CN114715984B - 一种自洁净发光光电协同催化电极及其应用 - Google Patents
一种自洁净发光光电协同催化电极及其应用 Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46119—Cleaning the electrodes
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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- Health & Medical Sciences (AREA)
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- Electrodes For Compound Or Non-Metal Manufacture (AREA)
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Abstract
本发明公开了一种自洁净发光光电协同催化电极,当电极为阳电极时,基底一面覆盖有空穴传输层,另一面覆盖有压电层,在空穴传输层上设置有量子点层,在量子点层上设置有催化材料层;当电极为阴电极时,基底一面覆盖有电子传输层,另一面覆盖有压电层,在电子传输层上设置有量子点层,在量子点层上设置有催化材料层;该电极能有效的耦合光电催化效应,提升电极的催化反应性能,通过连接交流电源能产生原位微振动达到电极自洁净的功能,同时制备方法工艺简单,适用于各种复杂环境中的光电催化反应。
Description
技术领域
本发明专利涉及水污染处理领域,具体涉及一种自洁净发光光电协同催化电极及其应用。
背景技术
高级氧化技术中光催化以无二次污染、操作简单等特点著称,但在实际应用中存在部分困难:常规光催化分解不完全,致使有机物降解不彻底并产生多种有机芳香族的中间体;在使用环境中水介质的吸光物质的吸收下,到达催化剂表面的有效光波段减少,光催化效果大打折扣;随着使用时间增加,污水中不可溶的细小颗粒物附着在电极表面,阻碍有机污染物在电极表面的吸附,使得电极催化性能下降。
发明内容
针对现有技术不足,本发明提供了一种用于少光环境中催化性能稳定、特定条件下能够自洁净的电极。
本发明利用半导体本身的特性及外加电场及催化助剂来加速电子转移,以实现在复杂环境中光电协同催化的效果;电极组成材料包含压电特性的材料,在接入一定频率的交流电能够产生原位微振动,附着在电极表面的固体污染物从电极表面脱落实现电极自洁净的功能。
当电极为阳电极时,本发明自洁净发光光电协同催化电极包括压电层、基底、空穴传输层、量子点层、催化材料层;基底一面覆盖有空穴传输层,另一面覆盖有压电层,在空穴传输层上设置有量子点层,在量子点层上设置有催化材料层;
当电极为阴电极时,本发明自洁净发光光电协同催化电极包括压电层、基底、电子传输层、量子点层、催化材料层,基底一面覆盖有电子传输层,另一面覆盖有压电层,在电子传输层上设置有量子点层,在量子点层上设置有催化材料层。
所述电极基底为钛、钌、ITO、聚二甲基硅氧烷(PDMS)中的一种。
所述空穴传输层的材料为铜化合物、过渡金属硫化物、共轭苯系聚合物中的一种,如Cu2O、CuSCN、FeS2、PTAA、TFB。
所述电子传输层的材料为过渡金属氧化物、过渡金属酸根化合物,如二氧化钛、氧化锌、氧化钨、锡酸钡的一种。
所述量子点层的材料由Ⅲ族元素和Ⅴ族元素按等摩尔量混合制得,或Ⅱ族元素和Ⅵ族元素按等摩尔量混合制得,其中Ⅲ族元素为B、Al、Ga、In中的一种或几种,Ⅴ族元素为N、P、As、Sb、Bi中的一种或几种,Ⅱ族元素为Zn、Mg、Cd、Be中的一种或几种,Ⅵ族元素为O、S、Se、Te中的一种或几种;Ⅲ族元素和Ⅴ族元素或Ⅱ族元素和Ⅵ族元素中所有元素加权平均原子序Z≤40。
所述压电层材料由压电聚合物与压电颗粒混合构成,压电聚合物为PVDF、聚对二甲苯、液晶聚合物、聚酰胺中的一种,压电颗粒为具有反演对称性的无机材料,如BiFeO3陶瓷颗粒、NaBiS2、钛酸铋钠基陶瓷颗粒、锰酸锂、铌酸锂中的一种。
所述催化材料层由d区元素、d区元素的氧化物中的一种或几种组成;或先由d区元素、d区元素的氧化物中的一种或几种形成底层,再在底层上形成表层,且底层元素的序数比表层元素序数高;例如铁锰合金为表层,铁为底层;氧化铁氧化铜混合形成表层,氧化铜为底层。
本发明另一目的是将上述自洁净发光光电协同催化电极应用在废水处理、电化学合成、电化学检测中。
本发明的有益效果在于:
(1)相比于传统光催化材料,光电催化材料应用场景更加广泛,本发明提出在传统光催化材料上制备发光材料的电极,可在复杂环境中进行光电催化反应;
