CN102442736B - Nickel ion separation and recovery device for treating wastewater on surface of aluminium material - Google Patents
Nickel ion separation and recovery device for treating wastewater on surface of aluminium material Download PDFInfo
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- CN102442736B CN102442736B CN2010105038223A CN201010503822A CN102442736B CN 102442736 B CN102442736 B CN 102442736B CN 2010105038223 A CN2010105038223 A CN 2010105038223A CN 201010503822 A CN201010503822 A CN 201010503822A CN 102442736 B CN102442736 B CN 102442736B
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Abstract
A nickel ion separation and recovery device for treating wastewater on the surface of an aluminium material. By destroying the complexation of nickel ions and a complexing agent, the nickel ions are separated and recovered. The device provided by the invention contains a wastewater pool, a chemical reactor, a pH sensor, a pH instrument, first, second and third dosing mechanisms and an ion exchange device. The chemical reactor is connected with the wastewater pool so as to introduce the aluminium material surface treatment wastewater. The first dosing mechanism is used to add acid into the wastewater in the chemical reactor until the pH value of the aluminium material surface treatment wastewater is 2-2.5 indicated by the pH instrument. Therefore, metallic nickel and aluminium ions in complex form migrate away. The second dosing mechanism is used to add a proper amount of aluminium into the wastewater in the chemical reactor. The third dosing mechanism is used to add alkali into the chemical reactor until the pH value of the wastewater is adjusted to 5.5-6.5 indicated by the pH instrument. Thus, the complexing agent and aluminium ions form a complex, and non-complexing aluminium ions form precipitates. By an ion exchange technology, the nickel ions which are remained in the wastewater are finally adsorbed by the ion exchange device.
Description
Technical field
The present invention relates to the separating and reclaiming device of nickel ion in a kind of waste water, it is for the treatment of the waste water that contains aluminum ion, nickel ion and complexing agent that produces in the aluminium material surface treating processes.
Background technology
The aluminum and its alloy material has a series of good physics, chemistry, mechanics and processing characteristics, thereby is widely used in the fields such as decoration, building, traffic, aerospace.But the aluminum and its alloy material also exists the deficiency as aspects such as hardness, wear resistance, erosion resistances simultaneously.In order to overcome these shortcomings, must carry out necessary surface treatment.
Surface treatment generally comprises the operations such as degreasing, alkaline etching, neutralization, anodic oxidation, painted, sealing of hole.Surface treatment has improved the aluminium material surface performance, also produces all kinds of waste water simultaneously, and the waste water and the waste liquid that come from the production links such as painted and sealing of hole are exactly one of them.The characteristics of this class waste water are the complexing agents that contains metallic nickel ions, aluminum ion and multiple organic or inorganic.Along with improving constantly of environmental requirement, the metallic pollution problem of aluminium processing industry becomes increasingly conspicuous.In order to meet the requirement of environmental protection standard, most enterprises separates this class nickel-containing waste water and other waste water, individual curing.
Owing in waste water, containing a large amount of aluminum ions, therefore can't be by nickel from waste water, adsorbing separately such as the disclosed ion exchange technique of CN1762602.Therefore at first must be by nickel from waste liquid, separating.
General treatment technology is that such nickel-containing waste water is adjusted to alkalescence, makes nickel ion be converted into the nickel hydroxide precipitate thing.And then, by precipitation and filtration, waste water being divided into to the solid-liquid two-phase, the solid state hydrogen nickel oxide send the processed in units of qualification, liquid water discharging.Yet this routine techniques can not meet environmental requirement, and the phenomenon that exceeds standard of heavy metal nickel ion is very general.
Some investigators select the mode of extraction to separate from contain aluminium nickel liquid and reclaim nickel resources.For example TaiWan, China patent TW082107216 has mentioned a kind of extraction agent that can be used for aluminium, cobalt and nickel ion in the separate sulfur aqueous acid.In the patent such as JP08026124, US19930163481, mention, with extraction agent, nickel and cobalt are extracted to the method for Separation and Recovery from contain a large amount of aluminum ions aqueous solution.But there is the shortcoming that complex process, extraction agent are expensive, equipment cost is high in extraction process.
