CN106232531B - The processing method of waste water containing cyanogen and ammonia - Google Patents
The processing method of waste water containing cyanogen and ammonia Download PDFInfo
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- CN106232531B CN106232531B CN201580019750.6A CN201580019750A CN106232531B CN 106232531 B CN106232531 B CN 106232531B CN 201580019750 A CN201580019750 A CN 201580019750A CN 106232531 B CN106232531 B CN 106232531B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/20—Oxygen compounds of bromine
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—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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Abstract
Even if providing in the case where dissolubility concentration of iron is high, the processing method for the water containing cyanogen and ammonia that can also make cyanogen and ammonia sufficiently be decomposed.A kind of processing method of the waste water containing cyanogen and ammonia has the process that addition decomposes cyanogen and ammoxidation comprising hypobromous acid and/or hypochlorous chemical solution in the waste water containing cyanogen and ammonia.The liquid that bromide solution and aqueous hypochlorite solution mix and generate hypobromous acid and/or hypobromite is added in the waste water containing cyanogen and ammonia.Aqueous sodium bromide and aqueous sodium hypochlorite solution are mixed by equimolar ratio or in such a way that sodium hypochlorite is excessive and added.
Description
Technical field
The present invention relates to the processing methods containing cyanogen and the waste water of ammonia, more particularly to using Pomolio-Celdecor process improved method to containing
The method that the waste water containing cyanogen and ammonia of dissolubility iron is handled.
Background technique
Contain cyanogen as what is be discharged from industrial plants such as electroplate factory, steel plant, Metallurgical Factory, power plant, coke manufacturing works
Waste water processing method, at present most extensively adopted method be Pomolio-Celdecor process.In this method, by chlorine source, such as sodium hypochlorite
It is added in the waste water containing cyanogen under alkalinity, oxidation processes (patent document 1,2) is carried out to the cyanogen in waste water.
In the Pomolio-Celdecor process of patent document 1, reacted with 2 steps of pH and ORP (oxidation-reduction potential) controlling value as follows
Make cyanogen compound oxygenolysis.
First step reaction: 300~350mV of pH10 or more, ORP controlling value
NaCN+NaOCl→NaCNO+NaCl…(1)
Second step reaction: 600~650mV of pH7~8, ORP controlling value
2NaCNO+3NaClO+H2O→N2+3NaCl+2NaHCO3…(2)
It is described in patent document 2 by the water reuse containing cyanogen comprising free cyanogen, cyano complex and ammonia with small
In the method that the Pomolio-Celdecor process of the 2nd oxidation operation of 80 DEG C of the 1st oxidation operation and 80 DEG C or more this 2 step process is handled.
It is described in patent document 3 and handles the waste water containing cyanogen and ammonium ion in pH11 Pomolio-Celdecor process utilized above
Method.In the method for the patent document 3, after cyanogen compound decomposition reaction, still so that free residual cl concn is 0.1mg/L
Above mode adds chlorine source.Described in patent document 3, most of dissolubility iron in the waste water containing cyanogen and ammonium ion with
The form of iron cyano complex exists；The iron cyano complex is difficult to be decomposed in Pomolio-Celdecor process, therefore, useless containing cyanogen and ammonium ion
Dissolubility concentration of iron in water should be 0.4mg/L or less (the 0025th section of patent document 3).
Patent document 1: Japanese Unexamined Patent Publication 2001-269674
Patent document 2: Japanese Unexamined Patent Publication 2006-334508
Patent document 3: Japanese Unexamined Patent Publication 2013-208550
As recorded in patent document 3, in the case that the dissolubility concentration of iron in the waste water containing cyanogen and ammonium ion is high,
Cyanogen is not sufficiently oxidized decomposition in existing Pomolio-Celdecor process.
There is the alkaline agent for making the waste water containing cyanogen and ammonium ion become pH11 or more in the method for above patent document 3
The project of increased costs.And then there are the different risks for generating chlorine of the additive amount according to chlorine source.
