CN100366663C - 纤维素和木素纤维素材料与树脂的组合物和复合材料、和制造它们的方法 - Google Patents

纤维素和木素纤维素材料与树脂的组合物和复合材料、和制造它们的方法 Download PDF

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CN100366663C
CN100366663C CNB03806636XA CN03806636A CN100366663C CN 100366663 C CN100366663 C CN 100366663C CN B03806636X A CNB03806636X A CN B03806636XA CN 03806636 A CN03806636 A CN 03806636A CN 100366663 C CN100366663 C CN 100366663C
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resin
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lignin
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马歇尔·梅多夫
亚瑟·P·拉加斯
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Abstract

本发明公开了纤维素材料或木素纤维素材料、和由它们制得的组合物和复合材料。

Description

纤维素和木素纤维素材料与树脂的组合物和复合材料、和制造它们的方法
相关申请的交叉参考
本申请是2003年1月6日提交的美国专利申请序列号10/336,972的部分继续，申请10/336,972是2002年3月21日提交的美国专利申请序列号10/104,414的部分继续申请，申请10/104,414是2001年1月30日提交的美国专利申请序列号09/772,593的部分继续申请，申请09/772,593是：(a)1999年6月22日提交的美国专利申请序列号09/337,580、现在公布为美国专利号6,207,729的部分继续申请，申请09/337,580是1997年10月31日提交的美国专利申请序列号08/961,863、现在公布为美国专利号5,973,035的部分继续申请；(b)1999年6月22日提交的美国专利申请序列号09/338,209的部分继续申请，申请09/338,209是1997年9月2日提交的美国专利申请序列号08/921,807、现在公布为美国专利号5,952,105的部分继续申请，和(c)1999年4月9日提交的美国专利申请序列号09/290,031、现在公布为美国专利号6,258,876的部分继续申请，申请09/290,031为1997年10月31日提交的美国专利申请号08/961,863、现在公布为美国专利号5,973,035的分案；和(2)2000年6月13日提交的美国专利申请序列号09/593,627的部分继续申请，申请09/593,627是美国专利申请序列号09/337,580和09/338,209的部分继续申请。所有上述申请和专利都全文引入本文以供参考。
发明背景
本发明涉及膨松的(texturized)纤维素材料或木素纤维素材料以及由这种膨松材料制造的组合物和复合材料。
在众多应用中都大量生产、加工和使用纤维素和木素纤维素材料。一旦这些材料被用过，它们就通常被丢弃。因此，废纤维素和木素纤维素材料的数量不断增加。
发明概述
本发明大体上涉及膨松纤维素材料或木素纤维素材料和由它们制造的组合物和复合材料。
在一个实施方案中，本发明涉及制造复合材料的方法。该方法包括以下步骤：(a)剪切纤维素纤维或木素纤维素纤维到其内部纤维充分暴露形成膨松纤维素纤维或木素纤维素纤维的程度，和(b)使纤维素纤维或木素纤维素纤维与树脂结合。可以任意顺序(即(a)然后(b)，或(b)然后(a))或同时(即在大约同一时间内)实施这些步骤。树脂可为例如热塑性树脂、热固性树脂、弹性体、焦油、沥青或木素。具体的例子包括聚苯乙烯、聚碳酸酯、聚丁烯、热塑性聚酯、聚醚、热塑性聚氨酯、PVC、尼龙、醇酸树脂、邻苯二甲酸二烯丙酯、环氧树脂、三聚氰胺、酚醛树脂、硅树脂、脲、热固性聚酯、天然橡胶、异戊二烯橡胶、苯乙烯-丁二烯共聚物、氯丁橡胶、丁腈橡胶、丁基橡胶、乙烯丙烯共聚物(即“EPM”)、三元乙丙共聚物(即“EPDM”)、海帕伦(hypalon)、丙烯酸类橡胶、聚硫橡胶、硅树脂、氨基甲酸乙酯、含氟弹性体、丁二烯或表氯醇橡胶。
纤维可为例如黄麻、洋麻、亚麻、大麻、棉、碎布、纸、纸制品或造纸副产品。具体的例子包括纸浆板、新闻纸、杂志纸、多涂层(poly-coated)纸和漂白的牛皮纸板。纤维可为天然的或合成的纤维素材料或木素纤维素材料，并可为织物材料或非织造材料。
在与树脂结合前，可使用旋转切断机或其它机械方法进行剪切步骤，或可在混合机或挤出机内原地进行剪切步骤。在一些情况下，在混合机或挤出机内的螺杆能有效地剪切材料。
