CN117338989B - 一种全汉麻纤维抗菌卫生巾及其制备方法 - Google Patents

一种全汉麻纤维抗菌卫生巾及其制备方法 Download PDF

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CN117338989B
CN117338989B CN202311396411.2A CN202311396411A CN117338989B CN 117338989 B CN117338989 B CN 117338989B CN 202311396411 A CN202311396411 A CN 202311396411A CN 117338989 B CN117338989 B CN 117338989B
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hemp
hemp fiber
china
water
solution
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CN117338989A (zh
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李娟�
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Tianzhicao Biological Medicine Hunan Co ltd
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Tianzhicao Biological Medicine Hunan Co ltd
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Abstract

本发明公开了一种全汉麻纤维抗菌卫生巾及其制备方法,涉及卫生巾技术领域;所述全汉麻纤维抗菌卫生巾由表层、吸收层和底层组成,所述表层为改性的汉麻纤维布,吸收层为功能性汉麻纤维气凝胶,底层为汉麻纤维布;汉麻纤维与汉麻蛋白在交联剂作用下形成了多孔、高粘结的纤维连接结构,使气凝胶具有快速解析液体的能力,增加液体的吸收量及吸收速度,有效减少侧漏;汉麻蛋白较好的吸水性、乳化性,有利于气凝胶对经血的吸收,还可缓解经期疼痛,减少炎症、过敏反应的发生;改性的汉麻纤维布有效去除了纤维网状结构中的堵塞物质,增加氧气含量,不利于厌氧菌的生长,因而最大程度的保留了汉麻纤维的抗菌性。

Description

一种全汉麻纤维抗菌卫生巾及其制备方法
技术领域
本发明属于卫生巾技术领域,具体是指一种全汉麻纤维抗菌卫生巾及其制备方法。
背景技术
卫生巾是女性经期使用的一种卫生用品,其主要材料是由棉花、无纺布、纸浆或上述材料制成的高分子或高分子复合纸,其侧边设计用于防止侧漏,从里到外分为三层:表层、吸收芯和底层;随着健康护理意识和消费能力不断提升,女性消费者更注重卫生巾的产品品质、功能性、材料安全性和产品体验感,越来越多的女性开始为因生理构造和生理期带来的一系列“隐秘”的苦痛发声,进而卫生巾市场不断地创造出全新的赛道,比如,如何帮助女性轻松度过经期,远离痛经和经血引起的炎症苦恼。
汉麻纤维是天然纤维中韧度高、可自然分解的环保纤维,具有抗霉抑菌作用,对金黄色葡萄球菌、绿脓杆菌、大肠杆菌、白色念珠菌有明显的抑菌效果;汉麻纤维中心有一个细长的空腔与纤维表面分布着的许多裂纹和小孔相连,优异的毛细效应使汉麻纤维具有良好的吸湿透气性,因而以汉麻纤维为材料制作的卫生巾,不仅具备优良的抗菌性、吸湿透气性,而且更好的满足了市场对“天然”、“可持续”产品的需求。
目前现有技术主要存在以下问题:
汉麻纤维具有天然的抗菌抑菌性能,但目前市面上销售的汉麻纤维类产品,其抗菌效果不佳,未能达到消费者的抗菌需求;同时,汉麻纤维吸收液体能力一般,容易导致侧漏。
发明内容
针对上述情况,为克服现有技术的缺陷,本发明提出了一种全汉麻纤维抗菌卫生巾,所述全汉麻纤维抗菌卫生巾由表层、吸收层和底层组成,所述表层为改性的汉麻纤维布,吸收层为功能性汉麻纤维气凝胶,底层为汉麻纤维布。
优选地,所述表层和底层,包括如下重量份的组份:汉麻纤维70-80份。
优选地,所述功能性汉麻纤维气凝胶,包括如下重量份的组份:汉麻纤维40-50份,汉麻蛋白30-50份,聚酰胺-环氧氯丙烷树脂30-40份。
所述功能性汉麻纤维气凝胶的制备方法,具体包括以下步骤:
