CN101402496A - Clean production process for treating electroplating poaching water with nona-filtering method - Google Patents
Clean production process for treating electroplating poaching water with nona-filtering method Download PDFInfo
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Abstract
一种一步纳滤法处理电镀漂洗水的清洁生产方法，属于电镀废水资源化处理技术领域。本发明包括预处理和纳滤浓缩工艺以及浓缩液回用方法，二价离子的截留率大于98％，料液可浓缩至22000mg/L，透过液可直接回用于漂洗槽，浓缩液可回用于电镀槽或经活性碳、弱电流电解、化学提纯中的一种或几种处理除去杂质回用于各种电镀工艺槽。本发明真正意义上做到电镀废水完全回用，实现了零排放的清洁生产工艺；采用纳滤膜处理电镀漂洗水，即使在较高的浓度下，仍保持较高的膜通量，具有流程简单、投资小、操作费用低、物料分配合理的特点，尤其适用于电镀工业应用。
The invention discloses a clean production method for treating electroplating rinsing water by a one-step nanofiltration method, belonging to the technical field of electroplating wastewater resource treatment. The invention includes pretreatment and nanofiltration concentration process and concentrated liquid reuse method, the interception rate of divalent ions is greater than 98%, the feed liquid can be concentrated to 22000 mg/L, the permeated liquid can be directly returned to the rinse tank, and the concentrated liquid can be It can be reused in electroplating tanks or treated by one or more of activated carbon, weak current electrolysis, and chemical purification to remove impurities and reused in various electroplating process tanks. In the true sense, the invention achieves the complete reuse of electroplating wastewater and realizes the clean production process of zero discharge; the nanofiltration membrane is used to treat the electroplating rinsing water, and even at a higher concentration, it still maintains a higher membrane flux and has a process flow The characteristics of simplicity, small investment, low operating cost and reasonable material distribution are especially suitable for electroplating industrial applications.
Description
Technical field
A kind of clean preparation method of process for treating electroplating poaching water with nona-filtering belongs to electroplating wastewater processing and resource recovery technology field.The present invention adopts nanofiltration membrane, single stage method concentration electroplating rinse water.See through liquid and be back to rinse tank, concentrated solution is back to plating tank after simple process, reclaimed water resources and heavy metal resources fully, truly accomplishes the process for cleanly preparing of process zero release.
Background technology
Can produce the waste water that contains heavy metal ion in a large number in the electroplating industry rinse cycle, heavy metal ion can generate water-soluble salt with multiple inorganics, organism complexing, and discharging pollutes the environment harm humans health arbitrarily.If the heavy metal ion in these waste water can be effectively by enrichment, rinse water just might be recycled.Handling at present with the main method that reclaims heavy metal has: chemical reduction precipitation, absorption, little electrolysis, evaporation, membrane sepn and ion-exchange etc.[[1] Hatfield T L, Kelvin T L, Pierce D T.Electrochemicalremediation of metal-bearing waste waters.Part 1:Copper removal form simulateddrainage waters[J] .Journal of Applied Electrochemical, 1996,26:567-574.[2] Tu Zhenmi, Li Deyu, Li Ning, Pan Li, Zhang Jingshuan. present situation and progress [J] that chemical nickle-plating wastewater is handled. electroplate and environmental protection, 2003,23 (2): 1-5.[3] DKNY Na, Ma Shaojian. cobalt in the waste material, the recovery of nickel [J]. coloured mining and metallurgy, 2005,21 (7): 113-114.], there are the following problems in these traditional technologies: (1) needs heavy dose of chemical substance; (2) eliminated the possibility of the heavy metal ion that directly is recycled; (3) need the mud of processing to contain a large amount of organism and heavy metal, form new solid pollutant, also quite difficult during processing.
