CN102515388A - Method for treating high-concentration cyanogen-containing waste water - Google Patents
Method for treating high-concentration cyanogen-containing waste water Download PDFInfo
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- CN102515388A CN102515388A CN2011104029467A CN201110402946A CN102515388A CN 102515388 A CN102515388 A CN 102515388A CN 2011104029467 A CN2011104029467 A CN 2011104029467A CN 201110402946 A CN201110402946 A CN 201110402946A CN 102515388 A CN102515388 A CN 102515388A
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Abstract
The invention relates to the field of environmental protection related to waste water treatment, and provides a method for treating high-concentration cyanogen-containing waste water. The method provided by the invention comprises the following steps that through pretreatment adopting an acidification-precipitation method, CN<-> existing in the form of [Cu(CN)3]<2->] in waste water is broken apart and dissociates in the waste water; and the CN<-> undergoes a three-stage alkaline chlorination-oxidation reaction to produce CO2 and N2 so that the CN<-> content of the waste water reaches a discharge standard. The method provided by the invention can effectively remove CN<-> of high-concentration cyanide-containing waste water, wherein a CN<-> removal rate is above 99.9%, and overcome the defect that the existing acidification stripping method can bring about the production of a mass of virulent HCN and has a high cost, high parameter control requirements and unstable treatment efficiency.
Description
Technical field
The present invention relates to the wastewater treatment field of environment protection, be specifically related to the gold smelting method of wastewater treatment of a kind of " high density contains prussiate ".
Technical background
At present, world's gold output great majority are to adopt cyanidation gold-extracted technology to obtain, though prussiate has severe toxicity, also do not have at present a kind ofly suitable soak golden solvent and can replace, and therefore cyanidation gold-extracted technology is still occupied an leading position at the gold production field.Needs along with the China's national economy steady progression; The gold development strategy is progressively abundant relatively to Mineral resources from now on; But ecotope quite fragile in, environment sensitive zone-transfer such as western and coastal basin, gold resource exploitation simultaneously begins to transfer to rapidly the difficult-treating gold mine resources domain that contains arsenic, sulphur and complicated metal from being prone to handle resource.
Extraction of gold by cyanidation is T&B, mainly contains two kinds of different cyanidation technologies at present, cyanogen zinc dust precipitation depositing technology (CCD) and carbon slurry process (CIP).Two kinds of technologies all produce the waste water that contains a large amount of prussiates, generally handle the 1t gold ore and will efflux 4m
3About cyanide wastewater, the concentration of its prussiate is at 50～500rng/L, and is that have even higher.
A lot of to treatment Methods of Cyanide Wastewater at present, high-concentration waste water considers that generally prussiate reclaims, and then considers to adopt the method for destroying cyanogen to handle for low concentration wastewater or the little high-concentration waste water of recovery economic worth.
Absorption method is prussiate regeneration in the cyanide wastewater, and reclaims valuable metal wherein, makes a silk purse out of a sow's ear.Main method has: acidifying aeration-alkali lye absorption method, solvent extration, liquid-film method, ion exchange method etc.
Acidifying aeration-alkali absorption method is under sour environment; In waste water, blasting air overflows the prussic acid volatilization; Reclaim with alkali lye again, high cyanide containing wastewater is had favorable economic benefit, but the waste water after this method is handled generally need carry out secondary treatment ability qualified discharge.
Solvent extration is to utilize harmful element Cu in a kind of amine solvent extraction solution, Zn etc., and free cyanogen is then stayed in the extraction liquid, and load organic phases is stripped with NaOH solution.The post-treatment aqueous phase retrieval system, to utilize prussiate and the recycle to extinction of realization lean solution wherein, Solvent Extraction Separation is effective, can reclaim useful metal and prussiate in the waste water, but this method only is applicable to the cyanide wastewater that concentration is very high.
Liquid-film method adopts water-in-oil-in-water (W/O/W) system; Liquid film is kerosene and tensio-active agent; Interior water is a NaOH solution; Outer water is pending cyanide wastewater, and the efficient height of this method Treatment of Cyanide-containing Wastewater, speed is fast, selectivity good, but cost is high, the investment big, power consumption greatly, only is applicable to that concentration is lower, is the cyanide wastewater that free state exists.
The ion exchange method investment cost is high, and can only be used for the mother liquor recovery, uses not extensive.
