CN106381716A - 一种织物光致变色整理液的制备方法 - Google Patents
一种织物光致变色整理液的制备方法 Download PDFInfo
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- CN106381716A CN106381716A CN201610756111.4A CN201610756111A CN106381716A CN 106381716 A CN106381716 A CN 106381716A CN 201610756111 A CN201610756111 A CN 201610756111A CN 106381716 A CN106381716 A CN 106381716A
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明公开了一种织物光致变色整理液的制备方法,其包括以下步骤:A、预处理:将水放入容器内,然后缓慢加入1~2份聚丙烯酸铵、1~5份月桂酸钠和1~2份三乙醇胺并不断搅拌,然后再缓慢加入0.1~5份功能剂并不断搅拌;B、乳化处理:预处理后的产物在乳化转速为5000‑6000r/min下乳化处理40~60min;C、超声处理:乳化处理后的产物在功率为1100~1300W下超声处理15~20min,即可获得所述织物光致变色整理液。本发明通过抗菌粉、纳米竹炭和光致变色复合物的合理搭配,两者协同作用,使得整理液具有优异的抗菌效果以及净化空气特性,同时具有光致变色特性,扩宽其应用范围。
Description
技术领域
本发明涉及了整理液技术领域,特别是涉及了一种织物光致变色整理液的制备方法。
背景技术
随着物质生活水平的提高,人们越来越关注人体的健康和保健。各种保健功能的纺织纤维及其纺织制品大量涌现,其中,具有保健功能的内衣越来越受到人们的关注,其亦成为服装制品领域的研究热点之一。
现有的纺织用整理剂中,使纺织品拥有抗紫外线功能的紫外线吸收剂都属于有机物,在接受长时间紫外线照射时容易导致分子分解。也有报道通过添加抗菌剂至整理剂中,以实现织物的抗菌效果,但直接添加纳米氧化锌或纳米银抗菌剂极易容易出现难分散、易团聚等现象,影响抗菌效果,有待进一步改善优化。
发明内容
本发明所要解决的技术问题是提供了一种织物光致变色整理液的制备方法。
本发明所要解决的技术问题通过以下技术方案予以实现:
一种织物光致变色整理液的制备方法,其包括以下步骤:
A、预处理:将水放入容器内,然后缓慢加入1~2份聚丙烯酸铵、1~5份月桂酸钠和1~2份三乙醇胺并不断搅拌,然后再缓慢加入0.1~5份功能剂并不断搅拌;
B、乳化处理:预处理后的产物在乳化转速为5000-6000r/min下乳化处理40~60min;
C、超声处理:乳化处理后的产物在功率为1100~1300W下超声处理15~20min,即可获得所述织物光致变色整理液;其中,
所述功能剂通过以下方法制得:
(1)称取0.3~1gC60粉末,量取80~100ml质量分数为98%的浓硫酸,将C60粉末和浓硫酸在烧杯中混合,烧杯放在冰水浴中,同时以500~600rpm的速度搅拌,得混合液;称取1~3g高锰酸钾粉末,缓慢的加入上述混合液中;移去冰水浴,换成水浴,保持水浴温度30~40℃,反应3~5h;快速加入100~150ml纯水,过滤,然后用截留分子量为1000的透析袋透析3~5天,得石墨烯量子点(GQDs)悬浮液;100~150rpm速度搅拌GQDs悬浮液,同时激光辐照30~60min,激光辐照功率为0.5~2W;备用;
(2)超声搅拌60~80mlGQDs悬浮液,滴加浓度为0.001~0.01mol/L硝酸银水溶液;逐滴加入浓度为0.1~0.5mol/L磷酸二氢铵溶液(磷酸二氢铵溶液与硝酸银水溶液体积比为2~3:1),超声搅拌10~20min;逐滴加入0.5~1mol/L氢氧化钠溶液,调节PH值至11,而后静置、离心,用去离子水和乙醇交替洗涤三次,真空干燥,得GQDs/Ag2O;