S1、将汉麻纤维粉碎后加入体积分数为10%氢氧化钠溶液中,调至pH为8-9,提取温度35-45℃,提取时间50-70min,收集上清液,向上清液中加入体积分数为10%的盐酸溶液调至pH为4.5-5,在25℃水浴中缓慢搅拌5min,离心,离心转速1000-3000rpm,离心时间10-15min,弃去上清液,收集沉淀凝乳,将沉淀凝乳用去离子水洗脱调至pH为7,得到洗脱液,减压浓缩,干燥,温度40-50℃,时间20-30min,得到汉麻蛋白;
S2、将汉麻纤维从茎上剥离,按照重量比1:(20-25)加入体积分数为5%的氢氧化钠溶液中脱去木质素,去离子水洗脱调至pH为7,再进行高速机械混合,旋转速度为3000-5000rpm,混合时间20-30min,得到汉麻纤维悬浮液;
S3、将二乙烯三胺、己二酸与水加入四颈瓶中,通入氮气保护,反应过程中用集水器排除副产物水,控制反应温度160-180℃,反应时间100-120min,反应结束后加入与获得产物同等重量的水,得到聚酰胺溶液,再将聚酰胺溶液加入四颈瓶中,通入氮气保护,向四颈瓶中滴加环氧氯丙烷溶液,调节pH至4-5,控制反应温度50-70℃,反应时间60-70min,得到聚酰胺-环氧氯丙烷树脂;
S4、将步骤S3所述的聚酰胺-环氧氯丙烷树脂加入步骤S2所述的汉麻纤维悬浮液中,搅拌15min,加入步骤S1所述的汉麻蛋白,温度控制45-55℃,搅拌50-60min,再进行高压均质,得到均匀悬浮液;
S5、将步骤S4所述的均匀悬浮液冷冻,冷冻温度-60至-50℃,冷冻时间6-8h,再进行冷冻干燥,冷冻干燥真空度5-10Pa,冷冻干燥温度-80至-40℃,冷冻干燥时间12-24h,得到功能性汉麻纤维气凝胶;
优选地,步骤S1中,汉麻纤维与氢氧化钠溶液的重量比为1:(10-20);
优选地,步骤S3中,二乙烯三胺、己二酸与水的重量比为2:5:(0.2-0.5);聚酰胺溶液与环氧氯丙烷溶液的重量比为1:(1.2-1.5);
优选地,步骤S4中,高压均质法过程中,均质压力600-800bar,均质时间2-3min。
本方案还提供了一种全汉麻纤维抗菌卫生巾的制备方法,具体包括以下步骤:
(1)将汉麻纤维加入水中,进行超声预处理,按照重量比1:30将预处理后的汉麻纤维加入体积分数为3%-8%的草酸铵溶液中,在100℃处理50min,在60℃温水中搓洗10min,取出经草酸铵处理后的汉麻纤维,再按照重量比1:30放入体积分数为5%的酸性果胶酶溶液中,在50℃条件下保温60min,在60℃温水中搓洗10min,取出经酸性果胶酶溶液处理后的汉麻纤维,最后按照重量比1:30再放入甘露聚糖酶和木聚糖酶混合溶液中,其中,甘露聚糖酶的体积分数为3%,木聚糖酶的体积分数为2%,在55℃条件下保温60min,在60℃温水中搓洗10min,取出汉麻纤维,烘干,通过水刺工艺常规制作纤维布,得到改性的汉麻纤维布;
(2)将步骤(1)所述的改性的汉麻纤维布与功能性汉麻纤维气凝胶压实后分切,凹道成型,覆上通过水刺工艺常规制得的汉麻纤维布作为底层,粘贴背翼离型纸,周封定型,外切成形,覆包膜及快易贴,横封、切断,得到全汉麻纤维抗菌卫生巾;
优选地,步骤(1)中,汉麻纤维与水的重量比为1:(10-20);
优选地,步骤(1)中,超声预处理过程中,超声温度25-40℃,超声频率20-40KHz,超声功率600-800W,超声时间20-30min;
优选地,步骤(1)中,酸性果胶酶溶液中果胶酶的酶活力为16000U/g;甘露聚糖酶和木聚糖酶混合溶液中,甘露聚糖酶的酶活力为10000U/g,木聚糖酶的酶活力为10000U/g。
本发明取得的有益效果如下:
本发明通过在改性的汉麻纤维布和汉麻纤维布中间,放置功能性汉麻纤维气凝胶作为吸收层,提高了卫生巾快速吸收液体的能力,有效改善侧漏,并且具有较强的抗菌性;所述功能性汉麻纤维气凝胶中,汉麻纤维与汉麻蛋白在交联剂作用下形成了多孔、高粘结的纤维连接结构,具有超轻、超弹性和柔软的性质,在各个方向均表现出良好的弹性,紧密贴合身体曲线,不易变形,同时高弹性多孔结构使气凝胶具有快速解析液体的能力,增加了液体的吸收量及吸收速度,表现出优异的液体吸收能力,有效减少侧漏;汉麻蛋白较好的吸水性、乳化性,有利于气凝胶对经血的吸收量和吸收速度,汉麻蛋白还是一种抗炎、抗过敏的蛋白质,具有缓解痛经、控制经期暴躁情绪的作用,丰富了气凝胶的功能性,气凝胶的超弹性有利于汉麻蛋白全面紧密贴合身体,更好的发挥作用,缓解经期疼痛造成的不适感,减少炎症、过敏反应的发生;卫生巾表层为草酸铵-复合酶改性的汉麻纤维布,有效去除了纤维网状结构中的堵塞物质,增加氧气含量,不利于厌氧菌的生长,因而最大程度的保留了汉麻纤维的抗菌性,使卫生巾具有较强的抗菌性;卫生巾底层为汉麻纤维布,吸湿透气,舒适凉爽,使用感极佳;本发明以改性的汉麻纤维布,功能性汉麻纤维气凝胶及汉麻纤维布制成一种全汉麻纤维抗菌卫生巾,提高了快速吸收液体的能力,有效改善侧漏,不仅具有较强的抗菌性,还具有缓解痛经的功能性。