Destroy method Treatment of Cyanide-containing Wastewater method has: chemical oxidization method, biological oxidation process, natural degradation method etc.
Biological oxidation process is the oxidation capacity that relies on mikrobe, the prussiate in the waste water is resolved into nitrate salt, vitriol and carbonate; This method can be decomposed thiocyanide, and heavy metal is mud to be removed, and it is good to efflux water quality; Cost is low, but technology is long, and investment is big; Operational condition is very strict, only suitable lower concentration treatment of cyanide waste water.
The natural degradation method is to remove prussiate with natural way, promptly according to abiogenous physics chemical action, photochemistry Decomposition, biological action and aeration, prussiate decomposition, concentration is reduced gradually, the heavy metal ion deposition, and sewage is purified.This method less investment, productive expense is low, but floor space is big, and process is slow, influenced by natural cause, and the waste discharge difficulty is up to standard.
The ultimate principle of chemical oxidization method is for breaking the stability of C-N chain through oxidation; Make its separation; Destroy the cyanogen root architecture thereby reach, contact its toxic purpose, its main method has methods such as alkaline chlorination process, hydrogen peroxide oxidation process, ozone oxidation method, active carbon adsorption.Hydrogen peroxide oxidation process, ozone oxidation method are mainly used in handles the lower concentration prussiate, and investment is bigger, and running cost is high; Alkaline chlorination process is the effective means of present Treatment of Cyanide-containing Wastewater; This method utilizes the strong oxidizing property of chlorine to make prussiate under alkaline condition, be oxidized to carbonic acid gas and nitrogen; This method technical maturity, treatment effect are good; But during with this method Treatment of Cyanide-containing Wastewater, then water outlet can not be up to standard if be higher than 300mg/L for concentration of cyanide in the waste water, cyanide wastewater before the alkaline chlorination process necessary preposition pre-treatment higher to concentration; Concentration of cyanide in the waste water is reduced to below the 300mg/L, adopts this method that it is handled to emission standard again.Conventional pretreatment process is: waste water is adjusted to acidity make H
+, CN
-Be combined into HCN, HCN has volatility, can from water, remove through stripping, but the HCN hypertoxicity need not absorb collection behind the stripping.Stripping operation processing cost is higher, and controlled variable requires highly, otherwise processing efficiency is unstable, has strengthened the processing of back segment and has loaded, and possibly cause the beol can't stably reaching standard.
The expert also is used for the cyanide wastewater processing with advanced persons' such as film processing, IX waste water treatment process both at home and abroad in recent years, but working cost is higher, uses on a large scale as yet and promotes, and the treatment Technology of Cyanide Wastewater progress is main with traditional treatment method still.
Summary of the invention
For remedying the deficiency of prior art, the invention provides a kind of high density cyanide wastewater treatment process, this method can effectively be removed the CN in the high density cyanide wastewater
-, CN
-Clearance reaches more than 99.9%, and has overcome existing acidifying blow-off method and produce a large amount of hypertoxic HCN, and cost is higher, and controlled variable require high, defectives such as processing efficiency instability.
Technical scheme of the present invention is: a kind of high density cyanide wastewater treatment process, and earlier the high density cyanide wastewater is carried out pre-treatment, and then pretreated waste water is carried out alkaline chloride oxidation;
Said pre-treatment is acidifying-precipitator method, and concrete steps are: at first in waste water, add sulfuric acid, the vitriolic consumption is so that the pH of waste water is 1.0-3.0 to be as the criterion, and reaction 10min-20min forms the deposition of cuprous cyanide, and makes other CN
-In water, exist with free state; Deposition is removed cuprous cyanide then, accomplishes the pre-treatment to waste water;
Said alkaline chloride oxidation is three sections alkaline chloride oxidations, and concrete steps are following:
(1) one section alkaline chloride oxidation: add calcium hydroxide at above-mentioned pretreated waste water; The consumption of calcium hydroxide is as the criterion at 10-11 with the pH of control waste water; The Youxiaolin that adds available chlorine>=10% again; Add-on is to add Youxiaolin 5ml-8ml in every liter of waste water, and reaction 20min-40min is with free CN in the water
-Be oxidized to cyanate;
(2) two sections alkaline chloride oxidations: transfer pH at 6.5-7.5 the waste water behind one section alkaline chloride oxidation; The Youxiaolin that adds available chlorine >=10% again; Add-on is to add Youxiaolin 8ml-12ml in every liter of waste water; Reaction 20min-40min is oxidized to carbonic acid gas and nitrogen with the cyanate in the waste water;
(3) three sections alkaline chloride oxidations: repeat two sections alkaline chloride oxidation processes, make in the waste water after the processing CN-stable and be lower than emission standard and get final product.
