CN113307420A - Method for removing COD (chemical oxygen demand) in metallurgical wastewater - Google Patents

Method for removing COD (chemical oxygen demand) in metallurgical wastewater Download PDF

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CN113307420A
CN113307420A CN202110617811.6A CN202110617811A CN113307420A CN 113307420 A CN113307420 A CN 113307420A CN 202110617811 A CN202110617811 A CN 202110617811A CN 113307420 A CN113307420 A CN 113307420A
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cod
metallurgical
removing cod
electrode
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CN113307420B (en
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蒋国民
赵次娴
雷吟春
岑家山
刘锐利
赵淑宏
陈龙
廖圆
郑九林
高伟荣
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Science Environmental Co ltd
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    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C02F1/463—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
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    • C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention discloses a method for removing COD (chemical oxygen demand) in metallurgical wastewater, which comprises the following steps: step one, carrying out pretreatment according to the characteristics of metallurgical wastewater; step two, carrying out electrocatalytic oxidation on the liquid treated in the step one; adding an oxidant into the liquid treated in the step two, and performing further deep oxidation treatment on the wastewater; and step four, performing solid-liquid separation on the liquid treated in the step three, and discharging the liquid after reaching the standard. The invention can be suitable for the treatment of metallurgical organic wastewater with inlet COD of 1000-50000mg/L and the treatment of high-salt high-COD refractory wastewater produced by other industrial production under the same conditions, the COD of the outlet water can reach 1-300mg/L, the removal rate of the COD is more than 95 percent, the COD in the high-salt high-COD refractory organic wastewater can be efficiently removed, the generated slag amount is small, the cost of the incomplete electrocatalytic oxidation treatment is low, the application range is wide and the like.

Description

Method for removing COD (chemical oxygen demand) in metallurgical wastewater
Technical Field
The invention belongs to the technology of non-ferrous metal metallurgy industrial wastewater treatment, and particularly relates to a method for removing COD (chemical oxygen demand) in metallurgical wastewater.
Background
Currently, the commonly used nickel-cobalt metallurgy processes are divided into a pyrogenic process and a wet process, wherein the wet process is the mainstream production process of nickel-cobalt metallurgy. The wet production method takes minerals and metal wastes as raw materials, and takes an acidic extraction technology as a core to selectively extract an acidic leaching solution of the raw materials so as to realize the purpose of metal separation and purification. The pollution sources generated in the production process comprise oily heavy metal-containing high-salinity wastewater, ammonia nitrogen wastewater, waste acid, waste gas, waste residue and waste organic solvent. The high-salt and high-COD organic wastewater comes from each link of the process, and comprises mineral processing wastewater, extraction wastewater, electrodeposition waste liquid, waste gas absorption liquid and workshop flushing water. The wastewater is mainly acidic and weakly acidic, wherein the pollution factors comprise heavy metals, COD and the like. The COD is mainly composed of acidic extractant, sulfonated kerosene, extraction modifier and micromolecular organic matter formed by degrading the extractant. Especially high-salt high-COD waste water of raffinate, wherein the main organic matters in the raffinate are ethylhexyl phosphate mono-2-ethylhexyl and di (2-ethylhexyl) phosphate.
At present, the method for removing COD in high-salt high-COD refractory organic wastewater mainly comprises physical methods such as coagulating sedimentation, activated carbon adsorption and the like, advanced oxidation methods such as ozone oxidation, Fenton oxidation, electrooxidation and the like, and biochemical methods such as aerobic/anaerobic microbial decomposition and the like. However, the existing methods have certain process limitations, such as low removal rate of soluble substances and low reuse rate of activated carbon by a coagulating sedimentation method; the traditional Fenton method has high treatment cost, and a large amount of iron-containing sludge is generated in the degradation process of organic matters, so that secondary pollution is caused; the electricity consumption of the electrooxidation method is too high, and the selection of an electrode is also particularly important; the high saline water environment is not beneficial to the growth of microorganisms, and the phenomenon of microbial poisoning and the like can occur.
