CN107200422A - A kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater - Google Patents

A kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater Download PDF

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CN107200422A
CN107200422A CN201710429690.6A CN201710429690A CN107200422A CN 107200422 A CN107200422 A CN 107200422A CN 201710429690 A CN201710429690 A CN 201710429690A CN 107200422 A CN107200422 A CN 107200422A
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organic matter
residual organic
waste water
gold mine
cyanide wastewater
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CN107200422B (en
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朱和林
吴冰
杨敏
裘伟民
鲁金甲
王庆生
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Kaiyuan Environmental Technology Group Co.,Ltd.
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HANGZHOU KAIYUAN ENVIRONMENTAL PROTECTION ENGINEERING Co Ltd
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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
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • 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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    • 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
    • C02F1/467—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
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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    • C02F1/70—Treatment of water, waste water, or sewage by reduction
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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
    • 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
    • C02F2001/007—Processes including a sedimentation step
    • 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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    • C02F2001/46142—Catalytic coating
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/16—Nitrogen compounds, e.g. ammonia
    • C02F2101/18—Cyanides
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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    • C02F2201/00—Apparatus for treatment of water, waste water or sewage
    • C02F2201/46—Apparatus for electrochemical processes
    • C02F2201/461—Electrolysis apparatus
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    • C02F2201/46105—Details relating to the electrolytic devices
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    • C02F2201/00—Apparatus for treatment of water, waste water or sewage
    • C02F2201/46—Apparatus for electrochemical processes
    • C02F2201/461—Electrolysis apparatus
    • C02F2201/46105—Details relating to the electrolytic devices
    • C02F2201/4616—Power supply
    • C02F2201/46175—Electrical pulses
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/026—Fenton's reagent

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Abstract

The present invention relates to field of waste water treatment, a kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater is disclosed, is comprised the following steps：（1）Electrocatalytic oxidation；（2）Flocculation, sedimentation, filtering；（3）Fenton is complexed；（4）Catalysis oxidation.The present invention is originally organically combined electrocatalytic oxidation, Fenton complexing and catalysis oxidation, residual organic matter and cyanide wastewater is handled, good purification, cost is low, is met national standard.

Description

A kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater
Technical field
Select smelting residual organic matter the present invention relates to field of waste water treatment, more particularly to a kind of electrochemical pre-treatment gold mine and contain The method of cyanogen waste water.
Background technology
At present, some organic floating agents are commonly used in ore dressing process both at home and abroad and comes concentration of valuable metals, vulcanized lead zinc Ore deposit is exactly one of them, more or less all contains noble metal in usual Pb-Zn deposits.Current general still using extraction of gold by cyanidation work Skill, the methods used have acidifying absorption method, extraction recycle method etc. more in the organic matter and cyanide wastewater for handle this kind of residual, adopt Although certain cyanide can be reclaimed with acidifying absorption method, it can be remained because recovery of cyanide is not thorough, in waste water next Quantitative cyanide and flotation agent, while thiocyanate and some heavy metal ion are not all removed effectively；Using extraction Recycle method is by valuable metal recovery, the impurity effect reuse in the aqueous phase being constantly enriched with, and organic phase recycles extraction yield and declined It must all handle, add after-treatment；Therefore, more satisfactory method is also still lacked in this field of wastewater of processing, and such as Modern country improves sewage drainage standard again, it is desirable to which water outlet COD is below 60mg/L, and cyanide is below 0.50mg/L and a huge sum of money Category must all reach national standard.And these conventional treatment methods are extremely difficult to, if being that this is directed to containing organic pollution and given up containing cyanogen Water can research and develop a kind of green energy conservation, efficient new technology, for handle high-concentration hardly-degradable organic pollution and Cyanide wastewater particularly has deep environment protection significance.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of electrochemical pre-treatment gold mine select smelting residual organic matter and The method of cyanide wastewater.The present invention is originally organically combined electrocatalytic oxidation, Fenton complexing and catalysis oxidation, right Residual organic matter and cyanide wastewater are handled, and good purification, cost is low, meet national standard.
The present invention concrete technical scheme be：A kind of electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater Method, it is characterised in that comprise the following steps：
(1) electrocatalytic oxidation：PH value after pre-filtering is subjected to electrocatalytic oxidation for 5.5-6.5 waste water with electrocatalysis oxidation apparatus Change 3.5-4.5h, the working method of the electrocatalysis oxidation apparatus is electrolysed for pulsed；
(2) flocculate, settle, filter：Waste water after electrocatalytic oxidation is shifted, addition flocculant is stirred flocculation 20- 30min, sedimentation, filtering；Take filtered fluid to add flocculant again pH value is adjusted to after 8.5-9.5, be again stirring for the 30- that flocculates 40min, sedimentation, filtering；
(3) Fenton is complexed：PH value is adjusted to 5.5- by addition ferrous sulfate heptahydrate after the filtered fluid transfer after step (2) processing 6.5, complex reaction 25-35min and when pH value is reduced to 2.5-3.5, add hydrogen peroxide, react 50-70min；
(4) catalysis oxidation：The pH value of waste water after step (3) processing is adjusted to 8-9, after sedimentation filtration, immigration, which is filled with, urges Catalysis oxidation 60-70min is carried out in the catalysis oxidizing tower of compound, is eventually passed after filtering, wastewater treatment is finished.