Said pre-treatment preferably adopts the sulfuric acid adjust pH to 2.5-3.0.
The pH of said one section alkaline chloride oxidation is preferably 10.5, the preferred Youxiaolin 5ml that adds in every liter of waste water, and the reaction times is 30min.
The pH of said two sections alkaline chloride oxidations is preferably 7, the preferred Youxiaolin 8ml that adds in every liter of waste water, and the reaction times is 30min.
The pH of said three sections alkaline chloride oxidations is preferably 7, the preferred Youxiaolin 3ml that adds in every liter of waste water, and the reaction times is 30min.
The concentration of CN-is greater than the waste water of 300mg/L in the high density cyanide wastewater according to the invention.
The concentration of CN-is preferably 300mg/L-700mg/L in the high density cyanide wastewater according to the invention.
The concentration of sulphur bronsted lowry acids and bases bronsted lowry of the present invention not necessarily will limit, and the amount of adding is as the criterion with the pH value in the control waste water.
Do further explanation and explanation in the face of the present invention down:
A kind of Study on Treatment for High Concentration Cyanide method that the invention provides, concrete steps and principle are following:
1) in waste water, add sulfuric acid acidation, acidifying pH is controlled at below 3.0, complete hybrid reaction 10-40min, and afterwards through deposition, with the cuprous cyanide particle separation that produces in the acidization, and recyclable copper.The acid precipitation process is a preprocessing process, is mainly the Cu2+ that exists with [Cu (CN) 3] 2-form is decomposed under acidic conditions, forms the deposition of cuprous cyanide, and CN-is existed with free state in water.This process is to CN-not removal effect basically, but CN-will have on a small quantity with HCN form and volatilization (HCN absorbs with alkali lye) under sour environment.
2) in the pretreated waste water of step 1), add calcium hydroxide, pH is at 10-11 in control, and the adding Youxiaolin carries out one section alkaline chloride oxidation.This process is mainly free CN-in the water is oxidized to cyanate, and the principal reaction formula is:
CN-+ClO-+H2O＝CNCl+2OH- (1)
CNCl+2OH-＝CNO-+Cl-+H2O (2)
3) step 2) water outlet transfers pH about 7.0 with sulfuric acid, and the adding Youxiaolin carries out two sections alkaline chloride oxidations.This process further is oxidized to carbonic acid gas and nitrogen with the cyanate of the overwhelming majority in the waste water, and the principal reaction formula is:
2CNO-+4OH-+3Cl2——2CO2+N2+6Cl+2H2O (3)
4) the step 3) water outlet adds Youxiaolin once more and carries out three sections alkaline chloride oxidations, reaction 30min.With being continued oxidation in two sections alkaline chloride oxidation processes by the cyanate of complete oxidation, realize the harmless treatment of prussiate fully, make in the waste water after the processing that CN-is stable to be lower than emission standard.This process can't be passed through step (3) and strengthen dosing, or the prolongation reaction times replaces.
Compared with prior art, advantage of the present invention is:
1, method of the present invention can effectively be removed the CN-in the high density cyanide wastewater, and the CN-clearance reaches more than 99.9%, and has overcome existing acidifying blow-off method and produce a large amount of hypertoxic HCN, and cost is higher, and controlled variable require high, defectives such as processing efficiency instability.
2, the present invention is primarily aimed at the high cyanide containing wastewater of CN-concentration greater than 300mg/L, has overcome the deficiency of prior art to the Study on Treatment for High Concentration Cyanide difficulty.
