CN109574153A - 一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺 - Google Patents

一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺 Download PDF

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CN109574153A
CN109574153A CN201811551124.3A CN201811551124A CN109574153A CN 109574153 A CN109574153 A CN 109574153A CN 201811551124 A CN201811551124 A CN 201811551124A CN 109574153 A CN109574153 A CN 109574153A
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孙治荣
王睿浩
朱凯
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Abstract

一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺，属于电化学水处理技术领域。本发明以优化后的Pd/RGO‑nafion/Ti电极为阴极，以溶胶凝胶法制备的SnO2‑Sb‑Ni电极为阳极，采用三联耦合装置，可以将阴极脱氯过程所需最适电流提高到与阳极苯酚降解所需最适电流相匹配，这就解决了阴极还原氯酚及阳极氧化苯酚所需最适电流密度不匹配的问题，使得阴阳极均在最优条件下降解污染物，同步实现电催化还原与氧化反应的高效进行。该耦合装置可以将目前电化学技术上单纯的阳极氧化和阴极还原过程耦合起来实现双重利用，解决了辅助电极只提供电路的问题，极大提高了能源的利用率。

Description

一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺
技术领域
本发明涉及电化学水处理技术领域，具体涉及一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺的构建，该工艺体系可实现阴阳极两种不同污染物的同步高效降解。
背景技术
电化学还原是指氯代有机物在电极阴极表面形成吸附态，再被电子攻击，从而造成吸附态氯代有机物的C-Cl键断裂的反应。通过阴极还原可将多氯代芳香族化合物部分或完全脱氯，转化为低毒的加氢产物，作为氧化法和生物法的预处理具有广阔的前景。
电催化氧化法处理废水中的有机污染物，就是使有机物在电极表面发生直接或间接氧化反应，最终生成H2O和CO2而从体系中除去。一般认为根据电极参与氧化反应的机理不同，电催化氧化过程可分为直接电化学氧化法和间接电化学氧化法两个过程。
传统的电化学催化只是单纯的研究电化学还原或电催化氧化，这就造成了辅助电极只是单纯提供电路，或者只是对工作电极提供少部分帮助的情况，这种单一的降解办法能耗大，成本高，制约了其在废水处理中的发展以及实际应用的可能性。因此，开发一种将单纯的阳极氧化和阴极还原过程耦合起来实现双重利用的工艺，具有十分重要的意义。
发明内容
本发明提供了一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺的构建。包括以下内容：
(1)一个阳极室对应两个并联阴极室的三联耦合装置；包括：两个实现阴极氯酚脱氯的并联阴极室；一个实现阳极苯酚开环降解的阳极室；阳极室分别和两个阴极室连通，阴阳极室之间采用用于区分阴阳极室的只允许阳离子自由通过的阳离子交换膜分隔；阳极室与电池的正极连接，阴极室分别与电池的负极连接；
(2)分别将相同体积、浓度的2，4，6-TCP溶液分别注入到三联耦合装置两端的两阴极室内，在阴极电化学还原作用下实现氯酚脱氯；将一定体积的苯酚溶液注入到阳极室内，在阳极电化学氧化作用下实现苯酚开环降解；阴极室和阳极室的支持电解质均为0.01-0.1mol/L的Na2SO4溶液；
(3)优化后的石墨烯镀钯电极为阴极分别放置在两个阴极室内，溶胶凝胶法制备的SnO2-Sb-Ni电极为阳极放置在阳极室内，调节阴阳极室pH，阴极室pH为1-3，阳极室pH为3-9；施加耦合降解总电流为40-120mA，阳极电流密度为5-15mA/cm2，阴极电流密度为0.5-1.5mA/cm2，进行阴阳极耦合降解污染物；
作为优选，负载石墨烯镀钯阴极的优化制备方法如下：首先，称取一定量的石墨烯和萘酚溶液超声分散于异丙醇溶液中(石墨烯，萘酚膜溶液在异丙醇溶液中的质量浓度分别为0.05％，6％)，采用表面涂覆的方法涂覆到预处理除油除氧化物后的4×5cm2钛网上，室温晾干，制得以钛网为基体的石墨烯-萘酚电极；其次，配制浓度为9mmol/L的氯化钯(PdCl2)溶液，以制备的石墨烯-萘酚电极为阴极，以铂片为阳极，在PdCl2溶液中采用恒定电流法电沉积制得Pd/RGO-nafion/Ti电极即石墨烯镀钯电极，沉积电流密度为2.5mA/cm2-4.5mA/cm2，沉积时间为30～90min。
