CN108939708A - 一种空气杀菌过滤膜的制备方法 - Google Patents
一种空气杀菌过滤膜的制备方法 Download PDFInfo
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- CN108939708A CN108939708A CN201810668930.2A CN201810668930A CN108939708A CN 108939708 A CN108939708 A CN 108939708A CN 201810668930 A CN201810668930 A CN 201810668930A CN 108939708 A CN108939708 A CN 108939708A
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- Chemical Kinetics & Catalysis (AREA)
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- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
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- Cosmetics (AREA)
Abstract
本发明公开了一种空气杀菌过滤膜的制备方法,属于空气净化材料技术领域。将预处理杀菌膜与改性壳聚糖混合物按质量比1:5~1:8混合,并加入预处理杀菌膜质量0.1~0.2倍的甘油,搅拌混合后过滤,得改性杀菌膜,将改性明胶与水按质量比1:10~1:15混合,并调节pH至2.2~2.5,得处理液,将改性杀菌膜与处理液按质量比1:10~1:15混合,并加入改性杀菌膜质量0.3~0.4倍的戊二醛,搅拌混合后,调节pH至4.2~4.5,过滤,真空干燥,得空气杀菌过滤膜。本发明技术方案制备的空气杀菌过滤膜具有优异的过滤性能和杀菌性能的特点,在空气净化材料行业的发展中具有广阔的前景。
Description
技术领域
本发明公开了一种空气杀菌过滤膜的制备方法,属于空气净化材料技术领域。
背景技术
PM2.5与PM10带来的危害已引起广泛的关注,而过滤是应用最为广泛的空气净化的方法,因此空气过滤设备成为了研究热点,其核心过滤材料的研究和开发更是成为了重中之重。传统的空气过滤材料主要包括石棉纤维、聚酯与聚丙烯腈等合成纤维、玻璃纤维等,但其仅对0.3μm以上的微粒有较高的过滤效率,对亚微米微粒以及其他较小的病原体难以实现有效过滤。过滤净化技术理论的研究在20世纪迅速发展,相应的过滤理论也逐渐建立,而空气过滤器的发展只有短短20多年的历史。
过滤是利用介质将悬浮液体或气体中的固体物质截留,而液体或气体则穿过介质被澄清或净化。人们在生产、生活中利用过滤技术已有几千年的历史了,用过滤材料滤除病毒、细菌是近几十年来伴随着新型材料的发展而兴起的新方向,也是近年来的研究热点,随着人们的环保意识日益增强,对生活品质的要求日益提高,过滤除菌用净化材料也得到了快速发展和广泛应用。过滤细菌用净化材料包括无机物和有机高聚物,无机物用于制备过滤除菌材料的时间比较早,在1915年,硅藻土过滤技术就被应用于小型水处理装置。由无机材料制成的孔径在微米或纳米级的过滤材料,具有结构稳定,耐高温高压、耐酸碱、耐有机溶剂、抗微生物侵蚀、不老化、寿命长、化学稳定性和机械强度大、孔径均一,易于进行化学清洗的特点。而传统的空气杀菌过滤膜还存在过滤效果和杀菌性不佳的缺点。
因此,如何改善传空气杀菌过滤膜存在的过滤效果和杀菌性不佳的缺点,以求探索研制出具有良好综合性能的空气杀菌过滤膜是待解决的问题。
发明内容
本发明主要解决的技术问题是:针对传空气杀菌过滤膜存在的过滤效果和杀菌性不佳的缺点,提供了一种空气杀菌过滤膜的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种空气杀菌过滤膜的制备方法,具体制备步骤为:
(1)将胶原蛋白与超纯水按质量比1:50~1:55混合,并加入超纯水质量0.5~0.6倍的硫氰酸钠,搅拌混合,得胶原蛋白溶液,将胶原蛋白溶液与丙烯腈按质量比55:1~60:1混合,并加入丙烯腈质量0.02~0.04倍的引发剂,搅拌反应后,得改性胶原蛋白混合物;