3, pre-treatment acidification reaction of the present invention mainly resolves into free state through acidification reaction with the CN-of complex state, directly adopts three sections alkaline chlorinations that the CN-of free state is decomposed into CO2 and N2 then.This treating processes increases the 3rd section alkaline chloride oxidation on the treatment process basis of the alkaline chlorating two-stage oxidizing of routine, treating processes is simple to operate, need not the strict condition control of stripping operation, and processing cost " stripping-alkaline chlorination process " is low.Through the medicament condition test, optimize each section dosing, guaranteed that under the dosing situation of minimum make processed waste water CN-concentration up to standard, treatment effect is stable.
Description of drawings
Fig. 1 is a high density cyanide wastewater treatment process course diagram according to the invention.
Embodiment
Below in conjunction with embodiment the present invention is done further explanation and explanation, the units/m3 among the embodiment represents in every m3 waste water the quality that adds material, represents like sulfuric acid 1.33kg/m3 that to add the vitriolic amount in every m3 waste water be 1.33kg.
Embodiment 1:
The cyanide wastewater concentration of this instance processes is 500mg/L.At first carry out pre-treatment, acidifying-precipitator method are adopted in pre-treatment, add the vitriol oil (98%) 1.33kg/m3 and make pH be controlled at 3.0.Acidization decomposes the Cu2+ that exists with [Cu (CN) 3] 2-form for being mainly under acidic conditions, form the deposition of cuprous cyanide, and CN-is existed with free state in water.Because CN-will have on a small quantity with HCN form and volatilization (HCN absorbs with alkali lye), so acid precipitation pre-treatment water outlet CN-has 4.97% volatilization removal approximately under sour environment.
Pretreated waste water is carried out three sections alkaline chloride oxidations through post precipitation.One section chloride oxidation control condition is pH=10.5 calcium hydroxide consumption 2.7kg/m3, Youxiaolin (available chlorine 10%) 5ml/L, reaction times 30min; Two sections chloride oxidation control conditions are pH=7.0 sulfuric acid consumption 0.4kg/m3, Youxiaolin (available chlorine 10%) 8ml/L, reaction times 30min; Three sections chloride oxidation control conditions are pH=7.0 sulfuric acid consumption 0.2kg/m3, Youxiaolin (available chlorine 10%) 3ml/L, reaction times 30min.
One section, two sections chloride oxidations are a tandem reactor process, and clearance is 98.17%, but in the water outlet CN-concentration still up to 26.22mg/L; Three sections chloride oxidations continue the incomplete reaction of oxidation on two sections basis, this section clearance is 98.17%, and final outflow water CN-concentration is 0.48mg/L.
This sewage treatment technology process figure is as shown in Figure 1, and wastewater treatment result and each section efficient are seen table 1.The total clearance 99.91% of CN-reaches " integrated wastewater discharge standard " (GB8978-1996) primary standard.
Each section of table 1 waste water treatment process treatment effect
Embodiment 2:
The cyanide wastewater concentration of this instance processes is 600mg/L.Concrete steps are with embodiment 1, and just controlled variable is different, and be specially: during pre-treatment, pH is controlled to be 2.5;
Three sections alkaline chloride oxidations.One section chloride oxidation control condition is pH=10 calcium hydroxide consumption 2.5kg/m3, Youxiaolin (available chlorine 10%) 6ml/L, reaction times 30min; Two sections chloride oxidation control conditions are pH=7.2 sulfuric acid consumption 0.39kg/m3, Youxiaolin (available chlorine 10%) 10ml/L, reaction times 30min; Three sections chloride oxidation control conditions are pH=7.1 sulfuric acid consumption 0.22kg/m3, Youxiaolin (available chlorine 10%) 5ml/L, reaction times 30min.
Wastewater treatment result and each section efficient are seen table 2.The total clearance 99.93% of CN-reaches " integrated wastewater discharge standard " (GB8978-1996) primary standard.
