CN106944076A - 铬掺杂磁铁矿异相芬顿催化剂及其制备方法 - Google Patents
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000011651 chromium Substances 0.000 title claims abstract description 33
- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000010790 dilution Methods 0.000 claims abstract description 5
- 239000012895 dilution Substances 0.000 claims abstract description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 150000004690 nonahydrates Chemical class 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
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- 238000002156 mixing Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 239000000975 dye Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- 125000000129 anionic group Chemical group 0.000 abstract description 5
- 230000007935 neutral effect Effects 0.000 abstract description 4
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- 229910052596 spinel Inorganic materials 0.000 abstract description 2
- 239000011029 spinel Substances 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 abstract 1
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000004042 decolorization Methods 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- -1 Iron ion Chemical class 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 239000010936 titanium Substances 0.000 description 1
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- 230000001052 transient effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明为铬掺杂磁铁矿异相芬顿催化剂及其制备方法，该催化剂为Fe2.5Cr0.5O4，该催化剂采用共沉淀法制备，包括如下步骤：首先按照Fe2+:Cr3+为2.5:0.5的摩尔比取的亚铁盐和九水合硝酸铬，并溶解为金属离子混合液。其次，取体积为1/4金属离子混合液体积的碱溶液，稀释一倍后，将金属离子混合液迅速倒入碱溶液中，搅拌反应。搅拌反应完毕后，经反复离心与洗涤、干燥、研磨、在400℃下煅烧3h。本发明制得的掺铬磁铁矿Fe2.5Cr0.5O4为立方晶系尖晶石结构，Fe2.5Cr0.5O4在中性条件下对阴离子型染料废水的降解效果好，具有很高的去除效果；且Fe2.5Cr0.5O4在外加磁场的作用下能够迅速的被分离，实现了催化剂的重复利用。
Description
技术领域
本发明属于染料废水处理和环境催化技术领域，具体涉及一种铬掺杂磁铁矿异相芬顿催化剂及其制备方法。
背景技术
Fenton法作为一种高级氧化工艺在处理染料废水时具有很多优点，如反应没有选择性，反应条件温和，操作简单等。但是传统的均相Fenton法存在一些弊端，如：较窄的pH范围，反应后产生大量铁污泥造成二次污染，Fe2+/Fe3+离子会使出水色度增加，难以实现催化剂的分离及重复使用等，使其在废水处理中的应用受到了限制。而以铁氧化物为催化剂的异相Fenton工艺因为其较高的反应活性，将铁离子固定在载体上，克服了均相的很多缺点而逐渐受到了重视。相比与其他铁氧化物，磁铁矿是一个高效理想的异相Fenton催化剂。
研究发现：过渡金属掺杂磁铁矿作为异相Fenton催化剂用于染料的降解，在中性pH条件下降解效率高，催化剂具有磁性，易于循环使用，且在地球表面天然矿物中普遍存在。阳离子型染料亚甲基蓝(MB)常用于掺杂磁铁矿Fenton催化活性的研究，研究结果表明钛掺杂对磁铁矿Fenton催化降解MB的效率有明显的提高，然而污染物本身类型对催化氧化效果的影响常被忽略了。大多掺杂磁铁矿在中性条件下对阴离子染料脱色和降解效果很不理想。
发明内容
本发明的目的是提供一种在中性条件下对阴离子型染料废水有很好的降解效果掺铬有磁性的异相芬顿催化剂。
本发明的目的可以通过以下技术方案实现：一种掺铬磁铁矿催化剂的制备，该催化剂为Fe2.5Cr0.5O4，该催化剂采用共沉淀法制备，包括如下步骤：
(1)按照Fe2+:Cr3+为2.5:0.5的摩尔比取的亚铁盐和九水合硝酸铬，并溶解为金属离子混合液。
(2)取体积为1/4金属离子混合液体积的碱溶液，稀释一倍后，将金属离子混合液迅速倒入碱溶液中，搅拌反应。
(3)搅拌反应完毕后，经反复离心与洗涤、干燥、研磨、在400℃下煅烧3h。