在某些实施方案中，该方法还可包括在步骤(a)后但在步骤(b)前使膨松纤维致密化。致密化步骤提高了膨松材料的堆密度，通常增加到至少2或3倍。在一些情况下，堆密度可增加到5至10倍或更多。致密化膨松纤维的堆密度的优选范围为约5-25磅/立方英尺。更优选的范围为约8-15磅/立方英尺。致密化步骤能将膨松纤维压缩成任意形状或大小的丸粒。
利用上述方法制造的复合材料也是本发明的一个方面。在本发明的一种典型复合材料中，至少约50％的纤维具有至少约5(如5、10、15、25、30、35、40、50或更高)的长度/直径比。
包括这种复合材料以及化学物质或化学制剂的组合物也是本发明的一个方面。这类化学制剂的例子包括能在其它不相容材料如亲水纤维和疏水树脂之间提供混合、键合、粘合、分相和/或连接界面的增容剂如FUSABOND。
在另一实施方案中，本发明涉及制备膨松纤维材料的方法。该方法包括剪切具有内部纤维的纤维素材料或木素纤维素材料(如亚麻；大麻；棉；黄麻；碎布；成品纸或非成品纸、纸制品，包括多涂层纸或造纸副产品如纸浆板；或合成纤维素材料或木素纤维素材料如人造纤维)到内部纤维充分暴露并产生膨松纤维材料的程度。纤维素材料或木素纤维素材料可为织物材料如机织物，或非织造材料如纸或草纸。膨松纤维材料的暴露纤维可具有至少约5(至少约5、10、25、50或更高)的长度/直径(L/D)比。例如，至少约50％的纤维可具有这种量级的L/D比。
在另一实施方案中，本发明涉及包括具有内部纤维的纤维素材料或木素纤维素材料的膨松纤维材料，其中剪切纤维素材料或木素纤维素材料到内部纤维充分暴露的长度。
膨松纤维材料可例如被包括(如联合、掺合、靠近、被环绕或在内部)到结构或载体(如网、膜、浮选设备、袋、壳或可生物降解物质)内。任选地，结构或载体本身可由膨松纤维材料(如本发明的膨松纤维材料)制成，或由膨松纤维材料的组合物或复合材料制成。
膨松纤维材料可具有小于约0.5克/立方厘米、或甚至小于约0.2g/cm3的堆密度。
包括上述膨松纤维材料和化学物质或化学制剂(例如药物如抗生素或避孕药与任选的赋形剂；农业化合物如肥料、除草剂或杀虫剂；或包括酶的制剂)的组合物也在本发明的范围内，包括膨松纤维材料和其它液体或固体成分(例如微粒状、粉末状或颗粒状固体如植物种子、食品或细菌)的组合物也在本发明范围内。
还考虑了包括热塑性树脂和膨松纤维材料的复合材料。树脂可为例如聚乙烯、聚丙烯、聚苯乙烯、聚碳酸酯、聚丁烯、热塑性聚酯、聚醚、热塑性聚氨酯、聚氯乙烯或聚酰胺，或两种或多种树脂的组合。
在一些情况下，复合材料中包括的纤维材料的至少约5wt％(如5％、10％、25％、50％、75％、90％、95％、99％或约100％)是膨松的。
复合材料可包括例如约30wt％至约70wt％的树脂和约30wt％至约70wt％的膨松纤维材料，尽管也可使用这些范围以外的比例。复合材料可相当坚固，在一些情况下具有至少约6000至10000psi的抗弯强度。
在另一实施方案中，本发明涉及包括树脂如热塑性树脂和至少约2wt％、更优选至少约5wt％的膨松纤维素纤维或木素纤维素纤维的复合材料。本发明还涉及包括聚乙烯和至少约50wt％的膨松纤维素纤维或木素纤维素纤维的复合材料。
本发明还涉及包括树脂和纤维素纤维或木素纤维素纤维、抗弯强度为至少约3000psi或抗拉强度为至少约3000psi的复合材料。
另外，本发明涉及制造复合材料的方法；该方法包括剪切纤维素纤维或木素纤维素纤维以形成膨松纤维素纤维或木素纤维素纤维，然后使膨松纤维与树脂结合。一种优选的方法包括用转刀切断机剪切纤维。本发明还涉及制造复合材料的方法，该方法包括剪切纤维素纤维或木素纤维素纤维并使纤维与树脂结合。
本发明还涉及一种方法，该方法包括剪切纤维素纤维或木素纤维素纤维到其内部纤维充分暴露形成膨松纤维素纤维或木素纤维素纤维的程度，和致密化膨松纤维素纤维或木素纤维素纤维。在致密化之前或之后可处理膨松纤维素纤维或木素纤维素纤维，或另外将其与其它物质结合。可用例如能有助于致密化纤维的致密化和/或随后重开启(reopening)的物质处理膨松纤维素纤维或木素纤维素纤维。
本发明还涉及致密化的膨松纤维素纤维或木素纤维素纤维。
上述复合材料还可包括无机添加剂如碳酸钙、石墨、石棉、硅灰石、云母、玻璃、纤维玻璃、白垩、滑石、硅石、陶瓷、地面建筑废弃物、轮胎用橡胶粉末、碳纤维或金属纤维(如不锈钢或铝)。这类无机添加剂可占例如复合材料总重量的约0.5％至约20％。
复合材料可为例如以下形式：垫衬(pallet)(如注射成型垫衬)、管、面板、铺面材料、板、外壳、薄片、棒、带、栅栏、构件、门、百叶窗、遮阳篷、帘、牌子、框架、窗子挡板(windown casing)、底板、墙板、地板、瓷砖、铁路枕木、模板、支架、工具把手、棚、基床、分配器、桶板(stave)、薄膜、外衣、大手提包(tote)、桶、箱、填料、篮、带、窄条、架、套、结合件、间隔物、墙、室内和室外地毯、垫子、织物，和席子、框架、书架、雕刻品、椅、桌、书桌、艺术品、玩具、比赛用具、锭盘、桥墩、舟、桅杆、污染控制产品、化粪池、汽车面板、基底、计算机外壳、地面上的和地面下的电保护性外套、家具、野餐用桌子、帐篷、运动场、长椅、掩体、体育用品、床、便盆、线、单丝、布、装饰板、支架、衣架、托盘、水池、绝缘体、小箱、图书封面、衣服、棍(cane)、拐杖、和其它建筑、农业、材料处理、运输、汽车、工业、环境、海军、电气、电子、娱乐、医疗、织物和消费产品。复合材料还可为纤维、单丝或薄膜的形式。
