CN112064142A - 硫化镍-石墨相氮化碳异质结光触媒纤维及其制备方法 - Google Patents
硫化镍-石墨相氮化碳异质结光触媒纤维及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种硫化镍‑石墨相氮化碳异质结光触媒纤维及其制备方法,向g‑C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,过滤得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,烘干后研磨得到硫化镍‑石墨相氮化碳异质结光触媒;称取聚对苯二甲酸乙二醇酯切粒与硫化镍‑石墨相氮化碳光触媒加入六氟异丙醇中,超声分散;对乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对纤维进行洗涤,烘干后得到硫化镍‑石墨相氮化碳光触媒纤维。石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍‑石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
Description
技术领域
本发明属于纺织工程领域,涉及一种硫化镍-石墨相氮化碳异质结光触媒纤维,还涉及该光触媒纤维的制备方法。
背景技术
随着科学技术的发展,人们对生活的质量要求越来越高,光触媒纺织品在自清洁领域的作用日益显著。纳米材料由于具有小尺寸效应、大比表面积和特殊的表面效应等特点,展示出与传统材料不同特性。当纺织品与具有优异性能的纳米粒子相结合时,整理出的具有纳米粒子性能的功能性纺织品将具有极大的优越性。如果在纺织品表面应用了纳米技术,当油污、油渍等污染物与纺织品接触时,就会自动滑落,可以防止其附着于表面造成污染,从而达到防水去污的作用。此外,当具有可见光光催化氧化能力的纳米颗粒附着于纺织材料表面时,当其受到太阳光照射时,纳米粒子会受到激发,与表面接触的氧气和水分反应生成具有强氧化能力的羟基自由基和超氧自由基,可以将纺织品表面的有机污染物进行氧化分解和去除。因此,光触媒自清洁纺织品不仅可以用于拒水、拒油、紫外屏蔽和抗静电,还可以用于降解有机污染物,抑制和杀灭细菌以及净化空气等方面。本发明的目的是提供一种硫化镍-石墨相氮化碳异质结光触媒及其制备方法和应用,将制备的硫化镍-石墨相氮化碳异质结光触媒加入有纤维浆料中,制备的纤维具有性能功能,尤其是自清洁功能。
发明内容
本发明的第一个目的是提供一种硫化镍-石墨相氮化碳异质结光触媒纤维,具有拒水拒油、紫外屏蔽和抗静电的特点。
本发明的另一个目的是提供一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,具有降解有机污染物,抑制和杀灭细菌以及净化空气的特点。
本发明所采用的第一个技术方案是,一种硫化镍-石墨相氮化碳异质结光触媒纤维,石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍-石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
本发明所采用的另一个技术方案是,一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,用于制备硫化镍-石墨相氮化碳异质结光触媒纤维,具体按照以下步骤实施:
步骤1、配制g-C3N4悬浊液,称取g-C3N4放入去离子水中,搅拌分散均匀;
步骤2、分散均匀后,向步骤1所得的g-C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,得到混合溶液;
步骤3、过滤混合溶液得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,直至洗涤液至中性,烘干后研磨成粉末,得到硫化镍-石墨相氮化碳异质结光触媒;
步骤4、称取聚对苯二甲酸乙二醇酯切粒与步骤3所得的硫化镍-石墨相氮化碳光触媒加入六氟异丙醇中,得到光触媒乳浊液,超声分散10~120分钟;
步骤5、对所述所得的乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对所述产物进行洗涤,烘干后得到硫化镍-石墨相氮化碳光触媒纤维。
本发明的特点还在于:
步骤1的g-C3N4悬浊液中g-C3N4与去离子水固液比为0.01~10g:5~200mL。
步骤2常温搅拌8~24小时。
步骤2的g-C3N4悬浊液与硝酸镍溶液体积比为5~200:0.01~5,所述硝酸镍溶液的浓度为0.01~5mmol/L。
步骤2的加入的硫化钠溶液与硝酸镍体积比为0.1~1.2:1,硫化钠溶液浓度为0.1mmol/L。
步骤3的烘干时间为12~24h,烘干为50~80℃。
步骤4的聚对苯二甲酸乙二醇酯与硫化镍-石墨相氮化碳光触媒质量比为0.1~10:0.01~1,聚对苯二甲酸乙二醇酯与六氟异丙醇固液比为0.5~50g:3~300mL,硫化镍-石墨相氮化碳光触媒与六氟异丙醇固液比为0.05~5g:3~300mL。
步骤5的静电纺丝参数为:电压为10~15kV,纺丝速度0.1~2mL/h,接收距离为10~50cm,水溶液中NaOH浓度为0.4~40g/L,水溶液中CTAB浓度为0.04~4g/L,水浴温度为65℃,水浴时间为0.5~5小时。