(3)取1~5gGQDs/Ag2O超声搅拌分散于80~120ml水溶液中;逐滴加入浓度为0.005~0.05mol/L硝酸铈水溶液,30~60min后逐滴加入浓度为0.005~0.05mol/L硝酸锌水溶液,GQDs/Ag2O水溶液、硝酸铈水溶液与硝酸锌水溶液体积比为1:0.1~0.2:0.2~0.4;继续超声搅拌,调节混合溶液PH值至7.0;边超声搅拌,边加入4~8mL质量分数为50%的水合肼,在30~40℃下还原反应0.5~1h;之后,再加入40~50mL质量分数为50%的水合肼,在85℃下还原反应30~48h后;过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/Ag-Zn-Ce;
(4)取1~5gGQDs/Ag2O超声搅拌分散于水溶液中;逐滴加入浓度为0.05~0.5g/100mlZnO量子点水溶液,超声功率搅拌速度各减半;60~90min后,静置,过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/ZnO;
(5)将GQDs/Ag2O/Ag-Zn-Ce和GQDs/Ag2O/ZnO按重量比1~3:2~4混合加入纯水中,配制成浓度为0.5~2g/100ml的混合溶液,搅拌均匀并加入0.1~0.5g分散助剂,球磨3~5h,得到研磨液;加入0.5~1g乳化剂,乳化处理得到抗菌分散液;
(6)取三维海绵状石墨烯超声搅拌分散于水溶液中,逐滴加入抗菌分散液中;10~100W超声60~120min,静置,去离子水洗涤数次,离心,置于密闭空间内,进行抽真空→加热加压循环3~8次(抽真空时间为20~30min;加热加压为通入高温高压气体,气体加热温度为90±3℃,加压至0.3~0.6Mpa,保压20~30min),得抗菌粉;
(7)取抗菌粉、纳米竹炭和光致变色复合物分散于100~200ml超纯水中,超声搅拌2~3h获得均匀和稳定的分散液,其中抗菌粉、纳米竹炭和光致变色复合物的重量比为3~5:1~5:3~5;将具有碳纳米管网状膜的基板置于约8℃时,将分散液加入内凹形状的基板中,同时,来回滚动滚轮,使该分散液均匀分散于该碳纳米管网状膜中,由于碳纳米管在8℃附近时具有亲水性,该分散液被吸附在碳纳米管网状膜的多个网洞;升温至约25℃,碳纳米管具有疏水性并将大部分水分子赶走留下吸附在碳纳米管网状膜的多个网洞中抗菌粉、纳米竹炭和光致变色复合物;去掉水分,置于密闭空间内,进行抽真空→加热加压循环3~5次(抽真空时间为20~30min;加热加压为通入高温高压气体,气体加热温度为80~90℃,加压至0.3~0.6Mpa,保压20~30min),然后将吸附有抗菌粉、纳米竹炭和光致变色复合物的碳纳米管网状膜刮离该基板,获得抗菌-光致变色功能剂。
其中,所述光致变色复合物制备方法如下:氮气环境下,将浓度为0.1mol/L的质子酸溶液和浓度为0.1mol/L的十二烷基苯磺酸以体积比3:2混合,同时加入光致变色粉,磁力搅拌60~120min后加入苯胺,光之变色粉与苯胺质量比为1:5~10;持续搅拌60~90min后,逐滴滴加过硫酸铵,苯胺与过硫酸铵摩尔比为1:1;20℃~30℃下反应12~36h;丙酮、去离子水洗涤数次后真空干燥,碾磨得纳米聚苯胺/光致变色粉复合物;将1~10g纳米聚苯胺/光致变色粉复合物超声搅拌分散于水溶液中;之后加入体积比4:1的水和氨水,搅拌均匀后加入正硅酸乙酯(与纳米聚苯胺/光致变色粉复合物的质量比为5:2),调节pH值为9~10,反应温度为20~25℃,反应60~90min;进行离心并依次用丙酮和去离子水清洗获得沉淀;将该沉淀在90℃下干燥3h,以得到纳米聚苯胺/光致变色粉复合物/SiO2;将纳米聚苯胺/光致变色粉复合物/SiO2置于氩气气氛下进行800~1000℃热处理1~2h,去除聚苯胺,光致变色粉/多孔SiO2,即光致变色复合物。
所述光致变色粉为稀土氧化物,所述稀土氧化物为Nd2O3、Er2O3、Pr2O3、CeO2、Sm2O3、La2O3、Y2O3、Yb2O3中至少一种。
所述三维海绵状石墨烯制备方法如下:将3g石墨粉,1g NaNO3在冰水浴中与250ml98%浓硫酸混合均匀,缓慢加入6g KMnO4。然后升温至在35℃,搅拌40min后,加入95ml去离子水,升温至98℃反应20min;再加入270ml水稀释,并用5ml 30%H2O2中和多余KMnO4,混合溶液的颜色为棕黄色,趁热过滤,用去离子水反复洗涤至中性,超声分散得到GO;取200ml质量分数为5mg/ml的氧化石墨烯溶液倒入直径25cm,高2cm的圆盘状反应皿中,加入抗坏血酸(VC)0.5g搅拌使其充分混合;然后密闭反应皿并置于80℃水热反应15h,反应皿中的氧化石墨烯自发收缩交联成三维海绵结构,冷冻干燥,得到柔性的三维海绵状石墨烯。