This technology is from the lead and zinc concentrate after flotation during extraction valuable metal, due to association in floating and enriching concentrate The content of the ore deposit association mineral content in raw ore that compares wants much higher valuable metal and noble metal, therefore the cyaniding during cyaniding Inevitable very big, the complicated component of the consumption of sodium, makes to generate substantial amounts of various sulfide, cyanide in waste water, is brought during flotation The organic pollutions such as xanthate, black powder, in addition the nonferrous heavy metal such as copper to be also complexed consumption cyanide.
Electrocatalytic oxidation principle：
The pH value for selecting the residual organic matter produced in smelting production process and cyanide wastewater raw water is 6.0 or so, can be direct after filtering It is electrolysed.Its principle is to utilize PbO2With higher electro catalytic activity when electrode is electrolysed in aqueous, in addition using height The frequency pulse power " power supply-power failure-power supply " circular flow equipment, the O constantly provided from outside2Trap external electric field and electricity is provided Son, forms oxygen radical ion O2 -Under the conditions of electro-catalysis, water body produces H2O2, and generation hydroxyl radical free radical ion is induced simultaneously OH.Partial organic substances are made to be mineralized into CO2And H2O；Or organic matter (COD) is generated electrically charged organic " fragment " so that organic matter is big Molecule chain rupture will increase into small molecule, BOD/COD ratios, it is ensured that the normal operation of follow-up anaerobic and aerobic treatment facility.
The mineralising mechanism of specific organic matter：
R+·OH→R·+H2O
R·+M3+→M2++R+
R++O2→ROO-→…→CO2+H2O
Annotation：R represents organic matter (COD), and M such as Fe, Cu etc. represents catalyst metal ion.
The present invention coordinates pulse signal simultaneously, and the pulse power is during pulse electrolysis, when current lead-through, pulse (peak Value) electric current is equivalent to several times even tens times of conventional DC electric current, and exactly this high instantaneous current density (refers to dynamic response Speed) organic matter or inorganic matter is destroyed under high overpotential；When switch off current, discharge ion near electrode district Initial concentration is returned to again, and concentration polarization is eliminated, and this is continuing with high pulse (peak value) electric current beneficial to the next pulse same period Density, simultaneously turns off in the phase and is also changed into the phenomenons such as electric energy with galvanic cell electrode reaction i.e. chemical energy.Such process same period Property run through the whole story of whole electrolytic process, the mechanism included in it constitutes the most basic principle of pulse electrolysis.Practice card Bright, the pulse power changes the physical and chemical performance of material, the oxidation processes of organic wastewater and going back for heavy metal in electrolytic process All there is incomparable superiority than Traditional DC electrolysis in terms of former and precipitation process, energy-conservation.
Fenton complex scheme：
Fe2+And Fe3+With the relation of 3 kinds of iron cyanogen complex ions
Because the no matter interior rail elemental iron of iron cyanogen complex ion is Fe2+Or Fe3+The complex compound of formation is all difficult degraded, but it whether there is The characteristic of evil transfer precipitation.It is illustrated first during Fenton chemical reaction handling, with Fe3+In concentration increase, waste water Free cyanide also increases, CN-With Fe2+、Fe3+[Fe (CN) is generated respectively6]4-[Fe (CN)6]3-, see below row chemical reaction side Formula exists：
Fe2++6CN6 -→[Fe(CN)6]4-
Fe3++6CN6 -→[Fe(CN)6]3-
3Fe2++6CN-→Fe2[Fe(CN)6] ↓ (, Green was white)
3Fe2++2Fe(CN)6 3-→Fe3[Fe(CN)6]2↓ (rising scholar blue)
4Fe3++3[Fe(CN)6]4 -→Fe4[Fe(CN)6]3↓ (Prussian blue)
Wherein, [Fe (CN)6]4 -Stability constant KSurely=1.0 × 1035, [Fe (CN)6]3 -Stability constant KSurely=1.0 × 1042, All it is iron formation inner-orbital configuration complex ion, it is sufficiently stable.Two kinds of complex ions compare, and the latter is more stable, contain Fe so working as2+'s During chemicals treatment cyanide wastewater, [Fe (CN) is firstly generated6]4 -。
Work as Fe2+、Fe3+With CN-After generation complex ion and its reaction are completed under mildly acidic conditions, to make iron cyano complex Precipitation generation, Fe2[Fe(CN)6] solubility product Ksp=1.0 × 10-35, and Fe4[Fe(CN)6]3Solubility product Ksp=3.3 × 10-41, tend to be more stable complete.