本发明的有益效果是:
1、本发明制备的硫化镍-石墨相氮化碳异质结光触媒纤维浆具有功能性能,尤其是自清洁功能。
2、本发明制备的硫化镍-石墨相氮化碳异质结光触媒纤维不仅可以用于拒水拒油、紫外屏蔽和抗静电,还可以用于降解有机污染物,抑制和杀灭细菌以及净化空气等方面。
附图说明
图1是本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维实施例1的扫描电镜图像;
图2为本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维实施例1的荧光光谱图谱;
图3是本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维实施例1的光催化降解罗丹明B评估图。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
实施例1
本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维,石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍-石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,具体按照以下步骤实施:
步骤1、配制g-C3N4悬浊液,称取g-C3N4放入去离子水中,搅拌分散均匀;
步骤2、分散均匀后,向步骤1所得的g-C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,得到混合溶液;
步骤3、过滤混合溶液得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,直至洗涤液至中性,烘干后研磨成粉末,得到硫化镍-石墨相氮化碳异质结光触媒。
步骤4、称取聚对苯二甲酸乙二醇酯切粒与步骤3所得的硫化镍-石墨相氮化碳光触媒加入六氟异丙醇中,得到光触媒乳浊液,超声分散10~120分钟;
步骤5、对所述所得的乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对所述产物进行洗涤,烘干后得到硫化镍-石墨相氮化碳光触媒纤维。
步骤1的g-C3N4悬浊液中g-C3N4与去离子水固液比为0.1g:50ml。
步骤2常温搅拌12小时。
步骤2的g-C3N4悬浊液与硝酸镍溶液体积比为50:0.1,硝酸镍溶液的浓度为0.1mmol/L。
步骤2的加入的硫化钠溶液与硝酸镍体积比为1:1,硫化钠溶液浓度为0.1mmol/L。
步骤3的烘干时间为18h,烘干为70℃。
步骤4的聚对苯二甲酸乙二醇酯与硫化镍-石墨相氮化碳光触媒质量比为8:0.7,聚对苯二甲酸乙二醇酯与六氟异丙醇固液比为44g:260mL,硫化镍-石墨相氮化碳光触媒与六氟异丙醇固液比为0.3g:3.6mL。
步骤5的静电纺丝参数为:电压为14kV,纺丝速度1.6mL/h,接收距离为40cm,水溶液中NaOH浓度为30g/L,水溶液中CTAB浓度为3.2g/L,水浴温度为65℃,水浴时间为3.2小时。
从图1中可看出:图中可以看出制备的石墨相氮化碳为二维薄片状结构,片状结构的优点:比表面积较大,能够提供较多的反应位点。
从图2中可看出:硫化镍-石墨相氮化碳异质结的荧光强度低于纯的石墨相氮化碳的荧光强度,说明生成的硫化镍-石墨相氮化碳异质结复合材料能够有效降低光生载流子的复合效率。
从图3中可看出:硫化镍-石墨相氮化碳异质结的光催化活性纯的石墨相氮化碳,表明适量的硫化镍修饰能够改善石墨相氮化碳的光催化活性。
实施例2
本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维,石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍-石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
本发明一种硫化镍-石墨相氮化碳异质结光触媒的制备方法,具体按照以下步骤实施:
步骤1、配制g-C3N4悬浊液,称取g-C3N4放入去离子水中,搅拌分散均匀;
步骤2、分散均匀后,向步骤1所得的g-C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,得到混合溶液;
步骤3、过滤混合溶液得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,直至洗涤液至中性,烘干后研磨成粉末,得到硫化镍-石墨相氮化碳异质结光触媒;
步骤4、称取聚对苯二甲酸乙二醇酯切粒与步骤3所得的硫化镍-石墨相氮化碳光触媒加入六氟异丙醇中,得到光触媒乳浊液,超声分散10~120分钟;
步骤5、对所述所得的乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对所述产物进行洗涤,烘干后得到硫化镍-石墨相氮化碳光触媒纤维。
步骤1的g-C3N4悬浊液中g-C3N4与去离子水固液比为0.01:5mL。
步骤2常温搅拌8小时。
步骤2的g-C3N4悬浊液与硝酸镍溶液体积比为5:0.01,硝酸镍溶液的浓度为0.01mmol/L。
步骤2的加入的硫化钠溶液与硝酸镍体积比为0.1:1,硫化钠溶液浓度为0.1mmol/L。
步骤3的烘干时间为12h,烘干为50℃。