Summary of the invention
The present inventor finds through research, causes the reason that nickel ion exceeds standard to be to contain and can form with nickel ion the complexing agent of stable comple in the solution such as painted and sealing of hole, as citric acid, ammoniacal liquor, fluorion etc.Nickel ion in case with these complexing agent complexings after, very stable, hindered the formation of nickel hydroxide.This deliquescent complex state nickel causes that waste water exceeds standard.
In view of this, the present invention proposes a kind of aluminium material surface and processes the nickel ion of waste water and separate and retrieving arrangement, and this device is by destroying the complexing of nickel ion and complexing agent, separates and reclaims nickel ion.
The nickel ion that aluminium material surface proposed by the invention is processed waste water separates and retrieving arrangement, comprises wastewater disposal basin, chemical reactor, pH sensor, pH instrument, the first to the 3rd medicating mechanism and ion-exchange unit.Wastewater disposal basin is processed waste water in order to collect aluminium material surface.Chemical reactor connects this wastewater disposal basin, to introduce this aluminium material surface, processes waste water.The pH sensor is located in this chemical reactor.This pH sensor of pH Instrument connection.The first medicating mechanism adds acid in order to the waste water in this chemical reactor, until the pH value that aluminium material surface is processed to waste water is adjusted to 2～2.5, thereby it is free out to make to be in metallic nickel and the aluminum ion of complex state.The second medicating mechanism adds aluminium in order to the waste water in this chemical reactor, makes the ratio of volumetric molar concentration of aluminum ions volumetric molar concentration in waste water and complex state nickel ion more than or equal to 1.The 3rd medicating mechanism, in order to this chemical reactor, to add alkali, until the pH value of waste water is adjusted to 5.5～6.5, make complexing agent and aluminum ion form complex compound, and the aluminum ion of non-complex state forms precipitation.Ion-exchange unit connects this chemical reactor, inputs the waste water of this chemical reactor, and uses ion exchange technique absorption to be retained in the nickel ion in waste water.
In one embodiment of this invention, said apparatus can comprise a controller, connects this pH instrument and this first to the 3rd medicating mechanism, in order to control the dosing flow process.
In one embodiment of this invention, this chemical reactor is the gap reactor, after the pH value of wherein aluminium material surface being processed to waste water is adjusted to 2-2.5, and reaction 20-60 minute.In another embodiment, the gap reactor adds aluminium in waste water after, reaction 20-60 minute.
In one embodiment of this invention, this first medicating mechanism and this second medicating mechanism are same medicating mechanism, to add the acid anodic oxidation waste liquid of the aluminium material surface processing that contains acid and aluminium.In this embodiment, this chemical reactor is the gap reactor, after adding acid anodic oxidation waste liquid, and reaction 20-60 minute.
In one embodiment of this invention, said apparatus also comprises a sludge pump and a pressure filter, and this sludge pump connects this chemical reactor bottom and this pressure filter by pipeline, so that this precipitation is transported to this pressure filter, after this pressure filter should precipitate dehydration, waste water returned to this wastewater disposal basin.
The present invention, owing to adopting above technical scheme, makes it compared with prior art, has following remarkable advantage:
1, the qualified discharge of aluminium nickel waste water and the efficient recovery of nickel resources have been realized simultaneously.
2, adopt acidifying contact break technology to carry out pre-treatment to waste water, the coupled ion switching technology, thoroughly solve the difficult problem that the aluminium nickel waste water can't be up to standard.
The accompanying drawing explanation
For above-mentioned purpose of the present invention, feature and advantage can be become apparent, below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated, wherein:
Fig. 1 is the principle schema that the aluminium material surface of one embodiment of the invention is processed the nickel ion Separation and Recovery of waste water.
Fig. 2 is that the nickel ion of one embodiment of the invention separates and the retrieving arrangement schematic diagram.
