CN114105260A - 一种防腐型Ti基阳极电极材料及其制备方法与应用 - Google Patents
一种防腐型Ti基阳极电极材料及其制备方法与应用 Download PDFInfo
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- CN114105260A CN114105260A CN202111621188.8A CN202111621188A CN114105260A CN 114105260 A CN114105260 A CN 114105260A CN 202111621188 A CN202111621188 A CN 202111621188A CN 114105260 A CN114105260 A CN 114105260A
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
- C02F1/4678—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction of metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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- C23F13/005—Anodic protection
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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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- Carbon And Carbon Compounds (AREA)
Abstract
本发明提供一种防腐型Ti基阳极电极材料以及其在电化学还原水中硝酸盐方面的应用。本发明通过原位聚合法制备氧化石墨烯/聚苯胺复合物,然后将制备的氧化石墨烯/聚苯胺复合物涂覆到Ti电极片上,烘干;最后,采用旋涂的方式在氧化石墨烯/聚苯胺/Ti极片表面涂覆BTA层,最终形成BTA改性氧化石墨烯/聚苯胺/Ti极片。本发明采用BTA改性氧化石墨烯‑聚苯胺复合材料,既具备较大的比表面积、耐高温、耐腐蚀和高强度,又具有良好的导电性能,可应用于电化学催化、防腐材料、导热材料、锂离子电池、超级电容器和军用航天材料等领域。
Description
(一)技术领域
本发明属于工业废水处理、电极防腐领域,特别涉及一种防腐型Ti基阳极电极材料及其制备方法和其于还原硝态氮中的应用。
(二)背景技术
不锈钢电镀废水中的硝酸盐含量较高,容易对人体造成严重危害。硝酸盐本身对人体并没有直接危害,但通过硝酸还原菌作用可以转变成亚硝酸盐,亚硝酸盐的毒性比硝酸盐毒性大11倍,亚硝酸盐能把血液中血红蛋白的二价铁转化成三价铁,生成变性红血球使其不再具有携氧能力,与血液中运输氧气的血红蛋白形成高铁血红蛋白,严重影响人体的血液输氧功能,甚至使人呼吸衰竭。除此之外,硝酸盐和亚硝酸盐还能和各种含氮化合物结合形成“三致”物质亚硝基氨和亚硝基酰胺等,它们能诱发各种肿瘤疾病,如脑、呼吸道、甲状腺、肠道、皮肤和神经骨骼***等,不仅如此,硝酸盐也会让鱼类等水生生物产生病变,影响水生生态***所以对于硝酸盐去除必须引起重视。
对于日益严重的硝酸盐污染问题,国内外学者提出了一系列针对硝酸盐污染的治理方法。目前,硝酸盐的常规处理技术主要包括物理、生物和化学处理技术。其中物理处理技术对地下水中的硝酸盐处理效率高,实验操作简单易控,但其处理成本较高,硝酸盐仅是进行了转移或浓缩并未完全去除,很可能引起二次污染。生物处理技术去除效率高、稳定性好、处理成本相对较低,但反应器的体积庞大,处理周期缓慢,很容易受到周围环境的影响,因而该方法在实际应用中有很多限制。化学法处理地下水中的硝酸盐,具有材料无毒易得、反应快速等优点,但是,该方法并不能将硝酸盐完全转化成无毒无害的氮气,还会产生金属离子等污染物对环境造成二次污染,应用前景受到限制。
