CN114698648A - 一种纳米银负载的抗菌纤维纳米颗粒的制备方法 - Google Patents
一种纳米银负载的抗菌纤维纳米颗粒的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米银负载的抗菌纤维纳米颗粒的制备方法,将纤维素进行TEMPO氧化,再将氧化后的纤维素进行高压均质处理,得到纳米纤维素悬浮液,将纳米纤维素悬浮液与银离子水溶液进行银离子负载,得到纳米纤维素和硝酸银混合液,最后对纳米纤维素和硝酸银混合液进行喷雾干燥,得到纳米银颗粒负载的纤维素抗菌纳米颗粒。本发明制备的米银负载的抗菌纤维纳米颗粒尺寸均匀,分散性好,兼具纳米纤维素和纳米银颗粒的优越性能,可用于伤口敷料、包装等领域。
Description
技术领域
本发明涉及纤维素技术领域,特别是一种纳米银负载的抗菌纤维纳米颗粒的制备方法。
背景技术
植物纤维是地球上储量最多的可再生资源。纤维材料由于具有良好的生物相容、可降解、易化学改性等特性被广泛应用在各行各业。近年来,随着生活水平的不断提高和科技的不断进步,纤维基纳米材料逐渐成为新型材料的热点方向。
在全球疫情的大环境下,对抗菌材料的需求量越来越高。纳米银是一种光谱抗菌剂,通过释放银粒子与微生物发生接触反应,造成微生物共有成分破坏或产生功能障碍,起到抗菌的作用。目前纳米纤维素与纳米银的复合材料兼具机械强度高、生物相容性好和抗菌性能优异的特点,目前已有纤维素纤维负载纳米银的抗菌材料,但是样品仅限于悬浮液状态,储存条件要求高,并且易造成团聚。专利CN CN201510323487.1公开了一种片状纤维素纳米晶/纳米银杂化粒子的制备方法,此发明添加还原剂和有机分散剂,最终干燥成片状结构。值得注意的是,干燥后的样品均一性差,并且添加了大量化学助剂,导致其生物相容性差。因此如何通过简单的工艺,制备尺寸均一且干燥后产品易分散的纳米银负载的抗菌纤维纳米复合材料是急需解决的技术难题。
发明内容
本发明的目的在于,提供一种纳米银负载的抗菌纤维纳米颗粒的制备方法。本发明制备的米银负载的抗菌纤维纳米颗粒尺寸均匀,分散性好,兼具纳米纤维素和纳米银颗粒的优越性能,可用于伤口敷料、包装等领域。
本发明的技术方案:一种纳米银负载的抗菌纤维纳米颗粒的制备方法,将纤维素进行TEMPO氧化,再将氧化后的纤维素进行高压均质处理,得到纳米纤维素悬浮液,将纳米纤维素悬浮液与银离子水溶液进行银离子负载,得到纳米纤维素和硝酸银混合液,最后对纳米纤维素和硝酸银混合液进行喷雾干燥,得到纳米银颗粒负载的纤维素抗菌纳米颗粒。
前述的纳米银负载的抗菌纤维纳米颗粒的制备方法,所述纤维素的TEMPO氧化是按重量份向0.5-1.5份的纤维素加入80-120份去离子水,在5000rpm搅拌,然后加入0.012-0.018份的TEMPO、0.05-0.2份的NaBr和8-15份的NaClO,搅拌1-3小时,搅拌过程中采用氢氧化钠溶液调节pH,最后加入无水乙醇终止反应。
前述的纳米银负载的抗菌纤维纳米颗粒的制备方法,所述纤维素的TEMPO氧化是按重量份向1份的纤维素加入100份去离子水,在5000rpm搅拌,然后加入0.016份的TEMPO、0.1份的NaBr和10份的NaClO,搅拌2小时,搅拌过程中采用0.5mol的氢氧化钠溶液调节pH10-10.5,最后加入5-10份无水乙醇终止反应。
前述的纳米银负载的抗菌纤维纳米颗粒的制备方法,所高压均质处理的压力为5000-25000psi,处理次数为1-10次。
前述的纳米银负载的抗菌纤维纳米颗粒的制备方法,所述的银离子负载是将浓度为0.1-2mmol的银离子溶液与纳米纤维素悬浮液混合,避光静置20-30小时,得到纳米纤维素和硝酸银混合液。
前述的纳米银负载的抗菌纤维纳米颗粒的制备方法,所述的喷雾干燥处理的条件为进气温度100℃-150℃,出口温度60℃-90℃,空气流速为3.5-3.9m/s,进样速度为400-700mL/h。
前述的纳米银负载的抗菌纤维纳米颗粒的制备方法,所述的纤维素为微晶纤维素、棉花、竹纤维、木浆、细菌纤维素、麻纤维中的一种或几种。
前述的纳米银负载的抗菌纤维纳米颗粒的制备方法,所述纳米银颗粒负载的纤维素抗菌纳米颗粒的直径为100-2000nm,其中的纳米银的粒径30-100nm。
与现有技术相比,本发明所用原料为植物纤维素,采用TEMPO进行选择性氧化纤维素,经过高压均质得到纳米纤维素,浸泡在含有银粒子溶液中,无需添加任何还原剂的前提下,通过喷雾干燥得到表明负载纳米银的纤维素纳米颗粒。本发明得到的是纳米银负载的抗菌纤维纳米颗粒,其颗粒均匀,在分散性好,抗菌性能优异,易保存和运输,在纳米材料、食品、医药等领域有着广泛的应用前景。同时本发明在不需要还原剂的基础上成功制备了纳米银负载的抗菌纤维纳米颗粒,采用喷雾干燥的方法制备,获得可调控颗粒大小的纳米银负载的抗菌纤维纳米颗粒,避免了添加还原剂造成的环境污染等问题。
