CN109562953B - 水滑石和纤维的复合体 - Google Patents
水滑石和纤维的复合体 Download PDFInfo
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- CN109562953B CN109562953B CN201780047191.9A CN201780047191A CN109562953B CN 109562953 B CN109562953 B CN 109562953B CN 201780047191 A CN201780047191 A CN 201780047191A CN 109562953 B CN109562953 B CN 109562953B
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- 239000000835 fiber Substances 0.000 title claims abstract description 127
- 239000002131 composite material Substances 0.000 title claims abstract description 121
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 84
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Abstract
本发明的课题是提供一种制造水滑石和纤维的复合体的技术。通过在纤维的存在下在水系中合成水滑石,能够有效率地合成水滑石和纤维的复合体。
Description
技术领域
本发明涉及水滑石和纤维的复合体及其制造方法。
背景技术
一般,水滑石是通式[M2+ 1-xM3+ x(OH)2][An- x/n·mH2O](式中,M2+表示2价的金属离子,M3+表示3价的金属离子,An- x/n表示层间阴离子。另外,0<x<1,n为A的价数,0≤m<1)表示的化合物的之一,是作为催化剂、医药品,树脂用添加剂等利用的物质(专利文献1~3、非专利文献1~3)。
水滑石是与滑石、蒙脱石同样具有层状的晶体结构的金属氢氧化物,水滑石的各个晶体片大多为叶片状或鳞片状。作为水滑石,已知属于水滑石的多型的水镁铝石(manasseite)、氢氧化物片中含有的金属为镁和铁的鳞镁铁矿(pyroaurite)、水镁铁石(sjgrenite)、以及在氢氧化物片中具有2价和3价的铁的绿锈(green rust)等。因为主骨架为双氢氧化物,所以也称为层状双氢氧化物(LDH:Layered Double Hydroxide)等。水滑石虽然也是天然产出的,但产出量少,因此主要使用合成品,已知各种合成方法。
专利文献4中提出了使水滑石等金属氢氧化物担载于聚氨酯纤维等而得的除臭性布帛。另外,非专利文献4中提出了使用水滑石担载纤维从排水中除去磷。
现有技术文献
专利文献
专利文献1:日本特开2015-193000号公报
专利文献2:日本特开2013-085568号公报
专利文献3:日本特开2009-143798号公报
专利文献4:日本特开2012-144829号公报
非专利文献
非专利文献1:“水滑石在水环境保全净化中的应用”,The Chemical Times,no.1,2005
非专利文献2:“Fe-Mg系和Al-Mg系水滑石样化合物的合成和阴离子交换特性”,J.Ion Exchange,vol.16,no.1,2005
非专利文献3:“层状双氢氧化物的表面活性剂吸附特性以及乳化凝胶体的结构稳定性”,东洋大学纪要,自然科学篇,第56号,43~52页,2012
非专利文献4:“水滑石担载纤维(HTCF)从实排水中除磷的性能”,水环境学会志,vol.30,no.11,pp671-676,2007
发明内容
本发明的课题在于提供高效率地制造水滑石和纤维的复合体的技术。
本发明人对上述课题进行了深入研究,结果发现通过在纤维的存在下合成水滑石,水滑石与纤维形成稳定的复合体,从而完成了本发明。
即,本发明包含但不限于以下的发明。
(1)一种水滑石和纤维的复合体的制造方法,包括:在含有纤维的溶液中合成水滑石。
(2)根据(1)所述的方法,其中,包括如下工序:在碱性溶液中浸渍纤维的工序、接着在经浸渍的纤维中添加酸溶液的工序。
(3)根据(1)所述的方法,其中,包括如下工序:在酸溶液中浸渍纤维的工序、接着在经浸渍的纤维中添加碱性溶液的工序。
(4)根据(1)~(3)中任一项所述的方法,其中,进一步包括:在水滑石和纤维的复合体中添加含有阴离子性物质的溶液。
(5)根据(1)~(4)中任一项所述的方法,其中,含有阴离子性物质的溶液为含有铜或者银的硫代硫酸盐配合物溶液。
(6)根据(1)~(5)中任一项所述的方法,其中,上述纤维为化学纤维、再生纤维或者天然纤维。
(7)根据(6)所述的方法,其中,上述纤维为纤维素纤维。
(8)根据(1)~(7)中任一项所述的方法,其中,上述酸溶液的2价的金属离子为镁或锌。
(9)根据(1)~(8)中任一项所述的方法,其中,上述酸溶液的3价的金属离子为铝。
(10)根据(1)~(9)中任一项所述的方法,其中,水滑石和纤维的复合体的灰分中含有10%以上的镁或锌。
(11)一种含有水滑石和纤维而成的复合体。
(12)根据(11)所述的复合体,其中,上述纤维为纤维素纤维。
(13)根据(11)或(12)所述的复合体,其中,纤维表面的15%以上被水滑石被覆。
(14)根据(11)~(13)中任一项所述的复合体,其中,上述水滑石的2价的金属离子为镁或锌。
(15)根据(11)~(14)中任一项所述的复合体,其中,上述水滑石的3价的金属离子为铝。
(16)根据(11)~(15)中任一项所述的复合体,其中,附着有铜或者银。
(17)一种含有(11)~(16)中任一项所述的复合体的产品。
(18)根据(17)所述的产品,其中,上述产品为卫生用品。
(19)根据(17)或(18)所述的产品,其中,上述产品用于除臭。
(20)根据(17)~(19)中任一项所述的产品,其中,上述产品用于抗菌。
