CN108744993B - 一种动态电化学沉积制备电催化炭膜的方法 - Google Patents
一种动态电化学沉积制备电催化炭膜的方法 Download PDFInfo
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- CN108744993B CN108744993B CN201810803015.XA CN201810803015A CN108744993B CN 108744993 B CN108744993 B CN 108744993B CN 201810803015 A CN201810803015 A CN 201810803015A CN 108744993 B CN108744993 B CN 108744993B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 167
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 166
- 239000012528 membrane Substances 0.000 title claims abstract description 121
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 230000008021 deposition Effects 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 8
- 239000012466 permeate Substances 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 239000008139 complexing agent Substances 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 5
- 235000015165 citric acid Nutrition 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000011133 lead Substances 0.000 claims description 3
- 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 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 3
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 3
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 3
- 229940116357 potassium thiocyanate Drugs 0.000 claims description 3
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011135 tin Substances 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 238000011161 development Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- 230000002572 peristaltic effect Effects 0.000 description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 229910017604 nitric acid Inorganic materials 0.000 description 8
- 229910052697 platinum Inorganic materials 0.000 description 7
- 229910001220 stainless steel Inorganic materials 0.000 description 7
- 239000010935 stainless steel Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 229940075397 calomel Drugs 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229940107698 malachite green Drugs 0.000 description 2
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 2
- MINVSWONZWKMDC-UHFFFAOYSA-L mercuriooxysulfonyloxymercury Chemical compound [Hg+].[Hg+].[O-]S([O-])(=O)=O MINVSWONZWKMDC-UHFFFAOYSA-L 0.000 description 2
- 229910000474 mercury oxide Inorganic materials 0.000 description 2
- 229910000370 mercury sulfate Inorganic materials 0.000 description 2
- 229910000371 mercury(I) sulfate Inorganic materials 0.000 description 2
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- GPQUEUOSGZMUQE-UHFFFAOYSA-N [O-2].[Hg+].[Hg+] Chemical compound [O-2].[Hg+].[Hg+] GPQUEUOSGZMUQE-UHFFFAOYSA-N 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
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229940101209 mercuric oxide Drugs 0.000 description 1
- RPZHFKHTXCZXQV-UHFFFAOYSA-N mercury(I) oxide Inorganic materials O1[Hg][Hg]1 RPZHFKHTXCZXQV-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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Abstract
本发明涉及一种动态电化学沉积制备电催化炭膜的方法,属于膜分离技术领域。一种动态电化学沉积制备电催化炭膜的方法,在电化学沉积体系中,以炭膜为电沉积电极,以待沉积的金属氧化物相应的金属盐溶液为电沉积液,在电沉积过程中,使电沉积液透过炭膜并使生成的金属氧化物沉积在炭膜表面和其内部的孔道内。通过动态电化学沉积技术可在炭膜表面和孔道内沉积催化剂,制备工艺简单,成本低,有效地提高了催化剂的利用效率和炭膜的电化学性能。电催化炭膜的制备与开发可以充分发挥膜分离与电催化的耦合优势,增强对难降解废水的处理能力,加速该技术的产业化进程。
Description
技术领域
本发明涉及一种动态电化学沉积制备电催化炭膜的方法,属于膜分离技术领域。
背景技术
炭膜是一种新型的多孔无机膜,它把炭材料优异的结构特性与膜材料的优势有机融合为一体,在分离领域展现出极大的应用潜力。通常,炭膜是由含碳的前驱体材料在惰性气体或者真空保护条件下,经过高温热解制备而成。近年来,本课题组开发了管状和平板状炭膜产品的制备工艺(中国专利ZL03134197.7;中国专利ZL03134196.9;中国专利ZL201110456881.4;中国专利ZL201310227547.0),并利用炭膜特有的导电性将其作为电极与电场耦合提高其对废水的处理能力(中国专利ZL201310222558.X)。然而,在应用过程中,炭膜和其他膜电极材料一样,都面临着由于膜电极材料自身的电化学降解能力有限,对高浓度有机废水的处理能力和效果不理想的问题。
为了进一步提高炭膜的电化学性能,在炭膜电极上担载催化剂材料,降低反应活化能,提升电化学降解的反应效率是解决这一问题有效方法。然而,到目前为止,国内外更多的研究工作主要集中在将催化剂担载到电极上,而将催化剂担载到膜上制备电催化膜方面的报道还很少。Zhang等通过浸渍-氢气还原法将铂做催化剂担载到经炭沉积改性的陶瓷膜上制备电催化膜(Zhang et al.,Advanced Materials Research.2010,156-157:30-35)。Yang等通过热分解法将IrO2附着在Al2O3陶瓷膜上处理含油废水,并展现出较强的抗污染能力(Yang et al.,Separation and Purification Technology.2015,156:931-941)。本课题组与天津工业大学的李建新教授合作,采用溶胶-凝胶涂覆方式把TiO2催化剂担载在炭膜表面上,率先在国际上成功制备出具有自清结功能的电催化导电炭膜材料(Yang etal.,Angewandte Chemie International Edition.2011,50:2148-2150;中国专利ZLCN200910069013.3)。李建新等利用水热合成法将一维金属氧化物负载在微孔导电钛膜上制备电催化膜(中国专利申请号CN201710259618.3)。
发明内容
本发明的目的是提供一种成本低、工艺简单、高污染物降解性能的电催化炭膜的制备方法,以解决目前炭膜在废水处理过程中电化学降解能力不足的问题。
一种动态电化学沉积制备电催化炭膜的方法,在电化学沉积体系中,以炭膜为电沉积电极,以待沉积的金属氧化物相应的金属盐溶液为电沉积液,在电沉积过程中,使电沉积液透过炭膜并使生成的金属氧化物沉积在炭膜表面和其内部的孔道内。
本发明所述“电化学沉积体系”为现有技术公开的电化学沉积体系,体系包括电化学沉积反应所必需的电沉积池、电沉积液、电极、电源等。本发明所述电化学沉积体系可为双电极体系或三电极体系。
对于双电极体系,包括阴极和阳极。所述炭膜为阳极;所述阴极,其材料选用不锈钢、钛、铂等,其形态可为金属片或网。
对于三电极体系,包括工作电极、对电极和参比电极。所述炭膜为工作电极;所述对电极为铂对电极、金对电极、镍对电极或碳对电极;所述参比电极为甘汞电极、银/氯化银电极、汞/硫酸亚汞电极、汞/氧化汞电极。
本发明所述炭膜为现有技术公开的炭膜,可商业购得或根据现有技术公开的方法制得。进一步地,所述炭膜为管状炭膜或板状炭膜。更进一步地,所述管状炭膜为单通道或多通道管状炭膜,所述板状炭膜为非中空板状炭膜或中空板状炭膜。
本发明所述利用电沉积方法制备电催化炭膜的过程中,可采用现有技术公开的手段使电沉积液透过炭膜并使生成的金属氧化物沉积在炭膜表面和其内部的孔道内。如,可利用流体输送装置使电沉积液发生流动并透过炭膜,所述流体输送装置可为现有技术公开的泵等,如蠕动泵。
本发明所述方法,优选利用流体输送装置使电沉积液从炭膜的一侧流动至另外一侧。利用流体输送装置使电沉积液发生流动,使电沉积液从炭膜的一侧流动至另外一侧,可使电沉积液在电沉积过程中流经炭膜内部的孔道,并使催化剂沉积在炭膜孔道的内部和表面。
本发明所述方法,当所述炭膜为管状炭膜时,利用泵使电沉积液从管状炭膜的外部流经炭膜,进入管状炭膜的通道内。
本发明所述方法,当所述炭膜为中空板状炭膜时,利用泵使电沉积液从中空板状炭膜的外部流经炭膜,进入中空板状炭膜的中空部。
本发明所述方法,当所述炭膜为非中空板状炭膜时,利用泵使电沉积液从非中空板状炭膜的一侧流动至另一侧。
本发明所述动态电化学沉积制备电催化炭膜的方法,优选所述金属盐溶液是由金属盐、络合剂、碱性物与水配置而成的水溶液,所述金属盐的质量分数为0.1~15%,所述络合剂的质量分数为0.1~15%,所述碱性物的质量分数为0.5~15%,其中,所述金属盐为锰、铁、钴、镍、铜、锌、银、锡、或铅的硝酸盐、硫酸盐、氯化物;所述络合剂为EDTA、柠檬酸、酒石酸、草酸、磺基水杨酸、甘氨酸、硫氰酸铵、硫氰酸钾或酒石酸钾钠;所述碱性物为氢氧化钠、氢氧化钾或氨水中的一种。
本发明所述电化学沉积过程中,所述电沉积液的流量可根据实际工况确定,其与待沉积的炭膜尺寸及数量有关,炭膜尺寸越大,数量越多,则电沉积液的流量越大。
优选地,所述电化学沉积过程中,电沉积液流量为0.001~10L/min。
本发明所述动态电化学沉积制备电催化炭膜的方法,进一步优选:
对于双电极体系,所述电沉积液流量为0.001~1L/min,沉积电压为0.1~10.0V之间,沉积时间为1~120min,沉积温度为5~90℃。
对于三电极体系,所述电沉积液流量为0.001~1L/min,沉积电压为-10.0V~10.0V之间,沉积时间为1~120min,沉积温度为5~90℃。
本发明所述动态电化学沉积制备电催化炭膜的方法,进一步优选所述方法包括后处理的步骤,具体为:将电沉积后所得电催化炭膜用水清洗,后于干燥箱中30~100℃干燥1~8h。