Disclosure of Invention
The technical problem solved by the invention is as follows: aiming at the treatment problem of high-salt high-COD refractory organic wastewater generated in the existing metallurgical process, the method for removing the COD in the metallurgical wastewater is low in treatment cost, good in treatment effect and small in slag amount.
The invention is realized by adopting the following technical scheme:
a method for removing COD in metallurgical wastewater comprises the following steps:
step one, pretreating according to the characteristics of metallurgical wastewater, adjusting the pH value of the wastewater, and removing insoluble impurities in the wastewater;
step two, carrying out electrocatalytic oxidation on the liquid treated in the step one, incompletely oxidizing organic phosphate substances and heavy metal cations in the wastewater into stable complexes, forming flocculating precipitates on hydroxides in the wastewater by utilizing the electric flocculation effect of an electrode, collecting and removing the part of precipitates, and decomposing and removing most organic matters in the wastewater through the step;
adding an oxidant into the liquid treated in the step two, further carrying out deep oxidation treatment on the wastewater, and removing the organic matters which are not completely oxidized in the step two;
and step four, performing solid-liquid separation on the liquid treated in the step three, and discharging the liquid after reaching the standard.
Specifically, in the method for removing COD in metallurgical wastewater of the present invention, the pretreatment mode in the first step includes at least one of acid adjustment, alkali adjustment, aeration, air flotation and coagulation, the pH environment of the wastewater is controlled by acid adjustment and alkali adjustment, and insoluble impurities in the wastewater are filtered by aeration, air flotation and coagulation.
Furthermore, the pH value of the liquid treated in the first step is 2.5-11, and the liquid is adjusted according to whether the liquid contains oil or not, so that the liquid is suitable for the oxidation reaction of organic matters in the wastewater.
Specifically, in the method for removing COD in metallurgical wastewater of the invention, the electrode used in the electrocatalytic oxidation in the second step is a special electrode, and comprises a BDD electrode, a titanium ruthenium iridium electrode, a three-dimensional electrode and Ti/SnO2Electrodes or Ti/PbO2One of the electrodes.
Specifically, in the method for removing COD in metallurgical wastewater, the electrocatalytic oxidation time of the wastewater in the second step is 1-30min, and the electrode electrifying current density is 15-150mA/cm2The operating voltage is 1-30V.
Specifically, in the method for removing COD from metallurgical wastewater of the present invention, in the second step, one of iron disulfide, activated carbon, iron carbide, sulfur, cobalt, zinc and their compounds is added as a catalyst to the wastewater during the electrocatalytic oxidation of the wastewater.
Furthermore, in the second step, the precipitate generated in the second step is removed by adopting adsorption, net catching or rolling.
Specifically, in the method for removing COD in metallurgical wastewater of the invention, in the third step, the solution treated in the second step is adjusted to be acidic, and the pH value is 2.5-4.0. .
Specifically, in the method for removing COD in metallurgical wastewater of the invention, the oxidant adopted in the third step is one of sodium hypochlorite, hypochlorous acid, chlorine, hydrogen peroxide, persulfuric acid and potassium ferrate, and the reaction time is 1-30 min.
Heavy metal cations in nickel cobalt organic wastewater suitable for the method of the invention comprise Cu2+、Ni2+、Pb2+At least one of (1).
The invention carries out electrocatalytic oxidation on the metallurgical wastewater with high salt content, high COD content and difficult degradation, the retention time is 1-30min, and the current density is 15-150mA/cm2Compared with the prior full electrocatalytic oxidation, the inventionThe method has the advantages that the method carries out incomplete oxidation on organic matters in the wastewater, the reaction time is shorter, the required current energy is lower, and the incomplete oxidation intermediate product can be combined with heavy metal ions in the wastewater to generate a stable complex so as to be efficiently removed by nascent state hydroxide. Compared with the prior complete oxidation, the incomplete electrooxidation and the electroflocculation have the synergistic effect of removing most electrooxidation intermediate products and saving the using amount of the oxidant in the next process step, thereby shortening the electrooxidation time and reducing the operation cost.