(21)根据(17)~(20)中任一项所述的产品,其中,上述产品用于抗病毒。
(22)根据(17)~(21)中任一项所述的产品,其中,上述产品为片材的形态。
根据本发明,能够得到水滑石和纤维的复合体。另外,能够得到产品的成品率高的水滑石和纤维的复合体。此外,能够得到除臭效果高的水滑石和纤维的复合体。
附图说明
图1是用于制造实验1(2)的样品1的装置的示意图(P:泵)。
图2是用于制造实验1(2)的样品5的装置的示意图。
图3是实验1(3)中测定的X射线衍射的结果。
图4-1是实验1(3)中制造的垫片的电子显微镜照片(T1)。
图4-2是实验1(3)中制造的垫片的电子显微镜照片(T2)。
图4-3是实验1(3)中制造的垫片的电子显微镜照片(样品2)。
图4-4是实验1(3)中制造的垫片的电子显微镜照片(T3)。
图4-5是实验1(3)中制造的垫片的电子显微镜照片(内添有水滑石的纸)。
图5是实验2中测定的X射线衍射的结果。
图6是表示实验3的除臭试验的结果的图(甲硫醇,上段:干燥条件,下段:湿润条件))。
图7是表示实验3的除臭试验的结果的图(硫化氢,上段:干燥条件,下段:湿润条件)。
图8是表示实验3的除臭试验的结果的图(吲哚,上段:干燥条件,下段:湿润条件)。
图9是表示实验3的除臭试验的结果的图(氨,上段:干燥条件,下段:湿润条件)
图10是表示实验3的除臭试验的结果的图(乙酸,上段:干燥条件,下段:湿润条件)
图11是表示实验3的除臭试验的结果的图(三甲胺,上段:干燥条件,下段:湿润条件)
图12是表示实验3的除臭试验的结果的图(吡啶,上段:干燥条件,下段:湿润条件)
图13是表示实验3的除臭试验的结果的图(壬烯醛,上段:干燥条件,下段:湿润条件)
具体实施方式
水滑石(HT)和纤维的复合体
一般地,水滑石由[M2+ 1-xM3+ x(OH)2][An- x/n·mH2O](式中,M2+表示2价的金属离子,M3 +表示3价的金属离子,An- x/n表示层间阴离子。另外,0<x<1,n为A的价数,0≤m<1)的通式表示。这里,作为2价的金属离子的M2+,例如可以举出Mg2+、Co2+、Ni2+、Zn2+、Fe2+、Ca2+、Ba2+、Cu2 +、Mn2+等,作为3价的金属离子的M3+,例如可以举出Al3+、Fe3+、Cr3+、Ga3+等,作为层间阴离子的An-,例如可以举出OH-、Cl-、CO3 -、SO4 -等n价的阴离子,x一般为0.2~0.33的范围。其中,作为2价的金属离子,优选Mg2+、Zn2+、Fe2+、Mn2+。晶体结构采用由具有正电荷的正八面体的水镁石(brucite)单元排列成的二维基本层和具有负电荷的中间层构成的层叠结构。
水滑石在发挥其阴离子交换功能的各种用途中的展开,例如,离子交换材料、吸附剂、除臭剂等用途中得到使用。另外,除此之外,利用构成的金属离子的组合,将各构成金属离子处于良好的混合状态的水滑石加热脱水,或者进一步加热煅烧,从而可容易得到均匀的组成的复合氧化物,也可见用于催化剂用途等的例子等。
水滑石在本发明的复合体中所占的比率可以为10%以上,也可以为20%以上,还可以优选为40%以上。水滑石和纤维的复合体的灰分可以根据JIS P 8251:2003进行测定。本发明中,水滑石和纤维的复合体的分灰分可以为10%以上,也可以为20%以上,可以优选为40%以上。另外,本发明的水滑石和纤维的复合体在灰分中优选含有10%以上的镁、铁、锰或者锌,更优选含有40%以上。灰分中的镁或锌的含量可以通过荧光X射线分析进行定量。
本发明涉及水滑石和纤维的复合体,但优选的方式中,纤维表面的15%以上被水滑石被覆。优选的方式中本发明的复合体的水滑石对纤维的被覆率(面积率)为25%以上,更优选为40%以上,但根据本发明也能够制造被覆率为60%以上、80%以上的复合体。另外,从电子显微镜观察的结果可知,本发明的水滑石和纤维的复合体的优选的方式中,水滑石不仅固着在纤维的外表面、管腔的内侧,而且也在微纤维的内侧生成。
利用本发明预先将水滑石和纤维复合体化时,与仅将水滑石与纤维混合的情况相比,能够得到水滑石不仅容易留在产品中、而且不凝聚地均匀分散而得的产品。即,根据本发明,能够使水滑石和纤维的复合体在产品中的成品率(投入的水滑石残留在产品中的重量比例)为65%以上,也能够为70%以上、85%以上。
水滑石和纤维的复合体的合成
本发明中,通过在纤维的存在下在溶液中合成水滑石来制造水滑石和纤维的复合体。
水滑石的合成方法可以利用公知的方法。例如,在反应容器内将纤维浸渍于含有构成中间层的碳酸根离子的碳酸盐水溶液和碱性溶液(氢氧化钠等),接着,添加酸溶液(含有构成基本层的二价金属离子和三价金属离子的金属盐水溶液),控制温度、pH等,通过共沉淀反应合成水滑石。另外,也可以在反应容器内将纤维浸渍于酸溶液(含有构成基本层的二价金属离子和三价金属离子的金属盐水溶液),接着,滴加含有构成中间层的碳酸根离子的碳酸盐水溶液和碱性溶液(氢氧化钠等),控制温度、pH等,通过共沉淀反应合成水滑石。常压下的反应是常见的,但这以外也有利用使用高压釜等的水热反应而得到的方法(日本特开昭60-6619号公报)。
本发明中,作为构成基本层的二价金属离子的供给源,可以使用镁、锌、钡、钙、铁、铜、钴、镍、锰的各种氯化物、硫化物、硝酸化物、硫酸化物。另外,作为构成基本层的三价金属离子的供给源,可以使用铝、铁、铬、镓的各种氯化物、硫化物、硝酸化物、硫酸化物。
本发明中,悬浮液的制备等使用水,作为该水,可以使用通常的自来水、工业用水、地下水、井水等,此外可以适当使用离子交换水、蒸馏水、超纯水、工业废水、制造工序中得到的水。
本发明中,作为层间阴离子,可以使用作为阴离子的碳酸根离子、硝酸根离子、氯化物离子、硫酸根离子、磷酸根离子等。将碳酸根离子作为层间阴离子时,使用碳酸钠作为供给源。但是,碳酸钠可以用含有二氧化碳(二氧化碳气体)的气体代替,也可以实质上是纯二氧化碳气体或与其它气体的混合物。例如,可以适当使用从造纸厂的焚烧炉、煤锅炉、重油锅炉等排出的废气作为含有二氧化碳的气体。此外,也可以使用由石灰煅烧工序产生的二氧化碳来进行碳酸化反应。
