CN108208003A - 一种Ag/多巴胺/g-C3N4可见光催化杀菌剂 - Google Patents
一种Ag/多巴胺/g-C3N4可见光催化杀菌剂 Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/08—Amines; Quaternary ammonium compounds containing oxygen or sulfur
- A01N33/10—Amines; Quaternary ammonium compounds containing oxygen or sulfur having at least one oxygen or sulfur atom directly attached to an aromatic ring system
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0271—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds also containing elements or functional groups covered by B01J31/0201 - B01J31/0231
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Pest Control & Pesticides (AREA)
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Abstract
本发明属于无机功能材料技术领域,特指一种Ag/多巴胺/g‑C3N4可见光催化杀菌剂。采用g‑C3N4为模板,硝酸银为前驱体,用硼氢化钠冰水浴还原反应制备Ag/多巴胺/g‑C3N4新型复合材料;该新型复合物具有优异的抗菌和杀菌性能,并且g‑C3N4和多巴胺都是生物相容性材料,本身对细胞没有毒性。多巴胺能够在无机材料表面通过自身氧化聚合形成超强黏附性的聚多巴胺层,聚多巴胺分子中的邻苯二酚基团具有一定的还原性,能够将金、银等贵金属离子还原成单质。同时,金属纳米颗粒与无机材料能够通过聚多巴胺上的邻苯二酚和氨基官能团产生共价与非共价的相互作用,使贵金属纳米粒子可以强力地附着于g‑C3N4材料表面上。
Description
技术领域
本发明属于无机功能材料技术领域,特指一种Ag/多巴胺/g-C3N4可见光催化杀菌剂,采用g-C3N4为模板,硝酸银为前驱体,硼氢化钠为还原剂,冰水浴反应制备Ag/多巴胺/g-C3N4新型杀菌复合材料。
背景技术
近年来随着工业的迅猛发展,污染水中的细菌滋生问题与我们愈加相关,抗菌及杀菌工作的重要性也就不言而喻。由于Ag纳米粒子优异的等离子效应和可见光催化活性、稳定性,从而受到广泛的关注。Ag纳米粒子可以释放出微量的Ag+,通过库伦引力牢固地吸附在带负电荷的大肠杆菌细胞膜上从而干扰DNA合成进而使细菌丧失分裂繁殖能力,可以有效地杀灭水体中的有害微生物,用于处理废水、废气中有机污染物。但是,在杀菌实验中单独使用银纳米颗粒存在诸多问题:(1)由于Ag为纳米颗粒,在实际杀菌实验中容易流失且对细胞具有一定毒性从而造成环境污染;(2)Ag纳米颗粒由于粒度小,表面原子比例大,比表面积大,表面能大,处于能量不稳定状态,因而很容易在水溶液中发生静电吸附作用而自身团聚。已有报道将Ag与石墨烯、Al2O3、凝胶、二氧化硅负载形成复合材料,但是大多数载体制备复杂、价格昂贵且对细胞具有一定的毒性,从而我们选择类石墨相氮化碳(g-C3N4)作为新型复合材料载体。
类石墨相氮化碳(g-C3N4)作为一种由三嗪(C3N4)和七嗪(C6N7)单元构成的碳氮聚合物,具有密度低、化学惰性和生物兼容性好等优点。g-C3N4作为半导体产生的h+,·O2 -和H2O2等可以有效地杀死带负电的大肠杆菌,令细菌丧失分裂繁殖能力而死亡。(Long Sun,etal.Acs Sustainable Chemistry&Engineering,2017,5(10):8693–8701)。