附图说明
图1为本发明实施例1所制备的功能性汉麻纤维气凝胶的扫描电镜图;
图2为本发明实施例1-4和对比例1-3的吸收时间结果图;
图3为本发明实施例1-4和对比例1-3的菌落总数结果图;
图4为本发明实施例1-4和对比例1-3的痛经缓解情况结果图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例;基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
除非另行定义,文中所使用的所有专业与科学用语与本领域技术人员所熟悉的意义相同。此外,任何与所记载内容相似或均等的方法及材料皆可应用于本发明中。文中所述的较佳实施方法与材料仅作示范之用,但不能限制本申请的内容。
下述实施例中的实验方法,如无特殊说明,均为常规方法;下述实施例中所用的试验材料,如无特殊说明,均为从商业渠道购买得到的。
实施例中所用试剂的来源如下:
氢氧化钠CASNo:1310-73-2,品牌Innochem,货号A36865;
盐酸CASNo:7647-01-0,品牌Innochem,货号I11253;
二乙烯三胺CASNo:111-40-0,品牌Innochem,货号A41119;
己二酸CASNo:124-04-9,品牌Innochem,货号A33263;
氮气CASNo:无,品牌Ierm,货号GSB07-1412-2001;
环氧氯丙烷CASNo:106-89-8,品牌Innochem,货号A18396;
草酸铵CASNo:6009-70-7,品牌Innochem,货号A89979;
果胶酶CASNo:9033-35-6,品牌复申生物,货号FS1259;
甘露聚糖酶CASNo:37288-54-3,品牌源叶,货号S27580;
木聚糖酶CASNo:9025-57-4,品牌Macklin,货号X875255。
实施例1
本实施例提出了一种全汉麻纤维抗菌卫生巾,全汉麻纤维抗菌卫生巾由表层、吸收层和底层组成,表层为改性的汉麻纤维布,吸收层为功能性汉麻纤维气凝胶,底层为汉麻纤维布。
表层和底层,包括如下重量份的组份:汉麻纤维80份。
功能性汉麻纤维气凝胶,包括如下重量份的组份:汉麻纤维50份,汉麻蛋白50份,聚酰胺-环氧氯丙烷树脂40份。
功能性汉麻纤维气凝胶的制备方法,具体包括以下步骤:
S1、将汉麻纤维粉碎后加入体积分数为10%氢氧化钠溶液中,汉麻纤维与氢氧化钠溶液的重量比为1:20,调至pH为9,提取温度45℃,提取时间70min,收集上清液,向上清液中加入体积分数为10%的盐酸溶液调至pH为5,在25℃水浴中缓慢搅拌5min,离心,离心转速3000rpm,离心时间15min,弃去上清液,收集沉淀凝乳,将沉淀凝乳用去离子水洗脱调至pH为7,得到洗脱液,减压浓缩,干燥,温度50℃,时间30min,得到汉麻蛋白;
S2、将汉麻纤维从茎上剥离,按照重量比1:25加入体积分数为5%的氢氧化钠溶液中脱去木质素,去离子水洗脱调至pH为7,再进行高速机械混合,旋转速度为5000rpm,混合时间30min,得到汉麻纤维悬浮液;
S3、将二乙烯三胺、己二酸与水加入四颈瓶中,二乙烯三胺、己二酸与水的重量比为2:5:0.5,通入氮气保护,反应过程中用集水器排除副产物水,控制反应温度180℃,反应时间120min,反应结束后加入与获得产物同等重量的水,得到聚酰胺溶液,再将聚酰胺溶液加入四颈瓶中,通入氮气保护,向四颈瓶中滴加环氧氯丙烷溶液,聚酰胺溶液与环氧氯丙烷溶液的重量比为1:1.5,调节pH至5,控制反应温度70℃,反应时间70min,得到聚酰胺-环氧氯丙烷树脂;
S4、将步骤S3所述的聚酰胺-环氧氯丙烷树脂加入步骤S2所述的汉麻纤维悬浮液中,搅拌15min,加入步骤S1所述的汉麻蛋白,温度控制55℃,搅拌60min,再进行高压均质,高压均质法过程中,均质压力800bar,均质时间3min,得到均匀悬浮液;
S5、将步骤S4所述的均匀悬浮液冷冻,冷冻温度-50℃,冷冻时间8h,再进行冷冻干燥,冷冻干燥真空度10Pa,冷冻干燥温度-40℃,冷冻干燥时间24h,得到功能性汉麻纤维气凝胶。
本实施例提供一种全汉麻纤维抗菌卫生巾的制备方法,具体包括以下步骤:
(1)将汉麻纤维加入水中,汉麻纤维与水的重量比为1:20,进行超声预处理,超声预处理过程中,超声温度40℃,超声频率40KHz,超声功率800W,超声时间30min,按照重量比1:30将预处理后的汉麻纤维加入体积分数为8%的草酸铵溶液中,在100℃处理50min,在60℃温水中搓洗10min,取出经草酸铵处理后的汉麻纤维,再按照重量比1:30放入体积分数为5%的酸性果胶酶溶液中,酸性果胶酶溶液中果胶酶的酶活力为16000U/g,在50℃条件下保温60min,在60℃温水中搓洗10min,取出经酸性果胶酶溶液处理后的汉麻纤维,最后按照重量比1:30再放入甘露聚糖酶和木聚糖酶混合溶液中,其中,甘露聚糖酶的体积分数为3%,木聚糖酶的体积分数为2%,甘露聚糖酶和木聚糖酶混合溶液中,甘露聚糖酶的酶活力为10000U/g,木聚糖酶的酶活力为10000U/g,在55℃条件下保温60min,在60℃温水中搓洗10min,取出汉麻纤维,烘干,通过水刺工艺常规制作纤维布,得到改性的汉麻纤维布;