制造本发明的复合体时,还可以添加公知的各种助剂。例如,可以将螯合剂添加于中和反应,具体而言,可举出柠檬酸、苹果酸、酒石酸等聚羟基羧酸,草酸等二羧酸,葡萄糖酸等糖酸,亚氨基二乙酸、乙二胺四乙酸等氨基聚羧酸以及它们的碱金属盐,六偏磷酸、三聚磷酸等聚磷酸的碱金属盐,谷氨酸、天冬氨酸等氨基酸以及它们的碱金属盐,乙酰丙酮、乙酰乙酸甲酯、乙酰乙酸烯丙酯等酮类,蔗糖等糖类,山梨糖醇等多元醇。另外,作为表面处理剂,可以添加棕榈酸、硬脂酸等饱和脂肪酸,油酸、亚油酸等不饱和脂肪酸,脂环族羧酸、枞酸等树脂酸、它们的盐或酯和醚,醇系活性剂、脱水山梨糖醇脂肪酸酯类、酰胺系或胺系表面活性剂、聚氧化烯烷基醚类、聚氧乙烯壬基苯基醚、α-烯烃磺酸钠、长链烷基氨基酸、氧化胺、烷基胺、季铵盐、氨基羧酸、膦酸、多元羧酸、缩合磷酸等。另外,根据需要也可以使用分散剂。作为该分散剂,例如有聚丙烯酸钠、蔗糖脂肪酸酯、甘油脂肪酸酯、丙烯酸-马来酸共聚物铵盐、甲基丙烯酸-萘氧基聚乙二醇丙烯酸酯共聚物、甲基丙烯酸-聚乙二醇单甲基丙烯酸酯共聚物铵盐、聚乙二醇单丙烯酸酯等。它们可以单独或者多种组合使用。另外,添加的时机可以在中和反应之前也可以在之后。这样的添加剂相对于水滑石可以优选以0.001~20%,更优选以0.1~10%的量添加。
(反应条件)
本发明中合成反应的温度例如可以为30~100℃,但优选40~80℃,更优选50~70℃,特别优选为60℃左右。如果温度过高或者过低,则有反应效率降低,成本变高的趋势。
另外,本发明中中和反应可以为间歇反应,也可以为连续反应。一般从排出中和反应后的残留物的便利性考虑,优选进行间歇反应工序。反应的规模没有特别限制,可以以100L以下的规模进行反应,也可以按超过100L的规模进行反应。反应容器的大小例如可以为10L~100L左右,也可以为100L~1000L左右。
此外,中和反应可以通过监测反应悬浮液的pH而进行控制,根据反应液的pH曲线,例如可以进行碳酸化反应直到达到小于pH9,优选小于pH8,更优选pH7时。
另一方面,也可以通过监测反应液的电导率来控制中和反应。优选进行碳酸化反应直到电导率降低至100mS/cm以下。
另外,合成反应可以通过反应时间进行控制,具体而言,可以通过调整反应物滞留在反应槽的时间来进行控制。此外,本发明中,也可以通过搅拌反应槽的反应液或使中和反应为多步反应来控制反应。
本发明中,为了以悬浮液的形式得到作为反应产物的复合体,根据需要,可以进行储罐中的储藏或浓缩、脱水、粉碎、分级、熟化、分散等处理。这些可以利用公知的工序,考虑用途、能量效率等而适当地决定即可。例如浓缩·脱水处理使用离心脱水机、沉降浓缩机等进行。作为该离心脱水机的例子,可举出滗析器、螺旋滗析器等。关于使用过滤机、脱水机的情况,对其种类也没有特别限制,可以使用一般的过滤机、脱水机,但优选使用例如压滤机、鼓式过滤器、带式压滤机、管压机等加压型脱水机、奥利弗过滤器等真空鼓脱水机等来制成碳酸钙饼块。作为粉碎的方法,可举出球磨机、砂磨机、冲击磨机、高压均化器、低压均化器、Dyno磨机、超声波磨机、神田磨床、磨碎机、石磨机、振动磨机、切碎机、喷射磨机、粉碎机、打浆机,短轴挤出机、双螺杆挤出机、超声波搅拌器、家用榨汁机搅拌机等。作为分级的方法,可举出筛网等筛、向外型或向内型狭缝或圆孔筛、振动筛、重质异物清洁剂、轻质异物清洁剂、反向清洁剂、筛分试验机等。作为分散的方法,可举出高速分散机,低速捏合机等。
由本发明得到的复合体也可以不完全脱水而以悬浮液的状态配合在填料、颜料中,但也可以干燥而制成粉体。对于这时的干燥机也没有特别限制,例如,可以适当使用空气干燥器、带式干燥器、喷雾干燥器等。
由发明得到的复合体可以通过用稀盐酸、稀硝酸等弱酸处理,嵌入氯化物离子、硝酸物离子等作为层间离子。作为嵌入的化合物,可举出阴离子性物质,例如,可举出铜或银的硫代硫酸盐配合物等。作为嵌入的方法,可以利用公知的方法,但可以在水滑石和纤维的复合体中添加含有阴离子性物质的溶液并混合。
另外,由本发明得到的复合体可以利用公知的方法改性。例如,在某方式中,能够将其表面疏水化而提高与树脂等的混和性能。
纤维
本发明中,将水滑石和纤维复合体化。构成复合体的纤维没有特别限制,例如当然可以使用纤维素等天然纤维,还可以无限制地使用由石油等的原料人工合成的合成纤维,以及人造丝、莱赛尔等再生纤维(半合成纤维),以及以陶瓷为代表的无机纤维等。作为天然纤维,除了上述之外,还可以举出羊毛、绢丝、胶原纤维等蛋白质纤维,甲壳质/壳聚糖纤维、海藻酸纤维等复合糖链系纤维等。
作为纤维素系的原料,可例示纸浆纤维(木材纸浆或非木材纸浆)、细菌纤维素,木材纸浆通过将木材原料制浆来制造即可。作为木材原料,可例示赤松、黑松、冷杉、云杉、红松、落叶松、日本冷杉、铁杉、日本柳杉、日本扁柏、落叶松、白叶冷杉、鱼鳞云杉、柏树、道格拉斯冷杉、加拿大铁杉、白冷杉、云杉、香脂冷杉、雪松、松树、南洋松、辐射松等针叶树,以及它们的混合材,日本山毛榉、桦木、日本桤木、橡树、红楠、栗树、白桦、黑杨、杨树、水曲柳、甜杨、桉树、红树、柳桉、金合欢等阔叶树以及它们的混合材。
将木材原料制浆的方法没有特别限定,可例示在造纸工业中常用的制浆方法。木材纸浆可以根据制浆方法分类,例如,可举出利用牛皮纸法、亚硫酸盐法、烧碱法、多硫化物法等方法蒸煮而得的化学纸浆;通过精磨机、磨床的机械力制浆而获得的机械纸浆;用化学品预处理后,通过机械力制浆而得到的半化学纸浆;废纸纸浆;脱墨纸浆等。木材纸浆可以是未漂白(漂白前)的状态,也可以是漂白(漂白后)的状态。
作为来自非木材的原料,可例示棉、麻、剑麻、马尼拉麻、亚麻、稻草、竹、甘蔗渣、洋麻、甘蔗、玉米、稻梗、小构树(葡蟠)、黄瑞香等。
纸浆纤维可以是未打浆或打浆中的任一种,根据复合体片的物性进行选择即可,但优选进行打浆。由此,可以期待促进片材强度的提高和碳酸钙的固定。
作为合成纤维,可举出聚酯、聚酰胺、聚烯烃、丙烯酸、尼龙、丙烯酸、维纶、陶瓷纤维等,作为半合成纤维,可举出人造丝、醋酸盐等,作为无机纤维,可举出玻璃纤维、碳纤维、各种金属纤维等。