目前,已有报道将Ag与类石墨相氮化碳通过静电吸附作用复合获得Ag/g-C3N4新型光催化剂(Tian K,et al.Acs Sustainable Chemistry&Engineering,2015,3(2):269;Adhikari S P,et al.Colloids &Surfaces A Physicochemical&Engineering Aspects,2015,482(13):477;Shouwei Z,et al.Acs Applied Materials&Interfaces,2014,6(24):22116.),但仍存在着不足:(1)g-C3N4上的Ag颗粒尺寸较大(约为50nm)且粒径不均,容易发生团聚和堆叠;(2)在简单的静电吸附作用下,Ag纳米粒子与g-C3N4的结合不紧密,容易从g-C3N4上脱落,从而显著地降低材料的性能。此外,关于Ag/g-C3N4在生物方面的研究还鲜有报道。
本发明的目的在于制备出颗粒较小且粒径均一的Ag纳米粒子并能强力附着于g-C3N4片层上,从而显著提高材料的抗菌、杀菌性能。负载的Ag纳米粒子可以加速g-C3N4产生了更多的·O2 -,·OH等自由基,而自由基可以有效地杀死带负电的大肠杆菌;多巴胺作为粘结剂,既可以将Ag纳米粒子固定到g-C3N4上,又作为转移电荷的桥梁,加速g-C3N4电子空穴分离;Ag纳米粒子的表面等离子体共振效应不仅可以拓宽g-C3N4半导体材料的可见光吸收范围,并且可以作为电子捕获阱捕获电子,加速光生电子与空穴的分离,有效抑制光生载流子的复合,同时g-C3N4表面上的Ag纳米粒子可以释放出微量的Ag+,通过库伦引力牢固地吸附在带负电荷的大肠杆菌细胞膜上,进而穿透细胞膜进入胞内,与巯基反应,使蛋白质凝固,从而破坏大肠杆菌合成酶的活性,并在短时间内使大肠杆菌产生机能障碍,干扰DNA合成的同时令细菌丧失分裂繁殖能力而死亡。
发明内容
本发明采用g-C3N4为模板,硝酸银为前驱体,用硼氢化钠冰水浴还原反应制备Ag/多巴胺/g-C3N4新型复合材料;该新型复合物具有优异的抗菌和杀菌性能,并且g-C3N4和多巴胺都是生物相容性材料,本身对细胞没有毒性。多巴胺能够在无机材料表面通过自身氧化聚合形成超强黏附性的聚多巴胺层,聚多巴胺分子中的邻苯二酚基团具有一定的还原性,能够将金、银等贵金属离子还原成单质。同时,金属纳米颗粒与无机材料能够通过聚多巴胺上的邻苯二酚和氨基官能团产生共价与非共价的相互作用,使贵金属纳米粒子可以强力地附着于g-C3N4材料表面上。
所述的一种新型的Ag/多巴胺/g-C3N4新型杀菌复合材料,所用原料为:尿素(分析纯)、AgNO3(分析纯)、盐酸多巴胺(分析纯)、硼氢化钠(分析纯)。
所述的制备工艺为:
(1)将盐酸多巴胺加入到g-C3N4水溶液,磁力搅拌后得盐酸多巴胺/g-C3N4溶液;
(2)将硝酸银水溶液,按照硝酸银水溶液和盐酸多巴胺/g-C3N4溶液体积比为1:1~1:4的比例混合,室温下磁力搅拌获得Ag+/盐酸多巴胺/g-C3N4悬浮液;
(3)将上述溶液置于冰水浴环境中,在磁力搅拌下,将硼氢化钠水溶液加入Ag+/盐酸多巴胺/g-C3N4悬浮液,搅拌后离心水洗,冷冻干燥后获得Ag/多巴胺/g-C3N4。
所述的步骤(1)中的盐酸多巴胺与g-C3N4水溶液的质量体积比为5-50mg:20ml,g-C3N4水溶液的浓度为1.5mg/ml,优选盐酸多巴胺与g-C3N4水溶液的质量体积比为40mg:20ml。
所述的步骤(2)中的硝酸银水溶液与盐酸多巴胺/g-C3N4溶液体积比为1:2;硝酸银水溶液的浓度为0.375mg/ml。
步骤(3)中,为了使硝酸银水溶液被充分还原,保证硝酸银与硼氢化钠物质的量之比应小于1:4,硼氢化钠水溶液与g-C3N4水溶液的体积比为5:2,硼氢化钠水溶液的浓度控制为27.5mM~6.9mM;硼氢化钠水溶液的加入速度为2ml/s;搅拌时间为12h。
所述的步骤(3)中的硼氢化钠溶液浓度13.7mM为佳。
