CN112522862B - 一种可见光驱动抗菌纳米纤维及其制备方法与应用 - Google Patents
一种可见光驱动抗菌纳米纤维及其制备方法与应用 Download PDFInfo
- Publication number
- CN112522862B CN112522862B CN202011266346.8A CN202011266346A CN112522862B CN 112522862 B CN112522862 B CN 112522862B CN 202011266346 A CN202011266346 A CN 202011266346A CN 112522862 B CN112522862 B CN 112522862B
- Authority
- CN
- China
- Prior art keywords
- pmma
- solution
- nanofiber membrane
- nanofiber
- visible light
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002121 nanofiber Substances 0.000 title claims abstract description 84
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 68
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 63
- 239000012528 membrane Substances 0.000 claims abstract description 60
- 239000000243 solution Substances 0.000 claims abstract description 49
- 238000002791 soaking Methods 0.000 claims abstract description 26
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 14
- 230000001681 protective effect Effects 0.000 claims abstract description 12
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 11
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 230000021523 carboxylation Effects 0.000 claims abstract description 6
- 238000006473 carboxylation reaction Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000007853 buffer solution Substances 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 4
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 claims description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 2
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 2
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000001523 electrospinning Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 4
- 229960003638 dopamine Drugs 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 210000004379 membrane Anatomy 0.000 description 49
- 241000894006 Bacteria Species 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 239000000443 aerosol Substances 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000872 buffer Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
Images
Classifications
-
