节至大于约6。当达到期望的粘度时，随后加入足够的水，将树脂溶液的固含量调节至约15％或更低，将产品冷却至约25℃，随后通过加入足够的酸来稳定，以将pH降至至少约6，并优选约5。可使用任何合适的酸来稳定产品，所述酸比如盐酸、硫酸、硝酸、甲酸、磷酸和乙酸。
本发明的纸网可具有任何常规的容重。在一个实施方案中，本发明的纸网的体积可大于约2cc/g。例如，纸网的体积可大于约5cc/g。纸网的干拉伸指数可为任何常规的值。例如，在一个实施方案中，纸网的干拉伸指数可大于约20Nm/g。在另一个实施方案中，纸网的干拉伸指数可大于约22Nm/g。在再一个实施方案中，干拉伸指数可大于约25Nm/g。总的来说，本发明的纸网的基础重量可为任何期望的基础重量。例如，在一个实施方案中，纸网的基础重量可在约5-约200gsm之间。
可用于本发明的造纸工艺的其他常规的化学添加剂为：松香胶、反应性胶(烯基琥珀酸酐或烷基乙烯酮二聚物)、表面胶、淀粉、助留剂、助滤剂、形成助剂、絮凝剂、起皱助剂(粘合剂和脱模剂)、干强度树脂(阳离子淀粉、瓜耳胶、聚丙烯酰胺)、消泡剂、用于阴离子废料和粘性控制的清除剂、填料(粘土、碳酸钙、二氧化钛)、光学增白助剂和染料。
阳离子强度添加剂
在造纸和湿法成网非织造织物液压制造过程期间，通常掺入化学添加剂以改进纸和纸板产品的湿强度和/或干强度。这些化学添加剂通常称为湿强度和干强度添加剂，并且可得自多个市售可得的来源。
持久的湿强度添加剂的实例包括聚酰胺表氯醇和聚酰氨基胺表氯醇，并且统称为PAE树脂。湿强度添加剂的实例基于化学品，比如聚丙烯酰胺和乙二醛化的聚丙烯酰胺(GPAM)树脂。
根据本发明，阳离子强度添加剂可由湿强度或干强度添加剂组成，并且包括乙二醛化的聚丙烯酰胺、聚丙烯酰胺、聚酰胺表氯醇(PAE)、淀粉和本领域技术人员公知的其他阳离子添加剂。
聚酰胺表氯醇、聚酰氨基胺表氯醇和聚胺表氯醇树脂统称为PAE树脂。PAE树脂由于能为众多纸产品(包括薄纸、纸巾、拭纸和皱纹板)赋予高程度的湿强度而广泛用于造纸行业。PAE树脂不改进纸或纸板的干强度，并且通常认为含有这些树脂的产品不可再制浆。含有湿强度添加剂的纸产品尽管通常可再制浆，但通常在许多应用中湿强度不够。在完全润湿时，源自湿强度添加剂的纸产品通常在数分钟至数小时内降解。
根据本发明使用的合适的阳离子强度添加剂包括PAE树脂、乙二醛化(glyoxylated)的聚丙烯酰胺树脂、淀粉、聚丙烯酰胺和本领域技术人员通常已知的其他湿强度和干强度添加剂。
制造PAE树脂的程序为文献中公知的，并且更详细地描述于美国专利3,772,076号，该专利通过引用结合到本文中。PAE树脂以商品名Kymene售自Ashland，Inc.，Wilmington，Delaware和以商品名Amres
Figure BPA00001449013200102
售自Georgia Pacific，Inc.，Atlanta，Georgia。合成PAE树脂的典型的程序如下所示。使聚亚烷基聚胺与脂族二羧酸反应，以形成聚酰氨基胺骨架。聚酰氨基胺的一个实例为二亚乙基三胺与己二酸或二羧酸衍生物的酯的反应产物。所得到的聚酰氨基胺随后与表氯醇在含水溶液中反应。将所得到的产品稀释并用强无机酸中和至pH低于3.0。
被乙二醛改性的丙烯酰胺聚合物称为乙二醛化的聚丙烯酰胺树脂。用于合成乙二醛化的聚丙烯酰胺的程序为文献中公知的，并且更详细地描述于美国专利3,556,932号，该专利通过引用结合到本文中。乙二醛化的聚丙烯酰胺树脂以商品名Parez
Figure BPA00001449013200103
售自Kemira，Inc.，Kennesaw，Georgia。丙烯酰胺聚合物可含有单体以改变离子性质。基于丙烯酰胺的聚合物与足够的乙二醛在含水碱性条件下反应，直至出现粘度轻微增加。所得到的产品随后用酸淬灭。大致一半加入的乙二醛保持未反应并溶解于水中。还可使丙烯酰胺聚合物与乙二醛以干颗粒状态预先共混，随后将该共混物加入到温水中，以形成乙二醛化的聚丙烯酰胺树脂。