本发明具有如下有益效果:
本方法在三维石墨烯上负载并固定抗菌剂,不仅防止其团聚,显著提高金属纳米粒子等抗菌剂的稳定性,使其能更好分散在整理液中,且具有更长效的抗菌活性以及银离子不会溢出氧化变色;同时复合了多种抗菌剂的抗菌性能,相比于单一的银纳米抗菌剂有着更好的抗菌效果,抗菌持久,而且均匀分散性更好。纳米竹炭含有炭、氢、氧等多种有益元素,细密多孔,既能阻断及吸收各种电器产生的有害射线的侵蚀,使人体彻底免除有害射线的危害,纳米竹炭还可产生负离子,吸附并分解各种游离的有害物质,自动调节干湿度,还可产生最适合人体的远红外线。光致变色复合物具有光致变色的效果,使产品更加丰富多彩,可随着照射光线强弱的不同而变化的各种颜色,异彩纷呈,瑰丽多姿,增添情调及艺术效果。
本整理液通过合理搭配抗菌粉、纳米竹炭和光致变色复合物,使其不仅具有优异持久的抗菌特性,还具有净化空气效果,同时具有防辐射和光致变色特性,进一步扩宽其使用范围。
具体实施方式
下面结合实施例对本发明进行详细的说明,实施例仅是本发明的优选实施方式,不是对本发明的限定。
实施例1
一种织物光致变色整理液的制备方法,其包括以下步骤:
A、预处理:将1000份水放入容器内,然后缓慢加入1份聚丙烯酸铵、2份月桂酸钠和1份三乙醇胺并不断搅拌,然后再缓慢加入0.1份功能剂并不断搅拌;
B、乳化处理:将容器安装在高速剪切乳化机上,插上高速剪切乳化机电源,并打开开关,待乳化机自动校对归零后,开始由低到高进行加速,加速时采用点动,每次加速100r/min,至5000r/min为止,保持乳化转速5000r/min进行乳化处理50min;
C、超声处理:超声处理:乳化产物再使用超声波细胞粉碎机在1200W的超声功率下将乳化过的整理液超声处理10min,得到织物光致变色整理液。
其中,所述功能剂通过以下方法制得:
(1)称取0.5gC60粉末,量取100ml质量分数为98%的浓硫酸,将C60粉末和浓硫酸在烧杯中混合,烧杯放在冰水浴中,同时以800rpm的速度搅拌,得混合液;称取1.2g高锰酸钾粉末,缓慢的加入上述混合液中;移去冰水浴,换成水浴,保持水浴温度40℃,反应3h;快速加入100ml纯水,过滤,然后用截留分子量为1000的透析袋透析4天,得石墨烯量子点(GQDs)悬浮液;100rpm速度搅拌GQDs悬浮液,同时激光辐照30min,激光辐照功率为1.2W;备用;
(2)超声搅拌70mlGQDs悬浮液,滴加浓度为0.001mol/L硝酸银水溶液;逐滴加入浓度为0.5mol/L磷酸二氢铵溶液(磷酸二氢铵溶液与硝酸银水溶液体积比为2:1),超声搅拌20min;逐滴加入1mol/L氢氧化钠溶液,调节PH值至11,而后静置、离心,用去离子水和乙醇交替洗涤三次,真空干燥,得GQDs/Ag2O;
(3)取3gGQDs/Ag2O超声搅拌分散于100ml水溶液中;逐滴加入浓度为0.03mol/L硝酸铈水溶液,30min后逐滴加入浓度为0.03mol/L硝酸锌水溶液,GQDs/Ag2O水溶液、硝酸铈水溶液与硝酸锌水溶液体积比为1:0.2:0.4;继续超声搅拌,调节混合溶液PH值至7.0;边超声搅拌,边加入8mL质量分数为50%的水合肼,在30℃下还原反应0.5h;之后,再加入45mL质量分数为50%的水合肼,在85℃下还原反应36h后;过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/Ag-Zn-Ce;
(4)取2gGQDs/Ag2O超声搅拌分散于水溶液中;逐滴加入10ml浓度为0.36g/100mlZnO量子点水溶液,超声功率搅拌速度各减半;80min后,静置,过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/ZnO;