- 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
- D04H1/70—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
- D04H1/72—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 the fibres being randomly arranged
- D04H1/728—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 the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- 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
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- 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
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/16—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated carboxylic acids or unsaturated organic esters, e.g. polyacrylic esters, polyvinyl acetate
-
- 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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/47—Oxides or hydroxides of elements of Groups 5 or 15 of the Periodic Table; Vanadates; Niobates; Tantalates; Arsenates; Antimonates; Bismuthates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/13—Physical properties anti-allergenic or anti-bacterial
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2509/00—Medical; Hygiene
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
本发明属于静电纺丝复合纳米纤维材料制备技术领域，公开了一种可见光驱动抗菌纳米纤维及其制备方法与应用。该方法包括：将PMMA溶于有机溶剂，搅拌均匀后进行静电纺丝，真空干燥后得到PMMA纳米纤维膜；制备盐酸多巴胺修饰的BiVO4溶液；将PMMA纳米纤维膜进行碱处理羧基化后浸泡在45～65℃的EDC/NHS混合溶液中振荡活化0.5～24h，取出干燥，然后浸泡在所述盐酸多巴胺修饰的BiVO4溶液中45～65℃温度条件下振荡12‑24h，取出后干燥，得可见光驱动的抗菌纳米纤维。本发明制备方法简单，制备得到的纳米纤维复合材料的抗菌性增强，且能循环再生，因而非常适合于医用防护过滤材料，提高其防护性能，同时增加使用寿命。
Description
技术领域
本发明属于静电纺丝复合纳米纤维材料制备技术领域，涉及一种可见光驱动抗菌纳米纤维及其制备方法与应用。
背景技术
使用医用防护品(医用防护口罩、防护服、手套等)阻断细菌进入呼吸道是抗病毒的有效手段。但人们在使用过程中会不自觉的触摸表面，使得手上粘黏更多的细菌，如果再用手去触碰眼睛、鼻子、嘴巴等粘膜组织就可能细菌感染，一方面降低了医用防护品的防护效果，另一方面导致医用防护品无法多次使用。因此，研究一种既能保证过滤效率，同时还能够杀灭细菌的医用防护材料具有重要意义。
发明内容
有鉴于此，本发明的目的在于发明一种可见光驱动抗菌纳米纤维，该纤维具有较好的过滤效率，且在可见光催化作用下，具有良好的抗菌效果。
为解决以上问题，本发明提供了一种可见光驱动抗菌纳米纤维的制备方法，包括以下步骤：
S1.将PMMA溶于有机溶剂，搅拌均匀后得到PMMA溶液；
S2.采用所述PMMA溶液进行静电纺丝，真空干燥后得到PMMA纳米纤维膜；
S3.将BiVO4与盐酸多巴胺按照质量比(1～2):1混合在10nM Tris盐酸缓冲液中，冰浴超声分散10-30min，然后放入60℃恒温水浴锅，振荡24～48h，得到盐酸多巴胺修饰的BiVO4溶液，所述Tris盐酸缓冲液的pH为8.5；
S4.将所述PMMA纳米纤维膜进行碱处理羧基化后浸泡在45～65℃的EDC/NHS混合溶液中振荡活化0.5～24h，取出干燥，得到活化后的PMMA纳米纤维膜；