Embodiment
Fig. 1 is the principle schema that the aluminium material surface of one embodiment of the invention is processed the nickel ion Separation and Recovery of waste water.With reference to shown in Figure 1, flow process is as follows:
Step S1, add acid, and the pH value of aluminium material surface being processed to waste water is adjusted to strongly-acid, and the pH value is 2-2.5, the reaction certain hour.This step utilizes aluminium material surface to process complexing agent commonly used, and for example citric acid, ammoniacal liquor, fluorion mostly lose or weaken the characteristics with the ability of complexing of metal ion under strong acidic condition, make the metallic nickel of complex state and aluminum ion free out.
Step S2, add appropriate aluminum ion (Al in waste water
3+), make it reach finite concentration.Like this, can utilize the characteristic of the complexing stability constant of aluminum ion and complexing agent commonly used greater than nickel ion, for the displacement of aluminium and nickel creates conditions.
Preferably, aluminum ions dosage should be according in waste water, by the nickel ion of complexing, being determined.Can be according to the molar concentration rate of aluminum ion and the complex state ratio-dependent more than or equal to 1: 1.In practical situation, need to determine dosage according to different water quality.Because complexing agent content relatively is difficult to determine, the way of therefore simplifying can add aluminum ion more than or equal to the ratio of 1: 1 according to the molar concentration rate of aluminum ion and all nickel ions (comprising complexing and not complexing).
Step S3, add alkali, regulates waste water to slightly acidic, and the pH value is 5.5-6.5.Waste water by strongly-acid in the process of slightly acidic transition, complexing agent forms complex compound with sufficient aluminum ion, and the aluminum ion of remaining non-complex state is due to (the Al (OH) of the difference with the nickel ion solubility product
3Solubility product 1.3 * 10
-33, Ni (OH)
2Solubility product 2.0 * 10
-15), will form aluminum hydroxide precipitation, nickel ion because of concentration and complex ability less than aluminum ion, still with simple Ni
2+State remaines among waste water.
Step S4, separate aluminum hydroxide precipitation with waste water.
In preferred embodiment, after the dehydration of the aluminium hydroxide solid of separation, can carry out extra harmlessness disposing.
Step S5, use ion exchange technique absorption to be retained in the nickel ion in waste water.
Nickel-containing wastewater ion through absorption can reach emission standard.On the other hand, after ion exchange resin is saturated, regenerate, the nickel concentrated solution that regeneration obtains, as the raw materials for production of nickel product, is realized resource circulation utilization.
Fig. 2 is that nickel ion separates and the retrieving arrangement schematic diagram according to an embodiment of the invention.This separation and retrieving arrangement, comprise wastewater disposal basin 10, step chemical reactor 20, pressure filter 30 and ion-exchange unit 40.Chemical reactor 20 is provided with pH sensor 21 and pH instrument 22, and first to fourth medicating mechanism 23-26.The pipeline that wastewater disposal basin 10 and chemical reactor are 20 is provided with the first water pump 51.The pipeline that chemical reactor 20 and ion-exchange unit are 40 is provided with the second water pump 52.The pipeline that chemical reactor 20 and pressure filter are 30 is provided with sludge pump 53.
In a preferred embodiment, can introduce automatic control flow chart.Specifically, use the controller (not shown) to connect pH instrument 22 and the first and the 3rd medicating mechanism 23,25, according to the pH value that pH instrument 22 provides, control the dosing flow process.In one embodiment, this controller can be built in pH instrument 22.
However, in one embodiment, still can control above-mentioned dosing flow process with the manpower monitoring instrument.
The aluminium dosage of the second medicating mechanism 24 can be according to nickel ion concentration current in waste liquid, aluminium ion concentration, and the nickel ion that will reach, aluminium ion concentration ratio preset.And, consider the fluctuation of chemical composition in waste liquid, the aluminium dosage preferably keeps certain allowance.
In another embodiment, the adding aluminium and also can automatically control of the second medicating mechanism 24, for example alum liquor, can set the speed of adding, and adds the time, valve automatic shutter etc.Correspondingly, controller is connected to chemical reactor 20 and the second medicating mechanism 24.
