CN105948180A - Modified graphite electrode and method for using same as anode for electrochemical treatment of dye wastewater - Google Patents
Modified graphite electrode and method for using same as anode for electrochemical treatment of dye wastewater Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000002351 wastewater Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 19
- 239000010439 graphite Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000010919 dye waste Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 21
- 239000012153 distilled water Substances 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 230000015556 catabolic process Effects 0.000 claims description 4
- 238000006731 degradation reaction Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000029087 digestion Effects 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000006174 pH buffer Substances 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 1
- 239000000975 dye Substances 0.000 description 18
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000006179 pH buffering agent Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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Abstract
本发明公开了一种改性石墨电极及作阳极电化学处理染料废水的方法，通过对石墨电极的预处理，然后将CO2O3与经3‑氨丙基三甲氧基硅烷改性后的MCM‑41(NH2‑MCM‑41)的混合物与电极混合，再经烘烤、冲洗，确定CO2O3与NH2‑MCM‑41的混合物黏结到石墨电极上。本发明制备的改性石墨电极CO2O3‑NH2‑MCM‑41/C作电化学处理的阳极，降低了生产成本，在适应不同的酸碱度环境的染料废水的同时，提高了利用电化学方法处理染料废水的效率和产率，尤其是在偏碱性环境下。
The invention discloses a modified graphite electrode and a method for electrochemically treating dye waste water as an anode. Through pretreatment of the graphite electrode, CO2O3 and 3 -aminopropyltrimethoxysilane modified The mixture of MCM‑41 (NH 2 ‑MCM‑41) was mixed with the electrode, and then baked and rinsed to confirm that the mixture of C O2 O 3 and NH 2 ‑MCM‑41 was bonded to the graphite electrode. The modified graphite electrode C O2 O 3 ‑NH 2 ‑MCM‑41/C prepared by the present invention is used as an anode for electrochemical treatment, which reduces the production cost, and improves the utilization of electrochemical wastewater while adapting to dye wastewater in different pH environments. The efficiency and yield of the method for treating dye wastewater, especially in an alkaline environment.
Description
技术领域technical field
本发明涉及一种改性石墨电极，具体涉及一种改性石墨电极及作阳极电化学处理染料废水的方法。The invention relates to a modified graphite electrode, in particular to a modified graphite electrode and a method for electrochemically treating dye wastewater as an anode.
背景技术Background technique
随着工业生产和人类社会的迅猛发展，环境污染问题日益加重，尤其是工业废水中有毒有害物质的量和种类数都在飞速增加，严重制约人类社会的可持续发展。染料废水占工业废水的比重很大，具有污染物的浓度高、色度大、毒性强、成分复杂、可生化性很差以及处理难度极大等特点，传统的生物处理技术很难有效的处理工业染料废水。With the rapid development of industrial production and human society, the problem of environmental pollution is becoming more and more serious, especially the amount and types of toxic and harmful substances in industrial wastewater are increasing rapidly, which seriously restricts the sustainable development of human society. Dye wastewater accounts for a large proportion of industrial wastewater. It has the characteristics of high concentration of pollutants, large chroma, strong toxicity, complex composition, poor biodegradability and extremely difficult treatment. Traditional biological treatment technology is difficult to effectively treat Industrial dye wastewater.
由于染料废水具有高COD、高盐等特点，常规方法难以处理，因此引入电化学方法氧化处理染料废水，其原理是在电化学阳极发生阳极氧化反应，将污染物转换为无机的无害无毒物质。电化学催化氧化技术，其运行指标主要为电位与电流，便于实现自动化全程检测，而且可以避免二次污染物的产生，设备简单，能耗低。Due to the characteristics of high COD and high salt in dye wastewater, conventional methods are difficult to treat, so an electrochemical method is introduced to oxidize dye wastewater. The principle is that an anodic oxidation reaction occurs at the electrochemical anode to convert pollutants into inorganic harmless and non-toxic substance. Electrochemical catalytic oxidation technology, its operating indicators are mainly potential and current, which is convenient for automatic whole-process detection, and can avoid the generation of secondary pollutants, with simple equipment and low energy consumption.