S5.将所述活化后的PMMA纳米纤维膜浸泡在所述盐酸多巴胺修饰的BiVO4溶液中45～65℃温度条件下振荡12-24h，取出后干燥，得可见光驱动的抗菌纳米纤维。
进一步的，所述PMMA溶液的浓度为20～30wt％。
进一步的，所述有机溶剂为二氯甲烷、二氯乙烷、三氯甲烷、丙酮、甲乙酮、苯、氯苯、醋酸乙酯、三氟乙醇和六氟异丙醇中的一种或几种的混合。更优选采用三氯甲烷。
进一步的，步骤S2中，所述静电纺丝具体操作条件如下：接收距离为10～15cm，注射速率为1mL/h。高压电压为10～12kV，纺丝时间为3h，湿度为45％～65％，温度为18～25℃。
进一步的，步骤S2中，所述真空干燥的时间为3～10天。
进一步的，所述碱处理羧基化处理的具体过程为：将所述PMMA纳米纤维膜浸泡在20％乙醇中30～60min，取出用PBS冲洗后浸泡在45～60℃、0.5～5mol/L的NaOH溶液或者KOH溶液中1～2h，取出用PBS冲洗。
进一步的，步骤S4中，所述EDC/NHS混合溶液中，1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐与N-羟基琥珀酰亚胺的质量比为(30～37):9。
本发明还提供了上述的制备方法制备得到的可见光驱动抗菌纳米纤维。
本发明还提供了上述的可见光驱动抗菌纳米纤维在医用防护材料中的应用。
与现有技术相比，本发明将利用静电纺丝技术制备的PMMA纳米纤维经过碱处理羧酸化后，再将多巴胺聚合修饰BiVO4经EDC/NHS接枝到PMMA纳米纤维上制备得到可见光驱动的抗菌纳米纤维膜，具有较好的过滤效率，在可见光催化下具有良好的抗菌效果。本发明提供的制备方法简单有效，操作简便，且所需时间较短。
附图说明
图1是实施例1制备出的抗菌纳米纤维膜形貌图。
图2是实施例1制备出的抗菌纳米纤维膜抗菌图，A图为大肠杆菌，B图为金黄色葡萄球菌。
具体实施方式
下面结合实施例和附图对本发明做更进一步地解释，下列实施例仅用于说明本发明，但并不用来限定本发明的实施范围。
实施例1
1)称取1g PMMA溶于5mL三氟乙醇，搅拌2h以上得到PMMA溶液。
2)将PMMA溶液进行静电纺丝，纺丝参数为：接收距离为15cm，注射速率为1mL/h。高压电压为10.9kV，纺丝时间为3h。湿度为65％，温度为21.5℃。取出真空干燥3天以上得到PMMA纳米纤维膜。
3)将0.3g Tris盐酸搅拌溶解于200mL蒸馏水中，用NaOH调pH等于8.5，得到Tris盐酸缓冲液。再称取100mg BiVO4及50mg盐酸多巴胺，混合在Tris盐酸缓冲液中，用封口膜封口。用超声波清洗机进行冰浴超声分散15min，然后放入60℃恒温水浴锅，振荡24h，制成聚多巴胺修饰的BiVO4溶液。
4)然后将PMMA纳米纤维膜浸泡在20％乙醇中30min后，用PBS冲洗后干燥；接着将PMMA纳米纤维膜浸泡在0.5mol/L NaOH(20％乙醇)中45℃、1h，用PBS冲洗后干燥，得到碱处理后的PMMA纳米纤维膜；
5)接着将碱处理过的PMMA纳米纤维膜浸泡在100mg/30mg EDC/NHS溶液中45℃、30min，用PBS冲洗后干燥，得到活化后的PMMA纳米纤维膜；
6)最后将活化好的PMMA纳米纤维膜浸泡在步骤3)得到的聚多巴胺修饰的BiVO4溶液中60℃振荡过夜，然后取出，真空干燥3天，得到本发明可见光驱动的抗菌纳米纤维，即BiVO4/PMMA纳米纤维膜，如图1所示，BiVO4/PMMA纳米纤维膜呈无纺布形式。在气体流量85L/min条件下，其对300-500nm氯化钠气溶胶的过滤效率为99.07％，高于N95口罩(95％)。评价细菌在BiVO4/PMMA纳米纤维膜上通过光照和黑暗条件培养的生长情况，如图2所示，发现光照条件下，BiVO4/PMMA纳米纤维膜可以减少革兰氏阴性大肠杆菌和革兰氏阳性金黄色葡萄球菌的生长。
实施例2
1)称取1g PMMA溶于5mL三氟乙醇，搅拌2h以上得到PMMA溶液。
2)将PMMA溶液进行静电纺丝，纺丝参数为：接收距离为15cm，注射速率为1mL/h。高压电压为10.9kV，纺丝时间为3h。湿度为57％，温度为23.5℃。取出真空干燥3天以上得到PMMA纳米纤维膜。
3)将0.3g Tris盐酸搅拌溶解于200mL蒸馏水中，用NaOH调pH等于8.5，得到Tris盐酸缓冲液。再称取50mg BiVO4及50mg盐酸多巴胺，混合在Tris盐酸缓冲液中，用封口膜封口。用超声波清洗机进行冰浴超声分散15min，然后放入60℃恒温水浴锅，振荡24h，制成聚多巴胺修饰的BiVO4溶液。
4)然后将PMMA纳米纤维膜浸泡在20％乙醇中30min后，用PBS冲洗后干燥；接着将PMMA纳米纤维膜浸泡在0.5mol/L NaOH(20％乙醇)中45℃、1h，用PBS冲洗后干燥，得到碱处理后的PMMA纳米纤维膜；
5)接着将碱处理过的PMMA纳米纤维膜浸泡在113mg/32mg EDC/NHS溶液中45℃、30min，用PBS冲洗后干燥，得到活化后的PMMA纳米纤维膜；