(5)将GQDs/Ag2O/Ag-Zn-Ce和GQDs/Ag2O/ZnO按重量比1:4混合加入纯水中,配制成浓度为2g/100ml的混合溶液,搅拌均匀并加入0.3g分散助剂,球磨4h,得到研磨液;加入0.8g乳化剂,乳化处理得到抗菌分散液;
(6)取5g三维海绵状石墨烯超声搅拌分散于50ml水溶液中,逐滴加入20ml抗菌分散液中;10~100W超声60~120min,静置,去离子水洗涤数次,离心,置于密闭空间内,进行抽真空→加热加压循环3次(抽真空时间为30min;加热加压为通入高温高压气体,气体加热温度为90±3℃,加压至0.5Mpa,保压30min),得抗菌粉;
(7)取抗菌粉、纳米竹炭和光致变色复合物分散于100~200ml超纯水中,超声搅拌2~3h获得均匀和稳定的分散液,其中抗菌粉、纳米竹炭(粒径介于100~300nm)和光致变色复合物的重量比为3:1:4;将具有碳纳米管网状膜的基板置于约8℃时,将分散液加入内凹形状的基板中,同时,来回滚动滚轮,使该分散液均匀分散于该碳纳米管网状膜中,由于碳纳米管在8℃附近时具有亲水性,该分散液被吸附在碳纳米管网状膜的多个网洞;升温至约25℃,碳纳米管具有疏水性并将大部分水分子赶走留下吸附在碳纳米管网状膜的多个网洞中抗菌粉、纳米竹炭和光致变色复合物;去掉水分,置于密闭空间内,进行抽真空→加热加压循环4次(抽真空时间为30min;加热加压为通入高温高压气体,气体加热温度为90℃,加压至0.6Mpa,保压30min),然后将吸附有抗菌粉、纳米竹炭和光致变色复合物的碳纳米管网状膜刮离该基板,获得抗菌-光致变色功能剂。
其中,所述光致变色复合物制备方法如下:氮气环境下,将浓度为0.1mol/L的质子酸溶液和浓度为0.1mol/L的十二烷基苯磺酸以体积比3:2混合,同时加入光致变色粉,磁力搅拌60~120min后加入苯胺,光致变色粉(由Er2O3、Pr2O3和Sm2O3等比例混合)与苯胺质量比为1:8;持续搅拌60~90min后,逐滴滴加过硫酸铵,苯胺与过硫酸铵摩尔比为1:1;20℃~30℃下反应12~36h;丙酮、去离子水洗涤数次后真空干燥,碾磨得纳米聚苯胺/光致变色粉复合物;将1~10g纳米聚苯胺/光致变色粉复合物超声搅拌分散于水溶液中;之后加入体积比4:1的水和氨水,搅拌均匀后加入正硅酸乙酯(与纳米聚苯胺/光致变色粉复合物的质量比为5:2),调节pH值为9~10,反应温度为20~25℃,反应60~90min;进行离心并依次用丙酮和去离子水清洗获得沉淀;将该沉淀在90℃下干燥3h,以得到纳米聚苯胺/光致变色粉复合物/SiO2;将纳米聚苯胺/光致变色粉复合物/SiO2置于氩气气氛下进行800~1000℃热处理1~2h,去除聚苯胺,光致变色粉/多孔SiO2,即光致变色复合物。
实施例2
一种织物光致变色整理液的制备方法,其包括以下步骤:
A、预处理:将1000份水放入容器内,然后缓慢加入1份聚丙烯酸铵、2份月桂酸钠和1份三乙醇胺并不断搅拌,然后再缓慢加入2份功能剂并不断搅拌;
B、乳化处理:将容器安装在高速剪切乳化机上,插上高速剪切乳化机电源,并打开开关,待乳化机自动校对归零后,开始由低到高进行加速,加速时采用点动,每次加速100r/min,至5000r/min为止,保持乳化转速5000r/min进行乳化处理50min;
C、超声处理:超声处理:乳化产物再使用超声波细胞粉碎机在1200W的超声功率下将乳化过的整理液超声处理10min,得到织物光致变色整理液。
其中,所述功能剂通过以下方法制得:
(1)称取0.5gC60粉末,量取100ml质量分数为98%的浓硫酸,将C60粉末和浓硫酸在烧杯中混合,烧杯放在冰水浴中,同时以800rpm的速度搅拌,得混合液;称取1.2g高锰酸钾粉末,缓慢的加入上述混合液中;移去冰水浴,换成水浴,保持水浴温度40℃,反应3h;快速加入100ml纯水,过滤,然后用截留分子量为1000的透析袋透析4天,得石墨烯量子点(GQDs)悬浮液;100rpm速度搅拌GQDs悬浮液,同时激光辐照30min,激光辐照功率为1.2W;备用;
(2)超声搅拌70mlGQDs悬浮液,滴加浓度为0.005mol/L硝酸银水溶液;逐滴加入浓度为0.3mol/L磷酸二氢铵溶液(磷酸二氢铵溶液与硝酸银水溶液体积比为2:1),超声搅拌20min;逐滴加入1mol/L氢氧化钠溶液,调节PH值至11,而后静置、离心,用去离子水和乙醇交替洗涤三次,真空干燥,得GQDs/Ag2O;