干强度添加剂包括各种材料，比如可为阳离子、四元(quaternary)或非离子性质的淀粉。适用于本发明的干强度添加剂的实例包括多糖(比如淀粉、瓜耳胶、纤维素和几丁质)的阳离子衍生物；聚胺；聚乙烯亚胺；乙烯醇-乙烯基胺共聚物；阳离子丙烯酸类均聚物和共聚物，比如聚丙烯酰胺、聚二烯丙基二甲基氯化铵以及丙烯酸、丙烯酸酯和丙烯酰胺与二烯丙基二甲基氯化铵的共聚物、丙烯酰氧基乙基三甲基氯化铵、甲基丙烯酰氧基乙基三甲基硫酸甲酯铵、甲基丙烯酰氧基乙基三甲基氯化铵和甲基丙烯基酰氨基丙基三甲基氯化铵。
可用于本发明的其他阳离子强度树脂为：氨基聚酰胺-epi树脂(例如，Kymene
Figure BPA00001449013200111
557H-树脂)；聚胺-epi树脂(例如，Kymene
Figure BPA00001449013200112
736树脂)；环氧树脂(例如，Kymene
Figure BPA00001449013200113
450和Kymene
Figure BPA00001449013200114
2064树脂)；聚乙烯亚胺；脲甲醛树脂；三聚氰胺-甲醛树脂；乙二醛化的聚丙烯酰胺(例如，Hercobond
Figure BPA00001449013200115
1000树脂，Parez 631NC)；聚异氰酸酯；和反应性淀粉(氧化淀粉、二醛淀粉、嵌段反应性基团淀粉)。
阳离子强度添加剂的量通常为约0.25-约3.00％重量干基，基于干纸的重量。例如在本发明的一些实施方案中，阳离子强度添加剂的量为约0.25-3.00％重量、0.25-2.00％重量或0.25-1.50％重量。在其他实施方案中，阳离子强度添加剂可为约2％重量干基，基于干纸的重量，或约1％重量或约0.5％重量。在本发明的一个实施方案中，使用类似量的湿强度添加剂和磺基聚酯。
磺基聚酯热塑性树脂
本发明的磺基聚酯包含二羧酸单体残基、磺基单体残基、二醇单体残基和重复单元。磺基单体可为二羧酸、二醇或羟基羧酸。由此，本文使用的术语“单体残基”是指二羧酸、二醇或羟基羧酸的残基。本文使用的“重复单元”是指具有2个通过羰基氧基基团键合的单体残基的有机结构。本发明的磺基聚酯含有基本上等摩尔比例的酸残基(100％摩尔)和二醇残基(100％摩尔)，它们以基本上等比例反应，使得重复单元的总摩尔数等于100％摩尔。因此，在本公开中所提供的摩尔百分比可基于酸残基的总摩尔数、二醇残基的总摩尔数或重复单元的总摩尔数。例如，含有30％摩尔的磺基单体(其可为二羧酸、二醇或羟基羧酸，基于重复单元的总量)的磺基聚酯是指磺基聚酯含有30％摩尔磺基单体，在总计100％摩尔重复单元中。由此，每100摩尔的重复单元中存在30摩尔的磺基单体残基。类似地，含有30％摩尔的二羧酸磺基单体(基于酸残基的总量)的磺基聚酯是指磺基聚酯含有30％摩尔磺基单体，在总计100％摩尔酸残基中。由此，在该后一种情况下，每100摩尔的酸残基中存在30摩尔的磺基单体残基。
本文所述的磺基聚酯的特性粘度(下文中简写为“Ih.V.”)为至少约0.1dL/g，优选约0.2-0.3dL/g，最优选大于约0.3dL/g，在60/40重量份苯酚/四氯乙烷溶剂溶液中，在25℃下、在约0.5g磺基聚酯/100mL溶剂的浓度下测定。本文使用的术语“聚酯”包括“均聚酯”和“共聚酯”二者，并且是指通过二官能的羧酸与二官能的羟基化合物缩聚而制备的合成聚合物。本文使用的术语“磺基聚酯”是指包含磺基单体的任何聚酯。典型的二官能的羧酸为二羧酸，而二官能的羟基化合物为二元醇，比如，例如二醇(glycol)和二醇(diol)。或者，二官能的羧酸可为羟基羧酸，比如，例如，对羟基苯甲酸，而二官能的羟基化合物可为带有2个羟基取代基的芳族核，比如，例如，氢醌。本文使用的术语“残基”是指通过涉及相应单体的缩聚反应掺入到聚合物中的任何有机结构。由此，二羧酸残基可源自二羧酸单体或其相关的酰卤、酯、盐、酸酐或它们的混合物。因此，本文使用的术语“二羧酸”意欲包括二羧酸和二羧酸的任何衍生物，包括其相关的酰卤、酯、半酯、盐、半盐、酸酐、混合酸酐或它们的混合物，其可用于与二醇的缩聚过程，以制备高分子量聚酯。