本发明的优点在于:硝酸银在硼氢化钠和邻苯二酚基团还原作用下形成Ag纳米粒子,盐酸多巴胺与硼氢化钠中和形成的多巴胺具有强黏附作用能够将g-C3N4与Ag纳米颗粒紧密结合,形成Ag/多巴胺/g-C3N4。本材料通过硼氢化钠及多巴胺分子中邻苯二酚基团的还原性,制备出了一系列较小的Ag纳米粒子,并均匀地分散在g-C3N4上,使得该复合材料具有优异的抗菌和杀菌性能;此外,经过多巴胺修饰后的g-C3N4复合物表面形成的聚多巴胺层带正电荷,可以更好的作用于带负电荷的细胞,提高其抗菌和杀菌性能;复合后的g-C3N4产生了更多的·O2 -,·OH等自由基,而自由基可以有效地杀死带负电的大肠杆菌。同时,g-C3N4上的多巴胺是一种生物分子,含有儿茶酪和氨基官能团,这些官能团不仅能改善复合材料表面的亲水性能,又能赋予复合材料优异的生物相容性,从而这种材料可以重新分散在水中形成单分散的悬浮液,因此具有很大的实际应用前景。
附图说明
图1为实施例1的g-C3N4的TEM图。
图2为实施例1的Ag/多巴胺/g-C3N4(1:2)的TEM图。
图3为实施例1的Ag/多巴胺/g-C3N4(1:2)的SEM图。
图4为实施例2的g-C3N4与Ag/多巴胺/g-C3N4(1:1;1:2;1:4)的XRD图。
图5为实施例2的Ag/多巴胺/g-C3N4(1:1)的TEM图。
图6为实施例3的Ag/多巴胺/g-C3N4(1:2)复合材料在黑暗条件下对大肠杆菌的抗菌曲线图。
图7为实施例4的Ag/多巴胺/g-C3N4(1:2)复合材料在可见光照射下对大肠杆菌的抗菌曲线图。
具体实施方式
实施例1
Ag/多巴胺/g-C3N4(1:2)制备方法:
将40mg盐酸多巴胺加入到20ml 1.5mg/ml g-C3N4溶液,磁力搅拌后得盐酸多巴胺/g-C3N4溶液;制备浓度为0.375mg/ml的硝酸银水溶液,将上述硝酸银水溶液和盐酸多巴胺/g-C3N4溶液混合,室温下磁力搅拌12h,获得Ag+/盐酸多巴胺/g-C3N4悬浮液;所述硝酸银水溶液与盐酸多巴胺/g-C3N4溶液体积比为1:2;在冰水浴环境下搅拌,用可调式移液枪将50ml浓度为13.7mM的硼氢化钠水溶液以2ml/s的速度滴加入Ag+/盐酸多巴胺/g-C3N4悬浮液,搅拌12h并离心水洗,冷冻干燥后获得Ag/多巴胺/g-C3N4(1:2)复合材料。
图1为实施例1的g-C3N4的TEM图,从图中可以看出g-C3N4片层较薄。
图2为实施例1中Ag/多巴胺/g-C3N4(1:2)复合物的TEM图,图3为实施例1中Ag/多巴胺/g-C3N4(1:2)复合物的SEM图,可以看到尺寸为15-20nm的球形Ag纳米粒子负载在g-C3N4上,并且Ag纳米粒子在g-C3N4上分散得非常均匀,粒径宽度范围窄,非常适合抗菌和杀菌实验。
实施例2
实施例2考察硝酸银的加入量对Ag/多巴胺/g-C3N4复合材料XRD的影响。制备浓度为0.375mg/ml的硝酸银水溶液,将硝酸银水溶液和实施例一中的盐酸多巴胺/g-C3N4溶液混合,室温下磁力搅拌12小时,获得Ag+/盐酸多巴胺/g-C3N4悬浮液;所述硝酸银水溶液与盐酸多巴胺/g-C3N4溶液体积比分别为1:1、1:2、1:4;在冰水浴环境的搅拌下,分别用可调式移液枪将50ml浓度分别为27.5mM(Ag/多巴胺/g-C3N4 1:1),13.7mM(Ag/多巴胺/g-C3N41:2)和6.9mM(Ag/多巴胺/g-C3N41:4))的硼氢化钠水溶液加入上述混合溶液中,搅拌12h并离心水洗,冷冻干燥后获得Ag/多巴胺/g-C3N4(1:1;1:2;1:4)。
图4为Ag/多巴胺/g-C3N4与g-C3N4复合材料的XRD谱图,在复合物的XRD衍射光谱中出现了Ag明显的特征峰;在2θ为38.1°、44.4°、64.4°及77.3°处出现明显的狭窄特征衍射峰,分别对应面心立方Ag的(111)、(200)、(220)、(311)晶面,此外在27.5°处出现了宽的特征衍射峰,这是g-C3N4的(002)晶面衍射峰,XRD结果说明Ag/多巴胺/g-C3N4制备成功。随着复合材料中Ag含量的增加,Ag的四个特征峰的强度也随之增加,相应的g-C3N4(002)晶面衍射峰发生略微的减弱,此外在XRD图中并没有出现Ag2O等其他杂峰,表明实验成功制备得到不同Ag含量的Ag/多巴胺/g-C3N4复合材料。