6)最后将活化好的PMMA纳米纤维膜浸泡在步骤3)得到的聚多巴胺修饰的BiVO4溶液中60℃振荡过夜，然后取出，真空干燥3天，得到本发明可见光驱动的抗菌纳米纤维，即BiVO4/PMMA纳米纤维膜。在气体流量85L/min条件下，其对300-500nm氯化钠气溶胶的过滤效率为99.18％，高于N95口罩(95％)。评价细菌在BiVO4/PMMA纳米纤维膜上通过光照和黑暗条件培养的生长情况，发现光照条件下，BiVO4/PMMA纳米纤维膜可以减少革兰氏阴性大肠杆菌和革兰氏阳性金黄色葡萄球菌的生长。
实施例3
1)称取1.5g PMMA溶于5mL三氟乙醇，搅拌2h以上得到PMMA溶液。
2)将PMMA溶液进行静电纺丝，纺丝参数为：接收距离为15cm，注射速率为1mL/h。高压电压为11kV，纺丝时间为3h。湿度为57％，温度为25℃。取出真空干燥3天以上得到PMMA纳米纤维膜。
3)将0.3g Tris盐酸搅拌溶解于200mL蒸馏水中，用NaOH调pH大于等于8.5，得到Tris盐酸缓冲液。再称取100mg BiVO4及50mg盐酸多巴胺，混合在Tris盐酸缓冲液中，用封口膜封口。用超声波清洗机进行冰浴超声分散15min，然后放入60℃恒温水浴锅，振荡24h，制成聚多巴胺修饰的BiVO4溶液。
4)然后将PMMA纳米纤维膜浸泡在0.5mol/L KOH(20％乙醇)中1h后，用PBS冲洗后干燥；接着将PMMA纳米纤维膜浸泡在0.5mol/L NaOH(20％乙醇)中45℃、1h，用PBS冲洗后干燥，得到碱处理后的PMMA纳米纤维膜；
5)接着将碱处理过的PMMA纳米纤维膜浸泡在138mg/37mg EDC/NHS溶液中45℃、30min，用PBS冲洗后干燥，得到活化后的PMMA纳米纤维膜；
6)最后将活化好的PMMA纳米纤维膜浸泡在步骤3)得到的聚多巴胺修饰的BiVO4溶液中60℃振荡过夜，然后取出，真空干燥3天，得到本发明可见光驱动的抗菌纳米纤维，即BiVO4/PMMA纳米纤维膜。在气体流量85L/min条件下，其对300-500nm氯化钠气溶胶的过滤效率为99.38％，高于N95口罩(95％)。评价细菌在BiVO4/PMMA纳米纤维膜上通过光照和黑暗条件培养的生长情况，发现光照条件下，BiVO4/PMMA纳米纤维膜可以减少革兰氏阴性大肠杆菌和革兰氏阳性金黄色葡萄球菌的生长。
实施例4
1)称取1g PMMA溶于5mL三氟乙醇，搅拌2h以上得到PMMA溶液。
2)将PMMA溶液进行静电纺丝，纺丝参数为：接收距离为15cm，注射速率为1mL/h。高压电压为10kV，纺丝时间为3h。湿度为57％，温度为25℃。取出真空干燥3天以上得到PMMA纳米纤维膜。
3)将0.3g Tris盐酸搅拌溶解于200mL蒸馏水中，用NaOH调pH大于等于8.5，得到Tris盐酸缓冲液。再称取100mg BiVO4及50mg盐酸多巴胺，混合在Tris盐酸缓冲液中，用封口膜封口。用超声波清洗机进行冰浴超声分散15min，然后放入60℃恒温水浴锅，振荡24h，制成聚多巴胺修饰的BiVO4溶液。
4)然后将PMMA纳米纤维膜浸泡在0.5mol/L KOH(20％乙醇)中1h后，用PBS冲洗后干燥；接着将PMMA纳米纤维膜浸泡在0.5mol/L NaOH(20％乙醇)中45℃、1h，用PBS冲洗后干燥，得到碱处理后的PMMA纳米纤维膜；
5)接着将碱处理过的PMMA纳米纤维膜浸泡在185mg/45mg EDC/NHS溶液中45℃、30min，用PBS冲洗后干燥，得到活化后的PMMA纳米纤维膜；
6)最后将活化好的PMMA纳米纤维膜浸泡在步骤3)得到的聚多巴胺修饰的BiVO4溶液中60℃振荡过夜，然后取出，真空干燥3天，得到本发明可见光驱动的抗菌纳米纤维，即BiVO4/PMMA纳米纤维膜。。在气体流量85L/min条件下，其对300-500nm氯化钠气溶胶的过滤效率为99.28％，高于N95口罩(95％)。评价细菌在BiVO4/PMMA纳米纤维膜上通过光照和黑暗条件培养的生长情况，发现光照条件下，BiVO4/PMMA纳米纤维膜可以减少革兰氏阴性大肠杆菌和革兰氏阳性金黄色葡萄球菌的生长。
本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (9)
1.一种可见光驱动抗菌纳米纤维的制备方法，其特征在于，包括以下步骤：
S1.将PMMA溶于有机溶剂，搅拌均匀后得到PMMA溶液；
S2.采用所述PMMA溶液进行静电纺丝，真空干燥后得到PMMA纳米纤维膜；
S3.将BiVO4与盐酸多巴胺按照质量比(1～2):1混合后溶于10nM Tris盐酸缓冲液中，冰浴超声分散10-30min，然后放入60℃恒温水浴锅，振荡24～48h，得到盐酸多巴胺修饰的BiVO4溶液，所述Tris盐酸缓冲液的pH为8.5；
S4.将所述PMMA纳米纤维膜进行碱处理羧基化后浸泡在45～65℃的EDC/NHS混合溶液中振荡活化0.5～24h，取出干燥，得到活化后的PMMA纳米纤维膜；