The electrocatalytic oxidation process of the refractory organics in the wastewater comprises the following steps: after the electrode is electrified, a large amount of OH with high oxidation activity is generated on the surface of the electrode, the organic phosphate substances in the solution are incompletely oxidized to produce short-chain fatty acid and phosphoric acid, 2 pairs of lone-pair electrons exist on the-OH oxygen in the molecular structure and can be mixed with Cu in the solution2+、Ni2+、Pb2+The hybridization orbitals of the heavy metal cations form coordination bonds to produce stable complexes.
The electric flocculation process in the electrocatalytic oxidation comprises the following steps: fe generated by induction anode in electrolytic process2+At pH>5 hydrolysis to produce substantial amounts of Fe (OH)2Rapidly oxidized to Fe (OH)3The nascent hydroxide is collected and filtered by means of adsorption, net capture, rolling sweep and the like, and has an efficient removing effect on incomplete oxidation products and complexes in the solution.
Heavy metal cations contained in wastewater to which the present invention is applicable include, but are not limited to, Cu2+、Ni2+、Pb2+The hybrid orbit in the electrocatalytic oxidation process is as follows: cu2+The electron arrangement is 3d94s0Copper ions are hybridized by adopting an empty 3d orbit, 4s and 24 p in a dsp mode2O atom lone pair electrons and hybrid orbital dsp2Forming a coordination bond; ni2+The electron arrangement is 3d8The nickel ions adopt empty 4s, 4p and 4d orbitals to perform sp3d2O atom lone pair of electrons and sp3d2Hybrid orbits; pb2+Outer nuclear electron arrangement: [ Xe]4f14 5d10 6s2The hybridization pattern is sp2d, O atom lone pair electrons may be coupled with sp2d hybridise to the empty orbital to form a coordination bond, thereby forming a stable complex.
The method can be suitable for treating the nickel-cobalt metallurgical organic wastewater with the inlet COD of 1000-50000mg/L and can also be suitable for treating the high-salt high-COD refractory organic wastewater produced by other nonferrous metal industrial production under the same conditions, the COD of the outlet water can reach 1-300mg/L, the removal rate of the COD is more than 95%, the COD in the high-salt high-COD refractory organic wastewater can be efficiently removed, the generated slag amount is small, the cost of incomplete electrocatalytic oxidation treatment is low, the application range is wide and the like.
The present invention will be further described with reference to the following embodiments.
Drawings
FIG. 1 is a schematic flow chart of the method for removing COD in metallurgical wastewater in the example.
Detailed Description
Example 1
Firstly, taking 1.5L of organic wastewater in the nickel-cobalt metallurgical industry, detecting that COD (chemical oxygen demand) of inlet water is 722mg/L, removing COD of sample wastewater according to the flow shown in figure 1, wherein the wastewater in the embodiment contains no or little oil, adding a proper amount of 10% alkaline solution according to the characteristics of the wastewater, adjusting the pH of the solution to 9.0, pouring the solution into a reaction container of a special electrode electrolysis device, adding 0.1g of active carbon as a catalyst, and adjusting the current density of electrode energization to be 50mA/cm2After the wastewater is subjected to incomplete electrocatalytic oxidation reaction for 10min, a small amount of acid solution is added into the liquid after electrocatalytic oxidation, the pH is adjusted to 3.5, and 1.5mg of H is added2O2The organic wastewater is further subjected to oxidation treatment as an oxidant, after the oxidation reaction is finished, solid-liquid separation is finished on the wastewater, effluent detection is carried out, COD (chemical oxygen demand) in the wastewater is reduced from 722mg/L to 27.2mg/L, the removal rate reaches 96.2%, the slag amount is 1/9 of the slag amount of the existing Fenton reaction, and the actual treatment cost of the organic wastewater in the embodiment is about 8 yuan/m3。
Example 2
