CN108083347A - 钴离子诱导花状钴锰氧化物的制备及其产品和应用 - Google Patents
钴离子诱导花状钴锰氧化物的制备及其产品和应用 Download PDFInfo
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 80
- 239000010941 cobalt Substances 0.000 title claims abstract description 43
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910000428 cobalt oxide Inorganic materials 0.000 title claims abstract description 40
- 229910001429 cobalt ion Inorganic materials 0.000 title claims abstract description 31
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 28
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 13
- 239000011572 manganese Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002351 wastewater Substances 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 4
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims 3
- KTPIHRZQGZDLSN-UHFFFAOYSA-N cobalt;nitric acid Chemical compound [Co].O[N+]([O-])=O KTPIHRZQGZDLSN-UHFFFAOYSA-N 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 238000004088 simulation Methods 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 18
- -1 hydroxyl radical free radical Chemical class 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 230000000977 initiatory effect Effects 0.000 abstract description 3
- 230000010718 Oxidation Activity Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 229910016978 MnOx Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000009415 formwork Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 229910002451 CoOx Inorganic materials 0.000 description 1
- 229910015189 FeOx Inorganic materials 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000006385 ozonation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
本发明公开一种钴离子诱导花状钴锰氧化物的制备及其产品和应用，以高锰酸钾为锰源，硝酸钴为钴源，二价钴离子为结构导向剂，水热条件下诱导合成花状钴锰氧化物。该方法制备的花状钴锰氧化物富含氧空位，有利于引发臭氧催化过程中强氧化羟基自由基的产生。花状钴锰氧化物的多级孔结构，有利于吸附水中有机污染物，并将其在表面催化降解，进一步提高催化剂的臭氧催化活性。该催化剂在草酸模拟废水臭氧催化过程中，具有很好的催化氧化活性。本发明催化剂工艺简单，催化性能优异，具有极好的应用前景。
Description
技术领域
本发明涉及纳米材料的制备领域，具体的涉及一种钴离子诱导花状钴锰氧化物的制备及其产品和应用。
背景技术
目前氧化技术如光催化、臭氧氧化、芬顿反应、湿式催化氧化等，是一种有效降解废水中难降解有机污染物的技术手段。其中，臭氧氧化技术具有氧化能力强、反应速度快，无二次污染、清洁环保，可现场制造臭氧、无需储运等特点，在水处理方面应用非常广泛。