另外,这些纤维素原料也可以通过进一步实施处理而作为粉末纤维素、氧化纤维素等化学改性纤维素,以及纤维素纳米纤维:CNF(微纤维化纤维素:MFC、TEMPO氧化CNF、磷酸酯化CNF、羧甲基化CNF、机械粉碎CNF等)使用。作为本发明中使用的粉末纤维素,例如,可以使用将精选纸浆进行酸水解后得到的未分解残渣进行精制、干燥、粉碎·筛分之类的方法而制造的棒轴状的具有一定的粒径分布的结晶性纤维素粉末,也可以使用KC Flock(日本制纸制)、Ceolus(Asahi Kasei Chemicals Corporation制)、Avicel(FMC公司制)等的市售品。粉末纤维素中的纤维素的聚合度优选为100~1500左右,基于X射线衍射法的粉末纤维素的结晶度优选为70~90%,基于激光衍射式粒度分布测定装置的体积平均粒径优选为1μm~100μm。本发明中使用的氧化纤维素例如可以通过在选自N-氧自由基化合物和溴化物、碘化物或它们的混合物中的化合物的存在下使用氧化剂在水中进行氧化而得到。作为纤维素纳米纤维,使用对上述纤维素原料进行解纤的方法。作为解纤方法,例如可以使用如下方法:通过对纤维素、氧化纤维素等化学改性纤维素的水悬浮液等利用精磨机、高压均质机、磨床、单轴或多轴混炼机、珠磨机等进行机械磨碎乃至打浆而解纤。也可以将上述方法1种或多种组合来制造纤维素纳米纤维。已制造的纤维素纳米纤维的纤维直径可以通过电子显微镜观察等进行确认,例如为5nm~1000nm、优选5nm~500nm、更优选5nm~300nm的范围。制造该纤维素纳米纤维时,在对纤维素进行解纤和/或微细化之前和/或之后,也可以进一步添加任意的化合物并使其与纤维素纳米纤维反应,制成羟基被修饰的纤维素。作为修饰的官能团,可举出乙酰基、酯基、醚基、酮基、甲酰基、苯甲酰基、缩醛、半缩醛、肟、异腈、丙二烯、硫醇基、脲基、氰基、硝基、偶氮基、芳基、芳烷基、氨基、酰胺基、酰亚胺基、丙烯酰基、甲基丙烯酰基、丙酰基、丙炔酰基、丁酰基、2-丁酰基、戊酰基、己酰基、庚酰基、辛酰基、壬酰基、癸酰基、十一酰基、十二酰基、肉豆蔻酰基、棕榈酰基、硬脂酰基、新戊酰基、苯甲酰基、萘甲酰基、烟酰基、异烟酰基、糠酰基、肉桂酰基等酰基、2-甲基丙烯酰氧乙基异氰酰基等异氰酸酯基、甲基、乙基、丙基、2-丙基、丁基、2-丁基、叔丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基、肉豆蔻基、棕榈基、硬脂基等烷基、环氧乙烷基、氧杂环丁烷基、氧基、硫杂环丙烷基、硫杂环丁烷基等。这些取代基中的氢可以被羟基、羧基等官能团所取代。另外,烷基中的一部分可以成为不饱和键。作为用于导入这些官能团的化合物,没有特别限定,例如可举出具有来自磷酸的基团的化合物、具有来自羧酸的基团的化合物、具有来自硫酸的基团的化合物、具有来自磺酸的基团的化合物、具有烷基的化合物、具有来自胺的基团的化合物等。作为具有磷酸基的化合物,没有特别限定,可举出磷酸、属于磷酸的锂盐的磷酸二氢锂、磷酸氢二锂、磷酸三锂、焦磷酸锂、聚磷酸锂。还可举出属于磷酸的钠盐的磷酸二氢钠、磷酸氢二钠、磷酸三钠、焦磷酸钠、聚磷酸钠。还可举出属于磷酸的钾盐的磷酸二氢钾、磷酸氢二钾、磷酸三钾、焦磷酸钾、聚磷酸钾。还可举出属于磷酸的铵盐的磷酸二氢铵、磷酸氢二铵、磷酸三铵、焦磷酸铵、聚磷酸铵等。其中,从导入磷酸基的效率高、易于工业应用的观点考虑,优选磷酸、磷酸的钠盐、磷酸的钾盐、磷酸的铵盐,更优选磷酸二氢钠、磷酸氢二钠,但没有特别限定。作为具有羧基的化合物,没有特别限定,可举出马来酸、琥珀酸、邻苯二甲酸、富马酸、戊二酸、己二酸、衣康酸等二羧酸化合物、或柠檬酸、乌头酸等三羧酸化合物。作为具有羧基的化合物的酸酐,没有特别限定,可举出马来酸酐、琥珀酸酐、邻苯二甲酸酐、戊二酸酐、己二酸酐、衣康酸酐等二羧酸化合物的酸酐。作为具有羧基的化合物的衍生物,没有特别限定,可举出具有羧基的化合物的酸酐的酰亚胺化物、具有羧基的化合物的酸酐的衍生物。作为具有羧基的化合物的酸酐的酰亚胺化物,没有特别限定,可举出马来酰亚胺、琥珀酰亚胺、邻苯二甲酰亚胺等二羧酸化合物的酰亚胺化物。作为具有羧基的化合物的酸酐的衍生物,没有特别限定。例如,可举出二甲基马来酸酐、二乙基马来酸酐、二苯基马来酸酐等具有羧基的化合物的酸酐中的至少一部分氢原子被取代基(例如,烷基、苯基等)取代而得的化合物。在上述具有来自羧酸的基团的化合物中,从易于工业应用、容易气化的方面考虑,优选马来酸酐、琥珀酸酐、邻苯二甲酸酐,但没有特别限定。另外,即使不进行化学键合,也可以以修饰的化合物物理吸附于纤维素纳米纤维的形式修饰纤维素纳米纤维。作为物理吸附的化合物,可举出表面活性剂等,可以使用阴离子性、阳离子性、非离子性中的任一种。在对纤维素进行解纤和/或粉碎之前进行上述修饰时,也可以在解纤和/或粉碎后使这些官能团脱离而恢复成原来的羟基。通过施加如上的修饰,能够促进纤维素纳米纤维的解纤,或者在使用纤维素纳米纤维时容易与各种物质混合。
以上示出的纤维可以单独使用,也可以混合多种使用。其中,优选含有木材纸浆、或含有木材纸浆与非木材纸浆和/或合成纤维的组合,更优选仅为木材纸浆。
在优选的方式中,构成本发明的复合体的纤维为纸浆纤维。另外,例如,可以将从造纸厂的排水中回收的纤维状物质在本发明中使用。通过将这样的物质供给到反应槽中,能够合成各种复合粒子,另外,在形状上也能够合成纤维状粒子等。
复合体的成形物
也可以使用本发明的复合体而适当地制造成型物(体)。例如,将由本发明得到的复合体片材化时能够容易地得到高灰分的片材。作为在片材制造中使用的抄纸机(抄造机),例如可举出长网抄纸机、圆网抄纸机、夹网成型器、混合成型器、多层抄纸机、组合有这些机器的抄纸方式的公知的抄造机等。抄纸机中的加压线压、在后段进行压光处理时的压光线压都可以在不妨碍作业性、复合体片材的性能的范围内决定。另外,也可以利用含浸、涂布对所形成的片材赋予淀粉、各种聚合物、颜料和它们的混合物。
在片材化时可以添加湿润和/或干燥纸力剂(纸力增强剂)。由此,能够提高复合体片材的强度。作为纸力剂,例如,可举出脲醛树脂、三聚氰胺甲醛树脂、聚酰胺、聚胺、表氯醇树脂、植物性橡胶、胶乳、聚乙烯亚胺、乙二醛、树胶、甘露半乳聚糖聚乙烯亚胺、聚丙烯酰胺树脂、聚乙烯胺、聚乙烯醇等树脂;由选自上述树脂中的2种以上构成的复合聚合物或共聚聚合物;淀粉和加工淀粉;羧甲基纤维素、瓜尔胶、脲树脂等。纸力剂的添加量没有特别限定。
