CN103910415B - A three-dimensional graphene nanomaterial electrochemical reactor for treating high-concentration organic wastewater - Google Patents
A three-dimensional graphene nanomaterial electrochemical reactor for treating high-concentration organic wastewater Download PDFInfo
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Abstract
本发明涉及一种处理高浓度有机废水的三维石墨烯纳米材料电化学反应器，该反应器包括密闭的反应器本体，反应器本体交错竖直设置有隔板，隔板将反应器本体分割成多个处理单元，处理单元中设置有夹槽，夹槽中设置有三维石墨烯纳米材料电极，反应器本体的内部顶端设置有钛电极，反应器本体的一侧上部设置有进水口，反应器本体与进水口相对的一侧的下部设置有出水口，设置在处理单元中的三维石墨烯纳米材料电极彼此并联且通过电源和钛电极连接，电源为直流电源。本发明将三维石墨烯作为电极通过施加电压来提高三维石墨烯处理有机物的效率，脱色率可达98％～100％、TOC量去除率可达96％以上。
The invention relates to a three-dimensional graphene nanomaterial electrochemical reactor for treating high-concentration organic wastewater. The reactor includes a closed reactor body, and the reactor body is staggered and vertically provided with partitions, and the partition divides the reactor body into two parts. A plurality of processing units, the processing unit is provided with a clamping groove, the clamping groove is provided with a three-dimensional graphene nanomaterial electrode, the inner top of the reactor body is provided with a titanium electrode, and the upper part of one side of the reactor body is provided with a water inlet. The lower part of the body opposite to the water inlet is provided with a water outlet, and the three-dimensional graphene nanomaterial electrodes arranged in the processing unit are connected in parallel to each other and connected to the titanium electrodes through a power supply, and the power supply is a DC power supply. The invention uses the three-dimensional graphene as an electrode to improve the efficiency of the three-dimensional graphene in treating organic matter by applying voltage, the decolorization rate can reach 98%-100%, and the TOC removal rate can reach more than 96%.
Description
技术领域technical field
本发明属于废水净化领域，涉及一种处理高浓度有机废水的三维石墨烯纳米材料电化学反应器。The invention belongs to the field of wastewater purification, and relates to a three-dimensional graphene nanomaterial electrochemical reactor for treating high-concentration organic wastewater.
背景技术Background technique
高浓度有机废水一般是指由造纸、皮革及食品等行业排出的COD在2000mg/L以上的废水。这种废水的成分非常的复杂、毒性强，在自然环境中难于光降解和生物降解，对生物以及环境造成很大的危害，如果直接排放，会造成严重的水环境污染，因此对染料废水的处理得到了广泛的重视。一般处理方法有：混凝法、氧化－吸附法、焚烧法、萃取法、湿式催化氧化法、电化学法和膜分离法、化学氧化法、电解法、光降解法、生物降解法等。其中吸附被认为是去除水中污染物非常有效的方法，并且它消耗的能源低，是环境友好型的方法。High-concentration organic wastewater generally refers to wastewater with COD above 2000mg/L discharged from papermaking, leather and food industries. The composition of this wastewater is very complex and highly toxic. It is difficult to photodegrade and biodegrade in the natural environment, causing great harm to organisms and the environment. If it is discharged directly, it will cause serious water pollution. Therefore, the dye wastewater Processing has received extensive attention. The general treatment methods are: coagulation method, oxidation-adsorption method, incineration method, extraction method, wet catalytic oxidation method, electrochemical method and membrane separation method, chemical oxidation method, electrolysis method, photodegradation method, biodegradation method, etc. Among them, adsorption is considered to be a very effective method for removing pollutants in water, and it consumes low energy, which is an environmentally friendly method.
石墨烯是碳原子按六边形晶格整齐排布而成的碳单质，具有蜂窝状品格结构的新型二维晶体碳纳米材料。基于它的化学结构，石墨烯具有许多独特的物理化学性质。例如石墨烯具有高比表面积，高吸附能力，表面也富含π电子可以与芳香结构的有机物形成强烈的π键作用，所以在水处理领域中得到了广泛的关注。但是由于二维石墨烯材料在水溶液中是悬浮性的，难以分离，容易造成二次污染，如用传统的过滤的方法分离，会造成滤器的堵塞和石墨烯材料的流失。Graphene is a simple carbon substance in which carbon atoms are neatly arranged in a hexagonal lattice, and a new two-dimensional crystalline carbon nanomaterial with a honeycomb lattice structure. Based on its chemical structure, graphene has many unique physicochemical properties. For example, graphene has a high specific surface area, high adsorption capacity, and the surface is also rich in π electrons, which can form a strong π bond with organic compounds with aromatic structures, so it has received extensive attention in the field of water treatment. However, because the two-dimensional graphene material is suspended in the aqueous solution, it is difficult to separate, and it is easy to cause secondary pollution. If the traditional filtration method is used for separation, the filter will be blocked and the graphene material will be lost.
