CN113358446A - 纤维素纳米纤维分散液的评价方法 - Google Patents
纤维素纳米纤维分散液的评价方法 Download PDFInfo
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- CN113358446A CN113358446A CN202110679002.8A CN202110679002A CN113358446A CN 113358446 A CN113358446 A CN 113358446A CN 202110679002 A CN202110679002 A CN 202110679002A CN 113358446 A CN113358446 A CN 113358446A
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- cellulose
- cellulose nanofiber
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- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical compound [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
本发明提供一种一种纤维素纳米纤维分散液,利用具备如下工序的方法进行评价时,观察不到150μm以上的大小的凝聚物,(1)准备纤维素纳米纤维分散液的工序,(2)在所述纤维素纳米纤维分散液中添加色料的工序,和(3)用光学显微镜观察添加了所述色料的纤维素纳米纤维分散液的工序。
Description
技术领域
本发明涉及纤维素纳米纤维分散液的评价方法。
背景技术
纤维素纳米纤维(CNF)是水系分散性优异的、具有约4~几百nm左右的纤维直径的微细纤维,期待作为保持树脂强化材料、食品、化妆品、医疗品或涂料等的粘度、强化食品原料面团、保持水分、提高食品稳定性的、低热量添加物或乳化稳定助剂的利用(专利文献1等)。使用CNF作为添加剂时,通常,CNF以分散于水中的状态(湿润状态)进行使用。
现有技术文献
专利文献
专利文献1:日本特开2008-1728号
发明内容
虽然是期待在各种用途中开展的CNF,但在CNF分散液中存在CNF彼此缔合的凝聚物时,有可能产生各种各样的问题。因此,需要事先确认CNF分散液中有无凝聚物,并且根据需要将CNF分散液中的凝聚物除去或解纤。然而,因为CNF是非常细的纤维,其分散液的透明性非常高,因此即便存在CNF彼此的凝聚物,无法通过目视确认也会成为问题。
鉴于上述情况,本发明的目的在于提供一种对无法通过目视判断的CNF分散液中的CNF彼此的凝聚物的有无进行评价的方法。
[1]一种纤维素纳米纤维分散液的评价方法,具备如下工序:
(1)准备纤维素纳米纤维分散液的工序;
(2)在上述纤维素纳米纤维分散液中添加色料的工序;和
(3)用光学显微镜观察添加了上述色料的纤维素纳米纤维分散液的工序。
[2]根据[1]所述的方法,其中,上述色料为有色颜料。
[3]根据[2]所述的方法,其中,上述有色颜料的平均粒径为10μm以下。
[4]根据[1]~[3]中任一项所述的方法,其中,上述工序(2)包含将有色颜料的分散液添加到纤维素纳米纤维分散液中的步骤。
[5]根据[1]~[4]中任一项所述的方法,其中,进一步包含(4)如下求出CNF分散指数的工序:
1)将分散液夹在两张玻璃板中,形成厚度0.15mm的膜,用显微镜观察该膜并测定凝聚物的长径,如下进行分级
粒大:100~150μm,粒中:50~100μm,粒小:20~50μm
2)由下式算出CNF分散指数
CNF分散指数=(粒大的个数×64+粒中的个数×8+粒小的个数×1)÷2。
[6]一种纤维素纳米纤维分散液,利用上述[1]~[4]中任一项所述的方法进行评价时,观察不到150μm以上的大小的凝聚物。
[7]一种纤维素纳米纤维分散液,由上述[5]所述的方法求出的CNF分散指数为500以下。
[8]根据[6]或[7]所述的分散液,其中,上述纤维素纳米纤维分散液是将一次制造而成的纤维素纳米纤维分散液干燥后再分散到分散介质中而得到的分散液。