电化处理技术去除硝酸盐是以金属或非金属材料作为阴极,通过施加外加电流依靠反应过程中电极表面的电解反应将硝酸盐还原为氮气、氨等产物的过程。相较于物理、生物和化学处理技术,电化学技术具有处理效率高、操作简便、能耗低、环境友好等优势受到普遍关注。专家学者们对于电化学去除硝酸盐的机理以及各种因素的影响作用,进行了大量的科学研究。在硝酸盐还原体系中,常向溶液中加入NaCl作为电解质,提高电流密度加强还原能力,但是在含有Cl-的介质中金属电极腐蚀更为严重。电化学还原硝态氮中的关键问题在于制备廉价抗腐蚀的金属阳极。
(三)发明内容
为了克服上述现有技术存在的问题,本发明提供一种防腐型Ti基阳极电极材料及其制备方法和其在还原硝态氮中的应用,所述防腐型Ti基阳极电极材料使用Ti为基底,在Ti电极表面涂覆新型防腐材料,在一个电化学反应槽内防止阳极腐蚀,有效地去除硝酸盐。
为实现上述目的,本发明采用的技术方案如下:
一种防腐型Ti基阳极电极材料的制备用于还原硝态氮,阳极选用廉价的Ti电极,阳极涂覆新型防腐材料,阴极选用铜电极,在一个电化学反应槽内有效地去除硝酸盐,涉及思路为具体包括如下步骤:
制备防腐涂料,将苯胺单体加到氧化石墨烯溶液中,通过溶液聚合法制备聚苯胺-氧化石墨烯复合材料,将制备的防腐涂料涂覆在Ti电极片上,之后再采用旋涂方法引入典型有机缓蚀剂苯并***(BTA)。
第一方面,本发明提供一种防腐型Ti基阳极电极材料,所述防腐型Ti基阳极电极材料按照如下方法制备:
(1)将氧化石墨烯均匀分散于溶剂A中,得到氧化石墨烯分散液;加入苯胺、0.1-2mol/L(优选1.5mol/L)酸的水溶液,搅拌下加入自由基引发剂,20~60℃(优选25℃)下反应2~12h进行原位聚合,所得反应液经后处理,得到聚苯胺-氧化石墨烯复合材料;
所述溶剂A为水、乙醇、乙二醇、异丙醇、正丁醇、N,N-二甲基甲酰胺、丙酮、甲苯中的一种或两种以上的混合液(优选为水或乙醇);所述酸的水溶液中的酸为无机酸、有机酸中一种或两种的混合物;所述氧化石墨烯、苯胺与自由基引发剂的质量比为1:5~40:5~20(优选1:10:7.5);所述苯胺与酸的水溶液的质量比为1:1~5(优选1:2);
(2)将步骤(1)所述的聚苯胺-氧化石墨烯复合材料、导电剂、粘结剂混合研磨均匀,加入溶剂B调配成浆料,所述浆料涂覆到Ti极片上后,干燥(50~120℃干燥6~18h,优选80℃真空干燥8h),得到电极极片;所述聚苯胺-氧化石墨烯复合材料、导电剂与粘结剂的质量比为80~95:12:3~10(优选84:12:6);所述导电剂为乙炔黑、碳纳米管、碳纳米线、炭黑KS-6、炭黑SP中的一种或两种以上的混合物;所述粘结剂为聚偏氟乙烯(PVDF)或聚四氟乙烯(PTFE);
(3)将0.1~1mol/L(优选0.2mol/L)苯并***的异丙醇溶液旋涂在步骤(2)所述的电极极片表面,干燥,即得所述防腐型Ti基阳极电极材料。
进一步,步骤(1)中所述溶剂A的体积以所述氧化石墨烯的质量计为0.5~3mL/mg(优选1mL/mg)。
进一步,步骤(1)中所述无机酸为氯化氢、硫酸、磷酸、硝酸中的一种或两种的混合物(优选氯化氢);所述有机酸为乙酸、酒石酸、柠檬酸、草酸、氨基磺酸中的一种或两种的混合物。
优选地,步骤(1)中所述自由基引发剂为过硫酸钠、过硫酸钾、过硫酸铵、偶氮二异丁腈、过氧化苯甲酰、过氧化苯甲酸叔丁酯、叔丁基过氧化氢中一种或两种以上的混合物。
进一步,步骤(1)中所述后处理为:所述反应液离心,取沉淀用纯水离心洗涤,在30~80℃(优选60℃)下真空干燥,得到所述聚苯胺-氧化石墨烯复合材料。
进一步,步骤(2)中所述溶剂B为水、乙醇、甲醇、正丁醇、异丙醇中的一种或两种以上的混合液。
进一步,步骤(2)中所述溶剂B的体积以所述导电剂的质量计为20~60mL/g(优选30mL/g)。
进一步,步骤(3)中所述干燥温度为50~80℃,真空干燥时间为1~6h。
更进一步,步骤(3)中所述旋涂的速度为2000~5000rpm,旋涂的时间为20~60s。
本发明中使用的氧化石墨烯通过改进的Hummers方法制备:
在冰浴条件(0~5℃)下将NaNO3和天然鳞片石墨加入到98%浓硫酸溶液中并搅拌均匀,加入高锰酸钾,继续在冰浴条件下搅拌2h,将所得混合物转移至35℃的油浴中反应1~2h,加入去离子水,将温度升至80~100℃反应30min,待所得混合溶液冷却至室温后,加入30wt%双氧水去除残留的高锰酸钾,离心,所得沉淀依次用稀盐酸、去离子水离心洗涤,30~60℃下真空干燥,得到所述氧化石墨烯;所述NaNO3、天然鳞片石墨与高锰酸钾的质量比为1:1:4;所述浓硫酸溶液的体积以所述天然鳞片石墨的质量计为20~50ml/g;所述去离子水与浓硫酸的体积比为1~1.5:1;所述双氧水与浓硫酸的体积比为0.05~0.1:1。
第二方面,本发明还提供一种上述防腐型Ti基阳极电极材料在还原硝态氮中的应用。尤其是在还原含氯废水中的硝态氮中的应用。
含氯废水会对普通电极造成严重腐蚀,而本发明的电极具有优异的抗腐蚀性能,且在防腐前体下进一步实现对硝酸根降解效果的提高。
具体地,所述应用为:以所述防腐型Ti基阳极电极材料为阳极,以铜电极为阴极,以含氯离子和硝酸根的废水为电解液,恒定电压下进行电解还原。
所述废水中氯离子的浓度为5~20g/L,硝酸根中氮的浓度为1.5~2g/L。
优选地,所述氯离子以氯化钠的形式加入。
在本发明中,所述废水池和所述电解槽之间的连接采用回流式,所述废水由蠕动泵提升,由所述电解槽底部流入,电解处理过的废水由电解槽上部流出,回流至所述出水收集装置中。
电化学处理酸洗废水主要包括两个催化反应,1)利用电解槽阳极区生成强氧化性物质(次氯酸,羟基自由基等),与污水中的氨氮(NH4 +,NH3·H2O)反应生成N2,从而达到污水脱氮的目的。2)利用电化学反应器阴极,将污水中的硝酸盐、亚硝酸盐(NO3 -,NO2 -)还原成为NH4 +,进而与阳极区生成的强氧化性物质反应生成无害N2。
阴极附近电化学反应历程:
在体系中存在氯离子或次氯酸根离子的条件下,电化学还原产物氨氮通过活性氯间接氧化为无害气体氮气,即溶液中氯离子被氧化为C12,C12溶于水生成氧化性极强的HClO、C1O-,将废水中产生的氨氮氧化去除。主要反应机理如式(5)-(11)所示:
阳极附近电化学反应历程:
2Cl-→Cl2+2e- (5)
Cl2+H2O→HClO+H++Cl- (6)
HClO→ClO-+H+ (7)
-OH-e-→·OH (8)
与现有技术相比,本发明的有益效果在于:
(1)首次设计双防腐层,即氧化石墨烯/聚苯胺和苯并***依次引入,促使阳极材料具有更好的防腐性;
(2)利用氧化石墨烯原位聚合苯胺单体制备氧化石墨烯/聚苯胺复合材料,促使聚苯胺与氧化石墨烯牢固结合,提高第一防腐层的稳定性;同时由于聚苯胺的特殊的电学、光学性质,经掺杂后Ti基阳极具有优异的导电性及电化学性能,在防腐条件下进一步实现对硝酸盐降解效果的提高;
(3)第二防腐层引入的典型有机缓蚀剂苯并***(BTA),特别对卤素介质中的金属具有很好的防腐性能,并且旋涂的引入方式简单快速且高效,具有很好的放大前景。
(四)附图说明
图1是本发明实施例1中的聚苯胺-氧化石墨烯的扫描电镜图。
(五)具体实施方式
下面结合具体实施例,对本发明加以详细描述,但本发明并不限于下述实施例,在不脱离本发明内容和范围内,变化实施都应包含在本发明的技术范围内。
本实施例中的氧化石墨烯的制备均采用下述方法制备所得:
在冰浴条件下将1.5g NaNO3和1.5g天然鳞片石墨加入到69ml的98%浓H2SO4溶液中并将混合物搅拌均匀。然后将6g KMnO4加入体系中,在冰浴条件下搅拌2h。将混合物转移至35℃的油浴中反应1h。随后将92ml去离子水加入混合溶液中,再将反应体系的温度升至98℃反应30min。待混合溶液冷却至室温后,加入6ml 30wt%H2O2,离心除去残留的KMnO4。用1wt%稀盐酸洗涤离心后的下层沉淀,然后用去离子水洗涤。最后将它们在50℃下真空干燥,得到氧化石墨烯。
实施例1:
(1)聚苯胺-氧化石墨烯复合材料制备
