CN113774562A - 一种改性纤维素水刺无纺布及其制备方法 - Google Patents
一种改性纤维素水刺无纺布及其制备方法 Download PDFInfo
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Abstract
本发明提出了一种改性纤维素水刺无纺布及其制备方法，属于水刺无纺布技术领域。由以下原料制备而成：改性纤维素、聚丙烯、钛酸四丁酯、去离子水；所述改性纤维素具有以下所示结构；其中，n＝100‑300。本发明制得的改性纤维素水刺无纺布不仅具有良好的抗菌、抑菌性能，还具有一定的甲醛净化能力，亲肤性佳，力学性能好，经过水刺加固后，无纺布中的纤维发生位移、穿插、缠结、抱合，形成无数个柔性缠结点，从而使无纺布得到加固，得到高性能的水刺无纺布。
Description
技术领域
本发明涉及水刺无纺布技术领域，具体涉及一种改性纤维素水刺无纺布及其制备方法。
背景技术
纤维素水刺无纺布以纤维素为原料，经水刺工艺加工而成，由于纤维素来源于植物，且加工过程中不添加化学粘合剂，使得该无纺布具有柔软、亲水、贴肤的特性，广泛应用于面料基布、湿纸巾、医用敷料等场合。
无纺布又称非织造布，是由定向的或随机的纤维而构成。因具有布的外观和某些性能而称其为布。简单的讲就是：它不是由一根一根的纱线交织、编结在一起的，而是将纤维直接通过物理或化学的方法粘合在一起的，所以，当你拿到你衣服里的粘称时，就会发现，是抽不出一根根的线头的。非织造布突破了传统的纺织原理，并具有工艺流程短、生产速率快，产量高、成本低、用途广、原料来源多等特点。与纺织布相比强度和耐久性较差，而且不能像其他布料一样耐清洗。因为纤维按一定方向排列，所以容易从直角方向裂开等等。另外，传统水刺无纺布强力较差，抗拉强度较低，抗菌性较差，为了不改变水刺无纺布的性能的情况下增加非织造布的强力、增加水刺无纺布附加值以及提高无纺布的抗菌性能，有必要提出一种改性水刺无纺布。
专利CN110565264A一种高透明高吸水性纤维素水刺无纺布的制备方法，包括如下步骤：将碱溶性改性纤维素溶解在碱溶液中配制成纤维素原液；将纤维素水刺无纺布置于制备好的纤维素原液中进行浸轧；将浸轧后的纤维素水刺无纺布进行干燥处理；将干燥后的纤维素水刺无纺布进行至少三次水洗，然后用酸溶液进行中和，使中和后的纤维素水刺无纺布的pH为中性；将中和后的纤维素水刺无纺布进行干燥和回潮处理，制得纤维素水刺无纺布成品。具有高透明性和高吸水性，而且其原料均来自于植物，使得纤维素水刺无纺布还具有良好的亲肤性，但是，该水刺无纺布力学性能较差，耐久性不佳。
发明内容
本发明的目的在于提出一种改性纤维素水刺无纺布及其制备方法，具有良好的抗衰老的效果。
本发明的技术方案是这样实现的：
本发明提供一种改性纤维素水刺无纺布，由以下原料制备而成：改性纤维素、聚丙烯、钛酸四丁酯、去离子水；
所述改性纤维素具有如下式Ⅰ所示结构：
其中，n＝100-300。
作为本发明的进一步改进，所述改性纤维素的制备方法如下：
S1.纤维素的处理：将纤维素浸泡在石油醚和乙酸乙酯混合溶剂中1-2h后，过滤，干燥，然后加入含硅烷偶联剂KH550的乙醇水溶液中，滴加氨水调节pH值为8-9，反应0.5-1h，过滤，于120-140℃下干燥0.5-1h，然后置于乙醇中，超声清洗0.5-1h，过滤，干燥，得到表面接枝的纤维素；
S2.中间体的制备：将3-溴丙胺溶于二氯甲烷中，加入步骤S1制得的表面接枝的纤维素，氮气保护下加热至30-50℃，搅拌反应2-4h，过滤，用乙醇洗涤，干燥，得到中间体，具有如式Ⅱ所示结构；
S3.改性纤维素的制备：将中间体加入盐酸溶液中，搅拌反应0.5-1h，过滤，清水洗涤，干燥，得到改性纤维素。
作为本发明的进一步改进，步骤S1中所述石油醚和乙酸乙酯混合溶剂中石油醚和乙酸乙酯的体积比为(3-5)：2；所述含硅烷偶联剂KH550的乙醇水溶液中KH550的含量为3-5wt％，乙醇的含量为35-40wt％，余量为水；所述超声功率为1000-2000W。