本发明的磺基聚酯包括一种或多种二羧酸残基。根据磺基单体的类型和浓度，二羧酸残基可构成酸残基的约60-约100％摩尔。二羧酸残基的浓度范围的其他实例为约60％摩尔-约95％摩尔和约70％摩尔-约95％摩尔。可使用的二羧酸的实例包括脂族二羧酸、脂环族二羧酸、芳族二羧酸或这些酸中的两种或更多种的混合物。由此，合适的二羧酸包括但不限于琥珀酸；戊二酸；己二酸；壬二酸；癸二酸；富马酸；马来酸；衣康酸；1，3-环己烷二甲酸；1，4-环己烷二甲酸；二甘醇酸；2，5-降冰片烷二甲酸；邻苯二甲酸；对苯二甲酸；1，4-萘二甲酸；2，5-萘二甲酸；联苯甲酸；4，4′-氧基二苯甲酸；4，4′-磺基二苯甲酸；和间苯二甲酸。优选的二羧酸残基为间苯二甲酸、对苯二甲酸和1，4-环己烷二甲酸，或者如果使用二酯，优选的二羧酸残基为对苯二甲酸二甲酯、间苯二甲酸二甲酯和1，4-环己烷-二甲酸二甲酯，其中特别优选间苯二甲酸和对苯二甲酸的残基。虽然二羧酸甲酯为最优选的实施方案，还可接受的是包括较高级的烷基酯，比如乙酯、丙酯、异丙酯、丁酯等。此外，还可采用芳族酯，特别是苯基酯。
基于重复单元的总量，磺基聚酯包括约4-约40％摩尔的至少一种磺基单体的残基，所述磺基单体具有2个官能团和一个或多个与芳族或脂环族环连接的磺酸盐基团，其中所述官能团为羟基、羧基或它们的组合。磺基单体残基的浓度范围的另外的实例为约4-约35％摩尔、约8-约30％摩尔和约8-约25％摩尔，基于重复单元的总量。磺基单体可为含有磺酸盐基团的二羧酸或其酯、含有磺酸盐基团的二醇或含有磺酸盐基团的羟基酸。术语“磺酸盐”是指具有结构“-SO3M”的磺酸的盐，其中M为磺酸盐的阳离子。磺酸盐的阳离子可为金属离子，比如Li+、Na+、K+、Mg++、Ca++、Ni++、Fe++等。或者，磺酸盐的阳离子可为非金属性的，比如，例如描述于美国专利号4,304,901的含氮碱。基于氮的阳离子源自含氮碱，其可为脂族、脂环族或芳族化合物。这种含氮碱的实例包括氨、二甲基乙醇胺、二乙醇胺、三乙醇胺、吡啶、吗啉和哌啶。由于含有基于氮的磺酸盐的单体通常在制备熔体聚合物所需的条件下热不稳定，用于制备含有基于氮的磺酸盐基团的磺基聚酯的本发明的方法为将含有所需量的其碱金属盐形式的磺酸盐基团的聚合物在水中分散、驱散或溶解，并随后将碱金属阳离子交换为基于氮的阳离子。
当一价碱金属离子用作磺酸盐的阳离子时，所得到的磺基聚酯可完全分散于水中，其中分散速率取决于聚合物中磺基单体的含量、水的温度、磺基聚酯的表面积/厚度等。当使用二价金属离子时，所得到的磺基聚酯不容易被冷水分散，但是更容易被热水分散。在单一聚合物组成中利用多于一种反离子是可能的，并且可提供方式，调节或微调所得到的制造制品的水-响应性。磺基单体残基的实例包括磺酸盐基团与芳族酸核或脂环族环连接的单体残基，芳族酸核比如，例如，苯；萘；二苯基；氧基二苯基；磺酰基二苯基；和亚己基二苯基，脂环族环比如，例如，环己基；环戊基；环丁基；环庚基；和环辛基。可用于本发明的磺基单体残基的其他实例为磺基邻苯二甲酸、磺基对苯二甲酸、磺基间苯二甲酸的金属磺酸盐或它们的组合。可使用的磺基单体的其他实例为5-钠代磺基间苯二甲酸及其酯。如果磺基单体残基来自5-钠代磺基间苯二甲酸，则典型的磺基单体浓度范围为约0.4-约35％摩尔、约8-约30％摩尔和约8-25％摩尔，基于酸残基的总摩尔数。
用于制备磺基聚酯的磺基单体为已知的化合物，并且可使用本领域公知的方法来制备。例如，其中磺酸盐基团与芳族环连接的磺基单体可通过如下制备：用发烟硫酸磺化芳族化合物，以得到相应的磺酸，接着与金属氧化物或碱(例如，乙酸钠)反应，以制备磺酸盐。用于制备各种磺基单体的程序例如描述于美国专利3,779,993；3,018,272；和3,528,947号。
还可例如使用磺酸钠盐和离子交换方法来制备聚酯，当聚合物为分散的形式时，用不同的离子(比如锌)替代钠。这种类型的离子交换程序通常优异于使用二价盐来制备聚合物，因为钠盐通常更可溶解于聚合物反应物熔融相。
磺基聚酯包括一种或多种二醇残基，其可包括脂族、脂环族和芳烷基二醇。可存在纯的顺式或反式异构体或顺式和反式异构体的混合物形式的脂环族二醇，例如，1，3-环己烷二甲醇和1，4-环己烷二甲醇。本文使用的术语“二醇(diol)”与术语“二醇(glycol)”同义，是指任何二元醇。二醇的实例包括乙二醇；一缩二乙二醇；二缩三乙二醇；聚乙二醇；1，3-丙二醇；2，4-二甲基-2-乙基己-1，3-二醇；2，2-二甲基-1，3-丙二醇；2-乙基-2-丁基-1，3-丙二醇；2-乙基-2-异丁基-1，3-丙二醇；1，3-丁二醇；1，4-丁二醇；1，5-戊二醇；1，6-己二醇；2，2，4-三甲基-1，6-己二醇；硫代二乙醇；1，2-环己烷二甲醇；1，3-环己烷二甲醇；1，4-环己烷二甲醇；2，2，4，4-四甲基-1，3-环丁二醇；对苯二甲醇或这些二醇中的一种或多种的组合。