[9]一种食品,含有上述[6]~[8]中任一项所述的纤维素纳米纤维分散液或来自该分散液的纤维素纳米纤维。
[10]一种化妆品,含有上述[6]~[8]中任一项所述的纤维素纳米纤维分散液或来自该分散液的纤维素纳米纤维。
[11]一种橡胶组合物,含有上述[6]~[8]中任一项所述的纤维素纳米纤维分散液或来自该分散液的纤维素纳米纤维。
根据本发明,能够提供一种对无法通过目视判断的CNF分散液中的CNF彼此的凝聚物的有无进行评价的方法。
附图说明
图1表示实施例1中的CNF分散液的利用光学显微镜得到的观察结果。
图2表示实施例2中的CNF分散液的利用光学显微镜得到的观察结果。
图3表示实施例3中的CNF分散液的利用光学显微镜得到的观察结果。
图4表示实施例4中的CNF分散液的利用光学显微镜得到的观察结果。
图5表示实施例5中的CNF分散液的利用光学显微镜得到的观察结果。
图6表示比较例1中的CNF分散液的利用光学显微镜得到的观察结果。
图7表示比较例2中的CNF分散液的利用光学显微镜得到的观察结果。
具体实施方式
本发明的纤维素纳米纤维(CNF)分散液的评价方法具备如下工序:(1)准备纤维素纳米纤维的分散液的工序;(2)在上述纤维素纳米纤维分散液中添加色料的工序;(3)用光学显微镜观察添加了色料的纤维素纳米纤维分散液的工序。本发明中“A~B”包含其端值即A和B。另外,“A或B”包含A、B中的任一者或两者。
本发明中,纤维素纳米纤维(CNF)彼此的凝聚物表示在后述的解纤处理时产生的解纤不充分的未解纤纤维物、在分散液中产生的CNF网络结构体或在CNF浓缩或干燥时产生的凝聚体等。这些凝聚物因其内部含有分散液的分散介质而在可见光区域的透明性高,从而目视难以辨别。
(纤维素纳米纤维)
纤维素纳米纤维(CNF)是纤维宽度为4~500nm左右、长径比为100以上的微细纤维,可以通过将经阳离子化或阴离子化等化学处理的纤维素解纤而得到。作为阴离子化处理,可举出羧基化(氧化)、羧甲基化、酯化、导入功能性官能团等。
(纤维素原料)
作为用于制造化学改性纤维素的纤维素原料,例如可举出植物性材料(例如、木材、竹、麻、黄麻、洋麻、农田废弃物、布、纸浆)、动物性材料(例如海鞘类)、藻类、以微生物(例如醋酸菌(醋酸杆菌,Acetobacter))产生物等为来源的物质。作为纸浆,可举出针叶树未漂白牛皮纸浆(NUKP)、针叶树漂白牛皮纸浆(NBKP)、阔叶树未漂白牛皮纸浆(LUKP)、阔叶树漂白牛皮纸浆(LBKP)、针叶树未漂白亚硫酸盐纸浆(NUSP)、针叶树漂白亚硫酸盐纸浆(NBSP)、热机械纸浆(TMP)、再生纸浆、废纸等。它们都可以使用,但优选来自植物或微生物的纤维素纤维,更优选来自植物的纤维素纤维。
(羧甲基化)
本发明中,使用羧甲基化的纤维素作为化学改性纤维素时,羧甲基化的纤维素可以用公知的方法将上述纤维素原料羧甲基化而得到,也可以使用市售品。任一情况下,优选纤维素的每个无水葡萄糖单元的羧甲基取代度为0.01~0.50。作为制造这样的羧甲基化的纤维素的方法的一个例子,可以举出如下方法。将纤维素作为起始原料,使用3~20质量倍的水或低级醇作为溶剂。具体而言,可以将水、甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、叔丁醇等单独使用或并用2种以上使用。使用水和低级醇的混合溶剂时,低级醇的混合比例为60~95质量%。作为丝光剂,使用相对于起始原料的无水葡萄糖残基为0.5~20倍摩尔的碱金属氢氧化物,具体而言,使用氢氧化钠、氢氧化钾。将起始原料与溶剂、丝光剂混合,在反应温度0~70℃、优选为10~60℃、使反应时间为15分钟~8小时、优选为30分钟~7小时的条件下进行丝光处理。其后,添加相对于葡萄糖残基为0.05~10.0倍摩尔的羧甲基化剂,在反应温度30~90℃、优选40~80℃、使反应时间为30分钟~10小时、优选为1小时~4小时的条件下进行醚化反应。
(羧基化)
本发明中,使用经羧基化(氧化)的纤维素作为化学改性纤维素时,羧基化纤维素(也称为“氧化纤维素”)可以通过利用公知的方法将上述纤维素原料羧基化(氧化)而得到。虽然没有限定,但羧基的量相对于阴离子改性纤维素纳米纤维的绝干质量,优选为0.6~2.0mmol/g,进一步优选为1.0mmol/g~2.0mmol/g。