S5.将所述活化后的PMMA纳米纤维膜浸泡在所述盐酸多巴胺修饰的BiVO4溶液中45～65℃温度条件下振荡12-24h，取出后干燥，得可见光驱动的抗菌纳米纤维。
2.如权利要求1所述的制备方法，其特征在于，所述PMMA溶液的浓度为20～30wt％。
3.如权利要求1所述的制备方法，其特征在于，所述有机溶剂为二氯甲烷、二氯乙烷、三氯甲烷、丙酮、甲乙酮、苯、氯苯、醋酸乙酯、三氟乙醇和六氟异丙醇中的一种或几种的混合。
4.如权利要求1所述的制备方法，其特征在于，步骤S2中，所述静电纺丝具体操作条件如下：接收距离为10～15cm，注射速率为1mL/h，高压电压为10～12kV，纺丝时间为3h，湿度为45％～65％，温度为18～25℃。
5.如权利要求1所述的制备方法，其特征在于，步骤S2中，所述真空干燥的时间为3～10天。
6.如权利要求1所述的制备方法，其特征在于，所述碱处理羧基化处理的具体过程为：将所述PMMA纳米纤维膜浸泡在20％乙醇中30～60min，取出用PBS冲洗后浸泡在45～60℃、0.5～5mol/L的NaOH溶液或者KOH溶液中1～2h，取出用PBS冲洗。
7.如权利要求1所述的制备方法，其特征在于，步骤S4中，所述EDC/NHS混合溶液中，1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐与N-羟基琥珀酰亚胺的质量比为(30～37):9。
8.根据权利要求1～7任一项所述的制备方法制备得到的可见光驱动抗菌纳米纤维。
9.权利要求8所述的可见光驱动抗菌纳米纤维在医用防护材料中的应用。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011266346.8A CN112522862B (zh) | 2020-11-13 | 2020-11-13 | 一种可见光驱动抗菌纳米纤维及其制备方法与应用 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011266346.8A CN112522862B (zh) | 2020-11-13 | 2020-11-13 | 一种可见光驱动抗菌纳米纤维及其制备方法与应用 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112522862A CN112522862A (zh) | 2021-03-19 |
| CN112522862B true CN112522862B (zh) | 2022-02-01 |
Family
ID=74982360
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011266346.8A Active CN112522862B (zh) | 2020-11-13 | 2020-11-13 | 一种可见光驱动抗菌纳米纤维及其制备方法与应用 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112522862B (zh) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113797649B (zh) * | 2021-08-12 | 2022-03-25 | 浙江大学 | 一种抗菌防病毒的空气过滤材料及其制备方法 |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103272576B (zh) * | 2013-06-26 | 2015-03-11 | 青岛农业大学 | 一种钒酸盐纳米纤维光催化剂及其制备方法 |
| CN103464014B (zh) * | 2013-09-25 | 2015-06-10 | 天津工业大学 | 一种抑制中空纤维膜表面细菌的方法 |
| CN105435847B (zh) * | 2015-11-17 | 2018-01-02 | 中国科学院海洋研究所 | 一种Bi2WO6/BiOI@季铵盐无机/有机复合光催化杀菌剂及其制备方法 |
| CN106521809B (zh) * | 2016-10-17 | 2019-04-30 | 安徽工程大学 | 一种功能性PMMA-MMT-TiO2复合纳米纤维膜的制备方法及其应用 |
| CN107064264B (zh) * | 2017-05-18 | 2019-04-30 | 江苏大学 | 一种用于无酶检测多巴胺的光电化学传感器的构建方法 |
| CN109078639A (zh) * | 2018-07-25 | 2018-12-25 | 华南师范大学 | 一种BiVO4/NiCo LDHs多孔纤维及其制备方法和应用 |
| CN109432825A (zh) * | 2018-10-23 | 2019-03-08 | 上海师范大学 | 一种具有油水分离及抗油污染双功能的图案化多孔纳米纤维材料及其制备方法和应用 |