Ion-exchange unit 40 connects chemical reactor 20, inputs the waste water of this chemical reactor, and uses ion exchange technique absorption to be retained in the nickel ion in waste water.
In one embodiment, device can comprise a sludge pump 53 and a pressure filter 30.Sludge pump 53 connects bottom and the pressure filter 30 of chemical reactor 20 by pipeline, so that this aluminum hydroxide precipitation is transported to pressure filter 30.After pressure filter 30 will precipitate dehydration, waste water returned to wastewater disposal basin 10.
Below with reference to equipment shown in Figure 2, then the Separation and Recovery flow process of an embodiment is described.
At first, the waste water shunting of containing nickel ion, aluminum ion and multiple complexing agent is collected in independently wastewater disposal basin 10.Generally speaking, the pH value of waste water is greater than 3, and nickel ion concentration is 20-100mg/L, the about 20-50mg/L of aluminium ion concentration.But these numerical ranges are not fixed, but can be because of the variation of operating mode difference to some extent.
Waste water is input to chemical reactor 20.In waste water, add sour A, regulate the pH value to 2-2.5.And add aluminium C, make aluminium ion concentration reach 50-200mg/L.The visual nickel ion of aluminum ions concentration is different with complexing agent concentration and adjust.
Afterwards, reaction 20-60 minute, with acidifying, destruction complex compound, make metallic nickel become free ionic condition.Be understandable that, the reaction times of 20-60 minute also can start before adding aluminium, and this is equivalent with after adding aluminium, starting to react substantially.
Then, in chemical reactor 20, add alkali B, regulate the pH value to 5.5-6.5.At this moment, part aluminum ion and complexing agent complexing, but not the aluminum ion of complex state is converted into insoluble aluminium hydroxide, fully precipitates.In the pH of 5.5-6.5 value scope, the complex ability of aluminum ion and complexing agent is better than nickel ion, and in the situation that has enough aluminum ions to exist, nickel ion keeps being present in water with the simple ion state.
The aluminium hydroxide solid that is deposited in chemical reactor 20 bottoms carries out harmlessness disposing after sludge pump 53 is delivered to pressure filter 30 dehydrations after, the waste water of deviating from can return to wastewater disposal basin 10 to be continued to use.
After this, at ion-exchange unit 40, waste water reclaims through sodium type cationic exchange resin adsorption, and the water outlet nickel ion reaches the emission standard of 0.1mg/L, can discharge or be back to production.
After ion exchange resin is saturated, can regenerate, the nickel concentrated solution that regeneration obtains is realized recycle as the raw material of nickel products production.
In one embodiment, ion-exchange unit 40 can use the disclosed equipment of Chinese publication number CN 101186356A, and its ion-exchanger can separate with ion-exchange unit, in another place, to regenerate separately.
Aluminium material surface treating processes Anodic Oxidation is a critical process, anodic oxidation working solution main component is sulfuric acid and aluminum ion, after use for some time, because of sulfuric acid concentration, reduce and the necessary discharge unit of aluminium ion concentration rising, the sulfuric acid concentration of relief liquor is approximately 10%, and aluminum ions concentration is 20 grams per liters approximately.Therefore in a preferred embodiment, can be using the anodic oxidation waste liquid as above-mentioned acidifying and the required acid of displacement of aluminium nickel and aluminum ions medicament, reach the treatment of wastes with processes of wastes against one another, cost-saving purpose.
In addition, in the aluminum profile extrusion wastewater treatment, a large amount of aluminium hydroxide that produces also can be used as the required aluminum ions source of aluminium nickel displacement after simple process.
Below, then for the example of the practical application of a recovery process of the present invention.
In the surface treatment waste water of certain aluminium section bar processing enterprise, contain the wastewater collection of metallic nickel ions in the Nickel-bearing Waste pond, in waste water, contain metallic nickel ions 45.4mg/L, aluminium ion concentration 51.2mg/L, pH value 3-3.5, wherein contain influential nickel ion complexing agent up to standard (such as citric acid etc.).
