CN113944049A - 一种柔韧吸水蔺草纤维材料及其制备方法 - Google Patents
一种柔韧吸水蔺草纤维材料及其制备方法 Download PDFInfo
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Abstract
本发明属于纺织新材料领域，公开了一种柔韧吸水蔺草材料及其制备方法。该方法包含以下步骤：第一步将蔺草剪成一小段放进烘箱中烘干备用。第二步配置反应所需要的混合溶液，将蔺草放入混合溶液当中，添加硫酸镁，密封条件下加热，反应结束后除去反应液，依次用去离子水，无水乙醇及丙酮清洗，干燥后得到改性的蔺草。本方明方法绿色，简单环保，所得到的纤维材料柔软性好，吸水速干，在输水，蒸腾方面具有广泛的应用前景。
Description
技术领域
本发明涉及一种柔韧吸水蔺草纤维材料及其制备方法，属于纺织新材料领域。
背景技术
环境问题和政府立法倾向于将科学界的兴趣转向使用天然材料，从而将研究主题集中在对自然影响较小的可回收、可再生和可持续材料上。因此，下一代材料和工艺的发展受到可持续性、生态效率和绿色化学原则的强烈影响。木质纤维素纤维，如亚麻，剑麻和黄麻已经被提出作为能够在许多应用中替代合成纤维，因为它们具有生物降解性、轻质和良好的物理和机械性能。蔺草就是其中的一种木质纤维素纤维且在自然界的储量丰富，因此值得我们深入研究。
蔺草是一种天然生物材料，将其研究可以为今后开发这种纤维作为生物复合材料的潜在增强剂奠定基础。蔺草本身柔韧性较差，吸水性较低，对其进行一定的处理后柔韧性和吸水性都将显著得到提高。
发明内容
本发明所要解决的技术问题是提出了一种柔软且吸水速干的纤维材料的制备方法，该方法所得材料制备过程简便，成本和能耗都较低。
一种柔软且吸水速干的纤维材料及其制备方法，包括以下步骤：
(1)先将样品剪成一小段，在烘箱中干燥一段时间后，取出备用；
(2)配置反应所需要的混合溶液，将样品放入溶液中,加入硫酸镁，密封条件下加热；
(3)反应结束后除去反应液，清洗，干燥；
(4)原始纤维材料柔韧性差，吸水性差，处理后的材料柔韧性和吸水性得到显著提高；
本发明技术中，第一步是将样品长度剪成50-100mm，样品长度太短则不利于后续柔韧度的测试，样品长度太长则不利于溶液反应的进行且反应后纤维容易变形，烘箱温度为50-100℃，烘箱温度太高会破坏纤维的柔韧性，太低则会影响干燥的时间，干燥时间为10-24小时。
本发明技术中，混合溶液可以是亚氯酸钠和冰醋酸或者氢氧化钠和亚硫酸钠或者氯化胆碱和草酸或者双氧水溶液，此外添加的硫酸镁对去除木质素具有良好的促进作用，一方面可以促进木质素的去除，另一方面加快了反应时间。
本发明技术中，混合溶液可以是质量分数为1-10％亚氯酸钠溶液，冰醋酸的添加量为使溶液的pH值为2-5，溶液的pH不可过低或过高否则都会影响反应的进行或者1-3mol/L的氢氧化钠和0.1-1mol/L的亚硫酸钠溶液，氢氧化钠的浓度不可过高否则会强烈的破坏纤维的完整性或者1:1-1:5(摩尔比)氯化胆碱和草酸的混合溶液，氯化胆碱的含量不可过低否则会影响木质素的去除或者5-10wt％的双氧水溶液，双氧水的浓度不可过高否则会氧化纤维造成纤维的柔韧性较低。
本发明技术中，混合溶液的加热温度为50-100℃，加热温度太低会影响反应的进行，太高则会影响纤维的结构完整性，反应时间为5-10小时。
本发明技术中，第二步是将样品浸没于混合液中，反应至样品变为白色。
本发明技术中，第三步是反应结束后将样品依次用去离子水，无水乙醇及丙酮清洗，或者依次用去离子水，体积比为1：1的无水乙醇-丙酮混合溶剂清洗，重复清洗三次。