(2)将步骤(1)所述的改性的汉麻纤维布与功能性汉麻纤维气凝胶压实后分切,凹道成型,覆上通过水刺工艺常规制得的汉麻纤维布作为底层,粘贴背翼离型纸,周封定型,外切成形,覆包膜及快易贴,横封、切断,得到全汉麻纤维抗菌卫生巾。
本实施例对所制备的功能性汉麻纤维气凝胶进行扫描电镜,观察其微观形貌,图1为实施例1所制备的功能性汉麻纤维气凝胶的SEM图像,如图,本实施例制备的功能性汉麻纤维气凝胶为一种有粘性的多孔载体。
实施例2
本实施例提出了一种全汉麻纤维抗菌卫生巾,全汉麻纤维抗菌卫生巾由表层、吸收层和底层组成,表层为改性的汉麻纤维布,吸收层为功能性汉麻纤维气凝胶,底层为汉麻纤维布。
表层和底层,包括如下重量份的组份:汉麻纤维70份。
功能性汉麻纤维气凝胶,包括如下重量份的组份:汉麻纤维40份,汉麻蛋白30份,聚酰胺-环氧氯丙烷树脂30份。
功能性汉麻纤维气凝胶的制备方法,具体包括以下步骤:
S1、将汉麻纤维粉碎后加入体积分数为10%氢氧化钠溶液中,汉麻纤维与氢氧化钠溶液的重量比为1:10,调至pH为8,提取温度35℃,提取时间50min,收集上清液,向上清液中加入体积分数为10%的盐酸溶液调至pH为4.5,在25℃水浴中缓慢搅拌5min,离心,离心转速1000rpm,离心时间10min,弃去上清液,收集沉淀凝乳,将沉淀凝乳用去离子水洗脱调至pH为7,得到洗脱液,减压浓缩,干燥,温度40℃,时间20min,得到汉麻蛋白;
S2、将汉麻纤维从茎上剥离,按照重量比1:20加入体积分数为5%的氢氧化钠溶液中脱去木质素,去离子水洗脱调至pH为7,再进行高速机械混合,旋转速度为3000rpm,混合时间20min,得到汉麻纤维悬浮液;
S3、将二乙烯三胺、己二酸与水加入四颈瓶中,二乙烯三胺、己二酸与水的重量比为2:5:0.2,通入氮气保护,反应过程中用集水器排除副产物水,控制反应温度160℃,反应时间100min,反应结束后加入与获得产物同等重量的水,得到聚酰胺溶液,再将聚酰胺溶液加入四颈瓶中,通入氮气保护,向四颈瓶中滴加环氧氯丙烷溶液,聚酰胺溶液与环氧氯丙烷溶液的重量比为1:1.2,调节pH至4,控制反应温度50℃,反应时间60min,得到聚酰胺-环氧氯丙烷树脂;
S4、将步骤S3所述的聚酰胺-环氧氯丙烷树脂加入步骤S2所述的汉麻纤维悬浮液中,搅拌15min,加入步骤S1所述的汉麻蛋白,温度控制45℃,搅拌50min,再进行高压均质,高压均质法过程中,均质压力600bar,均质时间2min,得到均匀悬浮液;
S5、将步骤S4所述的均匀悬浮液冷冻,冷冻温度-60℃,冷冻时间6h,再进行冷冻干燥,冷冻干燥真空度5Pa,冷冻干燥温度-80℃,冷冻干燥时间12h,得到功能性汉麻纤维气凝胶。
本实施例提供一种全汉麻纤维抗菌卫生巾的制备方法,具体包括以下步骤:
(1)将汉麻纤维加入水中,汉麻纤维与水的重量比为1:10,进行超声预处理,超声预处理过程中,超声温度25℃,超声频率20KHz,超声功率600W,超声时间20min,按照重量比1:30将预处理后的汉麻纤维加入体积分数为3%的草酸铵溶液中,在100℃处理50min,在60℃温水中搓洗10min,取出经草酸铵处理后的汉麻纤维,再按照重量比1:30放入体积分数为5%的酸性果胶酶溶液中,酸性果胶酶溶液中果胶酶的酶活力为16000U/g,在50℃条件下保温60min,在60℃温水中搓洗10min,取出经酸性果胶酶溶液处理后的汉麻纤维,最后按照重量比1:30再放入甘露聚糖酶和木聚糖酶混合溶液中,其中,甘露聚糖酶的体积分数为3%,木聚糖酶的体积分数为2%,甘露聚糖酶和木聚糖酶混合溶液中,甘露聚糖酶的酶活力为10000U/g,木聚糖酶的酶活力为10000U/g,在55℃条件下保温60min,在60℃温水中搓洗10min,取出汉麻纤维,烘干,通过水刺工艺常规制作纤维布,得到改性的汉麻纤维布;
(2)将步骤(1)所述的改性的汉麻纤维布与功能性汉麻纤维气凝胶压实后分切,凹道成型,覆上通过水刺工艺常规制得的汉麻纤维布作为底层,粘贴背翼离型纸,周封定型,外切成形,覆包膜及快易贴,横封、切断,得到全汉麻纤维抗菌卫生巾。
实施例3
本实施例提出了一种全汉麻纤维抗菌卫生巾,全汉麻纤维抗菌卫生巾由表层、吸收层和底层组成,表层为改性的汉麻纤维布,吸收层为功能性汉麻纤维气凝胶,底层为汉麻纤维布。