中国专利文献CN101812702A(申请号：201010168663.6)公开了一种三相三维电化学反应器。该三相三维电化学反应器,包括电解槽,所述电解槽设有阳极电极、两个阴极电极和工作电极,所述工作电极为导电的活性炭与经过绝缘处理的活性炭的混合物,导电性的活性炭与经过绝缘处理的活性炭质量比为1∶4～4∶1；所述工作电极负载微生物,形成生物膜。但是，上述专利文献公开的电化学反应器电极为活性炭材质，电化学处理效果不佳，而且电极与废水的接触面积小，不能充分的与废水电化学反应。Chinese patent document CN101812702A (application number: 201010168663.6) discloses a three-phase three-dimensional electrochemical reactor. The three-phase three-dimensional electrochemical reactor includes an electrolytic cell, and the electrolytic cell is provided with an anode electrode, two cathode electrodes and a working electrode, and the working electrode is a mixture of conductive activated carbon and insulating-treated activated carbon, and the conductive The mass ratio of activated carbon to activated carbon treated with insulation is 1:4 to 4:1; the working electrode is loaded with microorganisms to form a biofilm. However, the electrode of the electrochemical reactor disclosed in the above-mentioned patent document is made of activated carbon, and the electrochemical treatment effect is not good, and the contact area between the electrode and the wastewater is small, and the electrochemical reaction with the wastewater cannot be fully performed.
发明内容Contents of the invention
针对现有技术的不足，本发明提供一种处理高浓度有机废水的三维石墨烯纳米材料电化学反应器。Aiming at the deficiencies of the prior art, the present invention provides a three-dimensional graphene nanomaterial electrochemical reactor for treating high-concentration organic wastewater.
本发明的技术方案如下：Technical scheme of the present invention is as follows:
一种处理高浓度有机废水的三维石墨烯纳米材料电化学反应器，该反应器包括密闭的反应器本体，所述的反应器本体交错竖直设置有隔板，所述的隔板将反应器本体分割成多个处理单元，所述的处理单元中设置有夹槽，所述的夹槽中设置有三维石墨烯纳米材料电极，所述的反应器本体的内部顶端设置有钛电极，所述的反应器本体的一侧上部设置有进水口，所述的反应器本体与进水口相对的一侧的下部设置有出水口，所述的设置在处理单元中的三维石墨烯纳米材料电极彼此并联且通过电源和钛电极连接，所述的电源为直流电源；A three-dimensional graphene nanomaterial electrochemical reactor for treating high-concentration organic wastewater, the reactor includes a closed reactor body, and the reactor body is staggered and vertically provided with partitions, and the partitions connect the reactor The body is divided into a plurality of processing units, the processing unit is provided with a clamping groove, and the three-dimensional graphene nanomaterial electrode is arranged in the clamping groove, and the inner top of the reactor body is provided with a titanium electrode. The upper part of one side of the reactor body is provided with a water inlet, and the lower part of the opposite side of the reactor body to the water inlet is provided with a water outlet, and the three-dimensional graphene nanomaterial electrodes arranged in the processing unit are connected in parallel And the titanium electrode is connected through a power supply, and the power supply is a DC power supply;
所述的三维石墨烯纳米材料电极按如下方法制备得到：将浓度为1～1.5mg/ml的氧化石墨烯溶液超声10～30min后，加入氧化石墨烯溶液质量的0.5％～2％的抗坏血酸，再超声5～10min形成均一溶液，85～95℃的条件下加热1～1.5h；清洗，冷却，干燥，即得。The three-dimensional graphene nanomaterial electrode is prepared as follows: after ultrasonicating the graphene oxide solution with a concentration of 1 to 1.5 mg/ml for 10 to 30 minutes, add ascorbic acid of 0.5% to 2% of the mass of the graphene oxide solution, Sonicate again for 5-10 minutes to form a homogeneous solution, heat at 85-95° C. for 1-1.5 hours; wash, cool, and dry to obtain the product.
根据本发明，优选的，所述的反应器本体长35～50cm、高30～40cm、宽15～30cm。According to the present invention, preferably, the reactor body is 35-50 cm long, 30-40 cm high, and 15-30 cm wide.