作为本发明的进一步改进，步骤S2中所述3-溴丙胺和表面接枝的纤维素的质量比为(2-4)：10。
作为本发明的进一步改进，步骤S3中所述盐酸溶液的物质的量浓度为2-4mol/L。
本发明进一步保护一种上述改性纤维素水刺无纺布的制备方法，包括以下步骤：
(1)混合纤维的制备：将改性纤维素溶解在碱溶液中配制成纤维素原液，另将聚丙烯加入螺杆注塑机中，加热熔融喷丝，在热空气作用下拉伸后，将聚丙烯纤维置于制备好的纤维素原液中进行浸轧，得到混合纤维；
(2)熔喷纱的制备：将混合纤维将毛细喷丝孔喷出的超细纤维经牵伸气流牵引，吹向滚筒，并收集到滚筒上，依靠自身的热黏合成为单层纱；
(3)含层间水的熔喷布的制备：将单层熔喷纱叠放，称重为W1，置于水热反应釜中，超声制得含层间水的熔喷布，烘干，称重为W2，得到含层间水的熔喷布；
(4)TiO2插层熔喷布的制备：以含水量为W2-W1计，以钛酸四丁酯水解方程式为依据加入指定量的钛酸四丁酯；密封条件下超声分散至充分反应；清水清洗后抽滤，水热反应釜中一定温度下反应制得TiO2插层无纺布；
(5)水刺加固：将制得的TiO2插层无纺布送入水刺机加固，进行预加湿处理，在水射流直接冲击和反弹水流的双重作用下，无纺布中的纤维发生位移、穿插、缠结、抱合，形成无数个柔性缠结点，从而使无纺布得到加固，烘干，得到改性纤维素水刺无纺布。
作为本发明的进一步改进，步骤(1)中所述改性纤维素、聚丙烯的质量比为(50-70)：(25-30)；所述碱溶液为浓度为5-15wt％的NaOH溶液或KOH溶液；所述熔融温度为200-220℃。
作为本发明的进一步改进，步骤(3)中所述超声温度为50-60℃，超声功率为1500-2000W，烘干方法为80-100℃烘干0.5-1h。
作为本发明的进一步改进，步骤(4)中所述所述水热反应温度为80-100℃。
作为本发明的进一步改进，步骤(4)所述钛酸四丁酯和水的物质的量之比为1：2。
本发明具有如下有益效果：本发明首先通过水解聚合反应处理硅烷偶联剂KH550，进一步反应在纤维素表面，形成硅烷偶联剂接枝纤维素，同时，硅烷部分水解形成了二氧化硅，能明显提高后续制备的改性纤维素水刺无纺布的力学性能，进一步，连接了3-溴丙胺，经过盐酸质子化后，从而制备了一种具有双季铵盐位点的改性纤维素，具有明显的抗菌效果，将带负电荷的细菌细胞表面吸附在季铵盐位点，然后侵入细胞壁，进一步与细胞膜结合和引起细胞膜破裂，从而起到了广谱抗菌的效果。
本发明制备单层纱，并制备层间含水的熔喷纱，经过烘干后，其层间的水分子与混合纤维结合，不会烘干，进一步与钛酸四丁酯发生水解反应，在层间反应生成二氧化钛，进一步提高了水刺无纺布的光催化抗菌性能以及分解甲醛的性能。
本发明制得的改性纤维素水刺无纺布，首先进行预加湿处理，压实蓬松的无纺布，排除无纺布中的空气，使无纺布进入水刺区后能有效地吸收水射流的能量，以加强纤维缠结效果，进一步经过水刺加固后，无纺布中的纤维发生位移、穿插、缠结、抱合，形成无数个柔性缠结点，从而使无纺布得到加固，得到高性能的水刺无纺布。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1为本发明改性纤维素的合成路线图。
具体实施方式
下面将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。
制备例1改性纤维素
合成路线如图1，制备方法如下：
S1.纤维素的处理：将50g纤维素浸泡在200mL石油醚和乙酸乙酯混合溶剂(石油醚和乙酸乙酯的体积比为3：2)中1h后，过滤，干燥，然后加入100mL含硅烷偶联剂KH550的乙醇水溶液(KH550的含量为3wt％，乙醇的含量为35wt％，余量为水)中，滴加氨水调节pH值为8，反应0.5h，过滤，于120℃下干燥0.5h，然后置于100mL乙醇中，超声清洗0.5h，过滤，干燥，得到表面接枝的纤维素；