Each section of table 2 waste water treatment process treatment effect
Claims (7)
1. a high density cyanide wastewater treatment process is carried out pre-treatment with the high density cyanide wastewater earlier, and then pretreated waste water is carried out alkaline chloride oxidation, it is characterized in that:
Said pre-treatment is acidifying-precipitator method, and concrete steps are: at first in waste water, add sulfuric acid, the vitriolic consumption is so that the pH of waste water is 1.0-3.0 to be as the criterion, and reaction 10min-20min forms the deposition of cuprous cyanide, and makes other CN
-In water, exist with free state; Deposition is removed cuprous cyanide then, accomplishes the pre-treatment to waste water;
Said alkaline chloride oxidation is three sections alkaline chloride oxidations, and concrete steps are following:
(1) one section alkaline chloride oxidation: add calcium hydroxide at above-mentioned pretreated waste water; The consumption of calcium hydroxide is as the criterion at 10-11 with the pH of control waste water; The Youxiaolin that adds available chlorine >=10% again; Add-on is to add Youxiaolin 5ml-8ml in every liter of waste water, and reaction 20min-40min is oxidized to cyanate with free CN-in the water;
(2) two sections alkaline chloride oxidations: transfer pH at 6.5-7.5 the waste water behind one section alkaline chloride oxidation; The Youxiaolin that adds available chlorine >=10% again; Add-on is to add Youxiaolin 8ml-12ml in every liter of waste water; Reaction 20min-40min is oxidized to carbonic acid gas and nitrogen with the cyanate in the waste water;
(3) three sections alkaline chloride oxidations: repeat two sections alkaline chloride oxidation processes, make CN in the waste water after the processing
-Stablize and be lower than emission standard and get final product.
2. according to the said a kind of high density cyanide wastewater treatment process of claim 1, it is characterized in that said pre-treatment adopts the sulfuric acid adjust pH to 2.5-3.0.
3. according to the said a kind of high density cyanide wastewater treatment process of claim 1, it is characterized in that the pH of said one section alkaline chloride oxidation is 10.5, add Youxiaolin 5ml in every liter of waste water, the reaction times is 30min.
4. according to the said a kind of high density cyanide wastewater treatment process of claim 1, it is characterized in that the pH of said two sections alkaline chloride oxidations is 7, add Youxiaolin 8ml in every liter of waste water, the reaction times is 30min.
5. according to the said a kind of high density cyanide wastewater treatment process of claim 1, it is characterized in that the pH of said three sections alkaline chloride oxidations is 7, add Youxiaolin 3ml in every liter of waste water, the reaction times is 30min.
6. according to the said a kind of high density cyanide wastewater treatment process of one of claim 1-5, it is characterized in that CN in the said high density cyanide wastewater
-Concentration greater than 300mg/L.
7. according to the said a kind of high density cyanide wastewater treatment process of claim 6, it is characterized in that CN in the said high density cyanide wastewater
-Concentration be 300mg/L-700mg/L.
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| CN104163518A (en) * | 2014-05-15 | 2014-11-26 | 浙江海洋学院 | Printing and dyeing cyanide-containing wastewater treatment method |
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| CN106396201A (en) * | 2016-12-07 | 2017-02-15 | 云南大地绿坤环保科技有限公司 | Method for treating high-concentration organic cyanide-containing wastewater |
| CN106630069A (en) * | 2016-12-30 | 2017-05-10 | 四川师范大学 | Method for treating cyaniding and electroplating copper wastewater |
| CN106745669A (en) * | 2016-12-30 | 2017-05-31 | 四川师范大学 | The processing method of cyanide electroplating waste water |
| CN108137358A (en) * | 2015-10-29 | 2018-06-08 | 株式会社片山化学工业研究所 | The processing method of the waste water containing cyanide complex and the inorganic agent for this method |
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| CN112047525A (en) * | 2020-08-31 | 2020-12-08 | 营创三征(营口)精细化工有限公司 | Method and system for breaking cyanogen in resin |
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| CN104163518B (en) * | 2014-05-15 | 2016-07-06 | 浙江海洋学院 | A kind of processing method of cyanide wastewater of printing and dyeing |
| CN104402144A (en) * | 2014-12-02 | 2015-03-11 | 华侨大学 | Treatment method of cyanide-containing electroplating comprehensive wastewater |
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| CN106396201A (en) * | 2016-12-07 | 2017-02-15 | 云南大地绿坤环保科技有限公司 | Method for treating high-concentration organic cyanide-containing wastewater |
| CN106745669A (en) * | 2016-12-30 | 2017-05-31 | 四川师范大学 | The processing method of cyanide electroplating waste water |
| CN106630069A (en) * | 2016-12-30 | 2017-05-10 | 四川师范大学 | Method for treating cyaniding and electroplating copper wastewater |
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| CN112047525A (en) * | 2020-08-31 | 2020-12-08 | 营创三征(营口)精细化工有限公司 | Method and system for breaking cyanogen in resin |
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