CN104843911A - Method for degrading malachite green waste water - Google Patents
Method for degrading malachite green waste water Download PDFInfo
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- CN104843911A CN104843911A CN201510223264.8A CN201510223264A CN104843911A CN 104843911 A CN104843911 A CN 104843911A CN 201510223264 A CN201510223264 A CN 201510223264A CN 104843911 A CN104843911 A CN 104843911A
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Abstract
The invention discloses a method for degrading the malachite green waste water. The malachite green is degraded through oxidation after reduction, the malachite green can be reduced into the leucomalachite green to be precipitated in a short five hours, and accordingly a COD (Chemical Oxygen Demand) value of the waste water is reduced, meanwhile the chemical raw material leucomalachite green is obtained, malachite green large molecules are decomposed into small molecules of pollutants, and the further degradation of the malachite green is facilitated and the malachite green waste water which is not fully degraded is oxidized by an oxidation method and accordingly the degradation time is reduced and the energy consumption of the electrolysis is reduced.
Description
Technical field
The invention belongs to field of environment protection, particularly a kind of method of Victoria Green WPB waste water of degrading.
Background technology
Victoria Green WPB is a kind of organic dye, and soluble in water, the aqueous solution is blue-greenish colour, and industrial application is extensive, is mainly used in the dyeing of cotton, wool, gunny products, leather, ceramic etc.; In addition, Victoria Green WPB is remarkable to the killing effect of mould in fish body parasite and fish-egg etc., is thus also widely used in aquaculture.But Victoria Green WPB can produce toxicity to the fish in water body, shrimp, by food chain, the effects such as teratogenesis, carcinogenic, mutagenesis are produced to Mammals and the mankind, and promoter action is played to tumor growth, thus the biological accumulation of this material in land and aquatic ecosystem has impact to environment and human health.Therefore, Victoria Green WPB waste water is processed become the task of top priority.
The method of the degraded Victoria Green WPB of current research mainly comprises microbial method, absorption method, microwave method, photocatalytic method and Fenton reagent method etc., wherein with microbial method and photocatalytic degradation most study.Biological degradation to be mainly oxidized dye molecule by the related enzyme systems of microorganism or to reduce, destroy its chromophoric group or unsaturated link(age), make dye molecule finally be degraded to inorganics or become microorganism self need nutrition, Major degradation pathways is: Victoria Green WPB is after hydroxylation, and degraded generates michaelis ketone and phenol; In addition, Victoria Green WPB can also by demethylating reaction progressively, and degraded generates dimethylamino benzopheone and p-aminophenol, and dimethylamino benzopheone can by adding hydroxyl or demethylating reaction is progressively degraded further.The approach that photocatalysis degradation Victoria Green WPB is possible is central carbon atom and the hydroxyl radical free radical effect of Victoria Green WPB, the C-C bond rupture of central carbon atom generates 4-hydroxyl diethylin aniline and 4-dimethylamino benzophenone, the further ring-opening oxidation of these fragment molecules is P-hydroxybenzoic acid and phenylformic acid etc., the acidic substance of these band phenyl ring are further oxidized to oxalic acid again, butene dioic acid, the micromolecular acid such as formic acid.These methods easily produce poisonous phenols, aniline and letones in degradation process, degradation process is complicated, and reaction conditions is restive, meanwhile, in the reaction times longer (if photocatalytic degradation Victoria Green WPB is that micromolecular compound needs 40 hours), expend larger energy.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, there is provided a kind of method of Victoria Green WPB waste water of degrading, the method expends the degraded that less energy just can realize Victoria Green WPB, meanwhile, can also leucogentian violet be reclaimed, realize the recycling of Victoria Green WPB waste water.Leucogentian violet also claims leucomalachite green, is a kind of brown or pale blue green powder, can be used for Biochemical Research, do acid base indicator and developer, also may be used for the photometry of the mensuration of cerium, iridium and the hexacyanoferrate and gold, manganese.
