CN113442523B - 一种基于石墨烯的持久抗菌复合面料及其制备方法 - Google Patents

一种基于石墨烯的持久抗菌复合面料及其制备方法 Download PDF

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CN113442523B
CN113442523B CN202111017687.6A CN202111017687A CN113442523B CN 113442523 B CN113442523 B CN 113442523B CN 202111017687 A CN202111017687 A CN 202111017687A CN 113442523 B CN113442523 B CN 113442523B
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CN113442523A (zh
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倪张根
黄荣庆
曹建鹏
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Jiangsu Jiangshanhong Chemical Fiber Co ltd
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Abstract

本发明公开了一种基于石墨烯的持久抗菌复合面料，包括亲肤层、吸汗层、抗菌层、抗紫外线层；用水溶性酚醛树脂对竹纤维进行改性处理，使改性后的竹纤维具有高比表面积，大幅提高竹纤维的吸附性、抗菌、防臭和抗紫外线性；以氧化石墨烯量子点作为固定氧化铈纳米颗粒的基体，使氧化铈纳米颗粒在氧化石墨烯量子点纳米片上均匀分布，壳聚糖和甘油的添加，达到缓慢释放氧化铈纳米颗粒，持久抗菌的效果；在抗紫外线层中运用纳米氧化锌和花状二氧化钛有机结合，能够有效屏蔽太阳光紫外线中的UVA和UVB，而且还增加了面料的自洁性和抗污性。

Description

一种基于石墨烯的持久抗菌复合面料及其制备方法
技术领域
本发明属于纺织面料技术领域，具体地说，涉及一种基于石墨烯的持久抗菌复合面料及其制备方法。
背景技术
常规面料的原料主要为棉、麻、丝、涤纶、锦纶等，具有多孔结构的纺织纤维面料在使用过程中易吸附细菌，且人体排出的汗液、脱落的皮脂等都为菌类繁殖提供了丰富的营养，造成细菌滋生，细菌的滋生不仅产生异味，易造成交叉感染而传播疾病，也容易损伤纤维，随着生活水平的提高，人们越来越重视纺织品的舒适性与功能性，传统的面料已不能满足人们的使用要求。
氧化石墨烯可以破坏细菌的细胞膜，从而导致胞内物质外流并杀死细菌，而现有的石墨烯抗菌面料大多是通过直接在织物上设置粘结涂层制备，直接在面料上设置涂层会大幅降低织物的透气性，且耐洗度较差，无法发挥持久的抗菌效果。
发明内容
本发明的目的在于提供一种基于石墨烯的持久抗菌复合面料及其制备方法，以解决现有技术中的问题。
为了解决上述问题，本发明所采用的技术方案如下：
一种基于石墨烯的持久抗菌复合面料的制备方法，包括以下步骤：
步骤1，竹纤维编织形成吸汗层；
步骤2，以氧化石墨烯量子点作为基体，使氧化铈纳米颗粒在氧化石墨烯量子点上均匀分布，然后加入甘油和壳聚糖的混合液，用以浸渍竹纤维，得到抗菌纤维，编制形成抗菌层；
步骤3，将花状二氧化钛、纳米氧化锌、修饰剂、挥发性溶剂混合分散，得到分散液，将竹纤维浸渍在分散液中，得到抗紫外纤维，编织形成抗紫外线层；
步骤4，将亲肤层、吸汗层、抗菌层和抗紫外线层依次缝制或粘接，得到基于石墨烯的持久抗菌复合面料。
所述抗菌层的制备方法为：
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈混合溶液中加入氨水，调节pH为8-11，30-90℃下反应10-90min，然后离心、洗涤后得反应液；