步骤4的聚对苯二甲酸乙二醇酯与硫化镍-石墨相氮化碳光触媒质量比为0.1:0.01,聚对苯二甲酸乙二醇酯与六氟异丙醇固液比为0.5g:3mL,硫化镍-石墨相氮化碳光触媒与六氟异丙醇固液比为0.05g:3mL。
步骤5的静电纺丝参数为:电压为10kV,纺丝速度0.1mL/h,接收距离为10cm,水溶液中NaOH浓度为0.4g/L,水溶液中CTAB浓度为0.04g/L,水浴温度为65℃,水浴时间为0.5小时。
实施例3
本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维,石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍-石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,具体按照以下步骤实施:
步骤1、配制g-C3N4悬浊液,称取g-C3N4放入去离子水中,搅拌分散均匀;
步骤2、分散均匀后,向步骤1所得的g-C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,得到混合溶液;
步骤3、过滤混合溶液得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,直至洗涤液至中性,烘干后研磨成粉末,得到硫化镍-石墨相氮化碳异质结光触媒;
步骤4、称取聚对苯二甲酸乙二醇酯切粒与步骤3所得的硫化镍-石墨相氮化碳光触媒加入六氟异丙醇中,得到光触媒乳浊液,超声分散10~120分钟;
步骤5、对所述所得的乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对所述产物进行洗涤,烘干后得到硫化镍-石墨相氮化碳光触媒纤维。
步骤1的g-C3N4悬浊液中g-C3N4与去离子水固液比为2g:30ml。
步骤2常温搅拌11小时。
步骤2的g-C3N4悬浊液与硝酸镍溶液体积比为5~200:0.01~5,所述硝酸镍溶液的浓度为2mmol/L。
步骤2的加入的硫化钠溶液与硝酸镍体积比为0.8:1,硫化钠溶液浓度为0.1mmol/L。
步骤3的烘干时间为13h,烘干为55℃。
步骤4的聚对苯二甲酸乙二醇酯与硫化镍-石墨相氮化碳光触媒质量比为5:0.8,聚对苯二甲酸乙二醇酯与六氟异丙醇固液比为10g:50mL,硫化镍-石墨相氮化碳光触媒与六氟异丙醇固液比为3g:200mL。
步骤5的静电纺丝参数为:电压为14kV,纺丝速度1.2mL/h,接收距离为45cm,水溶液中NaOH浓度为35g/L,水溶液中CTAB浓度为3.7g/L,水浴温度为65℃,水浴时间为2.8小时。
实施例4
本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维,石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍-石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
本发明硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,具体按照以下步骤实施:
步骤1、配制g-C3N4悬浊液,称取g-C3N4放入去离子水中,搅拌分散均匀;
步骤2、分散均匀后,向步骤1所得的g-C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,得到混合溶液;
步骤3、过滤混合溶液得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,直至洗涤液至中性,烘干后研磨成粉末,得到硫化镍-石墨相氮化碳异质结光触媒;
步骤4、称取聚对苯二甲酸乙二醇酯切粒与步骤3所得的硫化镍-石墨相氮化碳光触媒加入六氟异丙醇中,得到光触媒乳浊液,超声分散10~120分钟;
步骤5、对所述所得的乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对所述产物进行洗涤,烘干后得到硫化镍-石墨相氮化碳光触媒纤维。
步骤1的g-C3N4悬浊液中g-C3N4与去离子水固液比为8g:180mL。
步骤2常温搅拌20小时。
步骤2的g-C3N4悬浊液与硝酸镍溶液体积比为110:2.7,所述硝酸镍溶液的浓度为0.3mmol/L。
步骤2的加入的硫化钠溶液与硝酸镍体积比为0.1~1.2:1,硫化钠溶液浓度为0.1mmol/L。
步骤3的烘干时间为14h,烘干为70℃。
步骤4的聚对苯二甲酸乙二醇酯与硫化镍-石墨相氮化碳光触媒质量质量比为0.6:0.09,聚对苯二甲酸乙二醇酯与六氟异丙醇固液比为3g:6mL,硫化镍-石墨相氮化碳光触媒与六氟异丙醇固液比为0.09g:4mL。
步骤5的静电纺丝参数为:电压为13kV,纺丝速度0.7mL/h,接收距离为30cm,水溶液中NaOH浓度为0.8g/L,水溶液中CTAB浓度为0.07g/L,水浴温度为65℃,水浴时间为0.9小时。
实施例5
本发明一种硫化镍-石墨相氮化碳异质结光触媒纤维,石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍-石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
