CN113522341A - 一种可见光催化的自清洁材料的制备方法 - Google Patents
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Abstract
本发明涉及一种可见光催化的自清洁材料的制备方法，特别是采用氮杂化介孔碳为模板制备的氮掺杂纳米二氧化钛的制备方法，具有可见光催化和自清洁功能，技术方案包括可溶性钛盐吸附负载，纳米二氧化钛水溶胶制备，氮掺杂纳米二氧化钛制备三个部分，形成氮掺杂纳米TiO2自清洁材料，其化学组成为Ti1‑xNxO2，x=0.01‑0.2，粒径为5‑20nm。本发明对纳米TiO2材料进行氮杂化介孔碳的负载或氮掺杂，使其光催化波长红移到可见光范围，提高其亲水性能，从而大大提高其光催化效率和自清洁性能。
Description
技术领域
本发明涉及一种可见光催化的自清洁材料的制备方法，特别是采用氮杂化介孔碳为模板制备的氮掺杂纳米二氧化钛的制备方法，具有可见光催化和自清洁功能，属于化工和新材料领域。
背景技术
随着人们生活质量要求的不断提高、环保和节能意识的不断增强，具有自清洁功能的表面得到了迅速的发展。自清洁表面是指表面的污染物或灰尘在重力、雨水、风力等外力作用下能够自动脱落或被降解的一种表面，通常分为超亲水性自清洁表面和超疏水性自清洁表面两种。涂覆纳米TiO2的表面通常是超亲水性的，也可以与其它材料复合为超疏水性。在实现自清洁的同时也希望能够兼顾材料的透明性，从而为自清洁材料的发展提出了新的需求．其中透明性是目前受到关注最多的方向．如在太阳能电池板、建筑外墙幕布和汽车玻璃等方面。
纳米TiO2材料由于其独特的紫外光催化和超亲水性能，被广泛用作日常生活中的自清洁材料。纳米TiO2可添加在日光灯， 玻璃等材料中， 可净化室内细菌； 还可以掺杂在建筑材料里， 有防水和防污的作用。工业上还有自清洁玻璃， 将 TiO2 镀膜在玻璃表面，利用 TiO2 其亲水性， 达到雨水冲刷下，实现玻璃自清洁的效果，可应用于太阳能电池面板和太阳能集热器面板。的
纳米TiO2材料在抗菌方面也有很大的应用，主要应用在生物、医学、食品包装以及工业和船舶设备等领域，而且应用范围正在逐步扩大，涂覆后可明显改善产品的抑菌性能。
纳米TiO2材料的自清洁性能目前还不能达到理想状态，主要原因是自清洁性能在紫外光照射下才能实现；另外纳米TiO2材料的折射率太高，大量采用和添加后产品的透光率明显下降。如果通过掺杂使纳米TiO2材料能够在可见光照射下能够发挥光催化自清洁功能，降低其折射率，将大大拓宽纳米TiO2材料的应用范围。
氮掺杂是实现纳米TiO2材料可见光催化的重要手段。例如，
中国专利CN109667139B（2021-06-29）公开一种防紫外自清洁组合物及其制备方法和应用，中国专利CN108912994B（2019-12-31）公开一种氮掺杂二氧化钛自清洁水性聚氨酯涂料的制备方法；中国专利CN109453799A（2019-03-12）公开氮掺杂碳材料包覆的纳米二氧化钛材料及其应用：中国专利CN102587610B（2014-10-29）公开一种表面涂覆氮掺杂纳米二氧化钛薄膜的可见光响应自清洁氟碳铝单板；但这些发明专利技术改进的空间仍很大，应用范围需要不断拓展。
中国专利CN111847446A（2020-10-30）公开一种氮杂化介孔碳及其制备方法，将对羟基苯海因生产废液与甲醛反应形成嵌段酚醛脲醛类树脂，进一步制备了氮杂化介孔碳，作为超级电容器材料。发明人将氮杂化介孔碳作为氮掺杂纳米TiO2材料制备的模板，可以方便地得到氮掺杂纳米TiO2材料，用于可见光催化自清洁目的。
发明内容
本发明的目的是提供一种可见光催化的自清洁材料的制备方法，特别是采用氮杂化介孔碳为模板制备的氮掺杂纳米二氧化钛的制备方法，具有可见光催化和自清洁功能，技术方案包括可溶性钛盐吸附负载，纳米二氧化钛水溶胶制备，氮掺杂纳米二氧化钛制备三个部分。
可溶性钛盐吸附负载是将四氯化钛、氯化氧钛、硫酸钛或硫酸氧钛溶解在去离子水中 ，搅拌溶解形成2mol/L的透明钛盐溶液；用氮杂化介孔碳浸渍，控制Ti/C的摩尔比为0.01-0.25:1，使钛离子吸附到载体表面上；再用4mol/L的氨水溶液中和，使钛离子以氢氧化钛形式沉淀在载体表面上；用去离子水冲洗，使氯化物或硫酸根离子去除干净，所述的氮杂化介孔碳材料中氮含量为2%-5%，碳含量为90%-95%，孔径为4-20nm，介孔率为70%-80%，比表面积为1500-2500m2/g。