At first, waste water enters a step chemical reactor 20 as shown in Figure 2, adds the anodic oxidation of this enterprise to scrap liquid A ', wherein contains aluminum ion 21g/L, and sulfuric acid concentration is 20%.The sulphur acid for adjusting pH value to 2.0 in liquid A ' is scrapped in utilization.PH regulator is controlled by online pH instrument 22.The aluminum ion of scrapping simultaneously in liquid A ' also enters waste water, makes the aluminum ion that contains in waste water total amount (waste water itself that contain with summation that scrap liquid and introduce) reach the 150mg/L left and right.Acidifying contact break reaction 60 minutes.Under strong acidic condition, the nickel of complex state is converted into the nickel ion of free state.
Then, the alkali lye B of automatic feeding such as sodium hydroxide, be adjusted to 6.5 by the pH value under the pH instrument is controlled.This moment, the part aluminum ion had precedence over nickel ion and complexing agent formation complex compound, and the residual Al ion forms aluminum hydroxide precipitation.Because most nickel ions under the condition of pH=6.5 are unconverted, be nickel hydroxide, and complexing agent is by the aluminum ion approach exhaustion, so metallic nickel is retained among waste water with the form of ion.
In waste water, add polymeric flocculant D, precipitate 1 hour, solid aluminum hydroxide is deposited to reactor 20 bottoms.Then be transported to pressure filter 30, after dehydration and drying, send the unit of qualification to carry out harmless treatment.
In addition, the nickel-containing waste water in reactor 20 is sent into the ion-exchange unit 40 that Zeo-karb is housed by the second water pump 52, and nickel ion is adsorbed on the cation exchange groups of resin.The water outlet nickel ion concentration of process ion-exchange, lower than 0.1mg/L, reaches the strictest emission standard.
After ion exchange resin is saturated, can entrust professional unit to regenerate, recover the resin of adsorption function and reuse.
In this application example, utilize the acid in manufacturing scrap liquid to realize simultaneously separating of acidifying decomplexing and aluminium nickel with aluminum ion, adopt ion exchange technique when nickel ion is reclaimed in absorption, to realize the qualified discharge of nickel ion.
In sum, the embodiment that aluminium material surface described in the invention is processed the nickel ion separating and reclaiming device of waste water, realized the qualified discharge of aluminium nickel waste water and the efficient recovery of nickel resources simultaneously.The advantage of these embodiment is, adopts acidifying contact break technology to carry out pre-treatment to waste water, and the coupled ion switching technology, thoroughly solve the difficult problem that the aluminium nickel waste water can't be up to standard.In addition, that in preferred embodiment, utilizes that enterprise produces contains the main medicament that aluminium spent acid and body refuse are processed as the acidifying contact break, and the treatment of wastes with processes of wastes against one another, can make processing cost cheap.
Although the present invention discloses as above with preferred embodiment; so it is not in order to limit the present invention, any those skilled in the art, without departing from the spirit and scope of the present invention; when doing a little modification and perfect, so protection scope of the present invention is worked as with being as the criterion that claims were defined.
Claims (7)
1. the nickel ion of an aluminium material surface processing waste water separates and retrieving arrangement, comprising:
Wastewater disposal basin, process waste water in order to collect aluminium material surface;
Chemical reactor, connect this wastewater disposal basin, to introduce this aluminium material surface, processes waste water;
The pH sensor, be located in this chemical reactor;
The pH instrument, connect this pH sensor;
The first medicating mechanism, add acid in order to the waste water in this chemical reactor, until the pH value that aluminium material surface is processed to waste water is adjusted to 2～2.5, thereby it is free out to make to be in metallic nickel and the aluminum ion of complex state;
The second medicating mechanism, add aluminium in order to the waste water in this chemical reactor, makes the ratio of volumetric molar concentration of aluminum ions volumetric molar concentration in waste water and complex state nickel ion more than or equal to 1;
The 3rd medicating mechanism, in order to this chemical reactor, to add alkali, until the pH value of waste water is adjusted to 5.5～6.5, make complexing agent and aluminum ion form complex compound, and the aluminum ion of non-complex state forms precipitation; And
Ion-exchange unit, connect this chemical reactor, inputs the waste water of this chemical reactor, and use ion exchange technique absorption to be retained in the nickel ion in waste water.