图5为Ag/多巴胺/g-C3N4(1:1)复合材料的TEM图,随着硝酸银加入量的增加,g-C3N4上负载的银纳米颗粒也相应地增加,但是片层上的银纳米颗粒易发生团聚和堆叠现象,导致负载颗粒的牢固性减弱。
实施例3
实施例3主要考察Ag/多巴胺/g-C3N4(1:2)复合物在无光照条件下的抗菌性能,我们选用常规菌种大肠杆菌来考察其抗菌效果;黑暗条件下抗菌操作如下:取四只已灭菌的干净试管,分别编号1-4,无菌操作下向每只试管中分别加入一定量的LB培养液,然后在黑暗的条件下向每只编号试管中依次加入等量的浓度分别为0mg/L(ppm),35ppm,55ppm,75ppm,和95ppm四个浓度梯度的Ag/多巴胺/g-C3N4(1:2)复合材料悬浮液;震荡摇匀,测量每只试管中液体的OD值,然后向每只试管中接入等量的大肠杆菌培养液,接菌量为5%,即200uL,轻晃摇匀,再用紫外可见分光光度计依次测量每只试管中液体在波长600nm处光密度吸收值(OD)值;将试管放入37℃黑暗恒温震荡培养箱中培养,每隔1h依次从试管中用可调移液器取出等量(约100uL)的培养液,测量其OD600值,以此来监测大肠杆菌的生长情况;记录每次试样的OD600值,修正OD600值后,并绘制曲线图(图6)。
从图6中可以看到空白对照组的大肠杆菌样品的生长都呈现典型的生长曲线,而加入Ag/多巴胺/g-C3N4(1:2)复合材料后大肠杆菌的生长发生明显的变化,当Ag/多巴胺/g-C3N4(1:2)复合材料的浓度达到75ppm时,大肠杆菌的生长已经完全被抑制。由于银属于贵金属且具有一定的毒性,所以从抗菌性能、经济效益以及生物相容性等方面考虑,Ag/多巴胺/g-C3N4(1:2)新型复合材料在黑暗下比较适合用于抗菌实验。
实施例4
实施例4主要考察Ag/多巴胺/g-C3N4(1:2)复合物在可见光照射下的抗菌性能,我们选用常规菌种大肠杆菌来考察其抗菌效果;可见光照射下的抗菌操作如下:前期准备工作与黑暗下实验相同(同实施例3),在黑暗的条件下向每只编号试管中依次加入等量的浓度分别为0ppm,25ppm,45ppm,65ppm和85ppm四个浓度梯度的Ag/多巴胺/g-C3N4(1:2)复合材料悬浮液;震荡摇匀,然后向每只试管中接入等量的大肠杆菌培养液,接菌量为5%,即200uL,轻晃摇匀,再用紫外可见分光光度计依次测量每只试管中液体在波长600nm处光密度吸收值(OD)值。将试管放入300W氙灯(可见光)照射的37℃恒温震荡培养箱中培养,每隔1h依次从试管中用可调移液器取出等量(约100uL)的培养液,测量其OD600值,以此来监测大肠杆菌的生长情况;记录每次试样的OD600值,修正OD600值后,并绘制曲线图(图7)。
图7中可以看到空白对照组的大肠杆菌样品的生长都呈现典型的生长曲线,而加入复合材料后大肠杆菌的生长发生明显的变化,当复合材料的浓度达到45ppm时,大肠杆菌的生长已经完全被抑制。综合三种材料的抗菌性能、经济效益等方面,Ag/多巴胺/g-C3N4(1:2)新型复合材料较适合用于抗菌实验。同时,材料在可见光下的抗菌性能明显优于黑暗下的抗菌性能(降低了30ppm),这主要是由于在可见光下三者协同作用而造成的。
在可见光照射下后,负载的Ag纳米粒子可以加速g-C3N4产生了更多的·O2 -、·OH、电子、空穴等自由基,而自由基可以有效地杀死带负电的大肠杆菌;多巴胺既作为粘结剂,将Ag纳米粒子固定到g-C3N4上,又作为转移电荷的桥梁,加速g-C3N4电子空穴分离;Ag纳米粒子的表面等离子体共振效应不仅可以拓宽g-C3N4半导体材料的可见光吸收范围,并且可以作为电子捕获阱捕获电子,加速光生电子与空穴的分离,有效抑制光生载流子的复合,同时g-C3N4表面的Ag纳米粒子可以释放出微量的Ag+,通过库伦引力牢固地吸附在带负电荷的大肠杆菌细胞膜上,进而穿透细胞膜进入胞内,与巯基反应,使蛋白质凝固,从而破坏大肠杆菌合成酶的活性,并在短时间内使大肠杆菌产生机能障碍,干扰DNA合成的同时令细菌丧失分裂繁殖能力而死亡。
