CN106835192B - 一种电解二氧化锰用钛基阳极表面复合涂层的制备方法 - Google Patents
一种电解二氧化锰用钛基阳极表面复合涂层的制备方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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- C23C24/00—Coating starting from inorganic powder
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- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- C—CHEMISTRY; METALLURGY
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- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
Abstract
本发明公开了一种电解二氧化锰用钛基阳极表面复合涂层的制备方法。对工业纯钛片依次进行打磨、碱洗、刻蚀处理；然后，将四氯化锡乙醇溶液和硝酸锰乙醇溶液按照Sn:Mn=6:4（摩尔比）充分混合，制得涂层混合液，对钛片进行涂刷，将涂刷好的钛片放入70~90℃的烘箱中烘干10~30分钟。再将烘干后的钛片在电炉上煅烧1~20分钟，煅烧结束后将其取出在室温下自然冷却；最后，将钛片放入马弗炉中于400~600℃下烧结1小时后自然冷却至室温，重复该操作2~4次，在钛片表面得到电解二氧化锰用钛基阳极表面复合涂层。本发明方法操作简单，降低能耗，且所制备的复合涂层致密呈凹凸不平的层状，该复合涂层修饰的钛基阳极应用到电解二氧化锰中，能够有效的降低电解槽压。
Description
技术领域
本发明属于电解阳极表面复合涂层技术领域，特别涉及一种电解二氧化锰用钛基阳极表面复合涂层的制备方法。
背景技术
在电解二氧化锰工业中，电解阳极对电极反应的速度、选择性(方向)、电流效率、能源消耗及最终产品电解二氧化锰的质量都有较大的影响，因此电解二氧化锰工业受阳极的约束非常大。在电解二氧化锰时对阳极材料来说，由于在阳极发生氧化反应而且通常反应条件比较苛刻，易导致阳极损耗，而且要求电极对沉积二氧化锰有电化学催化性能，有较低的过电位和较低的槽压，因此对于阳极材料的选择是电解二氧化锰工业的难题之一。
在电解二氧化锰工业中阳极通常选用不溶性阳极，主要有石墨阳极、铅及其合金阳极、钛及其复合涂层阳极和铂族贵金属DSA阳极，它们各有优缺点。但钛及其复合涂层阳极，因为其相比传统的石墨和铅合金阳极，具有更优秀的电催化活性和使用寿命，又比铂族贵金属DSA电极有更有利的经济成本优势，所以被广泛的用于氯碱行业、电镀行业、电解行业、污水处理等。因此，在电解二氧化锰工业上，使用钛基复合涂层阳极成为一种趋势。较早使用的涂层阳极是二氧化锰修饰钛基阳极，该阳极存在一定的缺点：二氧化锰涂层表面裂纹较多，孔隙率较大，使用一段时间后电解液会透过活性层与基体反应生成TiO2中间层，导致阳极电阻变大以致阳极钝化。为了提高钛基阳极的电流效率，降低电解槽压，本发明选用工业纯钛作为基体，二氧化锰和二氧化锡作为复合活性涂层，采用简易的热分解方法制备出钛基复合涂层阳极。该方法制备的阳极具有工艺简单，选择性和耐腐蚀性好、价格低廉、电解的二氧化锰产品纯度高等特点，具有较大的实用经济价值。
发明内容
本发明的目的是提供一种电解二氧化锰用钛基阳极表面复合涂层的制备方法。
具体步骤为：
(1) 选取工业纯钛片为基体材料，打磨除去钛片的表面氧化膜，然后放入质量百分比浓度为10%的微沸NaOH溶液中加热5~20分钟，再取出钛片用蒸馏水冲洗干净，然后放入质量百分比浓度为10~30%的微沸草酸溶液进行酸刻蚀1~2小时，最后用蒸馏水冲洗干净，得到表面呈灰色麻状的钛片，将其浸入无水乙醇中备用。
(2) 将0.1~0.5mol/L的四氯化锡乙醇溶液和0.1~0.5mol/L的硝酸锰乙醇溶液按照摩尔比Sn:Mn=6:4进行充分混合，制得涂层混合液。
(3) 用步骤(2)制得的涂层混合液对步骤(1)得到的钛片进行均匀涂刷，将涂刷好的钛片放入70~90℃的烘箱中烘干10~30分钟，再将烘干后的钛片在电炉上煅烧1~20分钟，煅烧时要让钛片的正反面受热均匀，煅烧结束后将钛片取出在室温中自然冷却，最后，将钛片放入马弗炉中于400~600℃下烧结1小时后自然冷却至室温，重复上述马弗炉高温烧结后冷却至室温的操作步骤2~4次，在钛片表面得到二氧化锰和二氧化锡复合涂层，即为电解二氧化锰用钛基阳极表面复合涂层。
所述NaOH、草酸、无水乙醇、四氯化锡和硝酸锰均为化学纯及以上纯度。
本发明方法操作简单，使用电炉煅烧工艺减少了在马弗炉中的烧结次数，降低能耗，且所制备的复合涂层致密呈凹凸不平的层状，表面虽存在少许的裂纹，但裂纹都比较浅，只停留在表面层，将该复合涂层修饰的钛基阳极应用到电解二氧化锰中，能够有效的降低电解槽压。