Iron cyanogen complex ion is except forming that Green is white, the complexing beyond the region of objective existence such as blue and Prussian blue of rising scholar, can also be with copper, zinc, cadmium, lead etc. Heavy metal forms the very stable complex compound that can integrally precipitate, and is removed for transfer.
Catalytic oxidation principle：
Because Fenton chemical reaction handling also obeys Le Chatelier's principle (balance moving principle), any chemical reaction process increases Big reactant concentration reduces product concentration, and chemical balance is moved to positive reaction direction；Reduce reactant concentration or increasing Big product concentration, chemical balance is moved to back reaction direction, according to its principle, and Fenton chemically reacts when reaching equalization point, Reaction just be stopped, and reaction product must just be got rid of, and broken its equalization point and just be can proceed with, catalysis oxygen is additionally arranged for this Change method.
Catalysis oxidation of the present invention, be add catalytic materials and being fed into waste water be loaded with enough oxygen, catalytic materials it is oxygen-containing Material can promote oxidation reaction, at the same catalytic materials can also adsorption reaction product, make reaction to positive reaction direction move.
Preferably, in step (1), the pulse duty factor of pulse signal is 20-35%.
As a result of the pulse power, electrocatalysis oxidation apparatus and the pulse power are connected to form electrolysis system, it enters Capable electrolytic process is exactly pulse electrolysis.Electric current is from the time T for being switched to disconnectiononFor the pulse duration, pulse width is also, The working time being electrolysed.Electric current is from the time T for being disconnected to connectionoffTo be electrolysed the intermittent time or being pulse interval.Pulse has 3 independent parameters, i.e. pulse voltage (or electric current) amplitude, pulse width TonWith pulse interval Toff.This 3 parameters can be entered Row adjustment.
Pulse period is pulse width and pulse interval sum, and pulse frequency is then the inverse of pulse period.If dutycycle For r, then r is the ratio between ON time (pulse width) and pulse period：R=Ton/(Ton+Toff).The present invention sets dutycycle Between 20-35%, within this range, electrocatalytic oxidation best results.
Waste water is handled using pulse electrolysis, due to applying the reaction on pulse signal, electrode off and on, is conducive to expanding Dissipate, concentration polarization reduced, so as to reduce power consumption.It just can obtain different energy-saving effects.Such as r=50%, then pulse voltage is flat 50% when average is direct current supply, equally, 50% when the average value of pulse current is also direct current supply.Because electrical power is The product of electric current and voltage, thus power consumption when being only direct current supply 25%.And for example r=75%, then power consumption is direct current The 9/16 of power supply.As can be seen here, pulse power supply can greatly save electric energy.
Preferably, the electrocatalysis oxidation apparatus includes the multiple units being sequentially connected, each unit includes one Individual anode and a negative electrode；The anode of previous unit is connected with the negative electrode of latter unit, the negative electrode of first unit and last The anode connection of individual unit.
Another innovative point of the present invention is to employ unit-combination type electrolytic cell connected mode.It is on open market to adopt more With acyclic type or bipolar electrolyzer structure, monopolar electrolyzer inside configuration power supply circuit is in parallel, as shown in Fig. 2, because This total current is the electric current sum by unit groove, and the voltage of unit groove is of substantially equal, so acyclic type is electrolysed The characteristics of groove is low-voltage and high-current.And bipolar electrolyzer then contrast, the circuit of unit groove is series connection, is such as schemed Shown in 3, electric current passes sequentially through unit groove, therefore the electric current of unit groove is equal, and its total voltage is unit groove Voltage sum, so being high voltage low current the characteristics of bipolar electrolyzer.
And the present invention uses the electrolytic cell of unique unit-combination type connection, it comprises single stage type and bipolar type are respective Advantage and disadvantage, due to restricting for the function technology by great power pulse power source, using single stage type electrolytic cell, current strength is excessive, The pulse power can not meet the high current of electrolytic cell at present；Using bipolar electrolyzer, voltage is high, and current strength is little, but one Electrode plate forked rubbing the two poles of the earth, but because electrocatalytic oxidation titanium coating electrode material only makees anode, can not reversal connection, bipolar type connects Method is unavailable.This technique employs unit-combination type connection, solve single stage type connection because electric current is excessive and by the generation of burning machine Possibility.Overcome bipolar type titanium coating electrode material again and only make anode, can not reversal connection characteristic, the pulse power and electrolytic cell Between combined type connection the power supply system of sewage disposal under required certain power, can be solved using suitable Current Voltage pattern System.Energy-conservation can be played simultaneously and improves the effect of electricity effect.