本发明技术中，第四步是清洗后的样品用冷冻干燥机在-10℃—-50℃冻干12-36小时。
有益效果：
本发明的柔韧吸水蔺草纤维材料的原始结构为双层多孔中空结构，，柔韧性和吸水性都较差，柔韧性为70-90mN,吸水率为0.1-0.2g/min。其主要成分是纤维素，半纤维素含量(15-20％)和木质素含量(25-30％)，经过处理后半纤维素和木质素的含量降低，分别为7-14％，5-10％。因为木质素是刚性的，因而纤维的柔韧性得到了提高。另一方面，处理后纤维的孔隙率得到了提高，由原来的35-45％提高到了75-90％这有助于纤维更好的吸水，吸水率由原来的的0.1-0.2g/min提高到了1.0-2.3g/min.，故纤维的柔韧性和吸水性都显著增强。
附图说明
图1a是原始蔺草的内部芯结构图。
图1b是经过反应后的蔺草内部芯结构图(1)。
图1c是经过反应后的蔺草内部芯结构图(2)。
图1d是经过反应后的蔺草内部芯结构图(3)。
图1e是经过反应后的蔺草内部芯结构图(4)。
图2a是原始蔺草的内部壳结构图。
图2b是经过反应后的蔺草内部壳结构图(1)。
图2c是经过反应后的蔺草内部壳结构图(2)。
图2d是经过反应后的蔺草内部壳结构图(3)。
图2e是经过反应后的蔺草内部壳结构图(4)。
具体实施方式
下面结合附图对本发明作进一步说明。
如图1a-e，2a-e所示：
实施例1
第一步取20根蔺草，将蔺草剪成80mm，在60℃的烘箱中烘10小时后取出备用；第二步配置质量分数为5％的亚氯酸钠溶液；第三步在第二步配置的溶液中滴加冰醋酸溶液数滴使得溶液的pH为4，混合均匀，加入0.5g硫酸镁；第四步将第一步准备好的样品放入第三步配置好的溶液当中，将溶液放到80℃的水浴中加热5个小时；第五步将第四步充分反应后的白色样品取出，用去离子水，体积比为1：1的无水乙醇-丙酮混合溶剂清洗，重复清洗三次，最后将清洗后的样品用冷冻干燥机在-30℃冻干12小时。
将制得的样品按照ASTM D570-98测得吸水率为900％，按照GB/T 8942-2016测得柔软度为20mN，按照GB/T21655.1—2008测得水分蒸发速率10.5g/h。
实施例2
第一步取20根蔺草，将蔺草剪成80mm，在60℃的烘箱中烘10小时后取出备用；第二步配置1∶1(摩尔比)氯化胆碱和草酸的混合溶液，；第三步将第二步中的溶液90℃下加热1小时，以产生透明和均匀的溶液。第四步将第一步准备好的蔺草放入第三步的溶液中，加入0.5g硫酸镁，80℃加热5小时；第五步将第四步充分反应后的蔺草取出，用去离子水，体积比为1：1的无水乙醇-丙酮混合溶剂清洗，重复清洗三次，最后将清洗后的样品用冷冻干燥机在-30℃冻干12小时。
将制得的样品按照ASTM D570-98测得吸水率为530％，按照GB/T 8942测得柔软度为41mN,按照GB/T21655.1—2008测得水分蒸发速率6.1g/h。
实施例3
第一步取20根蔺草，将蔺草剪成80mm，在60℃的烘箱中烘10小时后取出备用；第二步配置2mol·L-1的氢氧化钠溶液和0.4mol·L-1的亚硫酸钠溶液；第三步将第二步的两种溶液混合水浴加热到80℃，将第一步的样品加入混合溶液当中，加入0.5g硫酸镁，加热5小时；第四步将第三步充分反应后的蔺草取出，用去离子水，体积比为1：1的无水乙醇-丙酮混合溶剂清洗，重复清洗三次，最后将清洗后的样品用冷冻干燥机在-30℃冻干12小时。
将制得的样品按照ASTM D570-98测得吸水率为360％，按照GB/T 8942测得柔软度为32mN，按照GB/T21655.1—2008测得水分蒸发速率5.7g/h。
实施例4