然而，在将电化学催化氧化技术广泛应用到实践中依然存在一些问题，比如电化学催化氧化水处理技术中的很多反应途径依然处于假设和推测阶段，很多降解机理方面的问题依然需要更加深入的研究和探索，其中最重要的影响因素是阳极材料的选取。However, there are still some problems in the widespread application of electrochemical catalytic oxidation technology in practice. For example, many reaction pathways in electrochemical catalytic oxidation water treatment technology are still in the hypothetical and speculative stage, and many problems in degradation mechanism still need more in-depth research. Research and exploration, the most important factor is the selection of anode materials.
在实际应用中，染料废水的酸碱环境不特定，提高适用废酸酸碱环境且能够进一步提高废水中染料的去除率的电化学阳极电极材料有待研究。In practical application, the acid-base environment of dye wastewater is not specific, and the electrochemical anode electrode materials that can improve the acid-base environment of waste acid and further improve the removal rate of dye in wastewater need to be studied.
发明内容Contents of the invention
为解决现有技术的不足，本发明的目的在于提供一种改性石墨电极作为电化学处理的阳极应用在不同的酸碱度环境的染料废水中，尤其是在偏碱性环境下，进一步提高电化学处理染料废水的效率和产率。In order to solve the deficiencies of the prior art, the purpose of the present invention is to provide a modified graphite electrode as an anode for electrochemical treatment in dye wastewater with different pH environments, especially in alkaline environments, to further improve the electrochemical treatment. Efficiency and yield in treating dye wastewater.
为了实现上述目标，本发明采用如下的技术方案：In order to achieve the above object, the present invention adopts the following technical solutions:
一种改性石墨电极的制备方法，包括以下步骤：A preparation method for a modified graphite electrode, comprising the following steps:
A1、取若干石墨电极，砂纸打磨表面光滑平整，依次放入NaOH溶液和盐酸溶液中浸泡，冲洗并干燥，制得预备石墨电极；A1. Take a number of graphite electrodes, sand the surface smooth and flat, put them into NaOH solution and hydrochloric acid solution for soaking, rinse and dry, and prepare graphite electrodes;
A2、将MCM-41和3-氨丙基三甲氧基硅烷混入正己烷中，常温冷凝、过滤、冲洗、干燥后，制得NH2-MCM-41粉末；A2. Mix MCM-41 and 3-aminopropyltrimethoxysilane into n-hexane, condense at room temperature, filter, rinse, and dry to obtain NH 2 -MCM-41 powder;
A3、将上述NH2-MCM-41粉末和粉末混合溶于蒸馏水，封入反应釜内芯后，放置烘箱内烘烤，取出后过滤、冲洗、自然烘干，制得粉末；A3, the above NH 2 -MCM-41 powder and The powder is mixed and dissolved in distilled water, sealed in the inner core of the reaction kettle, placed in an oven to bake, filtered, rinsed and dried naturally after taking out to obtain powder;
A4、将制备好的粉末和聚环氧乙烷溶解于蒸馏水中，搅拌均匀，制得混合溶液，将步骤A1制得的预备石墨电极置于上述混合溶液中，经超声消解仪震动后自然干燥，制得改性石墨电极。A4, the prepared The powder and polyethylene oxide were dissolved in distilled water and stirred evenly to obtain a mixed solution. The prepared graphite electrode prepared in step A1 was placed in the above mixed solution and dried naturally after being vibrated by an ultrasonic digestion apparatus to obtain Modified graphite electrodes.
上述石墨电极为2cm×2cm，所述NaOH溶液为2-4mol/L，浸泡时间为60min，所述盐酸溶液为1-2mol/L，浸泡时间为20-30min，冲洗液为蒸馏水。The graphite electrode is 2cm×2cm, the NaOH solution is 2-4mol/L, soaking time is 60min, the hydrochloric acid solution is 1-2mol/L, soaking time is 20-30min, and the rinse solution is distilled water.
上述步骤A2中MCM-41为2.5-4g，3-氨丙基三甲氧基硅烷为2.5-4g，正己烷为50-80ml，所述冷凝时间为6-8h，冲洗液为正己烷，所述干燥温度为105℃，干燥时间为24h。In the above step A2, MCM-41 is 2.5-4g, 3-aminopropyltrimethoxysilane is 2.5-4g, n-hexane is 50-80ml, the condensation time is 6-8h, and the flushing liquid is n-hexane. The drying temperature is 105°C and the drying time is 24h.
