CN107326534A - 一种石墨烯微米银丝复合抗菌无纺布及其制作方法 - Google Patents

一种石墨烯微米银丝复合抗菌无纺布及其制作方法 Download PDF

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CN107326534A
CN107326534A CN201710515195.7A CN201710515195A CN107326534A CN 107326534 A CN107326534 A CN 107326534A CN 201710515195 A CN201710515195 A CN 201710515195A CN 107326534 A CN107326534 A CN 107326534A
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graphene
filamentary silver
spinning
woven fabrics
composite antibacterial
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张梓晗
吕鹏
张运奇
聂彪
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Hefei Yinpai Technology Co Ltd
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
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    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
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    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D01F1/103—Agents inhibiting growth of microorganisms
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
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Abstract

本发明公开了一种石墨烯微米银丝复合抗菌无纺布及其制作方法，其是由聚合物纤维经静电纺丝制成，在聚合物纤维中均匀嵌入有石墨烯和微米银丝。本发明制备的石墨烯微米银丝复合抗菌无纺布，其中的微米银丝不易脱落，对白色念珠菌、黑曲霉的抑制率能够达到99％，具有高效抑菌作用；且由于石墨烯的加入，极大地提高了无纺布的防静电能力和机械强度。

Description

一种石墨烯微米银丝复合抗菌无纺布及其制作方法
技术领域
本发明涉及抗菌无纺布领域，尤其涉及一种石墨烯微米银丝复合抗菌无纺布。
背景技术
无纺布由于其重量轻、可降解、成本低等优点，被广泛用于纺织、医疗等领域。随着社会经济的发展、基本科学素质的普及，人们对生活质量的要求越来越高，对日常生活中必须品的要求也越来越高，其中抗菌就是一项重要内容。
银作为一种抗菌材料受到广泛认可，而石墨烯也有报道其抗菌性。在现有技术中，银作为抗菌材料使用时有纳米银线、纳米银颗粒或者蒸镀的银膜三种形态。前两种形态中银的尺寸都非常小，用于纺织或医疗用品时极易通过皮肤进入人体内，对人体造成伤害，且由于银材料的尺寸极小，很难形成导电网络，所以防静电效果差；蒸镀的银膜制备工艺复杂，且在制备过程中使用银的量大、银的利用率低，且蒸镀工艺会产生大量污染物。而石墨烯作为抗菌材料在纺织品上的应用尚未报道。
发明内容
为避免上述现有技术所存在的不足之处，本发明提供了一种石墨烯微米银丝复合抗菌无纺布及其制作方法，以解决银脱落和防静电效果差的问题。
为了实现上述目的，本发明采取如下技术方案：
本发明的石墨烯微米银丝复合抗菌无纺布，是由聚合物纤维经静电纺丝制成，在所述聚合物纤维中均匀嵌入有石墨烯和微米银丝。
所述聚合物纤维为聚对苯二甲酸乙二醇酯或聚丙烯树脂。
所述微米银丝的直径为0.1-1000μm、长度为10-1000μm。
所述石墨烯为粒径在1-100μm的石墨烯粉体，其所含石墨烯为厚度不超过10层的石墨烯。
上述石墨烯微米银丝复合抗菌无纺布的制作方法，包括如下步骤：
(1)将聚合物纤维加入水中，获得质量浓度为1～25％的聚合物胶体溶液；
在所述聚合物胶体溶液中加入石墨烯和微米银丝，搅拌均匀，获得纺丝液；
在所述纺丝液中，石墨烯的质量占石墨烯、微米银丝和聚合物纤维三者总质量的0.01-1％，微米银丝的质量占石墨烯、微米银丝和聚合物纤维三者总质量的1-24％；
(2)通过静电纺丝法将步骤(1)所获得的纺丝液制成布，即为石墨烯微米银丝复合抗菌无纺布。具体方法如下：
将步骤(1)所获得的纺丝液加水稀释1～5倍，然后加入到静电纺丝机的注射器中，并以1-10mL/h的速度进行泵进，从而使纺丝液从所述注射器的出液口中喷出，形成纺丝细流；
在所述注射器的出液口处设置电压为12-24KV的高压电场，并采用铝箔接收所述纺丝细流；所述纺丝细流穿过所述高压电场，并夹带电荷喷射到铝箔上；所述纺丝细流在铝箔上固化后，即获得石墨烯微米银丝复合抗菌无纺布。
优选的，静电纺丝的纺丝温度为20-30℃、纺丝接收距离为20-25cm、纺丝时间为20-50min。
本发明的有益效果在于：
1、本发明制备的石墨烯微米银丝复合抗菌无纺布，其中的微米银丝不易脱落，且不能透过皮肤渗入人体内。
2、本发明制备的石墨烯微米银丝复合抗菌无纺布，使用石墨烯材料，可以极大地提高无纺布的防静电能力，且能增强无纺布的机械强度。
3、本发明制备的石墨烯微米银丝复合抗菌无纺布，制备工艺简单、银的利用率高、成本低。
4、本发明制备的石墨烯微米银丝复合抗菌无纺布，对白色念珠菌、黑曲霉的抑制率能够达到99％，具有高效抑菌作用。
附图说明
图1为本发明实施例1制备的石墨烯微米银丝复合抗菌无纺布的实物图；
图2为本发明实施例1制备的石墨烯微米银丝复合抗菌无纺布的抗菌检测报告；
图3为本发明实施例1制备的石墨烯微米银丝复合抗菌无纺布的安全性检测报告。
具体实施方式
实施例1
本实施例按如下步骤制备石墨烯微米银丝复合抗菌无纺布：
(1)将聚丙烯树脂纤维加入水中，获得质量浓度为10％的聚丙烯树脂胶体溶液；
取0.5g粒径为3～8μm的石墨烯粉体(其所含石墨烯为6-8层石墨烯)和10g微米银丝(直径为1.5～2.5μm、长度为300～600μm)加入到1kg的聚丙烯树脂胶体溶液中(固含量为100g)，搅拌均匀制备成纺丝液。
(2)将纺丝液加水稀释5倍，然后加入到静电纺丝机的注射器中，以2mL/h的速度进行泵进，使纺丝液从注射器的出液口喷出，形成纺丝细流；在注射器的出液口处设置电压为15kV的高压电场，用铝箔接收纺丝细流，纺丝细流穿过高压电场，并夹带电荷喷射到铝箔上，这些纺丝细流在铝箔上固化后即得到石墨烯微米银丝复合抗菌无纺布。其纺丝温度为20℃，纺丝接收距离为20cm，纺丝时间为40min。
图1(a)、(b)为本实施例所得无纺布的照片。
图2为本实施例所得无纺布的抗菌检测报告，其中对照样为没有加入石墨烯和微米银丝的样品。可以看出普通无纺布对白色念球菌和黑曲霉菌几乎没有抑制作用，而本实施例制备出的石墨烯微米银丝复合抗菌无纺布对白色念珠菌和黑曲霉菌具有99％的抑菌效果。
图3为本实施例所得无纺布的安全性检测报告，可以看出本实施例制备出的微米银丝复合抗菌无纺布完全符合无纺布的安全标准。溢出检测均安全通过，验证微米银丝不易脱落，且不能透过皮肤渗入人体内。
实施例2
本实施例按如下步骤制备石墨烯微米银丝复合抗菌无纺布：
(1)将聚对苯二甲酸乙二醇酯纤维加入水中，获得质量浓度为10％的胶体溶液；
取0.2g粒径为7～10μm的石墨烯粉体(其所含石墨烯为3～5层的石墨烯)和6g微米银丝 (直径为0.6～1.2μm、长度为90～120μm)加入到1kg的聚丙烯树脂胶体溶液中，搅拌均匀制备成纺丝液。
(2)将纺丝液加水稀释5倍，然后加入到静电纺丝机的注射器中，以4mL/h的速度进行泵进，使纺丝液从注射器的出液口喷出，形成纺丝细流；在注射器的出液口处设置电压为20kV的高压电场，用铝箔接收纺丝细流，纺丝细流穿过高压电场，并夹带电荷喷射到铝箔上，这些纺丝细流在铝箔上固化后即得到石墨烯微米银丝复合抗菌无纺布。其纺丝温度为25℃，纺丝接收距离为25cm，纺丝时间为50min。
经与实施例1相同的抗菌性检测和安全性检测，可知本实施例所得样品具备同实施例1 同样的抗菌性和安全性。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。