作为羧基化(氧化)方法的一个例子,可以举出如下方法:在N-氧自由基化合物与选自溴化物、碘化物和它们的混合物中的化合物的存在下使用氧化剂在水中氧化纤维素原料。能够通过该氧化反应而选择性地氧化纤维素表面的吡喃葡萄糖环的C6位的伯羟基,从而得到表面具有醛基和羧基(-COOH)或羧酸酯基(-COO-)的纤维素纤维。反应时的纤维素的浓度没有特别限定,但优选5质量%以下。
N-氧自由基化合物是指可产生氮氧自由基的化合物。作为N-氧自由基化合物,只要是促进目标氧化反应的化合物,就可以使用任意化合物。作为其例子,可举出2,2,6,6-四甲基哌啶-1-氧基自由基(TEMPO)及其衍生物(例如4-羟基TEMPO)。
N-氧自由基化合物的使用量只要是能够氧化作为原料的纤维素的催化剂量即可,没有特别限制。例如相对于绝干1g的纤维素,优选0.01~10mmol,更优选0.01~1mmol,进一步优选0.05~0.5mmol。相对于反应体系,优选0.1~4mmol/L左右。
溴化物是指含有溴的化合物,其例子中包含可以在水中解离而离子化的溴化碱金属。另外,碘化物是指含有碘的化合物,其例子中包含碘化碱金属。溴化物或碘化物的使用量可以在能够促进氧化反应的范围选择。溴化物和碘化物的合计量例如相对于绝干1g的纤维素,优选0.1~100mmol,更优选0.1~10mmol,进一步优选0.5~5mmol。
作为氧化剂,可以使用公知的氧化剂,例如可以使用卤素、次卤酸、亚卤酸、高卤酸或它们的盐、卤素氧化物、过氧化物等。其中,优选便宜且环境负荷少的次氯酸钠。氧化剂的使用量例如相对于绝干1g的纤维素,优选0.5~500mmol,更优选0.5~50mmol,进一步优选1~25mmol,最优选3~10mmol。对于N-氧自由基化合物而言,相对于该N-氧自由基化合物1mol优选1~40mol。
纤维素的氧化工序即便在比较温和的条件下也能够使反应高效地进行。因此,反应温度优选4~40℃,另外也可以为15~30℃左右的室温。随着反应进行而在纤维素中生成羧基,因此认为反应液的pH降低。为了使氧化反应高效地进行,优选添加氢氧化钠水溶液等碱性溶液而将反应液的pH维持在8~12、优选10~11左右。从操作性的容易性、不宜产生副反应等方面考虑,反应介质优选水。
氧化反应的反应时间可以根据氧化进行的程度而适当地设定,通常为0.5~6小时,例如为0.5~4小时左右。
另外,氧化反应可以分成2个阶段实施。例如可以使在第1阶段的反应结束后过滤分离而得到的氧化纤维素再次以相同或不同反应条件氧化,从而不受因在第1阶段的反应中副生成的盐所致的反应阻碍地高效氧化。
作为羧基化(氧化)方法的另一例子,可以举出使含有臭氧的气体与纤维素原料接触而进行氧化的方法。通过该氧化反应,从而吡喃葡萄糖环的至少2位和6位的羟基被氧化,同时发生纤维素链的分解。含有臭氧的气体中的臭氧浓度优选为50~250g/m3,更优选为50~220g/m3。将纤维素原料的固体成分设为100质量份时,相对于纤维素原料的臭氧添加量优选为0.1~30质量份,更优选为5~30质量份。臭氧处理温度优选为0~50℃,更优选为20~50℃。臭氧处理时间没有特别限定,但为1~360分钟左右,优选30~360分钟左右。如果臭氧处理的条件为这些范围内,则能够防止纤维素过度氧化和过度分解,氧化纤维素的收率变得良好。实施臭氧处理后,可以使用氧化剂进行追氧化处理。在追氧化处理中使用的氧化剂没有特别限定,可举出二氧化氯、亚氯酸钠等氯系化合物或氧、过氧化氢、过硫酸、过乙酸等。例如可以通过将这些氧化剂在水或醇等极性有机溶剂中溶解而制成氧化剂溶液,在溶液中浸渍纤维素原料而进行追氧化处理。
氧化纤维素的羧基的量可以通过控制上述氧化剂的添加量、反应时间等反应条件进行调整。
(阳离子化)
本发明中,作为化学改性纤维素,使用经阳离子化的纤维素时,可以通过在水或碳原子数1~4的醇的存在下使缩水甘油基三甲基氯化铵、3-氯-2羟丙基三烷基氢化铵(3-chloro-2hydroxypropyl trialkyl ammonium hydride)或其卤代醇型等的阳离子化剂和作为催化剂的碱金属氢氧化物(氢氧化钠、氢氧化钾等)与上述纤维素原料反应而得到经阳离子改性的纤维素。在该方法中,得到的经阳离子改性的纤维素的每个葡萄糖单元的阳离子取代度可以通过控制使其反应的阳离子化剂的添加量、混合溶剂时的水和上述醇的组成比率而进行调整。
