CN110436532A - 一种层状双氢氧化物纳米材料,制备方法及其应用 - Google Patents
一种层状双氢氧化物纳米材料,制备方法及其应用 Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims description 19
- 239000002086 nanomaterial Substances 0.000 claims abstract description 26
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- 230000015556 catabolic process Effects 0.000 claims abstract description 10
- 238000006731 degradation reaction Methods 0.000 claims abstract description 10
- 230000004913 activation Effects 0.000 claims abstract description 8
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- 229910016874 Fe(NO3) Inorganic materials 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 229910000863 Ferronickel Inorganic materials 0.000 claims description 23
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 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 claims 3
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 1
- QJSRJXPVIMXHBW-UHFFFAOYSA-J iron(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Fe+2].[Ni+2] QJSRJXPVIMXHBW-UHFFFAOYSA-J 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 8
- 239000000975 dye Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 231100000053 low toxicity Toxicity 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 241001062009 Indigofera Species 0.000 description 2
- 241000446313 Lamella Species 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
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- 238000001228 spectrum Methods 0.000 description 2
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- 241001614291 Anoplistes Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
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- 239000004927 clay Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- -1 persulfuric acid Salt Chemical class 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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Abstract
本发明属于一种层状双氢氧化物纳米材料，公开了一种由二价和三价金属(NI、Fe)氢氧化物组成的新型层状无机纳米材料及其在活化过硫酸盐降解污水中亚甲基蓝中的应用。本发明采用共沉淀法合成技术，首先将一定配比的九水合硝酸铁和六水合硝酸镍溶于水形成溶液A，然后将一定物质的量的氢氧化钠和碳酸钠溶于水形成溶液B，两种溶液混合后产生沉淀，将沉淀离心洗涤后烘干即得层状镍铁氢氧化物。该材料可高效稳定的活化过硫酸盐降解污水中亚甲基蓝。
Description
技术领域
本发明属于纳米材料制备及环保领域，具体涉及一种低毒、生物相容性好、保存条件要求低的新型层状无机纳米材料及其活化过硫酸盐降解亚甲基蓝的应用。
背景技术
目前染料行业是我国国民经济的重要支撑行业，主要用于涂料、医药、纺织品、化妆品等领域。但在染料的生产和使用过程中，染料废水未经处理或未达到排放标准直接排放导致的环境污染问题亟待解决。过硫酸盐活化后能产生·SO4 -，·OH，O2 -和h+活性自由基从而降解染料中主要有机物亚甲基蓝。
层状双氢氧化物，常被叫做阴离子粘土或水滑石，是一种低毒，生物相容性好，易保存的无机纳米材料。主要由二价和三金属氢氧化物组成，分子通式为层状双氢氧化物制备成本较低，操作简单，种类性质丰富。在催化(如酸碱催化剂、氧化还原催化剂及催化剂载体)、医药(如治疗胃病的抗酸药)、离子交换和吸附等方面用途广泛。
发明内容
本发明的目的是提供一种活化过硫酸盐从而降解亚甲基蓝的新型纳米材料及其制备方法，并将其应用于降解亚甲基蓝反应，其制备方法简单，生物相容性好，活化过硫酸盐稳定高效。
本发明采用共沉法原理合成得到层状双氢氧化物。
为实现上述目的，本发明采用的技术方案为：
一种层状双氢氧化物纳米材料，该纳米材料为镍铁层状双氢氧化物：所述的镍铁层状双氢氧化物为疏松多孔的超薄片层，表面存在晶格条纹，晶格间距d＝0.39nm：镍铁比例为2∶1～10∶1，优选为2∶1，3∶1，4∶1，5∶1，10∶1。进一步优选为镍铁比例为4∶1。
本发明所述的层状双氢氧化物纳米材料的制备方法包括以下几个步骤：
(1)将九水合硝酸铁(Fe(NO3)3·9H2O)和六水合硝酸镍(Ni(NO3)2·6H2O)以摩尔比2∶1～10∶1的比例溶于去离子水中形成溶液A。
(2)将氢氧化钠和碳酸钠溶于水中形成溶液B。
(3)将溶液B缓慢滴入A中，剧烈搅拌4h。所得沉淀离心，用去离子水洗涤至pH为中性。60℃条件下干燥12h即得层状双氢氧化物纳米材料。
本发明还提供一种将上述层状双氢氧化物材料在活化过硫酸盐从而去除水中亚甲基蓝的应用。具体步骤为将层状双氢氧化物纳米材料按1.0g/L的比例投加到10mg/L的亚甲基蓝溶液中，持续搅拌30min，后按比例加入过硫酸盐，反应在室自然光或黑暗条件下进行，反应温度为40℃，反应时间为120min，即可完成对亚甲基蓝的降解。
上述步骤中所述的活化过硫酸盐方法，所述的加入按比例加入的过硫酸盐与亚甲基蓝的比例为20∶1。
所述的亚甲基蓝广泛应用于化学指示剂、染料、生物染色剂和药物等方面。其结构中含有碱性基团，色泽浓艳，水溶性好，含有复杂的芳香基团因而难以去除色度，成为染料废水处理的难题。因此，寻找高效处理染料废水的技术方法成为国内外研究的热点。
附图说明
图1：为实施例制得的镍铁双氢氧化物纳米材料的SEM表征图。
图2：为实施例制得的镍铁双氢氧化物纳米材料的XRD图谱。
图3：为实施例制得的镍铁双氢氧化物纳米材料的TEM表征图。
图4：为实施例制得的镍铁双氢氧化物纳米材料的XPS谱图总谱。
图5：为实施例制得的镍铁双氢氧化物纳米材料的XPS谱图C1s谱图。
图6：为实施例制得的镍铁双氢氧化物纳米材料的XPS谱图Ni2p谱图。
图7：为实施例制得的镍铁双氢氧化物纳米材料的XPS谱图Fe2p谱图。
具体实施方式
下面结合具体实施案例，进一步阐述本发明，应理解此具体实施案例仅用于说明本发明而不用于限制本发明的范围，在阅读了本发明之后，本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定的范围。
实施例
1)将九水合硝酸铁(Fe(NO3)3·9H2O)和六水合硝酸镍(Ni(NO3)2·6H2O)以摩尔比4∶1的比例溶于40mL去离子水中形成溶液A。
2)将40mmol氢氧化钠和4mmol碳酸钠溶于40mL水中形成溶液B。
3)将溶液B缓慢滴入A中，剧烈搅拌4h。所得沉淀离心，用去离子水洗涤至pH为中性。60℃条件下干燥12h即得镍铁层状双氢氧化物纳米材料。
上述制备的镍铁层状双氢氧化物(NiFe-LDH)纳米材料的SEM表征图如图1所示，从中看出NiFe-LDH材料主要为疏松多孔的超薄片层，这种结构比表面积比较大，能够提供较多的活性位点，且片层间距离能够加快传质速率和电荷转移速率。
上述制备的镍铁层状双氢氧化物(NiFe-LDH)纳米材料的XRD图谱如图2所示，从中可以看出，NiFe-LDH样品在2θ＝34.6°处有明显的不对称特征衍射峰，反应出其形貌为纳米花状。这是由于这种超薄纳米片不同方向上的厚度存在差异而使窄尖峰和弱宽峰两个特征峰发生重叠，且前半峰宽远远低于后半峰，从而引起不对称峰的出现。NiFe-LDH在2θ＝11.5°、22.6°、34.3°、38.7°和61.2°处存在5个主要的特征峰，这表明生成的NiFe-LDH纯度较高，结晶度较好。晶面衍射峰的出现证明NiFe-LDH的层状结构。
上述制备的镍铁层状双氢氧化物(NiFe-LDH)纳米材料的TEM表征图如图3所示，从中看出有晶格条纹的存在，经测得晶格间距d＝0.39nm，对应于(006)晶面，与XRD测试相符。
上述制备的镍铁层状双氢氧化物(NiFe-LDH)纳米材料的XPS图谱总谱如图4所示，从中可以看出，NiFe-LDH包含Ni、Fe、O、H、C五种元素。
上述制备的镍铁层状双氢氧化物(NiFe-LDH)纳米材料的XPS图谱C1s谱图如图5所示，从中可以看出，C 1s在284.81eV、286.32eV和289.5eV处有三个明显的特征峰，分别对应不定型碳，sp3杂化的碳和N-C＝N上的sp2杂化的碳。
上述制备的镍铁层状双氢氧化物(NiFe-LDH)纳米材料的XPS图谱Ni2p谱图如图6所示，从中可以看出，Ni2p在855.81eV，861.59eV，873.58eV和879.87eV处有四个特征峰。分别可以与Ni2+2p3/2sat，2p3/2，Ni2+2p1/2sat，2p1/2的结合能相拟合。
上述制备的镍铁层状双氢氧化物(NiFe-LDH)纳米材料的XPS图谱Fe2p谱图如图7所示，从中可以看出，Fe2p在712.64eV，725.88eV处的特征峰可以与Fe3+2p3/2，Fe3+2p1/2的结合能相拟合。
将上述制备的镍铁层状双氢氧化物纳米材料进行活化过硫酸盐从而去除亚甲基蓝，将层状双氢氧化物纳米材料按1.0g/L的比例投加到10mg/L的亚甲基蓝溶液中，持续搅拌30min，后按比例加入过硫酸盐，反应在室自然光或黑暗条件下进行，反应温度为40℃，反应时间为120min，即可完成对亚甲基蓝的降解，降解率最高可达86.2％。
本发明的特点和优点，材料制备简单、低毒、生物相容性好、保存条件要求低，且降解过程不受PH值的影响。
Claims (10)
1.一种层状双氢氧化物纳米材料，其特征在于，该纳米材料为层状双氢氧化物：所述的层状双氢氧化物表面存在晶格，晶格间距为d＝0.39nm。
2.权利要求1所述的层状双氢氧化物，其特征在于，由镍铁组成。
3.权利要求1所述的层状双氢氧化物，其特征在于，镍铁比例为2∶1～10∶1。
4.权利要求1-3任一项所述层状双氢氧化物纳米材料的制备方法，其特征在于，包括如下步骤：
(1)将九水合硝酸铁和六水合硝酸镍溶于40mL去离子水中形成溶液A。
(2)将氢氧化钠和碳酸钠溶于40mL水中形成溶液B。
(3)将溶液B缓慢滴入A中，剧烈搅拌4h，得到沉淀。
(4)将得沉淀离心，用去离子水洗涤至pH为中性，60℃条件下干燥12h得到层状双氢氧化物纳米材料。
5.权利要求4所述层状双氢氧化物纳米材料的制备方法，其特征在于，步骤(1)中九水合硝酸铁和六水合硝酸镍的比例为2∶1～10∶1。
6.权利要求4所述层状双氢氧化物纳米材料的制备方法，其特征在于，步骤(2)中氢氧化钠物质的量为40mmol碳酸钠物质的量为4mmol。
7.权利要求1-6任一项所述层状双氢氧化物纳米材料在活化过硫酸盐降解水中亚甲基蓝上的应用。
8.权利要求7所述应用，其特征在于，具体步骤如下：将层状双氢氧化物纳米材料按1.0g/L的比例投加到10mg/L的亚甲基蓝溶液中，持续搅拌30min，后加入过硫酸盐，反应在室自然光或黑暗条件下进行，反应温度为40℃，反应时间为120min，即可完成对亚甲基蓝的降解。
9.权利要求8所述应用，其特征在于，本反应中层状双金属氢氧化物镍铁最优比为4∶1。
10.权利要求8所述应用，其特征在于，过硫酸盐与亚甲基蓝物质的量比为20∶1。
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