(2)将改性胶原蛋白混合物与水按质量比1:100~1:120混合,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:2~1:3混合,并加入改性胶原蛋白质量0.1~0.2倍的改性磁性颗粒和改性胶原蛋白质量40~50倍的N,N-二甲基甲酰胺,磁力搅拌混合后,得纺丝液,将纺丝液静电纺丝成膜后,真空干燥,得预处理杀菌膜;
(3)将壳聚糖与乙酸按质量比1:100~5:100混合,并加入壳聚糖质量2~3倍的硝酸铈溶液和壳聚糖质量0.5~0.6倍的混合单体,于氮气氛围下搅拌混合后,得改性壳聚糖混合物;
(4)将纳米四氧化三铁与无水乙醇按质量比1:50~1:60混合,超声分散后,加入无水乙醇质量0.1~0.2倍的钛酸四丁酯,密封静置后,洗涤干燥,煅烧,得预处理二氧化钛;
(5)将明胶与水按质量比1:8~1:12混合,并调节pH至7.0~7.5,加入明胶质量0.4~0.5倍的预处理二氧化钛和明胶质量0.1~0.2倍的硅烷偶联剂,搅拌混合后,调节pH至4.0~4.2,真空干燥,粉碎过筛,得改性明胶;
(6)将预处理杀菌膜与改性壳聚糖混合物按质量比1:5~1:8混合,并加入预处理杀菌膜质量0.1~0.2倍的甘油,搅拌混合后过滤,得改性杀菌膜,将改性明胶与水按质量比1:10~1:15混合,并调节pH至2.2~2.5,得处理液,将改性杀菌膜与处理液按质量比1:10~1:15混合,并加入改性杀菌膜质量0.3~0.4倍的戊二醛,搅拌混合后,调节pH至4.2~4.5,过滤,真空干燥,得空气杀菌过滤膜。
步骤(1)所述引发剂为过硫酸钾,过硫酸铵或过硫酸钠中任意一种。
步骤(2)改性磁性颗粒的制备方法为将正硅酸乙酯与无水乙醇按质量比1:6~1:8混合,并加入正硅酸乙酯质量0.5~0.8倍的四氧化三铁,超声分散后,加入正硅酸乙酯质量1~2倍的氨水,搅拌混合后,磁吸分离,洗涤,干燥,得预处理磁性颗粒,将预处理磁性颗粒与硅烷偶联剂KH-550按质量比1:5~1:8混合,浸泡,过滤,得改性磁性颗粒。
步骤(2)所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。
步骤(3)所述壳聚糖为脱乙酰度65~95%的壳聚糖混合物。
步骤(3)所述混合单体为将丙烯酰胺与丙烯酸按质量比1:1~2:1混合,得混合单体。
步骤(5)所述硅烷偶联剂为硅烷偶联剂KH-550,硅烷偶联剂KH-560或硅烷偶联剂KH-570中任意一种。
本发明的有益效果是:
(1)本发明在制备空气杀菌过滤膜时对杀菌膜进行预处理,首先,杀菌膜在经过预处理后,聚丙烯腈纤维内部含有胶原蛋白纤维,在加入产品中后,可使聚丙烯腈纤维具有较好的弹性,并且使聚丙烯腈纤维表面具有较多的活性基团,从而为基料膜后续处理提供反应的可能,其次,经过预处理后的杀菌膜内部含有改性磁性颗粒,改性磁性颗粒可在搅拌过程中在磁粒的作用下均匀分布于杀菌膜的纺丝液中,并且可在硅烷偶联剂的作用下与丙烯腈结合,从而使产品具有较好的杀菌效果;
(2)本发明在制备空气杀菌过滤膜时对预处理杀菌膜进行改性处理,并用处理液对改性杀菌膜进行后续处理,一方面,在改性处理后,预处理杀菌膜可与改性壳聚糖混合物中的改性壳聚糖发生交联,从而使预处理杀菌膜结构复杂化,进而使产品的过滤效果提高,并且由于壳聚糖在改性后具有絮凝性和杀菌性,从而使产品的过滤效果提高,杀菌性增强,另一方面,在用处理液对改性杀菌膜进行处理后,处理液中的明胶可在戊二醛和预处理二氧化钛的作用下吸附于聚丙烯腈纤维表面,从而增大产品与空气的接触面积,并且由于明胶中含有戊二醛,可在使用过程中缓慢释放,可与预处理二氧化钛一同起到杀菌作用,进而使产品的杀菌性能和过滤性能进一步提高。
具体实施方式
将正硅酸乙酯与无水乙醇按质量比1:6~1:8混合于烧杯中,并向烧杯中加入正硅酸乙酯质量0.5~0.8倍的四氧化三铁,于频率为45~55kHz的条件下超声分散15~20min后,向烧杯中加入正硅酸乙酯质量1~2倍的质量分数为15~25%的氨水,于温度为40~50℃,转速为200~250r/min的条件下搅拌混合12~15h后,磁吸分离,得预处理磁性颗粒坯料,将预处理磁性颗粒坯料用去离子水洗涤5~8次后,于温度为70~80℃的条件下干燥1~5h后,得预处理磁性颗粒,将预处理磁性颗粒与硅烷偶联剂KH-550按质量比1:5~1:8混合,于室温条件下浸泡2~3h后,过滤,得改性磁性颗粒;将