CN110170323A - 一种光催化剂的制备方法及其在光催化降解苯酚中的应用 - Google Patents
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
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Abstract
本发明公开了一种光催化剂的制备方法及其在光催化降解苯酚中的应用。以金属盐、聚乙二醇为原料,十二烷基苯磺酸钠作为活化剂,采用溶胶凝胶法合成Fe2O3,Al2O3,Fe/Zr,Zr‑Al2O3等一系列光催化剂。然后在不同的光照条件下,上述几种合成的催化剂用于苯酚的降解,均能体现较好的催化效果,并且Fe/Zr催化剂在日光光照时也能体现较好的催化降解效果。本发明制备方法简单,所得光催化剂在苯酚降解中能够体现非常好的降解效果。
Description
技术领域
本发明涉及环境材料的制备领域,特别涉及用一种光催化剂的制备方法及其在光催化降解苯酚中的应用。
背景技术
含苯酚的废水主要来自焦化厂、石化厂、树脂厂、绝缘材料厂、香料厂、塑料厂等。苯酚废水流入江河,对环境造成严重的污染,对人们的身体健康形成不容忽视的威胁。苯酚对人体任何组织都有显著腐蚀作用,可通过黏膜、皮肤的接触、吸入和误服而侵入人体内部。接触眼后,能引起角膜严重损害,甚至失明;接触皮肤后,不引起疼痛,但在暴露部位最初呈现白色,如不迅速冲洗清除, 能引起严重灼伤和全身性中毒;吸入后,可致头痛、头晕、乏力,视物模糊,肺水肿等,误服后,引起消化道灼伤,出现烧灼痛,呼吸气带酚气味,呕吐物或大便可带血液,有胃肠穿孔的可能。苯酚为细腻原浆毒物,它与细胞原浆中蛋白质接触时可发生化学反应,形成不溶性蛋白质,而使细胞失去活力。苯酚是造纸、炼焦、炼油、塑料、农药、医药合成等行业生产的原料和中间体。含酚废水对人类的危害非常严重。苯酚是一种高毒物质,主要存在于炼油、煤气洗涤、炼焦、造纸、合成氨、木材防腐、石油化工、化学、制药、油漆、涂料、塑料农药等企业的生产废水中。高浓度含酚废水主要通过物理化学方法使其循环再利用,而低浓度的含酚废水的处理仍是一项挑战。为了解决含酚废水的污染问题,寻找先进的低成本、高效率的水处理技术一直是众望所归。
发明内容
本发明的目的在于提供一种光催化剂的制备方法及其在光催化降解苯酚中的应用,通过研究掺杂引起的能带隙变窄的机理,来提升光催化剂的降解性能。
本发明采用的技术方案如下:
一种光催化剂的制备方法,包括如下步骤:
(1)将金属盐溶液与聚乙二醇溶液混合均匀,然后缓慢加入十二烷基苯磺酸钠溶液,然后将混合溶液在20~40℃搅拌2~4小时,金属盐、聚乙二醇、十二烷基苯磺酸钠的质量比为150~200:50~100:20~60,所述的金属盐为氯化亚铁FeCl2、AlCl3、ZrOCl2中的一种或两种以上;
(2)在步骤(1)所得混合溶液中加入浓氨水,将溶液的pH调节至9.2~9.3,静置老化10~18小时,然后把老化后的溶液进行抽滤,然后用蒸馏水水洗3~6遍,得到滤饼,并对滤饼进行干燥;
(3)将步骤(2)所得固体按固体、正丁醇1:8~15的质量体积比加入正丁醇,对其进行共沸精馏,然后把精馏后得到的固体进行研磨,再把研磨后的固体置于马弗炉中煅烧,所得固体即为Fe/Zr。
进一步地,步骤(1)中,所述的金属盐为FeCl2、AlCl3中的一种与ZrOCl2的混合盐。
