CN105561962B - 一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法 - Google Patents
一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法 Download PDFInfo
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Abstract
本发明涉及提供一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法,其特征在于该方法主要由减压蒸馏工艺、有机酸酯化、添加非离子表面活性剂、添加偶联剂KH570、调节pH和后处理工艺组成,其中有机酸可以是甲酸、乙酸和丁酸等,添加量为4克/升至10克/升;表面活性剂可以是OP‑10、平平加O和JFC等,添加量为添加量为2克/升。所得环境净化整理剂中纳米二氧化钛含量为1.0%,正丁醇残留量低于0.05%,可将该环境净化整理剂通过常用的轧烘焙方法负载到纤维织物上,从而使织物对空气中甲醛等污染物和水体中有机污染物具有更好催化降解性能。
Description
技术领域
本发明涉及化工催化剂技术,具体为一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法。
背景技术
近年来随着社会的不断发展,工业化进程加快,环境污染问题已然成为人们面临的亟待解决的突出问题之一。各国政府和科学家们纷纷开始致力于解决污染问题,尤其是空气污染和水污染的处理。作为一个廉价的环境友好的材料,纳米二氧化钛被广泛的用来空气环境中有害气体和水体中有机污染物的处理。环境有害气体可分为室内有害气体和大气污染气体。室内有害气体主要有装饰材料等放出的甲醛及生活环境中产生的甲硫醇、硫化氢及氨气等。其中甲醛对人体的危害最为严重,已经成为室内污染中危害最大的污染物,其对人体的眼睛、呼吸道以及皮肤等都有强烈刺激性,长期接触低浓度甲醛会引起恶心、支气管炎、结膜炎等症状。纳米二氧化钛通过光催化作用可将吸附于其表面的甲醛等空气污染物分解氧化,从而使空气中甲醛的浓度降低,减轻或消除环境不适感。纳米二氧化钛还可应用于水体中有机污染物的处理中,依靠其在光催化条件下的强氧化能力,可以快速将水体中有机污染物氧化降解。同时将纳米二氧化钛光催化剂应用于纺织品中,其在光照的作用下不仅能有效地降解空气中有毒有害气体,并能将细菌或真菌释放出的毒素分解及无害化处理,同时还具备除臭、抗污等功能。
制备纳米二氧化钛常用的方法有溶胶-凝胶法、沉淀法、水热法等,其中溶胶-凝胶法不仅是低温或温和条件下合成无机化合物或无机材料的重要方法,而且该方法所制备得到的纳米二氧化钛水溶胶能解决纳米二氧化钛粉体在纺织品的应用上存在的较多弊端,如分散性差,与织物结合牢度差以及会使纺织品纤维发生裂化等。然而,纳米二氧化钛水溶胶直接使用时仍存在一些问题,如酸性太强(pH值在1.5左右),当其应用于纺织品时对纤维机械性能损伤较大;水溶胶中纳米二氧化钛含固量较低且不能调节其含固量,使用时不方便;水溶胶中含有大量水解生成的正丁醇等气味特别刺鼻的副产物,在生产和使用时对工人的工作环境和身体健康有一定的影响。因此,为解决上述问题,本发明的目的就是提供一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法,使得纳米二氧化钛水溶胶能更好地应用于环境净化材料的制备和纺织品后整理中。
发明内容
针对现有技术的不足,本发明拟解决的技术问题是:提供一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法,其采用下述工艺处理:
1.纳米二氧化钛水溶胶的制备:首先在室温下将50毫升的钛酸丁酯溶解于75毫升的无水乙醇中形成钛酸丁酯的乙醇溶液。同时将规定体积的硝酸加入435毫升蒸馏水以获得稀硝酸的水溶液,然后将钛酸丁酯的乙醇溶液在室温和搅拌条件下滴入硝酸水溶液中,滴液完成后继续搅拌5小时得到乳白色水分散液,最后将其静置陈化数天形成微黄色半透明的约500毫升纳米二氧化钛水溶胶;
2.减压蒸馏工艺:将500毫升纳米二氧化钛水溶胶在40℃到60℃下进行减压蒸馏1.5小时至3.5小时得到300毫升浓缩纳米二氧化钛水溶胶;
3.有机酸酯化工艺:向300毫升浓缩纳米二氧化钛水溶胶中加入7.2克到18.0克有机酸并使其中的正丁醇在80℃进行酯化反应12小时到36小时;
4.添加非离子表面活性剂:向酯化反应后的浓缩纳米二氧化钛水溶胶中加入表面活性剂并搅拌30分钟;
5.添加偶联剂KH570:向添加非离子表面活性剂后的浓缩纳米二氧化钛水溶胶中加入添加偶联剂KH570并超声处理1小时;
6.调节pH工艺:向添加偶联剂后的浓缩纳米二氧化钛水溶胶中加入适量的加入少量1.0%的氢氧化钠水溶液调节pH为5-6;
7.后处理工艺:向已调节pH的浓缩纳米二氧化钛水溶胶中加入适量的蒸馏水使其中纳米二氧化钛含量为1.0%,并得到约1800毫升的环境净化整理剂。
其中有机酸可以是甲酸、乙酸和丁酸等;非离子表面活性剂可以是OP-10、平平加O或JFC等,添加量为2克/升。
与现有技术相比,本发明制备的一种基于纳米二氧化钛水溶胶的环境净化整理剂的pH值在中性偏弱酸性,当其应用于纺织品时对纤维机械性能损伤较小;纳米二氧化钛含固量较高且能大幅度调节,使用方便;整理剂中正丁醇含量极低,无刺激性味道。其不仅比现有纳米二氧化钛水溶胶具有更高的催化活性,用于室内空气净化时可使甲醛快速降解并在24小时内甲醛浓度低于国家标准。更为重要的是,本发明所述环境净化整理剂的制备方法成本低,容易操作,有利于工业化推广。
附图说明
图1为本发明所述实施例1、2和3中的环境净化整理剂负载织物和对比例中纳米二氧化钛水溶胶负载织物对甲醛的去除效果对比图。
图2为本发明所述实施例1、2和3中的环境净化整理剂负载织物和对比例中纳米二氧化钛水溶胶负载织物对偶氮染料酸性红88的光催化降解效果的对比图。
具体实施方式
本发明拟解决的技术问题是:提供一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法,其特征在于该方法主要由减压蒸馏工艺、有机酸酯化工艺、添加非离子表面活性剂、添加偶联剂KH570和后处理工艺组成,其中有机酸可以是甲酸、乙酸或丁酸等,添加量是4克/升至10克/升;表面活性剂可以是OP-10、平平加O或JFC等,添加量为2克/升。所得环境净化整理剂中纳米二氧化钛含量可达到1.0%,正丁醇的残余量低于0.05%。环境净化整理剂能够通过常用的轧烘焙方法使其负载到纤维织物上,从而使织物对空气中甲醛等污染物和水体中有机污染物具有优良的光催化降解性能。
与现有技术相比,本发明制备的一种基于纳米二氧化钛水溶胶的环境净化整理剂的pH值在中性偏弱酸性,当其应用于纺织品时对纤维机械性能几乎无损伤;纳米二氧化钛含固量较高且能大幅度调节,使用方便;整理剂中正丁醇含量极低,无刺激性味道。其不仅比现有纳米二氧化钛水溶胶具有更高的催化活性,用于室内空气净化时可使甲醛快速降解并在24小时内甲醛浓度低于国家室内空气质量标准。更为重要的是,本发明所述环境净化整理剂的制备方法成本低,容易操作,有利于工业化推广。
下面介绍本发明的具体实施例,但本发明权利要求不受这些具体实施例的限制。
实施例1