（2）将步骤（1）所得反应液加入到甘油和壳聚糖的混合液中，超声搅拌，静置后形成悬浊液；
（3）将竹纤维浸渍在步骤（2）所得悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理3-6次，完成后漂洗、干燥，得到石墨烯抗菌纤维，纺织形成抗菌层。
所述抗紫外线层的制备方法为：
（1）将花状二氧化钛粉末、纳米氧化锌粉末、修饰剂、挥发性烷烃混合搅拌，超声分散，得到分散液；
（2）将竹纤维浸渍在分散液中，得到抗紫外线纤维，纺织得到抗紫外线层；
花状二氧化钛粉末与纳米氧化锌粉末的质量比为（1-3）:1。
优选的，步骤1~3中的竹纤维采用高比表面积的改性竹纤维。
优选的，所述的改性竹纤维的制备方法为：对竹纤维进行浸渍、清洗至中性，烘干；将烘干后的竹纤维加入到水溶性酚醛树脂中浸泡24-36h，烘干；在氮气保护下，150-250℃保温1-3h，然后将温度升至600-900℃反应，冷却至20-25℃后加盐酸浸泡30-90min，反复洗涤至中性，烘干，得到改性竹纤维。
优选的，所述的花状二氧化钛粉末的制备方法为：将钛酸四丁酯、无水乙醇、甘油按照体积比1:15:(3-6)混合，然后在140℃-190℃下反应12-36h，冷却后经洗涤、干燥、煅烧、粉碎，得到花状二氧化钛粉末。
优选的，采用氢氧化钠、氢氧化钾、碳酸钾、磷酸、氯化锌中的一种或多种制成的溶液对竹纤维进行浸渍；水溶性酚醛树脂的固含量为33%-40%。
优选的，氧化石墨烯量子点与六水合硝酸铈的质量比为2:(1-3)。
优选的，所述修饰剂为全氟辛基三氯硅烷，修饰剂的浓度为0.3-1.5wt％。
前述方法制备得到的基于石墨烯的持久抗菌复合面料。
相比于现有技术，本发明的有益效果为：
（1）本发明使用的壳聚糖来源广、成本低，具有可生物降解性；
（2）本发明以竹纤维为原料，用水溶性酚醛树脂对竹纤维进行改性处理，使改性后的竹纤维具有高比表面积，大幅提高竹纤维的吸附性、抗菌、防臭和抗紫外线性；
（3）以氧化石墨烯量子点作为固定氧化铈纳米颗粒的基体，有效的阻碍了氧化铈纳米颗粒的聚集，使氧化铈纳米颗粒在氧化石墨烯量子点纳米片上均匀的分布，并限制了氧化铈纳米颗粒的粒径尺寸大小；氧化铈纳米颗粒粒径的减小使得比表面积增大，更有效的与细菌结合并杀死细菌，大大提高了面料的杀菌性能；壳聚糖和甘油的添加，达到缓慢释放氧化铈纳米颗粒，持久抗菌的效果；
（4）在抗紫外线层中运用纳米氧化锌和花状二氧化钛的有机结合，能够有效屏蔽太阳光紫外线中的UVA和UVB，而且还增加了面料的自洁性和抗污性。
具体实施方式
下面结合具体实施例对本发明进一步进行描述。
实施例1
S1：亲肤层的制备
棉纤维编织形成亲肤层；
S2：吸汗层的制备
（1）用2wt％氢氧化钠对竹纤维进行浸渍处理，用去离子水反复清洗竹纤维至中性，烘干；将烘干后的竹纤维加入到固含量33%的水溶性酚醛树脂中浸泡36h，烘干；在氮气保护下，在150℃下保温氧化3h，然后将温度升至600℃反应，冷却至20℃后加盐酸浸泡90min，用去离子水反复洗涤至中性，烘干，得到改性竹纤维；
（2）改性竹纤维编织，通过纤维丝缝制在亲肤层表面，形成吸汗层；
S3：抗菌层的制备
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈质量比为2：1的混合溶液中加入0.1mol/L氨水，调节pH为8，进行水热反应，水热反应的反应温度为30℃，反应时间90min，然后依次离心、水洗、乙醇洗涤后得反应液；
（2）将步骤S3（1）中所述反应液加入到甘油和壳聚糖含量比为5％的混合溶液中，超声搅拌，静置后形成悬浊液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S3（2）中悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理3次，完成后用无水乙醇、去离子水反复漂洗，漂洗后在60℃下干燥，得到石墨烯抗菌纤维，石墨烯抗菌纤维纺织形成抗菌层，通过改性聚丙烯酸酯乳液粘结在吸汗层表面；