Preferably, the anode of the electrocatalysis oxidation apparatus is brown lead oxide, negative electrode is titanium plate, and electrolyte is sulfuric acid Sodium.
Preferably, in step (1) and step (4), while being aerated to waste water.
Into waste water, aeration can improve the rate of oxygen in waste water, improve the catalysis oxidation efficiency.
Preferably, in step (1), to adding catalytic materials in waste water.
Catalytic materials are added while aeration, then into waste water, its catalysis oxidation efficiency can be further improved.
Preferably, the catalytic materials in step (1) and step (5) are to be loaded with the activated carbon of oxygen carrier or be loaded with containing The gas phase porous carbon materials of oxygen species.
If directly directly oxygen is improved into waste water by way of aeration, because oxygen can not be effectively converted into Dissolved oxygen, nearly more than 95% gas can occur to escape and can not effectively utilize, therefore can not directly translate into being provided O in gas2The linear relationship of concentration, therefore in air and pure O2Make influence difference of the gas phase media to system result not bery to show Write.And the present invention is that having O2System in there occurs adsorption reaction and catalytic oxidation simultaneously, catalytic oxidation due to It is relevant with the dissolved oxygen content that is loaded on activated carbon or gas phase porous carbon materials surface, following reaction just occurs on Carbon supports with complete Cyanogen is removed into oxidation：
CN-+2O2→2CNO-
2CNO-+2H2O (catalysis) → HCO3 -+NH3
The catalytic materials of the present invention are in addition to oxygen supply, moreover it is possible to effective adsorption reaction product, reaction is moved to positive reaction direction, at one stroke Two.
Preferably, the preparation method of the gas phase porous carbon materials of the oxygen carrier is：By furfural, water soluble phenolic resin Fat and water in mass ratio 4-6: 0.5-1.5: 80-100 is well mixed, and 1-2mol/L ammoniacal liquor is then slowly added dropwise while stirring, Regulation solution ph is 7.5-8.5；Then reacted 1-2 days at 55-65 DEG C, solution is turned into sol solutionses；Sol solutionses are stood After aging 1-3 days, line replacement is entered to the solvent in sol solutionses with n-hexane and absolute ethyl alcohol successively, wet gel is obtained；Then enter Row supercritical fluid drying, dries and removes after solvent, product is carbonized, gas phase porous carbon materials are obtained, and gas phase is porous Carbon material is cooled to 0-1 DEG C and addition mol ratio is 2: 1-1.2 into gas phase porous carbon materials sodium hydroxide and 30wt% Hydrogen peroxide；Fully after reaction, the gas phase porous carbon materials of oxygen carrier are made in draining, vacuum drying.
Gas phase porous carbon materials made from the above method compared with activated carbon, with specific surface area is bigger, load capacity is bigger, The higher advantage of adsorption efficiency.Although activated carbon is also porous material, but its distribution of pores is as the pore on skin, Hole is individualism rather than is interconnected, and this can cause its load capacity relatively low, and limit specific surface area.And on Gas phase porous carbon materials made from method are stated, with three-dimensional net structure, hole is interconnected as sponge mesopore , with higher specific surface area, therefore its load capacity, it is more preferable to the adsorption effect of dirt.In obtained gas phase porous carbon materials Afterwards, by special method, oxygen carrier sodium peroxide in load, its principle be under 0-1 DEG C of specified conditions, it is many in gas phase Following reaction occurs on the pore surface of hole carbon material：
2NaOH+H2O2→Na2O2+2H2O
Sodium peroxide is carried on after gas phase porous carbon materials, is respectively applied in step (1) and step (4).Input Following reaction can occur respectively in gas phase porous carbon materials pore surface after water：
Na2O2+2H2O=2NaOH+H2O2,
2Na2O2+2CO2=2Na2CO3+O2↑
Wherein H2O2Further occur following react：2H2O2=2H2O+O2↑
Because above-mentioned reaction is that occur in gas phase porous carbon materials pore surface, it can be adsorbed by gas phase porous carbon materials hole And be difficult to escape, it is possible to increase the oxygen content in water, utilization rate is high.Gas phase porous carbon materials hole is inhaled to dirt simultaneously It is attached, therefore can also occur oxidation reaction in gas phase porous carbon materials hole, play auxiliary catalysis effect.In addition, in step (1) In, it is degraded to carbon dioxide and water due to having an opportunity during electrocatalytic oxidation, and sodium peroxide can be with above-mentioned reaction Carbon dioxide is that reaction raw materials generate sodium carbonate and oxygen, therefore, it is possible to further improve electrocatalytic oxidation efficiency.
Preferably, the addition of catalytic materials is 20-40g/L, catalytic materials and waste water described in step (5) in step (1) Volume ratio 1: 1-1.2.