In recent years, adopt membrane separation technique to handle electroplating wastewater and obtain extensive studies, especially nanofiltration (NF) technology, since coming out, received people's very big concern always, and [[4] Petersen R J.Composite reverse osmosis and nanofiltration membrane[J] the .J MembrSci that is widely used rapidly, 1993,83:81.[5] Rautenbach R, Groschl A.Separation potential of nanofiltrationmembranes[J] .Desalination, 1990,77:73-84.].Nanofiltration membrane has following distinguishing feature in application: sieve effect is held back or held back to (1) physics, can hold back less dissolved constituent effectively; (2) charge [[6] Wang X L, Tsuru T, Nakao S, etal.Electrolyte transport throughnanofiltration membranes by the Space-charge model and the comparison withTeorell-Meyer-Sievers model[J] .J Membr Sci, 1995,103:117-133.], be that selectivity is held back, rejection to univalent ion lower (40%～80%) [[7] Ding Huanru, Du Fangzheng, Wang Lihai. application present situation and the prospect [J] of membrane technique in China's water treatment of power plant. Shanghai University Of Electric Power's journal, 2002,18 (3): 271.], rejection to divalence and polyvalent ion is then higher, so can hold back most of heavy metal ion, realizes the enrichment of heavy metal ion, can replace the desalination in traditional engineering, a plurality of steps such as concentrate, so both economical; (3) to compare working pressure low with reverse osmosis, see through big [[8] the Xu Y Z of flow rate, Lebrun R E.Comparison of nanofiltration properties of two membranes using electrolyte andnon-electrolyte solutes[J] .Desalination, 1999,122:95-106.].(4) compare with the treatment process that method of evaporation or other have " mutually " to become, embrane method do not have " phase " to become, thereby energy consumption is low to the treating processes of electroplating wastewater; (5) nano filtering process treatment facility floor space is little, facility compact, easily automatic control, but operate continuously.
Utilize membrane separating method to handle the method for Electroplating Production waste water at present, as Chinese patent application number be 03157655.9 " membrane separating method of electroplating wastewater processing zero release ", disclose the method that a kind of electroplating wastewater is administered, this method will be passed through the one-level nanofiltration again through pretreated electroplating wastewater, the condensed water that obtains after the nanofiltration continues to concentrate through secondary brackish water reverse osmosis membrane, condensed water is separated concentrated at last through three grades of seawater reverse osmosis membranes, and provide the example of an electronickelling wastewater treatment, operate at normal temperatures through total system, electronickelling waste water has been concentrated about 100 times.This technology has overcome the deficiency of traditional method, but for industrial application complicated operation, the production cost height, technology is loaded down with trivial details.Inventor's early-stage Study achievement patent 200610096133.9, adopting and holding back relative molecular mass is 80Da's
-S type nanofiltration membrane, processing contains Ni
2+Electroplating wastewater, Ni
2+The ionic rejection is greater than 99%, and feed liquid can be concentrated into 17000mg/L, and dope reaches the requirement of direct reuse in plating tank.In the concentration process 87.5% see through liquid divalent ion concentration less than 1.0mg/L, 9.62% see through liquid Ni
2+Ionic concn is less than 2.3mg/L, but this two-part liquid direct reuse that sees through in rinse tank, 2.88% see through liquid Ni
2+Ionic concn is less than 15mg/L, can with the feed liquid parallel feeding.Even under higher concentration ratio, still keep higher membrane flux, but the reuse technology of dope is subjected to some restrictions.
So the present invention adopts a step Nanofiltering membrane to handle and concentrates electroplating rinse water, dope is applicable to the reuse requirement of different electroplating technologies; It is simple to have technology, invests for a short time, and production cost is low, and recycle-water and heavy metal ion resource fully reach the process for cleanly preparing of process zero release.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, providing a kind of utilizes a new step nano filtering process to handle the method that concentrates electroplating rinse water, both can save the electroplating industry water resources, can make full use of heavy metal resources again, eliminate the production cost of pollution on the environment and reduction electroplating industry, realize the cleaner production of electroplating technology.
According to technical scheme provided by the invention, the clean preparation method of described treating electroplating waste water by nano filtering process comprises:
A, nanofiltration membrane concentrating and separating: electroplating wastewater is carried out concentrating and separating with nanofiltration membrane, working pressure is 0.8MPa～2.4MPa, see through liquid as the rinse water reuse for what the divalent ion concentration of electroplating wastewater after nanofiltration membrane treatment was less than or equal to 3mg/L, for bivalent ions concentration greater than 3mg/L see through liquid and the charging electroplating wastewater is mixed into nanofiltration membrane treatment; Bivalent ions rejection greater than 98%, is reached as high as more than 99.5%;
B, concentrated solution reuse: the nanofiltration membrane concentrated solution is back in the plating tank and uses; Or handle, remove to be back in the plating tank again behind the impurity through one or more processing modes in the following step and use; Described processing mode comprises: activated carbon, weak current electrolysis and with purifying with acid solution again after the alkali solution precipitate, and remove impurity and be back in the plating tank and use.
