CN106064845B - 一种用于污水处理的稀土元素掺杂石墨稀电极的制备方法 - Google Patents
一种用于污水处理的稀土元素掺杂石墨稀电极的制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于污水处理的稀土元素掺杂石墨稀电极的制备方法。采用铁、铂、钴或导电玻璃为基底，利用化学气相沉淀法制备基底薄片；将基底薄片在氩气下放入密闭的加热炉中进行高温预热处理4‑6小时；制成石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，在精密流量泵控制下，在氩气保护下通过毛细管将石墨烯与稀土元素硝酸盐、硫酸盐混合溶液缓慢注入密闭反应室，保持高温持续反应4‑6小时。本发明的有益效果为：1）对污水中的有机物进行高效的氧化降解，大幅度降低污水中的COD值；2）使用该电极处理污水的反应速度快；3）反应高效无毒；4）反应结束后电极经过处理后可重复使用。
Description
技术领域
本发明涉及污水处理领域，具体涉及一种用于污水处理的稀土元素掺杂石墨稀电极的制备方法。
背景技术
随着工业废水的排放量日益增加，不达标的工业废水排入水体后，会污染地表水和地下水；水体一旦受到污染，要想在短时间内恢复到原来的状态是不容易的，不仅会使其水质不符合饮用水、渔业用水的标准，还会使地下水中的化学有害物质和硬度增加，影响地下水利用，直接或间接地给人民生活和身体健康带来危害。特别是当COD值（是指在一定严格的条件下，水中的还原性物质在外加的强氧化剂的作用下被氧化分解时所消耗氧化剂的数量）很高时，就会增加处理工艺的负荷，对于工艺要求也相应的增加，同时出水很难保证，如果没有处理装置的直接排放进入自然水体的情况，就会造成自然水体水质的恶化；原因在于：水体自净需把这些有机物降解，COD 的降解肯定需要耗氧，而水体中的复氧能力不可能满足要求，水中DO就会直接降为0，成为厌氧状态，在厌氧状态也要继续分解（微生物的厌氧处理），水体就会发黑、发臭（厌氧微生物是看起来很黑，有硫化氢气体生成）；最终危害就是进入自然水体，破坏水体平衡，造成除微生物外几乎所有生物的死亡，进一步影响周边环境。另外，工业废水中的有机物含量普遍较高，且受有机物污染的程度变化很快，因此，COD值还可表征水中有机物的相对含量。自然生活在这种环境下的人群的健康状态就会每况愈下；一般高COD 的工业废水中都含有很多挥发性刺激性物质，而这些稠环芳香化合物长期滞留在人体内，损坏某些特定的组织器官，比如沉积在肺、肾等重要组织器官，或损害神经系统功能等，对于怀孕妇女人群来说，这些物质也是致畸胎的罪魁祸首。
用来降低水中COD值的传统方法主要包括氧化剂氧化法、电解法、生物处理法。其中，氧化剂氧化法原理简单，但是只能在形式上降低COD值，仍然存在造成二次污染的可能性；电解法仅适用于处理一般氧化剂难以氧化的还原性有机物，而且耗电量大、不经济；生物处理法相对自然且无污染，但是需要培养特殊微生物，速度较慢，仅适用于处理初始COD值并不高的水样。
目前，用于污水处理技术当中具有较好发展前景的方法为高级氧化技术，高级氧化技术（Advanced Oxidation Process,简称AOPs）可将废水直接矿化或者通过氧化提高污染物的可生化性，同时还在环境类激素等微量有害化学物质的处理方面具有很大的优势，能够使绝大部分有机物完全矿化或分解。因此，制备出高效的氧化电解物质是当下亟须解决的问题。
发明内容
本发明的目的是为了克服现有技术中存在的不足，提供一种用于污水处理的稀土元素掺杂石墨稀电极的制备方法，在高级氧化法的基础上，利用该电极对有机物含量较高的污水进行处理，可以快速地使污水中的COD值大幅下降。
为解决上述技术问题，本发明的技术方案为：
一种用于污水处理的稀土元素掺杂石墨稀电极的制备方法，包括以下步骤：
A.基底薄片的制备：采用铁、铂、钴或导电玻璃为基底，利用化学气相沉淀法制备基底薄片；