另外,为了促进填料固定于纤维,或提高填料、纤维的留着率,也可以添加高分子聚合物、无机物。例如作为凝聚剂,可以使用聚乙烯亚胺和含有叔铵基和/或季铵基的改性聚乙烯亚胺、聚亚烷基亚胺、二氰基二酰胺聚合物、聚胺、聚胺/表氯醇聚合物、以及二烷基二烯丙基季铵单体、二烷基氨基烷基丙烯酸酯、二烷基氨基烷基甲基丙烯酸酯、二烷基氨基烷基丙烯酰胺和二烷基氨基烷基甲基丙烯酰胺与丙烯酰胺的聚合物、由单胺类和表卤醇构成的聚合物、聚乙烯胺和具有乙烯基胺部的聚合物、它们的混合物等阳离子性的聚合物,除此以外,也可以使用在上述聚合物的分子内共聚有羧基、砜基等阴离子基团的富阳离子的两离子性聚合物、阳离子性聚合物和阴离子性或两离子性聚合物的混合物等。另外,作为助留剂,可以使用阳离子性或阴离子性、两性聚丙烯酰胺系物质。另外,除此以外,也可以应用并用至少一种以上的阳离子、阴离子性的聚合物的、所谓的被称为双聚合物的留着系统,还可以是多成分留着系统,该多成分留着系统并用至少一种以上的阴离子性的膨润土、胶体二氧化硅、聚硅酸、聚硅酸或聚硅酸盐微凝胶和它们的铝改性物等无机微粒、一种以上的丙烯酰胺进行交联聚合而成的所谓的被称为微聚合物的微粒100μm以下的有机系的微粒。特别是单独或组合使用的聚丙烯酰胺系物质在利用极限粘度法测得的重均分子量为200万道尔顿以上时,能够得到良好的留着率,在优选为500万道尔顿以上、进一步优选为1000万道尔顿以上且小于3000万道尔顿的上述丙烯酰胺系物质的情况下,能够得到非常高的留着率。该聚丙烯酰胺系物质的形态可以为乳液型,也可以为溶液型。作为其具体的组成,只要是在该物质中含有丙烯酰胺单体单元作为结构单元的组成,就没有特别限定,例如,可举出丙烯酸酯的季铵盐与丙烯酰胺的共聚物、或者使丙烯酰胺与丙烯酸酯共聚后,进行季铵化而得的铵盐。该阳离子性聚丙烯酰胺系物质的阳离子电荷密度没有特别限定。
此外,根据目的,可举出滤水性提高剂、内添施胶剂、pH调节剂、消泡剂、间距控制剂、粘泥控制剂、蓬松剂、碳酸钙、高岭土、滑石、二氧化硅等无机粒子(所谓的填料)等。各添加材料的使用量没有特别限定。
也可以使用除片材化以外的成型法,例如,通过像称为纸浆模塑那样向铸模中流入原料并使其吸引脱水·干燥的方法、或者在树脂、金属等成型物的表面涂开并干燥后从基材上剥离的方法等,可以得到具有各种形状的成型物。另外,也可以混合树脂而成型为塑料样,还可以添加二氧化硅、氧化铝等矿物,进行煅烧从而成型为陶瓷样。在以上示出的配合·干燥·成型中,可以仅使用1种复合体,也可以混合使用2种以上的复合体。使用2种以上的复合体时,可以使用预先将它们混合而得的物质,也可以将各自配合·干燥·成型而得的物质随后混合。
使用本发明的复合体而制造成型物(体)时,也可以赋予聚合物等各种有机物、颜料等各种无机物、纸浆纤维等各种纤维。另外,也可以在形成复合体的成型物后赋予聚合物等各种有机物、颜料等各种无机物、纸浆纤维等各种纤维。
由本发明得到的复合体可以用于各种用途,例如可以广泛用于纸、纤维、纤维素系复合材料、过滤器材料、涂料、塑料或其它树脂、橡胶、弹性体、陶瓷、玻璃、轮胎、建筑材料(沥青、石棉、水泥、板材、混凝土、砖、瓷砖、胶合板、纤维板等)、各种载体(催化剂载体、医药载体、农药载体、微生物载体等)、吸附剂(除去杂质、除臭、除湿等)、抗皱剂、粘土、研磨材料、改性剂、修补材料、绝热材料、防湿材料、防水材料、耐水材料、遮光材料、密封剂、屏蔽材料、防虫剂、粘接剂、油墨、化妆料、医用材料、糊料材料、食品添加剂、片剂赋形剂、分散剂、保形剂、保水剂、助滤材料、精油材料、油处理剂、油改性剂、电磁波吸收材料、绝缘材料、隔音材料、防振材料、半导体密封材料、放射线屏蔽材料、化妆品、肥料、饲料、香料、涂料·粘接剂·树脂用添加剂、防变色剂、导电材料、导热材料、卫生用品(一次性尿布、卫生巾、失禁者用衬垫、母乳衬垫等)等所有用途。另外,可以用于上述用途中的各种填充剂、涂敷剂等。其中,优选吸附剂(除去杂质、除臭、除湿等)、卫生用品(一次性尿布、卫生巾、失禁者用衬垫、母乳衬垫等)。
本发明的复合体可以应用于造纸用途,例如可举出印刷用纸、报纸、喷墨用纸、PPC用纸、牛皮纸、高级纸、铜版纸、微涂布纸、包装纸、薄页纸、彩色高级纸、铸涂纸、无碳纸、标签用纸、热敏纸、各种花式纸、水溶纸、剥离纸、工艺纸、壁纸用原纸、不燃纸、阻燃纸、层压板原纸、印刷电子用纸、电池用隔膜、缓冲纸、描图纸、含浸纸、ODP用纸、建材用纸、化妆材料用纸、信封用纸、胶带用纸、热交换用纸、化纤纸、灭菌纸、耐水纸、耐油纸、耐热纸、光催化纸、化妆纸(吸油纸等)、各种卫生纸(手纸、面巾纸、擦拭纸、尿布、生理用品等)、烟草用纸、板纸(裱面纸、中芯原纸、白板纸等)、纸盘原纸、杯原纸、烘焙用纸、砂纸、合成纸等。
实施例
以下举出实施例对于本发明进行具体的说明,但本发明不限定于所述实施例。另外,只要在本说明书中没有特别记载,则浓度、份等为重量基准,数值范围以包含其端点的形式进行记载。
实验1:水滑石与纤维的复合体
(1)碱性溶液与酸溶液的制备
准备用于合成水滑石(HT)的溶液。作为碱性溶液(A溶液),准备Na2CO3(和光纯药)和NaOH(和光纯药)的混合水溶液。另外,作为酸溶液(B溶液),制备MgCl2(和光纯药)和AlCl3(和光纯药)的混合水溶液、ZnCl2(和光纯药)和AlCl3(和光纯药)的混合水溶液。
·碱性溶液(A溶液,Na2CO3浓度:0.05M,NaOH浓度:0.8M)
·酸溶液(B溶液,Mg系,MgCl2浓度:0.3M,AlCl3浓度:0.1M)
·酸溶液(B溶液,Zn系,ZnCl2浓度:0.3M,AlCl3浓度:0.1M)
(2)复合体的合成
(样品0:Mg6Al2(OH)16CO3·4H2O)
将碱性溶液装入10L容量的反应容器中,边搅拌边滴加酸溶液(Mg系)而合成水滑石微粒。反应温度为60℃,滴加速度为15ml/min,在反应液的pH约为7的阶段停止滴加。滴加结束后,将反应液搅拌30分钟,使用约10倍量的水进行水洗而除去盐。
(样品1:Mg6Al2(OH)16CO3·4H2O和纸浆纤维的复合体)
作为进行复合体化的纤维,使用纤维素纤维。具体而言,使用以8:2的重量比包含阔叶树漂白牛皮纸浆(LBKP,日本制纸制)和针叶树漂白牛皮纸浆(NBKP,日本制纸制)并使用单盘式精磨机(SDR)将加拿大标准游离度调整为390ml而得的纸浆纤维。
向碱性溶液中添加纸浆纤维,准备含有纸浆纤维的水性悬浮液(纸浆纤维浓度:1.56%,pH:约12.4)。将该水性悬浮液(纸浆固体成分30g)装入到10L容量的反应容器中,一边搅拌水性悬浮液,一边滴加酸溶液(Mg系)而合成水滑石微粒与纤维的复合体。使用如图1所示的装置,反应温度为60℃,滴加速度为15ml/min,在反应液的pH约为7的阶段停止滴加。滴加结束后,将反应液搅拌30分钟,使用10倍量的水进行水洗而除去盐。
(样品2:Mg6Al2(OH)16CO3·4H2O与纸浆纤维的复合体)
使碱性溶液和酸溶液(Mg系)的添加顺序相反,除此以外,与样品1同样地制造复合体。滴加前的水性悬浮液的pH约为2.8,在反应液的pH约为7的阶段停止滴加碱性溶液。
(样品3:Zn6Al2(OH)16CO3·4H2O与纸浆纤维的复合体)
使用Zn系溶液作为酸溶液(B溶液),除此以外,与样品1同样地制成复合体。滴加前的水性悬浮液的pH约为12.3,在反应液的pH约为6.5的阶段停止滴加酸溶液(Zn系)。
(样品4:碳酸钙与纸浆纤维的复合体)
与日本特开2015-199655的实验1同样地制造碳酸钙与纸浆纤维的复合体。即,在阔叶树纸浆纤维(CV处理纸浆)的存在下在水系中合成碳酸钙,制造碳酸钙与纸浆纤维的复合体。
(样品5:碳酸镁与纸浆纤维的复合体)
将包含氢氧化镁140g(和光纯药)和阔叶树漂白牛皮纸浆140g(LBKP,CSF:370ml,平均纤维长:0.75mm)的水性悬浮液14L装入到45L容量的空化装置中,一边使反应溶液循环,一边向反应容器中吹入二氧化碳,利用二氧化碳法来合成碳酸镁微粒与纤维的复合体。反应温度约为36℃,二氧化碳以市售的液化气体为供给源,二氧化碳的吹入量为4L/min。在反应液的pH约为8的阶段停止导入CO2(反应前的pH约为9.5),其后30分钟,继续进行空化的产生和装置内的浆料的循环,得到碳酸镁与纸浆纤维的复合体。
在复合体的合成中,如图2所示地使反应溶液循环而向反应容器内喷射,从而使反应容器内产生空化气泡。具体而言,介由喷嘴(喷嘴直径:1.5mm)在高压下喷射反应溶液而产生空化气泡。喷流速度约为70m/s,入口压力(上游压力)为1.8MPa,出口压力(下游压力)为0.3MPa。
(3)复合体的评价
根据JIS P 8222,由合成的复合体制造垫片(克重:约100g/m2)。具体而言,使用滤纸(JIS P3801,定量分析用,5种B)对复合体的水性浆料(约0.5%)进行过滤,对得到的样品以1MPa施加5分钟压力而进行脱水后,以50℃进行2小时拉紧干燥,制造约200cm2的大小的复合体垫片。作为对照,还制造仅由纸浆构成的垫片(T1)、内添有水滑石的垫片(内添有水滑石的纸)。仅由纸浆构成的垫片是由LBKP/NBKP混合纸浆(CSF:390ml)的水性浆料(约0.5%)基于JIS P 8222制造而得的,内添有水滑石的纸是由在LBKP/NBKP混合纸浆(CSF:390ml)的水性浆料(约0.5%)中添加有水滑石(样品0)的悬浮液基于JIS P 8222制造而得的。
另外,利用X射线衍射对样品1(Mg系HT)和样品3(Zn系HT)进行分析,确认来自于水滑石的峰(图3,●标记)。
此外,使用电子显微镜(SEM)对得到的复合体进行观察,确认在纸浆纤维表面复合有粒子的情况(图4)。图4-1是仅由在样品1的制备中使用的牛皮纸浆制造的垫片的电子显微镜照片,在纤维表面看不到粒子。图4-2是由样品1的复合体制造的垫片的电子显微镜照片,但该复合体在纤维表面析出了许多的Mg系HT微粒。样品1的复合体(图4-2)的微粒对纸浆纤维的被覆率约为95%(微粒的一次粒径:40~60nm左右,平均一次粒径:50nm左右),样品2的复合体(图4-3)的微粒对纸浆纤维的被覆率约为75%。图4-4是由样品3的复合体制造的垫片的电子显微镜照片,在纤维表面析出了许多的Zn系HT微粒(微粒对纸浆纤维的被覆率为50~80%,微粒的一次粒径:100~900nm,平均一次粒径:400nm左右)。图4-5是对样品0和牛皮纸浆进行混抄而得的垫片的电子显微镜照片。在纤维表面看到了粒子,但微粒对纸浆纤维的被覆率为40~60%,与样品1的复合体相比,是低值。
另外,对样品1的复合体(Mg系HT与纤维的复合体)的灰分进行测定,结果为49.5重量%,与由原料(纸浆·氢氧化钙)的投料比算出的理论值(50重量%)几乎一致。样品3的复合体(Zn系HT与纤维的复合体)的灰分为49.8重量%,与由原料(纸浆·氢氧化钙)的投料比算出的理论值(50重量%)几乎一致。应予说明,复合体的灰分是根据将复合体在525℃加热约2小时后残留的灰的重量与原本的固体成分的比率而算出的(JISP 8251:2003)。但是,通过525℃下的灰化处理会因水滑石的脱碳酸、层间水的脱离而产生重量减少(Mg系HT:约40%,Zn系HT:约30%),因此由灰化处理后的实测重量根据重量减少份而算出灰分。另外,关于Mg与Zn的比率,基于水滑石的组成进行计算。
[表1]
表1.复合体垫片
实验2:复合体片材的制造和评价
(1)复合体片材的制造
(片材0)
根据JIS P 8222,由牛皮纸浆制造克重为60g/m2左右的手抄片材。使用的纸浆与实验1中记载的纸浆相同,是以8∶2的重量比包含阔叶树漂白牛皮纸浆(LBKP,日本制纸制)和针叶树漂白牛皮纸浆(NBKP,日本制纸制)并使用单盘式精磨机(SDR)将加拿大标准游离度调整为390ml而得的纸浆。
(片材1·2)
基于JIS P 8222,由实验1中制造的复合体(样品1·2)制造片材。具体而言,在复合体的水性浆料(约0.5%)中添加阳离子性助留剂(ND300,HYMO公司制)100ppm、阴离子性助留剂(FA230,HYMO公司制)100ppm,以500rpm进行搅拌而制备悬浮液后,根据JIS P 8222由所制备的悬浮液制造片材。
(片材3)
基于JIS P 8222,由实验1中记载的牛皮纸浆(CSF:390ml)和水滑石微粒(样品0)制造片材。具体而言,在LBKP/NBKP混合纸浆的水性浆料(约0.5%)中添加实验1中制造的水滑石,添加阳离子性助留剂(ND300,HYMO公司制)100ppm、阴离子性助留剂(FA230,HYMO公司制)100ppm,以500rpm进行搅拌而制备悬浮液后,根据JIS P 8222由所制备的悬浮液制造片材。
(片材4·5)
不使用阳离子性助留剂和阴离子性助留剂,除此以外,与片材1·2同样地制造复合体片材。
(片材6)
不使用阳离子性助留剂和阴离子性助留剂,除此以外,与片材3同样地制造复合体片材。此时的成品率为62.1%。
(2)复合体片材的评价
分别按照下述的评价顺序进行评价。
·克重:JIS P 8124:1998
·厚度:JIS P 8118:1998
·密度:根据厚度、克重的测定值进行计算
·灰分:JIS P 8251:2003
·白色度:JIS P 8212:1998
·不透明度:JIS P 8149:2000
·比散射系数(S值):根据TAPPIT425(ISO 9416)中规定的公式进行计算。
·透气阻力度:JIS P 8117:2009
·平滑度:JIS P 8155:2010
·弯曲负荷:根据ISO 2493利用L&W Bending Tester(Lorentzen&Wettre公司制)测定弯曲角度为15度的弯曲挺度而进行计算。
·裂断长度:JIS P 8113:2006
·X射线衍射:与实验1同样地分析片材样品(图5)。
·成品率:由片材制作时的投入量和所制造出的片材重量进行计算。
[表2]
根据上述的表可知:在纤维和碱的悬浮液中添加酸而合成的水滑石复合体与在纤维和酸的悬浮液中添加碱而合成的水滑石复合体相比,白色度和不透明度高,纤维的被覆率、灰分高。另一方面,在纤维和酸的悬浮液中添加碱而合成的水滑石复合体与在纤维和碱的悬浮液中添加酸而合成的水滑石复合体相比,片材的拉伸强度高。
实验3:除臭特性的评价
使用实验1(3)中制造的复合体垫片(克重:约100g/m2)来评价复合体的除臭特性。供于除臭试验的复合体垫片的大小为100cm2(10cm×10cm),但对于后述的湿润条件下的硫化氢、甲硫醇、吲哚,使样品的大小为25cm2。
除臭试验根据SEK标识纤维产品认证标准(JEC301,纤维评价技术协会)的方法而实施,评价对汗臭(氨、乙酸、异戊酸),排泄臭(氨、乙酸、硫化氢、甲硫醇、吲哚),老人臭(氨、乙酸、异戊酸、壬烯醛),生活垃圾臭(氨、硫化氢、甲硫醇、三甲胺)的除臭特性。氨、乙酸、硫化氢、甲硫醇、吡啶、三甲胺使用检测管进行定量,异戊酸和吲哚、壬烯醛使用气相色谱法进行定量。
(条件1:干燥条件)
以20℃、65%RH对样品进行24小时以上的湿度调节后,评价臭气成分的除臭特性(减少率,%)。这里,减少率(%)可以根据臭气成分的初期浓度和测定时的浓度由下式而求出。
减少率(%)=(1-测定时的浓度/初期浓度)×100
如下表和图6~13所示,在实施了除臭试验的样品中,T3的垫片(Zn系HT复合体)对作为对象的所有臭气成分表现出较高的除臭能力。
[表3]
表3.干燥条件下的除臭评价(臭气成分的减少率)
(条件2:湿润条件)
用移液管对以20℃、65%RH进行了24小时以上的湿度调节的样品赋予约1ml的水后,评价臭气成分的除臭特性。用于对纸尿布等水分多的环境下的除臭特性进行评价。
如下表和图6~13所示,关于相当于汗臭的臭气成分中的氨,湿润条件下除臭效果较高。认为是由于氨易溶于水,臭气变得容易吸附的影响。
[表4]
表4.湿润条件下的除臭评价(臭气成分的减少率)
实验4:抗菌特性的评价
根据JIS P 8222,由实验1(2)中制造的复合体(样品3)制造垫片(克重:约100g/m2,灰分:46%)。具体而言,将包含湿润纸力增强剂(产品名:WS4024,星光PMC公司制)5000ppm、阴离子助留剂(产品名:FA230,HYMO公司制)1200pm、阳离子助留剂(产品名:ND300,HYMO公司制)1000ppm的复合体的水性浆料(浓度:约0.5%)用滤纸(JIS P3801,定量分析用,5种B)进行过滤,将得到的样品以1MPa施加5分钟压力而进行脱水后,以50℃进行2小时拉紧干燥,制造复合体垫片。这里,复合体的灰分根据将复合体以525℃加热约2小时后残留的灰的重量与原本的固体成分的比率而算出(JIS P8251:2003)。
使用所制造的复合体垫片来评价抗菌特性。供于抗菌试验的复合体垫片的重量为0.4g。作为基准,使用标准棉布。抗菌性试验根据JISL1902中规定的菌液吸收法(将试验接种菌液直接接种在试验片上的定量试验方法)进行实施。作为试验菌种,使用金黄色葡萄球菌(Staphylococcus aureus NBRC 12732)和大肠杆菌(Escherichia coil NBRC 3301)这两种,利用稀释混合平板培养法测定培养18小时后的活菌数。以下示出试验顺序。
1.将试验片0.4g放入药瓶中,滴加试验菌液0.2ml(含有0.05%的表面活性剂(Tween80))后,将药瓶盖好盖。
2.将药瓶在37℃下培养18小时。
3.加入洗出液20ml,从试验片中洗出试验菌,利用稀释混合平板培养法或发光测定法测定洗出液中的活菌数。
4.按照下述的公式算出抗菌活性值。抗菌活性值为2.0以上是指菌的死亡率为99%以上。
抗菌活性值={log(对照试样·培养后活菌数)-log(对照试样·刚接种后活菌数)}-{log(试验试样·培养后活菌数)-log(试验试样·刚接种后活菌数)}
如下表所示,实施了抗菌性试验的Zn系HT复合体对作为对象的菌种表现出极高的抗菌性能。
[表5]
表5.抗菌活性值
样品 | Zn系HT复合体 |
金黄色葡萄球菌 | 6.0 |
大肠杆菌 | 6.2 |
应予说明,如下表所示,使用标准棉布进行抗菌性试验,结果增殖值为1.0以上,由此确认正确地进行了试验。
[表6]
表6.各试验菌种的增殖值
样品 | 标准棉布 |
金黄色葡萄球菌 | 2.9 |
大肠杆菌 | 3.1 |
实验5:抗病毒性的评价
用铜的硫代硫酸盐配合物溶液对实验1(2)中制造的合成复合体(样品3)进行处理,得到附着有铜的硫代硫酸盐配合物溶液的Zn系HT复合体(Zn6Al2(OH)16CO3·4H2O与纸浆纤维的复合体)(样品6)。
具体而言,溶解氯化铜,将该溶液和硫代硫酸钠五水合物的溶液混合,制备铜的硫代硫酸盐配合物溶液。对实验1(2)中制造的复合体(样品3)的浆料(浓度1.5%)以铜相对于固体成分为0.8~2.0%的方式添加该铜的硫代硫酸盐配合物溶液,以20℃~60℃的条件搅拌3小时(样品6-1~6-3)。
接下来,根据JIS P 8222,由所制造的复合体(样品6-1~6-3)制造垫片(克重:约100g/m2,灰分:46%)。具体而言,将复合体的水性浆料(浓度:约0.5%)用滤纸(JIS P3801,定量分析用,5种B)过滤,将得到的样品以1MPa施加5分钟压力而进行脱水后,以50℃进行2小时拉紧干燥,制造复合体垫片。
对所制造的复合体垫片评价抗病毒性能。抗病毒性试验根据JIS L 1922:2016纤维产品的抗病毒性试验方法进行实施。供于试验的复合体垫片的重量为0.4g,对照试样使用标准棉布。作为试验病毒种类,使用猫杯状病毒(Feline calicivirus;Strain:F-9ATCCVR-782)。以下示出试验顺序。
1.将试验片0.4g装入到药瓶中,滴加试验病毒液0.2ml后,将药瓶盖好盖。
2.将药瓶在25℃下静置2小时。
3.加入洗出液20ml,从试验片中洗出病毒,通过噬菌斑测量法而算出感染性滴度。
4.由下式算出抗病毒活性值(Mv)。应予说明,在JIS中,在Mv≥2.0时将抗病毒效果规定为有效果,在Mv≥3.0时规定为充分具有效果。
抗病毒活性值(Mv)=Log(Vb)-Log(Vc)
Mv:抗病毒活性值
Log(Vb):对照试样的2小时作用后的感染性滴度常用对数(3检体的平均值)
Log(Vc):抗病毒试样的2小时作用后的感染性滴度常用对数(3检体的平均值)
[表7]
如表中所示,吸附有铜的硫代硫酸盐配合物溶液的Zn系HT复合体(样品6)对作为对象的病毒种类表现出极高的抗病毒性能。
Claims (19)
1.一种水滑石和纤维的复合体的制造方法,包括在含有纤维的溶液中合成水滑石,所述方法包括如下工序:
(a)在含有构成中间层的碳酸根离子的碳酸盐水溶液和碱性溶液中浸渍纤维的工序,接着,在经浸渍的纤维中添加含有构成基本层的二价金属离子和三价金属离子的金属盐水溶液的工序;或者
(b)在含有构成基本层的二价金属离子和三价金属离子的金属盐水溶液中浸渍纤维的工序,接着,在经浸渍的纤维中添加含有构成中间层的碳酸根离子的碳酸盐水溶液和碱性溶液的工序。
2.根据权利要求1所述的方法,其中,进一步包括:在水滑石和纤维的复合体中添加含有阴离子性物质的溶液。
3.根据权利要求1或2所述的方法,其中,含有阴离子性物质的溶液为含有铜或银的硫代硫酸盐配合物溶液。
4.根据权利要求1或2所述的方法,其中,所述纤维为化学纤维、再生纤维或者天然纤维。
5.根据权利要求4所述的方法,其中,所述纤维为纤维素纤维。
6.根据权利要求1或2所述的方法,其中,所述金属盐水溶液的2价的金属离子为镁或锌。
7.根据权利要求1或2所述的方法,其中,所述金属盐水溶液的3价的金属离子为铝。
8.根据权利要求1或2所述的方法,其中,水滑石和纤维的复合体的灰分中含有10%以上的镁或锌。
9.一种含有水滑石和纤维素纤维而成的复合体,其中,纤维素纤维表面的60%以上被水滑石被覆,复合体的灰分为10%以上,复合体的灰分含有10%以上的镁或锌。
10.根据权利要求9所述的复合体,其中,所述水滑石的2价的金属离子为镁或锌。
11.根据权利要求9或10所述的复合体,其中,所述水滑石的3价的金属离子为铝。
12.根据权利要求9或10所述的复合体,其中,附着有铜或者银。
13.一种包含权利要求9~12中任一项所述的复合体的产品。
14.根据权利要求13所述的产品,其中,所述产品为卫生用品。
15.根据权利要求13或14所述的产品,其中,所述产品用于除臭。
16.根据权利要求13或14所述的产品,其中,所述产品用于抗菌。
17.根据权利要求13或14所述的产品,其中,所述产品用于抗病毒。
18.根据权利要求13或14所述的产品,其中,所述产品为片材的形态。
19.一种制造权利要求18所述的产品的方法,该方法包括对含有复合体的水性浆料进行片材化的工序。
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JP7034864B2 (ja) * | 2017-10-31 | 2022-03-14 | 日本製紙株式会社 | 機能性材料及びその利用 |
JP6786745B2 (ja) * | 2018-04-20 | 2020-11-18 | 日本製紙株式会社 | セルロース繊維と無機粒子の複合繊維およびその製造方法 |
CN109097856B (zh) * | 2018-08-15 | 2020-11-06 | 晋大纳米科技(厦门)有限公司 | 一种铜系抗菌母粒及其制备方法 |
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JP7264178B2 (ja) * | 2018-12-27 | 2023-04-25 | 東亞合成株式会社 | 非エンベロープ型抗ウイルス剤及びそれを含む組成物並びに抗ウイルス製品及びその製造方法 |
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CN115262234A (zh) * | 2022-08-09 | 2022-11-01 | 南京林业大学 | 高强度防腐大豆蛋白胶黏剂及其制备方法与应用 |
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KR102483817B1 (ko) | 2022-12-30 |
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KR20190039989A (ko) | 2019-04-16 |
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