胶原蛋白与超纯水按质量比1:50~1:55混合,并向胶原蛋白与超纯水的混合物中加入超纯水质量0.5~0.6倍的硫氰酸钠,于温度为50~55℃,转速为250~350r/min的条件下搅拌混合30~40min,得胶原蛋白溶液,将胶原蛋白溶液与丙烯腈按质量比55:1~60:1混合于烧瓶中,并向烧瓶中加入丙烯腈质量0.02~0.04倍的引发剂,于温度为68~75℃,转速为230~350r/min的条件下搅拌反应1~2h后,得改性胶原蛋白混合物;将改性胶原蛋白混合物与水按质量比1:100~1:120混合,于温度为45~55℃,转速为200~300r/min的条件下搅拌混合15~30min后,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:2~1:3混合于三口烧瓶中,并向三口烧瓶中加入改性胶原蛋白质量0.1~0.2倍的改性磁性颗粒和改性胶原蛋白质量40~50倍的N,N-二甲基甲酰胺,将三口烧瓶移入数显测速恒温磁力搅拌器,于温度为55~75℃,转速为300~350r/min的条件下搅拌混合6~8h后,得纺丝液,将纺丝液静电纺丝成膜后,于温度为60~80℃的条件下真空干燥30~40min后,得预处理杀菌膜;将壳聚糖与质量分数为20~28%的乙酸按质量比1:100~5:100混合于四口烧瓶中,并向四口烧瓶中加入壳聚糖质量2~3倍的质量分数为5~12%的硝酸铈溶液和壳聚糖质量0.5~0.6倍的混合单体,向四口烧瓶中以15~30mL/min的速率通入氮气,并于温度为40~45℃,转速为300~400r/min的条件下搅拌混合40~50min后,得改性壳聚糖混合物;将纳米四氧化三铁与无水乙醇按质量比1:50~1:60混合,于频率为45~55kHz的条件下超声分散15~25min后,向纳米四氧化三铁与无水乙醇的混合物中加入无水乙醇质量0.1~0.2倍的钛酸四丁酯,于温度为80~85℃的条件下密封静置10~15h后,得预处理二氧化钛坯料,将预处理二氧化钛坯料洗涤5~6次后,于温度为80~90℃的条件下干燥1~2h后,于氮气保护下,于温度为350~400℃的条件下煅烧1~2h后,得预处理二氧化钛;将明胶与水按质量比1:8~1:12混合,并用质量分数为10~15%的氨水调节明胶与水混合物的pH至7.0~7.5,向明胶与水的混合物中加入明胶质量0.4~0.5倍的预处理二氧化钛和明胶质量0.1~0.2倍的硅烷偶联剂,于温度为45~55℃,转速为300~400r/min的条件下搅拌混合30~60min后,得改性明胶坯料,用质量分数为10~15%的乙酸调节改性明胶坯料的pH至4.0~4.2后,真空干燥,粉碎过120目筛,得改性明胶;将预处理杀菌膜与改性壳聚糖混合物按质量比1:5~1:8混合于锥形瓶中,并向锥形瓶中加入预处理杀菌膜质量0.1~0.2倍的甘油,于温度为55~60℃,转速为150~250r/min的条件下搅拌混合1~3h后,过滤,得改性杀菌膜,将改性明胶与水按质量比1:10~1:15混合,于温度为45~55℃,转速为300~350r/min的条件下,搅拌混合30~50min后,并用质量分数为15~25%的乙酸调节改性明胶与水混合物的pH至2.2~2.5,得处理液,将改性杀菌膜与处理液按质量比1:10~1:15混合,并向改性杀菌膜与处理液的混合物中加入改性杀菌膜质量0.3~0.4倍的戊二醛,于温度为40~50℃,转速为180~280r/min的条件下搅拌混合30~60min后,用质量分数为20~25%的氨水调节改性杀菌膜与处理液混合物的pH至4.2~4.5后,过滤,得滤饼,将滤饼于温度55~60℃的条件下真空干燥1~2h后,得空气杀菌过滤膜。所述引发剂为过硫酸钾,过硫酸铵或过硫酸钠中任意一种。所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。所述壳聚糖为脱乙酰度65~95%的壳聚糖混合物。所述混合单体为将丙烯酰胺与丙烯酸按质量比1:1~2:1混合,得混合单体。所述硅烷偶联剂为硅烷偶联剂KH-550,硅烷偶联剂-560或硅烷偶联剂KH-570中任意一种。