表层和底层,包括如下重量份的组份:汉麻纤维75份。
功能性汉麻纤维气凝胶,包括如下重量份的组份:汉麻纤维45份,汉麻蛋白40份,聚酰胺-环氧氯丙烷树脂35份。
功能性汉麻纤维气凝胶的制备方法,具体包括以下步骤:
S1、将汉麻纤维粉碎后加入体积分数为10%氢氧化钠溶液中,汉麻纤维与氢氧化钠溶液的重量比为1:20,调至pH为9,提取温度45℃,提取时间50min,收集上清液,向上清液中加入体积分数为10%的盐酸溶液调至pH为5,在25℃水浴中缓慢搅拌5min,离心,离心转速3000rpm,离心时间10min,弃去上清液,收集沉淀凝乳,将沉淀凝乳用去离子水洗脱调至pH为7,得到洗脱液,减压浓缩,干燥,温度50℃,时间20min,得到汉麻蛋白;
S2、将汉麻纤维从茎上剥离,按照重量比1:25加入体积分数为5%的氢氧化钠溶液中脱去木质素,去离子水洗脱调至pH为7,再进行高速机械混合,旋转速度为5000rpm,混合时间20min,得到汉麻纤维悬浮液;
S3、将二乙烯三胺、己二酸与水加入四颈瓶中,二乙烯三胺、己二酸与水的重量比为2:5:0.5,通入氮气保护,反应过程中用集水器排除副产物水,控制反应温度180℃,反应时间100min,反应结束后加入与获得产物同等重量的水,得到聚酰胺溶液,再将聚酰胺溶液加入四颈瓶中,通入氮气保护,向四颈瓶中滴加环氧氯丙烷溶液,聚酰胺溶液与环氧氯丙烷溶液的重量比为1:1.5,调节pH至5,控制反应温度70℃,反应时间60min,得到聚酰胺-环氧氯丙烷树脂;
S4、将步骤S3所述的聚酰胺-环氧氯丙烷树脂加入步骤S2所述的汉麻纤维悬浮液中,搅拌15min,加入步骤S1所述的汉麻蛋白,温度控制55℃,搅拌50min,再进行高压均质,高压均质法过程中,均质压力800bar,均质时间2min,得到均匀悬浮液;
S5、将步骤S4所述的均匀悬浮液冷冻,冷冻温度-50℃,冷冻时间6h,再进行冷冻干燥,冷冻干燥真空度10Pa,冷冻干燥温度-40℃,冷冻干燥时间12h,得到功能性汉麻纤维气凝胶。
本实施例提供一种全汉麻纤维抗菌卫生巾的制备方法,具体包括以下步骤:
(1)将汉麻纤维加入水中,汉麻纤维与水的重量比为1:20,进行超声预处理,超声预处理过程中,超声温度40℃,超声频率40KHz,超声功率800W,超声时间20min,按照重量比1:30将预处理后的汉麻纤维加入体积分数为3%-8%的草酸铵溶液中,在100℃处理50min,在60℃温水中搓洗10min,取出经草酸铵处理后的汉麻纤维,再按照重量比1:30放入体积分数为5%的酸性果胶酶溶液中,酸性果胶酶溶液中果胶酶的酶活力为16000U/g,在50℃条件下保温60min,在60℃温水中搓洗10min,取出经酸性果胶酶溶液处理后的汉麻纤维,最后按照重量比1:30再放入甘露聚糖酶和木聚糖酶混合溶液中,其中,甘露聚糖酶的体积分数为3%,木聚糖酶的体积分数为2%,甘露聚糖酶和木聚糖酶混合溶液中,甘露聚糖酶的酶活力为10000U/g,木聚糖酶的酶活力为10000U/g,在55℃条件下保温60min,在60℃温水中搓洗10min,取出汉麻纤维,烘干,通过水刺工艺常规制作纤维布,得到改性的汉麻纤维布;
(2)将步骤(1)所述的改性的汉麻纤维布与功能性汉麻纤维气凝胶压实后分切,凹道成型,覆上通过水刺工艺常规制得的汉麻纤维布作为底层,粘贴背翼离型纸,周封定型,外切成形,覆包膜及快易贴,横封、切断,得到全汉麻纤维抗菌卫生巾。
实施例4
本实施例提出了一种全汉麻纤维抗菌卫生巾,全汉麻纤维抗菌卫生巾由表层、吸收层和底层组成,表层为改性的汉麻纤维布,吸收层为功能性汉麻纤维气凝胶,底层为汉麻纤维布。
表层和底层,包括如下重量份的组份:汉麻纤维70份。
功能性汉麻纤维气凝胶,包括如下重量份的组份:汉麻纤维50份,汉麻蛋白30份,聚酰胺-环氧氯丙烷树脂30份。
功能性汉麻纤维气凝胶的制备方法,具体包括以下步骤:
S1、将汉麻纤维粉碎后加入体积分数为10%氢氧化钠溶液中,汉麻纤维与氢氧化钠溶液的重量比为1:10,调至pH为8,提取温度35℃,提取时间70min,收集上清液,向上清液中加入体积分数为10%的盐酸溶液调至pH为4.5,在25℃水浴中缓慢搅拌5min,离心,离心转速1000rpm,离心时间15min,弃去上清液,收集沉淀凝乳,将沉淀凝乳用去离子水洗脱调至pH为7,得到洗脱液,减压浓缩,干燥,温度40℃,时间30min,得到汉麻蛋白;
S2、将汉麻纤维从茎上剥离,按照重量比1:20加入体积分数为5%的氢氧化钠溶液中脱去木质素,去离子水洗脱调至pH为7,再进行高速机械混合,旋转速度为3000rpm,混合时间30min,得到汉麻纤维悬浮液;