(3)取3gGQDs/Ag2O超声搅拌分散于100ml水溶液中;逐滴加入浓度为0.03mol/L硝酸铈水溶液,30min后逐滴加入浓度为0.03mol/L硝酸锌水溶液,GQDs/Ag2O水溶液、硝酸铈水溶液与硝酸锌水溶液体积比为1:0.1:0.3;继续超声搅拌,调节混合溶液PH值至7.0;边超声搅拌,边加入8mL质量分数为50%的水合肼,在30℃下还原反应0.5h;之后,再加入45mL质量分数为50%的水合肼,在85℃下还原反应36h后;过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/Ag-Zn-Ce;
(4)取2gGQDs/Ag2O超声搅拌分散于水溶液中;逐滴加入10ml浓度为0.36g/100mlZnO量子点水溶液,超声功率搅拌速度各减半;80min后,静置,过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/ZnO;
(5)将GQDs/Ag2O/Ag-Zn-Ce和GQDs/Ag2O/ZnO按重量比2:3混合加入纯水中,配制成浓度为1g/100ml的混合溶液,搅拌均匀并加入0.3g分散助剂,球磨4h,得到研磨液;加入0.8g乳化剂,乳化处理得到抗菌分散液;
(6)取5g三维海绵状石墨烯超声搅拌分散于50ml水溶液中,逐滴加入20ml抗菌分散液中;10~100W超声60~120min,静置,去离子水洗涤数次,离心,置于密闭空间内,进行抽真空→加热加压循环3次(抽真空时间为30min;加热加压为通入高温高压气体,气体加热温度为90±3℃,加压至0.5Mpa,保压30min),得抗菌粉;
(7)取抗菌粉、纳米竹炭和光致变色复合物分散于100~200ml超纯水中,超声搅拌2~3h获得均匀和稳定的分散液,其中抗菌粉、纳米竹炭(粒径介于100~300nm)和光致变色复合物的重量比为4:5:3;将具有碳纳米管网状膜的基板置于约8℃时,将分散液加入内凹形状的基板中,同时,来回滚动滚轮,使该分散液均匀分散于该碳纳米管网状膜中,由于碳纳米管在8℃附近时具有亲水性,该分散液被吸附在碳纳米管网状膜的多个网洞;升温至约25℃,碳纳米管具有疏水性并将大部分水分子赶走留下吸附在碳纳米管网状膜的多个网洞中抗菌粉、纳米竹炭和光致变色复合物;去掉水分,置于密闭空间内,进行抽真空→加热加压循环4次(抽真空时间为30min;加热加压为通入高温高压气体,气体加热温度为90℃,加压至0.6Mpa,保压30min),然后将吸附有抗菌粉、纳米竹炭和光致变色复合物的碳纳米管网状膜刮离该基板,获得抗菌-光致变色功能剂。
其中,所述光致变色复合物制备方法如下:氮气环境下,将浓度为0.1mol/L的质子酸溶液和浓度为0.1mol/L的十二烷基苯磺酸以体积比3:2混合,同时加入光致变色粉,磁力搅拌60~120min后加入苯胺,光致变色粉(由Er2O3、Pr2O3和Sm2O3等比例混合)与苯胺质量比为1:8;持续搅拌60~90min后,逐滴滴加过硫酸铵,苯胺与过硫酸铵摩尔比为1:1;20℃~30℃下反应12~36h;丙酮、去离子水洗涤数次后真空干燥,碾磨得纳米聚苯胺/光致变色粉复合物;将1~10g纳米聚苯胺/光致变色粉复合物超声搅拌分散于水溶液中;之后加入体积比4:1的水和氨水,搅拌均匀后加入正硅酸乙酯(与纳米聚苯胺/光致变色粉复合物的质量比为5:2),调节pH值为9~10,反应温度为20~25℃,反应60~90min;进行离心并依次用丙酮和去离子水清洗获得沉淀;将该沉淀在90℃下干燥3h,以得到纳米聚苯胺/光致变色粉复合物/SiO2;将纳米聚苯胺/光致变色粉复合物/SiO2置于氩气气氛下进行800~1000℃热处理1~2h,去除聚苯胺,光致变色粉/多孔SiO2,即光致变色复合物。
实施例3
一种织物光致变色整理液的制备方法,其包括以下步骤:
A、预处理:将1000份水放入容器内,然后缓慢加入1份聚丙烯酸铵、2份月桂酸钠和1份三乙醇胺并不断搅拌,然后再缓慢加入2份功能剂并不断搅拌;
B、乳化处理:将容器安装在高速剪切乳化机上,插上高速剪切乳化机电源,并打开开关,待乳化机自动校对归零后,开始由低到高进行加速,加速时采用点动,每次加速100r/min,至5000r/min为止,保持乳化转速5000r/min进行乳化处理50min;