将正硅酸乙酯与无水乙醇按质量比1:8混合于烧杯中,并向烧杯中加入正硅酸乙酯质量0.8倍的四氧化三铁,于频率为55kHz的条件下超声分散20min后,向烧杯中加入正硅酸乙酯质量2倍的质量分数为25%的氨水,于温度为50℃,转速为250r/min的条件下搅拌混合15h后,磁吸分离,得预处理磁性颗粒坯料,将预处理磁性颗粒坯料用去离子水洗涤8次后,于温度为80℃的条件下干燥5h后,得预处理磁性颗粒,将预处理磁性颗粒与硅烷偶联剂KH-550按质量比1:8混合,于室温条件下浸泡3h后,过滤,得改性磁性颗粒;将胶原蛋白与超纯水按质量比1:55混合,并向胶原蛋白与超纯水的混合物中加入超纯水质量0.6倍的硫氰酸钠,于温度为55℃,转速为350r/min的条件下搅拌混合40min,得胶原蛋白溶液,将胶原蛋白溶液与丙烯腈按质量比60:1混合于烧瓶中,并向烧瓶中加入丙烯腈质量0.04倍的引发剂,于温度为75℃,转速为350r/min的条件下搅拌反应2h后,得改性胶原蛋白混合物;将改性胶原蛋白混合物与水按质量比1:120混合,于温度为55℃,转速为300r/min的条件下搅拌混合30min后,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:3混合于三口烧瓶中,并向三口烧瓶中加入改性胶原蛋白质量0.2倍的改性磁性颗粒和改性胶原蛋白质量50倍的N,N-二甲基甲酰胺,将三口烧瓶移入数显测速恒温磁力搅拌器,于温度为75℃,转速为350r/min的条件下搅拌混合8h后,得纺丝液,将纺丝液静电纺丝成膜后,于温度为80℃的条件下真空干燥40min后,得预处理杀菌膜;将壳聚糖与质量分数为28%的乙酸按质量比5:100混合于四口烧瓶中,并向四口烧瓶中加入壳聚糖质量3倍的质量分数为12%的硝酸铈溶液和壳聚糖质量0.6倍的混合单体,向四口烧瓶中以30mL/min的速率通入氮气,并于温度为45℃,转速为400r/min的条件下搅拌混合50min后,得改性壳聚糖混合物;将纳米四氧化三铁与无水乙醇按质量比1:60混合,于频率为55kHz的条件下超声分散25min后,向纳米四氧化三铁与无水乙醇的混合物中加入无水乙醇质量0.2倍的钛酸四丁酯,于温度为85℃的条件下密封静置15h后,得预处理二氧化钛坯料,将预处理二氧化钛坯料洗涤6次后,于温度为90℃的条件下干燥2h后,于氮气保护下,于温度为400℃的条件下煅烧2h后,得预处理二氧化钛;将明胶与水按质量比1:12混合,并用质量分数为15%的氨水调节明胶与水混合物的pH至7.5,向明胶与水的混合物中加入明胶质量0.5倍的预处理二氧化钛和明胶质量0.2倍的硅烷偶联剂,于温度为55℃,转速为400r/min的条件下搅拌混合60min后,得改性明胶坯料,用质量分数为15%的乙酸调节改性明胶坯料的pH至4.2后,真空干燥,粉碎过120目筛,得改性明胶;将预处理杀菌膜与改性壳聚糖混合物按质量比1:8混合于锥形瓶中,并向锥形瓶中加入预处理杀菌膜质量0.2倍的甘油,于温度为60℃,转速为250r/min的条件下搅拌混合3h后,过滤,得改性杀菌膜,将改性明胶与水按质量比1:15混合,于温度55℃,转速为350r/min的条件下,搅拌混合50min后,并用质量分数为25%的乙酸调节改性明胶与水混合物的pH至2.5,得处理液,将改性杀菌膜与处理液按质量比1:15混合,并向改性杀菌膜与处理液的混合物中加入改性杀菌膜质量0.4倍的戊二醛,于温度为50℃,转速为280r/min的条件下搅拌混合60min后,用质量分数为25%的氨水调节改性杀菌膜与处理液混合物的pH至4.5后,过滤,得滤饼,将滤饼于温度60℃的条件下真空干燥2h后,得空气杀菌过滤膜。所述引发剂为过硫酸钾。所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。所述壳聚糖为脱乙酰度95%的壳聚糖混合物。所述混合单体为将丙烯酰胺与丙烯酸按质量比2:1混合,得混合单体。所述硅烷偶联剂为硅烷偶联剂KH-550。
将胶原蛋白与水按质量比1:120混合,于温度为55℃,转速为300r/min的条件下搅拌混合30min后,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:3混合于三口烧瓶中,并向三口烧瓶中加入改性胶原蛋白质量0.2倍的改性磁性颗粒和改性胶原蛋白质量50倍的N,N-二甲基甲酰胺,将三口烧瓶移入数显测速恒温磁力搅拌器,于温度为75℃,转速为350r/min的条件下搅拌混合8h后,得纺丝液,将纺丝液静电纺丝成膜后,于温度为80℃的条件下真空干燥40min后,得预处理杀菌膜;将壳聚糖与质量分数为28%的乙酸按质量比5:100混合于四口烧瓶