S3、将二乙烯三胺、己二酸与水加入四颈瓶中,二乙烯三胺、己二酸与水的重量比为2:5:0.2,通入氮气保护,反应过程中用集水器排除副产物水,控制反应温度160℃,反应时间120min,反应结束后加入与获得产物同等重量的水,得到聚酰胺溶液,再将聚酰胺溶液加入四颈瓶中,通入氮气保护,向四颈瓶中滴加环氧氯丙烷溶液,聚酰胺溶液与环氧氯丙烷溶液的重量比为1:1.2,调节pH至4,控制反应温度50℃,反应时间70min,得到聚酰胺-环氧氯丙烷树脂;
S4、将步骤S3所述的聚酰胺-环氧氯丙烷树脂加入步骤S2所述的汉麻纤维悬浮液中,搅拌15min,加入步骤S1所述的汉麻蛋白,温度控制45℃,搅拌60min,再进行高压均质,高压均质法过程中,均质压力600bar,均质时间3min,得到均匀悬浮液;
S5、将步骤S4所述的均匀悬浮液冷冻,冷冻温度-60℃,冷冻时间8h,再进行冷冻干燥,冷冻干燥真空度5Pa,冷冻干燥温度-80℃,冷冻干燥时间24h,得到功能性汉麻纤维气凝胶。
本实施例提供一种全汉麻纤维抗菌卫生巾的制备方法,具体包括以下步骤:
(1)将汉麻纤维加入水中,汉麻纤维与水的重量比为1:10,进行超声预处理,超声预处理过程中,超声温度25℃,超声频率20KHz,超声功率600W,超声时间30min,按照重量比1:30将预处理后的汉麻纤维加入体积分数为3%-8%的草酸铵溶液中,在100℃处理50min,在60℃温水中搓洗10min,取出经草酸铵处理后的汉麻纤维,再按照重量比1:30放入体积分数为5%的酸性果胶酶溶液中,酸性果胶酶溶液中果胶酶的酶活力为16000U/g,在50℃条件下保温60min,在60℃温水中搓洗10min,取出经酸性果胶酶溶液处理后的汉麻纤维,最后按照重量比1:30再放入甘露聚糖酶和木聚糖酶混合溶液中,其中,甘露聚糖酶的体积分数为3%,木聚糖酶的体积分数为2%,甘露聚糖酶和木聚糖酶混合溶液中,甘露聚糖酶的酶活力为10000U/g,木聚糖酶的酶活力为10000U/g,在55℃条件下保温60min,在60℃温水中搓洗10min,取出汉麻纤维,烘干,通过水刺工艺常规制作纤维布,得到改性的汉麻纤维布;
(2)将步骤(1)所述的改性的汉麻纤维布与功能性汉麻纤维气凝胶压实后分切,凹道成型,覆上通过水刺工艺常规制得的汉麻纤维布作为底层,粘贴背翼离型纸,周封定型,外切成形,覆包膜及快易贴,横封、切断,得到全汉麻纤维抗菌卫生巾。
对比例1
本对比例提供一种全汉麻纤维抗菌卫生巾,其与实施例1的区别在于全汉麻纤维抗菌卫生巾中不含功能性汉麻纤维气凝胶;全汉麻纤维抗菌卫生巾的制备方法与实施例1相同。
对比例2
本对比例提供一种全汉麻纤维抗菌卫生巾,其与实施例1的区别在于功能性汉麻纤维气凝胶中不包含汉麻蛋白;功能性汉麻纤维气凝胶的制备方法不包括步骤S1;全汉麻纤维抗菌卫生巾的制备方法与实施例1相同。
对比例3
本对比例提供一种全汉麻纤维抗菌卫生巾,其与实施例1的区别在于全汉麻纤维抗菌卫生巾中不包含改性的汉麻纤维布;功能性汉麻纤维气凝胶的制备方法与实施例1相同;全汉麻纤维抗菌卫生巾的制备方法不包括步骤(1)。
实验例1
吸水性实验
测试样品:实施例1-4以及对比例1-3所制备得到的全汉麻纤维抗菌卫生巾。
测试方法:向测试样品上方倾倒125mL的10g/100mL血红蛋白的生理盐水,测试其完全吸收所需要的时间(单位为s)。
图2为实施例1-4和对比例1-3的吸收时间结果图;如图,实施例1-4的吸收时间为4-8s,吸收迅速,说明吸水性较好;对比例1-2的吸收时间为15-17s,吸收较慢,说明吸水性较差;对比例3的吸收时间为6s,吸收迅速,说明吸水性较好;对比例1的全汉麻纤维抗菌卫生巾中不含功能性汉麻纤维气凝胶,不具有多孔、高粘结的纤维连接结构,因而不具有快速吸收液体的能力,导致吸收较慢,吸水性较差;对比例2的功能性汉麻纤维气凝胶中不包含汉麻蛋白,不利于气凝胶对经血的吸收,降低了吸收速度,导致吸收较慢,吸水性较差;对比例3的全汉麻纤维抗菌卫生巾中不包含改性的汉麻纤维布,不影响功能性汉麻纤维气凝胶的吸收能力,从而不影响吸收液体的能力,因此吸收迅速,吸水性较好。
实验例2
抗菌性实验
测试样品:实施例1-4以及对比例1-3所制备得到的全汉麻纤维抗菌卫生巾。
测试方法:向测试样品中倒入含10g/100mL血红蛋白的生理盐水125mL,待其完全吸收后,将所述的卫生巾产品置于封闭环境(37℃,相对湿度为75%),在所述的封闭环境中放置敞口培养的大肠杆菌培养物、白色假丝酵母菌培养物和链球菌培养物,放置8h后,将测试样品的表层剪碎后分散在100mL的去离子水中,浸泡3h,过滤,取1mL试样在37℃下培养48h,测定菌落总数(CFU/mL)。
