CN115676892B - 一种三价锰的制备方法 - Google Patents
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- 239000011572 manganese Substances 0.000 title claims abstract description 53
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
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- 238000000034 method Methods 0.000 claims abstract description 18
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 13
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 13
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- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 claims description 23
- 229960001680 ibuprofen Drugs 0.000 claims description 23
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 description 7
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- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 5
- 229940048086 sodium pyrophosphate Drugs 0.000 description 5
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 5
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- 239000000356 contaminant Substances 0.000 description 4
- 229940077478 manganese phosphate Drugs 0.000 description 4
- HDMGAZBPFLDBCX-UHFFFAOYSA-M potassium;sulfooxy sulfate Chemical compound [K+].OS(=O)(=O)OOS([O-])(=O)=O HDMGAZBPFLDBCX-UHFFFAOYSA-M 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
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- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical group Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
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- 231100000086 high toxicity Toxicity 0.000 description 1
- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- MMIPFLVOWGHZQD-UHFFFAOYSA-N manganese(3+) Chemical compound [Mn+3] MMIPFLVOWGHZQD-UHFFFAOYSA-N 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
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- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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Abstract
本发明涉及一种三价锰的制备方法，属于环境保护领域。一种三价锰的制备方法，室温下，将MXene材料、二价锰无机盐和过硫酸盐置于水中混合，反应，原位制备三价锰溶液。一种去除水体有机污染物的方法，将三价锰溶液与待处理受污染水体混合，或将MXene材料、二价锰无机盐和过硫酸盐按比例直接投入到受污染水体中，以去除水体中的有机污染物。该制备方法具备以下优势：实现三价锰在水体中的原位制备，不消耗高锰酸钾和其他还原剂，能够高效制备高活性三价锰。与现有的高锰酸钾法相比，本发明制备方法简单，工艺操作流程简化。
Description
技术领域
本发明涉及一种三价锰的制备方法，属于环境保护领域。
背景技术
传统污水处理方法对水中的难降解有机污染物如抗生素类药物、内分泌干扰物、个人护理用品、合成农药等去除效果较差。难降解污染物具有持久性高、毒性大的特点，不仅对水环境造成破坏，还会对人体和动植物健康产生威胁[1,2]。研究表明，高活性的三价锰能够快速降解水中存在的难降解有机物[3]。目前合成三价锰常用的方法为亚硫酸盐活化高锰酸钾生成高活性的三价锰[3]。上述合成反应需要消耗过量的亚硫酸盐还原剂，反应条件苛刻，生成三价锰的效率较低。
参考文献
[1]郭倩,唐光贝,彭稳,罗永明,高晓亚.卡马西平及其衍生物的环境行为及其去除研究进展[J].环境化学,2019,38(08):1708-1715.
[2]Sze Yee Wee,AhmadZaharinAris.Endocrine disrupting compounds indrinking water supply system and human health risk implication[J].EnvironmentInternational,2017,106:207-233.
[3]Sun B,Guan X,Fang J,Paul G.Tratnyek.Activation of ManganeseOxidants with Bisulfite for Enhanced Oxidation of Organic Contaminants:TheInvolvement of Mn(III)[J].Environmental Science&Technology,2015,49(20):12414-12421.