S2.中间体的制备：将20g 3-溴丙胺溶于200mL二氯甲烷中，加入100g步骤S1制得的表面接枝的纤维素，氮气保护下加热至30℃，搅拌反应2h，过滤，用乙醇洗涤，干燥，得到中间体；
S3.改性纤维素的制备：将10g中间体加入100mL 2mol/L盐酸溶液中，搅拌反应0.5h，过滤，清水洗涤，干燥，得到改性纤维素。
制备例2改性纤维素
合成路线如图1，制备方法如下：
S1.纤维素的处理：将50g纤维素浸泡在200mL石油醚和乙酸乙酯混合溶剂(石油醚和乙酸乙酯的体积比为5：2)中2h后，过滤，干燥，然后加入100mL含硅烷偶联剂KH550的乙醇水溶液(KH550的含量为5wt％，乙醇的含量为40wt％，余量为水)中，滴加氨水调节pH值为9，反应1h，过滤，于140℃下干燥1h，然后置于100mL乙醇中，超声清洗1h，过滤，干燥，得到表面接枝的纤维素；
S2.中间体的制备：将40g 3-溴丙胺溶于200mL二氯甲烷中，加入100g步骤S1制得的表面接枝的纤维素，氮气保护下加热至50℃，搅拌反应4h，过滤，用乙醇洗涤，干燥，得到中间体；
S3.改性纤维素的制备：将10g中间体加入100mL 4mol/L盐酸溶液中，搅拌反应1h，过滤，清水洗涤，干燥，得到改性纤维素。
制备例3改性纤维素
合成路线如图1，制备方法如下：
S1.纤维素的处理：将50g纤维素浸泡在200mL石油醚和乙酸乙酯混合溶剂(石油醚和乙酸乙酯的体积比为4：2)中1.5h后，过滤，干燥，然后加入100mL含硅烷偶联剂KH550的乙醇水溶液(KH550的含量为4wt％，乙醇的含量为37wt％，余量为水)中，滴加氨水调节pH值为8.5，反应1h，过滤，于130℃下干燥1h，然后置于100mL乙醇中，超声清洗1h，过滤，干燥，得到表面接枝的纤维素；
S2.中间体的制备：将30g 3-溴丙胺溶于200mL二氯甲烷中，加入100g步骤S1制得的表面接枝的纤维素，氮气保护下加热至40℃，搅拌反应3h，过滤，用乙醇洗涤，干燥，得到中间体；
S3.改性纤维素的制备：将10g中间体加入100mL 3mol/L盐酸溶液中，搅拌反应1h，过滤，清水洗涤，干燥，得到改性纤维素。
对比制备例1
与实施例3相比，没有接枝3-溴丙胺，其他条件均不改变。
制备方法如下：
S1.纤维素的处理：将50g纤维素浸泡在200mL石油醚和乙酸乙酯混合溶剂(石油醚和乙酸乙酯的体积比为4：2)中1.5h后，过滤，干燥，然后加入100mL含硅烷偶联剂KH550的乙醇水溶液(KH550的含量为4wt％，乙醇的含量为37wt％，余量为水)中，滴加氨水调节pH值为8.5，反应1h，过滤，于130℃下干燥1h，然后置于100mL乙醇中，超声清洗1h，过滤，干燥，得到表面接枝的纤维素；
S2.改性纤维素的制备：将10g表面接枝的纤维素加入100mL 3mol/L盐酸溶液中，搅拌反应1h，过滤，清水洗涤，干燥，得到改性纤维素。
实施例1改性纤维素水刺无纺布
制备方法包括以下步骤：
(1)混合纤维的制备：将50g制备例1制得的改性纤维素溶解100mL 5wt％在NaOH溶液中配制成纤维素原液，另将25g聚丙烯加入螺杆注塑机中，加热至200℃熔融喷丝，在热空气作用下拉伸后，将聚丙烯纤维置于制备好的纤维素原液中进行浸轧，得到混合纤维；
(2)熔喷纱的制备：将混合纤维将毛细喷丝孔喷出的超细纤维经牵伸气流牵引，吹向滚筒，并收集到滚筒上，依靠自身的热黏合成为单层纱；
(3)含层间水的熔喷布的制备：将单层熔喷纱叠放，称重为18.5g，置于水热反应釜中，超声制得含层间水的熔喷布，超声温度为50℃，超声功率为1500W，80℃烘干0.5h，称重为19.7g，得到含层间水的熔喷布；
(4)TiO2插层熔喷布的制备：以含水量为1.2g计，加入11.4g钛酸四丁酯；密封条件下超声分散至充分反应，水热反应温度为80℃；清水清洗后抽滤，水热反应釜中一定温度下反应制得TiO2插层无纺布；