Summary of the invention
It is a first object of the present invention to provide can make in the case that the dissolubility concentration of iron even if in waste water is high
The processing method for the waste water containing cyanogen and ammonia that cyanogen is fully decomposed.
It is a second object of the invention to provide cyanogen can be made to be sufficiently oxidized containing for decomposition even if pH11 or less
The processing method of the waste water of cyanogen and ammonia.
It includes time that the processing method of waste water containing cyanogen and ammonia of the invention, which has the addition in the waste water containing cyanogen and ammonia,
Bromic acid and/or hypochlorous chemical solution and the process for making cyanogen oxygenolysis.It should be noted that in the present invention, " ammonia " includes
" ammonium ion ".In addition, " cyanogen " expression " cyanide ion " and " cyanogen compounds such as cyano complex ".
In one embodiment of the present invention, chemical solution is substantially only comprising hypobromous acid and/or hypobromite as oxidant
Ingredient.In another way of the invention, chemical solution includes hypobromous acid and/or hypobromite and hypochlorous acid and/or hypochlorous acid
Salt is as oxidizer composition.
The effect of invention
In the processing method of waste water containing cyanogen and ammonia of the invention, by hypobromite ion, ammonia according to the following formula anti-
Decomposition should be oxidized.
OBr-+NH4 +→NH3Br++OH-…………………(3)
2NH3Br++OBr-→N2+3Br-+H2O+2H+………(4)
2NH4 ++3OBr-→N2+3Br-+3H2O+2H+………(5)
In addition, by the oxidisability of hypobromous acid, cyanogen is decomposed.
In the method for the present invention, such as (3) formula, hypobromite ion are reacted with ammonia, are generated bromo-amine (bromoamine), but bromo-amine
The oxidisability of chloramines than being generated by chlorine agent is strong.Therefore, can also cyanogen be made to decompose with bromo-amine.
It is few due to not adding chlorine agent or its additive amount in the present invention, caused by the reacting of bonding chlorine and organic matter
Cyanogen generation is prevented or suppressed, and is handled in such a way that cyanogen concentration is sufficiently lower.
In the present invention, iron cyano complex also the oxidation of the strength of dimension bromate ion, bromo-amine and be decomposed.Cause
This, in the case that the dissolubility concentration of iron in the waste water containing cyanogen and ammonia is up to 0.1mg/L or more, cyanogen is also fully divided
Solution.In addition, in pH11 hereinafter, cyanogen is also fully decomposed.
Specific embodiment
In the following, illustrating in further detail to the present invention.
In the present invention, for becoming the waste water containing cyanogen and ammonia of process object, steel plant wastewater is instantiated, electroplate factory gives up
The waste water containing cyanogen and ammonia such as water, electronics industry waste water, oil refinery waste water, but not limited to this.
In normal circumstances, the total cyanogen concentration of such waste water containing cyanogen and ammonia is 0.1~400mg/L or so, ammonia
Concentration 10mg/L or more is calculated as with ammonium ion, is, for example, 10~10000mg/L or so.In addition, pH is 6~10 or so.
Waste water containing cyanogen and ammonia is sometimes with the organic matter from coal, coke etc..The concentration of organic matter is usually 1mg/L
It above, is, for example, 1~1500mg/L or so.
The dissolubility iron for including in plant chimney stalk more than the pH neutrality containing cyanogen compound is most of with iron cyano complex
Form exist.In cyanogen compound oxidative decomposition according to the method for the present invention, iron cyano complex is also decomposed, therefore as this
Even if the waste water containing cyanogen of the process object of inventive method includes dissolubility iron 0.1mg/L or more, such as 0.1~5mg/L, outstanding
Its 1~3mg/L also fully can carry out resolution process to cyanogen and ammonia.
From the viewpoint of the generation for avoiding HCN gas, containing when adding hypobromous acid and/or hypobromite and being handled
The pH for having the waste water of cyanogen and ammonia is preferably 9 or more.
Make to add the ORP 400mV or more, preferably of the waste water containing cyanogen and ammonia after hypobromous acid and/or hypobromite
For 500mV or more.By making ORP 400mV or more, the oxidisability being able to maintain that in water system can decompose hard-decomposed iron
Cyano complex.It on the other hand, is 800mV hereinafter, preferably chemically from the perspective of reagent cost about the upper limit of ORP
650mV or less.
In the present invention, chemistry of the addition comprising hypobromous acid and/or hypobromite in such waste water containing cyanogen and ammonia
Solution decomposes cyanogen.
In one embodiment of the present invention, chemical solution is substantially only comprising hypobromous acid and/or hypobromite as oxidant
Ingredient.In another way of the invention, chemical solution includes hypobromous acid and/or hypobromite and hypochlorous acid and/or hypochlorous acid
Salt is as oxidizer composition.
As above-mentioned salt, sodium salt or sylvite, particularly preferred sodium salt can be enumerated.
Hypobromous acid or hypobromite preferably make hypochlorous acid or its salt (preferably sodium hypochlorite) and bromine and/or bromide, excellent
Sodium bromide is selected to react and generate.Hypochlorous acid and sodium bromide generate hypobromous acid according to the following formula with reaction with same mole.
HOCl+NaBr→HOBr+NaCl
Sodium hypochlorite and sodium bromide generate sodium hypobromite according to the following formula with reaction with same mole.
NaOCl+NaBr→NaOBr+NaCl
It should be noted that the hypochlorous acid reacted with bromine and/or bromide is also possible to make chlorine be dissolved in the water and generate
The hypochlorous water dissolved with chlorine.
For containing hypobromous acid and/or hypobromite or containing hypobromous acid and/or hypobromite and hypochlorous acid and/
Or the liquid (chemical solution) of hypochlorite is relative to the additive amount containing cyanogen and the waste water of ammonia, can side measure water-based ORP value
While being determined.Specifically, reaching 400mV or more as previously mentioned, being added to ORP value, preferably reaching 500mV or more.
When adding hypobromous acid and/or hypobromite and hypochlorous acid and/or hypochlorite in the waste water containing cyanogen and ammonia,
Make the 0.1~1.0 of the addition mole hypochlorous acid of hypobromous acid and/or hypobromite and/or the addition mole of hypochlorite
Again, particularly preferably 0.3~0.5 times.
For the processing containing cyanogen and the waste water of ammonia, can intermittently be carried out in slot；It can also make containing cyanogen and ammonia
Waste water be continuously flowed into reactive tank, and be allowed to continuously flow out from the reactive tank, carried out in the reactive tank cyanogen decompose it is anti-
It answers；It can also make the waste water flow ipe containing cyanogen and ammonia, add chemical solution in the pipeline and carry out pipeline.
In the present invention, can make the waste water containing cyanogen and ammonia water temperature become 40 DEG C or more, for example, 40~80 DEG C, especially
It is 50~70 DEG C or so, thus increases cyanogen decomposition reaction velocity.In order to inhibit heating cost, make 80 DEG C of water temperature or less, especially
Preferably 70 DEG C or less.
Embodiment
In the following, being illustrated to embodiment and comparative example.It should be noted that in the following examples and comparative example, it is molten
Solution property concentration of iron, ammonium concentration and total cyanogen analysis are measured according to JIS K 0102.Total residual chlorine and free residual chlorine
It is to be measured using DPD reagent and using the residual chlorine meter of Hach Company manufacture.
[embodiment 1 (utilizing the processing of the liquid containing sodium hypobromite)]
As test water, the steel plant wastewater of following water quality is used.