1.纳米二氧化钛水溶胶的制备:首先在室温下将50毫升的钛酸丁酯溶解于75毫升的无水乙醇中形成钛酸丁酯的乙醇溶液。同时将规定体积的硝酸加入435毫升蒸馏水以获得稀硝酸的水溶液,然后将钛酸丁酯的乙醇溶液在室温和搅拌条件下滴入硝酸水溶液中,滴液完成后继续搅拌5小时得到乳白色水分散液,最后将其静置陈化数天形成微黄色半透明的约500毫升纳米二氧化钛水溶胶,其中纳米二氧化钛含量为2.62%,正丁醇含量为7.65%;
2.减压蒸馏工艺:将500毫升纳米二氧化钛水溶胶在40℃进行减压蒸馏3.5小时得到300毫升浓缩纳米二氧化钛水溶胶,其中纳米二氧化钛含量为3.91%;由气相色谱法测定其中正丁醇含量为0.35%;
3.有机酸酯化工艺:向添加得到300毫升浓缩纳米二氧化钛水溶胶中加入18克乙酸并在80℃进行酯化反应36小时,其中正丁醇含量为0.03%;
4.添加非离子表面活性剂:向酯化反应后的浓缩纳米二氧化钛水溶胶中加入表面活性剂JFC,添加量为2克/升并搅拌30分钟;
5.添加偶联剂KH570:向添加非离子表面活性剂后的浓缩纳米二氧化钛水溶胶中加入添加1.0克偶联剂KH570并超声处理1小时;
6.调节pH工艺:向添加偶联剂后的浓缩纳米二氧化钛水溶胶中加入适量的加入少量1%的氢氧化钠水溶液调节pH为5-6;
7.后处理工艺:向调节pH后的浓缩纳米二氧化钛水溶胶中加入适量的蒸馏水使其中纳米二氧化钛含量为1.0%,并得到约1800毫升环境净化整理剂I。
实施例2
1.工艺与实施例1中的1步工艺相同。
2.所述减压蒸馏温度为60℃,时间为2.5小时,纳米二氧化钛含量为3.86%,正丁醇含量为0.21%,其余与实施例1中的第2步工艺相同。
3.所述乙酸添加量为10.8克,反应温度为60℃,反应时间为24小时,其余与实施例1中的第2步工艺相同,其中正丁醇含量为0.015%;
4.工艺与实施例1中的4步工艺相同;
5.工艺与实施例1中的5步工艺相同;
6.工艺与实施例1中的6步工艺相同;
7.工艺与实施例1中的7步工艺相同,得到环境净化整理剂II。
实施例3
1.工艺与实施例1中的1步工艺相同。
2.所述减压蒸馏温度为80℃,时间为1.5小时,纳米二氧化钛含量为3.97%,正丁醇含量为0.09%,其余与实施例1中的第2步工艺相同。
3.所述乙酸添加量为7.2克,反应温度为40℃,反应时间为12小时,其余与实施例1中的第2步工艺相同,其中正丁醇含量为0.023%。
4.工艺与实施例1中的4步工艺相同;
5.工艺与实施例1中的5步工艺相同;
6.工艺与实施例1中的6步工艺相同;
7.工艺与实施例1中的7步工艺相同,得到环境净化整理剂III。
对比例:
本实施例为效果对比例,其纳米二氧化钛水溶胶的制备方法如下:首先在室温下将50毫升的钛酸丁酯溶解于75毫升的无水乙醇中形成钛酸丁酯的乙醇溶液。同时将规定体积的硝酸加入435毫升蒸馏水以获得稀硝酸的水溶液,然后将钛酸丁酯的乙醇溶液在室温和搅拌条件下滴入硝酸水溶液中,滴液完成后继续搅拌5小时得到乳白色水分散液,最后将其静置陈化数天形成微黄色半透明的约500毫升纳米二氧化钛水溶胶,并通过添加蒸馏水使其中纳米二氧化钛含量为1.0%。
对所得实施例中所述的环境净化整理剂和对比例中纳米二氧化钛水溶胶的效果分别进行测定。首先通过常轧烘焙方法将所述整理剂和水溶胶分别对纤维织物进行整理得到相应负载织物,然后再测定它们对空气中的甲醛和水中的酸性红88的光催化降解性能,其过程如下:
织物的整理工艺:首先将10克的涤纶机织物放入500毫升的实施例所述环境净化整理剂或对比例中所述纳米二氧化钛水溶胶中浸渍2分钟,并利用轧车对浸渍后的织物进行处理以去除多余水分并保持轧余率为75-80%。然后将织物在100℃预烘1.5分钟,最后在170℃焙烘1.0分钟得到相应整理织物。