The object of the invention is to be achieved through the following technical solutions: a kind of method of Victoria Green WPB waste water of degrading, the method comprises the following steps:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 10 ~ 40 DEG C, regulates pH to 4 ~ 10, the metal ion in precipitation solution, filters, obtain filtrate after 1 hour;
(3) filtrate after processing with step 2, for electrolytic solution, in three-electrode system, under the condition of-0.9 ~-1.2 V, reduces 5 hours, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation; By the electrolyte filtering after reduction, obtain leucogentian violet crystal; Wherein, reducing electrode adopts the one in Graphite Electrodes, Ti electrode, iron electrode, gold electrode, plating Ruthenium Ti electrode, copper electrode, nanolithographic silver electrode and wolfram varbide electrode;
(4) filtrate after step 3 is filtered is re-started electrochemical oxidation as electrolytic solution in three-electrode system, the oxidizing electrode adopted is the one in BDD electrode, gold electrode or nanosized platinum electrode, be be oxidized 5 hours under the condition of 1.0-1.3 V at oxidation voltage, remaining organism is degraded, the COD<60mg/L of waste water.
Beneficial effect of the present invention is: adopt the method degraded Victoria Green WPB of first reducing and reoxidizing, within shorter 5 hours, Victoria Green WPB can be reduced to leucogentian violet be precipitated out, while reducing the COD value of waste water, obtain industrial chemicals leucogentian violet, also make Victoria Green WPB macromole be decomposed into more micromolecular pollutent, be conducive to the further degraded of Victoria Green WPB; Then adopt the Victoria Green WPB waste water that oxidation style oxidation is not yet degradable, decrease degradation time, reduce electrolysis energy consumption.
Accompanying drawing explanation
Fig. 1 is the reaction principle schematic diagram of electrochemical reduction Victoria Green WPB;
Fig. 2 is the reaction principle schematic diagram of electrochemical oxidation Victoria Green WPB waste water.
Embodiment
The present invention is by Victoria Green WPB waste water, and after grid precipitation, regulator solution pH value, sedimentation and filtration removes the Fe (OH) generated in solution
2, Fe (OH)
3after throw out, electrochemical reduction Victoria Green WPB waste water in electrolyzer, until the leucogentian violet precipitation generating blue brown; Filtering-depositing, proceeds electrochemical oxidation, until Victoria Green WPB waste water is degraded further.As shown in Figure 1, easily there is de-electric charge hydrogenation electrochemical reducting reaction at negative electrode in Victoria Green WPB to the reaction path of electrochemical reduction Victoria Green WPB, generates precipitation, greatly reduce the COD value of solution, decreases electric energy and time that solution continues the consumption of electrochemical oxidation needs.
It should be noted that, the present invention is in the three-electrode system of electrochemical reduction, reference electrode can adopt saturated calomel electrode, can adopt platinum electrode to electrode, reducing electrode adopts the one in Graphite Electrodes, Ti electrode, iron electrode, gold electrode, plating Ruthenium Ti electrode, copper electrode, nanolithographic silver electrode and wolfram varbide electrode.In the three-electrode system of electrochemical oxidation, reference electrode can adopt saturated calomel electrode, can adopt platinum electrode to electrode, and oxidizing electrode can adopt the one in BDD electrode, gold electrode or nanosized platinum electrode.
Below in conjunction with embodiment, the invention will be further described; following examples are used for explaining and the present invention are described, instead of limit the invention, in the protection domain of spirit of the present invention and claim; the any amendment make the present invention and change, all fall into protection scope of the present invention.
Embodiment 1:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 15 DEG C, regulates pH to 4, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2 is for electrolytic solution, and employing Ti electrode is reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-0.9 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after filtration is re-started electrochemical oxidation, the oxidizing electrode of employing is BDD electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.0 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 60%, and the COD in the water after electrochemicial oxidation is 50 mg/L.
Embodiment 2:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 15 DEG C, regulates pH to 6, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2 is for electrolytic solution, and employing Ti electrode is reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.1 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is BDD electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.3 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 72%, and the COD in the water after electrochemicial oxidation is 50 mg/L.
Embodiment 3:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 25 DEG C, regulates pH to 7, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2 is for electrolytic solution, and employing Graphite Electrodes is reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.2V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is BDD electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.3 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 75%, and the COD in the water after electrochemicial oxidation is 45 mg/L.
Embodiment 4:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 30 DEG C, regulates pH to 8, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2 is for electrolytic solution, and employing gold electrode is reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.2 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is BDD electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.3V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 80%, and the COD in the water after electrochemicial oxidation is 45 mg/L.