称取1g制备的氧化石墨烯分散在1L纯水中,经超声分散后,加入10g苯胺单体及20ml浓度为1.5mol/L的盐酸溶液,搅拌过程中加入7.5g过硫酸铵,25℃下搅拌2h完成原位聚合。然后经纯水洗涤离心后在60℃下真空烘干。
(2)Ti电极片涂覆聚苯胺-氧化石墨烯复合材料
分别称取1.4g聚苯胺-氧化石墨烯复合材料,0.2g乙炔黑,0.1g聚四氟乙烯,在研钵中混合研磨成细粉,加入6ml乙醇调配浆料为糊状,涂覆到Ti极片上,80℃真空干燥8h。
(3)苯并***(BTA)改性的聚苯胺-氧化石墨烯/Ti电极
配制0.2mol/L的BTA的异丙醇溶液,以4000rpm速率,在电极片表面旋涂BTA溶液30s,60℃真空干燥4h。
实施例2:
(1)聚苯胺-氧化石墨烯复合材料制备
称取1g制备的氧化石墨烯分散在1L纯水中,经超声分散后,加入25g苯胺单体及20ml浓度为1.5mol/L的盐酸溶液,搅拌过程中加入7.5g过硫酸铵,25℃下搅拌2h完成原位聚合。然后经纯水洗涤离心后在60℃下真空烘干。
(2)Ti电极片涂覆聚苯胺-氧化石墨烯复合材料
分别称取1.4g聚苯胺-氧化石墨烯复合材料,0.2g乙炔黑,0.1g聚四氟乙烯,在研钵中混合研磨成细粉,加入6ml乙醇调配浆料为糊状,涂覆到Ti极片上,80℃真空干燥8h。
(3)苯并***(BTA)改性的聚苯胺-氧化石墨烯/Ti电极
配制0.2mol/L的BTA的异丙醇溶液,以4000rpm速率,在电极片表面旋涂BTA溶液30s,60℃真空干燥4h。
实施例3:
(1)聚苯胺-氧化石墨烯复合材料制备
称取1g上述制备的氧化石墨烯分散在1L纯水中,经超声分散后,加入10g苯胺单体及20ml浓度为1.5mol/L的盐酸溶液,搅拌过程中加入7.5g过硫酸铵,25℃下搅拌2h完成原位聚合。然后经纯水洗涤离心后在60℃下真空烘干。
(2)Ti电极片涂覆聚苯胺-氧化石墨烯复合材料
分别称取1.5g聚苯胺-氧化石墨烯复合材料,0.2g乙炔黑,0.08g聚四氟乙烯,在研钵中混合研磨成细粉,加入6ml乙醇调配浆料为糊状,涂覆到Ti极片上,80℃真空干燥8h。。
(3)苯并***(BTA)改性的聚苯胺-氧化石墨烯/Ti电极
配制0.2mol/L的BTA的异丙醇溶液,以4000rpm速率,在电极片表面旋涂BTA溶液30s,60℃真空干燥4h。
实施例4:
(1)聚苯胺-氧化石墨烯复合材料制备
称取1g制备的氧化石墨烯分散在1L纯水中,经超声分散后,加入10g苯胺单体及20ml浓度为1.5mol/L的盐酸溶液,搅拌过程中加入7.5g过硫酸铵,25℃下搅拌2h完成原位聚合。然后经纯水洗涤离心后在60℃下真空烘干。
(2)Ti电极片涂覆聚苯胺-氧化石墨烯复合材料
分别称取1.4g聚苯胺-氧化石墨烯复合材料,0.2g乙炔黑,0.1g聚四氟乙烯,在研钵中混合研磨成细粉,加入6ml乙醇调配浆料为糊状,涂覆到Ti极片上,80℃真空干燥8h。
(3)苯并***(BTA)改性的聚苯胺-氧化石墨烯/Ti电极
配制0.8mol/L的BTA的异丙醇溶液,以4000rpm速率,在电极片表面旋涂BTA溶液30s,60℃真空干燥4h。
对比例1:
(1)聚苯胺-氧化石墨烯复合材料制备
称取1g制备的氧化石墨烯分散在1L纯水中,经超声分散后,加入10g苯胺单体及20ml浓度为1.5mol/L的盐酸溶液,搅拌过程中加入7.5g过硫酸铵,25℃下搅拌2h完成原位聚合。然后经纯水洗涤离心后在60℃下真空烘干。
(2)Ti电极片涂覆聚苯胺-氧化石墨烯复合材料
分别称取1.4g聚苯胺-氧化石墨烯复合材料,0.2g乙炔黑,0.1g聚四氟乙烯,在研钵中混合研磨成细粉,加入6ml乙醇调配浆料为糊状,涂覆到Ti极片上,80℃真空干燥8h。
对比例2:
(1)Ti电极片涂覆BTA材料
配制0.2mol/L的BTA的异丙醇溶液,以4000rpm速率,在Ti电极片表面旋涂BTA溶液30s,60℃真空干燥4h。
配制1500ppm NO3 --N模拟废水(称取1.625g经110℃烘干的硝酸钾,溶于150mL去离子水中),同时加入2g NaCl固体。以所述防腐型Ti基电极作为阳极材料,以铜电极作为阴极材料,在恒定电压10V下催化还原配制的含高浓度Cl-的硝酸盐溶液,将本发明技术方案制备的苯并***(BTA)改性的聚苯胺-氧化石墨烯/Ti电极在室温下采用四探针法测定其电导率,具体测试结果如下表1所示:
表1性能测试表
电极 | 120min后还原率% | 腐蚀电压/mV | 腐蚀电流/μA |
实施例1 | 57.22% | 541.9 | 5.5 |
实施例2 | 69.2% | 523.6 | 5.1 |
实施例3 | 59.1% | 533.8 | 5.4 |
实施例4 | 34.7% | 556.5 | 7.2 |
对比例1 | 20.6% | 582.3 | 14.9 |
对比例2 | 27.3% | 578.1 | 15.7 |
Ti电极 | 22.1% | 1216.6 | 33.9 |
Claims (10)
1.一种防腐型Ti基阳极电极材料,其特征在于所述防腐型Ti基阳极电极材料按照如下方法制备:
(1)将氧化石墨烯均匀分散于溶剂A中,得到氧化石墨烯分散液;加入苯胺、0.1-2mol/L酸的水溶液,搅拌下加入自由基引发剂,20~60℃下反应2~12h进行原位聚合,所得反应液经后处理,得到聚苯胺-氧化石墨烯复合材料;
所述溶剂A为水、乙醇、乙二醇、异丙醇、正丁醇、N,N-二甲基甲酰胺、丙酮、甲苯中的一种或两种以上的混合液;所述酸的水溶液中的酸为无机酸、有机酸中一种或两种的混合物;所述氧化石墨烯、苯胺与自由基引发剂的质量比为1:5~40:5~20;所述苯胺与酸的水溶液的质量比为1:1~5;
(2)将步骤(1)所述的聚苯胺-氧化石墨烯复合材料、导电剂、粘结剂混合研磨均匀,加入溶剂B调配成浆料,所述浆料涂覆到Ti极片上后,干燥,得到电极极片;所述聚苯胺-氧化石墨烯复合材料、导电剂与粘结剂的质量比为80~95:12:3~10;所述导电剂为乙炔黑、碳纳米管、碳纳米线、炭黑KS-6、炭黑SP中的一种或两种以上的混合物;所述粘结剂为聚偏氟乙烯或聚四氟乙烯;
(3)将0.1~1mol/L苯并***的异丙醇溶液旋涂在步骤(2)所述的电极极片表面,干燥,即得所述防腐型Ti基阳极电极材料。
2.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于:步骤(1)中所述溶剂A的体积以所述氧化石墨烯的质量计为0.5~3mL/mg。
3.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于:步骤(1)中所述无机酸为氯化氢、硫酸、磷酸、硝酸中的一种或两种的混合物。
4.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于:步骤(1)中所述有机酸为乙酸、酒石酸、柠檬酸、草酸、氨基磺酸中的一种或两种的混合物。
5.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于:步骤(1)中所述自由基引发剂为过硫酸钠、过硫酸钾、过硫酸铵、偶氮二异丁腈、过氧化苯甲酰、过氧化苯甲酸叔丁酯、叔丁基过氧化氢中一种或两种以上的混合物。
6.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于步骤(1)中所述后处理为:所述反应液离心,取沉淀用纯水离心洗涤,在30~80℃下真空干燥,得到所述聚苯胺-氧化石墨烯复合材料。
7.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于:步骤(2)中所述溶剂B为水、乙醇、甲醇、正丁醇、异丙醇中的一种或两种以上的混合液。
8.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于:步骤(2)中所述溶剂B的体积以所述导电剂的质量计为20~60mL/g。
9.如权利要求1所述的防腐型Ti基阳极电极材料,其特征在于:步骤(3)中所述旋涂的速度为2000~5000rpm,旋涂的时间为20~60s。
10.一种如权利要求1所述的防腐型Ti基阳极电极材料在还原硝态氮中的应用。
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