Claims (7)

1.一种石墨烯微米银丝复合抗菌无纺布，其特征在于：是由聚合物纤维经静电纺丝制成，在所述聚合物纤维中均匀嵌入有石墨烯和微米银丝。
2.根据权利要求1所述的石墨烯微米银丝复合抗菌无纺布，其特征在于：所述聚合物纤维为聚对苯二甲酸乙二醇酯或聚丙烯树脂。
3.根据权利要求1或2所述的石墨烯微米银丝复合抗菌无纺布，其特征在于：所述微米银丝的直径为0.1-1000μm、长度为10-1000μm。
4.根据权利要求1或2所述的石墨烯微米银丝复合抗菌无纺布，其特征在于：所述石墨烯为粒径在1-100μm的石墨烯粉体，其所含石墨烯的厚度不超过10层石墨烯。
5.一种权利要求1～4中任意一项所述石墨烯微米银丝复合抗菌无纺布的制作方法，其特征在于，包括如下步骤：
(1)将聚合物纤维加入水中，获得质量浓度为1～25％的聚合物胶体溶液；
在所述聚合物胶体溶液中加入石墨烯和微米银丝，搅拌均匀，获得纺丝液；
在所述纺丝液中，石墨烯的质量占石墨烯、微米银丝和聚合物纤维三者总质量的0.01-1％，微米银丝的质量占石墨烯、微米银丝和聚合物纤维三者总质量的1-24％；
(2)通过静电纺丝法将步骤(1)所获得的纺丝液制成布，即为石墨烯微米银丝复合抗菌无纺布。
6.根据权利要求5所述的制作方法，其特征在于，步骤(2)的具体方法如下：
将步骤(1)所获得的纺丝液加水稀释1～5倍，然后加入到静电纺丝机的注射器中，并以1-10mL/h的速度进行泵进，从而使纺丝液从所述注射器的出液口中喷出，形成纺丝细流；
在所述注射器的出液口处设置电压为12-24KV的高压电场，并采用铝箔接收所述纺丝细流；所述纺丝细流穿过所述高压电场，并夹带电荷喷射到铝箔上；所述纺丝细流在铝箔上固化后，即获得石墨烯微米银丝复合抗菌无纺布。
7.根据权利要求6所述的制备方法，其特征在于：静电纺丝的纺丝温度为20-30℃、纺丝接收距离为20-25cm、纺丝时间为20-50min。
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