阳极面积与单个阴极面积比为1:1-1:5。
与现有技术相比，本发明具有以下优异效果：
(1)优化后的石墨烯镀钯电极与原始电极相比具有更高的氢吸附峰电流值，意味着具有更高的电催化还原脱氯能力。
(2)将阴极的面积由原始的2×2cm2扩大为4×5cm2，阴极降解氯酚最适电流密度相近的情况下，大幅提高了最适降解电流；
(3)三联耦合装置进一步解决了阴阳极电催化污染物所需最适电流密度不匹配的问题，实现了阴极还原氯酚与阳极氧化苯酚的同步高效耦合，解决了辅助电极单纯提供电路的问题，极大提高了能源的利用率；
(4)由于阴阳极室之间加了阳离子交换膜，使得阳极降解苯酚不受阴极的影响，从而展示出更高的降解能力；
(5)采用三联耦合装置将阴极还原氯酚与阳极氧化苯酚同步耦合，由于并联所以总电阻变为单联阴极降解装置的一半。相同电压下，同一时间污染物的处理量增长为原始阴极降解装置的一倍。
附图说明
图1为实施例1所优化后的的Pd/RGO-nafion/Ti电极和原始的Pd/RGO-nafion/Ti电极的CV曲线图。
图2为实施例1优化后的的Pd/RGO-nafion/Ti电极在耦合体系中对氯酚的降解率以及同时阳极对苯酚的转化率(conversion efficiency)。
图3耦合体系与非耦合体系下同一阳极对苯酚的降解情况(phenolconcentration)。
图4为三联耦合降解装置
具体实施方式
下面实施例和对比例将结合附图对本发明作进一步的说明，但本发明并不限于以下实施例。
实施例1：
(1)将120mL相同体积浓度为150mg/L的2，4，6-TCP溶液分别注入到两端的阴极室内，在阴极电化学还原作用下实现氯酚脱氯；阳极室内注入60mL浓度为50mg/L的苯酚溶液，在阳极电化学氧化作用下实现苯酚开环降解。支持电解质均为0.05mol/L的Na2SO4溶液。
(2)调节阴极室内pH为2.3，阳极室内pH为5.8。区分阴阳极室的离子交换膜为只允许阳离子自由通过的阳离子交换膜。
(3)优化后的石墨烯镀钯电极为阴极分别放置在两个阴极室内，溶胶凝胶法制备的SnO2-Sb-Ni电极(Zhirong Sun,Huan Zhang1,Xuefeng Wei,Xiaoyue Ma,Xiang Hu(2015)Preparation and electrochemical properties of SnO2-Sb-Ni-Ce oxide anodefor phenol oxidation.Journal of Solid State Electrochemistry 19:2445–2456)为阳极放置在阳极室内，阳极面积与单个阴极面积比为1:5，施加80mA的总电流进行阴阳极耦合降解污染物。氯酚的降解率如图2中曲线(1)所示。苯酚的转化率(conversionefficiency)如图2中曲线(2)所示。
(4)作为优选，负载石墨烯镀钯阴极的优化制备方法如下：首先，称取一定量的石墨烯和萘酚溶液超声分散于异丙醇溶液中(石墨烯，萘酚膜溶液在异丙醇溶液中的质量浓度分别为0.05％，6％)，采用表面涂覆的方法涂覆到预处理除油除氧化物后的4×5cm2钛网上，室温晾干，制得以钛网为基体的石墨烯-萘酚电极；其次，配制浓度为9mmol/L的氯化钯(PdCl2)溶液，以制备的石墨烯-萘酚电极为阴极，以铂片为阳极，在PdCl2溶液中采用恒定电流法电沉积制得Pd/RGO-nafion/Ti电极，沉积电流为4mA/cm2，沉积时间为70min。
(5)电化学性能测试：以优化后的Pd/RGO-nafion/Ti电极作为工作电极，铂片为对电极，Hg/Hg2SO4电极为参比电极，以0.5mol/L H2SO4为电解质溶液，采用循环伏安法(CV)测定电极的电化学性能，扫描速率为50mV/s。测得该电极循环伏安曲线如图1中曲线(2)所示。
实施例2：
制备原始的Pd/RGO-nafion/Ti电极。
电化学性能测试：以原始的Pd/RGO-nafion/Ti电极作为工作电极，铂片为对电极，Hg/Hg2SO4电极为参比电极，以0.5mol/L H2SO4为电解质溶液，采用循环伏安法(CV)测定电极的电化学性能，扫描速率为50mV/s。测得该电极循环伏安曲线如图1中曲线(1)所示。
实施例3：
具体制备过程同实施例1，耦合情况下苯酚的降解情况(phenol concentration)如图3中曲线(1)所示
在非耦合装置单个反应器内注入60mL浓度为50mg/L的苯酚溶液，调节pH为5.8，铂片为对电极，溶胶凝胶法制备的SnO2-Sb-Ni电极为阳极，施加80mA的总电流在阳极降解苯酚，支持电解质为0.05mol/L的Na2SO4溶液。苯酚的降解情况(phenol concentration)如图3中曲线(2)所示。