反应方程式如下：
Ti(OCH2CH2CH2CH3)4+2H2O＝TiO2+4CH3CH2CH2CH2OH
(5)水刺加固：将制得的TiO2插层无纺布送入水刺机加固，进行预加湿处理，在水射流直接冲击和反弹水流的双重作用下，无纺布中的纤维发生位移、穿插、缠结、抱合，形成无数个柔性缠结点，从而使无纺布得到加固，烘干，得到改性纤维素水刺无纺布。
实施例2改性纤维素水刺无纺布
制备方法包括以下步骤：
(1)混合纤维的制备：将70g制备例2制得的改性纤维素溶解100mL 5wt％在NaOH溶液中配制成纤维素原液，另将30g聚丙烯加入螺杆注塑机中，加热至220℃熔融喷丝，在热空气作用下拉伸后，将聚丙烯纤维置于制备好的纤维素原液中进行浸轧，得到混合纤维；
(2)熔喷纱的制备：将混合纤维将毛细喷丝孔喷出的超细纤维经牵伸气流牵引，吹向滚筒，并收集到滚筒上，依靠自身的热黏合成为单层纱；
(3)含层间水的熔喷布的制备：将单层熔喷纱叠放，称重为19.9g，置于水热反应釜中，超声制得含层间水的熔喷布，超声温度为60℃，超声功率为2000W，100℃烘干1h，称重为21.7g，得到含层间水的熔喷布；
(4)TiO2插层熔喷布的制备：以含水量为1.2g计，加入17g钛酸四丁酯；密封条件下超声分散至充分反应，水热反应温度为100℃；清水清洗后抽滤，水热反应釜中一定温度下反应制得TiO2插层无纺布；
(5)水刺加固：将制得的TiO2插层无纺布送入水刺机加固，进行预加湿处理，在水射流直接冲击和反弹水流的双重作用下，无纺布中的纤维发生位移、穿插、缠结、抱合，形成无数个柔性缠结点，从而使无纺布得到加固，烘干，得到改性纤维素水刺无纺布。
实施例3改性纤维素水刺无纺布
制备方法包括以下步骤：
(1)混合纤维的制备：将60g制备例3制得的改性纤维素溶解100mL 5wt％在NaOH溶液中配制成纤维素原液，另将27g聚丙烯加入螺杆注塑机中，加热至210℃熔融喷丝，在热空气作用下拉伸后，将聚丙烯纤维置于制备好的纤维素原液中进行浸轧，得到混合纤维；
(2)熔喷纱的制备：将混合纤维将毛细喷丝孔喷出的超细纤维经牵伸气流牵引，吹向滚筒，并收集到滚筒上，依靠自身的热黏合成为单层纱；
(3)含层间水的熔喷布的制备：将单层熔喷纱叠放，称重为19.1g，置于水热反应釜中，超声制得含层间水的熔喷布，超声温度为55℃，超声功率为1700W，90℃烘干1h，称重为20.7g，得到含层间水的熔喷布；
(4)TiO2插层熔喷布的制备：以含水量为1.2g计，加入15.1g钛酸四丁酯；密封条件下超声分散至充分反应，水热反应温度为90℃；清水清洗后抽滤，水热反应釜中一定温度下反应制得TiO2插层无纺布；
(5)水刺加固：将制得的TiO2插层无纺布送入水刺机加固，进行预加湿处理，在水射流直接冲击和反弹水流的双重作用下，无纺布中的纤维发生位移、穿插、缠结、抱合，形成无数个柔性缠结点，从而使无纺布得到加固，烘干，得到改性纤维素水刺无纺布。
对比例1
与实施例3相比，制备例3制得的改性纤维素由对比制备例1制得的替代，其他条件均不改变。
对比例2
与实施例3相比，制备例3制得的改性纤维素由普通纤维素的替代，其他条件均不改变。
对比例3
与实施例3相比，未添加钛酸四丁酯，其他条件均不改变。
测试例1抗菌抗螨性能测试
将实施例1-3以及对比例1-2制得改性纤维素水刺无纺布采用振荡法(GB/T20944.3-2008)测试。结果见表1。
表1
将实施例1-3以及对比例1-2制得改性纤维素水刺无纺布进行防螨测试，测试指标按照国标GBT24253-2009，结果见表2。
表2
| 组别 | 防螨率(％) |
| 实施例1 | 97 |
| 实施例2 | 98 |
| 实施例3 | 98 |
| 对比例1 | 70 |
| 对比例2 | 52 |
| 对比例3 | 89 |
由上表可知，本发明制得的改性纤维素水刺无纺布具有良好的抗菌、防螨性能。
测试例2性能测试