PH:8.3,
Total cyanogen concentration: 0.8mg/L,
Ammonium concentration: 532mg/L,
TOC:22mg/L,
Dissolubility iron: 1.3mg/L
ORP:90mV
For the liquid containing sodium hypobromite as chemical solution, using by the sodium bromide solution of 40wt% concentration and
The liquor natrii hypochloritis of 12wt% concentration mixes in a manner of NaBr:NaOCl=1:1 (molar ratio) and generates time of sodium hypobromite
Sodium bromate and aqueous sodium hypochlorite solution.
Test water 1000mL is stored in glass container, water temperature is held in 50 DEG C, so that pH is become 12 using NaOH
Later, above-mentioned chemical solution (sodium hypobromite and aqueous sodium hypochlorite solution) is added under conditions of table 1.By the anti-of cyanogen decomposition reaction
It is set as 1 hour between seasonable.
By chemical reagent additive amount (wherein, NaBr adding rate, the NaOCl adding rate of conversion back-to-back test water) and pass through
Free residual cl concn, ORP, total cyanogen concentration, total cyanogen resolution ratio, ammonium concentration and ammonium ion after the above-mentioned reaction time
Resolution ratio is shown in table 1.
[embodiment 2]
As test water, the steel plant wastewater of following water quality is used.
PH:8.15,
Total cyanogen concentration: 0.7mg/L,
Ammonium concentration: 354mg/L,
TOC:17mg/L,
Dissolubility iron: 1.4mg/L
ORP:230mV
For the liquid containing sodium hypobromite as chemical solution, liquid same as Example 1 is used.Moreover, removing
Become pH other than 9 using NaOH, is similarly to Example 1 handled.By chemical reagent additive amount, by previous reaction
Free residual cl concn, ORP, total cyanogen concentration, total cyanogen resolution ratio, ammonium concentration and ammonium ion resolution ratio after time show
In table 1.
[embodiment 3]
As test water, the steel plant wastewater of following water quality is used.
PH:8.6,
Total cyanogen concentration: 1.2mg/L,
Ammonium concentration: 410mg/L,
TOC:18mg/L,
Dissolubility iron: 1.0mg/L
ORP:264mV
Other than adding NaOH in such a way that pH becomes 9.6, water is tested in processing similarly to Example 2.Result is shown
In table 1.
[comparative example 1 (utilizing the processing of sodium hypochlorite)]
As test water, the steel plant wastewater of following water quality is used.
PH:8.7,
Total cyanogen concentration: 0.7mg/L,
Ammonium concentration: 451mg/L,
TOC:13mg/L,
Dissolubility iron: 1.3mg/L
ORP:230mV
It substitutes the liquid containing sodium hypobromite and uses sodium hypochlorite (12wt% aqueous solution), in such a way that pH becomes 11.1
Addition NaOH is added NaOCl with additive amount shown in table 1, in addition to this, similarly to Example 1 to test water
It is handled.Show the result in table 1.
[comparative example 2 (utilizing the processing of sodium hypochlorite)]
As test water, the steel plant wastewater of following water quality is used.
PH:8.7,
Total cyanogen concentration: 3.0mg/L,
Ammonium concentration: 120mg/L,
TOC:10mg/L,
Dissolubility iron: 0.1mg/L
ORP:210mV
It substitutes sodium hypobromite and uses sodium hypochlorite (12wt% aqueous solution), add NaOH in such a way that pH becomes 11.3,
It for NaOCl, is added with additive amount shown in table 1, in addition to this, test water is handled similarly to Example 1.
Show the result in table 1.
Table 1
Such as table 1, according to the Examples 1 to 3 for using the liquid containing sodium hypobromite, with the comparative example that sodium hypochlorite is used only
1, it 2 compares, cyanogen is fully decomposed.It should be noted that dissolubility concentration of iron it is high, using only the comparative example 1 of sodium hypochlorite
In, processing as a result, total cyanogen concentration than test water also increase.In the present invention, even if dissolubility concentration of iron is high, and even if small
Under conditions of pH11, cyanogen is also fully decomposed.