S4：抗紫外线层的制备
（1）钛酸四丁酯、无水乙醇、甘油按照体积比1:15:3在超声作用下混合搅拌，在140℃下水热反应36h，冷却至18℃后反复离心洗涤，真空干燥后在400℃下煅烧1.5h，冷却后粉碎细化处理，得到花状二氧化钛粉末；
（2）花状二氧化钛粉末与纳米氧化锌粉末质量比1:1，全氟辛基三氯硅烷浓度为0.3wt％，将花状二氧化钛粉末、纳米氧化锌粉末、全氟辛基三氯硅烷、正乙烷混合搅拌，超声分散，得到分散液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S4（2）分散液中，得到抗紫外线纤维，抗紫外线纤维纺织形成抗紫外线层，通过纤维丝缝制在抗菌层表面，得到一种基于石墨烯的持久抗菌复合面料。
实施例2
S1：亲肤层的制备
棉纤维编织形成亲肤层；
S2：吸汗层的制备
（1）用3wt％氢氧化钠对竹纤维进行浸渍处理，用去离子水反复清洗竹纤维至中性，烘干；将烘干后的竹纤维加入到固含量36%的水溶性酚醛树脂中浸泡30h，烘干；在氮气保护下，在200℃下保温氧化2h，然后将温度升至800℃反应，冷却至22℃后加盐酸浸泡80min，用去离子水反复洗涤至中性，烘干，得到改性竹纤维；
（2）改性竹纤维编织，通过纤维丝缝制在亲肤层表面，形成吸汗层；
S3：抗菌层的制备
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈质量比为1:1的混合溶液中加入0.3mol/L氨水，调节pH为9，进行水热反应，水热反应的反应温度为30℃，反应时间80min，然后依次离心、水洗、乙醇洗涤后得反应液；
（2）将步骤S3（1）中所述反应液加入到甘油和壳聚糖含量比为6％的混合溶液中，超声搅拌，静置后形成悬浊液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S3（2）中悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理4次，完成后用无水乙醇、去离子水反复漂洗，漂洗后在65℃下干燥，得到石墨烯抗菌纤维，石墨烯抗菌纤维纺织形成抗菌层，通过改性聚丙烯酸酯乳液粘结在吸汗层表面；
S4：抗紫外线层的制备
（1）钛酸四丁酯、无水乙醇、甘油按照体积比1:15:4在超声作用下混合搅拌，在150℃下水热反应30h，冷却至20℃后反复离心洗涤，真空干燥后在450℃下煅烧2h，冷却后粉碎细化处理，得到花状二氧化钛粉末；
（2）花状二氧化钛粉末与纳米氧化锌粉末质量比2:1，全氟辛基三氯硅烷浓度为1wt％，将花状二氧化钛粉末、纳米氧化锌粉末、全氟辛基三氯硅烷、正乙烷混合搅拌，超声分散，得到分散液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S4（2）分散液中，得到抗紫外线纤维，抗紫外线纤维纺织形成抗紫外线层，通过纤维丝缝制在抗菌层表面，得到一种基于石墨烯的持久抗菌复合面料。
实施例3
S1：改性竹纤维的制备
S1：亲肤层的制备
棉纤维编织形成亲肤层；
S2：吸汗层的制备
（1）用10wt％氢氧化钠对竹纤维进行浸渍处理，用去离子水反复清洗竹纤维至中性，烘干；将烘干后的竹纤维加入到固含量40%的水溶性酚醛树脂中浸泡24h，烘干；在氮气保护下，在250℃下保温氧化1h，然后将温度升至900℃反应，冷却至25℃后加盐酸浸泡30min，用去离子水反复洗涤至中性，烘干，得到改性竹纤维；
（2）改性竹纤维编织，通过纤维丝缝制在亲肤层表面，形成吸汗层；
S3：抗菌层的制备
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈质量比为2:3的混合溶液中加入3mol/L氨水，调节pH为11，进行水热反应，水热反应的反应温度为90℃，反应时间10min，然后依次离心、水洗、乙醇洗涤后得反应液；