基于二醇残基的总量，二醇残基可包括约25％摩尔-约100％摩尔的具有结构H-(OCH2-CH2)n-OH的聚(乙二醇)的残基，其中n为2-约500的整数。较低分子量的聚乙二醇(例如，其中n为2-6)的非限制性实例为一缩二乙二醇、二缩三乙二醇和三缩四乙二醇。在这些较低分子量二醇中，最优选一缩二乙二醇和二缩三乙二醇。较高分子量聚乙二醇(本文中缩写为“PEG”)(其中n为7-约500)包括市售可得的产品，名为CARBOWAX.RTM.，为Dow Chemical Company(前身UnionCarbide)的产品。通常，PEG与其他二醇，比如，例如，一缩二乙二醇或乙二醇组合使用。基于n的值，其范围从大于6至500，分子量可从大于300至约22,000g/mol。分子量和％摩尔彼此成反比；具体地，当分子量增加时，％摩尔将降低，以便实现指定程度的亲水性。例如，举例说明本观念，认为分子量为1000的PEG可构成至多二醇总量的10％摩尔，而分子量为10,000的PEG通常以小于二醇总量的1％摩尔的水平掺入。
由于通过改变工艺条件可控制的副反应，可原位形成某些二聚物、三聚物和四聚物二醇。例如，可由酸-催化的脱水反应，由乙二醇形成不同量的一缩二乙二醇、二缩三乙二醇和三缩四乙二醇，当在酸性条件下进行缩聚反应时，可容易地发生该脱水反应。可将本领域技术人员公知的存在的缓冲溶液加入到反应混合物中，以延缓这些副反应。另外的组成自由度是可能的，然而，如果省略缓冲液，则允许进行二聚、三聚和四聚反应。
基于重复单元的总量，本发明的磺基聚酯可包括0-约25％摩尔的具有3个或更多个官能团的支化单体的残基，其中所述官能团为羟基、羧基或它们的组合。支化单体的非限制性实例为1，1，1-三羟甲基丙烷、1，1，1-三羟甲基乙烷、甘油、季戊四醇、赤藓醇、苏糖醇、二季戊四醇、山梨糖醇、偏苯三酸酐、苯均四酸二酐、二羟甲基丙酸或它们的组合。支化单体浓度范围的其他实例为0-约20％摩尔和0-约10％摩尔。存在支化单体可导致对本发明的磺基聚酯多个可能的益处，包括但不限于，能调整流变性、溶解性和拉伸性质。例如，在恒定的分子量下，与线性类似物相比，支化的磺基聚酯还具有更大浓度的端基，这些端基可促进后聚合交联反应。然而，在高浓度的支化剂下，磺基聚酯可易于凝胶化。
使用标准技术，比如本领域技术人员公知的差示扫描量热法(“DSC”)，对干聚合物进行测定，本发明的磺基聚酯的玻璃化转变温度(本文中缩写为“Tg”)为至少25℃。本发明的磺基聚酯的Tg测定使用“干聚合物”进行，也就是，通过将聚合物加热至约200℃的温度并使样品返回至室温而除去其中外来的或吸收的水的聚合物样品。通常，通过进行第一次热扫描将磺基聚酯在DSC设备中干燥，其中将样品加热至超过水蒸发温度的温度，将样品在该温度下保持，直至在聚合物中吸收的水完全蒸发(由大的、宽的吸热所表示)，将样品冷却至室温，随后进行第二次热扫描，以得到Tg测定值。磺基聚酯表现出的玻璃化转变温度的其他实例为至少30℃、至少35℃、至少40℃、至少50℃、至少60℃、至少65℃、至少80℃和至少90℃。虽然其他Tg也是可能的，但是本发明的干磺基聚酯的典型的玻璃化转变温度为约30℃、约48℃、约55℃、约65℃、约70℃、约75℃、约85℃和约90℃。
本发明还提供了磺基聚酯，所述磺基聚酯包含：(i)基于酸残基的总量，约50-约96％摩尔的一种或多种间苯二甲酸或对苯二甲酸的残基；(ii)基于酸残基的总量，约4-约30％摩尔的钠代磺基间苯二甲酸的残基；(iii)一种或多种二醇残基，其中基于二醇残基的总量，至少25％摩尔为具有结构H-(OCH2-CH2)n-OH的聚(乙二醇)，其中n为2-约500的整数；(iv)基于重复单元的总量，0-约20％摩尔的具有3个或更多个官能团的支化单体的残基，其中所述官能团为羟基、羧基或它们的组合。