Claims (5)

1.一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺方法，其特征在于，包括以下内容：
(1)一个阳极室对应两个并联阴极室的三联耦合装置；包括：两个实现阴极氯酚脱氯的并联阴极室；一个实现阳极苯酚开环降解的阳极室；阳极室分别和两个阴极室连通，阴阳极室之间采用用于区分阴阳极室的只允许阳离子自由通过的阳离子交换膜分隔；阳极室与电源的正极连接，阴极室分别与电源的负极连接；
(2)分别将相同体积、浓度的2，4，6-TCP溶液分别注入到三联耦合装置两端的两阴极室内，在阴极电化学还原作用下实现氯酚脱氯；将一定体积的苯酚溶液注入到阳极室内，在阳极电化学氧化作用下实现苯酚开环降解；阴极室和阳极室的支持电解质均为0.01-0.1mol/L Na2SO4溶液；
(3)优化后的石墨烯镀钯电极为阴极分别放置在两个阴极室内，溶胶凝胶法制备的SnO2-Sb-Ni电极为阳极放置在阳极室内，调节阴阳极室pH，阴极室pH为1-3，阳极室pH为3-9；阳极电流密度为5-15mA/cm2，阴极电流密度为0.5-1.5mA/cm2；进行阴阳极耦合降解污染物。
2.按照权利要求1所述的一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺方法，其特征在于，Na2SO4的浓度为0.05mol/L。
3.按照权利要求1所述的一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺方法，其特征在于，负载石墨烯镀钯阴极的优化制备方法如下：首先，称取一定量的石墨烯和萘酚溶液超声分散于异丙醇溶液中(石墨烯，萘酚膜溶液在异丙醇溶液中的质量浓度分别为0.05％，6％)，采用表面涂覆的方法涂覆到预处理除油除氧化物后的4×5cm2钛网上，室温晾干，制得以钛网为基体的石墨烯-萘酚电极；其次，配制浓度为9mmol/L的氯化钯(PdCl2)溶液，以制备的石墨烯-萘酚电极为阴极，以铂片为阳极，在PdCl2溶液中采用恒定电流法电沉积制得Pd/RGO-nafion/Ti电极即石墨烯镀钯电极，沉积电流密度为2.5mA/cm2-180mA/cm2，沉积时间为30～90min。
4.按照权利要求1所述的一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺方法，其特征在于，阳极面积与单个阴极面积比为1:1-1:5。
5.按照权利要求1所述的一种阴极还原氯酚与阳极氧化苯酚的同步高效耦合工艺方法，其特征在于，施加耦合降解总电流为40-120mA，阳极电流密度为5-15mA/cm2，阴极电流密度为0.5-1.5mA/cm2。
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