CN113649031B - 一种TiO2/Na3NiF6复合光催化剂及其制备方法 - Google Patents
一种TiO2/Na3NiF6复合光催化剂及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 8
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- 229910052742 iron Inorganic materials 0.000 claims abstract description 69
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
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- 239000002131 composite material Substances 0.000 claims abstract description 28
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 claims abstract description 14
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- 230000000844 anti-bacterial effect Effects 0.000 description 1
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- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
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Abstract
本发明公开了一种TiO2/Na3NiF6复合光催化剂及制备方法，属于光催化技术领域，本申请的TiO2/Na3NiF6复合光催化剂制备方法为将铁尾矿砂中加入NaOH进行熔融处理制备得到铁尾矿溶液，铁尾矿溶液和氟钛酸铵进行水热反应制得。本申请制得的TiO2/Na3NiF6复合光催化剂具有优良的光催化性能，并且充分利用了固体废物铁尾矿砂，变废为宝。
Description
技术领域
本发明属于光催化技术领域，涉及一种TiO2/Na3NiF6复合光催化剂及制备方法。
背景技术
全球变暖、臭氧层破坏和生物多样性的消失等环境问题已经严重的威胁着人类的继续繁衍和生存。在各种环境污染中，最普遍、最主要和影响最大的是化学污染。
光触媒也叫光催化剂，是一种以纳米级二氧化钛为代表的具有光催化功能的半导体材料的总称。半导体光催化技术作为一种新型的环境污染物削减技术，它利用半导体氧化物材料在光照下表面能够受激活化，有效氧化分解有机物、还原重金属离子等特性，抗菌和清除异味。具有代表性的光触媒材料是二氧化钛，它能在光照射下产生强氧化性的物质(如羟基自由基、氧气等)，并且可用于分解有机化合物、部分无机化合物、细菌及病毒等。日常生活中，光触媒能有效地降解空气中有毒有害气体如甲醛等，高效净化空气；同时，能够有效杀灭多种细菌，并能将细菌或真菌释放出的毒素分解及无害化处理。
国内不同地区的铁尾矿以及典型国外铁尾矿中主要矿物成分为石英、方解石、蒙脱石、白云石、赤铁矿以及长石等，由此，铁尾矿砂的主要成分包括硅、铝、铁、钙、镁等元素。根据铁尾矿砂的组成可知，铁尾矿砂中含有多种有价金属，这一特点使得铁尾矿砂具有更为广泛的应用。若能将固体废物铁尾矿砂引入到光催化领域，进而资源化利用，不但可以创造可观的经济价值，还可以变废为宝，为工业废物的回收再利用提供新出路。
发明内容
本发明提供了一种TiO2/Na3NiF6复合光催化剂及制备方法，该复合光催化剂充分利用铁尾矿砂作为原料，制备工艺简单，制得的TiO2/Na3NiF6复合光催化剂性能稳定、具有优良的光催化性能。
为实现上述目的，本发明的技术方案如下：
一种TiO2/Na3NiF6复合光催化剂，该光催化剂由铁尾矿砂加碱处理后和氟钛酸铵进行水热反应制得。