上步骤A3中NH2-MCM-41粉末为1-2g,粉末为1-2g,蒸馏水80ml,所述烘箱温度为105℃，烘干时间10h。The NH 2 -MCM-41 powder in step A3 is 1-2g, The powder is 1-2g, distilled water is 80ml, the oven temperature is 105°C, and the drying time is 10h.
上述步骤A4中粉末为0.5g,聚环氧乙烷为0.1g,蒸馏水20ml,所述震动时间为20-40min。In step A4 above Powder is 0.5g, polyethylene oxide is 0.1g, distilled water is 20ml, and the shaking time is 20-40min.
基于上述的改性石墨电极作阳极电化学处理染料废水的方法，包括以下步骤：Based on above-mentioned modified graphite electrode, make the method for anode electrochemical treatment of dye wastewater, comprising the following steps:
B1、将染料加入蒸馏水中，形成溶液A；B1, adding the dye to distilled water to form solution A;
B2、采用盐酸或氢氧化钠作pH缓冲剂，调节溶液A的pH值，制得溶液B；B2. Using hydrochloric acid or sodium hydroxide as a pH buffer to adjust the pH value of solution A to prepare solution B;
B3、将上述步骤A4制得的改性石墨电极作为阳极，以铂电极或石墨电极作阴极，放入溶液B中，连接电源后降解染料。B3. The modified graphite electrode prepared in the above step A4 is used as an anode, and a platinum electrode or a graphite electrode is used as a cathode, put into solution B, and degrade the dye after connecting to a power source.
上述步骤B1中染料为0.2g酸性红,所述蒸馏水为2000ml。In the above step B1, the dye is 0.2g acid red, and the distilled water is 2000ml.
上述步骤B2中PH值为3-9。The pH value in the above step B2 is 3-9.
优选的，上述步骤B2中的PH值为7。Preferably, the pH value in the above step B2 is 7.
上述步骤B3中电源电压为5V，降解时间为2h。In the above step B3, the power supply voltage is 5V, and the degradation time is 2h.
本发明的有益之处在于：本发明提供的一种改性石墨电极的制备方法通过对石墨电极的改性，增加石墨电极的比表面积，提升电极的催化活性、氧化性等，从而提高对染料废水的降解速度和去除效率，克服了现有的电化学氧化染料废水处理时间较长、出料效果不高等缺陷；降低了生产成本，进一步提高改性石墨电极在碱性环境下对废水中染料的去除率，扩大了实际应用范围，尤其是在偏碱性的染料废水的环境下。The benefit of the present invention is that: the preparation method of a modified graphite electrode provided by the present invention increases the specific surface area of the graphite electrode by modifying the graphite electrode, improves the catalytic activity, oxidation, etc. of the electrode, thereby improving the dye The degradation speed and removal efficiency of wastewater overcome the defects of the existing electrochemical oxidation dye wastewater, such as long treatment time and low discharge effect; reduce production costs, and further improve the effect of modified graphite electrodes on dyes in wastewater in an alkaline environment. The removal rate has expanded the scope of practical application, especially in the environment of alkaline dye wastewater.
附图说明Description of drawings
图1为本发明的一种改性石墨电极的制备工艺流程示意图。Fig. 1 is a schematic diagram of the preparation process of a modified graphite electrode of the present invention.
具体实施方式detailed description
以下结合附图和具体实施例对本发明作具体的介绍。The present invention will be specifically introduced below in conjunction with the accompanying drawings and specific embodiments.