附图说明
图1为实施例3制得的纳米银负载的抗菌纤维纳米颗粒的形貌图;
图2为实施例4制得的纳米银负载的抗菌纤维纳米颗粒的形貌图;
图3为实施例5制得的纳米银负载的抗菌纤维纳米颗粒的形貌图;
图4为纳米银负载的抗菌纤维纳米颗粒的放大形貌图。
具体实施方式
下面结合附图和实施例对本发明作进一步说明,但并不作为对本发明限制的依据。
实施例1:一种纳米银负载的抗菌纤维纳米颗粒的制备方法
(1)取1g绝干木浆加入,加入100mL去离子水,5000rpm搅拌制得纤维素溶液,向纤维素溶液中加入0.022g的TEMPO(2,2,6,6-四甲基哌啶-1-氧自由基,下同)和0.09g的NaBr,再加入9mL的NaClO,搅拌1小时,搅拌过程中用0.5Mol的氢氧化钠溶液调节pH值维持在10-10.5,最后加入5mL无水乙醇终止反应;
(2)将(1)所得氧化的纤维悬浮液进行高压均质,在6000psi压力下均质3次,8000psi压力下均质2次,得到纳米纤维素悬浮液;
(3)将0.5mmol的硝酸银溶液与(2)得到纳米纤维素悬浮液混合静置,避光25h,得到纳米纤维素和硝酸银混合液;
(4)将(3)得到的纳米纤维素和硝酸银进行喷雾干燥,进气温度120℃,出口温度70℃,空气流速为3.5m/s,进样速度为400mL/h,即得到纳米银负载的抗菌纤维纳米颗粒。
实施例2:一种纳米银负载的抗菌纤维纳米颗粒的制备方法
(1)取1g绝干木浆加入,加入100mL去离子水,5000rpm搅拌制得纤维素溶液,向纤维素溶液中加入0.025g的TEMPO(2,2,6,6-四甲基哌啶-1-氧自由基,下同)和0.12g的NaBr,再加入12mL的NaClO,搅拌1小时,搅拌过程中用0.5Mol的氢氧化钠溶液调节pH值维持在10-10.5,最后加入5mL无水乙醇终止反应;
(2)将(1)所得氧化的纤维悬浮液进行高压均质,在5000psi压力下均质4次,7000psi压力下均质3次,得到纳米纤维素悬浮液;
(3)将0.5mmol的硝酸银溶液与(2)得到纳米纤维素悬浮液混合静置,避光30,得到纳米纤维素和硝酸银混合液;
(4)将(3)得到的纳米纤维素和硝酸银进行喷雾干燥,进气温度140℃,出口温度80℃,空气流速为3.8m/s,进样速度为600mL/h,即得到纳米银负载的抗菌纤维纳米颗粒。
实施例3:一种纳米银负载的抗菌纤维纳米颗粒的制备方法
(1)取1g绝干木浆加入,加入100mL去离子水,5000rpm搅拌,制得纤维素溶液,向纤维素溶液中加入0.016g的TEMPO和0.1g的NaBr,再加入10mL的NaClO,搅拌过程中用0.5Mol的氢氧化钠溶液调节pH值维持在10-10.5,最后加入5mL无水乙醇终止反应;
(2)将(1)所得氧化的纤维悬浮液进行高压均质,在5000psi压力下均质2次,10000psi压力下均质2次,得到纳米纤维素悬浮液;
(3)将0.5mmol的硝酸银溶液与(2)得到纳米纤维素悬浮液混合静置,避光24h,得到纳米纤维素和硝酸银混合液;
(4)将(3)得到的混合液进行喷雾干燥,进气温度120℃,出口温度70℃,空气流速为3.5m/s,进样速度为400mL/h,即得到纳米银负载的抗菌纤维纳米颗粒。
实施例4:一种纳米银负载的抗菌纤维纳米颗粒的制备方法
(1)取1g绝干木浆加入,加入100mL去离子水,5000rpm搅拌,制得纤维素溶液,向纤维素溶液中加入0.016g的TEMPO、0.1g的NaBr,再加入10mL的NaClO,搅拌过程中用0.5mol的氢氧化钠溶液调节pH值维持在10-10.5,搅拌2小时,最后加入5mL无水乙醇终止反应;
(2)将(1)所得氧化的纤维悬浮液进行高压均质,在5000psi压力下均质2次,10000psi压力下均质2次,20000psi压力下均质3次,得到纳米纤维素悬浮液;
(3)将1mmol的硝酸银溶液与(2)得到纳米纤维素悬浮液混合静置,避光24h,得到纳米纤维素/硝酸银混合液;
(4)将(3)得到的混合液进行喷雾干燥,进气温度130℃,出口温度80℃,空气流速为3.8m/s,进样速度为500mL/h,即得到纳米银负载的抗菌纤维纳米颗粒。
实施例5:一种纳米银负载的抗菌纤维纳米颗粒的制备方法