一种TiO2/Na3NiF6复合光催化剂的制备方法包括以下步骤：
S1：前处理：镍坩埚在高温下灼烧，冷却备用，铁尾矿砂烘干，研磨，过筛；
S2：铁尾矿溶液制备：准确称取步骤S1中的铁尾矿砂，置于镍坩埚中，灼烧，放冷，加NaOH颗粒，混匀，加热熔融，取出放冷，交替加入少量热水和稀硝酸将熔融物浸出，倒入烧杯中，再滴加稀硝酸使铁尾矿溶液澄清，然后转移至容量瓶中，加入去离子水定容；
S3：在烧杯中加入氟钛酸铵，加入少量去离子水，搅拌，溶化，另取步骤 S2中的铁尾矿溶液，将氟钛酸铵溶液倒入铁尾矿溶液中，搅拌，滴加NaOH溶液调节pH值，停止搅拌，倒入水热釜内，然后将水热釜加热；
S4：取出水热釜，将水热釜中的溶液过滤，之后洗涤、抽滤三次，得到粉体；
S5：向粉体中加入去离子水，超声4h后进行离心；重复三次，将所得粉体放入干燥箱中烘干10h；
S6：粉体烘干后放在研钵内研磨，密封。
本发明技术方案的进一步改进在于：步骤S2中制得的铁尾矿溶液的浓度为2mg/mL，铁尾矿砂与NaOH颗粒用量的质量比为1:6-1:10。
本发明技术方案的进一步改进在于：步骤S3中氟钛酸铵和铁尾矿溶液加入的比例为3～5g：200mL，水热釜内的填充比为60％。
本发明技术方案的进一步改进在于：步骤S1中镍坩埚的灼烧温度为850～ 900℃，灼烧3～5min，铁尾矿烘干温度为105℃～110℃，烘干2h。
本发明技术方案的进一步改进在于：步骤S2中铁尾矿灼烧温度850～ 900℃，灼烧3～5min，加入NaOH颗粒后加热熔融10min。
本发明技术方案的进一步改进在于：步骤S3中NaOH溶液的浓度为 4mol/L，调节pH值为8-9，水热釜的加热温度170℃～190℃，加热时间为10～ 12h。
本发明技术方案的进一步改进在于：步骤S4中前两次洗涤溶液为去离子水，第三次的洗涤溶液为无水乙醇。
本发明技术方案的进一步改进在于：步骤S5中烘干温度为70～90℃。
本发明技术方案的进一步改进在于：步骤S1中过筛步骤所用的过滤筛为 200目。
由于采用了上述技术方案，本发明取得的技术效果如下：
本申请将固体废物铁尾矿砂引入到光催化领域，制备得到TiO2/Na3NiF6复合光催化剂，制备工艺简单，制得的产品光催化性能好，又充分利用了工业废物铁尾矿砂，实现了资源利用，变废为宝。
附图说明
图1是本申请实施例制得的粉体的XRD检测图。
具体实施方式
下面结合具体实施方式对本发明的技术方案进行详细说明。
实验设备：
电热恒温鼓风干燥箱 DHG-9030AD
循环水式真空泵 SHD-Ⅲ
水热釜 50mL
实施例1
前期处理工作：将铁尾矿在105℃～110℃下烘干2h、研磨、过200目筛，镍坩锅在850～900℃下灼烧3～4min，冷却备用。
铁尾矿溶液的制备：准确称取约0.5g处理好的铁尾矿砂，置于镍坩埚中，在850～900℃的温度下灼烧3～5min。将坩埚放冷，加5g固体氢氧化钠颗粒，用细玻璃棒将铁尾矿砂与氢氧化钠混匀，盖上坩埚盖，再于750～850℃的温度下熔融10min，取出放冷后，交替用少量热水和稀硝酸将熔融物浸出，倒入 500mL烧杯中，坩埚以少量稀硝酸和水洗净。在500毫升烧杯中滴加入20毫升硝酸使铁尾矿溶液澄清，然后倒入250毫升容量瓶中，加入去离子水至刻度线。
水热法制备TiO2/Na3NiF6复合光催化剂
在烧杯中加入0.3g氟钛酸铵，加入少量去离子水，放入一个转子，置于磁力搅拌器之上，使其熔化。取另一个烧杯加入20毫升铁尾矿溶液，将氟钛酸铵溶液倒入放有铁尾矿溶液得烧杯之中，加入氢氧化钠溶液调节pH值，当出现淡黄色絮状物时，开始一滴滴的加入，调节溶液pH值为8，取出转子，溶液保持在30毫升，如不够加入去离子水补齐，倒入水热釜内。然后将水热釜在鼓风干燥箱中180℃下加热10个小时。
将水热釜中的溶液过滤，洗涤，抽滤，反复三次，前两次用去离子水最后一次用无水乙醇，将得到的粉体放在烧杯中，加入100mL去离子水，超声4h 后进行离心；如此重复三次，将所得粉体放入鼓风干燥箱中在80℃下烘干10h。烘干结束后取出，放在研钵内研磨，取出放在密封袋内。
实施例2