C、超声处理:超声处理:乳化产物再使用超声波细胞粉碎机在1200W的超声功率下将乳化过的整理液超声处理10min,得到织物光致变色整理液。
其中,所述功能剂通过以下方法制得:
(1)称取0.5gC60粉末,量取100ml质量分数为98%的浓硫酸,将C60粉末和浓硫酸在烧杯中混合,烧杯放在冰水浴中,同时以800rpm的速度搅拌,得混合液;称取1.2g高锰酸钾粉末,缓慢的加入上述混合液中;移去冰水浴,换成水浴,保持水浴温度40℃,反应3h;快速加入100ml纯水,过滤,然后用截留分子量为1000的透析袋透析4天,得石墨烯量子点(GQDs)悬浮液;100rpm速度搅拌GQDs悬浮液,同时激光辐照30min,激光辐照功率为1.2W;备用;
(2)超声搅拌70mlGQDs悬浮液,滴加浓度为0.01mol/L硝酸银水溶液;逐滴加入浓度为0.1mol/L磷酸二氢铵溶液(磷酸二氢铵溶液与硝酸银水溶液体积比为2:1),超声搅拌20min;逐滴加入1mol/L氢氧化钠溶液,调节PH值至11,而后静置、离心,用去离子水和乙醇交替洗涤三次,真空干燥,得GQDs/Ag2O;
(3)取3gGQDs/Ag2O超声搅拌分散于100ml水溶液中;逐滴加入浓度为0.03mol/L硝酸铈水溶液,30min后逐滴加入浓度为0.03mol/L硝酸锌水溶液,GQDs/Ag2O水溶液、硝酸铈水溶液与硝酸锌水溶液体积比为1:0.1:0.4;继续超声搅拌,调节混合溶液PH值至7.0;边超声搅拌,边加入8mL质量分数为50%的水合肼,在30℃下还原反应0.5h;之后,再加入45mL质量分数为50%的水合肼,在85℃下还原反应36h后;过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/Ag-Zn-Ce;
(4)取2gGQDs/Ag2O超声搅拌分散于水溶液中;逐滴加入10ml浓度为0.36g/100mlZnO量子点水溶液,超声功率搅拌速度各减半;80min后,静置,过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/ZnO;
(5)将GQDs/Ag2O/Ag-Zn-Ce和GQDs/Ag2O/ZnO按重量比3:2混合加入纯水中,配制成浓度为0.5g/100ml的混合溶液,搅拌均匀并加入0.3g分散助剂,球磨4h,得到研磨液;加入0.8g乳化剂,乳化处理得到抗菌分散液;
(6)取5g三维海绵状石墨烯超声搅拌分散于50ml水溶液中,逐滴加入20ml抗菌分散液中;10~100W超声60~120min,静置,去离子水洗涤数次,离心,置于密闭空间内,进行抽真空→加热加压循环3次(抽真空时间为30min;加热加压为通入高温高压气体,气体加热温度为90±3℃,加压至0.5Mpa,保压30min),得抗菌粉;
(7)取抗菌粉、纳米竹炭和光致变色复合物分散于100~200ml超纯水中,超声搅拌2~3h获得均匀和稳定的分散液,其中抗菌粉、纳米竹炭(粒径介于100~300nm)和光致变色复合物的重量比为5:3:5;将具有碳纳米管网状膜的基板置于约8℃时,将分散液加入内凹形状的基板中,同时,来回滚动滚轮,使该分散液均匀分散于该碳纳米管网状膜中,由于碳纳米管在8℃附近时具有亲水性,该分散液被吸附在碳纳米管网状膜的多个网洞;升温至约25℃,碳纳米管具有疏水性并将大部分水分子赶走留下吸附在碳纳米管网状膜的多个网洞中抗菌粉、纳米竹炭和光致变色复合物;去掉水分,置于密闭空间内,进行抽真空→加热加压循环4次(抽真空时间为30min;加热加压为通入高温高压气体,气体加热温度为90℃,加压至0.6Mpa,保压30min),然后将吸附有抗菌粉、纳米竹炭和光致变色复合物的碳纳米管网状膜刮离该基板,获得抗菌-光致变色功能剂。