发明内容
本发明目的在于提供一种简单、高效的三价锰制备方法，本发明合成的高活性三价锰能够快速去除水体中有机污染物。
一种三价锰的制备方法，包括下工艺步骤：
室温下，将MXene材料、二价锰无机盐和过硫酸盐置于水中混合，反应，原位制备三价锰溶液。
优选地，所述二价锰无机盐为MnCl2、MnSO4、Mn(NO3)2或Mn3(PO3)2。
优选地，所述过硫酸盐为单过硫酸盐。
优选地，所述MXene为Mn+1Xn结构的二维材料，n＝1，2，3或4；M为过渡金属元素，包括Ti、Sc、V、Cr、Zr、Mo、Nb、Hf或Ta；X为C、N或B。
进一步优选地，所述的MXene为Ti3C2MXene或NbC MXene。
优选地，所述MXene材料与二价锰无机盐的质量比为1:0.1～1:10。
优选地，所述MXene材料与单过硫酸盐的质量比为1:0.1～1:10。
本发明所述方法中，将MXene材料、二价锰无机盐和过硫酸盐置于水中混合，其中用水量满足反应完成即可。
优选地，MXene材料与水的比例为1g：100～1000mL。
优选地，反应的水溶液的pH小于7.0。
本发明所述反应水溶液的pH需小于7.0，可利用稀盐酸、稀硫酸或者稀硝酸溶液将反应水溶液的pH调节至小于7.0。
本发明的另一目的是提供利用上述三价锰去除水体有机污染物的方法。
一种去除水体有机污染物的方法，将所得三价锰溶液与待处理受污染水体混合，或将MXene材料、二价锰无机盐和过硫酸盐按比例直接投入到受污染水体中，以去除水体中的有机污染物。
进一步地，所述有机污染物为布洛芬。
进一步地，当将MXene材料、二价锰无机盐和过硫酸盐按比例直接投入到受污染水体中时，MXene材料与受污染水体中污染物的比例为1g：0.01～10g。
进一步地，当将所得三价锰溶液与待处理受污染水体混合时，按照MXene材料与受污染水体中污染物的比例为1g：0.01～10g进行混合。
本发明的有益效果为：本发明所述的三价锰是以二价Mn的无机盐作为锰源，在常温常压条件下将MXene材料、二价锰盐与过硫酸盐混合反应原位制得的。该制备方法具备以下优势：实现三价锰在水体中的原位制备，不消耗高锰酸钾和其他还原剂，能够高效制备高活性三价锰。与现有的高锰酸钾法相比，本发明制备方法简单，工艺操作流程简化。
附图说明
图1为本发明实施例1制备的三价锰的紫外可见分光光谱图。由图可见，在258nm处出现一处明显特征峰，这是三价锰和焦磷酸钠形成的稳定络合物的吸收峰。
图2为本发明实施例2制备的三价锰降解合成药物布洛芬(IBP)的效果。
图3为本发明实施例3制备的三价锰降解合成药物布洛芬(IBP)的效果。
图4为本发明实施例4制备的三价锰降解合成药物布洛芬(IBP)的效果。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。
下述实施例中所述试验方法，如无特殊说明，均为常规方法；所述试剂和材料，如无特殊说明，均可从商业途径获得。
一种三价锰的制备方法，具体步骤如下：将MXene材料、二价锰无机盐和过硫酸盐加入到水溶液中，搅拌混合反应制得三价锰。
优选地，所述的MXene为指多层或少层的二维过渡金属碳化物或氮化物。
优选地，所述MXene是结构式为Mn+1Xn的二维材料，n＝1、2、3或4，M为Ti、Sc、V、Cr、Zr、Mo、Nb、Hf或Ta，X为C、N或B。
优选地，所述的MXene为Ti3C2MXene或NbCMXene。
优选地，所述的锰盐为二氯化锰、硫酸锰、硝酸锰或磷酸锰。
优选地，所述过硫酸盐过一硫酸盐。
优选地，MXene与二价锰无机盐的质量比为1:0.1～1:10。
优选地，MXene与单过硫酸盐的质量比为1:0.1～1:10。
优选地，水溶液pH值小于7.0。
下述实施例中，为了检测原位合成的三价锰，在合成三价锰后加入焦磷酸钠，使三价锰与焦磷酸钠形成络合物后便于检测。
实施例1
将10mg Ti3C2MXene，2mg MnCl2粉末和20mg过硫酸氢钾加入到100mL pH＝4.0的水溶液(利用浓度为10mM盐酸调节)中，搅拌反应1分钟后，加入焦磷酸钠稳定剂。反应2分钟后，取3mL溶液过膜，放入紫外可见分光光度计中进行吸光度测定(如图1所示)。258nm处明显的吸收峰属于三价锰与焦磷酸钠形成络合物的吸收峰。
实施例2
将10mg Ti3C2MXene，1mgMnCl2粉末和5mg过硫酸氢钾加入到100mL含有10μM布洛芬的pH＝5.0的水溶液(利用浓度为10mM硫酸调节)中，在不同时间点取样，使用液相色谱测定布洛芬(IBP)的降解速率。如图2所示，布洛芬(IBP)在10min内去除率可达100％。
实施例3
将50mg Nb2C MXene，5mg MnSO4粉末和20mg过硫酸氢钾加入到100mL含有20μM布洛芬的经过稀硝酸(浓度为5mM)调节pH＝3.0的水溶液中，测定布洛芬(IBP)的降解速率。布洛芬(IBP)在8min内去除率达到100％。
实施例4
将30mg V2C MXene，50mg MnSO4粉末和100mg过硫酸氢钾加入到100mL含有10μM布洛芬的经过稀硝酸(浓度为5mM)调节pH＝2.0的水溶液中，测定布洛芬(IBP)的降解速率。布洛芬(IBP)在3min内去除率达到100％。
Claims (5)
1.一种三价锰的制备方法，其特征在于，室温下，将MXene材料、二价锰无机盐和过硫酸盐置于水中混合，反应，原位制备三价锰溶液，
所述二价锰无机盐为MnCl2、MnSO4、Mn(NO3)2或Mn3(PO3)2；所述过硫酸盐为单过硫酸盐；反应的水溶液的pH小于7.0。
2.根据权利要求1所述的方法，其特征在于，所述MXene为Mn+1Xn结构的二维材料，n＝1，2，3或4；M为过渡金属元素，包括Ti、Sc、V、Cr、Zr、Mo、Nb、Hf或Ta；X为C、N或B。
3.根据权利要求1所述的方法，其特征在于，所述MXene材料与二价锰无机盐的质量比为1:0.1～1:10。
4.根据权利要求1所述的方法，其特征在于，所述MXene材料与单过硫酸盐的质量比为1:0.1～1:10。
5.一种去除水体有机污染物的方法，其特征在于：将权利要求1所得三价锰溶液与待处理受污染水体混合，或将MXene材料、二价锰无机盐和过硫酸盐按比例直接投入到受污染水体中，以去除水体中的有机污染物，其中，所述有机污染物为布洛芬。
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