一种改性石墨电极的制备方法，其特征在于，包括以下步骤：A kind of preparation method of modified graphite electrode is characterized in that, comprises the following steps:
A1、取2cm×2cm的石墨电极，砂纸打磨表面至光滑平整，依次放入2mol/L NaOH溶液中浸泡60min，再放入1mol/L的盐酸溶液中浸泡20min，蒸馏水冲洗并干燥，制得预备石墨电极；A1. Take a 2cm×2cm graphite electrode, grind the surface with sandpaper until it is smooth, put it into 2mol/L NaOH solution for 60min, then put it into 1mol/L hydrochloric acid solution for 20min, wash it with distilled water and dry it to prepare the preparation Graphite electrode;
A2、将2.5g MCM-41和2.5g 3-氨丙基三甲氧基硅烷混入50mL正己烷中，常温冷凝6h、过滤，用正己烷冲洗后放入烘箱在105℃下干燥24h，制得NH2-MCM-41粉末；A2. Mix 2.5g of MCM-41 and 2.5g of 3-aminopropyltrimethoxysilane into 50mL of n-hexane, condense at room temperature for 6h, filter, rinse with n-hexane and dry in an oven at 105°C for 24h to obtain NH 2 - MCM-41 powder;
A3、将1g NH2-MCM-41粉末和1g粉末混合溶于80ml蒸馏水，封入反应釜内芯，放置烘箱内105℃下烘烤10h后过滤，蒸馏水冲洗三次后自然烘干，制得粉末；A3, 1g NH 2 -MCM-41 powder and 1g The powder is mixed and dissolved in 80ml of distilled water, sealed into the inner core of the reactor, placed in an oven, baked at 105°C for 10 hours, filtered, rinsed with distilled water three times, and dried naturally to obtain powder;
A4、将0.5g制备好的粉末和0.1聚环氧乙烷溶解于20mL蒸馏水中，搅拌均匀，制得混合溶液，将步骤A1制得的预备石墨电极置于上述混合溶液中，经超声消解仪震动20min后自然干燥，制得改性石墨电极。A4. Prepare 0.5g Dissolve the powder and 0.1 polyethylene oxide in 20mL of distilled water, stir evenly to prepare a mixed solution, place the prepared graphite electrode prepared in step A1 in the above mixed solution, vibrate for 20 minutes with an ultrasonic digestion apparatus, and then dry naturally to obtain Modified graphite electrodes.
碱洗可除石墨片表面的油类杂质。Alkali washing can remove oil impurities on the surface of graphite sheet.
酸洗可增强石墨表面粗糙度，使得改性负载物的负载更加容易。Acid washing can enhance the surface roughness of graphite, making loading of modified supports easier.
以上述制备的改性石墨电极作阳极电化学处理染料废水的方法，包括以下步骤：The method for electrochemically treating dye wastewater with the modified graphite electrode prepared above as an anode comprises the following steps:
B1、将酸性红加入蒸馏水中，制备300mL100mg/L的酸性红模拟废水；B1, add acid red into distilled water, prepare 300mL100mg/L acid red simulated waste water;
B2、采用盐酸或氢氧化钠作pH缓冲剂，调节上述模拟废水的pH值分别为3、5、7、9，制得溶液B3、B5、B7、B9；B2. Using hydrochloric acid or sodium hydroxide as a pH buffering agent, adjust the pH values of the above-mentioned simulated wastewater to 3, 5, 7, and 9 respectively to prepare solutions B 3 , B 5 , B 7 , and B 9 ;
B3、将步骤A4制得的改性石墨电极作为阳极，以铂电极作阴极，放入上述溶液B3、B5、B7、B9中，连接5V电源后降解2h该模拟废水。B3. Put the modified graphite electrode prepared in step A4 as the anode and the platinum electrode as the cathode, put them into the above solutions B 3 , B 5 , B 7 , and B 9 , and degrade the simulated wastewater for 2 hours after connecting to a 5V power supply.
上述实施例中制备的改性石墨电极对酸性红模拟废水降解有机污染物的去除能力如表1所示：The modified graphite electrode prepared in the above-mentioned embodiment is as shown in table 1 to the removal ability of acid red simulated wastewater degrading organic pollutants:
表1Table 1
由表1可见，调节模拟废水的pH分别为3、5、7、9，相应的酸性红的去除率分别为82.81％，97.34％，99.52％，92.37％；在pH为7的时候，酸性红的去除率最高。It can be seen from Table 1 that the pH of the simulated wastewater is adjusted to be 3, 5, 7, and 9 respectively, and the corresponding removal rates of acid red are 82.81%, 97.34%, 99.52%, and 92.37% respectively; highest removal rate.
以上显示和描述了本发明的基本原理、主要特征和优点。本行业的技术人员应该了解，上述实施例不以任何形式限制本发明，凡采用等同替换或等效变换的方式所获得的技术方案，均落在本发明的保护范围内。The basic principles, main features and advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the above-mentioned embodiments do not limit the present invention in any form, and all technical solutions obtained by means of equivalent replacement or equivalent transformation fall within the protection scope of the present invention.
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