中,并向四口烧瓶中加入壳聚糖质量3倍的质量分数为12%的硝酸铈溶液和壳聚糖质量0.6倍的混合单体,向四口烧瓶中以30mL/min的速率通入氮气,并于温度为45℃,转速为400r/min的条件下搅拌混合50min后,得改性壳聚糖混合物;将纳米四氧化三铁与无水乙醇按质量比1:60混合,于频率为55kHz的条件下超声分散25min后,向纳米四氧化三铁与无水乙醇的混合物中加入无水乙醇质量0.2倍的钛酸四丁酯,于温度为85℃的条件下密封静置15h后,得预处理二氧化钛坯料,将预处理二氧化钛坯料洗涤6次后,于温度为90℃的条件下干燥2h后,于氮气保护下,于温度为400℃的条件下煅烧2h后,得预处理二氧化钛;将明胶与水按质量比1:12混合,并用质量分数为15%的氨水调节明胶与水混合物的pH至7.5,向明胶与水的混合物中加入明胶质量0.5倍的预处理二氧化钛和明胶质量0.2倍的硅烷偶联剂,于温度为55℃,转速为400r/min的条件下搅拌混合60min后,得改性明胶坯料,用质量分数为15%的乙酸调节改性明胶坯料的pH至4.2后,真空干燥,粉碎过120目筛,得改性明胶;将预处理杀菌膜与改性壳聚糖混合物按质量比1:8混合于锥形瓶中,并向锥形瓶中加入预处理杀菌膜质量0.2倍的甘油,于温度为60℃,转速为250r/min的条件下搅拌混合3h后,过滤,得改性杀菌膜,将改性明胶与水按质量比1:15混合,于温度55℃,转速为350r/min的条件下,搅拌混合50min后,并用质量分数为25%的乙酸调节改性明胶与水混合物的pH至2.5,得处理液,将改性杀菌膜与处理液按质量比1:15混合,并向改性杀菌膜与处理液的混合物中加入改性杀菌膜质量0.4倍的戊二醛,于温度为50℃,转速为280r/min的条件下搅拌混合60min后,用质量分数为25%的氨水调节改性杀菌膜与处理液混合物的pH至4.5后,过滤,得滤饼,将滤饼于温度60℃的条件下真空干燥2h后,得空气杀菌过滤膜。所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。所述壳聚糖为脱乙酰度95%的壳聚糖混合物。所述混合单体为将丙烯酰胺与丙烯酸按质量比2:1混合,得混合单体。所述硅烷偶联剂为硅烷偶联剂KH-550。
将胶原蛋白与超纯水按质量比1:55混合,并向胶原蛋白与超纯水的混合物中加入超纯水质量0.6倍的硫氰酸钠,于温度为55℃,转速为350r/min的条件下搅拌混合40min,得胶原蛋白溶液,将胶原蛋白溶液与丙烯腈按质量比60:1混合于烧瓶中,并向烧瓶中加入丙烯腈质量0.04倍的引发剂,于温度为75℃,转速为350r/min的条件下搅拌反应2h后,得改性胶原蛋白混合物;将改性胶原蛋白混合物与水按质量比1:120混合,于温度为55℃,转速为300r/min的条件下搅拌混合30min后,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:3混合于三口烧瓶中,并向三口烧瓶中加入改性胶原蛋白质量50倍的N,N-二甲基甲酰胺,将三口烧瓶移入数显测速恒温磁力搅拌器,于温度为75℃,转速为350r/min的条件下搅拌混合8h后,得纺丝液,将纺丝液静电纺丝成膜后,于温度为80℃的条件下真空干燥40min后,得预处理杀菌膜;将壳聚糖与质量分数为28%的乙酸按质量比5:100混合于四口烧瓶中,并向四口烧瓶中加入壳聚糖质量3倍的质量分数为12%的硝酸铈溶液和壳聚糖质量0.6倍的混合单体,向四口烧瓶中以30mL/min的速率通入氮气,并于温度为45℃,转速为400r/min的条件下搅拌混合50min后,得改性壳聚糖混合物;将纳米四氧化三铁与无水乙醇按质量比1:60混合,于频率为55kHz的条件下超声分散25min后,向纳米四氧化三铁与无水乙醇的混合物中加入无水乙醇质量0.2倍的钛酸四丁酯,于温度为85℃的条件下密封静置15h后,得预处理二氧化钛坯料,将预处理二氧化钛坯料洗涤6次后,于温度为90℃的条件下干燥2h后,于氮气保护下,于温度为400℃的条件下煅烧2h后,得预处理二氧化钛;将明胶与水按质量比1:12混合,并用质量分数为15%的氨水调节明胶与水混合物的pH至7.5,向明胶与水的混合物中加入明胶质量0.5倍的预处理二氧化钛和明胶质量0.2倍的硅烷偶联剂,于温度为55℃,转速为400r/min的条件下搅拌混合60min后,得改性明胶坯料,用质量分数为15%的乙酸调节改性明胶坯料的pH