空气中甲醛的净化实验:在一个内设轴流风机、温度控制器、高压汞灯以及试样架的324升不锈钢环境试验舱中进行净化空气中甲醛的实验。首先在试样架上悬挂两块重量分别为6.0克的整理织物(约15厘米×15厘米)。密闭后从进样孔向其中加入0.02毫升甲醛,开启轴流风机和温度控制器使其中的甲醛在30℃的空气中进行挥发,混合均匀后甲醛浓度为1.2毫克/米3。然后开启设置在试样架中间的紫外灯,使用POT-400型甲醛检测器(深圳万安迪科技有限公司)每间隔一定时间测量一次舱中甲醛浓度的变化。
染料的降解反应实验:首先将规定质量的整理织物放入酸性红88水溶液中,然后将其置于光化学反应器中使染料在室温和光辐射条件下发生光催化降解反应。每隔一定反应时间取出少许染料溶液,使用723型分光光度计在染料的最大吸收波长处测定其吸光度值并按公式计算染料的脱色率。(测试条件:酸性红88浓度:0.04毫摩尔/升,体积:50毫升,pH=6.0;降解时间:90分钟;辐射光:紫外光(365nm):457μW/cm2,可见光(400-1000nm):4987μW/cm2)。
实验研究表明,三种实施例中的负载织物存在时,甲醛的去除率随着时间的延长而逐渐升高,反应420分钟后均能达到75%-84%,而对比例整理织物存在时,反应420分钟后甲醛的去除率仅约为61%,这表明本发明实施例中负载织物存在时,甲醛的去除率高于对比例中负载织物存在时甲醛的去除率。更为重要的是,实施例中负载织物存在24小时后试验舱内甲醛去除率能达到99.1%,甲醛浓度仅为0.01毫克/升,低于国家室内空气质量标准的要求。
另外,在本发明的实施例的负载织物存在时,酸性红88的脱色率随着时间的延长而逐渐升高,反应90分钟后均能达到89%-93%,而对比例的负载织物存在时,反应90分钟后甲醛的去除率仅为71.5%,低于本发明实施例存在下酸性红88的脱色率。这证明本发明的实施例对染色废水中染料的氧化降解反应具有更好的催化作用,在相同的反应时间内能够使更多的染料降解,使用效果显著。
Claims (2)
1.一种基于纳米二氧化钛水溶胶的环境净化整理剂的制备方法,其采用下述工艺处理:
步骤1纳米二氧化钛水溶胶的制备:首先在室温下将50毫升的钛酸丁酯溶解于75毫升的无水乙醇中形成钛酸丁酯的乙醇溶液,同时将规定体积的硝酸加入435毫升蒸馏水以获得稀硝酸的水溶液,然后将钛酸丁酯的乙醇溶液在室温和搅拌条件下滴入硝酸水溶液中,滴液完成后继续搅拌5小时得到乳白色水分散液,最后将其静置陈化数天形成微黄色半透明的550毫升纳米二氧化钛水溶胶;
步骤2减压蒸馏工艺:将500毫升纳米二氧化钛水溶胶在40℃到60℃下进行减压蒸馏1.5小时至3.5小时得到300毫升浓缩纳米二氧化钛水溶胶;
步骤3有机酸酯化工艺:向300毫升浓缩纳米二氧化钛水溶胶中加入3.6克到9.0克有机酸并使其中的正丁醇在80℃进行酯化反应12小时到36小时;
步骤4添加非离子表面活性剂:向酯化反应后的浓缩纳米二氧化钛水溶胶中加入表面活性剂并搅拌30分钟;
步骤5添加偶联剂KH570:向添加非离子表面活性剂后的浓缩纳米二氧化钛水溶胶中加入添加偶联剂KH570并超声处理1小时;
步骤6调节pH工艺:向添加偶联剂后的浓缩纳米二氧化钛水溶胶中加入1.0%的氢氧化钠水溶液调节pH为5到6;
步骤7后处理工艺:向已调节pH的浓缩纳米二氧化钛水溶胶中加入蒸馏水使其中纳米二氧化钛含量为1.0%,并得到1800毫升的环境净化整理剂。
2.根据权利要求1所述的制备方法,其特征在于有机酸是甲酸、乙酸和丁酸,添加量是4克/升至9克/升;非离子表面活性剂是OP-10、平平加O或JFC,添加量为2克/升。
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