CN102225797B - Rare earth doped Ti-based manganese dioxide electrode and preparation method thereof - Google Patents
Rare earth doped Ti-based manganese dioxide electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a rare earth cerium doped Ti-based manganese dioxide electrocatalytic electrode and a preparation method thereof. The electrode consists of an internal layer of Ti substrate, an interlayer of tin-antimony oxide and a surface coating of cerium doped manganese dioxide, wherein, the internal layer of Ti substrate is a pure titanium plate, the interlayer of tin-antimony oxide is a mixture consisting of SnO2 and Sb2O5, the molar ratio of tin to antimony is 3.7:1, and in the surface coating, the molar ratio of cerium to manganese dioxide is 1:25-50. The preparation method comprises the following steps: polishing, alkali washing, pickling and acid embossing the pure titanium plate, then repeatedly painting a coating solution, carrying out a thermal decomposition process on the Ti substrate to prepare the interlayer of tin-antimony oxide and the surface coating of cerium doped manganese dioxide in order. The cerium doped Ti-based manganese dioxide electrode disclosed in the invention has low potential of chlorine evolution and high electrocatalysis capability, and can be used for treating the dyeing and finishing effluents.
Description
Technical field
The invention belongs to Material Field and technical field of waste water processing, be specifically related to a kind of rare-earth element cerium doped titanium-base Manganse Dioxide electro catalytic electrode and preparation method thereof.
Background technology
Electrochemical techniques present good application prospect with its distinctive electrocatalysis function, good treatment effect and compatible preferably in water treatment field.The exploitation of electrode is a key in all too many levels of electrochemical techniques, how to develop cost is low, toxicity is little, environmentally friendly, electro catalytic activity is high water treatment electrode and be scientific and technological researchist institute outline.
The DSA(titanium-based metal oxide electrode that uses at present) electrode mainly contains ruthenium system, iridium system, tin system, plumbous system, manganese system etc., Ti/RuO
2Electrode and Ti/irO
2Electrode belongs to noble metal electrode, Ti/SnO
2Stable not ideal, the Ti/PbO of electrode
2Plumbously in the electrode may stripping causing secondary pollution, the BDD(boron-doped diamond electrode) cost is too high and easily polluted etc.; Ti/MnO
2Electrode pair dyestuff, aldehydes matter, endocrine disrupter etc. have stronger oxidation capacity, can also be used to process heavy metal ion-containing waste water, therefore at environmental area stronger application prospect are arranged.But Ti/MnO
2The electroconductibility of electrode, stability and catalytic activity are desirable not enough, and the adding in middle layer and rare earth doped manganese bioxide coated effect are carried out for this problem just.
Summary of the invention
One of the object of the invention provides that a kind of cost is low, toxicity is little, and environmentally friendly, electro catalytic activity is higher
Rare-earth cerium doped Ti supported manganese dioxide electrode
Two of the object of the invention provides a kind of above-mentioned
Rare-earth cerium doped Ti supported manganese dioxide electrodeThe preparation method.
Technical scheme of the present invention
A kind of rare earth doped Ti-based manganese dioxide electrode, its structure is made of internal layer titanium matrix 1, tin-antimony oxide middle layer 2 and rare earth doped Manganse Dioxide top coat 3, as shown in Figure 1.
Described internal layer titanium matrix is pure titanium plate, titanium plate thickness 3mm;
Tin-antimony oxide is respectively SnO in the described tin-antimony oxide middle layer
2And Sb
2O
5The mixture that forms, the mol ratio of tin and antimony element is 3.7:1 in the mixture; The thickness in described tin-antimony oxide middle layer is about 30 μ m;
The thickness of described rare earth doped Manganse Dioxide top coat is about 100 μ m;
The mol ratio of described rare earth doped Manganse Dioxide top coat rare earth elements and Manganse Dioxide is 1:25～50, and described rare earth element is cerium (Ce).
The preparation method of above-mentioned a kind of rare earth doped Ti-based manganese dioxide electrode, namely thermal decomposition method mainly is divided into three steps, i.e. the preparation of the preparation in the pre-treatment of internal layer titanium matrix, middle layer and top coat.Specifically comprise the steps:
(1) pre-treatment of titanium matrix
Pure titanium plate is as matrix, and before the use, after the titanium plate was polished successively through abrasive paper for metallograph from coarse to fine, oil removal treatment was removed oxide film with acid soak again, then to its acid etching, formed the titanium matrix of pitted skin;
Namely use 200#, 600#, 1200#, the abrasive paper for metallograph of 1500# to the surface of titanium matrix polish successively to smooth smooth after, use saturated sodium hydroxide solution to boil 30min and carry out oil removal treatment, soak 2h with 1:1 nitric acid+sulfuric acid again, then in 10% oxalic acid solution, corrode approximately 25min, treat that the sorrel material occurs, form pitted skin titanium matrix, with after the washed with de-ionized water, be immersed in the dehydrated alcohol for subsequent use at last;
(2) preparation in tin-antimony oxide middle layer
Take by weighing SnCl
45H
2O 0.85g, SbCl
30.15g, measure concentrated hydrochloric acid 1ml, propyl carbinol 4ml is mixed with the middle layer masking liquid, with hairbrush the even scrubbing brush of this masking liquid is passed through on the titanium matrix surface of pre-treatment in step (1), at 500 ℃ of lower sintering 10min, this process repetitive coatings 6 times is at last at 550 ℃ of lower sintering 30min after the oven dry, finally obtain tin-antimony oxide compound middle layer electrode, the tin-antimony oxide intermediate layer thickness is about 30 μ m;
(3) preparation of rare earth doped Manganse Dioxide top coat
Preparation contains the upper layer masking liquid of manganous nitrate and cerous nitrate, with hairbrush this masking liquid is coated in step (2) equably and has prepared tin-antimony oxide compound middle layer electrode surface, 90 ℃ of lower dry 10min, afterwards at 200 ℃ of lower thermolysis 5min, this process repetitive coatings 30 times, sintering time under 350 ℃ is 20min, finally obtains rare earth doped Ti-based manganese dioxide electrode of the present invention;
The mol ratio of Ce elements and Manganse Dioxide is 1:25～50 in the described upper layer masking liquid of step (3).
Rare earth doped Ti-based manganese dioxide electrode of the present invention can be used for dyeing waste water is processed.Its principle of work that dyeing waste water is processed is: at the ClO of electrolysis generation
-Attack under, the methylene blue molecule since electrochemical oxidation process produced scission of link, the condensed ring conjugated structure is destroyed, and changes CO into by macromolecular substance
2(or low molecule organic matter) and water make the solution decolouring.
Beneficial effect of the present invention
Rare earth doped Ti-based manganese dioxide electrode of the present invention, compare with the Ti supported manganese dioxide electrode of prior art, adopt Sn-Sb oxide compound middle layer and rare earth doped, stability and the electroconductibility of electrode have been improved, simultaneously because the promoting catalysis of doped with rare-earth elements has further improved the catalytic activity of electrode.
In addition, electrode of the present invention adopts the thermal decomposition method preparation, and is easy and simple to handle, again because the employing rare earth element is doped raw material, raw materials cost is low, therefore rare-earth doped titanium-base manganese dioxide electrode of the present invention be that a kind of cost is low and stable, the equal higher electrode of electroconductibility and electro catalytic activity.
Description of drawings
The structural representation of Fig. 1, rare-earth cerium doped Ti supported manganese dioxide electrode
The impact that Fig. 2, electrolysis time are removed simulating color degree of dyeing waste water and COD.
Embodiment
Also by reference to the accompanying drawings the present invention is set forth below by embodiment, but do not limit the present invention.
Various instruments and medicine that the present invention is used:
SU-1500 scanning electronic microscope (BeiJing ZhongKe's tech Technology Dev Company Ltd.);
The program control cabinet-type electric furnace of SXL-1208 type (the upper grand testing installation of Nereid company limited);
Electric heating constant-temperature blowing drying box DHG-9076A type (the accurate experimental installation in Shanghai company limited);
SW171501SL-2A type voltage stabilized source (regulator factory, Shanghai);
WFJ-7200 type ultraviolet-visible photometer (Shanghai You Nike Instr Ltd.);
The accurate pH meter (Shanghai Precision Scientific Apparatus Co., Ltd) of PHS-3C.
The all ingredients that the present invention is used
50% manganese nitrate solution (Shanghai permanent letter chemical reagent company limited);
Crystallization tin tetrachloride (Chemical Reagent Co., Ltd., Sinopharm Group);
Butter of antimony (Shishewei Chemical Co., Ltd., Shanghai);
Cerous nitrate (those chemical reagent company limiteds of Shanghai dust);
Methylene blue (upper seamount Pu chemical industry company limited);
Potassium bichromate (those chemical reagent company limiteds of Shanghai dust);
Above reagent is the analytical pure rank.