多相臭氧氧化过程中，臭氧在催化剂存在的情况下，产生大量强氧化性羟基自由基，能够将废水中的有机物直接氧化，达到降解的目的。与臭氧直接氧化相比，基于羟基自由基的多相臭氧氧化反应速度更快，且不具选择性，能够高效降解大部分难降解有机污染物。
常用的臭氧氧化催化剂有金属氧化物，如MnOx、FeOx、TiO2、CoOx等，和担载型金属氧化物，常用Al2O3、沸石、活性炭等作为载体。因此，提高臭氧催化效率的根本在于提高金属氧化物的臭氧活化能力。MnOx具有较高的臭氧催化性能，同时锰的可变价态最多，适当的调变MnOx微观结构，有望实现其多相臭氧催化性能的显著提高。
发明内容
为克服现有技术的不足，本发明目的在于提供一种钴离子诱导花状钴锰氧化物的制备方法。
本发明的再一目的在于：提供一种上述方法制备的钴离子诱导花状钴锰氧化物产品。
本发明的又一目的在于：提供一种上述产品的应用。
本发明目的通过下述方案实现：一种钴离子诱导花状钴锰氧化物的制备方法，其特征在于：以高锰酸钾为锰源，硝酸钴为钴源，二价钴离子为结构导向剂，水热条件下诱导合成花状钴锰氧化物；其中，
所述高锰酸钾与硝酸钴的质量比为1:1–1:1.5；
所述高锰酸钾，其溶液浓度为30–60g/L；
所述硝酸钴，其溶液浓度为40–90g/L；
所述水热条件为，100-150℃水热反应18-30小时，制得钴离子诱导花状钴锰氧化物。
具体包括如下步骤：
（1）按上述比例称取高锰酸钾和硝酸钴，分别溶于35mL去离子水中，得到充分混合溶液；
（2）将上述溶液充分混合，转移至聚四氟乙烯内衬的高压反应釜中，100-150℃水热反应18-30小时。所得沉淀抽滤、洗涤、50-100℃干燥，得钴离子诱导花状钴锰氧化物（KσCo(1+δ)Mn(2-δ)Ox，0＜σ≤0.2，0＜δ≤0.2）。
本发明提供一种钴离子诱导花状钴锰氧化物，根据上述所述方法制备得到。
本发明提供一种钴离子诱导花状钴锰氧化物作为催化剂应用于草酸模拟废水臭氧催化反应。
其中，模拟草酸废水初始TOC为130 mg/L，加入适量花状钴锰氧化物，分散均匀后通臭氧，臭氧发生器产生的臭氧量为300 mL/min。
本发明产品在多相臭氧催化净化草酸模拟废水过程中，具有很好的催化净化活性。本发明催化剂原料易得，工艺简单，催化性能良好，具有极好的应用前景。
利用反应体系中的钴离子诱导制备花状钴锰氧化物，无需添加有机模板剂，制备方法简单。该方法制备的花状钴锰氧化物富含氧空位，有利于引发臭氧催化过程中强氧化羟基自由基的产生。花状钴锰氧化物的多级孔结构，有利于吸附水中有机污染物，并将其在表面催化降解，进一步提高催化剂的臭氧催化活性。
与现有技术相比，本发明具有以下优势：
（1）利用反应体系中的钴离子诱导制备花状钴锰氧化物，无需添加有机模板剂，制备方法简单。
（2）该方法制备的花状钴锰氧化物富含氧空位，有利于引发臭氧催化过程中强氧化羟基自由基的产生。
（3）花状钴锰氧化物的多级孔结构，有利于吸附水中有机污染物，并将其在表面催化降解，进一步提高催化剂的臭氧催化活性。
附图说明
图1为实施例1中钴离子诱导花状钴锰氧化物的TEM图；
图2为实施例1中钴离子诱导花状钴锰氧化物的SEM图。
具体实施方式
实施例1
称取2g高锰酸钾和2.5g硝酸钴，分别溶于35mL去离子水中；将上述溶液充分混合，转移至聚四氟乙烯内衬的高压反应釜中，100℃水热反应21小时；所得沉淀抽滤、洗涤、50℃干燥，得钴离子诱导花状钴锰氧化物（KσCo(1+δ)Mn(2-δ)Ox，0＜σ≤0.2，0＜δ≤0.2），记为KCM-1。图1为KCM-1的TEM图，为花状钴锰氧化物。图2为KCM-1的SEM图。
实施例2
称取2g高锰酸钾和2g硝酸钴，分别溶于35mL去离子水中；将上述溶液充分混合，转移至聚四氟乙烯内衬的高压反应釜中，100℃水热反应21小时；所得沉淀抽滤、洗涤、50℃干燥，得钴离子诱导花状钴锰氧化物（KσCo(1+δ)Mn(2-δ)Ox，0＜σ≤0.2，0＜δ≤0.2），记为KCM-2。
实施例3
称取2g高锰酸钾和3g硝酸钴，分别溶于35mL去离子水中；将上述溶液充分混合，转移至聚四氟乙烯内衬的高压反应釜中，100℃水热反应21小时；所得沉淀抽滤、洗涤、50℃干燥，得钴离子诱导花状钴锰氧化物（KσCo(1+δ)Mn(2-δ)Ox，0＜σ≤0.2，0＜δ≤0.2），记为KCM-3。
实施例4
称取2g高锰酸钾和2.5g硝酸钴，分别溶于35mL去离子水中；将上述溶液充分混合，转移至聚四氟乙烯内衬的高压反应釜中，150℃水热反应18小时；所得沉淀抽滤、洗涤、100℃干燥，得钴离子诱导花状钴锰氧化物（KσCo(1+δ)Mn(2-δ)Ox，0＜σ≤0.2，0＜δ≤0.2），记为KCM-4。