磺基聚酯可含有其他浓度的间苯二甲酸残基，例如，约60-约95％摩尔和约75-约95％摩尔。间苯二甲酸残基浓度范围的其他实例为约70-约85％摩尔、约85-约95％摩尔和约90-约95％摩尔。磺基聚酯还可包含约25-约95％摩尔的一缩二乙二醇的残基。一缩二乙二醇残基浓度范围的其他实例包括约50-约95％摩尔、约70-约95％摩尔和约75-约95％摩尔。磺基聚酯还可包括乙二醇和/或1，4-环己烷二甲醇(缩写为“CHDM”)的残基。CHDM残基的典型的浓度范围为约10-约75％摩尔、约25-约65％摩尔和约40-约60％摩尔。乙二醇残基的典型的浓度范围为约10-约75％摩尔、约25-约65％摩尔和约40-约60％摩尔。在另一个实施方案中，磺基聚酯包含约75-约96％摩尔的间苯二甲酸的残基和约25-约95％摩尔的一缩二乙二醇的残基。
使用典型的缩聚反应条件，本发明的磺基聚酯可由适当的二羧酸、酯、酸酐或盐、磺基单体和适当的二醇或二醇混合物容易地制备。可通过连续、半连续和间歇操作方式进行，并且可利用多种反应器类型。合适的反应器类型的实例包括但不限于搅拌槽、连续搅拌槽、浆料、管式、刮板式薄膜、降膜或挤出反应器。本文使用的术语“连续”是指这样的工艺，其中以不间断的方式同时引入反应物并取出产物。“连续”是指该工艺基本上或完全连续操作，并且与“间歇”工艺相反。“连续”不是以任何方式指禁止工艺的连续性中正常的中断，例如由于启动、反应器维修或预定的停工周期。本文使用的术语“间歇”工艺是指这样的工艺，其中将所有的反应物加入到反应器中，随后根据预定的反应过程进行加工，在该过程中不向反应器中加入或移入材料。术语“半连续”是指这样的工艺，其中一些反应物在工艺开始时加入，而剩余的反应物随着反应的进行连续地加入。
或者，半连续工艺还可包括与间歇工艺类似的工艺，其中所有的反应物在工艺开始时加入，只是随着反应的进行连续地移出一种或多种产品。由于如果让磺基聚酯在反应器中在升高的温度下停留太长的持续时间外观会劣化，为了产生优异的聚合物着色，以及，出于经济的原因，该工艺有利地以连续工艺操作。
本发明的磺基聚酯通过本领域技术人员已知的程序来制备。最通常将磺基单体直接加入到制备聚合物的反应混合物中，但是已知其他工艺并且还可采用其他工艺，例如描述于美国专利3,018,272、3,075,952和3,033,822号中的那些工艺。可使用常规的聚酯聚合条件进行磺基单体、二醇组分和二羧酸组分的反应。例如，当通过酯交换反应制备磺基聚酯时，即，由二羧酸组分的酯形式制备，反应过程可包括两步。在第一步，在升高的温度(通常，约150℃-约250℃)下，在约0.0kPa表压-约414kPa表压(60磅/平方英寸，“psig”)压力下，使二醇组分和二羧酸组分(比如，例如，间苯二甲酸二甲酯)反应约0.5-约8小时。优选，酯交换反应的温度范围为约180℃-约230℃，进行约1-约4小时，并且优选的压力范围为约103kPa表压(15psig)-约276kPa表压(40psig)。随后，将反应产物在较高的温度和降低的压力下加热，以形成磺基聚酯，同时除去二醇，二醇在这些条件下容易挥发并从系统中除去。该第二步(或缩聚步骤)在较高的真空和温度(通常约230℃-约350℃，优选约250℃-约310℃，最优选约260℃-约290℃)下持续约0.1-约6小时，或优选进行约0.2-约2小时，直至得到具有期望的聚合度(通过特性粘度确定)的聚合物。缩聚步骤可在降低的压力下进行，该压力为约53kPa(400托)-约0.013kPa(0.1托)。搅拌或适当的条件用于这两个阶段，用于确保反应混合物的足够传热和表面更新。两个阶段的反应均通过适当的催化剂促进，所述催化剂比如，例如，烷氧基钛化合物、碱金属金属氢氧化物和醇盐、有机羧酸的盐、烷基锡化合物、金属氧化物等。还可使用与美国专利5,290,631号所描述的类似的三阶段制造程序，特别是当采用酸和酯的混合单体物料时。
为了确保通过酯交换反应机理的二醇组分和二羧酸组分的反应趋于完全，优选采用约1.05-约2.5摩尔的二醇组分：1摩尔二羧酸组分。然而，本领域技术人员将理解，二醇组分与二羧酸组分的比率通常通过其中发生反应过程的反应器的设计而确定。