本文使用的术语“膨松的纤维素材料或木素纤维素材料”和“膨松的纤维材料”是指纤维素材料或木素纤维素材料已被剪切到其内部纤维充分暴露的程度。这些纤维的至少约50％、更优选至少约70％具有至少5、更优选至少25、或至少50的长度/直径(L/D)比。图1中示出了膨松的纤维素材料的一个例子。
本发明的膨松纤维素材料具有能使它们用于各种用途的性能。例如，膨松的纤维素材料具有吸收性能，这可被开发用于例如污染控制。纤维通常是可生物降解的，这使它们适用于例如药物或化学物质递送(如在人类、动物的治疗中，或在农业应用中)。还可使用膨松的纤维材料增强聚合树脂。
本文中使用的术语“热固性树脂”是指能固化、凝固或硬化为永久形状的塑料(如有机聚合物)。固化为不可逆化学反应，典型地涉及利用热或辐射(如UV辐射)的分子交联。可在例如室温或高温下引发或完成热固性材料的固化。固化反应中发生的交联由两个线性高聚物之间或穿过这两个线性高聚物的原子的连接引起，产生三维硬化化学结构。
热固性树脂的例子包括但不限于：硅树脂、醇酸树脂、邻苯二甲酸二烯丙酯(烯丙基树脂)、环氧树脂、三聚氰胺、酚醛树脂、某些聚酯、硅树脂、脲、聚氨酯、聚烯烃基热固性树脂如TELENETM(BFGoodrich)和METTONTM(Hercules)。
本文使用的术语“弹性体”是指在变形并接着释放之后能迅速恢复到接近其初始尺寸和形状的大分子材料。
弹性体的例子包括但不限于：天然橡胶、异戊二烯橡胶、苯乙烯-丁二烯共聚物、氯丁橡胶、丁腈橡胶、丁基橡胶、乙烯丙烯共聚物(即“EPM”)和三元乙丙共聚物(即“EPDM”)、海帕伦、丙烯酸类橡胶、聚硫橡胶、硅树脂、氨基甲酸乙酯、含氟弹性体、丁二烯或表氯醇橡胶。
本文使用的术语“焦油”是指通过蒸馏木材、泥煤、煤、页岩或其它植物或矿物材料得到的烃类及其衍生物的典型地为深褐色到黑色的液体混合物。一个例子是煤焦油，其通过烟煤或原油(例如包含萘、甲苯、喹啉、苯胺和甲酚)的分解蒸馏制得。
本文使用的术语“木素”是指从木材、植物、再循环木材或植物制品中分离出的无定形物质、混合物或粉末，或为造纸副产品。在性质上，木素和纤维素一起形成植物的木质细胞壁和在它们之间的粘结材料。它们一般为聚合的，并可通过以下因素与纤维素区分开：(1)比纤维素高的碳含量，和(2)包含丙基-苯单元、甲氧基和/或羟基。它们一般不会被酸水解，但可溶于热碱和亚硫酸氢盐中，并可被容易地氧化。可从制造纤维素纸浆的硫酸盐法或苏打法得到的液体中或从亚硫酸盐废液中回收木素。因此术语“木素”包括亚硫酸盐木素或木素-磺酸盐。
本文使用的术语“沥青(asphalt)”是指例如通过氧气作用由高沸点矿物油产生的烃、黑褐色沥青(pitch)或沥青(bitument)的无定形固体或半固体混合物。沥青既包括沥青质，又包括碳置沥青。沥青通常用于铺路、盖屋顶和防水材料。
新型组合物具有能使它们用于各种用途的性能。包括膨松纤维材料和基质的组合物为例如坚固、轻质和便宜的。
膨松纤维提供的其它优点包括：
(1)基质材料如弹性体和热固性树脂的密度降低。
(2)由于基质和膨松纤维间的界面面积增加和当膨松纤维与基质分层时吸收的能量增加而使抗冲击性增加。
(3)表面摩擦降低。
(4)高润滑性表面。
(5)基质中的疏水和亲水组分的耐受性和增容作用增强。
(6)定制组合物的性质用于特定需求的能力提高。
用于制造组合物的原料可为新料或再循环料；例如，它们可包括由树脂组成的废弃容器、和废纤维素纤维或木素纤维素纤维。
本发明的其它特征和优点将在以下详细描述和权利要求书中变得显而易见。
附图简述
图1为放大50倍的膨松新闻纸的照片；
图2为放大50倍的膨松多涂层纸的照片；
图3为半加仑聚合板(polyboard)果汁纸盒的照片；
图4为粉碎的半加仑聚合板果汁纸盒的照片；和
图5为通过剪切图4的粉碎的半加仑聚合板果汁纸盒制备的膨松纤维材料的照片。
发明详述
纤维素原料的例子包括纸和纸制品如新闻纸、多涂层纸和造纸得到的废水；木素纤维素原料的例子包括木材、木质纤维和与木材有关的材料，以及得自洋麻、草、稻壳、甘蔗渣、棉、黄麻、其它茎类植物(如大麻、亚麻、竹；韧皮纤维和包芯纤维)、叶类植物(如剑麻、蕉麻)和农业纤维(如谷草、玉米穗轴、稻壳和椰子毛)的材料。除了新料外，消费后物品(post-consumer)、工业品(如废物)和生产废料(如废水)也可用作纤维源。
膨松纤维材料的制备
如果使用废纤维素材料或木素纤维素材料，则它们应优选是清洁和干燥的，尽管也可在用水、溶剂、增容剂或树脂润湿后剪切材料。可使用大量机械手段中的任意一种或其组合来膨松化原料。一种膨松化方法包括首先将纤维素材料或木素纤维素材料切成1/4至1/2英寸的片，如果需要，使用标准切割装置来切割。也可使用反向旋转螺杆粉碎机和分段旋转螺杆粉碎机如Munson(Utica，NY)制造的那些，也可使用在许多办公室中可找到的标准的文件粉碎机。