至4.2后,真空干燥,粉碎过120目筛,得改性明胶;将预处理杀菌膜与改性壳聚糖混合物按质量比1:8混合于锥形瓶中,并向锥形瓶中加入预处理杀菌膜质量0.2倍的甘油,于温度为60℃,转速为250r/min的条件下搅拌混合3h后,过滤,得改性杀菌膜,将改性明胶与水按质量比1:15混合,于温度55℃,转速为350r/min的条件下,搅拌混合50min后,并用质量分数为25%的乙酸调节改性明胶与水混合物的pH至2.5,得处理液,将改性杀菌膜与处理液按质量比1:15混合,并向改性杀菌膜与处理液的混合物中加入改性杀菌膜质量0.4倍的戊二醛,于温度为50℃,转速为280r/min的条件下搅拌混合60min后,用质量分数为25%的氨水调节改性杀菌膜与处理液混合物的pH至4.5后,过滤,得滤饼,将滤饼于温度60℃的条件下真空干燥2h后,得空气杀菌过滤膜。所述引发剂为过硫酸钾。所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。所述壳聚糖为脱乙酰度95%的壳聚糖混合物。所述混合单体为将丙烯酰胺与丙烯酸按质量比2:1混合,得混合单体。所述硅烷偶联剂为硅烷偶联剂KH-550。
将正硅酸乙酯与无水乙醇按质量比1:8混合于烧杯中,并向烧杯中加入正硅酸乙酯质量0.8倍的四氧化三铁,于频率为55kHz的条件下超声分散20min后,向烧杯中加入正硅酸乙酯质量2倍的质量分数为25%的氨水,于温度为50℃,转速为250r/min的条件下搅拌混合15h后,磁吸分离,得预处理磁性颗粒坯料,将预处理磁性颗粒坯料用去离子水洗涤8次后,于温度为80℃的条件下干燥5h后,得预处理磁性颗粒,将预处理磁性颗粒与硅烷偶联剂KH-550按质量比1:8混合,于室温条件下浸泡3h后,过滤,得改性磁性颗粒;将胶原蛋白与超纯水按质量比1:55混合,并向胶原蛋白与超纯水的混合物中加入超纯水质量0.6倍的硫氰酸钠,于温度为55℃,转速为350r/min的条件下搅拌混合40min,得胶原蛋白溶液,将胶原蛋白溶液与丙烯腈按质量比60:1混合于烧瓶中,并向烧瓶中加入丙烯腈质量0.04倍的引发剂,于温度为75℃,转速为350r/min的条件下搅拌反应2h后,得改性胶原蛋白混合物;将改性胶原蛋白混合物与水按质量比1:120混合,于温度为55℃,转速为300r/min的条件下搅拌混合30min后,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:3混合于三口烧瓶中,并向三口烧瓶中加入改性胶原蛋白质量0.2倍的改性磁性颗粒和改性胶原蛋白质量50倍的N,N-二甲基甲酰胺,将三口烧瓶移入数显测速恒温磁力搅拌器,于温度为75℃,转速为350r/min的条件下搅拌混合8h后,得纺丝液,将纺丝液静电纺丝成膜后,于温度为80℃的条件下真空干燥40min后,得预处理杀菌膜;将纳米四氧化三铁与无水乙醇按质量比1:60混合,于频率为55kHz的条件下超声分散25min后,向纳米四氧化三铁与无水乙醇的混合物中加入无水乙醇质量0.2倍的钛酸四丁酯,于温度为85℃的条件下密封静置15h后,得预处理二氧化钛坯料,将预处理二氧化钛坯料洗涤6次后,于温度为90℃的条件下干燥2h后,于氮气保护下,于温度为400℃的条件下煅烧2h后,得预处理二氧化钛;将明胶与水按质量比1:12混合,并用质量分数为15%的氨水调节明胶与水混合物的pH至7.5,向明胶与水的混合物中加入明胶质量0.5倍的预处理二氧化钛和明胶质量0.2倍的硅烷偶联剂,于温度为55℃,转速为400r/min的条件下搅拌混合60min后,得改性明胶坯料,用质量分数为15%的乙酸调节改性明胶坯料的pH至4.2后,真空干燥,粉碎过120目筛,得改性明胶;将预处理杀菌膜于锥形瓶中,并向锥形瓶中加入预处理杀菌膜质量0.2倍的甘油,于温度为60℃,转速为250r/min的条件下搅拌混合3h后,过滤,得改性杀菌膜,将改性明胶与水按质量比1:15混合,于温度55℃,转速为350r/min的条件下,搅拌混合50min后,并用质量分数为25%的乙酸调节改性明胶与水混合物的pH至2.5,得处理液,将改性杀菌膜与处理液按质量比1:15混合,并向改性杀菌膜与处理液的混合物中加入改性杀菌膜质量0.4倍的戊二醛,于温度为50℃,转速为280r/min的条件下搅拌混合60min后,用质量分数为25%的氨水调节改性杀菌膜与处理液混合物的pH至4.5后,过滤,得滤饼,将滤饼于温度60℃的条件下真空干燥2h后,得空气杀菌过滤膜。所述引发剂为过硫酸钾。所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。所述混合单体为将丙烯酰胺与丙烯酸按质量比2:1混合,得混合单体。所述硅烷偶联剂为硅烷偶联剂KH-550。