经阳离子改性的纤维素的每个葡萄糖单元的阳离子取代度优选为0.02~0.50。通过在纤维素中导入阳离子取代基,从而纤维素彼此进行电排斥。因此,导入了阳离子取代基的纤维素能够容易地进行纳米化解纤。如果每个葡萄糖单元的阳离子取代度小于0.02,则无法充分地进行纳米化解纤。另一方面,如果每个葡萄糖单元的阳离子取代度大于0.50,则进行溶胀或溶解,因此有时难以作为纳米纤维而得到。为了高效地进行解纤,优选清洗上述得到的经阳离子化的纤维素系原料。
(酯化)
作为纤维素,也可以使用经酯化的纤维素。作为酯化,可举出在纤维素系原料中混合磷酸系化合物A的粉末或水溶液的方法、在纤维素系原料的浆料中添加磷酸系化合物A的水溶液的方法等。作为磷酸系化合物A,可举出磷酸、多磷酸、亚磷酸、膦酸、多膦酸或它们的酯。它们也可以为盐的形态。其中,由于低成本、容易处理、而且向纸浆纤维的纤维素中导入磷酸基而实现解纤效率的提高等理由,优选具有磷酸基的化合物。作为具有磷酸基的化合物,可举出磷酸、磷酸二氢钠、磷酸氢二钠、磷酸三钠、焦磷酸钠、偏磷酸钠、磷酸二氢钾、磷酸氢二钾、磷酸三钾、焦磷酸钾、偏磷酸钾、磷酸二氢铵、磷酸氢二铵、磷酸三铵、焦磷酸铵、偏磷酸铵等。它们可以使用1种或并用2种以上。其中,从导入磷酸基的效率高、在下述解纤工序容易解纤且容易在工业上应用的观点考虑,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。另外,从能够均匀地进行反应且导入磷酸基的效率变高的方面考虑,上述磷酸系化合物A优选以水溶液的形式使用。从导入磷酸基的效率变高的方面考虑,磷酸系化合物A的水溶液的pH优选为7以下,但从抑制纸浆纤维的水解的观点考虑,优选pH3~7。
作为磷酸酯化纤维素的制造方法的例子,可以举出以下的方法。将磷酸系化合物一边搅拌一边添加到固体成分浓度0.1~10重量%的纤维素系原料的悬浊液中,从而向纤维素中导入磷酸基。将纤维素系原料设为100重量份时,磷酸系化合物A的添加量以磷元素量计,优选为0.2~500重量份,更优选为1~400重量份。只要磷酸系化合物A的比例为上述下限值以上,就能够进一步提高微细纤维状纤维素的收率。但是,如果超过上述上限值,则收率提高的效果达到极限,因此从成本上考虑并不优选。
除磷酸系化合物A以外也可以混合化合物B的粉末或水溶液。化合物B没有特别限定,优选显示碱性的含氮化合物。这里的“碱性”定义为在酚酞指示剂的存在下水溶液显粉~红色,或者水溶液的pH大于7。本发明中使用的显示碱性的含氮化合物只要起到本发明的效果,就没有限定,但优选具有氨基的化合物。作为该化合物,可举出脲、甲胺、乙胺、三甲胺、三乙胺、单乙醇胺、二乙醇胺、三乙醇胺、吡啶、乙二胺、己二胺等。其中,优选成本低且操作性优异的脲。化合物B的添加量相对于纤维素原料的固体成分100重量份,优选2~1000重量份,更优选100~700重量份。反应温度优选0~95℃,更优选30~90℃。反应时间没有特别限定,为1~600分钟左右,更优选30~480分钟。如果酯化反应的条件在这些范围内,则能够防止纤维素过度酯化而易于溶解,磷酸酯化纤维素的收率变得良好。在将得到的磷酸酯化纤维素悬浊液脱水后,从抑制纤维素水解的观点考虑,优选以100~170℃进行加热处理。进而,优选在加热处理时含有水的期间以130℃以下、优选110℃以下进行加热,除去水后,以100~170℃进行加热处理。
经磷酸酯化的纤维素的每个葡萄糖单元的磷酸基取代度优选为0.001~0.40。通过在纤维素中导入磷酸基取代基,从而纤维素彼此进行电排斥。因此,导入了磷酸基的纤维素能够容易地进行纳米化解纤。如果每个葡萄糖单元的磷酸基取代度小于0.001,则无法充分进行纳米化解纤。另一方面,如果每个葡萄糖单元的磷酸基取代度大于0.40,则发生溶胀或溶解,因此有时无法以纳米纤维的形式得到。为了高效地进行解纤,优选上述得到的经磷酸酯化的纤维素系原料煮沸后,用冷水清洗而进行清洗。
(色料)
色料是指具有白、黑、蓝、红、黄、绿等颜色的材料。在本发明中作为色料,可以使用有色颜料或染料。
(有色颜料)