| CN109794291B (zh) * | 2019-01-08 | 2021-07-20 | 江苏大学 | 一种Ti@BiOI-pDA@CA自清洁膜的仿生构建方法及其用途 |
| CN111501347B (zh) * | 2019-01-30 | 2021-12-24 | 宁波方太厨具有限公司 | 一种催化纳米纤维的制备方法 |
| CN110075923A (zh) * | 2019-04-30 | 2019-08-02 | 江苏大学 | 一种g-C3N4/BiOI-pDA@PVDF光催化膜的仿生构建方法及其用途 |
| CN110052263A (zh) * | 2019-04-30 | 2019-07-26 | 广东工业大学 | 一种光催化纳米纤维材料及其制备方法和应用 |
| CN111822028B (zh) * | 2020-07-21 | 2023-01-03 | 西安工业大学 | 一种基于MXene的铋基光催化复合膜及其制备方法 |
-
2020
- 2020-11-13 CN CN202011266346.8A patent/CN112522862B/zh active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112522862A (zh) | 2021-03-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Rechargeable polyamide-based N-halamine nanofibrous membranes for renewable, high-efficiency, and antibacterial respirators | |
| Yan et al. | Electrospun in-situ hybrid polyurethane/nano-TiO 2 as wound dressings | |
| CN108425238B (zh) | 口罩用抗菌、低阻力、高过滤效率石墨烯无纺布的制备方法 | |
| JP6858330B2 (ja) | 抗ウイルス性素材 | |
| CN108993167A (zh) | 一种抗菌的静电纺丝纳米纤维空气过滤材料的制备及应用 | |
| CN109224878A (zh) | 一种空气净化用复合抗菌膜及制备方法 | |
| CN112522862B (zh) | 一种可见光驱动抗菌纳米纤维及其制备方法与应用 | |
| CN114086394B (zh) | 一种口罩用无纺布的处理工艺 | |
| CN106582148A (zh) | 一种电纺复合微纳米纤维空气过滤膜及其制备方法 | |
| CN113152101B (zh) | 一种抗病毒聚乳酸无纺布的制备方法 | |
| CN101352630A (zh) | 一种多功能纳米滤材及其制备方法 | |
| CN103726224A (zh) | 一种无纺膜及其制备的荷电非织造生物防护口罩及制备方法 | |
| CN112007426B (zh) | 一种高性能介孔二氧化硅-壳聚糖复合的抗菌过滤片的制备方法 | |
| CN108505143A (zh) | 一种纳米纤维及其制备方法 | |
| CN111449318A (zh) | 一种抗菌抗病毒口罩及其制备方法 | |
| CN112471173B (zh) | 石墨烯抗菌复合膜的制备方法、制得的抗菌复合膜 | |
| CN113152090A (zh) | 一种抗菌抗病毒纤维素纳米纤维过滤防护膜及其制备方法 | |
| CN111394996A (zh) | 一种医用口罩用熔喷无纺布的长效荷正电处理工艺 | |
| CN106436316A (zh) | 一种高耐磨的静电纺/驻极体复合纤维膜过滤材料及其制备方法 | |
| CN111636213A (zh) | 一种聚四氟乙烯口罩纤维面层的制备方法 | |
| Yang et al. | Nanopatterning of beaded poly (lactic acid) nanofibers for highly electroactive, breathable, UV-shielding and antibacterial protective membranes | |
| CN106319758A (zh) | 一种静电纺制备pei/壳聚糖接枝物复合驻极纤维膜过滤材料及其制备方法 | |
| CN108456998A (zh) | 一种高强度抑菌纳米纤维膜及其制备方法 | |
| CN110205808B (zh) | 一种基于等离子体、纳米碳粉处理的烯丙基海因纳米纤维的制备方法 | |
| CN107485578A (zh) | 一种静电纺制备壳聚糖/寡肽生物美白面膜的方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |