CN105174524B - Pretreatment unit and method before a kind of coking chemical waste water chemical oxygen demand detection - Google Patents
Pretreatment unit and method before a kind of coking chemical waste water chemical oxygen demand detection Download PDFInfo
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- CN105174524B CN105174524B CN201410252838.XA CN201410252838A CN105174524B CN 105174524 B CN105174524 B CN 105174524B CN 201410252838 A CN201410252838 A CN 201410252838A CN 105174524 B CN105174524 B CN 105174524B
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Abstract
Pretreatment unit and method before a kind of coking chemical waste water chemical oxygen demand detection, including heated at constant temperature rod, liquid level charactron, reaction chamber, pH analyzers, agitator and illumination plate, agitator, pH analyzers, heated at constant temperature rod and charge door are respectively equipped with reaction chamber, liquid level charactron is housed outside reaction chamber, it is front and rear to set up illumination plate separately.Coking chemical waste water injection reaction chamber after Fenton is handled, first adds sodium hydroxide solution, control solution is between 9 10；Heated at constant temperature rod is opened after adding solution of sodium bisulfite, 2 4h of reaction again, solution temperature is controlled at 45 55 DEG C, opens illumination plate, then is reacted after 4 6h, adds the concentrated sulfuric acid, pH value reacts 1 2h between 23.Agitator, heated at constant temperature rod and illumination plate are closed, deionized water is injected, i.e. sampling carries out COD after liquid level is recoveredcrDetermine.The present invention can effectively remove Oxidizing and Reducing Agents remaining in coking chemical waste water, the interference factor of the coking chemical waste water COD that eliminates the effects of the act detections, improve CODcrThe accuracy of testing result.
Description
Technical field
Carrying out chemistry the invention belongs to the coking chemical waste water after water-treatment technology field, more particularly to a kind of processing to Fenton needs
Pretreatment unit and preprocess method before oxygen amount (COD) detection.
Background technology
Coking industry can produce substantial amounts of coking chemical waste water, and its water quality is poisonous and harmful, and water fluctuation is very big, and COD therein refers to
Mark enjoys the concern of people.COD (COD) refers under certain condition, oxygen be consumed when handling water sample with strong oxidizer
The amount of agent, is as a result converted to the content of oxygen (in terms of mg/l).It is to characterize the comprehensive finger that reducing substances pollutes in water body
Mark, generally using potassium dichromate method measurement COD (CODcr)。
It has developed rapidly in recent years using chemical oxidation process Treatment of Wastewater in Coking, the selection of oxidant is also varied.It is double
Oxygen water (H2O2) it is a kind of oxidizing species, in the advanced treating and height of waste water in the form of Fenton (Fenton) oxidation system
It is used widely in the fields such as concentration organic wastewater with difficult degradation thereby processing.Although H2O2There is powerful oxidability, but in the reaction
Stronger oxidation material such as potassium permanganate is such as run into, it can then serve as reducing substances and be oxidized.So in National Standard Method, being used as oxygen
The potassium bichromate of agent can react with remaining hydrogen peroxide, so as to have a strong impact on the accuracy of its measurement result.
By taking the chemical plant of certain iron and steel enterprise in Liaoning Province as an example, given up using the coking after Fenton oxidation technique advanced treating
Water, the COD results detected using existing measurement standard always do not reach design requirement but.《Liaoning Province's provincial standard》(DB21/
1627-2008) allow concentration of emission to be 50mg/L the COD highests in waste water, therefore detect the true COD numbers of waste discharge
Value, the ecological environment around production run and protection for enterprise, all has important practical significance.
The content of the invention
The present invention is intended to provide a kind of can reduce the oxidant in coking chemical waste water to be detected, and reducing agent is set fully to divide
Solution, so that the interference factor that coking chemical waste water COD is detected after Fenton processing of eliminating the effects of the act, improves CODcrTesting result accuracy, very
Pretreatment unit and method before the coking chemical waste water chemical oxygen demand detection of real reflection water treatment effect.