步骤(1)中，亚铁盐为七水合硫酸亚铁，混合溶液中金属离子浓度约为0.3mol/L。
步骤(2)中，碱溶液为为氨水或氢氧化钠，质量浓度为25.0-28.0％，搅拌时间2h。
步骤(3)中，干燥温度为100℃，干燥时间为12h，研磨的目数为40～60目。
本发明相对于现有技术相比具有显著优点：
(1)本发明合成的掺铬磁铁矿Fe2.5Cr0.5O4为立方晶系尖晶石结构，是纳米级的磁性材料；
(2)本发明掺铬磁铁矿Fe2.5Cr0.5O4在中性条件下对阴离子型染料废水的降解效果好，具有很高的去除效果；
(3)本发明掺铬磁铁矿Fe2.5Cr0.5O4在外加磁场的作用下能够迅速的被分离，实现了催化剂的重复利用。
附图说明
图1是本发明制得的Fe2.5Cr0.5O4的X射线衍射(XRD)图。
图2是本发明制得的Fe2.5Cr0.5O4的SEM图。
图3是本发明制得的Fe2.5Cr0.5O4异相芬顿脱色酸性橙Ⅱ动力学曲线图。
具体实施方式
下面结合本发明的较佳实施例，对发明进行详细阐述：
实施例：Fe2.5Cr0.5O4的制备及对酸性橙Ⅱ的脱色：
按照Fe2+:Cr3+为2.5:0.5的摩尔比取0.05mol的七水合硫酸亚铁和0.01mol的九水合硝酸铬，用200mL去离子水混合，该混合溶液中金属离子浓度约为0.3mol/L。取50mL质量浓度为25.0-28.0％的NH3·H2O加入等体积的去离子水稀释，将上述的金属离子混合液迅速倒入氨水中，反应体系以800r/min的速度搅拌反应2h。搅拌反应完毕后，离心分离出Fe2.5Cr0.5O4，洗涤，再次离心。反复操作5次后，在100℃下干燥12h。待干燥后的样品冷却后，样品研磨成40～60目，置于马弗炉中400℃煅烧3h，得到掺铬磁铁矿Fe2.5Cr0.5O4。
Fe2.5Cr0.5O4的X射线衍射(XRD)图谱可参见图1
图1为所制备的Fe2.5Cr0.5O4的X射线衍射图。合成掺铬磁铁矿的特征衍射峰与磁铁矿的标准卡(JCPDS：19-0629)基本吻合，表明合成的Fe2.5Cr0.5O4和Fe3O4为立方晶系尖晶石结构。Fe2.5Cr0.5O4的主要衍射峰出现且尖锐，表明合成的Fe2.5Cr0.5O4的结晶度很好。
Fe2.5Cr0.5O4的SEM图谱可参见图2
图2为Fe2.5Cr0.5O4的SEM照片，由图2可以看出，样品颗粒分散均匀、大小均一，样品团聚小，呈现规则的形貌状态。
以Fe2.5Cr0.5O4为异相芬顿催化剂对阴离子型染料酸性橙Ⅱ废水的脱色
酸性橙Ⅱ(AOII)异相Fenton脱色实验在500mL碘量瓶中进行。实验条件如下：酸性橙Ⅱ初始浓度为100mg/L，初始pH为7.0，磁力搅拌器以450r/min搅拌，使磁铁矿处于悬浮状态。在20℃条件下迅速加入H2O2(0.1mol/L)溶液并开始计时，于设定时刻取样测定酸性橙Ⅱ浓度的变化。
从图3中可以看出，反应1410min后，空白对照(仅加入H2O2)体系，AOII没有被去除，表明仅H2O2对AOII没有降解脱色能力。加入Fe2.5Cr0.5O4后，AOII的脱色速度非常快，在反应330min时脱色率就达到83.3％，1410min后脱色率达到90.7％。表明Fe2.5Cr0.5O4催化剂的加入可以显著提高对酸性橙II的Fenton的脱色。
Claims (7)
1.一种铬掺杂磁铁矿异相芬顿催化剂，其特征在于，该掺铬磁铁矿催化剂为Fe2.5Cr0.5O4。
2.根据权利要求1所述的铬掺杂磁铁矿异相芬顿催化剂，其特征在于，催化剂采用共沉淀法制备，包括如下具体步骤：
(1)按照Fe2+:Cr3+为2.5:0.5的摩尔比取的亚铁盐和九水合硝酸铬，并溶解为金属离子混合液；
(2)取体积为1/4金属离子混合液体积的碱溶液，稀释一倍后，将金属离子混合液迅速倒入碱溶液中，搅拌反应；
(3)搅拌反应完毕后，经反复离心与洗涤、干燥、研磨、在400℃下煅烧3h。
3.根据权利要求2所述的铬掺杂磁铁矿异相芬顿催化剂，其特征在于，步骤(1)中，亚铁盐为七水合硫酸亚铁，混合溶液中金属离子浓度约为0.3mol/L。
4.根据权利要求2所述的掺铬磁铁矿催化剂，其特征在于，步骤(2)中，碱溶液为氨水或氢氧化钠，质量浓度为25.0-28.0％。
5.根据权利要求2所述的掺铬磁铁矿催化剂，其特征在于，步骤(2)中，搅拌反应时间为2h。
6.根据权利要求2所述的掺铬磁铁矿催化剂，其特征在于，步骤(3)中，干燥温度为100℃，干燥时间为12h，研磨的目数为40～60目。
7.根据权利要求2-6所述的掺铬磁铁矿催化剂的制备方法。
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| CN112520902A (zh) * | 2020-12-17 | 2021-03-19 | 梅征 | 不锈钢酸洗刷洗水资源化利用的方法 |
| CN113058602A (zh) * | 2021-04-08 | 2021-07-02 | 南京大学 | 一种调控铁基芬顿催化剂氧化活性物选择性生成的方法 |
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| CN108786852A (zh) * | 2018-07-11 | 2018-11-13 | 常州大学 | 一种用于光芬顿反应材料的制备方法 |
| CN112520902A (zh) * | 2020-12-17 | 2021-03-19 | 梅征 | 不锈钢酸洗刷洗水资源化利用的方法 |
| CN113058602A (zh) * | 2021-04-08 | 2021-07-02 | 南京大学 | 一种调控铁基芬顿催化剂氧化活性物选择性生成的方法 |
| CN113058602B (zh) * | 2021-04-08 | 2022-03-18 | 南京大学 | 一种调控铁基芬顿催化剂氧化活性物选择性生成的方法 |
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