Claims (10)
1.一种Ag/多巴胺/g-C3N4可见光催化杀菌剂,其特征在于:所述的Ag/多巴胺/g-C3N4可见光催化杀菌剂具有优异的抗菌和杀菌性能;粒径均一的Ag纳米粒子均匀地附着于g-C3N4片层上,能够加速g-C3N4产生更多的e-,h+,·O2 -,·OH自由基,而自由基可以有效地杀死带负电的大肠杆菌;多巴胺作为粘结剂,既可以将Ag纳米粒子固定到g-C3N4上,又作为转移电荷的桥梁,加速g-C3N4电子空穴分离;Ag纳米粒子的表面等离子体共振效应不仅可以拓宽g-C3N4半导体材料的可见光吸收范围,并且可以作为电子捕获阱捕获电子,加速光生电子与空穴的分离,有效抑制光生载流子的复合,同时g-C3N4表面上的Ag纳米粒子可以释放出微量的Ag+,通过库伦引力牢固地吸附在带负电荷的大肠杆菌细胞膜上,并在短时间内使大肠杆菌产生机能障碍,干扰DNA合成的同时令细菌丧失分裂繁殖能力而死亡。
2.如权利要求1所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂,其特征在于:Ag纳米粒子的粒径为15-20nm。
3.如权利要求1所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:
(1)将盐酸多巴胺加入到g-C3N4水溶液,磁力搅拌后得盐酸多巴胺/g-C3N4溶液;
(2)将硝酸银水溶液,按照硝酸银水溶液和盐酸多巴胺/g-C3N4溶液体积比为1:1~1:4的比例与盐酸多巴胺/g-C3N4溶液混合,室温下磁力搅拌获得Ag+/盐酸多巴胺/g-C3N4悬浮液;
(3)将Ag+/盐酸多巴胺/g-C3N4悬浮液置于冰水浴环境中,在磁力搅拌下,将硼氢化钠水溶液加入Ag+/盐酸多巴胺/g-C3N4悬浮液中,搅拌后离心水洗,冷冻干燥后获得Ag/多巴胺/g-C3N4。
4.如权利要求3所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:所述的步骤(1)中的盐酸多巴胺与g-C3N4水溶液的质量体积比为5-50mg:20ml,g-C3N4水溶液的浓度为1.5mg/ml。
5.如权利要求4所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:盐酸多巴胺与g-C3N4水溶液的质量体积比为40mg:20ml。
6.如权利要求3所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:所述的步骤(2)中的硝酸银水溶液与盐酸多巴胺/g-C3N4溶液体积比为1:2;硝酸银水溶液的浓度为0.375mg/ml。
7.如权利要求3所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:步骤(3)中,为了使硝酸银水溶液被充分还原,保证硝酸银与硼氢化钠物质的量之比应小于1:4。
8.如权利要求7所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:硼氢化钠水溶液与g-C3N4水溶液的体积比为5:2,硼氢化钠水溶液的浓度控制为27.5mM~6.9mM。
9.如权利要求3所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:步骤(3)中,硼氢化钠水溶液的加入速度为2ml/s;所述搅拌时间为12h。
10.如权利要求8所述的一种Ag/多巴胺/g-C3N4可见光催化杀菌剂的制备方法,其特征在于:所述的步骤(3)中的硼氢化钠溶液浓度13.7mM。
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