本发明中,有色颜料是指具有白、黑、蓝、红、黄、绿等颜色的颜料,其形状为板状、球状、鳞片状等,也没有特别限定。作为有色颜料,可举出无机颜料、有机颜料。作为无机颜料,可以例示炭黑、铁黑、复合金属氧化物黑、铬酸锌、铬酸铅、铅丹、磷酸锌、磷酸钒、磷酸钙、磷钼酸铝、钼酸钙、三聚磷酸铝、氧化铋、氢氧化铋、碱式碳酸铋、硝酸铋、硅酸铋、水滑石、锌粉末、云母氧化铁、碳酸钙、硫酸钡、氧化铝白、二氧化硅、硅藻土、高岭土、滑石、粘土、云母、氧化钡、有机膨润土、白炭黑、氧化钛、氧化锌、氧化锑、锌钡白、铅白、苝黑、钼红、镉红、氧化铁红、硫化铈、铬黄、镉黄、黄色氧化铁、黄土、铋黄、土黄赭(Siena)、棕土(umber)、绿土、马尔斯紫、群蓝、深蓝、碱式硫酸铅、碱式硅酸铅、硫化锌、三氧化锑、钙复合物、酞菁蓝、酞菁绿、赭石(ochre)、铝粉、铜粉、黄铜粉、不锈钢粉、氧化钛被覆云母、氧化铁被覆云母、氧化铜锌、银粒子、锐钛矿型氧化钛、氧化铁系烧制颜料、导电性金属粉、电磁波吸收铁素体等。作为有机颜料,可以例示喹吖啶酮红、多偶氮黄、蒽醌红、蒽醌黄、多偶氮红、偶氮色淀黄、苝、酞菁蓝、酞菁绿、异吲哚啉酮黄、沃丘格红(Watching Red)、永固红、对位红、甲苯胺红褐(Toluidine Maroon)、联苯胺黄、坚牢天蓝(Fast Sky Blue)、亮胭脂红6B等。这些颜料可以单独使用或并用2种以上使用。
有色颜料的平均粒径为10μm以下,优选为0.01~10μm,更优选为0.03~1μm。如果平均粒径为10μm以下、优选为1μm以下,则在CNF分散液中有色颜料的分散性稳定,因此容易评价。另一方面,下限值没有限制,但如果平均粒径小于0.01μm,则存在有色颜料进入到凝聚物中的可能性,因此有时难以利用光学显微镜来观察凝聚物。平均粒径利用激光衍射式粒度分布测定装置(作为例子,Malvern公司制MASTERSIZER 3000或Zetasizer Nano ZS)进行测定。颜料不是球形时将最长直径的平均值作为平均粒径。
(染料)
染料是指在选择吸收或反射可见光线而具有固有颜色的有机色素中的利用适当的染色法对纤维或颜料等染色的物质。作为染料,可举出偶氮染料、二苯基甲烷和三苯基甲烷染料、吖嗪染料、嗪染料、噻嗪染料等。这些染料可以单独使用,也可以并用2种以上。
(颜料分散液)
本发明中,优选将使用分散剂等使有色颜料稳定地分散在水系溶剂中的有色颜料分散液添加到CNF分散液中。通过使用有色颜料分散液而使利用光学显微镜进行的观察变得容易。
作为上述水系溶剂,可举出水、甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、叔丁醇、直链或支链戊二醇、脂肪族酮(例如,丙酮、甲乙酮、二丙酮醇等)、多元醇(例如,乙二醇、二乙二醇、三乙二醇等)、具有200~2000g/摩尔的摩尔质量的聚乙二醇、丙二醇、二丙二醇、三丙二醇、三羟甲基丙烷、甘油、硫二甘醇、2-吡咯烷酮、N-甲基吡咯烷酮、N-乙基吡咯烷酮、1,3-二甲基咪唑啉酮、二甲基乙酰胺、二甲基甲酰胺和它们的组合。
作为分散剂,可举出高级脂肪酸、高级脂肪酸酰胺、金属皂、甘油酯、水滑石、聚乙烯蜡、聚丙烯蜡、动物胶、明胶等的单独或2种以上的混合物。
有色颜料分散液中的有色颜料的含量没有限定,但优选为5~20质量%左右。如果有色颜料的含量少,则光学显微镜的观察照片变淡,另一方面,如果有色颜料的含量多,则有可能产生有色颜料的凝聚物。
本发明中,优选在用光学显微镜进行观察时明暗清晰且不易透过光的(容易吸收光)有色颜料,更优选黑色颜料。另外,优选在观察中不发生二次凝聚或不因与CNF的相互作用而发生凝聚的有色颜料。例如,作为有色颜料分散液,可以使用墨汁、墨滴、喷墨打印机用的颜料油墨等。墨是用水系树脂被覆了表面的表面处理炭黑,与粘结剂树脂混合时具有优异的分散性,不易发生二次凝聚,因而即便是较低浓度的CNF分散液,也能够充分发挥较高的黑色度。墨汁或墨滴是含有表面处理炭黑的水系分散液,例如可以通过如下方式制造:将利用使石油系或煤系的油在高温气体中不完全燃烧的炉法等制造的不定形的炉黑的表面用水系树脂被覆,根据需要添加二元醇系的防冻剂和防腐剂,进行混合、浆料化。在本发明中,可以使用市售品(例如,株式会社吴竹制“墨滴”等)。表面处理炭黑或其水系分散液也可以按照已知的方法(例如,日本特开平7-188597号公告、日本特开平6-234946号公告)进行制备。墨汁、墨滴、喷墨打印机用的颜料油墨可以单独使用,也可以组合2种以上使用。
(利用光学显微镜进行的观察)