第一步取20根蔺草，将蔺草剪成80mm，在60℃的烘箱中烘10小时后取出备用；第二步配置30％的双氧水溶液；第三步将第一步制备好的蔺草置于双氧水溶液上方，用双氧水蒸汽处理蔺草3小时；第四步将第三步充分反应后的蔺草取出，用去离子水，体积比为1：1的无水乙醇-丙酮混合溶剂清洗，重复清洗三次，最后将清洗后的样品用冷冻干燥机在-30℃冻干12小时。
将制得的样品按照ASTM D570-98测得吸水率为260％，按照GB/T 8942测得柔软度为35mN，按照GB/T21655.1—2008测得水分蒸发速率4.5g/h。
| 吸水率(g/min) | |
| 原始蔺草 | 0.1-0.2 |
| 亚氯酸钠法处理的蔺草 | 2.0-2.3 |
| 氢氧化钠法处理的蔺草 | 1.5-1.9 |
| 氯化胆碱法处理的蔺草 | 1.0-1.6 |
| 双氧水法处理的蔺草 | 1.2-1.7 |
表1.各种蔺草的吸水率。
Claims (9)
1.一种柔韧吸水蔺草纤维材料的制备方法，其特征在于，包括以下步骤：
(1)先将样品剪成一小段，在烘箱中干燥一段时间后，取出备用；
(2)配置反应所需要的混合溶液，将样品放入溶液中，再加硫酸镁，密封条件下加热；
(3)反应结束后除去反应液，清洗，干燥；
(4)原始纤维材料柔韧性差，吸水性差，处理后的材料柔韧性和吸水性得到显著提高。
2.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(1)中，样品长度剪成50-100mm，烘箱温度为50-100℃，干燥时间为10-24小时。
3.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(2)中，混合溶液可以是亚氯酸钠和冰醋酸或者氢氧化钠和亚硫酸钠或者氯化胆碱和草酸或者双氧水溶液。
4.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(2)中，混合溶液可以是质量分数为1-10％亚氯酸钠溶液冰醋酸的添加量为使溶液的pH值为2-5或者1-3mol/L的氢氧化钠和0.1-1mol/L的亚硫酸钠溶液或者1:1-1:5(摩尔比)氯化胆碱和草酸的混合溶液或者20wt％的双氧水溶液，所加硫酸镁的质量为0.5-1g。
5.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(2)中加热温度为50-100℃，反应时间为5-10小时。
6.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(2)中将样品浸没于混合液中，反应至样品变为白色。
7.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(3)中反应结束后依次用去离子水，无水乙醇及丙酮清洗，或者依次用去离子水，体积比为1：1的无水乙醇-丙酮混合溶剂清洗，重复清洗三次。
8.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(3)中清洗后的样品用冷冻干燥机在-10℃—-50℃冻干12-36小时。
9.如权利要求1所述的柔韧吸水蔺草纤维材料的制备方法，其特征在于，步骤(4)中该材料的原始结构为双层多孔中空结构，柔韧性和吸水性都较差，柔韧性为70-90mN,吸水率为0.1-0.2g/min；其主要成分是纤维素，半纤维素含量(15-20％)和木质素含量(25-30％)，经过处理后半纤维素和木质素的含量降低，分别为7-14％，5-10％。
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