进一步地,步骤(1)中,所述的金属盐溶液的浓度为0.5~2mol/L。
进一步地,步骤(1)中,所述的聚乙二醇溶液的质量分数为6~10%;所述的十二烷基苯磺酸钠溶液的质量分数为6~9%。
进一步地,步骤(2)中,干燥温度为80~120℃,干燥时间为2~3小时。
进一步地,步骤(3)中,煅烧采用程序升温,升温速率为2~5℃/min,升温至500~700℃,煅烧时间为2~4小时。
上述制备方法得到的光催化剂应用于光催化降解苯酚中。
本发明的有益效果在于:
本发明制备方法简单,所得光催化剂在苯酚降解中能够体现非常好的降解效果。
附图说明
图1在可见光照射的条件下,3种合成催化剂对于苯酚的降解图。
图2在紫外光照射的条件下,3种合成催化剂对于苯酚的降解图。
图3 Fe/Zr催化剂的XRD图。
具体实施方式
下面结合具体实施例对本发明做进一步详细说明,但本发明并不限于此。
实施例1
Fe2O3的合成
取1 mol/L FeCl2溶液100 mL,7 wt.%的聚乙二醇溶液100mL,首先将两者置于500 mL的烧杯中均匀混合,其次缓慢地加入7wt.%的十二烷基苯磺酸钠溶液50 mL,然后将混合溶液在25℃的条件下搅拌3小时;在混合溶液中加入浓氨水,将溶液的pH调节至9.2~9.3,然后静置老化12个小时,之后,把老化后的溶液进行抽滤,然后用蒸馏水水洗4遍,得到滤饼。将滤饼在105℃的条件下干燥3小时;把得到的固体按照固体:正丁醇=1:10(m/V)加入正丁醇,对其进行共沸精馏,然后把精馏后得到的固体进行研磨,之后把研磨后的固体置于马弗炉中,以3.2℃/min 的速率升温至600℃,并在600℃ 下维持4小时,所得固体即为Fe2O3。
实施例2
Al2O3的合成
取1 mol/L AlCl3溶液100 mL,7 wt.%的聚乙二醇溶液100mL,首先将两者于500 mL的烧杯中均匀混合,其次缓慢的加入7wt.%的十二烷基苯磺酸钠溶液50 mL,然后将混合溶液在25℃的条件下搅拌3小时;在混合溶液中加入浓氨水,将溶液的pH调节至9.2~9.3,然后静置老化12个小时,之后把老化后的溶液进行抽滤,然后用蒸馏水水洗4遍,得到滤饼。将滤饼在105℃的条件下干燥3小时;把得到的固体按照固体:正丁醇=1:10(m/V)对其进行共沸精馏。然后把精馏后得到的固体进行研磨,之后把研磨后的固体置于马弗炉中,以3.2℃/min的速率升温至650℃,并在650℃下维持3小时,所得固体即为Al2O3。
实施例3
Fe/Zr的合成
取50 mL的1 mol/LFeCl2溶液加上50 mL 1 mol/L ZrOCl2溶液,7 wt.%的聚乙二醇溶液100mL,首先将三者于500 mL的烧杯中均匀混合,其次缓慢的加入7wt.%的十二烷基苯磺酸钠溶液50 mL,然后将混合溶液在25℃的条件下搅拌3小时;在混合溶液中加入浓氨水,将溶液的pH调节至9.2~9.3,然后静置老化12个小时。之后,把老化后的溶液进行抽滤,然后用蒸馏水水洗5遍,得到滤饼,将滤饼在105℃的条件下干燥3小时;把得到的固体按照固体:正丁醇=1:10(m/V)对其进行共沸精馏,然后把精馏后得到的固体进行研磨,之后把研磨后的固体置于马弗炉中,以3℃/min 的速率升温至600℃,并在600℃下维持3小时,所得固体即为Fe/Zr。
实施例4
Zr-Al2O3的合成