本发明中,CNF分散液的浓度没有特别限定,优选0.01~10质量%左右,更优选0.1~2质量%左右。如果浓度低,则凝聚物的量减少,因此,另一方面,如果浓度高,则粘度高而有色颜料的分散变得困难,从而精度降低。
本发明中,用于观察添加了色料的纤维素纳米纤维分散液的光学显微镜没有特别限定,可以使用一般的光学显微镜(包括显微镜)。利用光学显微镜观察CNF分散液时的倍率没有限定,但优选50~1000倍。
本发明中,用光学显微镜观察CNF分散液时,将观察不到150μm以上的大小的凝聚物的情况判断为分散性良好。
此外,可以使用CNF分散指数来评价CNF分散液的分散性。CNF分散指数是指将作为纤维的分散性的指标的NEP指数(例如在日本特开平08-134329中公开的)修正成CNF用的指标。具体而言,CNF分散指数如下求出。
1)将分散液夹在两张玻璃板中,形成厚度0.15mm的膜,用显微镜观察分散液并测定凝聚物的长径,如下进行分级。
粒大:100~150μm,粒中:50~100μm,粒小:20~50μm
2)由下式算出CNF分散指数。
CNF分散指数=(粒大的个数×64+粒中的个数×8+粒小的个数×1)÷2
3)如下进行评价。
CNF分散指数为500以下:分散性良好
CNF分散指数为100以下:分散性非常良好
根据本发明评价为在分散介质中的分散性良好的CNF再分散液因为在食品、化妆品、化学合成品等用途中不仅溶解性良好,而且未分散物也少,所以触感光滑,在食品等中添加时口感得到改善。因此,在化妆品等液态产品中使用该CNF时透明性、透光度、粘度再现性等得到改善,而且,在用于光学膜等化学合成品时透明性、透光度等得到改善。
本发明中的食品包含CNF分散液或来自该分散液的CNF。作为这样的食品,可举出烘焙点心(饼干、咸饼干等)、米果(脆饼、仙贝、年糕片等)、点心面包(面包干等)、油性点心(油炸点心等)、巧克力、西式点心、糖果·焦糖、干点心、模制点心、豆点心、羊羹等点心类、以及馒头、谷物、小吃类、面包、面条等面皮类。本发明中的食品优选通过如下方式得到的食品,即在制造饼干、曲奇、咸饼干、威化、小吃、谷物、面包等、脆饼、年糕片、仙贝等米果等以小麦、玉米、黑麦、燕麦、大米等的谷物粉为主要原料的食品时,添加CNF,根据需要添加糖类、油脂、鸡蛋、乳制品、膨松剂、食盐、乳化剂、香料等副原料而制备面团,然后经过混炼、烧制的工序或混炼、发酵、烧制的工序而得到。另外,也包括在烧制中使用油进行炸制。
本发明中的化妆品包含CNF分散液或来自该分散液的CNF。作为这样的化妆品,可举出霜、乳液、化妆水、美容液等基础化妆品、香皂、洗面奶、洗发水、护发素等清洁用化妆品、生发液、整法液等头发用化妆品、粉底、眼线笔、睫毛膏、口红等彩妆化妆品、牙膏等口腔化妆品、浴用化妆品等。
本发明中的橡胶组合物包含CNF分散液或来自该分散液的CNF。该橡胶成分通常是以有机高分子为主成分的弹性极限高且弹性率低的成分。橡胶成分大致分为天然橡胶和合成橡胶,在本发明中可以使用任一者,也可以组合两者。作为天然橡胶,可以是不实施化学修饰、狭义的天然橡胶,另外,可举出氯化天然橡胶、氯磺化天然橡胶、环氧化天然橡胶、氢化天然橡胶、脱蛋白天然橡胶这样地对天然橡胶进行化学修饰而得的橡胶。作为合成橡胶,例如可举出丁二烯橡胶(BR)、苯乙烯-丁二烯共聚物橡胶(SBR)、异戊二烯橡胶(IR)、丁基橡胶(IIR)、丙烯腈-丁二烯橡胶(NBR)、氯丁橡胶(CR)、苯乙烯-异戊二烯共聚物橡胶、苯乙烯-异戊二烯-丁二烯共聚物橡胶、异戊二烯-丁二烯共聚物橡胶等二烯系橡胶、乙烯-丙烯橡胶(EPM,EPDM)、丙烯酸橡胶(ACM)、表氯醇橡胶(CO,ECO)、氟橡胶(FKM)、硅橡胶(Q)、聚氨酯橡胶(U)、氯磺化聚乙烯(CSM)。
实施例
<CNF分散液的制造>
将来自针叶树的漂白过的未打浆牛皮纸浆(白色度85%)5g(绝干)加入到溶解了TEMPO(Sigma Aldrich公司)39mg和溴化钠514mg的水溶液500ml中,搅拌直到纸浆均匀分散。在反应体系中以成为5.5mmol/g的方式添加次氯酸钠水溶液,开始氧化反应。反应中体系内的pH降低,但逐次添加3M氢氧化钠水溶液,调节至pH10。消耗次氯酸钠,在体系内的pH不再变化的时刻结束反应。将反应后的混合物用玻璃过滤器过滤进行纸浆分离,将纸浆充分水洗,由此得到被氧化的纸浆(羧基化纤维素)。纸浆收率为90%,氧化反应所需的时间为90分钟,羧基量为1.6mmol/g。
将上述工序中得到的氧化纸浆用水调节为1.0%(w/v)(=1.0质量%),用超高压均质机(20℃,150MPa)处理3次,得到阴离子改性纤维素纳米纤维分散液。得到的纤维的平均纤维直径为40nm,长径比为150。
(羧基量的测定方法)
制备羧基化纤维素的0.5质量%浆料(水分散液)60ml,加入0.1M盐酸水溶液调节为pH2.5后,滴加0.05N的氢氧化钠水溶液而pH变为11为止测定电导率。根据在电导率的变化平缓的弱酸的中和阶段消耗的氢氧化钠量(a),利用下式进行计算。
羧基量〔mmol/g羧基化纤维素〕=a〔ml〕×0.05/羧基化纤维素质量〔g〕
(平均纤维直径、长径比的测定方法)
阴离子改性CNF的平均纤维直径和平均纤维长度使用场发射型扫描电子显微镜(FE-SEM)对随机选择的200根纤维进行解析。长径比利用下述式进行计算。
长径比=平均纤维长度/平均纤维直径
<实施例1>
作为CNF,使用上述的羧基化CNF(羧基量:1.6mmol/g,平均纤维直径:40nm,长径比:150)。在CNF的1.0质量%水性悬浊液1g中滴入2滴墨滴(株式会社吴竹制,固体成分10%),利用涡旋混合器搅拌1分钟。使用Zetasizer Nano ZS(Malvern公司制)测定该墨滴的平均粒径3次,结果其平均值为0.22μm。使用光学显微镜(数字显微镜KH-8700(株式会社HIROX制))以倍率100倍观察该分散液。将结果示于图1。CNF分散指数为0。
<实施例2>
将实施例1中使用的CNF在105℃的空气干燥器中干燥,再次加入水来调整CNF水分散液(固体成分1.0质量%),使用TK均质机(6000rpm)搅拌60分钟。与实施例1同样地在该分散液中滴入2滴墨滴,利用涡旋混合器搅拌1分钟。用光学显微镜观察该分散液。将结果示于图2。CNF分散指数为1825。
<实施例3>
将来自针叶树的漂白过的未打浆牛皮纸浆(白色度85%)5g(绝干)加入到溶解了TEMPO(Sigma Aldrich公司)39mg和溴化钠514mg的水溶液500ml中,搅拌直到纸浆均匀分散。将次氯酸钠水溶液以成为5.7mmol/g的方式添加到反应体系中,开始氧化反应。反应中体系内的pH降低,但逐次添加3M氢氧化钠水溶液,调节至pH10。消耗次氯酸钠,在体系内的pH不再变化的时刻结束反应。将反应后的混合物用玻璃过滤器过滤进行纸浆分离,将纸浆充分水洗,由此得到被氧化的纸浆(羧基化纤维素)。纸浆收率为90%,氧化反应所需的时间为90分钟,羧基量为1.67mmol/g。
将上述工序中得到的氧化纸浆用水调节为1.0%(w/v)(=1.0质量%),利用超高压均质机(20℃,150MPa)处理5次,得到阴离子改性纤维素纳米纤维分散液。得到的纤维的平均纤维直径为4nm,长径比为150。
将这样得到的CNF在105℃的空气干燥器中干燥,再次加入水和相对于CNF绝干固体成分100重量份为40份的羧甲基纤维素来调节CNF水分散液(固体成分1.0质量%),除此以外,与实施例2同样地进行实验,用光学显微镜观察该分散液。将结果示于图3。CNF分散指数为24。
<实施例4>
将在实施例3中使用的CNF在105℃的空气干燥器中干燥,再次加入水和相对于CNF绝干固体成分100重量份为40份的羧甲基纤维素来调节CNF水分散液(固体成分1.0质量%),使用TK均质机(1000rpm)搅拌60分钟。与实施例1同样地在该分散液中滴入2滴墨滴,利用涡旋混合器搅拌1分钟。用光学显微镜观察该分散液。将结果示于图4。CNF分散指数为252。
<实施例5>
将在实施例3中使用的CNF在105℃的空气干燥器中干燥,再次加入水和相对于CNF绝干固体成分100重量份为40份的羧甲基纤维素来调节CNF水分散液(固体成分1.0质量%),使用TK均质机(600rpm)搅拌180分钟。与实施例1同样地在该分散液中滴入2滴墨滴,利用涡旋混合器搅拌1分钟。用光学显微镜观察该分散液。将结果示于图5。CNF分散指数为942。
<实施例6>
将使用的墨滴从墨滴(株式会社吴竹制)变更为墨滴(开明株式会公司制),除此以外,与实施例1同样地用光学显微镜进行观察。其结果可以确认CNF分散液中无凝聚物。使用Zetasizer Nano ZS(Malvern公司制)测定该墨滴的平均粒径3次,结果其平均值为0.09μm。
<实施例7>
将使用的墨滴变更为将固体墨(株式会社吴竹制)用砚台和水磨墨而得到的墨滴,除此以外,与实施例1同样地用光学显微镜进行观察。其结果可以确认CNF分散液中无凝聚物。使用Zetasizer Nano ZS(Malvern公司制)测定该墨滴的平均粒径3次,结果其平均值为0.51μm。
<实施例8>
将使用的墨滴变更为按照日本特开2015-199966的“实施例1”中记载的制造方法制造的“水性颜料油墨”,除此以外,与实施例1同样地用光学显微镜进行观察。其结果可以确认CNF分散液中无凝聚物。
<比较例1>
在不滴加墨滴的情况下用光学显微镜观察在实施例1中使用的CNF。将结果示于图6。CNF分散指数为0。
<比较例2>
在不滴加墨滴的情况下用光学显微镜观察在实施例2中使用的CNF。将结果示于图7。CNF分散指数为0。
<结果>
在不进行干燥处理、没有凝聚物的CNF分散液的观察结果(图1、图6)中,看不到因墨滴有无所致的差异,但在进行干燥处理、含有凝聚物的CNF分散液的观察结果(图2~5、图7)中,看到了因墨滴有无所致的差异。根据该结果,可知通过用光学显微镜观察添加了墨滴的CNF分散液,能够容易地判断以往困难的CNF分散液中的凝聚物的有无。
Claims (10)
1.一种纤维素纳米纤维分散液,利用具备如下工序的方法进行评价时,观察不到150μm以上的大小的凝聚物,
(1)准备纤维素纳米纤维分散液的工序,
(2)在所述纤维素纳米纤维分散液中添加色料的工序,和
(3)用光学显微镜观察添加了所述色料的纤维素纳米纤维分散液的工序。
2.根据权利要求1所述的纤维素纳米纤维分散液,其中,所述色料为有色颜料。
3.根据权利要求2所述的纤维素纳米纤维分散液,其中,所述有色颜料的平均粒径为10μm以下。
4.根据权利要求1~3中任一项所述的纤维素纳米纤维分散液,其中,所述工序(2)包含将有色颜料的分散液添加到纤维素纳米纤维分散液中的步骤。
5.根据权利要求1~4中任一项所述的纤维素纳米纤维分散液,其中,进一步包含(4)如下求出CNF分散指数的工序:
1)将分散液夹在两张玻璃板中,形成厚度0.15mm的膜,用显微镜观察该膜并测定凝聚物的长径,如下进行分级,
粒大:100~150μm,粒中:50~100μm,粒小:20~50μm
2)由下式算出CNF分散指数
CNF分散指数=(粒大的个数×64+粒中的个数×8+粒小的个数×1)÷2。
6.根据权利要求5所述的纤维素纳米纤维分散液,其中,CNF分散指数为500以下。
7.根据权利要求1~6中任一项所述的纤维素纳米纤维分散液,其中,所述纤维素纳米纤维分散液是将一次制造而成的纤维素纳米纤维分散液干燥后再分散到分散介质中而得到的分散液。
8.一种食品,含有权利要求1~7中任一项所述的纤维素纳米纤维分散液或来自该分散液的纤维素纳米纤维。
9.一种化妆品,含有权利要求1~7中任一项所述的纤维素纳米纤维分散液或来自该分散液的纤维素纳米纤维。
10.一种橡胶组合物,含有权利要求1~7中任一项所述的纤维素纳米纤维分散液或来自该分散液的纤维素纳米纤维。
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CA2976452A1 (en) | 2016-08-25 |
CN107250790B (zh) | 2021-07-06 |
JP6769947B2 (ja) | 2020-10-14 |
US20210349072A1 (en) | 2021-11-11 |
WO2016133076A1 (ja) | 2016-08-25 |
US20180045706A1 (en) | 2018-02-15 |
JPWO2016133076A1 (ja) | 2018-01-18 |
EP3699586A1 (en) | 2020-08-26 |
EP3260861A4 (en) | 2019-10-09 |
EP3260861A1 (en) | 2017-12-27 |
CN107250790A (zh) | 2017-10-13 |
CA2976452C (en) | 2023-08-22 |
US11092587B2 (en) | 2021-08-17 |
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