其中,所述光致变色复合物制备方法如下:氮气环境下,将浓度为0.1mol/L的质子酸溶液和浓度为0.1mol/L的十二烷基苯磺酸以体积比3:2混合,同时加入光致变色粉,磁力搅拌60~120min后加入苯胺,光致变色粉(由Er2O3、Pr2O3和Sm2O3等比例混合)与苯胺质量比为1:8;持续搅拌60~90min后,逐滴滴加过硫酸铵,苯胺与过硫酸铵摩尔比为1:1;20℃~30℃下反应12~36h;丙酮、去离子水洗涤数次后真空干燥,碾磨得纳米聚苯胺/光致变色粉复合物;将1~10g纳米聚苯胺/光致变色粉复合物超声搅拌分散于水溶液中;之后加入体积比4:1的水和氨水,搅拌均匀后加入正硅酸乙酯(与纳米聚苯胺/光致变色粉复合物的质量比为5:2),调节pH值为9~10,反应温度为20~25℃,反应60~90min;进行离心并依次用丙酮和去离子水清洗获得沉淀;将该沉淀在90℃下干燥3h,以得到纳米聚苯胺/光致变色粉复合物/SiO2;将纳米聚苯胺/光致变色粉复合物/SiO2置于氩气气氛下进行800~1000℃热处理1~2h,去除聚苯胺,光致变色粉/多孔SiO2,即光致变色复合物。
对比例1
基于实施例1的制备方法,不同之处在于:所述抗菌粉为纳米银抗菌剂;所述光致变色复合物为光致变色粉。
对比例2
基于实施例1的制备方法,不同之处在于:所述抗菌粉为氧化锌抗菌剂;未添加纳米竹炭。
对比例3
基于实施例1的制备方法,不同之处在于:所述抗菌粉为有机抗菌剂;未添加所述光致变色复合物。
将各实施例和对比例配制好的光致变色整理液倒进整理容器中,加入称量好的粘合剂并搅拌均匀,得到整理剂;将水洗并烘干后的织物,均匀放入整理容器中浸泡(35℃),要求织物都没入液体,浸泡20min后,取出织物,进行脱水处理;将脱水后的织物按其原料的不同按照正常定型烘干工艺要求进行定型烘干处理即可,最后对其进行性能测试,结果如下:
灭菌均匀性评价:在同一织物上选取100个区域进行灭菌测试,对测得的数据进行均匀度分析,通过均匀度=100*(1-标准偏差/平均值)。当均匀度大于95%,则标记为▲;当均匀度大于90%且小于95%,则标记为☆;当均匀度低于90%,则标记为╳。
以上所述实施例仅表达了本发明的实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制,但凡采用等同替换或等效变换的形式所获得的技术方案,均应落在本发明的保护范围之内。
Claims (7)
1.一种织物光致变色整理液的制备方法,其包括以下步骤:
A、预处理:将水放入容器内,然后缓慢加入1~2份聚丙烯酸铵、1~5份月桂酸钠和1~2份三乙醇胺并不断搅拌,然后再缓慢加入0.1~5份功能剂并不断搅拌;
B、乳化处理:预处理后的产物在乳化转速为5000-6000r/min下乳化处理40~60min;
C、超声处理:乳化处理后的产物在功率为1100~1300W下超声处理15~20min,即可获得所述织物光致变色整理液;其中,
所述功能剂通过以下方法制得:
(1)超声搅拌60~80mlGQDs悬浮液,滴加浓度为0.001~0.01mol/L硝酸银水溶液;逐滴加入浓度为0.1~0.5mol/L磷酸二氢铵溶液,超声搅拌10~20min;逐滴加入氢氧化钠溶液,调节PH值至11,而后静置、离心,用去离子水和乙醇交替洗涤三次,真空干燥,得GQDs/Ag2O;
(2)取1~5gGQDs/Ag2O超声搅拌分散于80~120ml水溶液中;逐滴加入浓度为0.005~0.05mol/L硝酸铈水溶液,30~60min后逐滴加入浓度为0.005~0.05mol/L硝酸锌水溶液;继续超声搅拌,调节混合溶液PH值至7.0;边超声搅拌,边加入4~8mL质量分数为50%的水合肼,在30~40℃下还原反应0.5~1h;之后,再加入40~50mL质量分数为50%的水合肼,在85℃下还原反应30~48h后;过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/Ag-Zn-Ce;
(3)取1~5gGQDs/Ag2O超声搅拌分散于水溶液中;逐滴加入浓度为0.05~0.5g/100mlZnO量子点水溶液,超声功率搅拌速度各减半;60~90min后,静置,过滤,用去离子水洗涤数次,真空干燥,得GQDs/Ag2O/ZnO;
(4)将GQDs/Ag2O/Ag-Zn-Ce和GQDs/Ag2O/ZnO按重量比1~3:2~4混合加入纯水中,配制成浓度为0.5~2g/100ml的混合溶液,搅拌均匀并加入0.1~0.5g分散助剂,球磨3~5h,得到研磨液;加入0.5~1g乳化剂,乳化处理得到抗菌分散液;