取1 mol/L ZrOCl2 溶液100 mL,7 wt.%的聚乙二醇溶液100mL,再加入4g Al2O3于500mL的烧杯中均匀混合,其次缓慢的加入7wt.%的十二烷基苯磺酸钠溶液50 mL,然后将混合溶液在25℃的条件下搅拌3小时;在混合溶液中加入浓氨水,将溶液的PH调节至9.2~9.3,然后静置老化12个小时。之后,把老化后的溶液进行抽滤,然后用蒸馏水水洗4遍,得到滤饼。将滤饼在105℃的条件下干燥3小时;把得到的固体按照固体:正丁醇=1:10(m/V)对其进行共沸精馏,然后把精馏后得到的固体进行研磨,之后把研磨后的固体置于马弗炉中,以3℃/min 的速率,升温至600℃,并在600℃下维持3小时,所得固体即为Zr-Al2O3。
实施例5
所合成的催化剂的光催化性能主要通过苯酚降解实验来表征,分别在紫外光和可见光的条件下进行的。所降解苯酚溶液的初始浓度为100 mg/L,在苯酚溶液中分别加入不同的催化剂(Al2O3,Zr- Al2O3, Fe2O3, Fe/Zr)每一种催化剂的用量为1 g/L,首先进行暗吸附30min,然后进行取样,之后加入H2O2,然后在不同的光照条件下照射2小时。每隔30分钟取样,并在可见光和紫外光照射的前30分钟根据具体情况减少取样时间,增加取样次数。苯酚降解结果如图1和图2所示。
实施例6
苯酚含量的测定方法
采用分光光度法测定-苯酚溶液经质量分数为2%的4-铵基安替吡啉显色后,用分光光度计测定吸光度。苯酚类在pH=10.0±0.2和以质量分数为8%的铁氰化钾为氧化剂的溶液中,与4-氨基安替比林反应形成有色的安替比林染料。此染料的最大吸收波长在510nm处,颜色在30min内稳定。
Claims (7)
1.一种光催化剂的制备方法,其特征在于,包括如下步骤:
(1)将金属盐溶液与聚乙二醇溶液混合均匀,然后缓慢加入十二烷基苯磺酸钠溶液,然后将混合溶液在20~40℃搅拌2~4小时,金属盐、聚乙二醇、十二烷基苯磺酸钠的质量比为150~200:50~100:20~60,所述的金属盐为氯化亚铁FeCl2、AlCl3、ZrOCl2中的一种或两种以上;
(2)在步骤(1)所得混合溶液中加入浓氨水,将溶液的pH调节至9.2~9.3,静置老化10~18小时,然后把老化后的溶液进行抽滤,然后用蒸馏水水洗3~6遍,得到滤饼,并对滤饼进行干燥;
(3)将步骤(2)所得固体按固体、正丁醇1:8~15的质量体积比加入正丁醇,对其进行共沸精馏,然后把精馏后得到的固体进行研磨,再把研磨后的固体置于马弗炉中煅烧,所得固体即为Fe/Zr。
2.根据权利要求1所述的光催化剂的制备方法,其特征在于,所述的金属盐为FeCl2、AlCl3中的一种与ZrOCl2的混合盐。
3.根据权利要求1所述的光催化剂的制备方法,其特征在于,所述的金属盐溶液的浓度为0.5~2mol/L。
4.根据权利要求1所述的光催化剂的制备方法,其特征在于,所述的聚乙二醇溶液的质量分数为6~10%;所述的十二烷基苯磺酸钠溶液的质量分数为6~9%。
5.根据权利要求1所述的光催化剂的制备方法,其特征在于,干燥温度为80~120℃,干燥时间为2~3小时。
6.根据权利要求1所述的光催化剂的制备方法,其特征在于,煅烧采用程序升温,升温速率为2~5℃/min,升温至500~700℃,煅烧时间为2~4小时。
7.权利要求1至6任一项所述的制备方法得到的光催化剂在光催化降解苯酚中的应用。
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