纳米二氧化钛水溶胶制备是用饱和草酸水溶液浸渍吸附了氢氧化钛的氮杂化介孔碳，并在60-70℃水浴上加热2-4h，使团聚的氢氧化钛全部胶溶和纳米化，以便扩散到氮杂化介孔碳内部和提高负载率，在105-130℃下烘干1-2 h，得到氮杂化介孔碳负载的纳米TiO2自清洁材料。
氮掺杂纳米二氧化钛制备是将氮杂化介孔碳负载的纳米TiO2自清洁材料放在600-800℃的高温炉中，焙烧2-4 h，使氮杂化介孔碳氧化分解，形成氮掺杂纳米TiO2自清洁材料，其化学组成为Ti1-xNxO2，x=0.01-0.2，粒径为5-20nm。
纳米二氧化钛的同质异形体有锐钛矿型、金红石型和板钛矿型，其性能强烈地依赖于结构、结晶度及晶粒尺寸，其中锐钛矿型纳米二氧化钛的光催化性能优异，成为氮掺杂纳米TiO2自清洁材料的优选品种，可应用于太阳能光电转换或光热转换玻璃、家用灯罩玻璃、建筑玻璃屏幕、废水处理的自清洁材料。
氯化氧钛和硫酸氧钛的价格低廉和原料易得，且直接得到锐钛矿相纳米TiO2水溶胶，目前已成为制备纳米TiO2的基本原料。由于纳米TiO2粒子表面积高达数百平方米， 纳米粒子将会相互吸引聚焦， 纳米TiO2水溶胶的稳定期因制备方法不同，直观表现为纳米二氧化钛水溶胶的透明度随着存贮时间延长而逐渐下降和粒子直径逐渐变大，澄清的水溶胶逐渐变浑浊和产生少量胶团或沉淀，最终水溶胶完全变成凝胶。
将纳米TiO2粒子负载在氮杂化介孔碳表面上或者进一步加工为氮掺杂纳米TiO2粒子，不仅可以有效防止纳米TiO2粒子的团聚，而且由于氮负载或氮掺杂使其光催化波长红移到可见光范围，提高其亲水性能，从而大大提高其光催化效率和自清洁性能。
本发明的有益效果体现在：
（1）氮掺杂纳米TiO2是粉体材料，克服了纳米TiO2易凝聚和需要光催化的缺陷；
（2）氮掺杂纳米TiO2以氮杂化介孔碳为模板制备，将氮杂化介孔碳的应用范围从超级电容器和锂离子电池材料拓展到了自清洁光催化领域；
（3）对纳米TiO2材料进行氮杂化介孔碳的负载或氮掺杂，使其光催化波长红移到可见光范围，提高其亲水性能，从而大大提高其光催化效率和自清洁性能。
具体实施方式
本发明是采用以下方式实现的，下面结合实施例详细说明：
将硫酸氧钛32g(0.2mol)溶解在去离子水中 ，搅拌溶解形成2mol/L的透明钛盐溶液；用氮杂化介孔碳24 g(2mol)浸渍，使钛离子吸附到载体表面上；再用4mol/L的氨水溶液中和到pH10，使钛离子以氢氧化钛形式沉淀在载体表面上；用去离子水冲洗，使硫酸根离子去除干净。用饱和草酸水溶液(0.2mol)浸渍以上吸附了氢氧化钛的氮杂化介孔碳，并在60-70℃水浴上加热2h，使团聚的氢氧化钛全部胶溶和纳米化，过滤沉淀，在105-130℃下烘干2h，得到氮杂化介孔碳负载的纳米TiO2自清洁材料40g。
将氮杂化介孔碳负载的纳米TiO2自清洁材料40g放在600-800℃的高温炉中，焙烧2 h，使氮杂化介孔碳氧化分解，形成氮掺杂纳米TiO2自清洁材料17.4g，其化学组成为Ti0.9N0.1O2，x=0. 1，粒径为5-20nm，可应用于太阳能光。
Claims (1)
1.一种可见光催化的自清洁材料的制备方法，其特征是采用氮杂化介孔碳为模板制备的氮掺杂纳米二氧化钛的制备方法，具有可见光催化和自清洁功能，技术方案包括可溶性钛盐吸附负载，纳米二氧化钛水溶胶制备，氮掺杂纳米二氧化钛制备三个部分：
（1）可溶性钛盐吸附负载是将四氯化钛、氯化氧钛、硫酸钛或硫酸氧钛溶解在去离子水中 ，搅拌溶解形成2mol/L的透明钛盐溶液；用氮杂化介孔碳浸渍，控制Ti/C的摩尔比为0.01-0.25:1，使钛离子吸附到载体表面上；再用4mol/L的氨水溶液中和，使钛离子以氢氧化钛形式沉淀在载体表面上；用去离子水冲洗，使氯化物或硫酸根离子去除干净，所述的氮杂化介孔碳材料中氮含量为2%-5%，碳含量为90%-95%，孔径为4-20nm，介孔率为70%-80%，比表面积为1500-2500m2/g；
（2）纳米二氧化钛水溶胶制备是用饱和草酸水溶液浸渍吸附了氢氧化钛的氮杂化介孔碳，并在60-70℃水浴上加热2-4h，使团聚的氢氧化钛全部胶溶和纳米化，以便扩散到氮杂化介孔碳内部和提高负载率，在105-130℃下烘干1-2 h，得到氮杂化介孔碳负载的纳米TiO2自清洁材料；
（3）氮掺杂纳米二氧化钛制备是将氮杂化介孔碳负载的纳米TiO2自清洁材料放在600-800℃的高温炉中，焙烧2-4 h，使氮杂化介孔碳氧化分解，形成氮掺杂纳米TiO2自清洁材料，其化学组成为Ti1-xNxO2，x=0.01-0.2，粒径为5-20nm。
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