Therefore, this invention takes following technical solution：
Pretreatment unit before a kind of coking chemical waste water chemical oxygen demand detection, it is characterised in that including heated at constant temperature rod, liquid level
Display tube, reaction chamber, pH analyzers, agitator and illumination plate, reaction chamber are a rectangular box for carrying case lid, and case lid center is set
Have and agitator is installed in poke hole, poke hole, flabellum is stirred close to reaction chamber bottom, poke hole one in the puddler lower end of agitator
Side determines and pH measure is respectively equipped with hole and bottoming hole provided with hole, opposite side is determined successively to charge door and bottoming hole is externally provided with
Instrument and heated at constant temperature rod, the liquid level charactron lower end outside reaction chamber are connected in the middle of the reaction chamber side wall of pH analyzers side
On position, two blocks of illumination plates are separately positioned on the front and back of reaction chamber.
Preprocess method before a kind of coking chemical waste water chemical oxygen demand detection, its specific processing method and process are：
Coking chemical waste water after Fenton oxidation is handled is injected in reaction chamber by charge door, carved by liquid level charactron
Degree shows liquid level position and constant volume.Under stirring, by adding hydroxide in coking chemical waste water of the charge door into reaction chamber
Sodium solution, makes coking chemical waste water pH value be maintained between 9.0-10.0；Then, solution of sodium bisulfite is added by charge door, it is sub-
The dosage of sodium bisulfate is identical with the dosage of hydrogen peroxide in Fenton processing procedure, and the reaction time was controlled at 2-4 hours,
Sodium hydrogensulfite is set fully to carry out redox reaction with hydrogen peroxide, by hydrogen peroxide Restore All；Reaction opens constant temperature after terminating
Heating rod, makes solution temperature be maintained at 45-55 DEG C, while opening illumination plate, reacts again on this condition 4-6 hours, promotes sub-
The decomposition of niter cake；After secondary response terminates, the concentrated sulfuric acid is added by charge door, solution ph is between 2-3, is continued
Reaction 1-2 hours, excludes the sulfur dioxide and sulfur trioxide dissolved in water；In above-mentioned addition solution and course of reaction, locate all the time
In under stirring.After third-order reaction terminates, close agitator, heated at constant temperature rod and illumination plate, by charge door injection go from
Sub- water, makes liquid level return to after the initial constant volume scale of liquid level charactron, you can sampling carries out potassium dichromate method COD and is
CODcrMeasure.
Beneficial effects of the present invention are：
After above-mentioned pretreatment, the oxidants such as hydrogen peroxide remaining in coking chemical waste water in reaction chamber can be both consumed,
The reducing agents such as removal sodium hydrogensulfite can be decomposed, and can guarantee that original organic species material in coking chemical waste water does not become
Change, and the presence of the concentrated sulfuric acid is for CODcrTesting result have no effect so that eliminate the effects of the act Fenton processing after coking chemical waste water
The interference factor of COD detections, improves CODcrThe accuracy of testing result, reflects the actual place of sewage treatment plant objective reality
Effect is managed, reliable data basis is provided for Optimizing Process Parameters.
Brief description of the drawings
Fig. 1 is pretreatment unit front view；
Fig. 2 is pretreatment unit top view；
Fig. 3 is pretreating process flow chart.
In figure：Reaction chamber 1, liquid level charactron 2, case lid 3, pH analyzers 4, agitator 5, charge door 6, heated at constant temperature rod 7,
Illumination plate 8, stirring flabellum 9.
Embodiment
Before Fig. 1,2, coking chemical waste water chemical oxygen demand detection of the present invention pretreatment unit mainly by reaction chamber 1,
Liquid level charactron 2, pH analyzers 4, agitator 5, heated at constant temperature rod 7 and illumination plate 8 are constituted.Agitator 4 includes motor, stirring
Bar and stirring flabellum 8, and motor speed can adjust.Reaction chamber 2 is a rectangular box for carrying case lid 3, in case lid 3
A poke hole is provided with heart position, the puddler of agitator 5 is stretched into poke hole, the stirring flabellum 9 of puddler lower end, which is located at, to be leaned on
The bottom center of proximal response case 1, to ensure that the mixing of the material in reaction chamber 1 is complete.It is provided with the left side of the poke hole of case lid 3
One determines hole, determines in hole and is installed on pH analyzers 4,；The right side of poke hole, on the right side of stirring centerline hole and reaction chamber 1
Centre position between wall is provided with a charge door 6, for filling coking chemical waste water and solution.Close to reaction on the right side of poke hole
It is provided with the position of the right side wall of case 1 in bottoming hole, bottoming hole and is fixed with heated at constant temperature rod 7.Liquid level charactron 2 is arranged on reaction chamber
Outside 1 left side wall, the lower end of liquid level charactron 2 is connected on the centre position of the left side wall of reaction chamber 1, upper end level and case lid 3
Upper surface is concordant, and liquid level charactron 2 can not only record the liquid level before reaction, and can be to reacted liquor capacity
Constant volume plays mark effect, so that it is guaranteed that the liquor capacity before and after reaction is consistent.Two blocks of illumination plates 8 are then separately positioned on reaction chamber
1 front and back, to provide another thermal source for coking chemical waste water so that the waste water inside reaction chamber 1 keeps fixing with solution
Temperature.
The specific method and process (see Fig. 3) pre-processed before coking chemical waste water chemical oxygen demand detection of the present invention be：
Coking chemical waste water after Fenton oxidation is handled is injected in reaction chamber 1 by charge door 6, passes through liquid level charactron
2 scales show liquid level position and constant volume.Under stirring, sodium hydroxide solution is added by charge door 6, makes coking chemical waste water pH
Value is maintained between 9.0-10.0；Then, solution of sodium bisulfite is added by charge door 6, solution of sodium bisulfite is added
Amount is identical with the dosage of hydrogen peroxide in Fenton processing procedure, and the reaction time was controlled at 2-4 hours, made sodium hydrogensulfite and dioxygen
Water fully carries out redox reaction, by hydrogen peroxide Restore All；Reaction opens heated at constant temperature rod 7 after terminating, and makes solution temperature
45-55 DEG C is maintained at, while opening illumination plate 8, is reacted again on this condition 4-6 hours, promotes the decomposition of sodium hydrogensulfite；Two
After secondary response terminates, the concentrated sulfuric acid is added by charge door 6, solution ph is between 2-3, continues to react 1-2 hours, excludes
The sulfur dioxide and sulfur trioxide dissolved in water；In above-mentioned addition solution and course of reaction, all the time under stirring.Three times
After reaction terminates, agitator 5, heated at constant temperature rod 7 and illumination plate 8 are closed, deionized water is injected by charge door 6, makes liquid level extensive
Arrive again after the initial constant volume scale of liquid level charactron 2, you can it is COD that sampling, which carries out potassium dichromate method COD,crMeasure.
Processing method of the present invention is described in detail with reference to embodiment.
Embodiment 1
First, the coking chemical waste water water sample injected into reaction chamber 1 after the processing of 2000mL Fentons, puts into the state of stirring
Sodium hydroxide solution, it is 9.0 to make coking chemical waste water pH.Thereafter, hydrogen peroxide is added to after coking chemical waste water according in Fenton technology
Concentration is 7.5mmol/L, therefore adding makes coking chemical waste water concentration be similarly 7.5mmol/L after sodium hydrogensulfite, in the shape of stirring
2h is reacted under state.Then so that water sample is in the state of illumination, and 45 DEG C of constant temperature is kept, is reacted in the state of stirring
4h.Finally use the concentrated sulfuric acid to adjust water sample pH for 2.0,1h is reacted in the state of stirring.
Embodiment 2
The coking chemical waste water water sample injected into reaction chamber 1 after the processing of 2000mL Fentons, puts into hydrogen-oxygen in the state of stirring
Change sodium solution, it is 9.5 to make its pH；Thereafter it is 7.5mmol/ according to hydrogen peroxide is added into concentration after coking chemical waste water in Fenton technology
L, therefore adding makes its concentration be similarly 7.5mmol/L after sodium hydrogensulfite, 3h is reacted in the state of stirring；Then so that water
Sample is in the state of illumination, and keeps 50 DEG C of constant temperature, and 5h is reacted in the state of stirring；Finally adjusted using the concentrated sulfuric acid
Water sample pH is 2.5, and 1.5h is reacted in the state of stirring.