本发明所述动态电化学沉积制备电催化炭膜的方法,进一步优选所述方法包括前处理的步骤,具体为:将炭膜放入强氧化性酸溶液(如硝酸或硫酸)中进行表面改性处理,用水清洗至中性后,放置于30~100℃烘箱中干燥1~8h。
本发明所述动态电化学沉积制备电催化炭膜的方法一个优选的技术方案为:
一种动态电化学沉积制备电催化炭膜的方法,包括下述工艺步骤:
(1)前处理:将炭膜放入强氧化性酸溶液(如硝酸或硫酸)中进行表面改性处理,用水清洗至中性后,放置于30~100℃烘箱中干燥1~8h;
(2)配制电化学沉积液:所述金属盐溶液是由金属盐、络合剂、碱性物与水配置而成的水溶液,所述金属盐的质量分数为0.1~15%,所述络合剂的质量分数为0.1~15%,所述碱性物的质量分数为0.5~15%,其中,所述金属盐为锰、铁、钴、镍、铜、锌、银、锡、或铅的硝酸盐、硫酸盐、氯化物;所述络合剂为EDTA、柠檬酸、酒石酸、草酸、磺基水杨酸、甘氨酸、硫氰酸铵、硫氰酸钾或酒石酸钾钠;所述碱性物为氢氧化钠、氢氧化钾或氨水中的一种。
(3)动态电化学沉积:动态电化学沉积可以采用双电极体系或三电极体系,
I.双电极体系电化学沉积:将炭膜设置为阳极,与阴极材料同时浸入电化学沉积液中,其中使炭膜与蠕动泵相连,在电化学沉积过程中利用蠕动泵抽取电沉积液使其透过炭膜,使得沉积过程炭膜表面和孔道内同时发生,阴极材料为钛、不锈钢、铂,其形态为金属片或网,电沉积温度为5~90℃,电沉积电压控制在0.1~10.0V,电沉积液流量控制在0.001~1L/min,电沉积时间为1~120min。
II.三电极体系电化学沉积:将炭膜设置为工作电极,与对电极和参比电极构成三电极体系,对电极为铂对电极、金对电极、镍对电极或碳对电极,参比电极为甘汞电极、银/氯化银电极、汞/硫酸亚汞电极、汞/氧化汞电极;将工作电极,与对电极和参比电极同时浸入电化学沉积液中,使炭膜与蠕动泵相连,在电化学沉积过程中利用蠕动泵抽取电沉积液使其透过炭膜,使得沉积过程炭膜表面和孔道内同时发生,电沉积温度为5~90℃,沉积电压控制在-10.0~10.0V,电沉积液流量控制在0.001~1L/min,电沉积时间为1~120min。
(4)用水将电沉积后的炭膜清洗至中性,放入置于30~100℃烘箱中干燥1~8h后,便得到电催化炭膜。
本发明的有益效果为:通过动态电化学沉积技术可在炭膜表面和孔道内沉积催化剂,制备工艺简单,成本低,有效地提高了催化剂的利用效率和炭膜的电化学性能。电催化炭膜的制备与开发可以充分发挥膜分离与电催化的耦合优势,增强对难降解废水的处理能力,加速该技术的产业化进程。
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。
实施例1
将单通道管状炭膜(平均孔径:0.4μm,孔隙率:40%)放入硝酸水溶液(硝酸与水体积比为1:2.5)中浸泡2h,用去水清洗至中性后置于60℃烘箱中干燥2h。将硫酸锌、柠檬酸和氢氧化钠分别加入到水中配置成电沉积液,其中硫酸锌、柠檬酸、氢氧化钠的浓度分别为1.0%,0.5%,1.0%(质量百分比)。将炭膜设置为阳极,不锈钢片设置为阴极,同时浸入电沉积液中构成双电极电沉积体系。将管状炭膜以管状中心轴垂直地面的方向置于电沉积液中,将管状炭膜的底端密封,将另一端与蠕动泵的软管连通,利用蠕动泵产生的负压将电沉积液由管状炭膜的外部吸入管状炭膜的通道内进行动态电化学沉积,电沉积温度为25℃,电沉积电压控制在3.0V。电沉积液流量控制在0.05L/min,电沉积时间为20min。然后用水将炭膜清洗至中性,放入置于60℃烘箱中干燥2h后,便得到电催化炭膜。
以该电催化膜作为阳极,钛板作为阴极,在2.0V电压下处理罗丹明B废水4h效果如表1所示,电催化炭膜对高浓度罗丹明B废水仍展现出较高的去除率。
实施例2
将七通道管状炭膜(平均孔径:0.6μm,孔隙率:42%)放入硝酸水溶液(硝酸与水体积比为1:2)中浸泡1h,用去水清洗至中性后置于80℃烘箱中干燥1h。将四氯化锡、硫氰酸铵和氢氧化钾分别加入到水中配置成电沉积液,其中四氯化锡、硫氰酸铵和氢氧化钾的浓度分别为2.0%,1.5%,4.0%(质量百分比)。将炭膜设置为工作电极,铂片电极设置为对电极,甘汞电极设置为参比电极,同时浸入电沉积液中构成三电极电沉积体系,将管状炭膜以管状中心轴垂直地面的方向置于电沉积液中,将管状炭膜的底端密封,将各个通道均连通蠕动泵的软管,利用蠕动泵产生的负压将电沉积液由管状炭膜的外部吸入管状炭膜的通道内进行动态电化学沉积,电沉积温度为50℃,电沉积电压控制在5.0V。电沉积液流量控制在0.02L/min,电沉积时间为10min。然后用水将炭膜清洗至中性,放入置于80℃烘箱中干燥1h后,便得到电催化炭膜。