根据本发明，优选的，所述的隔板的个数为2～5块。According to the present invention, preferably, the number of the separators is 2-5.
根据本发明，优选的，所述的夹槽的高度为20～30cm，夹槽与反应器本体底部的间距为5cm。According to the present invention, preferably, the height of the clamping groove is 20-30 cm, and the distance between the clamping groove and the bottom of the reactor body is 5 cm.
根据本发明，优选的，所述的电源电压为0.5～1.5V。According to the present invention, preferably, the power supply voltage is 0.5-1.5V.
根据本发明，优选的，所述的三维石墨烯纳米材料电极的制备方法中，氧化石墨烯溶液的浓度为1.2～1.5mg/ml，抗坏血酸的加入量为氧化石墨烯溶液质量的1％～1.5％，清洗方式为透析的方式，冷却温度为-10～-20℃，干燥方式为在-40～-50℃的真空冷冻干燥仪器中干燥24～48h。According to the present invention, preferably, in the preparation method of the three-dimensional graphene nanomaterial electrode, the concentration of the graphene oxide solution is 1.2 to 1.5 mg/ml, and the amount of ascorbic acid added is 1% to 1.5 mg/ml of the mass of the graphene oxide solution. %, the cleaning method is dialysis, the cooling temperature is -10~-20°C, and the drying method is drying in a vacuum freeze-drying apparatus at -40~-50°C for 24~48h.
本发明三维石墨烯纳米材料的形状可根据不从的需要制作成不同的形状，优选长方体状。制备时，将加入抗坏血酸的氧化石墨烯溶液放入所需形状的容器中反应后，清洗，冷却，干燥，即可得到所需形状的三维石墨烯纳米材料电极。The shape of the three-dimensional graphene nanomaterial of the present invention can be made into different shapes according to different needs, preferably cuboid shape. During preparation, the graphene oxide solution added with ascorbic acid is put into a container of a desired shape for reaction, and then cleaned, cooled and dried to obtain a three-dimensional graphene nanomaterial electrode of a desired shape.
本发明将氧化石墨烯和抗坏血酸反应，通过石墨烯碳原子层内π-π堆积作用，以及疏水作用，制成三维石墨烯材料，三维石墨烯吸附有机物的同时，利用电化学原理对有机物进行处理。The present invention reacts graphene oxide and ascorbic acid, through the π-π stacking effect in the graphene carbon atomic layer, and the hydrophobic effect, to make a three-dimensional graphene material. While the three-dimensional graphene absorbs organic matter, it uses electrochemical principles to treat organic matter. .
本发明的有益效果：Beneficial effects of the present invention:
1、本发明的三维石墨烯纳米材料电极不但具有高比表面积，并且还易于与水分离不会造成二次污染，可以替代石墨烯来用于有机废水的处理。1. The three-dimensional graphene nanomaterial electrode of the present invention not only has a high specific surface area, but also is easy to separate from water without causing secondary pollution, and can replace graphene for the treatment of organic wastewater.
2、石墨烯中电子的运动速率达到了光速的1/300，远超过了电子在一般导体中的运动速度，利用这一特性本发明将三维石墨烯作为电极通过施加电压来提高三维石墨烯处理有机物的效率，脱色率可达98％～100％、TOC量去除率可达96％以上。2. The movement speed of electrons in graphene has reached 1/300 of the speed of light, far exceeding the movement speed of electrons in general conductors. Using this characteristic, the present invention uses three-dimensional graphene as an electrode to improve the three-dimensional graphene processing by applying voltage. The efficiency of organic matter, the decolorization rate can reach 98% to 100%, and the removal rate of TOC can reach more than 96%.
3、本发明以氧化石墨烯作为原材料，成本低廉，通入低的电压(仅0.5～1.5V)能起到很好的去除效果，能耗低。3. The present invention uses graphene oxide as a raw material, which is low in cost, and a low voltage (only 0.5-1.5V) can be applied to achieve a good removal effect and low energy consumption.
4、本发明三维石墨烯材料电极韧性强、不易破碎，反应器稳定性好，处理效率高，出水水质稳定，流程简单，设备紧凑，占地面积小，经济可行、无二次污染易、实现自动控制，运行管理简单。4. The three-dimensional graphene material electrode of the present invention has strong toughness, is not easy to break, has good reactor stability, high treatment efficiency, stable effluent quality, simple process, compact equipment, small footprint, economical feasibility, no secondary pollution and easy realization. Automatic control, simple operation and management.