然后可用旋转切断机如Sprout，Waldron Companies制造的那种机器剪切纤维素材料或木素纤维素材料，这在Perry的Chem.Eng.Handbook，第6版第8-29页(1984)上有描述。尽管可使用其它设置值，但旋转切断机的转刀和底刀之间的间距一般被设置到0.020″或更小，刀片旋转被设置到750rpm或更高。在加工过程中可使用例如水夹套将旋转切断机冷却至100℃或更低。
使膨松材料通过卸料筛。在大规模生产中可使用较大的筛(如大至6mm)。通常保持纤维素或木素纤维素给料与旋转切断机的刀片接触直到纤维被撕开；较小的筛(如2mm筛目)能提供较长的停留时间和更完全的膨松化，但会导致较低的长度/直径(L/D)纵横比。可将真空抽吸器连接到筛上以最大化并保持纤维长度/直径纵横比。
膨松的纤维材料可直接储存在密封袋中，或可在使用前立即在大约105℃下干燥4-18小时(如直到水分含量小于约0.5％)。图1为膨松的新闻纸的SEM照片。
替代的膨松化方法包括石磨、机械撕裂或撕开、和将材料内部纤维暴露的其它方法(如针磨、空气磨碎)。这些其它方法的例子还可包括在用于混合纤维和树脂的混合机内或在挤出机内原地剪切。例如可在加入树脂之前、之后或同时加入纤维材料，而不管树脂为固体形式(如粉状或粒状)还是液体形式(如熔体或在溶液中)。
在材料被膨松化后，可任选地将其“致密化”或压缩，以有利于运输、储存、处理、加工和/或给料到混合或挤出设备中。例如可使用轧制机(其能形成丸粒或其它形状)或造粒机进行致密化。可使用或改造在农业、制药业(如“造丸”机)、冶金和其它工业领域中使用的造粒机用于致密化膨松纤维。造粒机可从例如California Pellet Mill(Model Lab Mill)得到。
在致密化过程中，提高了膨松材料的堆密度。例如，尽管新多涂层纸可能具有例如60-90磅/立方英尺的堆密度，而膨松的多涂层纸可能具有约2-6磅/立方英尺(即约0.03-0.1g/cc)的堆密度，由其得到的致密化材料可具有例如10-50磅/立方英尺、或15-35磅/立方英尺、或20-30磅/立方英尺如25磅/立方英尺的堆密度。优选地，致密化纤维的堆密度不会超过起始未致密化材料的堆密度。上述范围内的堆密度允许在挤出过程中有相对高的进料速度(即比堆密度为2.8的材料的进料速度大将近10倍)而不破坏膨松纤维的完整性。在许多应用中可用致密化膨松纤维代替非致密化膨松纤维，因为即使致密化膨松纤维具有相对高的堆密度，但一旦致密化纤维被送入混合、挤出或其它加工设备中，纤维就可容易地重“开启”以重新暴露纤维。
任选地，可在致密化前向膨松材料中加入有助于致密化的物质。这些物质的例子包括抗静电剂、润湿剂、硬化剂、增容剂、加工助剂、稳定剂和粘合剂。另外，还可加入有助于致密化材料的重开启的物质；可在致密化前将这些物质加入到膨松材料中，或可以将它们直接加入到致密化材料中。
膨松纤维材料的应用
可制备膨松纤维材料和这类纤维与其它化学物质和化学制剂的组合物和复合材料以利用材料性能。可使用这些材料吸收化学物质，例如，潜在地吸收其自身重量的很多倍。可在这些应用中以其未致密化形式或致密化形式使用这些膨松纤维材料。因此，这些材料能用于例如吸收溢出的油、或清除如水中、空气中或陆地上的环境污染。同样，材料的吸收性能及其可生物降解性还使它们用于化学物质或化学制剂的递送。例如，可用酶或药物如抗生素、营养素或避孕药以及任何必需的赋形剂的溶液处理这些材料用于药物递送(如人类或动物的治疗，或在动物饲料和/或动物草垫中使用)，以及用肥料、杀草剂或杀虫剂的溶液处理。可任选地化学处理这些材料以提高吸收率性质。例如，可用硅烷处理材料以为它们提供亲油性。膨松纤维材料可任选地与化学物质或化学制剂结合，或另外进行处理，然后致密化。另外，致密化膨松纤维材料可任选地与化学物质或化学制剂结合，或另外进行处理。
也可制备包括膨松材料与液体或微粒状、粉状或颗粒状固体结合的组合物。例如，可将膨松材料与种子(即用肥料、杀虫剂等的溶液处理或没有处理的)、食品或细菌(如消化毒素的细菌)混合。纤维材料与组合物其它组分的比取决于组分的性质，并可被容易地调整用于特定产品应用。任选地，膨松材料可与其它组分结合，并致密化结合物。另外，膨松材料可在致密化后与其它组分结合。
在一些情况下，使膨松纤维材料或这类材料的组合物或复合材料与结构或载体如网、膜、浮选设备、袋、壳或可生物降解物质联合可能是有利的。任选地，载体结构本身可由膨松纤维材料(如本发明的材料)或其组合物或复合材料制成。
膨松纤维材料和树脂的复合材料
膨松纤维材料(任选地为致密化形式)还可与树脂结合形成坚固轻质的复合材料。如上所述，已用化学物质或化学制剂处理的材料可同样与可生物降解或不可生物降解树脂结合，从而形成复合材料，并允许引入例如亲水物质到另外的疏水聚合物基质内。或者，可用化学物质或化学制剂处理包括膨松纤维材料和树脂的复合材料。
膨松纤维素材料或木素纤维素材料为复合材料提供强度。复合材料可包括约10wt％至约90wt％、例如约30wt％至约70wt％的膨松纤维素材料或木素纤维素材料。
树脂在复合材料中封装膨松纤维素材料或木素纤维素材料，并帮助控制复合材料的形状。树脂还转移外部负荷到纤维材料，并保护纤维不受环境和结构损害。复合材料可包括例如约10wt％至约90wt％、更优选约30wt％至约70wt％的树脂。