以该电催化膜作为阳极,不锈钢板作为阴极,在2.5V电压下处理孔雀石绿废水5h效果如表2所示,电催化炭膜对高浓度孔雀石绿废水仍展现出较高的去除率。
实施例3
将非中空板状炭膜(平均孔径:0.8μm,孔隙率:41%)放入硝酸水溶液(硝酸与水体积比为1:4)中浸泡3h,用去水清洗至中性后置于50℃烘箱中干燥2h。将氯化钴、磺基水杨酸和氢氧化钠分别加入到水中配置成电沉积液,其中氯化钴、磺基水杨酸和氢氧化钠的浓度分别为3.0%,1.5%,5.0%(质量百分比)。将炭膜设置为阳极,不锈钢网设置为阴极,同时浸入电沉积液中构成双电极电沉积体系,利用蠕动泵在炭膜一侧产生的负压使电沉积液由炭膜的另一侧渗透至炭膜的另一侧,进行动态电化学沉积,电沉积温度为20℃,电沉积电压控制在6.0V。电沉积液流量控制在0.1L/min,电沉积时间为5min。然后水将炭膜清洗至中性,放入置于50℃烘箱中干燥2h后,便得到电催化炭膜。
以该电催化膜作为阳极,石墨板作为阴极,在3.0V电压下处理甲基橙废水3h效果如表3所示,电催化炭膜对高浓度甲基橙废水仍展现出较高的去除率。
实施例4
将中空平板炭膜(内部三通道,平均孔径:1.0μm,孔隙率:38%)放入硫酸水溶液(硫酸与水体积比为1:1)中浸泡1h,用去水清洗至中性后置于40℃烘箱中干燥3h。将硝酸镍、EDTA和氨水分别加入到水中配置成电沉积液,其中硝酸镍、EDTA和氨水的浓度分别为0.5%,2.0%,6.0%(质量百分比)。将炭膜设置为工作电极,与金对电极和银/氯化银参比电极构成三电极体系。将中空平板炭膜以通道中心轴垂直地面的方向置于电沉积液中,将中空平板炭膜的底端密封,将各个通道均连通蠕动泵的软管,利用蠕动泵产生的负压将电沉积液由中空平板炭膜的外部吸入中空平板炭膜的通道内进行动态电化学沉积,电沉积液流量控制在0.1L/min,电沉积电压控制在-2.0~2.0V。电沉积时间为5min。电沉积温度设为50℃,电沉积时间为5min。电沉积后,用水将炭膜清洗至中性,放入置于40℃烘箱中干燥3h后,便得到电催化炭膜。
以该电催化膜作为阳极,铂片作为阴极,在3.5V电压下处理苯酚废水2h效果如表4所示,电催化炭膜对高浓度苯酚废水仍展现出较高的去除率。
Claims (5)
1.一种动态电化学沉积制备电催化炭膜的方法,其特征在于:在电化学沉积体系中,以炭膜为电沉积电极,以待沉积的金属氧化物相应的金属盐溶液为电沉积液,在电沉积过程中,利用泵抽取电沉积液使电沉积液透过炭膜并使生成的金属氧化物沉积在炭膜表面和其内部的孔道内,
所述方法包括前处理的步骤,具体为:将炭膜放入强氧化性酸溶液中进行表面改性处理,用水清洗至中性后,放置于30~100℃烘箱中干燥1~8h;
所述金属盐溶液是由金属盐、络合剂、碱性物与水配置而成的水溶液,所述金属盐的质量分数为0.1~15 %,所述络合剂的质量分数为0.1~15 %,所述碱性物的质量分数为0.5~15%,其中,所述金属盐为锰、铁、钴、镍、铜、锌、银、锡、或铅的硝酸盐、硫酸盐、氯化物;所述络合剂为EDTA、柠檬酸、酒石酸、草酸、磺基水杨酸、甘氨酸、硫氰酸铵、硫氰酸钾或酒石酸钾钠;所述碱性物为氢氧化钠、氢氧化钾或氨水中的一种;
所述电化学沉积体系为双电极体系或三电极体系,对于双电极体系,所述炭膜为阳极;对于三电极体系,所述炭膜为工作电极;
对于双电极体系,所述电沉积液流量为0.001~1 L/min,沉积电压为0.1~10.0 V之间,沉积时间为1~120 min,沉积温度为5~90℃;
对于三电极体系,所述电沉积液流量为0.001~1 L/min,沉积电压为-10.0V~10.0V之间,沉积时间为1~120 min,沉积温度为5~90℃。
2.根据权利要求1所述的方法,其特征在于:所述炭膜为管状炭膜或板状炭膜。
3.根据权利要求2所述的方法,其特征在于:所述管状炭膜为单通道或多通道管状炭膜,所述板状炭膜为非中空板状炭膜或中空板状炭膜。
4.根据权利要求3所述的方法,其特征在于:利用泵使电沉积液从管状炭膜的外部流经炭膜,进入管状炭膜的通道内;或利用泵使电沉积液从中空板状炭膜的外部流经炭膜,进入中空板状炭膜的中空部。
5.根据权利要求3所述的方法,其特征在于:利用泵使电沉积液从非中空板状炭膜的一侧流动至另一侧。
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