（2）将步骤S3（1）中所述反应液加入到甘油和壳聚糖含量比为20％的混合溶液中，超声搅拌，静置后形成悬浊液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S3（2）中悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理4次，完成后用无水乙醇、去离子水反复漂洗，漂洗后在80℃下干燥，得到石墨烯抗菌纤维，石墨烯抗菌纤维纺织形成抗菌层，通过改性聚丙烯酸酯乳液粘结在吸汗层表面；
S4：抗紫外线层的制备
（1）钛酸四丁酯、无水乙醇、甘油按照体积比1:15:6在超声作用下混合搅拌，在190℃下水热反应12h，冷却至25℃后反复离心洗涤，真空干燥后在500℃下煅烧1.5h，冷却后粉碎细化处理，得到花状二氧化钛粉末；
（2）花状二氧化钛粉末与纳米氧化锌粉末质量比3:1，全氟辛基三氯硅烷浓度为1.5wt％，将花状二氧化钛粉末、纳米氧化锌粉末、全氟辛基三氯硅烷、正已烷混合搅拌，超声分散，得到分散液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S4（2）分散液中，得到抗紫外线纤维，抗紫外线纤维纺织形成抗紫外线层，通过纤维丝缝制在抗菌层表面，得到一种基于石墨烯的持久抗菌复合面料。
实施例4
S1：亲肤层的制备
棉纤维编织形成亲肤层；
S2：吸汗层的制备
（1）用3wt％碳酸钾对竹纤维进行浸渍处理，用去离子水反复清洗竹纤维至中性，烘干；将烘干后的竹纤维加入到固含量36%的水溶性酚醛树脂中浸泡30h，烘干；在氮气保护下，在200℃下保温氧化2.5h，然后将温度升至800℃反应，冷却至22℃后加盐酸浸泡80min，用去离子水反复洗涤至中性，烘干，得到改性竹纤维；
（2）改性竹纤维编织，通过纤维丝缝制在亲肤层表面，形成吸汗层；
S3：抗菌层的制备
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈质量比为2：1的混合溶液中加入0.3mol/L氨水，调节pH为9，进行水热反应，水热反应的反应温度为30℃，反应时间80min，然后依次离心、水洗、乙醇洗涤后得反应液；
（2）将步骤S3（1）中所述反应液加入到甘油和壳聚糖含量比为6％的混合溶液中，超声搅拌，静置后形成悬浊液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S3（2）中悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理5次，完成后用无水乙醇、去离子水反复漂洗，漂洗后在65℃下干燥，得到石墨烯抗菌纤维，石墨烯抗菌纤维纺织形成抗菌层，通过改性聚丙烯酸酯乳液粘结在吸汗层表面；
S4：抗紫外线层的制备
（1）钛酸四丁酯、无水乙醇、甘油按照体积比1:15:4在超声作用下混合搅拌，在150℃下水热反应30h，冷却至20℃后反复离心洗涤，真空干燥后在450℃下煅烧2h，冷却后粉碎细化处理，得到花状二氧化钛粉末；
（2）花状二氧化钛粉末与纳米氧化锌粉末质量比2:1，全氟辛基三氯硅烷浓度为1wt％，将花状二氧化钛粉末、纳米氧化锌粉末、全氟辛基三氯硅烷、正乙烷混合搅拌，超声分散，得到分散液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S4（2）分散液中，得到抗紫外线纤维，抗紫外线纤维纺织形成抗紫外线层，通过纤维丝缝制在抗菌层表面，得到一种基于石墨烯的持久抗菌复合面料。
实施例5
S1：亲肤层的制备
棉纤维编织形成亲肤层；
S2：吸汗层的制备
（1）用3wt％磷酸对竹纤维进行浸渍处理，用去离子水反复清洗竹纤维至中性，烘干；将烘干后的竹纤维加入到固含量36%的水溶性酚醛树脂中浸泡30h，烘干；在氮气保护下，在200℃下保温氧化2h，然后将温度升至800℃反应，冷却至22℃后加盐酸浸泡80min，用去离子水反复洗涤至中性，烘干，得到改性竹纤维；
（2）改性竹纤维编织，通过纤维丝缝制在亲肤层表面，形成吸汗层；
S3：抗菌层的制备