(1)取1g绝干木浆加入,加入100mL去离子水,5000rpm搅拌,制得纤维素溶液,向纤维素溶液中加入0.016g的TEMPO和0.1g的NaBr,再加入10mL的NaClO,搅拌过程中用0.5mol的氢氧化钠溶液调节pH值维持在10-10.5,搅拌4小时,最后加入5mL无水乙醇终止反应;
(2)将(1)所得氧化的纤维悬浮液进行高压均质,在5000psi压力下均质2次,10000psi压力下均质2次,20000psi压力下均质3次,25000psi压力下均质3次,得到纳米纤维素悬浮液;
(3)将2mmol的硝酸银溶液与(2)得到纳米纤维素悬浮液混合静置,避光24h,得到纳米纤维素/硝酸银混合液;
(4)将(3)得到的混合液进行喷雾干燥,进气温度150℃,出口温度90℃,空气流速为3.9m/s,进样速度为600mL/h,即得到纳米银负载的抗菌纤维纳米颗粒。
申请人对实施例3-5制得的纳米银负载的抗菌纤维纳米颗粒进行形貌观察,得到了如图1所示的实施例3制得的纳米银负载的抗菌纤维纳米颗粒的形貌图,如图2所示实施例4制得的纳米银负载的抗菌纤维纳米颗粒的形貌图和如图3所示的实施例5制得的纳米银负载的抗菌纤维纳米颗粒的形貌图,同时对纳米银负载的抗菌纤维纳米颗粒形貌进行了放大观察,其结果如图4所示。从图1-4中可以看出,本发明制备得到的纳米银负载的抗菌纤维纳米颗粒,其颗粒均匀,分散性好,一致性好,无团聚现象,兼具纳米纤维素和纳米银颗粒的优越性能抗菌性能优异,易保存和运输,在纳米材料、食品、医药等领域有着广泛的应用前景。同时本发明在不需要还原剂的基础上成功制备了纳米银负载的抗菌纤维纳米颗粒,采用喷雾干燥的方法制备,获得可调控颗粒大小的纳米银负载的抗菌纤维纳米颗粒,避免了添加还原剂造成的环境污染等问题。
Claims (8)
1.一种纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:将纤维素进行TEMPO氧化,再将氧化后的纤维素进行高压均质处理,得到纳米纤维素悬浮液,将纳米纤维素悬浮液与银离子水溶液进行银离子负载,得到纳米纤维素和硝酸银混合液,最后对纳米纤维素和硝酸银混合液进行喷雾干燥,得到纳米银颗粒负载的纤维素抗菌纳米颗粒。
2.根据权利要求1所述的纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:所述纤维素的TEMPO氧化是按重量份向0.5-1.5份的纤维素加入80-120份去离子水,然后加入0.008-0.025份的TEMPO、0.05-0.2份的NaBr和8-15份的NaClO,搅拌1-5小时,搅拌过程中采用氢氧化钠溶液调节pH,最后加入无水乙醇终止反应。
3.根据权利要求2所述的纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:所述纤维素的TEMPO氧化是按重量份向1份的纤维素加入100份去离子水,在5000rpm搅拌,然后加入0.016份的TEMPO、0.1份的NaBr和10份的NaClO,搅拌2小时,搅拌过程中采用0.5mol的氢氧化钠溶液调节pH10-10.5,最后加入5-10份无水乙醇终止反应。
4.根据权利要求1所述的纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:所高压均质处理的压力为5000-25000psi,处理次数为1-10次。
5.根据权利要求1所述的纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:所述的银离子负载是将浓度为0.1-2mmol的银离子溶液与纳米纤维素悬浮液混合,避光静置20-30小时,得到纳米纤维素和硝酸银混合液。
6.根据权利要求1所述的纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:所述的喷雾干燥处理的条件为进气温度100℃-150℃,出口温度60℃-90℃,空气流速为3.5-3.9m/s,进样速度为400-700mL/h。
7.根据权利要求1所述的纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:所述的纤维素为微晶纤维素、棉花、竹纤维、木浆、细菌纤维素、麻纤维中的一种或几种。
8.根据权利要求1所述的纳米银负载的抗菌纤维纳米颗粒的制备方法,其特征在于:所述纳米银颗粒负载的纤维素抗菌纳米颗粒的直径为100-2000nm,其中的纳米银的粒径30-100nm。
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