Firstly, 1.5L of high-salt refractory organic wastewater in the nonferrous metallurgy industry is taken, the COD of the inlet water is detected to be 24120mg/L, and the sample is checked according to the flow of a figure 1Removing COD from the product wastewater, adding a proper amount of acid solution to adjust the solution to acidity until the organic matters in the wastewater are separated out to facilitate subsequent oxidation, pouring the pretreated wastewater into a reaction container of a special electrode electrolysis device, adding 0.1g of iron-carbon catalyst as the catalyst, and adjusting the current density of the electrified electrode to be 45mA/cm2After the wastewater is subjected to incomplete electrocatalytic oxidation reaction for 5min, 0.20mg of H is added into the liquid after electrocatalytic oxidation2O2Adjusting the pH value to 3 as an oxidant, further carrying out oxidation treatment on the organic wastewater, carrying out solid-liquid separation on the wastewater after the oxidation reaction is finished, detecting effluent, reducing COD (chemical oxygen demand) in the wastewater from 24120mg/L to 272.6mg/L, wherein the removal rate can reach 98.66%, the slag amount is about 1/10 of the slag amount of the existing Fenton reaction, and the actual treatment cost of the organic wastewater of the embodiment is about 9.5 yuan/m3。
Example 3
Firstly taking 1.0L of high-salt refractory organic wastewater in nonferrous metallurgy industry, detecting the COD of inlet water to be 1630mg/L, removing the COD of sample wastewater according to the flow shown in figure 1, adding a proper amount of dilute acid solution according to the characteristics of the wastewater, adjusting the pH of the solution to be 8, pouring the solution into a reaction container of a special electrode electrolysis device, adding 0.1g of iron carbon as a catalyst, and adjusting the current density of the electrified electrode to be 150mA/cm2And the voltage is 4.6V, after the wastewater is subjected to incomplete electrocatalytic oxidation reaction for 3min, 0.40mg of NaClO is added into the liquid after the electrocatalytic oxidation as an oxidant, the organic wastewater is further subjected to oxidation treatment, after the oxidation reaction is finished, the wastewater is subjected to solid-liquid separation, the effluent is detected, the COD in the wastewater is reduced to 58.3mg/L from 1630mg/L, the removal rate can reach 96.36%, the slag amount is about 1/10 of the slag amount of the existing Fenton reaction, and the actual treatment cost of the organic wastewater in the embodiment is about 8.5 yuan/m3。
Example 4
Firstly, taking 1.5L of high-salt refractory organic wastewater in the nonferrous metallurgy industry, detecting the COD of inlet water to be 2732mg/L, removing the COD of sample wastewater according to the flow shown in figure 1, adding a proper amount of dilute acid solution according to the characteristics of the wastewater, adjusting the pH of the solution to be 7, pouring the solution into a special container0.1g of iron carbon is added into a reaction container of an electrode electrolysis device as a catalyst, and the current density of the electrified electrode is adjusted to be 15mA/cm2Under the voltage of 4.2V, after the wastewater is subjected to incomplete electrocatalytic oxidation reaction for 30min, 1.35mg of H is added into the liquid after electrocatalytic oxidation2O2Adjusting the pH value to 3 as an oxidant, further carrying out oxidation treatment on the organic wastewater, carrying out solid-liquid separation on the wastewater after the oxidation reaction is finished, detecting effluent, reducing COD (chemical oxygen demand) in the wastewater from 2732mg/L to 92.4mg/L, wherein the removal rate can reach 96.62%, and the slag amount is 1/8 of the existing Fenton reaction slag amount, wherein the actual treatment cost of the organic wastewater in the embodiment is about 8.9 yuan/m3。
Comparative example
Firstly, taking 1.5L of high-salt refractory organic wastewater in the nonferrous metallurgy industry, detecting the COD of inlet water to be 2732mg/L, adding a proper amount of dilute acid solution according to the characteristics of the wastewater, adjusting the pH of the solution to be 7, and adjusting the current density of the electrified electrode to be 42mA/cm in a reaction container of an electrode electrolysis device2And the voltage is 8V, after the wastewater is subjected to complete electrocatalytic oxidation reaction for 120min, the effluent is detected, the COD in the wastewater is reduced from 2732mg/L to 753.21mg/L, the removal rate can reach 72.43%, and the actual treatment cost of the organic wastewater in the embodiment is about 45.71 yuan/m3。
As shown in the table below, the examples 1, 2, 3 and 4 for removing COD in high-salt refractory organic wastewater generated in nonferrous metallurgy industry by using the method of the invention in FIG. 1 have the advantages of shorter treatment time, higher COD removal rate and lower treatment cost compared with the existing comparative example adopting a complete electrocatalytic oxidation process.