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈质量比为2:1的混合溶液中加入0.3mol/L氨水，调节pH为9，进行水热反应，水热反应的反应温度为30℃，反应时间80min，然后依次离心、水洗、乙醇洗涤后得反应液；
（2）将步骤S3（1）中所述反应液加入到甘油和壳聚糖含量比为6％的混合溶液中，超声搅拌，静置后形成悬浊液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S3（2）中悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理4次，完成后用无水乙醇、去离子水反复漂洗，漂洗后在65℃下干燥，得到石墨烯抗菌纤维，石墨烯抗菌纤维纺织形成抗菌层，通过改性聚丙烯酸酯乳液粘结在吸汗层表面；
S4：抗紫外线层的制备
（1）钛酸四丁酯、无水乙醇、甘油按照体积比1:15:4在超声作用下混合搅拌，在150℃下水热反应30h，冷却至20℃后反复离心洗涤，真空干燥后在450℃下煅烧2h，冷却后粉碎细化处理，得到花状二氧化钛粉末；
（2）花状二氧化钛粉末与纳米氧化锌粉末质量比2:1，全氟辛基三氯硅烷浓度为1wt％，将花状二氧化钛粉末、纳米氧化锌粉末、全氟辛基三氯硅烷、正乙烷混合搅拌，超声分散，得到分散液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S4（2）分散液中，得到抗紫外线纤维，抗紫外线纤维纺织形成抗紫外线层，通过纤维丝缝制在抗菌层表面，得到一种基于石墨烯的持久抗菌复合面料。
实施例6
S1：亲肤层的制备
棉纤维编织形成亲肤层；
S2：吸汗层的制备
（1）用3wt％氯化锌对竹纤维进行浸渍处理，用去离子水反复清洗竹纤维至中性，烘干；将烘干后的竹纤维加入到固含量36%的水溶性酚醛树脂中浸泡30h，烘干；在氮气保护下，在200℃下保温氧化2h，然后将温度升至800℃反应，冷却至22℃后加盐酸浸泡80min，用去离子水反复洗涤至中性，烘干，得到改性竹纤维；
（2）改性竹纤维编织，通过纤维丝缝制在亲肤层表面，形成吸汗层；
S3：抗菌层的制备
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈质量比为2:1的混合溶液中加入0.3mol/L氨水，调节pH为9，进行水热反应，水热反应的反应温度为30℃，反应时间80min，然后依次离心、水洗、乙醇洗涤后得反应液；
（2）将步骤S3（1）中所述反应液加入到甘油和壳聚糖含量比为6％的混合溶液中，超声搅拌，静置后形成悬浊液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S3（2）中悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理4次，完成后用无水乙醇、去离子水反复漂洗，漂洗后在65℃下干燥，得到石墨烯抗菌纤维，石墨烯抗菌纤维纺织形成抗菌层，通过改性聚丙烯酸酯乳液粘结在吸汗层表面；
S4：抗紫外线层的制备
（1）钛酸四丁酯、无水乙醇、甘油按照体积比1:15:4在超声作用下混合搅拌，在150℃下水热反应30h，冷却至20℃后反复离心洗涤，真空干燥后在450℃下煅烧2h，冷却后粉碎细化处理，得到花状二氧化钛粉末；
（2）花状二氧化钛粉末与纳米氧化锌粉末质量比2:1，全氟辛基三氯硅烷浓度为1wt％，将花状二氧化钛粉末、纳米氧化锌粉末、全氟辛基三氯硅烷、正乙烷混合搅拌，超声分散，得到分散液；
（3）将步骤S2（1）中所述改性竹纤维浸渍在步骤S4（2）分散液中，得到抗紫外线纤维，抗紫外线纤维纺织形成抗紫外线层，通过纤维丝缝制在抗菌层表面，得到一种基于石墨烯的持久抗菌复合面料。
依据标准GB/T 20944.3-2008的检测方法对实施例1-6制备的面料进行抗菌性能检测，革兰氏阴性菌大肠杆菌和革兰氏阳性菌金黄色葡萄球菌为试验菌种；
测得实施例1-6抗菌复合面料对大肠杆菌和金黄色葡萄球菌的抑菌率分别如表1所示；