在各种应用例如在食品包装中使用树脂。由树脂制成的食品容器一般使用一次，然后丢弃。适于与膨松纤维结合的树脂的例子包括聚乙烯(包括例如低密度聚乙烯和高密度聚乙烯)、聚丙烯、聚苯乙烯、聚碳酸酯、聚丁烯、热塑性聚酯(如PET)、聚醚、热塑性聚氨酯、PVC、聚酰胺(如尼龙)和其它树脂。优选树脂具有低熔体流动指数。优选的树脂包括熔体流动指数小于3g/10min、更优选小于1g/10min的聚乙烯和聚丙烯。
可购买树脂作为新料，或以废料形式获得树脂，并可购买丸粒或颗粒形式。一种废树脂源是使用过的聚乙烯牛奶瓶。但是，如果在丸粒或颗粒树脂上存在表面水分，则应在使用前干燥。
复合材料还可包括偶联剂。偶联剂有助于将亲水纤维键合到疏水树脂上。偶联剂的例子包括马来酸酐改性的聚乙烯，如FUSABOND(得自Dupont，Delaware)和POLYBOND(得自Uniroyal Chemical，Connecticut)系列中的那些。一种合适的偶联剂为马来酸酐改性的高密度聚乙烯如FUSABONDMB100D。
复合材料还可包含混合领域中那些技术人员已知的添加剂，如增塑剂、润滑剂、抗氧化剂、遮光剂、热稳定剂、着色剂、阻燃剂、抗微生物剂、抗冲改性剂、光稳定剂和抗静电剂。
复合材料还可包括无机添加剂如碳酸钙、石墨、石棉、硅灰石、云母、玻璃、纤维玻璃、白垩、硅石、滑石、陶瓷、地面建筑废弃物、轮胎用橡胶粉末、碳纤维或金属纤维(如铝、不锈钢)。当包括这类添加剂时，它们的存在量一般为约0.5wt％直到约20-30wt％。例如，可向纤维和树脂的复合材料中加入亚微碳酸钙以提高抗冲改性特性或提高复合材料强度。
上述树脂、偶联剂和其它添加剂可与膨松材料结合，并可任选地致密化得到的复合材料。
组合物的制备
可制备包含膨松纤维素材料或木素纤维素材料和化学物质、化学制剂或其它固体的组合物，例如在各种浸涂、喷涂或混合装置中，所述装置包括但不限于：螺条混合器、单锥鼓式搅拌机、双锥鼓式搅拌机和Patterson-Kelly“V”型混合器。
例如，可在单锥鼓式搅拌机中制备包含90wt％的膨松纤维素材料或木素纤维素材料和10wt％的磷酸铵或碳酸氢钠的组合物以制造用于吸收油的阳燃材料。
膨松纤维和树脂的复合材料的制备
可按如下方法制备膨松纤维材料和树脂的复合材料。将标准的混合橡胶/塑料的2辊轧制机加热到325-400。将树脂(通常为丸粒或颗粒的形式)加入到加热的轧制机中。约5-10分钟后，向轧制机中加入偶联剂。再过5分钟后，将膨松纤维素材料或木素纤维素材料加入到熔融的树脂/偶联剂混合物中。在约10分钟的时段内加入膨松材料。
从轧制机中移出复合材料，切成片并冷却至室温。然后使用标准压模技术将其压模成薄板(plaque)。
或者，在混合器如Banbury封闭式混合器中装入成分。在优选地保持温度不小于约190℃下混合成分。然后可压模混合物。
在另一实施方案中，可在挤出机混合器如装有同步旋转螺杆的双螺杆挤出机内混合成分。在挤出机进料喉处引入树脂和偶联剂；在沿挤出机长度向下路径约1/3处将膨松纤维素材料或木素纤维素材料引入到熔融树脂内。挤出机内部温度优选保持在小于约190℃，但是在某些剖面的挤出过程中可能会遇到较高的温度(如270℃)。在出口处，例如可通过冷绞线切割(cold strand cutting)来使复合材料成为粒子。
或者，可首先在混合器内制备混合物，然后转移到挤出机中。
在另一实施方案中，可使用本领域那些技术人员已知的纤维形成技术将复合材料形成为纤维，或形成为用于针织、整经、机织、编织或制作非织造织物的单丝。在又一实施方案中，可将复合材料制成膜。
膨松纤维材料和树脂的复合材料的性质
得到的复合材料包括密封在树脂基质内的纤维网络。纤维形成晶格网络，其能为复合材料提供强度。由于纤维素材料或木素纤维素材料是膨松的，因此与用非膨松纤维素材料或木素纤维素材料制备的复合材料相比，可用于与树脂粘合的表面积的量增加。树脂粘合到暴露纤维的表面上，造成纤维网络与树脂基质的紧密混合。纤维与树脂基质的紧密混合进一步加强了复合材料。
这些组合物还可包括无机添加剂如碳酸钙、石墨、石棉、硅灰石、云母、玻璃、纤维玻璃、白垩、硅石、滑石、阻燃剂如三水合氧化铝或氢氧化镁、地面建筑废弃物、轮胎用橡胶粉末、碳纤维或金属纤维(如铝、不锈钢)。这些添加剂可增强、扩展、改变电性能或机械性能或相容性，并可提供其它的益处。当包括这类添加剂时，它们的装填量可为低于1wt％至高达80wt％。典型的装填量范围为0.5wt％至50wt％。
聚合的弹性组合物还可包括偶联剂。偶联剂有助于将膨松纤维材料的亲水纤维粘合到树脂上。
具有热固性或弹性体基质的组合物还可包含混合领域中那些技术人员已知的添加剂，如增塑剂、润滑剂、抗氧化剂、遮光剂、热稳定剂、着色剂、抗冲改性剂、光稳定剂、抗微生物剂、抗静电剂、有机或无机阻燃剂、生物降解剂和分散剂。当特殊的配方需要特殊的性能改进时，可使用特殊的纤维表面处理和添加剂。
下面是组合物的非限制性实施例。
热固性树脂：可制备膨松纤维材料和热固性树脂的组合物作为整体模塑成型料(bulk molding compound)(BMC)、片状模塑成型料(sheetmolding compound)(SMC)或其它制剂。