[embodiment 4 (utilizing the processing of the liquid containing sodium hypobromite)]
As test water, the steel plant wastewater of following water quality is used.
PH:8.2
Ammonium concentration: 410mg/L
TOC:21mg/L
Dissolubility iron: 0.8mg/L
ORP:187mV
As chemical solution (liquid containing sodium hypobromite and sodium hypochlorite), using the sodium bromide of 40wt% concentration is molten
Liquid is mixed in a manner of becoming NaBr:NaOCl=1:1 (molar ratio) with the aqueous sodium hypochlorite solution of 12wt% concentration and is generated secondary
The liquid of sodium bromate.
Test water 1000mL is stored in glass container, water temperature is held in 50 DEG C, so that pH is become 9.6 using NaOH
Later, above-mentioned chemical solution is added.It will be set as in reaction time 5 minutes.
By chemical reagent additive amount (wherein, NaBr adding rate, the NaOCl adding rate of conversion back-to-back test water) and pass through
Concentration of residual chlorine after the above-mentioned reaction time is shown in table 2.
[comparative example 3 (utilizing the processing of sodium hypochlorite)]
As chemical solution, sodium hypochlorite (12wt% aqueous solution) is added only with additive amount shown in table 2, in addition to this,
Same test water is handled similarly to Example 4.Show the result in table 2.
[embodiment 5~9 (utilizing the processing of the liquid containing sodium hypobromite)]
As test water, the steel plant wastewater of following water quality is used.
PH:8.3
Ammonium concentration: 532mg/L
TOC:22mg/L
Dissolubility iron: 1.3mg/L
ORP:90mV
As chemical solution (liquid containing sodium hypobromite or sodium hypobromite and sodium hypochlorite), using by 40wt%
The sodium bromide solution of concentration is mixed with the compounding amount of table 2 with the aqueous sodium hypochlorite solution of 12wt% concentration and generates sodium hypobromite
Liquid.
Test water 1000mL is stored in glass container, water temperature is held in 50 DEG C, so that pH is become 9.7 using NaOH
After (embodiment 5) or 9.6 (embodiments 6~9), sodium hypobromite aqueous solution is added.It will be set as in reaction time 5 minutes.
By chemical reagent additive amount (wherein, NaBr adding rate, the NaOCl adding rate of conversion back-to-back test water) and pass through
Concentration of residual chlorine after the above-mentioned reaction time is shown in table 2.
Table 2
Table 2-1
Table 2-2
<investigation>
Such as table 2, according to the embodiment 4~9 for being added to the liquid containing sodium hypobromite and sodium hypochlorite, even if dissolubility iron
Concentration is high, and compared with the comparative example 3 for only adding sodium hypochlorite, residual chlorine is also few.Thus, it can be known that being able to suppress halogen in the present invention
The generation of gas.
Although the present invention is illustrated in detail using specific mode, the intent and scope of the present invention are not departed from
It can make various changes, be apparent to those skilled in the art.
The Japanese patent application 2014-084692 that the application was proposed based on April 16th, 2014, full text pass through reference
It is incorporated herein.
Claims (3)
1. a kind of processing method of the waste water containing cyanogen and ammonia, having the addition in the waste water containing cyanogen and ammonia includes hypobromous acid
And/or the chemical solution of hypobromite, the process of cyanogen oxygenolysis is made at pH9~less than 11,
The chemical solution is to mix bromine and/or bromide solution with hypochlorous acid and/or aqueous hypochlorite solution and generate
The liquid of hypobromous acid and/or hypobromite, wherein the bromine and/or bromide and the hypochlorous acid and/or hypochlorite is mixed
Resultant is equimolar amounts,
Dissolubility concentration of iron in the waste water containing cyanogen and ammonia is 1mg/L or more.
2. the processing method of the waste water according to claim 1 containing cyanogen and ammonia, which is characterized in that bromide is bromination
Sodium, hypochlorite are sodium hypochlorite.