实施例5
称取2g高锰酸钾和2.5g硝酸钴，分别溶于60mL去离子水中；将上述溶液充分混合，转移至聚四氟乙烯内衬的高压反应釜中，100℃水热反应24小时；所得沉淀抽滤、洗涤、50℃干燥，得钴离子诱导花状钴锰氧化物（KσCo(1+δ)Mn(2-δ)Ox，0＜σ≤0.2，0＜δ≤0.2），记为KCM-5。
应用例1
将实施例1中的钾离子掺杂的钴离子诱导花状钴锰氧化物进行臭氧催化性能评价，模拟草酸废水初始TOC为130mg/L，催化剂相对废水的投加量为12.5g/L，臭氧发生器产生的臭氧量为300 mL/min，经过10 min的臭氧催化，TOC的去除比活性为32 mgTOC·gcat -1·h-1（毫克TOC/克催化剂/小时）。
以上对本发明的具体实施例进行了描述。应当指出的是，本发明并不局限于上述特定实施方式，本领域技术人员可以在权利要求的范围内做出各种变形或修改，这并不影响本发明的实质内容。
Claims (5)
1.一种钴离子诱导花状钴锰氧化物的制备方法，其特征在于：以高锰酸钾为锰源，硝酸钴为钴源，二价钴离子为结构导向剂，水热条件下诱导合成花状钴锰氧化物；其中，
所述高锰酸钾与硝酸钴的质量比为1:1–1:1.5；
所述高锰酸钾，其溶液浓度为30–60g/L；
所述硝酸钴，其溶液浓度为40–90g/L；
所述水热条件为，100-150℃水热反应18-30小时，制得钴离子诱导花状钴锰氧化物。
2.根据权利要求1所述的钴离子诱导花状钴锰氧化物的制备方法，其特征在于：包括如下步骤：
（1）称取高锰酸钾和硝酸钴，分别溶于35mL去离子水中，得到充分混合的溶液；
（2）将上述溶液转移至聚四氟乙烯内衬的高压反应釜中，100-150℃水热反应18-30小时，所得的沉淀物经抽滤、洗涤、50-100℃干燥，制得钴离子诱导花状钴锰氧化物（KσCo(1+δ)Mn(2-δ)Ox，0＜σ≤0.2，0＜δ≤0.2）。
3.一种钴离子诱导花状钴锰氧化物，其特征在于，根据权利要求1或2所述方法制备得到。
4.一种根据权利要求3所述的钴离子诱导花状钴锰氧化物作为催化剂应用于草酸模拟废水臭氧催化反应。
5.根据权利要求3所述的钴离子诱导花状钴锰氧化物作为催化剂应用，其特征在于：所述的模拟草酸废水初始TOC为130 mg/L，加入适量花状钴锰氧化物，分散均匀后通臭氧，臭氧发生器产生的臭氧量为300 mL/min。
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| CN110627126A (zh) * | 2019-10-24 | 2019-12-31 | 福州大学 | 一种自支撑超薄二维花状锰氧化物纳米片的制备及应用 |
| CN112156791A (zh) * | 2020-10-16 | 2021-01-01 | 上海纳米技术及应用国家工程研究中心有限公司 | 一种臭氧催化净化材料的制备方法及其产品和应用 |
| CN114558588A (zh) * | 2022-03-17 | 2022-05-31 | 天津大学 | 锰基复合催化剂及其制备方法、烟气处理方法 |
| CN115337935A (zh) * | 2022-07-26 | 2022-11-15 | 北方民族大学 | 具有高催化活性的Cu-MnO2纳米催化剂、其制备方法和应用及印染废水处理方法 |
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| CN110627126A (zh) * | 2019-10-24 | 2019-12-31 | 福州大学 | 一种自支撑超薄二维花状锰氧化物纳米片的制备及应用 |
| CN112156791A (zh) * | 2020-10-16 | 2021-01-01 | 上海纳米技术及应用国家工程研究中心有限公司 | 一种臭氧催化净化材料的制备方法及其产品和应用 |
| CN114558588A (zh) * | 2022-03-17 | 2022-05-31 | 天津大学 | 锰基复合催化剂及其制备方法、烟气处理方法 |
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| CN115337935A (zh) * | 2022-07-26 | 2022-11-15 | 北方民族大学 | 具有高催化活性的Cu-MnO2纳米催化剂、其制备方法和应用及印染废水处理方法 |
| CN115337935B (zh) * | 2022-07-26 | 2024-01-23 | 北方民族大学 | 具有高催化活性的Cu-MnO2纳米催化剂、其制备方法和应用及印染废水处理方法 |
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