在通过直接酯化制备磺基聚酯时，即，由二羧酸组分的酸形式制备，通过二羧酸或多种二羧酸的混合物与二醇组分或多种二醇组分的混合物反应，制备磺基聚酯。该反应在约7kPa表压(1psig)-约1379kPa表压(200psig)，优选小于689kPa(100psig)压力下进行，以制备平均聚合度为约1.4-约10的低分子量、线性或支化的磺基聚酯产物。在直接酯化反应期间采用的温度通常为约180℃-约280℃，更优选约220℃-约270℃。该低分子量聚合物可随后通过缩聚反应而聚合。
热塑性磺基聚酯树脂的量通常为约0.25-约3.00％重量干基，基于干纸的重量。例如，在一个实施方案中，磺基聚酯的量为约0.25-3.00％重量、0.25-2.00％重量或0.25-1.50％重量。在另一个实施方案中，热塑性磺基聚酯的量可为约0.05％重量干基或约0.1％重量或约0.2％重量。通常热塑性磺基聚酯树脂与阳离子强度添加剂的比率为约5∶1-约1∶5。在一个实施方案中，磺基聚酯与阳离子强度添加剂的比率为约1∶1。
再制浆工艺
可使用任何常规的方法进行再制浆工艺。通常，得到再循环的纸浆纤维的纸再制浆的工艺可通过将干浆纤维分散在纸浆纤维的含水悬浮液中的任何机械行为进行。再制浆的条件以及工业上所用的设备讨论于“Handbook for Pulp & Paper Technologists，第2版”，G.A.Smook，Angus Wilde Publications，1992，第194-195和211-212页，该参考文献通过全文引用结合到本文中。
已发现，通过本发明的工艺制备的纸可在比在约相同水平的湿强度下相同的纸再制浆所需的时间实质更短的时间内再制浆。
本发明的纸产品适用于以下领域：纸巾；餐巾纸；面巾纸；液体包装板(牛奶硬纸盒、果汁硬纸盒)；禽肉箱；产品箱；载体板；肉贩包装材料；漂白的袋；海报板；桌布；墙板带；货币纸；地图纸；茶袋；波纹介质；纸板；模塑产品(鸡蛋硬纸盒)；层压级别；地板毡；咖啡滤纸；面包包装材料；多层袋；木瓦包装材料等。
通过本发明的再制浆工艺制备的再循环的纸浆纤维可用于通过常规的造纸工艺来造纸，所述工艺包括提供再循环的纸浆纤维的含水悬浮液，以及将含水悬浮液形成片材和干燥，以得到纸。
已具体参考优选的实施方案详细描述了本发明，但是应理解的是，在本发明的精神和范围内，可实现变体和修改。
通过可能的实施方案的以下实施例可进一步举例说明本发明，但是应理解的是，除非另外具体说明，否则包括这些实施例仅用于举例说明的目的，而不是意欲限制本发明的范围。除非另外说明，否则份和百分比是指重量份和重量百分比。
实施例
使用EastONE S85030磺基聚酯分散体进行以下实施例，以与市售可得的添加剂(比如Kymene
Figure BPA00001449013200201
和Hercobond
Figure BPA00001449013200202
产品，得自HerculesIncorporated，Wilmington，DE)相比，确定加入该磺基聚酯对纸的湿强度、干强度和再制浆能力的影响。
磺基聚酯和聚酰胺表氯醇(PAE)溶液的制备
如下制备3％重量的磺基聚酯溶液。将500g蒸馏水放置在在热板上加热至约88℃的烧杯中。加入15.5g磺基聚酯粒料并继续搅拌，同时在88℃F的温度下保持10-15分钟或直至所有的磺基聚酯已溶解。将混合物冷却，加入蒸馏水，使得溶液的总重量为515.5g。
如下制备3％重量的PAE溶液。将500g蒸馏水放置在烧杯中。将160g 12.5％重量的市售可得的PAE溶液加入到烧杯中，搅拌。
涂布程序：
使用蒸馏水将每一种3％重量溶液分别稀释，使得当将3ml溶液施用于纸片材时，得到0.5％重量的目标附加浓度。
向每一种溶液中加入3滴食品着色剂作为目视助剂，以确保溶液在纸上均匀覆盖。将
Figure BPA00001449013200211
Lydall纸片材放置在较大片的脱模纸上。使用重量为1.87±0.01g的Lydall 18-1/2# Manning 514油纸片材。脱模纸为与铝箔层压的羊皮纸。