通过在揉面机中混合树脂和碎纤维，然后混合直到纤维充分润湿，并且材料具有制模用粘土的稠度，从而制得整体模塑成型料(BMC)。多数BMC基于聚酯，但有时使用乙烯基酯和环氧树脂。将预称重量的化合物放在压模内，然后密闭压模并在压力下加热以交联热固性聚合物。许多电子部件使用BMC化合物和加工制得。其它应用包括微波天线、桌面和电绝缘箱。
通过混合聚酯树脂和填充剂、颜料、催化剂、脱模剂和/或能与聚合物反应以大大提高粘度的特定增稠剂，制得片状模塑成型料(SMC)。将树脂混合物铺展到移动的尼龙膜上面。树脂在分散膨松纤维的进料器下通过。在顶部放置第二层膜，将化合物夹在里面。然后材料穿过能帮助树脂润湿纤维的辊，并卷起材料。使用前，除去尼龙膜并模塑化合物。
可使用其它技术和制备方法制备和固化热固性体系。
弹性体：可通过已知的方法制备膨松纤维材料和弹性体的组合物。在一种方法中，例如，将弹性体加入到混合橡胶/塑料的2辊轧制机中。几分钟后，把其它组分(包括硫化剂)加入到轧制机中。一旦使弹性体混合，就将膨松纤维材料加入到轧制机中。在约10分钟的时段内加入膨松纤维材料。从轧制机中移出混合的材料并切成片。然后使用标准压模方法将其压模成所需的形状。
或者，可使用混合器如Banbury封闭式混合器或合适的双螺杆或单螺杆混合机。如果使用Banbury混合器，则例如可将配制的混合物卸出并落到轧制机上用于压片。单螺杆或双螺杆混合机产生片作为挤出物。然后可压模混合物。同样地，单螺杆或双螺杆混合机可挤出能被直接硫化的型材。组合物能被模塑、挤出、压缩、切割或磨碎。
膨松纤维材料和树脂的复合材料的应用
可在大量应用中使用树脂/纤维材料复合材料。复合材料坚固轻质；它们可用作例如木材替代品。树脂涂层使复合材料耐水，因此可在户外应用中使用它们。例如，复合材料可用于制造垫衬(其经常被长期存放在户外)、酒桶板、小船、家具、滑雪橇和桨。考虑许多其它应用，包括面板、管、铺面材料、板、外壳、薄片、棒、带、栅栏、构件、门、百叶窗、遮阳篷、帘、牌子、框架、窗子挡板、底板、墙板、地板、瓷砖、铁路枕木、模板、支架、工具把手、棚、基座、分配器、桶板、薄膜、外衣、大手提包、桶、箱、填料、篮、带、窄条、架、套、结合件、间隔物、墙、室内和室外地毯、垫子、织物，和席子、框架、书架、雕刻品、椅、桌、书桌、艺术品、玩具、比赛用具、锭盘、桥墩、舟、桅杆、污染控制产品、化粪池、汽车面板、基底、计算机外壳、地面上的和地面下的电保护性外套、家具、野餐用桌子、帐篷、运动场、长椅、掩体、体育用品、床、便盆、线、单丝、布、装饰板、支架、衣架、托盘、水池、绝缘体、小箱、图书封面、衣服、棍、拐杖、和其它建筑、农业、材料处理、运输、汽车、工业、环境、海军、电气、电子、娱乐、医疗、织物和消费产品。还可以想象到大量其它应用。还可使用复合材料例如作为镶边制品的底座或构架，或夹在纸或其它材料层之间。此外，复合材料可被例如表面处理、开槽、磨碎、成型、压印、变形、压缩、冲孔或着色。
下面的实施例描述了本发明的某些实施方案和方面，但并不能被视为限制本发明的范围。
实施例
实施例1
从International Paper得到由多涂层白牛皮纸板制成的1500磅新半加仑果汁纸盒的垫板(skid)。图3中示出了一个这样的纸盒。每个纸盒被展平。
将纸盒以大约15-20磅/小时的速度送入3马力的Flinch Baugh粉碎机。粉碎机装有两个旋转刀片，每个12″长，两个固定刀片，和0.3″卸料筛。旋转刀片和固定刀片间的间隙为0.10″。
图4中示出了粉碎机输出物的一个样品，其主要由宽约0.1″-0.5″、长约0.25″-1″的碎花纸状片组成。将粉碎机输出物送到Thomas WileyMill Model 2D5旋转切断机内。旋转切断机具有四个旋转刀片、四个固定刀片和2mm的卸料筛。每个刀片大约2″长。设定刀片间隙为0.020″。
旋转切断机剪切碎花纸状片横过刀口，撕开纸片，并以约1磅/小时的速度释放出细微的膨松纤维。纤维具有在5至100之间或更高的平均最小L/D比。膨松纤维的堆密度为约0.1g/cc。图5中示出了正常放大倍数的一个膨松纤维样品，图2中则为50倍放大倍数的膨松纤维样品。
实施例2
按如下方法制备膨松纤维和树脂的复合材料。将标准的混合橡胶/塑料的2辊轧制机加热到325-400。将树脂(通常为丸粒或颗粒形式)加入到加热的轧制机中。约5-10分钟后，树脂结合到辊上(即其熔融和熔化到辊上)。然后向轧制机中加入偶联剂。再过5分钟后，将膨松纤维素材料或木素纤维素材料加入到熔融的树脂/偶联剂混合物中。在约10分钟的时段内加入纤维素纤维或木素纤维素纤维。
然后从轧制机中移出复合材料，切成片并冷却至室温。使用标准压模方法将每批约80g的批料压模成6″×6″×1/8″的薄板。
一种组合物包含以下成分：
1号组合物
成分             量(g)
高密度聚乙烯1    160
旧新闻纸2        240
偶联剂3          8
1Marlex 16007
2使用2mm筛目的旋转切断机膨松化
3FUSABOND100D
将薄板机加工成合适的试样，并根据指定方法中描述的步骤测试。测试三种不同试样的各种性能，计算每次测试的平均值。
1号组合物的性能如下：
抗弯强度(103psi)    9.81(ASTM D790)
抗弯模量(105psi)    6.27(ASTM D790)
第二种组合物包含以下成分：