(2)在应用于污水处理时利用其输入交流电产生振动的特性抖落附着在电极上的污泥,重新暴露电极上的活性位点,延长电极的使用寿命。
具体实施方式
下面结合具体实施方式对本发明进行详细说明,但本发明保护范围不局限于所述内容;实施例中方法如无特殊说明均为常规方法。
实施例1:自洁净发光的光电协同催化电极及用于废水中有机物降解
以钛作为基底,空穴传输层的材料为CuSCN,量子点层的材料为AlNP,催化材料层为铱铁合金、压电层材料为PVDF与BiFeO3陶瓷;
阳电极制备过程如下:
1、使用砂纸抛光打磨钛片后,在硝酸、氢氟酸、水的混合液(体积比3:1:3)中浸泡20s,用去离子水超声清洗干净后保存在酒精溶液中备用;
2、步骤1中的基底置于70℃的加热板上,准备0.1mol/L的CuSCN丙烷溶液,通过氮气将上述溶液吹喷至基底一面上,循环8次,形成空穴传输层;
3、将步骤2中制备的材料移至金属有机化合物气相沉积(MOCVD)系统中,反应室内压力调至10-2Pa,温度升至970℃,控制NH3:PH3:三甲基铝气体的体积比为72:48:1,在空穴传输层上进行AlNP层的制备;
4、依次用丙酮、无水乙醇、去离子水清洗步骤3中制得的材料后,配制含有0.12mol/L的氯化铱、0.02mol/L的氯化铁、0.01mol/L硼酸的电解液,将步骤4制得的材料置于电解液中作为工作极,铂电极和饱和甘汞电极分别作为对电极与参比电极,在-0.7V电位下沉积25min,步骤3中的AlNP层表面形成铱铁合金催化层;
5、将 Fe2O3、Bi2O3、TiO2 和 BaCO3按照1:1:0.2:0.1的质量比混合干燥后球磨,筛分后放入坩埚在740℃下保温4h,冷却后再次球磨制得陶瓷颗粒;将PVDF、PVP、NMP混合搅拌2h制得基膜液(10:1:80),将前述制备的陶瓷颗粒与ZnO NPs混合后,按5%的添加量加入膜基液中继续搅拌6h;上述浆液铸成膜后在蒸馏水中浸泡12h后进行极化处理,极化电压24kV、时间15min;成膜后粘附在步骤4中基底的另一面,制得阳极。
采用单室电解池,双电极体系,上述方法制得的电极为阳电极(导线与基底连接),钛板为阴极;设计正交实验选出最佳电流密度为15.2mA/cm2,以1000mg/L浓度的焦化废水为降解对象,30min内去除率82%;使用超过5h后外接90Hz的电源清洗20min后用作降解,循环使用8次去除率基本持平。
实施例2:本自洁净发光光电协同催化电极及用于CO2电化学还原
选用ITO作为基底、电子传输层材料为TiO2、量子点层材料为ZnS、催化材料层为银-氧化钴、压电材料为PVDF与钛酸铋钠基陶瓷;
阴电极过程如下:
1、依次使用丙酮、无水乙醇、去离子水超声清洗ITO衬底各5min;
2、TiO2 NPs分散在在正辛烷中后旋涂至步骤1中的基底一面上,在60℃下干燥1h;
3、将4mmol Zn(Ac)2、17.6 mmol油酸和 20 mL十八烯放入圆瓶中加热至150℃,在氮气保护下进一步加热至310℃以形成Zn(OA) 2 ,在此温度下,将4mmol S粉末溶解在3mL的TOP(三(2-乙基己基)磷酸酯)溶液中后,快速注入反应烧瓶中, 注入后,将反应瓶的温度设置为300℃以促进量子点的生长,然后将其冷却至室温以停止生长;加入20mL 氯仿和过量丙酮纯化量子点,后分散于己烷中;取上述量子点溶液旋涂于步骤2中的TiO2层上,40℃下干燥30min;
4、配制含0.1mol/L硝酸银、0.02mol/L硝酸钴、0.01mol/L硼酸的电解液,将步骤4制得的材料置于电解液中作为工作极,铂电极和饱和甘汞电极分别作为对电极与参比电极,在-0.5V电位下电沉积30min,清洗电极后置于空气中在200℃条件下氧化2h,在步骤3中的量子点层表形成银-氧化钴催化材料层;
5、将Bi2O3、Na2CO3、K2CO3、MgCO3、TiO2以5:4:1:4:8的比例混合干燥球磨后,筛分后放入坩埚在840℃下保温4h,冷却后再次球磨制得陶瓷颗粒;将PVDF、PVP、NMP混合搅拌2h制得基膜液(10:1:80),将前述制备的陶瓷颗粒与SiO2 NPs混合后,按5%的量加入膜基液中继续搅拌6h;上述浆液铸成膜后在蒸馏水中浸泡12h后进行极化处理,极化电压24kV、时间15min;成膜后粘附在步骤4中基底的另一面,制得阴极。
采用三电极体系,上述方法制得的电极为工作电极(导线与基底连接),饱和甘汞电极为参比电极,银丝作为对电极,以离子液体[HMIm]BF4作为电解质,通入CO2使其吸收量达到饱和;通过CV法得出还原电位后,采用恒电位计时法在还原峰电位位置进行CO2还原,1小时反应结束,期间可得到CO、CH4等气体产物;电极使用超过10h后外接80Hz的电源清洗20min后用作降解,循环使用8次去产率基本持平。
实施例3:本自洁净发光光电协同催化电极及用于废气NOX、SO2检测