Embodiment 3
The coking chemical waste water water sample injected into reaction chamber 1 after the processing of 2000mL Fentons, puts into hydrogen-oxygen in the state of stirring
Change sodium solution, it is 10.0 to make its pH；Thereafter it is according to hydrogen peroxide is added into concentration after coking chemical waste water in Fenton technology
7.5mmol/L, therefore adding makes its concentration be similarly 7.5mmol/L after sodium hydrogensulfite, 4h is reacted in the state of stirring；So
Afterwards so that water sample is in the state of illumination, and 45 DEG C of constant temperature is kept, 6h is reacted in the state of stirring；Finally using dense
Sulfuric acid regulation water sample pH is 3.0, and 2h is reacted in the state of stirring.
Water sample after above-mentioned processing is carried out to be settled to 2000mL, COD is then measured by samplingcr, the concrete outcome such as institute of table 1
Show.
The testing result of each embodiment of table 1 and contrast
As a result show, the oxidant that the present invention can be remained effectively in shield water is for CODcrInfluence during detection, is obtained
Obtain real numerical value.
Claims (1)
1. preprocess method before a kind of coking chemical waste water chemical oxygen demand detection, it is characterised in that described including pretreatment unit
Pretreatment unit includes heated at constant temperature rod, liquid level charactron, reaction chamber, pH analyzers, agitator and illumination plate, and reaction chamber is one
Rectangular box with case lid, case lid center is provided with poke hole, poke hole and is provided with agitator, the puddler lower end of agitator
Flabellum is stirred close to reaction chamber bottom, poke hole side to charge door and bottoming hole is externally provided with, is surveyed successively provided with hole, opposite side is determined
Determine to be respectively equipped with pH analyzers and heated at constant temperature rod in hole and bottoming hole, the liquid level charactron lower end connection outside reaction chamber exists
On the reaction chamber side wall centre position of pH analyzers side, two blocks of illumination plates are separately positioned on the front and back of reaction chamber, tool
Body processing method and process are：Coking chemical waste water after Fenton oxidation is handled is injected in reaction chamber by charge door, passed through
Liquid level charactron scale shows liquid level position and constant volume；Under stirring, pass through coking chemical waste water of the charge door into reaction chamber
In add sodium hydroxide solution, coking chemical waste water pH value is maintained between 9.0-10.0；Then, sulfurous acid is added by charge door
Hydrogen sodium solution, the dosage of solution of sodium bisulfite is identical with the dosage of hydrogen peroxide in Fenton processing procedure, reaction time control
System made sodium hydrogensulfite fully carry out redox reaction with hydrogen peroxide, by hydrogen peroxide Restore All at 2-4 hours；Reaction knot
Heated at constant temperature rod is opened after beam, solution temperature is maintained at 45-55 DEG C, while opening illumination plate, 4-6 is reacted again on this condition
Hour, promote the decomposition of sodium hydrogensulfite；After secondary response terminates, the concentrated sulfuric acid is added by charge door, solution ph is in
Between 2-3, continue to react 1-2 hours, exclude the sulfur dioxide and sulfur trioxide dissolved in water；Above-mentioned addition solution and reacted
Cheng Zhong, all the time under stirring；After third-order reaction terminates, agitator, heated at constant temperature rod and illumination plate are closed, passes through charging
Mouth injection deionized water, makes liquid level return to after the initial constant volume scale of liquid level charactron, you can sampling carries out potassium dichromate method
It is COD to learn oxygen demandcrMeasure.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374520A (en) * | 2001-02-02 | 2002-10-16 | 饭岛电子工业株式会社 | Method for measuring chemical oxygen requirement and its apparatus |
| CN101694471A (en) * | 2009-10-15 | 2010-04-14 | 承慰才 | Drinking water COD online automatic detection method and detection instrument |
| CN203922898U (en) * | 2014-06-09 | 2014-11-05 | 鞍钢股份有限公司 | Pretreatment unit before a kind of coking chemical waste water chemical oxygen demand detection |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| ZA915130B (en) * | 1990-07-04 | 1993-01-27 | Commw Scient Ind Res Org | Continuous rbcod measurement |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374520A (en) * | 2001-02-02 | 2002-10-16 | 饭岛电子工业株式会社 | Method for measuring chemical oxygen requirement and its apparatus |
| CN101694471A (en) * | 2009-10-15 | 2010-04-14 | 承慰才 | Drinking water COD online automatic detection method and detection instrument |
| CN203922898U (en) * | 2014-06-09 | 2014-11-05 | 鞍钢股份有限公司 | Pretreatment unit before a kind of coking chemical waste water chemical oxygen demand detection |
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