2号组合物
成分             量(g)
高密度聚乙烯1    160
旧杂志2          240
偶联剂3          8
2号组合物的性能如下：
抗弯强度(103psi)    9.06(ASTM D790)
抗弯模量(105psi)    6.78(ASTM D790)
第三种组合物包含以下成分：
3号组合物
成分             量(g)
HDPE1            160
纤维纸2          216
3.1mm膨松洋麻    24
偶联剂3          8
3号组合物的性能如下：
抗弯强度(103psi)  11.4(ASTM D790)
抗弯模量(105psi)  6.41(ASTM D790)
第四种组合物包含以下成分：
4号组合物
成分                     量(g)
SUPERFLEXCaCO3         33
纤维2，4                 67
HDPE(w/3％增容剂)1，3    100
4新的多涂层牛奶纸盒
4号组合物的性能如下：
抗弯强度(105psi)  8.29(ASTM D790)
极限伸长(％)      ＜5(ASTM D638)
抗弯模量(105psi)  10.1(ASTM D790)
Izod切口(ft-lb/in)1.39(ASTM D256-97)
第五种组合物包含以下成分：
5号组合物
成分                     量(份数)
SUPERFLEXCaCO3         22
纤维2，4                 67
HDPE(w/3％增容剂)1，3    100
5号组合物的性能如下：
抗弯强度(105psi)    8.38(ASTM D790)
极限伸长(％)        ＜5(ASTM D638)
抗弯模量(105psi)    9.86(ASTM D790)
Izod切口(ft-lb/in)  1.37(ASTM D256-97)
第六种组合物包含以下成分：
6号组合物
成分                量(份数)
ULTRAFLEXCaCO3    33
纤维2，4            67
HDPE/增容剂1，3     100
6号组合物的性能如下：
抗弯强度(105psi)    7.43(ASTM D790)
极限伸长(％)        ＜5(ASTM D638)
抗弯模量(105psi)    11.6(ASTM D790)
Izod切口(ft-lb/in)  1.27(ASTM D256-97)
第七种组合物包含以下成分：
7号组合物
成分                    量(pbw)
HDPE(w/3％增容剂)3，5   60
牛皮纸板2               40
5HDPE熔体流动指数       ＜1
7号组合物的性能如下：
抗弯强度(105psi)    7.79(ASTM D790)
极限伸长(％)        ＜5(ASTM D638)
抗弯模量(105psi)    7.19(ASTM D790)
实施例3
在需要极好的耐水性和高温性能的热绝缘应用中使用泡沫环氧树脂。可用根据实施例3的方法制备的膨松纤维增强这类环氧树脂。可任选地使用填充剂如碳酸钙以获得一些成本降低。但是，用填充剂过量装填会削弱泡沫泡孔壁的强度，尤其是当泡沫密度为5磅/立方英尺或更低的范围内时，因为这种低泡沫密度会在泡沫内产生薄的易碎壁。填充剂装填量一般为4-5磅/100重量(phr)树脂。用膨松纤维增强还能提供降低的重量和成本。另外，由于膨松纤维的高的长度/直径(L/D)比，从而能实现提高的强度。使用直到30phr的纤维是合理的。
典型的配方包括：
成分                            份数
DGEBA(双酚A的缩水甘油醚)        100
MPDA(间苯二胺)                  10
Celogen(p，p-氧双苯磺酰肼)    10
(Uniroyal Chemical Company)
表面活性剂                      0.15
氧化苯乙烯                      5
膨松纤维                        30
使用标准环氧树脂混合技术混合该配方。它在120℃的固化温度下产生非常高的放热量，并产生约7磅/立方英尺的泡沫密度。
其它实施方案在权利要求内。

Claims (38)

1.一种制造复合材料的方法，该方法包括(a)剪切纤维素纤维或木素纤维素纤维到其内部纤维充分暴露以形成膨松纤维素纤维或木素纤维素纤维的程度，(b)致密化膨松纤维，和然后(c)使致密化的纤维素纤维或木素纤维素纤维与树脂结合。
2.如权利要求1所述的方法，其中树脂为热塑性树脂。
3.如权利要求1所述的方法，其中树脂选自聚苯乙烯、聚碳酸酯、聚丁烯、热塑性聚酯、聚醚、热塑性聚氨酯、PVC和尼龙。
4.如权利要求1所述的方法，其中树脂选自热固性树脂、弹性体、焦油、沥青和木素。