2. device as claimed in claim 1, is characterized in that, comprises a controller, connects this pH instrument and this first to the 3rd medicating mechanism, in order to control the dosing flow process.
3. device as claimed in claim 1, is characterized in that, this chemical reactor is intermittent reactor, after the pH value of wherein aluminium material surface being processed to waste water is adjusted to 2-2.5, and reaction 20-60 minute.
4. device as claimed in claim 1, is characterized in that, this chemical reactor is intermittent reactor, after wherein in waste water, adding aluminium, and reaction 20-60 minute.
5. device as claimed in claim 1, is characterized in that, this first medicating mechanism and this second medicating mechanism are same medicating mechanism, to add the acid anodic oxidation waste liquid of the aluminium material surface processing that contains acid and aluminium.
6. device as claimed in claim 5, is characterized in that, this chemical reactor is intermittent reactor, after adding acid anodic oxidation waste liquid, and reaction 20-60 minute.
7. device as claimed in claim 1, is characterized in that, also comprises a sludge pump and a pressure filter, this sludge pump connects this chemical reactor bottom and this pressure filter by pipeline, so that this precipitation is transported to this pressure filter, after this pressure filter should precipitate dehydration, waste water returned to this wastewater disposal basin.
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| CN2010105038223A CN102442736B (en) | 2010-10-08 | 2010-10-08 | Nickel ion separation and recovery device for treating wastewater on surface of aluminium material |
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| CN2010105038223A CN102442736B (en) | 2010-10-08 | 2010-10-08 | Nickel ion separation and recovery device for treating wastewater on surface of aluminium material |
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| CN102442736B true CN102442736B (en) | 2013-11-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018086750A1 (en) * | 2016-11-09 | 2018-05-17 | Dr. Ing. H.C. F. Porsche Aktiengesellschaft | Wastewater-processing method |
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| CN104030500B (en) * | 2014-06-03 | 2015-12-23 | 湖州上德水处理设备有限公司 | A kind of Processes and apparatus removing nickel ion in section aluminum waste water |
| CN105819593B (en) * | 2016-05-28 | 2018-09-28 | 嘉兴佳源多彩铝业有限公司 | The waste water treatment system and wastewater treatment method that industrial aluminum production of articles generates |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4009101A (en) * | 1973-03-29 | 1977-02-22 | Kayabakogyo-Kabushiki-Kaisha | Recycle treatment of waste water from nickel plating |
| JPS6125693A (en) * | 1984-07-13 | 1986-02-04 | Hitachi Ltd | Treatment of waste liquid containing heavy metal chelate |
| CN1371875A (en) * | 2001-02-28 | 2002-10-02 | 上海理日科技发展有限公司 | Complete set waste water treatment technology and automatic controller thereof |
| CN101148297A (en) * | 2007-08-29 | 2008-03-26 | 浙江大学 | Method for processing surface treatment integrated waste water |
| CN101456637A (en) * | 2008-11-25 | 2009-06-17 | 天津大学 | Treatment process and method of electroplating wastewater |
| CN201325915Y (en) * | 2008-12-30 | 2009-10-14 | 上海轻工业研究所有限公司 | Treatment device for nickel plating waste liquid and nickel plating rinse water containing complex |
| CN101864631B (en) * | 2010-03-25 | 2012-01-04 | 江阴市海江纱厂有限公司 | Aramid fiber and carbon fiber blended yarn and production method thereof. |
| CN201864631U (en) * | 2010-10-08 | 2011-06-15 | 上海轻工业研究所有限公司 | Nickel ion separating and recovering device for aluminum surface treatment waste water |
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| WO2018086750A1 (en) * | 2016-11-09 | 2018-05-17 | Dr. Ing. H.C. F. Porsche Aktiengesellschaft | Wastewater-processing method |
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