前期处理工作：将铁尾矿在105℃～110℃下烘干2h、研磨、过200目筛，镍干锅在850～900℃下灼烧3～4min，冷却备用。
铁尾矿溶液的制备：准确称取约0.5g处理好的铁尾矿砂，置于镍坩埚中，在850～900℃的温度下灼烧3～5min。将坩埚放冷，加3g固体氢氧化钠颗粒，用细玻璃棒混匀，盖上坩埚盖，再于750～850℃的温度下熔融10min，取出放冷后，交替用少量热水和稀硝酸将熔融物浸出，倒入500毫升烧杯中，坩埚以少量稀硝酸和水洗净。在500毫升烧杯中加入20毫升硝酸使铁尾矿溶液澄清，然后装入250毫升容量瓶中，加入去离子水至刻度线。
水热法制备TiO2/Na3NiF6复合光催化剂
在烧杯中加入0.4g氟钛酸铵，加入少量去离子水，放入一个转子，置于磁力搅拌器之上，使其融化。取另一个烧杯加入20毫升铁尾矿溶液，将氟钛酸铵溶液倒入放有铁尾矿溶液得烧杯之中，加入氢氧化钠溶液调节pH值，当出现淡黄色絮状物时，开始一滴滴的加入，调节pH值为9，取出转子，溶液保持在 30毫升，不够加入去离子水补齐，倒入水热釜内。然后将水热釜在鼓风干燥箱中190℃下加热12个小时。
将水热釜中的溶液过滤，洗涤，抽滤，反复三次，前两次用蒸馏去离子水水最后一次用酒精无水乙醇，将得到的粉体放在烧杯中，加入100mL去离子水，超声4h后进行离心；如此重复三次，将所得粉体放入鼓风干燥箱中在70℃下烘干10h。烘干结束后取出，放在研钵内研磨，取出放在密封袋内。
实施例3
前期处理工作：将铁尾矿在105℃～110℃下烘干2h、研磨、过200目筛，镍干锅在850～900℃下灼烧3～4min，冷却备用。
铁尾矿溶液的制备：准确称取约0.5g处理好的铁尾矿砂，置于镍坩埚中，在850～900℃的温度下灼烧3～5min。将坩埚放冷，加4g固体氢氧化钠颗粒，用细玻璃棒混匀，盖上坩埚盖，再于750～850℃的温度下熔融10min，取出放冷后，交替用少量热水和稀硝酸将熔融物浸出，倒入500毫升烧杯中，坩埚以少量稀硝酸和水洗净。在500毫升烧杯中加入20毫升硝酸使铁尾矿溶液澄清，然后装入250毫升容量瓶中，加入去离子水至刻度线。
水热法制备TiO2/Na3NiF6复合光催化剂
在烧杯中加入0.5g氟钛酸铵，加入少量去离子水，放入一个转子，置于磁力搅拌器之上，使其融化。取另一个烧杯加入20毫升铁尾矿溶液，将氟钛酸铵溶液倒入放有铁尾矿溶液得烧杯之中，加入氢氧化钠溶液调节pH值，当出现淡黄色絮状物时，开始一滴滴的加入，调节pH值为8.5，取出转子，溶液保持在30毫升，不够加入去离子水补齐，倒入水热釜内。然后将水热釜在鼓风干燥箱中170℃下加热11个小时。
将水热釜中的溶液过滤，洗涤，抽滤，反复三次，前两次用去离子水水最后一次用无水乙醇，将得到的粉体放在烧杯中，加入100mL去离子水，超声 4h后进行离心；如此重复三次，将所得粉体放入鼓风干燥箱中在90℃下烘干 10h。烘干结束后取出，放在研钵内研磨，取出放在密封袋内。
性能测试
将实施例1中制得粉体进行XRD测试，XRD图谱如图1所示，从图中可以看出，所制备的粉体具有较强的衍射峰，通过将实验数据与PDF标准卡片对比可知，在2θ为19.4°、19.95°、22.77°、32.4°、46.4°和58.4°的位置有明显衍射峰，分别对应于Na3NiF6(标准卡片PDF#22-1389)晶体的(011)、(101)、(002)、
和(312)晶面；在2θ为25.2°、37.9°、48.14°、53.96°、55.05°和62.7°的位置有明显衍射峰，分别对应于TiO2(标准卡片PDF#21-1272)晶体的(101)、 (004)、(200)、(105)、(211)和(204)晶面；由此说明所合成的多晶粉末的主晶相为锐钛矿TiO2和Na3NiF6的复合物。
光催化性能检测
吸附试验
吸附实验在暗室内进行。具体操作：分别称取0.05g TiO2/Na3NiF6复合光催化剂和二氧化钛P25，量取15mL的罗丹明B溶液于石英试管内，之后将 TiO2/Na3NiF6复合光催化剂和二氧化钛P25分别放入到装有罗丹明B溶液的石英试管内，同时石英试管内放入磁转子，然后将石英试管放入到光反应器中，未打开光源的情况下，打开磁力搅拌进行暗室吸附反应，每隔5min取试样，离心取上层清液进行吸光度值测定，分析溶液浓度变化，直到浓度不再变化，即粉体与罗丹明B体系达到了吸附和脱附平衡。