如下制备对照物。使用5m1体积移液管将5ml蒸馏水加入到纸片材中。使用2英寸橡胶手动辊将水小心地滚动到片材中。将带有连接的脱模片材的纸片材在93℃的对流烘箱中干燥5分钟。将已干燥的片材在2磅平坦重量下储存4天。该样品称为对照物。
如下制备含有0.5％重量PAE树脂的样品。使用5ml体积移液管将5ml蒸馏水加入到纸片材中。使用手动辊将水小心地滚动到片材中。使用3ml注射器向预先润湿的纸中加入3ml已稀释的PAE溶液。使用手动辊将溶液小心地滚动到片材中，直至得到均匀的颜色。将带有连接的脱模片材的纸片材在93℃的对流烘箱中干燥5分钟。将已干燥的片材在2磅平坦重量下储存4天。该样品称为样品1。
如下制备含有0.5％重量磺基聚酯树脂的样品。使用5ml体积移液管将5ml蒸馏水加入到纸片材中。使用手动辊将水小心地滚动到片材中。使用3ml注射器向预先润湿的纸中加入3ml已稀释的磺基聚酯溶液。使用手动辊将溶液小心地滚动到片材中，直至得到均匀的颜色。将带有连接的脱模片材的纸片材在93℃的对流烘箱中干燥5分钟。将已干燥的片材在2磅平坦重量下储存4天。该样品称为样品2。
如下制备含有0.25％重量PAE和0.25％重量磺基聚酯的本发明的实例。使用5ml体积移液管将5ml蒸馏水加入到纸片材中。使用手动辊将水小心地滚动到片材中。使用3ml注射器向预先润湿的纸中加入3ml已稀释的PAE溶液。使用手动辊将溶液小心地滚动到片材中，直至得到均匀的颜色。让片材静置2分钟。随后使用3ml注射器向纸中加入3ml已稀释的磺基聚酯溶液。将磺基聚酯溶液小心地手动滚动到纸中。将带有连接的脱模片材的纸片材在93℃的对流烘箱中干燥5分钟。将已干燥的片材在2磅平坦重量下储存4天。该样品称为样品3。
使用以下TAPPI测试方法评价对照物和样品1、样品2和样品3的干强度和湿强度：
●T494-om-88：纸和纸板的拉伸断裂性质(使用恒定速率拉伸装置)
●T456-om-87：水-饱和的纸和纸板的拉伸断裂强度(“湿拉伸强度”)
如下确定纸样品的再制浆能力。由Hermann ManufacturingCompany制造的黄铜浆料稀释器用于测试。该浆料稀释器为2升容器，具有3000rpm、3/4马力的三转子。浆料稀释器的直径为6英寸，高10英寸。
将样品切成两个1英寸方块。将2升水样品保持在20℃，并倒入浆料稀释器中。计数器设定为零，将两个样品均放置在浆料稀释器中。以500转的间隔将样品制浆。每一个500转之后，将浆料稀释器暂时停止，将荧光检查灯保持在盆上，以确定样品是否已被完全制浆。记录每500转的组的数值。在15,000转之后，认为样品不可再制浆，并停止测试。测试结果示于下表1。
表1对照物、样品1、样品2和样品3的测试结果
Figure BPA00001449013200221
*注：在15,000转之后，认为样品不可再制浆，并停止测试。

Claims (21)

1.一种可再制浆的纸产品，所述纸产品包含：造纸纤维；阳离子强度添加剂；和热塑性磺基聚酯树脂。
2.权利要求1的可再制浆的纸产品，其中所述磺基聚酯树脂包含(i)一种或多种二羧酸的残基；(ii)基于重复单元的总量，约4-约40％摩尔的至少一种磺基单体的残基，所述磺基单体具有2个官能团和一个或多个与芳族或脂环族环连接的磺酸盐基团，其中所述官能团为羟基、羧基或它们的组合；(iii)一种或多种二醇残基，其中基于二醇残基的总量，至少25％摩尔为具有结构H-(OCH2-CH2)n-OH的聚(乙二醇)，其中n为2-约500的整数；和(iv)基于重复单元的总量，0-约25％摩尔的具有3个或更多个官能团的支化单体的残基，其中所述官能团为羟基、羧基或它们的组合。
3.权利要求2的可再制浆的纸产品，其中所述二羧酸选自脂族二酸、脂环族二羧酸、芳族二羧酸和它们的组合。
4.权利要求3的可再制浆的纸产品，其中所述二羧酸选自琥珀酸、戊二酸、己二酸、壬二酸、癸二酸、富马酸、马来酸、衣康酸、1，3-环己烷二甲酸、1，4-环己烷二甲酸、二甘醇酸、2，5-降冰片烷二甲酸、邻苯二甲酸、对苯二甲酸、1，4-萘二甲酸、2，5-萘二甲酸、2，6-萘二甲酸、2，7-萘二甲酸、联苯甲酸、4，4′-氧基二苯甲酸、4，4′-磺酰基二苯甲酸、间苯二甲酸和它们的组合。