将实施例1-3以及对比例1-2制得改性纤维素水刺无纺布进行性能测试，按照GB/T21295-2014服装理化性能的技术要求方法检测，结果见表3。
表3
由上表可知，本发明制得的改性纤维素水刺无纺布具有良好的抗菌、防螨性能。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种改性纤维素水刺无纺布，其特征在于，由以下原料制备而成：改性纤维素、聚丙烯、钛酸四丁酯、去离子水；
所述改性纤维素具有如下式Ⅰ所示结构：
其中，n＝100-300。
2.根据权利要求1所述改性纤维素水刺无纺布，其特征在于，所述改性纤维素的制备方法如下：
S1.纤维素的处理：将纤维素浸泡在石油醚和乙酸乙酯混合溶剂中1-2h后，过滤，干燥，然后加入含硅烷偶联剂KH550的乙醇水溶液中，滴加氨水调节pH值为8-9，反应0.5-1h，过滤，于120-140℃下干燥0.5-1h，然后置于乙醇中，超声清洗0.5-1h，过滤，干燥，得到表面接枝的纤维素；
S2.中间体的制备：将3-溴丙胺溶于二氯甲烷中，加入步骤S1制得的表面接枝的纤维素，氮气保护下加热至30-50℃，搅拌反应2-4h，过滤，用乙醇洗涤，干燥，得到中间体，具有如式Ⅱ所示结构；
S3.改性纤维素的制备：将中间体加入盐酸溶液中，搅拌反应0.5-1h，过滤，清水洗涤，干燥，得到改性纤维素。
3.根据权利要求2所述改性纤维素水刺无纺布，其特征在于，步骤S1中所述石油醚和乙酸乙酯混合溶剂中石油醚和乙酸乙酯的体积比为(3-5)：2；所述含硅烷偶联剂KH550的乙醇水溶液中KH550的含量为3-5wt％，乙醇的含量为35-40wt％，余量为水；所述超声功率为1000-2000W。
4.根据权利要求2所述改性纤维素水刺无纺布，其特征在于，步骤S2中所述3-溴丙胺和表面接枝的纤维素的质量比为(2-4)：10。
5.根据权利要求2所述改性纤维素水刺无纺布，其特征在于，步骤S3中所述盐酸溶液的物质的量浓度为2-4mol/L。
6.一种如权利要求1-5任一项所述改性纤维素水刺无纺布的制备方法，其特征在于，包括以下步骤：
(1)混合纤维的制备：将改性纤维素溶解在碱溶液中配制成纤维素原液，另将聚丙烯加入螺杆注塑机中，加热熔融喷丝，在热空气作用下拉伸后，将聚丙烯纤维置于制备好的纤维素原液中进行浸轧，得到混合纤维；
(2)熔喷纱的制备：将混合纤维将毛细喷丝孔喷出的超细纤维经牵伸气流牵引，吹向滚筒，并收集到滚筒上，依靠自身的热黏合成为单层纱；
(3)含层间水的熔喷布的制备：将单层熔喷纱叠放，称重为W1，置于水热反应釜中，超声制得含层间水的熔喷布，烘干，称重为W2，得到含层间水的熔喷布；
(4)TiO2插层熔喷布的制备：以含水量为W2-W1计，以钛酸四丁酯水解方程式为依据加入指定量的钛酸四丁酯；密封条件下超声分散至充分反应；清水清洗后抽滤，水热反应釜中一定温度下反应制得TiO2插层无纺布；
(5)水刺加固：将制得的TiO2插层无纺布送入水刺机加固，进行预加湿处理，在水射流直接冲击和反弹水流的双重作用下，纤网中的纤维发生位移、穿插、缠结、抱合，形成无数个柔性缠结点，从而使纤网得到加固，烘干，得到改性纤维素水刺无纺布。
7.根据权利要求6所述的制备方法，其特征在于，步骤(1)中所述改性纤维素、聚丙烯的质量比为(50-70)：(25-30)；所述碱溶液为浓度为5-15wt％的NaOH溶液或KOH溶液；所述熔融温度为200-220℃。
8.根据权利要求6所述的制备方法，其特征在于，步骤(3)中所述超声温度为50-60℃，超声功率为1500-2000W，烘干方法为80-100℃烘干0.5-1h。
9.根据权利要求6所述的制备方法，其特征在于，步骤(4)中所述所述水热反应温度为80-100℃。
10.根据权利要求6所述的制备方法，其特征在于，步骤(4)所述钛酸四丁酯和水的物质的量之比为1：2。
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