图3为实施例1-4和对比例1-3的菌落总数结果图;如图,实施例1-4的菌落总数为80-98CFU/mL,均<100CFU/mL,菌落总数较少,说明抗菌性较好;对比例1-2的菌落总数为90-95CFU/mL,均<100CFU/mL,菌落总数较少,说明抗菌性较好;对比例3的菌落总数为298CFU/mL,均>100CFU/mL,菌落总数较多,说明抗菌性较差;对比例1的全汉麻纤维抗菌卫生巾中不含功能性汉麻纤维气凝胶,不影响表层改性的汉麻纤维布的抗菌性,从而不影响抗菌能力,因此菌落总数较少,抗菌性较好;对比例2的功能性汉麻纤维气凝胶中不包含汉麻蛋白,对气凝胶有不利影响,但对表层改性的汉麻纤维布无不良影响,从而不影响抗菌性,因此菌落总数较少,抗菌性较好;对比例3的全汉麻纤维抗菌卫生巾中不包含改性的汉麻纤维布,无法有效去除纤维网状结构中的堵塞物质,降低氧气含量,有益于厌氧菌的生长,导致菌落总数较多,抗菌性较差。
实验例3
缓解痛经的效果实验
测试样品:实施例1-4以及对比例1-3所制备得到的全汉麻纤维抗菌卫生巾。
测试方法:于某医院妇科门诊招募志愿者,所招募的志愿者的条件为:具有痛经病史的女性,年龄分布为15-45岁,共招募志愿者70人,分为7组,每组10人;向每组志愿者派发3个月用量的测试样品,每月每组发放与上月相同的测试样品,每月经期结束后需向实验人员提供缓解痛经的具体情况,3个月后,对痛经缓解情况(具体为缓解痛经效果显著、缓解痛经效果一般、缓解痛经无效果)进行统计分析,标准如下:
痛经程度降低60%-90%,即为缓解痛经效果显著;痛经程度降低20%-50%,即为缓解痛经效果一般;痛经程度降低0%-10%,即为缓解痛经无效果。
图4为实施例1-4和对比例1-3的痛经缓解情况的结果图;如图,实施例1-4缓解痛经效果显著、缓解痛经效果一般、缓解痛经无效果的人数分别为4-7、3-4、0-2人,说明缓解痛经效果较好;对比例1-2缓解痛经效果显著、缓解痛经效果一般、缓解痛经无效果的人数占比分别为0、2-3、7-8人,说明缓解痛经效果一般;对比例3缓解痛经效果显著、缓解痛经效果一般、缓解痛经无效果的人数分别为5、3、2人,说明缓解痛经效果较好;对比例1的全汉麻纤维抗菌卫生巾中不含功能性汉麻纤维气凝胶,不具有功能性汉麻蛋白,也无法紧密贴合身体发挥作用,导致缓解痛经效果较差;对比例2的功能性汉麻纤维气凝胶中不包含汉麻蛋白,不具有抗炎、缓解痛经的作用,导致缓解痛经的效果较差;对比例3的全汉麻纤维抗菌卫生巾中不包含改性的汉麻纤维布,不影响汉麻蛋白发挥缓解痛经的作用,从而不影响缓解痛经的效果,因此缓解痛经的效果较好。
上述实验结果表明,本发明实施例1-4的吸水性、抗菌性及缓解痛经的效果明显优于对比例1-3样品,其中,使用功能性汉麻纤维气凝胶和改性的汉麻纤维布的实施例1的吸水性更好、抗菌性更强及缓解痛经的效果更好,汉麻纤维与汉麻蛋白在交联剂作用下形成了多孔、高粘结的纤维连接结构,具有超轻、超弹性和柔软的性质,使气凝胶具有快速解析液体的能力,增加了液体的吸收量及吸收速度,有效减少侧漏;汉麻蛋白较好的吸水性、乳化性,有利于气凝胶对经血的吸收量和吸收速度,汉麻蛋白还具有缓解痛经、控制经期暴躁情绪的作用,气凝胶的超弹性有利于汉麻蛋白全面紧密贴合身体,更好的发挥作用,缓解经期疼痛造成的不适感,减少炎症、过敏反应的发生;卫生巾表层为草酸铵-复合酶改性的汉麻纤维布,有效去除了纤维网状结构中的堵塞物质,增加氧气含量,不利于厌氧菌的生长,使卫生巾具有较强的抗菌性。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
以上对本发明及其实施方式进行了描述,这种描述没有限制性,附图中所示的也只是本发明的实施方式之一,实际的应用并不局限于此。总而言之如果本领域的普通技术人员受其启示,在不脱离本发明创造宗旨的情况下,不经创造性的设计出与该技术方案相似的方式及实施例,均应属于本发明的保护范围。

Claims (8)

1.一种全汉麻纤维抗菌卫生巾,其特征在于:所述全汉麻纤维抗菌卫生巾由表层、吸收层和底层组成,所述表层为改性的汉麻纤维布,吸收层为功能性汉麻纤维气凝胶,底层为汉麻纤维布;所述表层和底层,包括如下重量份的组份:汉麻纤维70-80份;所述功能性汉麻纤维气凝胶,包括如下重量份的组份:汉麻纤维40-50份,汉麻蛋白30-50份,聚酰胺-环氧氯丙烷树脂30-40份;
所述全汉麻纤维抗菌卫生巾的制备方法,具体包括以下步骤:
(1)将汉麻纤维加入水中,进行超声预处理,按照重量比1:30将预处理后的汉麻纤维加入体积分数为3%-8%的草酸铵溶液中,在100℃处理50min,在60℃温水中搓洗10min,取出经草酸铵处理后的汉麻纤维,再按照重量比1:30放入体积分数为5%的酸性果胶酶溶液中,在50℃条件下保温60min,在60℃温水中搓洗10min,取出经酸性果胶酶溶液处理后的汉麻纤维,最后按照重量比1:30再放入甘露聚糖酶和木聚糖酶混合溶液中,其中,甘露聚糖酶的体积分数为3%,木聚糖酶的体积分数为2%,在55℃条件下保温60min,在60℃温水中搓洗10min,取出汉麻纤维,烘干,通过水刺工艺常规制作纤维布,得到改性的汉麻纤维布;