Embodiment 5:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 30 DEG C, regulates pH to 9, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2 is for electrolytic solution, and adopt plating Ruthenium Ti electrode to be reducing electrode, adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.1 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is BDD electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.3V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 85%, and the COD in the water after electrochemicial oxidation is 45 mg/L.
Embodiment 6:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 30 DEG C, regulates pH to 9, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2, for electrolytic solution, adopts nanolithographic silver electrode to be reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.0 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is BDD electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.2 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 90%, and the COD in the water after electrochemicial oxidation is 40 mg/L.
Embodiment 7:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 35 DEG C, regulates pH to 9, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2, for electrolytic solution, adopts ferroelectric very reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.1 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is BDD electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.2 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 80%, and the COD in the water after electrochemicial oxidation is 40 mg/L.
Embodiment 8:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 40 DEG C, regulates pH to 9, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2 is for electrolytic solution, and employing gold electrode is reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.2 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain the waste water after leucogentian violet crystal and reduction;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is nanosized platinum electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.2 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 84%, and the COD in the water after electrochemicial oxidation is 35 mg/L.
Embodiment 9:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 30 DEG C, regulates pH to 10, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2, for electrolytic solution, adopts wolfram varbide electrode to be reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.2 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is nanosized platinum electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.2 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 85%, and the COD in the water after electrochemicial oxidation is 30 mg/L.
Embodiment 10:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 25 DEG C, regulates pH to 9, filters after 1 hour; Fe in waste water
2+, Fe
3+, Ca
2+deng formation precipitation, and being cut, being for further processing filtering the filtrate obtained;
(3) filtrate after processing with step 2, for electrolytic solution, adopts wolfram varbide electrode to be reducing electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be reduce 5 hours under the condition of-1.2 V at recovery voltage, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation.By the electrolyte filtering after reduction, obtain leucogentian violet crystal;
(4) waste water after reduction is re-started electrochemical oxidation, the oxidizing electrode of employing is gold electrode, and adopting saturated calomel electrode to do reference electrode, take platinum electrode as working electrode; Be be oxidized 5 hours under the condition of 1.1 V at oxidation voltage, make remaining organism oxidized.
Obtain leucogentian violet crystal after being degraded by the present embodiment, yield is 85%, and the COD in the water after electrochemicial oxidation is 30 mg/L.
Claims (1)
1. a method for Victoria Green WPB of degrading waste water, it is characterized in that, the method comprises the following steps:
(1) by Victoria Green WPB waste water grid desilting;
(2) the Victoria Green WPB waste water after step 1 being processed is heated to 10 ~ 40 DEG C, regulates pH to 4 ~ 10, the metal ion in precipitation solution, filters, obtain filtrate after 1 hour;
(3) filtrate after processing with step 2, for electrolytic solution, in three-electrode system, under the condition of-0.9 ~-1.2 V, reduces 5 hours, Victoria Green WPB waste water generation electrochemical reducting reaction, generates leucogentian violet precipitation; By the electrolyte filtering after reduction, obtain leucogentian violet crystal; Wherein, reducing electrode adopts the one in Graphite Electrodes, Ti electrode, iron electrode, gold electrode, plating Ruthenium Ti electrode, copper electrode, nanolithographic silver electrode and wolfram varbide electrode;
(4) using the filtrate after step 3 is filtered as electrolytic solution, electrochemical oxidation is re-started in three-electrode system, the oxidizing electrode adopted is the one in BDD electrode, gold electrode or nanosized platinum electrode, be be oxidized 5 hours under the condition of 1.0-1.3 V at oxidation voltage, remaining organism is degraded, the COD<60mg/L of waste water.
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Cited By (3)
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| CN108017118A (en) * | 2017-06-15 | 2018-05-11 | 武汉科技大学 | A kind of method based on electrochemical modification method processing cationic dyes waste water |
| CN108083519A (en) * | 2017-12-27 | 2018-05-29 | 黄山学院 | A kind of method of rhodamine B degradation waste water |
| WO2020057673A1 (en) * | 2018-09-21 | 2020-03-26 | Yanbo Li | Method for controlling an electro-oxidation process using boron doped diamond electrodes |
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