由上表可以看出，本申请制备的TiO2/Na3NiF6复合光催化剂的吸附率明显优于TiO2 P25。
光催化试验
分别称取0.05g TiO2/Na3NiF6复合光催化剂和二氧化钛P25，量取15mL 的罗丹明B溶液于石英试管内，之后将TiO2/Na3NiF6复合光催化剂和二氧化钛 P25分别放入到装有罗丹明B溶液的石英试管内，同时石英试管内放入磁转子，然后将石英试管放入光反应器中,在未开光源的情况下先进行暗反应20min,使光催化粉体与罗丹明B溶液反应体系达到吸附/脱吸附平衡，之后打开汞灯光源，对罗丹明B溶液进行光降解，每隔10min取样一次，使用离心机离心，取上层清液，用紫外分光光度计测降解后的吸光度，计算不同时间罗丹明B溶液的浓度。C为检测时罗丹明B溶液的浓度，C0为初始罗丹明B溶液的浓度。
结果显示，在光照20min后，使用本申请的TiO2/Na3NiF6复合光催化剂后罗丹明B溶液的降解率为95％，优于市售TiO2 P25在相同条件下对罗丹明B 的降解效果，说明TiO2/Na3NiF6复合光催化剂粉体具有较强的光催化性能。
Claims (9)
1.一种TiO2/Na3NiF6复合光催化剂，其特征在于：该TiO2/Na3NiF6复合光催化剂由以下方法制备得到，该方法的具体步骤为：
S1：前处理：镍坩埚在高温下灼烧，冷却备用，铁尾矿砂烘干，研磨，过筛；
S2：铁尾矿溶液制备：准确称取步骤S1中的铁尾矿砂，置于镍坩埚中，灼烧，放冷，加NaOH颗粒，混匀，加热熔融，取出放冷，交替加入少量热水和稀硝酸将熔融物浸出，倒入烧杯中，再滴加稀硝酸使铁尾矿溶液澄清，然后转移至容量瓶中，加入去离子水定容；
S3：在烧杯中加入氟钛酸铵，加入少量去离子水，搅拌，溶化，另取步骤S2中的铁尾矿溶液，将氟钛酸铵溶液倒入铁尾矿溶液中，搅拌，滴加NaOH溶液调节pH值，停止搅拌，倒入水热釜内，然后将水热釜加热；
S4：取出水热釜，将水热釜中的溶液过滤，之后洗涤、抽滤三次，得到粉体；
S5：向粉体中加入去离子水，超声4h后进行离心；重复三次，将所得粉体放入干燥箱中烘干10h；
S6：粉体烘干后放在研钵内研磨，密封。
2.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S2中制得的铁尾矿溶液的浓度为2mg/mL，铁尾矿砂与NaOH颗粒用量的质量比为1:6-1:10。
3.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S3中氟钛酸铵和铁尾矿溶液加入的比例为3~5g：200mL，水热釜内的填充比为60%。
4.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S1中镍坩埚的灼烧温度为850～900℃，灼烧3~5min，铁尾矿烘干温度为105℃～110℃，烘干2h。
5.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S2中铁尾矿灼烧温度850～900℃，灼烧3~5min，加入NaOH颗粒后加热熔融10min。
6.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S3中NaOH溶液的浓度为4mol/L，调节pH值为8-9，水热釜的加热温度170℃～190℃，加热时间为10～12h。
7.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S4中前两次洗涤溶液为去离子水，第三次的洗涤溶液为无水乙醇。
8.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S5中烘干温度为70～90℃。
9.根据权利要求1所述的一种TiO2/Na3NiF6复合光催化剂，其特征在于：步骤S1中过筛步骤所用的过滤筛为200目。
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