Preferably, the addition of hydrogen peroxide described in step (3) is 2-2.5vol%.
It is compared with the prior art, the beneficial effects of the invention are as follows：Electrocatalytic oxidation, Fenton are originally complexed by the present invention And catalysis oxidation is organically combined, residual organic matter and cyanide wastewater are handled, good purification, cost is low, accorded with Close national standard.
(1) the inventive method is to use electrocatalysis oxidation apparatus and pollution-free chemical reagent organically new technology of combined, is filled Distribution waves the function of respective unit to act synergistically from each other, and the electrocatalysis oxidation apparatus used is that electric energy is changed into The electrolytic cell electrode reaction of chemical energy, the useless of high-concentration hardly-degradable can effectively be handled by being combined with reagent chemical Treatment Water.
(2) practice have shown that：Using inventive method, being down to by 11810mg/L for Pb-Zn deposits organic wastewater COD can be made Below 60mg/L, total removal rate is that 99.8%, TCN is down to below 0.5mg/L, clearance nearly 100% by 2360mg/L.
(3) the inventive method is carried out under normal temperature and pressure conditionses, and electrocatalytic oxidation equipment is relatively easy, technology Flexibly, can Hour process cycle, greatly reduce occupation area of equipment, electrocatalytic oxidation water technology can be used for inorganic With organic multiple water treatment fields, this technology employs the pulse power again so that energy consumption, whole technique can be greatly lowered in technique It is a kind of environmentally safe " green environment is friendly " water technology.
Brief description of the drawings
Fig. 1 is the connection diagram of electrocatalysis oxidation apparatus of the present invention；
Fig. 2 is a kind of structural representation of the connection diagram of monopolar electrolyzer in the prior art；
Fig. 3 is a kind of structural representation of the connection diagram of bipolar electrolyzer in the prior art.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater, comprises the following steps：
(1) electrocatalytic oxidation：PH value after pre-filtering is subjected to electrocatalytic oxidation 4h for 6 waste water with electrocatalysis oxidation apparatus, The working method of the electrocatalysis oxidation apparatus is electrolysed for pulsed, and the pulse duty factor of pulse signal is 28%.The electricity is urged Change 10 units that oxidation unit includes being sequentially connected, as shown in figure 3, each unit includes an anode and a moon Pole；The anode of previous unit is connected with the negative electrode of latter unit, and the negative electrode of first unit connects with the anode of last unit Connect.Its Anodic is brown lead oxide, and negative electrode is titanium plate, and electrolyte is sodium sulphate.While electrocatalytic oxidation, waste water is carried out Air Exposure.
(2) flocculate, settle, filter：Waste water after electrocatalytic oxidation is shifted, addition flocculant is stirred flocculation 25min, sedimentation, filtering；Take filtered fluid to add again after pH value is adjusted to 9 by flocculant, be again stirring for flocculation 35min, sedimentation, mistake Filter.
(3) Fenton is complexed：PH value is adjusted to 6 by addition ferrous sulfate heptahydrate after the filtered fluid transfer after step (2) processing, Complex reaction 30min and when pH value is reduced to 3, adds hydrogen peroxide 2.25vol% with respect to waste water, reacts 60min.
(4) catalysis oxidation：The pH value of waste water after step (3) processing is adjusted to 8.5, after sedimentation filtration, immigration is filled out There is progress catalysis oxidation 60min in the catalysis oxidizing tower of catalytic materials, while carrying out Air Exposure, the body of the catalytic materials and waste water Product ratio 1: 1.1.Eventually pass after filtering, wastewater treatment is finished.
Wherein, the catalytic materials are the activated carbon for being loaded with oxygen carrier.
Embodiment 2
A kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater, comprises the following steps：
(1) electrocatalytic oxidation：PH value after pre-filtering is subjected to electrocatalytic oxidation 4h for 6 waste water with electrocatalysis oxidation apparatus, The working method of the electrocatalysis oxidation apparatus is electrolysed for pulsed, and the pulse duty factor of pulse signal is 28%.The electricity is urged Change 10 units that oxidation unit includes being sequentially connected, each unit includes an anode and a negative electrode；Previous unit Anode be connected with the negative electrode of latter unit, the negative electrode of first unit is connected with the anode of last unit.Its Anodic For brown lead oxide, negative electrode is titanium plate, and electrolyte is sodium sulphate.While electrocatalytic oxidation, to waste water carry out Air Exposure and Catalytic materials are added into waste water, the addition of catalytic materials is 30g/L.
(2) flocculate, settle, filter：Waste water after electrocatalytic oxidation is shifted, addition flocculant is stirred flocculation 25min, sedimentation, filtering；Take filtered fluid to add again after pH value is adjusted to 9 by flocculant, be again stirring for flocculation 35min, sedimentation, mistake Filter.