附图说明Description of drawings
图1为本发明实施例1三维石墨烯纳米材料电化学反应器的主体结构示意图。Fig. 1 is a schematic diagram of the main structure of a three-dimensional graphene nanomaterial electrochemical reactor in Example 1 of the present invention.
图2为本发明实施例1三维石墨烯纳米材料电化学反应器的侧视图。Fig. 2 is a side view of the three-dimensional graphene nanomaterial electrochemical reactor in Example 1 of the present invention.
图3为本发明实施例1三维石墨烯纳米材料电化学反应器的俯视图。3 is a top view of the three-dimensional graphene nanomaterial electrochemical reactor in Example 1 of the present invention.
其中，1、反应器本体，2、隔板，3、夹槽，4、三维石墨烯纳米材料电极，5、钛电极，6、进水口，7、出水口，8、电源，9、泵。Among them, 1. Reactor body, 2. Separator, 3. Gutter, 4. Three-dimensional graphene nanomaterial electrode, 5. Titanium electrode, 6. Water inlet, 7. Water outlet, 8. Power supply, 9. Pump.
具体实施方式detailed description
下面通过具体实施例对本发明做进一步说明，但不限于此。The present invention will be further described below through specific examples, but not limited thereto.
实施例1Example 1
一种处理高浓度有机废水的三维石墨烯纳米材料电化学反应器，该反应器包括密闭的反应器本体1，所述的反应器本体1交错竖直设置有隔板2，所述的隔板2将反应器本体1分割成多个处理单元，所述的处理单元中设置有夹槽3，所述的夹槽3中设置有三维石墨烯纳米材料电极4，所述的反应器本体1的内部顶端设置有钛电极5，所述的反应器本体1的一侧上部设置有进水口6，所述的反应器本体1与进水口6相对的一侧的下部设置有出水口7，所述的设置在处理单元中的三维石墨烯纳米材料电极4彼此并联且通过电源8和钛电极5连接，所述的电源8为直流电源；A three-dimensional graphene nanomaterial electrochemical reactor for treating high-concentration organic wastewater, the reactor includes a closed reactor body 1, and the reactor body 1 is staggered and vertically provided with partitions 2, and the partitions 2 The reactor body 1 is divided into a plurality of processing units, the processing unit is provided with a clamping groove 3, and the three-dimensional graphene nanomaterial electrode 4 is arranged in the clamping groove 3, and the reactor body 1 A titanium electrode 5 is provided at the top of the interior, a water inlet 6 is provided at the upper part of one side of the reactor body 1, and a water outlet 7 is provided at the lower part of the opposite side of the reactor body 1 to the water inlet 6. The three-dimensional graphene nanomaterial electrodes 4 arranged in the processing unit are connected in parallel with each other and connected with the titanium electrode 5 through a power supply 8, and the power supply 8 is a DC power supply;
所述的三维石墨烯纳米材料电极4按如下方法制备得到：将浓度为1.5mg/ml的氧化石墨烯溶液超声30min后，加入氧化石墨烯溶液质量的2％的抗坏血酸，再超声10min形成均一溶液，90℃的条件下加热1h；通过透析的方式清洗，冷却至-20℃，在-50℃的真空冷冻干燥仪器中干燥24h，即得。The three-dimensional graphene nanomaterial electrode 4 is prepared according to the following method: after supersonicating the graphene oxide solution with a concentration of 1.5 mg/ml for 30 minutes, adding 2% ascorbic acid of the mass of the graphene oxide solution, and then supersonicating for 10 minutes to form a homogeneous solution , heated at 90°C for 1h; washed by dialysis, cooled to -20°C, and dried in a vacuum freeze-drying apparatus at -50°C for 24h to obtain the obtained product.
本实施例中反应器本体1长36cm、高30cm、宽15cm，隔板2的个数为2块，夹槽3的高度为20cm，夹槽3与反应器本体1底部的间距为5cm；三维石墨烯纳米材料电极4的形状为长方体，钛电极5为钛金属板，电源电压为1.2V。In the present embodiment, the reactor body 1 is 36cm long, 30cm high, and 15cm wide. The number of partitions 2 is 2, the height of the clamping groove 3 is 20cm, and the distance between the clamping groove 3 and the bottom of the reactor body 1 is 5cm; three-dimensional The shape of the graphene nanomaterial electrode 4 is a cuboid, the titanium electrode 5 is a titanium metal plate, and the power supply voltage is 1.2V.