5.权利要求2的可再制浆的纸产品，其中所述磺基单体为磺基邻苯二甲酸、磺基对苯二甲酸、磺基间苯二甲酸的金属磺酸盐或它们的组合。
6.权利要求2的可再制浆的纸产品，其中所述二醇残基选自乙二醇、一缩二乙二醇、二缩三乙二醇、聚乙烯二醇、1，3-丙二醇、2，4-二甲基-2-乙基己-1，3-二醇、2，2-二甲基-1，3-丙二醇、2-乙基-2-丁基-1，3-丙二醇、2-乙基-2-异丁基-1，3-丙二醇、1，3-丁二醇、1，4-丁二醇、1，5-戊二醇、1，6-己二醇、2，2，4-三甲基-1，6-己二醇、硫代二乙醇、1，2-环己烷二甲醇、1，3-环己烷二甲醇、1，4-环己烷二甲醇、2，2，4，4-四甲基-1，3-环丁二醇、对苯二甲醇和它们的组合。
7.权利要求2的可再制浆的纸产品，其中所述支化单体为1，1，1-三羟甲基丙烷、1，1，1-三羟甲基乙烷、甘油、季戊四醇、赤藓醇、苏糖醇、二季戊四醇、山梨糖醇、偏苯三酸酐、苯均四酸二酐、二羟甲基丙酸或它们的组合。
8.权利要求1的可再制浆的纸产品，其中所述阳离子强度添加剂选自聚丙烯酰胺树脂、聚酰胺表卤代醇树脂、聚胺表卤代醇树脂、聚酰氨基胺表卤代醇树脂、聚亚烷基亚胺树脂、脲-甲醛树脂、三聚氰胺-甲醛树脂、阳离子多糖或它们的组合。
9.权利要求8的可再制浆的纸产品，其中所述阳离子强度添加剂选自阳离子乙二醛化的聚丙烯酰胺树脂或聚酰氨基胺表氯醇树脂。
10.权利要求1的可再制浆的纸产品，其中所述造纸纤维选自木质纤维、软木纤维、硬木纤维、非木质纤维、合成聚合物纤维、再循环的纤维、玻璃纤维或它们的组合。
11.权利要求10的可再制浆的纸产品，其中所述合成聚合物纤维大于造纸纤维总量的50％。
12.权利要求11的可再制浆的纸产品，其中所述合成聚合物纤维的平均纤维直径小于5微米。
13.权利要求1的可再制浆的纸产品，其中阳离子强度添加剂的量为约0.25％重量-约3％重量干基，并且热塑性磺基聚酯树脂的量为约0.25-约3.00％重量干基，相对于造纸纤维的重量。
14.权利要求1的可再制浆的纸产品，其中热塑性磺基聚酯树脂与阳离子强度添加剂的比率为约5∶1-约1∶5。
15.权利要求1的可再制浆的纸产品，其中磺基聚酯与阳离子强度添加剂的比率为约1∶1。
16.一种改进纤维素纸的湿强度的方法，所述方法包括在造纸过程期间向造纸纤维中加入阳离子强度添加剂；和磺基聚酯热塑性树脂。
17.权利要求16的方法，其中在造纸过程期间将所述阳离子强度添加剂和磺基聚酯热塑性树脂加入到造纸纤维的含水浆料中。
18.权利要求16的方法，其中将所述阳离子强度添加剂加入到造纸纤维的含水浆料中，并将所述磺基聚酯热塑性树脂施用于由所述造纸纤维脱水得到的纸网上。
19.权利要求18的方法，其中通过喷涂将所述热塑性磺基聚酯树脂施用于纸网。
20.权利要求16的方法，其中所得到的纸产品表现出增强的再制浆能力。
21.一种纸产品，所述纸产品包含：
造纸纤维，其由木质纤维、软木纤维、硬木纤维、非木质纤维、合成聚合物纤维、再循环的纤维或玻璃纤维中的一种或多种组成；
阳离子强度添加剂，其由聚丙烯酰胺树脂、聚酰胺表卤代醇树脂、聚胺表卤代醇树脂、聚酰氨基胺表卤代醇树脂、聚亚烷基亚胺树脂、脲-甲醛树脂、三聚氰胺-甲醛树脂或阳离子多糖中的一种或多种组成；和
热塑性磺基聚酯树脂，所述磺基聚酯树脂包含(i)一种或多种二羧酸的残基；(ii)基于重复单元的总量，约4-约40％摩尔的至少一种磺基单体的残基，所述磺基单体具有2个官能团和一个或多个与芳族或脂环族环连接的磺酸盐基团，其中所述官能团为羟基、羧基或它们的组合；(iii)一种或多种二醇残基，其中基于二醇残基的总量，至少25％摩尔为具有结构H-(OCH2-CH2)n-OH的聚(乙二醇)，其中n为2-约500的整数；和(iv)基于重复单元的总量，0-约25％摩尔的具有3个或更多个官能团的支化单体的残基，其中所述官能团为羟基、羧基或它们的组合。
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BRPI1014169A2 (pt) 2016-04-05
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