附图说明
图1为本发明实施例制备的电解二氧化锰用钛基阳极表面复合涂层的微观形貌图。
具体实施方式
实施例：
(1) 选取TA2级别的工业纯钛片为基体材料，打磨除去钛片的表面氧化膜，然后放入质量百分比浓度为10%的微沸NaOH溶液中加热10分钟，再取出钛片用蒸馏水冲洗干净，然后放入质量百分比浓度为20%的微沸草酸溶液进行酸刻蚀2小时，最后用蒸馏水冲洗干净，得到表面呈灰色麻状的钛片，将其浸入无水乙醇中备用。
(2) 将0.3mol/L的四氯化锡乙醇溶液和0.3mol/L的硝酸锰乙醇溶液按照摩尔比Sn:Mn=6:4进行充分混合，制得涂层混合液。
(3) 用步骤(2)制得的涂层混合液对步骤(1)得到的钛片进行均匀涂刷，将涂刷好的钛片放入80℃的烘箱中烘干15分钟，再将烘干后的钛片在电炉上煅烧15分钟，煅烧时要让钛片的正反面受热均匀，煅烧结束后将钛片取出在室温中自然冷却，最后，将钛片放入马弗炉中于450℃下烧结1小时后自然冷却至室温，重复上述马弗炉高温烧结后冷却至室温的操作步骤3次，在钛片表面得到二氧化锰和二氧化锡复合涂层，即为电解二氧化锰用钛基阳极表面复合涂层。
所述NaOH、草酸、无水乙醇、四氯化锡和硝酸锰均为化学纯。
本实施例制得的复合涂层通过SEM表征表明，复合涂层致密呈凹凸不平的层状，表面存在少许的裂纹，但裂纹都比较浅，只停留在表面层。
将本实施例制得的复合涂层修饰的钛基阳极应用到电解二氧化锰中，观察其槽压和电流效率的变化。使用复合涂层修饰钛片作为阳极，阴极使用工业纯钛片。极间距为80mm，阳极电流密度为100 A/m2，电解液为0.3 mol/L H2SO4 和 0.8 mol/L MnSO4的混合溶液，电解温度为90 ℃。得到其电解槽压只有2.3V而电流效率达到90%以上，产物容易剥离，不含杂质，说明经该复合涂层修饰的钛片较适合作为电解二氧化锰用阳极。
Claims (1)
1.一种电解二氧化锰用钛基阳极表面复合涂层的制备方法，其特征在于具体步骤为：
(1) 选取工业纯钛片为基体材料，打磨除去钛片的表面氧化膜，然后放入质量百分比浓度为10%的微沸NaOH溶液中加热5~20分钟，再取出钛片用蒸馏水冲洗干净，然后放入质量百分比浓度为10~30%的微沸草酸溶液进行酸刻蚀1~2小时，最后用蒸馏水冲洗干净，得到表面呈灰色麻状的钛片，将其浸入无水乙醇中备用；
(2) 将0.1~0.5mol/L的四氯化锡乙醇溶液和0.1~0.5mol/L的硝酸锰乙醇溶液按照摩尔比Sn:Mn=6:4进行充分混合，制得涂层混合液；
(3) 用步骤(2)制得的涂层混合液对步骤(1)得到的钛片进行均匀涂刷，将涂刷好的钛片放入70~90℃的烘箱中烘干10~30分钟，再将烘干后的钛片在电炉上煅烧1~20分钟，煅烧时要让钛片的正反面受热均匀，煅烧结束后将钛片取出在室温中自然冷却，最后，将钛片放入马弗炉中于400~600℃下烧结1小时后自然冷却至室温，重复上述马弗炉高温烧结后冷却至室温的操作步骤2~4次，在钛片表面得到二氧化锰和二氧化锡复合涂层，即为电解二氧化锰用钛基阳极表面复合涂层；
所述NaOH、草酸、无水乙醇、四氯化锡和硝酸锰均为化学纯及以上纯度。
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Application publication date: 20170613 Assignee: Guilin Changlong Machinery Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044482 Denomination of invention: A preparation method of titanium based anode surface composite coating for electrolytic manganese dioxide Granted publication date: 20181221 License type: Common License Record date: 20231027 Application publication date: 20170613 Assignee: Guilin Xinglong Metal Products Processing Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044405 Denomination of invention: A preparation method of titanium based anode surface composite coating for electrolytic manganese dioxide Granted publication date: 20181221 License type: Common License Record date: 20231026 |