Embodiment 1
The preparation of 5% cerium doped titanium-base manganese dioxide electrode comprises the steps:
(1), the pre-treatment of titanium matrix
Namely use 200#, 600#, 1200#, the abrasive paper for metallograph of 1500# to the surface of titanium matrix polish successively to smooth smooth after, use saturated sodium hydroxide solution to boil 30min and carry out oil removal treatment, soak 2h with 1:1 nitric acid+sulfuric acid again, then harsh approximately 25min in 10% oxalic acid solution treats that the sorrel material occurs, and forms pitted skin titanium matrix, use at last washed with de-ionized water, be immersed in the dehydrated alcohol;
(2), the preparation in tin-antimony oxide middle layer
Get SnCl
45H
2O0.85g, SbCl
30.15g, HCl (36%) 1mL, propyl carbinol 4ml mixes as masking liquid, with hairbrush with the even scrubbing brush of this masking liquid on the titanium matrix surface, the oven dry after in 500 ℃ of lower sintering 10min, repetitive coatings 6 times, at 550 ℃ of lower sintering 30min, just generate the SnO of even thickness at last
2+ Sb
2O
5Middle layer, thickness are about 30 μ m;
(3), the preparation of rare earth doped Manganse Dioxide top coat
Use 50wt%Mn(NO3) 2 solution, be that the 25:1 ratio adds cerous nitrate in manganese and cerium mol ratio, be mixed with the upper layer masking liquid of 1moldm-3 with distilled water diluting, masking liquid is coated in equably on the electrode surface that has prepared the middle layer with hairbrush, at 90 ℃ of lower dry 10min, then at 200 ℃ of lower thermolysis 5min, this process repetitive coatings 30 times, at last at 350 ℃ of lower sintering 20min, final 5% cerium doped titanium-base manganese dioxide electrode of the present invention, its top coat thickness is about 100 μ m, and the electrode of gained is grey black.
Embodiment 2
The preparation of 10% cerium doped titanium-base manganese dioxide electrode comprises the steps:
(1), the pre-treatment of titanium matrix (with embodiment 1);
(2), the preparation in tin-antimony oxide middle layer (with embodiment 1);
(3), the preparation of rare earth doped Manganse Dioxide top coat
Use 50wt%Mn(NO
3)
2Solution is that the 25:1 ratio adds cerous nitrate in manganese and cerium mol ratio, is mixed with 1moldm with distilled water diluting
-3The upper layer masking liquid, masking liquid is coated in equably on the electrode surface that has prepared the middle layer with hairbrush, at 90 ℃ of lower dry 10min, then at 200 ℃ of lower thermolysis 5min, this process repetitive coatings 30 times, at 350 ℃ of lower sintering 20min, finally obtain 10% cerium doped titanium-base manganese dioxide electrode of the present invention at last, its top coat thickness is about 100 μ m.
Application Example
Utilize the 5% cerium doped titanium-base manganese bioxide electrode material treatment of simulated dyeing waste water test of embodiment 1 gained.
Adopting 5% cerium doped titanium-base manganese dioxide electrode is anode, and the titanium plate is negative electrode, and interelectrode distance is 7cm, and to the sodium chloride electrolysis matter of 600ml simulation methylene blue waste water at normal temperature, 0.1mol/L, electrolysis density is 30mA/cm
2, pH is 9, carries out electrolysis treatment under the electrolysis time 1.5h condition, chroma removal rate is that 96.9%, COD clearance is 91.8% after the wastewater treatment.Simulation dyeing waste water water quality: COD is 317.6mg/L, and colourity spectrophotometry, waste water record its absorbance under 660nm be 2.623.
Accompanying drawing 2 is for utilizing the degradation effect figure of 5% cerium doped titanium-base manganese dioxide electrode treatment of simulated dyeing waste water.As can be seen from Figure 2 along with the increase of electrolysis time, the COD clearance raises gradually, and when electrolysis time was 60min, COD and chroma removal rate were all more than 80 percent, and when electrolysis time was 80min, the COD clearance reached more than 90 percent; Chroma removal rate is then close to a hundred per cent.
The present invention has only carried out the explanation of rare earth doped Ti-based manganese dioxide electrode and its preparation method and application aspect as an example of cerium example, because rare earth doped Ti-based manganese dioxide electrode of the present invention is to have utilized the catalysis of thulium or helped catalytic property, and so that rare earth doped Ti-based manganese dioxide electrode has good catalytic activity, and other rare earth elements such as lanthanum or neodymium etc., those skilled in the art can be prepared and obtain the rare earth doped Ti-based manganese dioxide electrodes such as a kind of lanthanum or neodymium with reference to the preparation method embodiment of rare earth doped Ti supported manganese dioxide electrode of the present invention equally.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (4)
1. a cerium doped titanium-base manganese dioxide electrode is characterized in that described electrode is made of internal layer titanium matrix, tin-antimony oxide middle layer and rare earth doped Manganse Dioxide top coat; Described internal layer titanium matrix is pure titanium plate, titanium plate thickness 3mm;
The thickness 30 μ m in described tin-antimony oxide middle layer; The thickness of described rare earth doped Manganse Dioxide top coat is 100 μ m; Rare earth element in the described rare earth doped Manganse Dioxide top coat is cerium; The mol ratio of cerium doped titanium-base manganese dioxide electrode top coat middle-weight rare earths cerium and Manganse Dioxide is 1:25～50; Cerium doped titanium-base manganese dioxide electrode, described tin-antimony oxide middle layer is SnO
2And Sb
2O
5The mixture that forms, the mol ratio of tin and antimony element is 3.7:1 in the mixture.
2. the preparation method of cerium doped titanium-base manganese dioxide electrode as claimed in claim 1 is characterized in that comprising the steps:
(1), the pre-treatment of titanium matrix:
Pure titanium plate is as matrix, and through polishing and oil removal treatment, acid soak is removed oxide film, then to its acid etching, forms the titanium matrix of pitted skin;
(2), the preparation in tin-antimony oxide middle layer:
Take by weighing SnCl
45H
2O 0.85g, SbCl
30.15g, measure concentrated hydrochloric acid 1ml, propyl carbinol 4ml is mixed with the middle layer masking liquid, with hairbrush this masking liquid is brushed equably on the surface of step (1) through the titanium matrix of the pitted skin of pre-treatment, oven dry is rear at 500 ℃ of lower sintering 10min, this process repetitive coatings 6 times at last at 550 ℃ of lower sintering 30min, finally obtains tin-antimony oxide compound middle layer electrode;
(3), the preparation of rare-earth cerium doped manganese dioxide electrode top coat
Preparation contains the upper layer masking liquid of manganous nitrate and cerous nitrate, with hairbrush this masking liquid is coated in step (2) equably and has prepared tin-antimony oxide compound middle layer electrode surface, 90 ℃ of lower dry 10min, afterwards at 200 ℃ of lower thermolysis 5min, 30 layers of this process repetitive coatings, sintering time under 350 ℃ is 20min, final rare-earth cerium doped Ti supported manganese dioxide electrode.
3. the preparation method of cerium doped titanium-base manganese dioxide electrode as claimed in claim 2 is characterized in that the pre-treating process of the matrix in the step (1) is specific as follows:
Use abrasive paper for metallograph from coarse to fine to polish successively the titanium matrix to smooth smooth, oil removal treatment uses saturated sodium hydroxide solution to boil 30 minutes, 1:1 nitric acid+sulfuric acid soaks 2h, then in 10% oxalic acid solution, corrode 25min, treat that the sorrel material occurs, form pitted skin titanium matrix, use at last washed with de-ionized water, be immersed in the dehydrated alcohol for subsequent use.
4. the rare-earth cerium doped Ti supported manganese dioxide electrode of method preparation as claimed in claim 2 can be used for the processing of dyeing waste water.
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| CN105084467A (en) * | 2014-05-05 | 2015-11-25 | 潘映昆 | Catalytic electrode printing and dyeing wastewater treatment reactor |
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| CN110104739B (en) * | 2019-05-27 | 2022-02-11 | 中国华能集团清洁能源技术研究院有限公司 | Efficient electrode for treating industrial circulating cooling water and preparation method thereof |
| CN111705328B (en) * | 2020-06-30 | 2021-09-21 | 江苏锕电尔科技有限公司 | Oxygen-suppressing electrode capable of reducing oxygen content of electrolytic cell and preparation method thereof |
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