实施例1-6抗菌复合面料对大肠杆菌和金黄色葡萄球菌的抑菌率均在99.5%以上，具有优异的抗菌性能。
表1 抗菌性能测试结果
实施例1 实施例2 实施例3 实施例4 实施例5 实施例6
大肠杆菌抑菌率 100% 99.8% 100% 99.9% 99.7% 100%
金黄色葡萄球菌抑菌率 99.8% 100% 99.9% 100% 99.9% 99.6%
面料的抗菌耐久性按照标准GB/T 20944.3-2008评价，通过对待测抗菌试样进行50次标准洗涤，测得实施例1-6抗菌复合面料对大肠杆菌和金黄色葡萄球菌的抑菌率分别如表2所示，考察其抗菌耐久性。
表2 抗菌耐久性测试结果
实施例1 实施例2 实施例3 实施例4 实施例5 实施例6
大肠杆菌抑菌率 98.2% 98.1% 98.9% 97.9% 98.1% 98.2%
金黄色葡萄球菌抑菌率 98.3% 99.1% 98.4% 98.1% 97.9% 98%
从表2中可以看出，实施例1-6抗菌复合面料对大肠杆菌和金黄色葡萄球菌的抑菌率均在98%以上，抗菌耐久性高。

Claims (9)

1.一种基于石墨烯的持久抗菌复合面料的制备方法，其特征在于，包括以下步骤：
步骤1，竹纤维编织形成吸汗层；
步骤2，以氧化石墨烯量子点作为基体，使氧化铈纳米颗粒在氧化石墨烯量子点上均匀分布，然后加入甘油和壳聚糖的混合液，用以浸渍竹纤维，得到抗菌纤维，编织 形成抗菌层；
步骤3，将花状二氧化钛、纳米氧化锌、修饰剂、挥发性溶剂混合分散，得到分散液，将竹纤维浸渍在分散液中，得到抗紫外纤维，编织形成抗紫外线层；
步骤4，将亲肤层、吸汗层、抗菌层和抗紫外线层依次缝制或粘接，得到基于石墨烯的持久抗菌复合面料；
所述抗菌层的制备方法为：
（1）超声作用下，向氧化石墨烯量子点与六水合硝酸铈混合溶液中加入氨水，调节pH为8-11，30-90℃下反应10-90min，然后离心、洗涤后得反应液；
（2）将步骤（1）所得反应液加入到甘油和壳聚糖的混合液中，超声搅拌，静置后形成悬浊液；
（3）将竹纤维浸渍在步骤（2）所得悬浊液中，取出后紫外线照射处理，重复浸渍处理和紫外线处理3-6次，完成后漂洗、干燥，得到石墨烯抗菌纤维，纺织形成抗菌层。
2.根据权利要求1所述的制备方法，其特征在于，所述抗紫外线层的制备方法为：
（1）将花状二氧化钛粉末、纳米氧化锌粉末、修饰剂、挥发性烷烃混合搅拌，超声分散，得到分散液；
（2）将竹纤维浸渍在分散液中，得到抗紫外线纤维，纺织得到抗紫外线层；
花状二氧化钛粉末与纳米氧化锌粉末的质量比为（1-3）:1。
3.根据权利要求1所述的制备方法，其特征在于，步骤1~3中的竹纤维采用高比表面积的改性竹纤维。
4.根据权利要求3所述的制备方法，其特征在于，所述的改性竹纤维的制备方法为：对竹纤维进行浸渍、清洗至中性，烘干；将烘干后的竹纤维加入到水溶性酚醛树脂中浸泡24-36h，烘干；在氮气保护下，150-250℃保温1-3h，然后将温度升至600-900℃反应，冷却至20-25℃后加盐酸浸泡30-90min，反复洗涤至中性，烘干，得到改性竹纤维。
5.根据权利要求2所述的制备方法，其特征在于，所述的花状二氧化钛粉末的制备方法为：将钛酸四丁酯、无水乙醇、甘油按照体积比1:15:(3-6)混合，然后在140℃-190℃下反应12-36h，冷却后经洗涤、干燥、煅烧、粉碎，得到花状二氧化钛粉末。
6.根据权利要求4所述的制备方法，其特征在于，采用氢氧化钠、氢氧化钾、碳酸钾、磷酸、氯化锌中的一种或多种制成的溶液对竹纤维进行浸渍；水溶性酚醛树脂的固含量为33%-40%。
7.根据权利要求1所述的制备方法，其特征在于，氧化石墨烯量子点与六水合硝酸铈的质量比为2:(1-3)。
8.根据权利要求2所述的制备方法，其特征在于，所述修饰剂为全氟辛基三氯硅烷，修饰剂的浓度为0.3-1.5wt％。
9.权利要求1~8中任一项所述的方法制备得到的基于石墨烯的持久抗菌复合面料。
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