以钛作为基底,空穴传输材料为TFB(1,2,4,5-四(三氟甲基)苯)、量子点材料为ZnCdS、催化层材料为铅铜合金、压电材料为聚酰胺与铌酸锂(LiNbO3)晶体。
阳电极制备过程如下:
1、使用砂纸抛光打磨钛片后,在硝酸、氢氟酸、水的混合液(体积比3:1:3)8中浸泡20s,用去离子水超声清洗干净后保存在酒精溶液中备用;
2、在基底上旋涂TFB,在60℃下干燥1h;
3、将 1mmol CdO、10mmol Zn(Ac)2和7mL油酸置于100mL圆瓶中,将混合物加热至150℃,加入15mL 十八烯,后在氮气保护下进一步加热至310℃,形成澄清的Cd(OA)2和Zn(OA)2溶液;将溶解在3mL 1-ODE中的2mmol S粉末快速注入反应烧瓶中,反应8min后将8mmol S粉末溶解在6ml 磷酸三丁酯注入反应器,反应完成后加入20mL 氯仿和过量丙酮纯化量子点,后分散于己烷中;取上述量子点溶液旋涂于步骤2中的TFB层上,40℃下干燥30min;
4、配制含有0.1mol/L的硫酸铅、0.01mol/L的硫酸铜、0.01mol/L硼酸的电解液,将步骤4制得的材料置于电解液中作为工作极,铂电极和饱和甘汞电极分别作为对电极与参比电极,在-0.3V电位下沉积30min,在量子点层表层形成铅铜合金层催化层;
5、将Nb2O5、Li2CO3按质量1:1研磨后放入坩埚,放入马弗炉温度设置1020℃,持续恒温11h。取出后研磨再放入马弗炉内设置温度为1120℃烧结10h获得铌酸锂晶体颗粒;将聚酰胺颗粒加热至200℃融化,加入前述制备的晶体颗粒与ZnO NPs混合后,按10%的量加入膜基液中继续搅拌1h;上述浆液铸成膜后在蒸馏水中浸泡12h后进行极化处理,极化电压24kV、时间15min;成膜后粘附在步骤4中基底的另一面,制得阳极;
采用三电极体系,制备的阳电极为工作电极(导线与基底连接),银丝为参比电极,铂网作为对电极,以0.2mol/L NaOH及0.1mol/L氨水配置成吸收液并作为电解质,通入被测气体后开始测量,采用线性伏安法设定采样间隔0.1s,扫描范围-0.3-1V,NO2与SO2对应的峰位置为0.7V与0.2V,其峰高度(电流大小)与通入气体浓度成正比;电极使用超过8h后外接70Hz的电源清洗30min后用作降解,循环使用11次去产率基本持平。
Claims (3)
1.一种自洁净发光光电协同催化电极,其特征在于:当电极为阳电极时,基底一面覆盖有空穴传输层,另一面覆盖有压电层,在空穴传输层上设置有量子点层,在量子点层上设置有催化材料层;
当电极为阴电极时,基底一面覆盖有电子传输层,另一面覆盖有压电层,在电子传输层上设置有量子点层,在量子点层上设置有催化材料层;
所述基底为钛、钌、ITO、聚二甲基硅氧烷中的一种;
空穴传输层的材料为铜化合物、过渡金属硫化物、共轭苯系聚合物中的一种;
电子传输层的材料为过渡金属氧化物、过渡金属酸根化合物中的一种;
量子点层的材料由Ⅲ族元素和Ⅴ族元素按等摩尔量混合制得,或Ⅱ族元素和Ⅵ族元素按等摩尔量混合制得;
催化材料层由d区元素、d区元素的氧化物中的一种或几种组成;或先由d区元素、d区元素的氧化物中的一种或几种形成底层,再在底层上形成表层,且底层元素的序数比表层元素序数高;
所述Ⅲ族元素为B、Al、Ga、In中的一种或几种,Ⅴ族元素为N、P、As、Sb、Bi中的一种或几种,Ⅱ族元素为Zn、Mg、Cd、Be中的一种或几种,Ⅵ族元素为O、S、Se、Te中的一种或几种;
Ⅲ族元素和Ⅴ族元素中所有元素加权平均原子序数Z≤40;
Ⅱ族元素和Ⅵ族元素中所有元素加权平均原子序数Z≤40。
2.根据权利要求1所述的自洁净发光光电协同催化电极,其特征在于:压电层材料由压电聚合物与压电颗粒混合组成。
3.权利要求1-2中任一项所述的自洁净发光光电协同催化电极在废水处理、电化学合成、电化学检测中的应用。
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CN113526607A (zh) * | 2020-04-16 | 2021-10-22 | 中国环境科学研究院 | 基于碳点的有机物降解同步重金属还原光催化电极及应用 |
CN113264573A (zh) * | 2021-04-16 | 2021-08-17 | 西安理工大学 | 一种双极性电极及其制备方法、及废水处理系统 |
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CN113896275A (zh) * | 2021-10-18 | 2022-01-07 | 广东工业大学 | 一种光电催化反应器 |
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