本发明硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,具体按照以下步骤实施:
步骤1、配制g-C3N4悬浊液,称取g-C3N4放入去离子水中,搅拌分散均匀;
步骤2、分散均匀后,向步骤1所得的g-C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,得到混合溶液;
步骤3、过滤混合溶液得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,直至洗涤液至中性,烘干后研磨成粉末,得到硫化镍-石墨相氮化碳异质结光触媒。
步骤4、称取聚对苯二甲酸乙二醇酯切粒与步骤3所得的硫化镍-石墨相氮化碳光触媒加入六氟异丙醇中,得到光触媒乳浊液,超声分散10~120分钟;
步骤5、对所述所得的乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对所述产物进行洗涤,烘干后得到硫化镍-石墨相氮化碳光触媒纤维。
步骤1的g-C3N4悬浊液中g-C3N4与去离子水固液比为10g:200mL。
步骤2常温搅拌24小时。
步骤2的g-C3N4悬浊液与硝酸镍溶液体积比为200:5,所述硝酸镍溶液的浓度为5mmol/L。
步骤2的加入的硫化钠溶液与硝酸镍体积比为1.2:1,硫化钠溶液浓度为0.1mmol/L。
步骤3的烘干时间为24h,烘干为80℃。
步骤4的聚对苯二甲酸乙二醇酯与硫化镍-石墨相氮化碳光触媒质量比为10:1,聚对苯二甲酸乙二醇酯与六氟异丙醇固液比为50g:300mL,硫化镍-石墨相氮化碳光触媒与六氟异丙醇固液比为5g:300mL。
步骤5的静电纺丝参数为:电压为15kV,纺丝速度2mL/h,接收距离为50cm,水溶液中NaOH浓度为40g/L,水溶液中CTAB浓度为4g/L,水浴温度为65℃,水浴时间为5小时。
Claims (9)
1.一种硫化镍-石墨相氮化碳异质结光触媒纤维,其特征在于,石墨相氮化碳呈现出二维的薄片状结构,硫化镍纳米颗粒分散在石墨相氮化碳的表面上,硫化镍-石墨相氮化碳光触媒一部分嵌入纤维的内部,一部分裸露在外。
2.一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,用于制备如权利要求1所述的硫化镍-石墨相氮化碳异质结光触媒纤维,其特征在于,具体按照以下步骤实施:
步骤1、配制g-C3N4悬浊液,称取g-C3N4放入去离子水中,搅拌分散均匀;
步骤2、分散均匀后,向步骤1所得的g-C3N4悬浊液中加入硝酸镍溶液与硫化钠溶液,常温搅拌反应,得到混合溶液;
步骤3、过滤混合溶液得到沉淀物,使用无水乙醇和去离子水离心洗涤沉淀物,直至洗涤液至中性,烘干后研磨成粉末,得到硫化镍-石墨相氮化碳异质结光触媒;
步骤4、称取聚对苯二甲酸乙二醇酯切粒与步骤3所得的硫化镍-石墨相氮化碳光触媒加入六氟异丙醇中,得到光触媒乳浊液,超声分散10~120分钟;
步骤5、对所述所得的乳浊液进行静电纺丝,将产物加入将含有NaOH和CTAB的水溶液进行水浴加热后,再用去离子水和无水乙醇对所述产物进行洗涤,烘干后得到硫化镍-石墨相氮化碳光触媒纤维。
3.根据权利要求2所述的一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,其特征在于,所述步骤1的g-C3N4悬浊液中g-C3N4与去离子水固液比为0.01~10g:5~200mL。
4.根据权利要求2所述的一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,其特征在于,步骤2常温搅拌8~24小时。
5.根据权利要求2所述的一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,其特征在于,步骤2的g-C3N4悬浊液与硝酸镍溶液体积比为5~200:0.01~5,所述硝酸镍溶液的浓度为0.01~5mmol/L。
6.根据权利要求5所述的一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,其特征在于,步骤2的硫化钠溶液与硝酸镍体积比为0.1~1.2:1,所述硫化钠溶液浓度为0.1mmol/L。
7.根据权利要求2所述的一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,其特征在于,步骤3的烘干时间为12~24h,烘干为50~80℃。
8.根据权利要求2所述的一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,其特征在于,所述步骤4的聚对苯二甲酸乙二醇酯与硫化镍-石墨相氮化碳光触媒质量比为0.1~10:0.01~1,所述聚对苯二甲酸乙二醇酯与六氟异丙醇固液比为0.5~50g:3~300mL,硫化镍-石墨相氮化碳光触媒与六氟异丙醇固液比为0.05~5g:3~300mL。
9.根据权利要求2所述的一种硫化镍-石墨相氮化碳异质结光触媒纤维的制备方法,其特征在于,步骤5的静电纺丝参数为:电压为10~15kV,纺丝速度0.1~2mL/h,接收距离为10~50cm,水溶液中NaOH浓度为0.4~40g/L,水溶液中CTAB浓度为0.04~4g/L,水浴温度为65℃,水浴时间为0.5~5小时。
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