5.如权利要求1所述的方法，其中树脂选自醇酸树脂、邻苯二甲酸二烯丙酯、环氧树脂、三聚氰胺、酚醛树脂、硅树脂、脲、热固性聚酯、天然橡胶、异戊二烯橡胶、苯乙烯-丁二烯共聚物、氯丁橡胶、丁腈橡胶、丁基橡胶、乙烯丙烯共聚物、三元乙丙共聚物、海帕伦、丙烯酸类橡胶、聚硫橡胶、硅树脂、氨基甲酸乙酯、含氟弹性体、丁二烯或表氯醇橡胶。
6.如权利要求1所述的方法，其中纤维选自黄麻、洋麻、亚麻、大麻、棉、碎布、纸、纸制品和造纸副产品。
7.如权利要求6所述的方法，其中纤维素材料或木素纤维素材料为纸浆板。
8.如权利要求6所述的方法，其中纸选自新闻纸、杂志纸、多涂层纸和漂白的牛皮纸板。
9.如权利要求1所述的方法，其中纤维素材料或木素纤维素材料为合成材料。
10.如权利要求1所述的方法，其中纤维素材料或木素纤维素材料为非织造材料。
11.如权利要求1所述的方法，其中剪切纤维素纤维或木素纤维素纤维的步骤包括在混合机或挤出机内用螺杆剪切。
12.如权利要求1所述的方法，其中复合材料包括约30wt％至约70wt％的树脂和约30wt％至约70wt％的纤维。
13.如权利要求1所述的方法，其中致密化步骤包括将至少一些膨松纤维压缩成丸粒。
14.一种通过权利要求1的方法制造的复合材料。
15.如权利要求14所述的复合材料，其中至少约50％的纤维具有至少约5的长度/直径比。
16.如权利要求14所述的复合材料，其中至少约50％的纤维具有至少约25的长度/直径比。
17.如权利要求14所述的复合材料，其中至少约50％的纤维具有至少约50的长度/直径比。
18.一种组合物，该组合物包括权利要求14的复合材料和化学物质或化学制剂。
19.如权利要求18所述的组合物，其中化学制剂包括增容剂。
20.如权利要求14所述的复合材料，该复合材料还包括无机添加剂。
21.如权利要求20所述的复合材料，其中无机添加剂选自碳酸钙、石墨、石棉、硅灰石、云母、玻璃、纤维玻璃、白垩、滑石、硅石、陶瓷、地面建筑废弃物、轮胎用橡胶粉末、碳纤维和金属纤维。
22.如权利要求20所述的复合材料，其中无机添加剂占复合材料总重量的约0.5％至约20％。
23.如权利要求14所述的复合材料，其中所述复合材料为垫衬形式。
24.如权利要求14所述的复合材料，其中所述复合材料为选自以下制品的形式：面板、管、铺面材料、板、外壳、薄片、棒、带、栅栏、构件、门、百叶窗、遮阳篷、帘、牌子、框架、窗子挡板、底板、墙板、地板、瓷砖、铁路枕木、模板、支架、工具把手、棚、基座、分配器、桶板、薄膜、外衣、大手提包、桶、箱、填料、篮、带、窄条、架、套、结合件、间隔物、墙、室内和室外地毯、垫子、织物，和席子、框架、书架、雕刻品、椅、桌、书桌、艺术品、玩具、比赛用具、锭盘、桥墩、舟、桅杆、污染控制产品、化粪池、汽车面板、基底、计算机外壳、地面上的和地面下的电保护性外套、家具、野餐用桌子、帐篷、运动场、长椅、掩体、体育用品、床、便盆、线、单丝、布、装饰板、支架、衣架、托盘、水池、绝缘体、小箱、图书封面、衣服、棍、拐杖、和其它建筑、农业、材料处理、运输、汽车、工业、环境、海军、电气、电子、娱乐、医疗、织物和消费产品。
25.如权利要求14所述的复合材料，其中所述复合材料为纤维、单丝或薄膜的形式。
26.一种方法，该方法包括：
(a)剪切纤维素纤维或木素纤维素纤维到其内部纤维充分暴露以形成膨松纤维素纤维或木素纤维素纤维的程度，和
(b)在无树脂存在的情况下，致密化膨松的纤维素纤维或木素纤维素纤维。
27.如权利要求26所述的方法，其中致密化步骤包括将至少一些膨松纤维压缩成丸粒。
28.如权利要求26所述的方法，该方法还包括在致密化步骤前使膨松的纤维素纤维或木素纤维素纤维与有助于致密化的物质结合。
29.如权利要求26所述的方法，该方法还包括在致密化步骤后使膨松的纤维素纤维或木素纤维素纤维与树脂结合。
30.如权利要求26所述的方法，该方法还包括在致密化前使膨松的纤维素纤维或木素纤维素纤维与另一种物质结合。
31.如权利要求30所述的方法，其中结合步骤包括用酶或药物的溶液处理膨松的纤维素纤维或木素纤维素纤维。
32.如权利要求30所述的方法，其中结合步骤包括将膨松的纤维素纤维或木素纤维素纤维与固体或酶和/或细菌掺合。
33.一种通过权利要求26的方法制造的复合材料。
34.致密化的膨松纤维素纤维或木素纤维素纤维，其中致密化的膨松纤维素纤维或木质纤维素纤维不包含树脂。
35.如权利要求34所述的致密化纤维，其中该致密化纤维具有10-50磅/立方英尺的容积密度。
36.如权利要求34所述的致密化纤维，其中该致密化纤维具有20-30磅/立方英尺的容积密度。
37.如权利要求34所述的致密化纤维，该致密化纤维为丸粒的形式。
38.如权利要求34所述的致密化纤维，该致密化纤维还包含酶和/或细菌。
CNB03806636XA 2002-03-21 2003-03-13 纤维素和木素纤维素材料与树脂的组合物和复合材料、和制造它们的方法 Expired - Fee Related CN100366663C (zh)

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US20080146702A1 (en) 2008-06-19
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