3. the processing method of the waste water according to claim 1 containing cyanogen and ammonia, which is characterized in that make ORP 400mV with
On.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2014084692A JP5867538B2 (en) | 2014-04-16 | 2014-04-16 | Treatment method for wastewater containing cyanide and ammonia |
| JP2014-084692 | 2014-04-16 | ||
| PCT/JP2015/058833 WO2015159653A1 (en) | 2014-04-16 | 2015-03-24 | Method for treating wastewater containing cyanogen and ammonia |
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| CN106232531A CN106232531A (en) | 2016-12-14 |
| CN106232531B true CN106232531B (en) | 2019-08-30 |
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| JP (1) | JP5867538B2 (en) |
| CN (1) | CN106232531B (en) |
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| CN106745961B (en) * | 2016-11-25 | 2019-03-01 | 中冶赛迪工程技术股份有限公司 | A kind of method and system of coking wastewater deep treatment decarburization decoloration decyanation |
| TWI690496B (en) * | 2019-02-01 | 2020-04-11 | 兆聯實業股份有限公司 | System of water treatment |
| CN109911975B (en) * | 2019-03-20 | 2020-12-01 | 江南大学 | Halamine macromolecular compound modified mesoporous material and preparation method and application thereof |
| CN111111086B (en) * | 2019-12-24 | 2021-06-11 | 东北大学 | Treatment method of cyanide-containing barren solution precipitation slag |
| CN113003800A (en) * | 2021-02-25 | 2021-06-22 | 上海金厦实业有限公司 | Wastewater quality-based treatment process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1503763A (en) * | 2001-03-02 | 2004-06-09 | Stabilised hypobromous acid solutions |
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| JPS60129182A (en) * | 1983-12-17 | 1985-07-10 | Hakutou Kagaku Kk | Method for preventing biological fault of service and waste water system |
| JP2716126B2 (en) * | 1987-07-10 | 1998-02-18 | 日本シリカ工業株式会社 | Slime control method |
| JPH07328663A (en) * | 1994-06-01 | 1995-12-19 | Japan Organo Co Ltd | Device for treating ammoniacal nitrogen-containing waste water |
| JPH08155463A (en) * | 1994-12-02 | 1996-06-18 | Permelec Electrode Ltd | Method and apparatus for decomposing ammoniacal nitrogen nitric-nitrogen and/or nitrous-nitrogen |
| EP1405827A4 (en) * | 2001-05-21 | 2005-08-17 | Mitsubishi Electric Corp | Process and apparatus for treating nitrogen compound containing water |
| US6994793B2 (en) * | 2002-04-19 | 2006-02-07 | Hydro-Trace Incorporated | Process for remediating ground water containing one or more nitrogen compounds |
| JP2005296863A (en) * | 2004-04-14 | 2005-10-27 | Ebara Kogyo Senjo Kk | Method for treating waste liquid containing thiourea and apparatus |
| JP4656379B2 (en) * | 2004-07-14 | 2011-03-23 | 栗田工業株式会社 | Method of treating wastewater containing iron cyanide |
| JP2006334508A (en) * | 2005-06-02 | 2006-12-14 | Nippon Parkerizing Co Ltd | Method and apparatus for simultaneously and continuously treating cyanide/ammonia-containing liquid waste continuously |
| JP5617862B2 (en) * | 2012-03-30 | 2014-11-05 | 栗田工業株式会社 | Cyanide wastewater treatment method |
| DE112013001804T5 (en) * | 2012-03-30 | 2014-12-11 | Kurita Water Industries Ltd. | Process for treating cyanide-containing wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1503763A (en) * | 2001-03-02 | 2004-06-09 | Stabilised hypobromous acid solutions |
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| CN106232531A (en) | 2016-12-14 |
| WO2015159653A1 (en) | 2015-10-22 |
| JP2015202482A (en) | 2015-11-16 |
| TW201607899A (en) | 2016-03-01 |
| JP5867538B2 (en) | 2016-02-24 |
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