(2)将步骤(1)所述的改性的汉麻纤维布与功能性汉麻纤维气凝胶压实后分切,凹道成型,覆上通过水刺工艺常规制得的汉麻纤维布作为底层,粘贴背翼离型纸,周封定型,外切成形,覆包膜及快易贴,横封、切断,得到全汉麻纤维抗菌卫生巾。
2.一种如权利要求1所述的全汉麻纤维抗菌卫生巾的制备方法,其特征在于:具体包括以下步骤:
(1)将汉麻纤维加入水中,进行超声预处理,按照重量比1:30将预处理后的汉麻纤维加入体积分数为3%-8%的草酸铵溶液中,在100℃处理50min,在60℃温水中搓洗10min,取出经草酸铵处理后的汉麻纤维,再按照重量比1:30放入体积分数为5%的酸性果胶酶溶液中,在50℃条件下保温60min,在60℃温水中搓洗10min,取出经酸性果胶酶溶液处理后的汉麻纤维,最后按照重量比1:30再放入甘露聚糖酶和木聚糖酶混合溶液中,其中,甘露聚糖酶的体积分数为3%,木聚糖酶的体积分数为2%,在55℃条件下保温60min,在60℃温水中搓洗10min,取出汉麻纤维,烘干,通过水刺工艺常规制作纤维布,得到改性的汉麻纤维布;
(2)将步骤(1)所述的改性的汉麻纤维布与功能性汉麻纤维气凝胶压实后分切,凹道成型,覆上通过水刺工艺常规制得的汉麻纤维布作为底层,粘贴背翼离型纸,周封定型,外切成形,覆包膜及快易贴,横封、切断,得到全汉麻纤维抗菌卫生巾。
3.根据权利要求2所述的全汉麻纤维抗菌卫生巾的制备方法,其特征在于:在步骤(1)中,汉麻纤维与水的重量比为1:10-20;超声预处理过程中,超声温度25-40℃,超声频率20-40KHz,超声功率600-800W,超声时间20-30min。
4.根据权利要求3所述的全汉麻纤维抗菌卫生巾的制备方法,其特征在于:在步骤(1)中,酸性果胶酶溶液中果胶酶的酶活力为16000U/g;甘露聚糖酶和木聚糖酶混合溶液中,甘露聚糖酶的酶活力为10000U/g,木聚糖酶的酶活力为10000U/g。
5.根据权利要求4所述的全汉麻纤维抗菌卫生巾的制备方法,其特征在于:所述功能性汉麻纤维气凝胶的制备方法,具体包括以下步骤:
S1、将汉麻纤维粉碎后加入体积分数为10%氢氧化钠溶液中,调至pH为8-9,提取温度35-45℃,提取时间50-70min,收集上清液,向上清液中加入体积分数为10%的盐酸溶液调至pH为4.5-5,在25℃水浴中缓慢搅拌5min,离心,离心转速1000-3000rpm,离心时间10-15min,弃去上清液,收集沉淀凝乳,将沉淀凝乳用去离子水洗脱调至pH为7,得到洗脱液,减压浓缩,干燥,温度40-50℃,时间20-30min,得到汉麻蛋白;
S2、将汉麻纤维从茎上剥离,按照重量比1:20-25加入体积分数为5%的氢氧化钠溶液中脱去木质素,去离子水洗脱调至pH为7,再进行高速机械混合,旋转速度为3000-5000rpm,混合时间20-30min,得到汉麻纤维悬浮液;
S3、将二乙烯三胺、己二酸与水加入四颈瓶中,通入氮气保护,反应过程中用集水器排除副产物水,控制反应温度160-180℃,反应时间100-120min,反应结束后加入与获得产物同等重量的水,得到聚酰胺溶液,再将聚酰胺溶液加入四颈瓶中,通入氮气保护,向四颈瓶中滴加环氧氯丙烷溶液,调节pH至4-5,控制反应温度50-70℃,反应时间60-70min,得到聚酰胺-环氧氯丙烷树脂;
S4、将步骤S3所述的聚酰胺-环氧氯丙烷树脂加入步骤S2所述的汉麻纤维悬浮液中,搅拌15min,加入步骤S1所述的汉麻蛋白,温度控制45-55℃,搅拌50-60min,再进行高压均质,得到均匀悬浮液;
S5、将步骤S4所述的均匀悬浮液冷冻,冷冻温度-60至-50℃,冷冻时间6-8h,再进行冷冻干燥,冷冻干燥真空度5-10Pa,冷冻干燥温度-80至-40℃,冷冻干燥时间12-24h,得到功能性汉麻纤维气凝胶。
6.根据权利要求5所述的全汉麻纤维抗菌卫生巾的制备方法,其特征在于:在步骤S1中,汉麻纤维与氢氧化钠溶液的重量比为1:10-20。
7.根据权利要求6所述的全汉麻纤维抗菌卫生巾的制备方法,其特征在于:在步骤S3中,二乙烯三胺、己二酸与水的重量比为2:5:0.2-0.5;聚酰胺溶液与环氧氯丙烷溶液的重量比为1:1.2-1.5。
8.根据权利要求7所述的全汉麻纤维抗菌卫生巾的制备方法,其特征在于:在步骤S4中,高压均质法过程中,均质压力600-800bar,均质时间2-3min。
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