将正硅酸乙酯与无水乙醇按质量比1:8混合于烧杯中,并向烧杯中加入正硅酸乙酯质量0.8倍的四氧化三铁,于频率为55kHz的条件下超声分散20min后,向烧杯中加入正硅酸乙酯质量2倍的质量分数为25%的氨水,于温度为50℃,转速为250r/min的条件下搅拌混合15h后,磁吸分离,得预处理磁性颗粒坯料,将预处理磁性颗粒坯料用去离子水洗涤8次后,于温度为80℃的条件下干燥5h后,得预处理磁性颗粒,将预处理磁性颗粒与硅烷偶联剂KH-550按质量比1:8混合,于室温条件下浸泡3h后,过滤,得改性磁性颗粒;将胶原蛋白与超纯水按质量比1:55混合,并向胶原蛋白与超纯水的混合物中加入超纯水质量0.6倍的硫氰酸钠,于温度为55℃,转速为350r/min的条件下搅拌混合40min,得胶原蛋白溶液,将胶原蛋白溶液与丙烯腈按质量比60:1混合于烧瓶中,并向烧瓶中加入丙烯腈质量0.04倍的引发剂,于温度为75℃,转速为350r/min的条件下搅拌反应2h后,得改性胶原蛋白混合物;将改性胶原蛋白混合物与水按质量比1:120混合,于温度为55℃,转速为300r/min的条件下搅拌混合30min后,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:3混合于三口烧瓶中,并向三口烧瓶中加入改性胶原蛋白质量0.2倍的改性磁性颗粒和改性胶原蛋白质量50倍的N,N-二甲基甲酰胺,将三口烧瓶移入数显测速恒温磁力搅拌器,于温度为75℃,转速为350r/min的条件下搅拌混合8h后,得纺丝液,将纺丝液静电纺丝成膜后,于温度为80℃的条件下真空干燥40min后,得预处理杀菌膜;将壳聚糖与质量分数为28%的乙酸按质量比5:100混合于四口烧瓶中,并向四口烧瓶中加入壳聚糖质量3倍的质量分数为12%的硝酸铈溶液和壳聚糖质量0.6倍的混合单体,向四口烧瓶中以30mL/min的速率通入氮气,并于温度为45℃,转速为400r/min的条件下搅拌混合50min后,得改性壳聚糖混合物;将纳米四氧化三铁与无水乙醇按质量比1:60混合,于频率为55kHz的条件下超声分散25min后,向纳米四氧化三铁与无水乙醇的混合物中加入无水乙醇质量0.2倍的钛酸四丁酯,于温度为85℃的条件下密封静置15h后,得预处理二氧化钛坯料,将预处理二氧化钛坯料洗涤6次后,于温度为90℃的条件下干燥2h后,于氮气保护下,于温度为400℃的条件下煅烧2h后,得预处理二氧化钛;将预处理杀菌膜与改性壳聚糖混合物按质量比1:8混合于锥形瓶中,并向锥形瓶中加入预处理杀菌膜质量0.2倍的甘油,于温度为60℃,转速为250r/min的条件下搅拌混合3h后,过滤,得改性杀菌膜,将明胶与水按质量比1:15混合,于温度55℃,转速为350r/min的条件下,搅拌混合50min后,并用质量分数为25%的乙酸调节明胶与水混合物的pH至2.5,得处理液,将改性杀菌膜与处理液按质量比1:15混合,并向改性杀菌膜与处理液的混合物中加入改性杀菌膜质量0.4倍的戊二醛,于温度为50℃,转速为280r/min的条件下搅拌混合60min后,用质量分数为25%的氨水调节改性杀菌膜与处理液混合物的pH至4.5后,过滤,得滤饼,将滤饼于温度60℃的条件下真空干燥2h后,得空气杀菌过滤膜。所述引发剂为过硫酸钾。所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。所述壳聚糖为脱乙酰度95%的壳聚糖混合物。所述混合单体为将丙烯酰胺与丙烯酸按质量比2:1混合,得混合单体。所述硅烷偶联剂为硅烷偶联剂KH-550。
对比例:江苏某科技有限公司生产的空气杀菌过滤膜。
将实例1至实例5所得的空气杀菌过滤膜及对比例产品进行性能检测,具体检测方法如下:
1.过滤效率:空气过滤性能的测试:采用滤料综合性能测试台测试试件的过滤性能。其中,测试粒径为0.5μm,过滤效率(η,%),按式(1)计算。
η=(1-p)×100%
(1)式中,p为复合滤料对颗粒的透过率,%。