B.预热处理：将步骤A中所述的基底薄片在氩气下放入密闭的加热炉中进行高温预热处理4-6小时，保持反应室温度恒定且氩气流速恒定；
C. 稀土元素掺杂石墨烯薄膜的制备：将石墨烯均匀分散在水、甲醇、乙醇、异丙醇溶剂中，将所述溶剂与稀土元素硝酸盐和硫酸盐的混合溶液混合制成石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，在精密流量泵控制下，在氩气保护下通过毛细管将石墨烯与稀土元素硝酸盐、硫酸盐混合溶液缓慢注入密闭反应室，保持高温持续反应4-6小时；
D.后处理：反应结束后，停止注入所述石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，关闭电炉且保持氩气了流速不变，待电极自然冷却至室温。
与现有技术相比，本发明的有益效果为：1）该电极具有很高的电解氧化处理污水效果，稀土元素的引入使得电极表面在通电后可高效产生羟基自由基等高活性氧化中间体，对污水中的有机物进行高效的氧化降解，大幅度降低污水中的COD值；2）使用该电极处理污水的反应速度快，反应过程中不会产生有毒有害气体，反应后的产物稳定，不会产生气体有害物质；3）反应高效无毒，反应前后对人体安全，对设备无污染；4）反应结束后电极经过处理后可重复使用，高效环保。
具体实施方式
为使对本发明的结构特征及所达成的功效有更进一步的了解与认识，用以较佳的实施例详细的说明，说明如下：
实施例1
本发明实施例的用于污水处理的稀土元素掺杂石墨稀电极的制备方法，包括以下步骤：
A.基底薄片的制备：采用铁、铂、钴或导电玻璃为基底，利用化学气相沉淀法制备基底薄片；B.预热处理：将步骤A中所述的基底薄片在氩气下放入密闭的加热炉中进行高温预热处理5小时，保持反应室温度恒定且氩气流速恒定；C. 稀土元素掺杂石墨烯薄膜的制备：将石墨烯均匀分散在水中，将所述溶剂与稀土元素硝酸盐和硫酸盐的混合溶液混合制成石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，在精密流量泵控制下，在氩气保护下通过毛细管将石墨烯与稀土元素硝酸盐、硫酸盐混合溶液缓慢注入密闭反应室，保持高温持续反应5小时；石墨烯与稀土元素在基底薄片上逐渐沉积并形成连续的稀土元素掺杂石墨烯薄膜；D.后处理：反应结束后，停止注入所述石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，关闭电炉且保持氩气了流速不变，待电极自然冷却至室温。制备出的稀土元素掺杂石墨烯电极用于污水处理，能够产生具有很强氧化能力的羟基自由基使污水中的有机物氧化降解为二氧化碳、水和其他无毒的小分子化合物，污水的COD值可以快速的大幅度下降。
实施例2
本发明实施例的用于污水处理的稀土元素掺杂石墨稀电极的制备方法，包括以下步骤：
基底薄片的制备：采用铁、铂、钴或导电玻璃为基底，利用化学气相沉淀法制备基底薄片；B.预热处理：将步骤A中所述的基底薄片在氩气下放入密闭的加热炉中进行高温预热处理5.5小时，保持反应室温度恒定且氩气流速恒定；C. 稀土元素掺杂石墨烯薄膜的制备：将石墨烯均匀分散在甲醇中，将所述溶剂与稀土元素硝酸盐和硫酸盐的混合溶液混合制成石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，在精密流量泵控制下，在氩气保护下通过毛细管将石墨烯与稀土元素硝酸盐、硫酸盐混合溶液缓慢注入密闭反应室，保持高温持续反应5.5小时；石墨烯与稀土元素在基底薄片上逐渐沉积并形成连续的稀土元素掺杂石墨烯薄膜；D.后处理：反应结束后，停止注入所述石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，关闭电炉且保持氩气了流速不变，待电极自然冷却至室温。制备出的稀土元素掺杂石墨烯电极用于污水处理，能够产生具有很强氧化能力的羟基自由基使污水中的有机物氧化降解为二氧化碳、水和其他无毒的小分子化合物，污水的COD值可以快速的大幅度下降。
实施例3