(3) Fenton is complexed：PH value is adjusted to 6 by addition ferrous sulfate heptahydrate after the filtered fluid transfer after step (2) processing, Complex reaction 30min and when pH value is reduced to 3, adds hydrogen peroxide 2.25vol% with respect to waste water, reacts 60min.
(4) catalysis oxidation：The pH value of waste water after step (3) processing is adjusted to 8.5, after sedimentation filtration, immigration is filled out There is progress catalysis oxidation 60min in the catalysis oxidizing tower of catalytic materials, while carrying out Air Exposure, the body of the catalytic materials and waste water Product ratio 1: 1.1.Eventually pass after filtering, wastewater treatment is finished.
Wherein, the catalytic materials are the gas phase porous carbon materials for being loaded with oxygen carrier for being loaded with oxygen carrier.It is described The preparation method of the gas phase porous carbon materials of oxygen carrier is：By furfural, water soluble phenol resin and water in mass ratio 5: 1: 90 It is well mixed, 1.5mol/L ammoniacal liquor is then slowly added dropwise while stirring, regulation solution ph is 8；Then reacted at 60 DEG C 1.5 days, solution is set to turn into sol solutionses；After sol solutionses are stood into aging 2 days, successively with n-hexane and absolute ethyl alcohol in sol solutionses Solvent enter line replacement, obtain wet gel；Then supercritical fluid drying is carried out, dries and removes after solvent, charcoal is carried out to product Change, obtain gas phase porous carbon materials, gas phase porous carbon materials are cooled to 0 DEG C and mol ratio are added into gas phase porous carbon materials The hydrogen peroxide of sodium hydroxide and 30wt% for 2: 1.1；Fully after reaction, the gas phase of oxygen carrier is made in draining, vacuum drying Porous carbon materials.
Embodiment 3
A kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater, comprises the following steps：
(1) electrocatalytic oxidation：PH value after pre-filtering is subjected to electrocatalytic oxidation for 5.5 waste water with electrocatalysis oxidation apparatus 3.5h, the working method of the electrocatalysis oxidation apparatus is electrolysed for pulsed, and the pulse duty factor of pulse signal is 20%.It is described Electrocatalysis oxidation apparatus includes 8 units being sequentially connected, and each unit includes an anode and a negative electrode；Previous list The anode of member is connected with the negative electrode of latter unit, and the negative electrode of first unit is connected with the anode of last unit.Its middle-jiao yang, function of the spleen and stomach Extremely brown lead oxide, negative electrode is titanium plate, and electrolyte is sodium sulphate.While electrocatalytic oxidation, Air Exposure is carried out to waste water With add catalytic materials into waste water, the addition of catalytic materials is 20g/L.
(2) flocculate, settle, filter：Waste water after electrocatalytic oxidation is shifted, addition flocculant is stirred flocculation 20min, sedimentation, filtering；Take filtered fluid to add again after pH value is adjusted to 8.5 by flocculant, be again stirring for flocculation 40min, sedimentation, Filtering.
(3) Fenton is complexed：PH value is adjusted to by addition ferrous sulfate heptahydrate after the filtered fluid transfer after step (2) processing 5.5, complex reaction 25min and when pH value is reduced to 3.5, add hydrogen peroxide 2.0vol% with respect to waste water, react 50min.
(4) catalysis oxidation：The pH value of waste water after step (3) processing is adjusted to 8, after sedimentation filtration, immigration is filled with Catalysis oxidation 50min is carried out in the catalysis oxidizing tower of catalytic materials, while carrying out Air Exposure, the volume of the catalytic materials and waste water Than 1: 1.Eventually pass after filtering, wastewater treatment is finished.
Wherein, the catalytic materials are the gas phase porous carbon materials for being loaded with oxygen carrier.The gas phase of the oxygen carrier is more The preparation method of hole carbon material is：Furfural, water soluble phenol resin and water in mass ratio 4: 0.5: 80 is well mixed, then side 1mol/L ammoniacal liquor is slowly added dropwise in stirring side, and regulation solution ph is 7.5；Then reacted 2 days at 55 DEG C, solution is turned into molten Glue；After sol solutionses are stood into aging 1 day, line replacement is entered to the solvent in sol solutionses with n-hexane and absolute ethyl alcohol successively, obtained To wet gel；Then supercritical fluid drying is carried out, dries and removes after solvent, product is carbonized, gas phase porous carbon is obtained Material, by gas phase porous carbon materials be cooled to 1 DEG C and into gas phase porous carbon materials add mol ratio for 2: 1 sodium hydroxide and 30wt% hydrogen peroxide；Fully after reaction, the gas phase porous carbon materials of oxygen carrier are made in draining, vacuum drying.