TABLE comparison of the parameters of the examples with those of the comparative examples
Figure BDA0003098283780000051

Claims (10)

1. A method for removing COD in metallurgical wastewater is characterized by comprising the following steps:
step one, carrying out pretreatment according to the characteristics of metallurgical wastewater;
step two, carrying out electrocatalytic oxidation on the liquid treated in the step one, incompletely oxidizing organic phosphate substances and heavy metal cations in the wastewater into stable complexes, forming flocculating precipitates of hydroxides in the wastewater by utilizing the electric flocculation effect of an electrode, and collecting and removing the part of precipitates;
adding an oxidant into the liquid treated in the step two, and performing further deep oxidation treatment on the wastewater;
and step four, performing solid-liquid separation on the liquid treated in the step three, and discharging the liquid after reaching the standard.
2. The method for removing COD in metallurgical wastewater according to claim 1, characterized in that: the pretreatment mode in the first step comprises at least one of acid regulation, alkali regulation, aeration, air flotation and coagulation.
3. The method for removing COD in metallurgical wastewater according to claim 2, characterized in that: the pH value of the liquid treated in the first step is 2.5-11.
4. The method for removing COD in metallurgical wastewater according to claim 1, characterized in that: the electrode adopted by the electrocatalytic oxidation in the second step is a special electrode and comprises a BDD electrode, a titanium ruthenium iridium electrode, a three-dimensional electrode and Ti/SnO2Electrodes or Ti/PbO2One of the electrodes.
5. The method for removing COD in metallurgical wastewater according to claim 4, characterized in that: the electrocatalytic oxidation time of the wastewater in the second step is 1-30min, and the current density of the electrode is 15-150mA/cm2The operating voltage is 1-30V.
6. The method for removing COD in metallurgical wastewater according to claim 1, characterized in that: and in the second step, one of iron disulfide, activated carbon, iron carbide, sulfur, cobalt, zinc and a compound thereof is added into the wastewater as a catalyst in the process of electrocatalytic oxidation of the wastewater.
7. The method for removing COD in metallurgical wastewater according to claim 1, characterized in that: and in the second step, the precipitate generated in the second step is removed by adopting adsorption, net capture or rolling.
8. The method for removing COD in metallurgical wastewater according to claim 1, characterized in that: in the third step, the solution treated in the second step is adjusted to be acidic, and the pH value is 2.5-4.0.
9. The method for removing COD in metallurgical wastewater according to claim 8, characterized in that: the oxidant adopted in the third step is one of sodium hypochlorite, hypochlorous acid, chlorine, hydrogen peroxide, persulfuric acid and potassium ferrate, and the reaction time is 1-30 min.
10. A method for removing COD from metallurgical waste water according to any one of claims 1 to 9, wherein: the heavy metal cations in the metallurgical wastewater comprise Cu2+、Ni2+、Pb2+At least one of (1).
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CN114477572A (en) * 2022-03-01 2022-05-13 薛量 Harmless treatment method for wastewater containing organic phosphorus
CN114477572B (en) * 2022-03-01 2023-12-08 薛量 Harmless treatment method for wastewater containing organic phosphorus
CN114853220A (en) * 2022-05-30 2022-08-05 赛恩斯环保股份有限公司 Method for removing COD (chemical oxygen demand) and recycling high-ammonia nitrogen high-salt organic wastewater

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