(5)取三维海绵状石墨烯超声搅拌分散于水溶液中,逐滴加入抗菌分散液中;10~100W超声60~120min,静置,去离子水洗涤数次,离心,置于密闭空间内,进行抽真空→加热加压循环3~8次,得抗菌粉;
(6)取抗菌粉、纳米竹炭和光致变色复合物分散于100~200ml超纯水中,超声搅拌2~3h获得均匀和稳定的分散液,其中抗菌粉、纳米竹炭和光致变色复合物的重量比为3~5:1~5:3~5;将具有碳纳米管网状膜的基板置于约8℃时,将分散液加入内凹形状的基板中,同时,来回滚动滚轮,使该分散液均匀分散于该碳纳米管网状膜中,由于碳纳米管在8℃附近时具有亲水性,该分散液被吸附在碳纳米管网状膜的多个网洞;升温至约25℃,碳纳米管具有疏水性并将大部分水分子赶走留下吸附在碳纳米管网状膜的多个网洞中抗菌粉、纳米竹炭和光致变色复合物;去掉水分,置于密闭空间内,进行抽真空→加热加压循环3~5次,然后将吸附有抗菌粉、纳米竹炭和光致变色复合物的碳纳米管网状膜刮离该基板,获得抗菌-光致变色功能剂。
2.根据权利要求2所述的织物光致变色整理液的制备方法,其特征在于,所述GQDs悬浮液通过以下方法制得:称取0.3~1gC60粉末,量取80~100ml质量分数为98%的浓硫酸,将C60粉末和浓硫酸在烧杯中混合,烧杯放在冰水浴中,同时以500~600rpm的速度搅拌,得混合液;称取1~3g高锰酸钾粉末,缓慢的加入上述混合液中;移去冰水浴,换成水浴,保持水浴温度30~40℃,反应3~5h;快速加入100~150ml纯水,过滤,然后用截留分子量为1000的透析袋透析3~5天,即得。
3.根据权利要求2所述的织物光致变色整理液的制备方法,其特征在于,所述三维海绵状石墨烯制备方法如下:将3g石墨粉,1g NaNO3在冰水浴中与250ml 98%浓硫酸混合均匀,缓慢加入6g KMnO4;然后升温至在35℃,搅拌40min后,加入95ml去离子水,升温至98℃反应20min;再加入270ml水稀释,并用5ml 30%H2O2中和多余KMnO4,混合溶液的颜色为棕黄色,趁热过滤,用去离子水反复洗涤至中性,超声分散得到GO;取200ml质量分数为5mg/ml的氧化石墨烯溶液倒入直径25cm,高2cm的圆盘状反应皿中,加入抗坏血酸(VC)0.5g搅拌使其充分混合;然后密闭反应皿并置于80℃水热反应15h,反应皿中的氧化石墨烯自发收缩交联成三维海绵结构,冷冻干燥,得到柔性的三维海绵状石墨烯。
4.根据权利要求2所述的织物光致变色整理液的制备方法,其特征在于,在步骤(2)中,GQDs/Ag2O水溶液、硝酸铈水溶液与硝酸锌水溶液体积比为1:0.1~0.2:0.2~0.4。
5.根据权利要求2所述的织物光致变色整理液的制备方法,其特征在于,在步骤(1)中,磷酸二氢铵溶液与硝酸银水溶液体积比为2~3:1。
6.根据权利要求2所述的织物光致变色整理液的制备方法,其特征在于,所述抽真空→加热加压循环具体为真空时间为20~30min;加热加压为通入高温高压气体,气体加热温度为80~90℃,加压至0.3~0.6Mpa,保压20~30min。
7.根据权利要求2所述的织物光致变色整理液的制备方法,其特征在于,所述光致变色复合物制备方法如下:氮气环境下,将浓度为0.1mol/L的质子酸溶液和浓度为0.1mol/L的十二烷基苯磺酸以体积比3:2混合,同时加入光致变色粉,磁力搅拌60~120min后加入苯胺,光致变色粉与苯胺质量比为1:5~10;持续搅拌60~90min后,逐滴滴加过硫酸铵,苯胺与过硫酸铵摩尔比为1:1;20℃~30℃下反应12~36h;丙酮、去离子水洗涤数次后真空干燥,碾磨得纳米聚苯胺/光致变色粉复合物;将1~10g纳米聚苯胺/光致变色粉复合物超声搅拌分散于水溶液中;之后加入体积比4:1的水和氨水,搅拌均匀后加入正硅酸乙酯,调节pH值为9~10,反应温度为20~25℃,反应60~90min;进行离心并依次用丙酮和去离子水清洗获得沉淀;将该沉淀在90℃下干燥3h,以得到纳米聚苯胺/光致变色粉复合物/SiO2;将纳米聚苯胺/光致变色粉复合物/SiO2置于氩气气氛下进行800~1000℃热处理1~2h,去除聚苯胺,光致变色粉/多孔SiO2,即光致变色复合物。
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