2.细菌平均消除率:在相同的房间和相同的试验条件,进行消毒前无人活动下采样,作为对照组,随后,启动装有试件的净化器,人员进入室内进行常规作业活动,作业人员控制在5人以内,每人每小时进入房间的次数不超过两次,并且在进出房间的同时要随手关闭房间门,空气净化器仍然持续运行,每隔60分钟进行采样,采样方法同上,作为实验组。将所有的培养基放入37℃的恒温箱培养48h后,察结果,根据培养基和菌落数,计算得出每立方米的细菌平均消除率。
具体检测结果如表1所示:
表1空气杀菌过滤膜性能检测结果
检测项目 | 过滤效率/% | 细菌平均消除率/% |
实例1 | 99.97 | 98.1 |
实例2 | 95.16 | 95.3 |
实例3 | 92.63 | 90.5 |
实例4 | 90.03 | 83.6 |
实例5 | 86.49 | 81.1 |
对比例 | 81.95 | 74.2 |
由表1检测结果可知,本发明技术方案制备的空气杀菌过滤膜具有优异的过滤性能和杀菌性能的特点,在空气净化材料行业的发展中具有广阔的前景。
Claims (7)
1.一空气杀菌过滤膜的制备方法,其特征在于,具体制备步骤为:
(1)将胶原蛋白与超纯水按质量比1:50~1:55混合,并加入超纯水质量0.5~0.6倍的硫氰酸钠,搅拌混合,得胶原蛋白溶液,将胶原蛋白溶液与丙烯腈按质量比55:1~60:1混合,并加入丙烯腈质量0.02~0.04倍的引发剂,搅拌反应后,得改性胶原蛋白混合物;
(2)将改性胶原蛋白混合物与水按质量比1:100~1:120混合,过滤,得改性胶原蛋白,将改性胶原蛋白与丙烯腈按质量比1:2~1:3混合,并加入改性胶原蛋白质量0.1~0.2倍的改性磁性颗粒和改性胶原蛋白质量40~50倍的N,N-二甲基甲酰胺,磁力搅拌混合后,得纺丝液,将纺丝液静电纺丝成膜后,真空干燥,得预处理杀菌膜;
(3)将壳聚糖与乙酸按质量比1:100~5:100混合,并加入壳聚糖质量2~3倍的硝酸铈溶液和壳聚糖质量0.5~0.6倍的混合单体,于氮气氛围下搅拌混合后,得改性壳聚糖混合物;
(4)将纳米四氧化三铁与无水乙醇按质量比1:50~1:60混合,超声分散后,加入无水乙醇质量0.1~0.2倍的钛酸四丁酯,密封静置后,洗涤干燥,煅烧,得预处理二氧化钛;
(5)将明胶与水按质量比1:8~1:12混合,并调节pH至7.0~7.5,加入明胶质量0.4~0.5倍的预处理二氧化钛和明胶质量0.1~0.2倍的硅烷偶联剂,搅拌混合后,调节pH至4.0~4.2,真空干燥,粉碎过筛,得改性明胶;
(6)将预处理杀菌膜与改性壳聚糖混合物按质量比1:5~1:8混合,并加入预处理杀菌膜质量0.1~0.2倍的甘油,搅拌混合后过滤,得改性杀菌膜,将改性明胶与水按质量比1:10~1:15混合,并调节pH至2.2~2.5,得处理液,将改性杀菌膜与处理液按质量比1:10~1:15混合,并加入改性杀菌膜质量0.3~0.4倍的戊二醛,搅拌混合后,调节pH至4.2~4.5,过滤,真空干燥,得杀菌空气过滤膜。
2.根据权利要求1所述的一空气杀菌过滤膜的制备方法,其特征在于:步骤(1)所述引发剂为过硫酸钾,过硫酸铵或过硫酸钠中任意一种。
3.根据权利要求1所述的一空气杀菌过滤膜的制备方法,其特征在于:步骤(2)改性磁性颗粒的制备方法为将正硅酸乙酯与无水乙醇按质量比1:6~1:8混合,并加入正硅酸乙酯质量0.5~0.8倍的四氧化三铁,超声分散后,加入正硅酸乙酯质量1~2倍的氨水,搅拌混合后,磁吸分离,洗涤,干燥,得预处理磁性颗粒,将预处理磁性颗粒与硅烷偶联剂KH-550按质量比1:5~1:8混合,浸泡,过滤,得改性磁性颗粒。
4.根据权利要求1所述的一空气杀菌过滤膜的制备方法,其特征在于:步骤(2)所述静电纺丝条件为外加电压为16kV,注射速率为0.5mL/h,接收距离为12cm,喷口直径为0.34mm。
5.根据权利要求1所述的一空气杀菌过滤膜的制备方法,其特征在于:步骤(3)所述壳聚糖为脱乙酰度65~95%的壳聚糖混合物。
6.根据权利要求1所述的一空气杀菌过滤膜的制备方法,其特征在于:步骤(3)所述混合单体为将丙烯酰胺与丙烯酸按质量比1:1~2:1混合,得混合单体。
7.根据权利要求1所述的一空气杀菌过滤膜的制备方法,其特征在于:步骤(5)所述硅烷偶联剂为硅烷偶联剂KH-550,硅烷偶联剂-560或硅烷偶联剂KH-570中任意一种。
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