本发明实施例的用于污水处理的稀土元素掺杂石墨稀电极的制备方法，包括以下步骤：
A.基底薄片的制备：采用铁、铂、钴或导电玻璃为基底，利用化学气相沉淀法制备基底薄片；B.预热处理：将步骤A中所述的基底薄片在氩气下放入密闭的加热炉中进行高温预热处理5小时，保持反应室温度恒定且氩气流速恒定；C. 稀土元素掺杂石墨烯薄膜的制备：将石墨烯均匀分散在乙醇中，将所述溶剂与稀土元素硝酸盐和硫酸盐的混合溶液混合制成石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，在精密流量泵控制下，在氩气保护下通过毛细管将石墨烯与稀土元素硝酸盐、硫酸盐混合溶液缓慢注入密闭反应室，保持高温持续反应5小时；石墨烯与稀土元素在基底薄片上逐渐沉积并形成连续的稀土元素掺杂石墨烯薄膜；D.后处理：反应结束后，停止注入所述石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，关闭电炉且保持氩气了流速不变，待电极自然冷却至室温。制备出的稀土元素掺杂石墨烯电极用于污水处理，能够产生具有很强氧化能力的羟基自由基使污水中的有机物氧化降解为二氧化碳、水和其他无毒的小分子化合物，污水的COD值可以快速的大幅度下降。
实施例4
本发明实施例的用于污水处理的稀土元素掺杂石墨稀电极的制备方法，包括以下步骤：
A.基底薄片的制备：采用铁、铂、钴或导电玻璃为基底，利用化学气相沉淀法制备基底薄片；B.预热处理：将步骤A中所述的基底薄片在氩气下放入密闭的加热炉中进行高温预热处理5.5小时，保持反应室温度恒定且氩气流速恒定；C. 稀土元素掺杂石墨烯薄膜的制备：将石墨烯均匀分散在异丙醇中，将所述溶剂与稀土元素硝酸盐和硫酸盐的混合溶液混合制成石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，在精密流量泵控制下，在氩气保护下通过毛细管将石墨烯与稀土元素硝酸盐、硫酸盐混合溶液缓慢注入密闭反应室，保持高温持续反应5.5小时；石墨烯与稀土元素在基底薄片上逐渐沉积并形成连续的稀土元素掺杂石墨烯薄膜；D.后处理：反应结束后，停止注入所述石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，关闭电炉且保持氩气了流速不变，待电极自然冷却至室温。制备出的稀土元素掺杂石墨烯电极用于污水处理，能够产生具有很强氧化能力的羟基自由基使污水中的有机物氧化降解为二氧化碳、水和其他无毒的小分子化合物，污水的COD值可以快速的大幅度下降。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是本发明的原理，在不脱离本发明精神和范围的前提下本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明的范围内。本发明要求的保护范围由所附的权利要求书及其等同物界定。
Claims (1)
1.一种用于污水处理的稀土元素掺杂石墨稀电极的制备方法，其特征在于，包括以下步骤：
A.基底薄片的制备：采用铁、铂、钴或导电玻璃为基底，利用化学气相沉淀法制备成基底薄片；
B.预热处理：将步骤A中所述的基底薄片在氩气下放入密闭的加热炉中进行高温预热处理4-6小时，保持加热炉温度恒定且氩气流速恒定；
C.稀土元素掺杂石墨烯薄膜的制备：将石墨烯均匀分散在水、甲醇、乙醇和异丙醇溶剂中，将所述溶剂与稀土元素硝酸盐和硫酸盐的混合溶液混合制成石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，在精密流量泵控制下，在氩气保护下通过毛细管将石墨烯与稀土元素硝酸盐、硫酸盐混合溶液缓慢注入加热炉，保持高温持续反应4-6小时；
D.后处理：反应结束后，停止注入所述石墨烯与稀土元素硝酸盐、硫酸盐混合溶液，关闭加热炉且保持氩气流速不变，待电极自然冷却至室温。
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