本实施例的三维石墨烯纳米材料电化学反应器使用时，关闭反应器的出水口7，用泵9将高浓度有机废水从进水口6泵入到反应器中，开通电源8，三维石墨烯纳米材料电极4对高浓度有机废水进行电化学处理，处理完成后，打开出水口7，即完成对高浓度有机废水的电化学处理。When the three-dimensional graphene nanomaterial electrochemical reactor of the present embodiment is in use, the water outlet 7 of the reactor is closed, and the high-concentration organic wastewater is pumped into the reactor from the water inlet 6 with a pump 9, and the power supply 8 is turned on, and the three-dimensional graphene The nanomaterial electrode 4 performs electrochemical treatment on the high-concentration organic wastewater. After the treatment is completed, the water outlet 7 is opened to complete the electrochemical treatment of the high-concentration organic wastewater.
实验例1Experimental example 1
利用实施例1的三维石墨烯纳米材料电化学反应器对酸性红27(Acid Red27)高浓度有机废水电化学处理，Acid Red27高浓度有机废水的原始指标为Acid red27：2000mg/L、总有机碳含量(TOC)720mg/L。Utilize the three-dimensional graphene nano material electrochemical reactor of embodiment 1 to acid red 27 (Acid Red27) high-concentration organic waste water electrochemical treatment, the original index of Acid Red27 high-concentration organic waste water is Acid red27: 2000mg/L, total organic carbon Content (TOC) 720mg/L.
步骤如下：Proceed as follows:
关闭反应器的出水口7，用泵9将Acid Red27高浓度有机废水从进水口6泵入到反应器中，开通电源8(电源电压1.2V)，三维石墨烯纳米材料电极4对Acid Red27高浓度有机废水进行电化学处理1h，处理完成后，打开出水口7，在出水口7收集出水并测脱色率、TOC量，并且同Acid Red27高浓度有机废水的原始指标比较计算其脱色率以及TOC去除率。Close the water outlet 7 of the reactor, pump Acid Red27 high-concentration organic waste water into the reactor from the water inlet 6 with the pump 9, turn on the power supply 8 (power supply voltage 1.2V), and the three-dimensional graphene nanomaterial electrode 4 is high to Acid Red27 Concentrated organic wastewater is electrochemically treated for 1 hour. After the treatment is completed, open the water outlet 7, collect the effluent at the water outlet 7 and measure the decolorization rate and TOC amount, and compare it with the original index of Acid Red27 high-concentration organic wastewater to calculate its decolorization rate and TOC removal rate.
经计算，在施加1.2V的恒电压的条件下处理1h，Acid Red27高浓度有机废水脱色率为100％，TOC量去除率为99％。It is calculated that the decolorization rate of Acid Red27 high-concentration organic wastewater is 100%, and the removal rate of TOC is 99% under the condition of applying a constant voltage of 1.2V for 1 hour.
实施例2Example 2
如实施例1所述的三维石墨烯纳米材料电化学反应器，不同的是反应器本体1长40cm、高35cm、宽20cm，隔板2的个数为3块，夹槽3的高度为25cm，夹槽3与反应器本体1底部的间距为5cm；三维石墨烯纳米材料电极4的形状为长方体，钛电极5为钛金属板，电源电压为0.6V。The three-dimensional graphene nanomaterial electrochemical reactor as described in Example 1, the difference is that the reactor body 1 is 40cm long, 35cm high, and 20cm wide, the number of separators 2 is 3, and the height of the clamping groove 3 is 25cm , the distance between the clamp groove 3 and the bottom of the reactor body 1 is 5cm; the shape of the three-dimensional graphene nanomaterial electrode 4 is a cuboid, the titanium electrode 5 is a titanium metal plate, and the power supply voltage is 0.6V.
实施例3Example 3
如实施例1所述的三维石墨烯纳米材料电化学反应器，不同的是反应器本体1长50cm、高40cm、宽30cm，隔板2的个数为5块，夹槽3的高度为30cm，夹槽3与反应器本体1底部的间距为5cm；三维石墨烯纳米材料电极4的形状为长方体，钛电极5为钛金属板，电源电压为1.0V。The three-dimensional graphene nanomaterial electrochemical reactor as described in Example 1, the difference is that the reactor body 1 is 50cm long, 40cm high, and 30cm wide, the number of separators 2 is 5, and the height of the clamping groove 3 is 30cm , the distance between the clamp groove 3 and the bottom of the reactor body 1 is 5cm; the shape of the three-dimensional graphene nanomaterial electrode 4 is a cuboid, the titanium electrode 5 is a titanium metal plate, and the power supply voltage is 1.0V.
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