Embodiment 4
A kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater, comprises the following steps：
(1) electrocatalytic oxidation：PH value after pre-filtering is subjected to electrocatalytic oxidation for 6.5 waste water with electrocatalysis oxidation apparatus 4.5h, the working method of the electrocatalysis oxidation apparatus is electrolysed for pulsed, and the pulse duty factor of pulse signal is 35%.It is described Electrocatalysis oxidation apparatus includes the multiple units being sequentially connected, and each unit includes an anode and a negative electrode；It is previous The anode of unit is connected with the negative electrode of latter unit, and the negative electrode of first unit is connected with the anode of last unit.Wherein Anode is brown lead oxide, and negative electrode is titanium plate, and electrolyte is sodium sulphate.While electrocatalytic oxidation, waste water is carried out at aeration Manage and catalytic materials are added into waste water, the addition of catalytic materials is 40g/L.
(2) flocculate, settle, filter：Waste water after electrocatalytic oxidation is shifted, addition flocculant is stirred flocculation 30min, sedimentation, filtering；Take filtered fluid to add again after pH value is adjusted to 9.5 by flocculant, be again stirring for flocculation 30min, sedimentation, Filtering.
(3) Fenton is complexed：PH value is adjusted to by addition ferrous sulfate heptahydrate after the filtered fluid transfer after step (2) processing 6.5, complex reaction 35min and when pH value is reduced to 2.5, add hydrogen peroxide 2.5vol% with respect to waste water, react 70min.
(4) catalysis oxidation：The pH value of waste water after step (3) processing is adjusted to 9, after sedimentation filtration, immigration is filled with Catalysis oxidation 70min is carried out in the catalysis oxidizing tower of catalytic materials, while carrying out Air Exposure, the volume of the catalytic materials and waste water Than 1: 1.2.Eventually pass after filtering, wastewater treatment is finished.
Wherein, the catalytic materials are the gas phase porous carbon materials for being loaded with oxygen carrier.The gas phase of the oxygen carrier is more The preparation method of hole carbon material is：Furfural, water soluble phenol resin and water in mass ratio 6: 1.5: 100 is well mixed, then 2mol/L ammoniacal liquor is slowly added dropwise while stirring, regulation solution ph is 8.5；Then reacted 1 day at 65 DEG C, turn into solution Sol solutionses；After sol solutionses are stood into aging 3 days, line replacement is entered to the solvent in sol solutionses with n-hexane and absolute ethyl alcohol successively, Obtain wet gel；Then supercritical fluid drying is carried out, dries and removes after solvent, product is carbonized, gas phase is obtained porous Gas phase porous carbon materials are cooled to 0 DEG C and the hydroxide that mol ratio is 2: 1.2 are added into gas phase porous carbon materials by carbon material The hydrogen peroxide of sodium and 30wt%；Fully after reaction, the gas phase porous carbon materials of oxygen carrier are made in draining, vacuum drying.
Contrast on effect：The water treatment efficiency of the embodiment of the present invention 1 and embodiment 2 is contrasted.
Wherein before processing waste water quality situation is as follows：
Title COD TCN Au Ag Cu Fe Zn Pb
Content 7931.8 1332.2 0.6~1.8 0.24~1.6 1485.2 About 100 It is atomic It is micro
Note：Unit：mg/L.
After processing, waste water quality situation is as follows：
Title COD TCN Au Ag Cu Fe Zn Pb
Embodiment 1 25.0 0.26 It is atomic It is atomic It is atomic It is atomic It is atomic It is atomic
Embodiment 2 15.05 0.19 It is atomic It is atomic It is atomic It is atomic It is atomic It is atomic
Note：Unit：mg/L.
Raw materials used in the present invention, equipment, is the conventional raw material, equipment of this area unless otherwise noted；In the present invention Method therefor, is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention Any simple modification, change and equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side The protection domain of case.

Claims (10)

1. a kind of method that electrochemical pre-treatment gold mine selects smelting residual organic matter and cyanide wastewater, it is characterised in that including following step Suddenly：
（1）Electrocatalytic oxidation：PH value after pre-filtering is subjected to electrocatalytic oxidation for 5.5-6.5 waste water with electrocatalysis oxidation apparatus Change 3.5-4.5h, the working method of the electrocatalysis oxidation apparatus is electrolysed for pulsed；
（2）Flocculation, sedimentation, filtering：Waste water after electrocatalytic oxidation is shifted, addition flocculant is stirred flocculation 20- 30min, sedimentation, filtering；Take filtered fluid to add flocculant again pH value is adjusted to after 8.5-9.5, be again stirring for the 30- that flocculates 40min, sedimentation, filtering；
（3）Fenton is complexed：By step（2）PH value is adjusted to 5.5- by addition ferrous sulfate heptahydrate after filtered fluid transfer after processing 6.5, complex reaction 25-35min and when pH value is reduced to 2.5-3.5, add hydrogen peroxide, react 50-70min；
（4）Catalysis oxidation：By step（3）The pH value of waste water after processing is adjusted to 8-9, after sedimentation filtration, and immigration, which is filled with, urges Catalysis oxidation 60-70min is carried out in the catalysis oxidizing tower of compound, is eventually passed after filtering, wastewater treatment is finished.
2. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 1 selects smelting residual organic matter and cyanide wastewater, its It is characterised by, step（1）In, the pulse duty factor of pulse signal is 20-35%.
3. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 1 or 2 selects smelting residual organic matter and cyanide wastewater, Characterized in that, the electrocatalysis oxidation apparatus includes the multiple units being sequentially connected, each unit includes an anode With a negative electrode；The anode of previous unit is connected with the negative electrode of latter unit, the negative electrode of first unit and last unit Anode connection.
4. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 3 selects smelting residual organic matter and cyanide wastewater, its It is characterised by, the anode of the electrocatalysis oxidation apparatus is brown lead oxide, and negative electrode is titanium plate, and electrolyte is sodium sulphate.
5. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 1 selects smelting residual organic matter and cyanide wastewater, its It is characterised by, in step（1）And step（4）In, while being aerated to waste water.
6. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 1 selects smelting residual organic matter and cyanide wastewater, its It is characterised by, in step（1）In, to adding catalytic materials in waste water.
7. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 6 selects smelting residual organic matter and cyanide wastewater, its It is characterised by, step（1）And step（5）In catalytic materials be to be loaded with the activated carbon of oxygen carrier or be loaded with oxygen carrier Gas phase porous carbon materials.
8. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 7 selects smelting residual organic matter and cyanide wastewater, its It is characterised by, the preparation method of the gas phase porous carbon materials of the oxygen carrier is：Furfural, water soluble phenol resin and water are pressed Mass ratio 4-6:0.5-1.5:80-100 is well mixed, and 1-2mol/L ammoniacal liquor is then slowly added dropwise while stirring, adjusts solution PH value is 7.5-8.5；Then reacted 1-2 days at 55-65 DEG C, solution is turned into sol solutionses；Sol solutionses are stood into aging 1-3 days Afterwards, line replacement is entered to the solvent in sol solutionses with n-hexane and absolute ethyl alcohol successively, obtains wet gel；Then shooting flow is carried out Soma is dry, dries and removes after solvent, product is carbonized, gas phase porous carbon materials are obtained, gas phase porous carbon materials are cooled It is 2 that mol ratio is added to 0-1 DEG C and into gas phase porous carbon materials:1-1.2 sodium hydroxide and 30wt% hydrogen peroxide；Fully After reaction, the gas phase porous carbon materials of oxygen carrier are made in draining, vacuum drying.
9. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 7 or 8 selects smelting residual organic matter and cyanide wastewater, Characterized in that, step（1）The addition of middle catalytic materials is 20-40g/L, step（5）Described in catalytic materials and waste water volume Than 1:1-1.2.
10. the method that a kind of electrochemical pre-treatment gold mine as claimed in claim 1 selects smelting residual organic matter and cyanide wastewater, its It is characterised by, step（3）Described in hydrogen peroxide addition be 2-2.5vol%.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110918264A (en) * 2019-12-17 2020-03-27 中南大学 Application of combined inhibitor in flotation separation of copper-lead bulk concentrates
CN113307420A (en) * 2021-06-03 2021-08-27 赛恩斯环保股份有限公司 Method for removing COD (chemical oxygen demand) in metallurgical wastewater
CN117509841A (en) * 2024-01-02 2024-02-06 北京禹涛环境工程有限公司 Tandem bipolar thin plate blade electrocatalytic sewage treatment device

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* Cited by examiner, † Cited by third party
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CN105293790A (en) * 2015-12-01 2016-02-03 安洁士环保（上海）股份有限公司 Comprehensive treatment method for oily sewage in oil field

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105293790A (en) * 2015-12-01 2016-02-03 安洁士环保（上海）股份有限公司 Comprehensive treatment method for oily sewage in oil field

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110918264A (en) * 2019-12-17 2020-03-27 中南大学 Application of combined inhibitor in flotation separation of copper-lead bulk concentrates
CN113307420A (en) * 2021-06-03 2021-08-27 赛恩斯环保股份有限公司 Method for removing COD (chemical oxygen demand) in metallurgical wastewater
CN113307420B (en) * 2021-06-03 2022-05-31 赛恩斯环保股份有限公司 Method for removing COD (chemical oxygen demand) in metallurgical wastewater
CN117509841A (en) * 2024-01-02 2024-02-06 北京禹涛环境工程有限公司 Tandem bipolar thin plate blade electrocatalytic sewage treatment device
CN117509841B (en) * 2024-01-02 2024-04-05 北京禹涛环境工程有限公司 Tandem bipolar thin plate blade electrocatalytic sewage treatment device

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