Before the nanofiltration membrane concentrating and separating, earlier electroplating wastewater is carried out pre-treatment: cause electroplating wastewater that nanofiltration membrane pollutes with in strainer, activated carbon adsorption, the ultra-filtration membrane one or more to meeting, remove the impurity such as the anode sludge, debris particle impurity, suspended substance and organism in the electroplating wastewater.
Handled electroplating wastewater is the electroplating wastewater that contains divalence or trivalent metal ion.It is 80Da～200Da that nanofiltration membrane characterizes trapped molecular weight.Described alkaline solution is one or more solution in sodium hydroxide, potassium hydroxide, yellow soda ash and the salt of wormwood; Described acid solution is one or more solution in sulfuric acid, hydrochloric acid, the nitric acid.
The used equipment of aforesaid method is as follows:
Water outlet at water pump utilizes the pipe connection pretreater; The electroplating wastewater that causes nanofiltration membrane to pollute to meeting is removed the anode sludge, debris particle impurity, suspended substance and organism in the electroplating wastewater with pretreater;
Outlet at pretreater utilizes pipe connection to concentrate liquid bath;
Connect topping-up pump and stage pump in the outlet that concentrates liquid bath;
Utilize pipe connection nanofiltration membrane concentrating and separating device at multistage pump outlet, electroplating wastewater is carried out concentrating and separating with nanofiltration membrane; Divalent ion concentration is set on the nanofiltration membrane concentrating and separating device is less than or equal to exporting of 3mg/L through liquid, and divalent ion concentration exporting greater than 3mg/L through liquid, and utilize pipeline to be connected with concentrated liquid bath in the liquid outlet that sees through that divalent ion concentration is less than or equal to 3mg/L, utilize pipeline and be connected in of the liquid outlet that sees through of divalent ion concentration, and on described pipeline, under meter is set respectively through liquid bath greater than 3mg/L.
Compared with prior art, beneficial effect of the present invention is embodied in:
1, since this nanofiltration membrane to hold back relative molecular mass little of 80Da, so can hold back most of organism substantially, and through checking, it can hold back the divalent ion greater than 98%; In the operating process, need not to add chemical substance, do not have phase transformation; Seeing through liquid can complete-reclaiming, can not cause secondary pollution; And flow process is simple, less investment, equipment take up an area of little, process cost is low.
2, system adopts the method for nanofiltration, electroplating rinse water can be concentrated, and concentrated solution is directly got back to plating tank, and salt such as most of sodium-chlor etc. at a low price see through membrane element, and Ni
2+Be trapped concentratedly, the solution after concentrating can direct reuse be done to produce to full light nickel plating tank and is used; Or concentrated solution NaOH solution-treated, produce throw out, throw out is separated from solution, to throw out H
2SO
4After solution-treated and the purification, obtain highly purified single nickel salt, can be back to plating tanks such as mute nickel; Or, obtain highly purified nickelous chloride to throw out usefulness HCl solution-treated and after purifying, can be back to the chemical nickel plating tank; Go for the heavy metal resources reuse of various electroplating technologies, see through liquid as the rinse water reuse, reclaim the process for cleanly preparing of factory effluent reuse for electroplating industry provides a kind of waste chemicals, reduced the pollution of producing, realized the zero release of electroplating wastewater environment.
3, after the inventive method was handled, total reclamation rate of water was greater than 90% in the electronickelling waste water, and the rate of recovery of heavy metal resources is greater than 95%.
Description of drawings
Fig. 1 process flow diagram.
Fig. 2 process unit synoptic diagram.
Embodiment
As shown in Figure 2: the water outlet at water pump 1 utilizes pipe connection pretreater 2; The electroplating wastewater that causes nanofiltration membrane to pollute to meeting is removed the anode sludge, debris particle impurity, suspended substance and organism in the electroplating wastewater with pretreater;
Outlet at pretreater 2 utilizes pipe connection to concentrate liquid bath 3;
Connect topping-up pump 4 and stage pump 5 in the outlet that concentrates liquid bath 3;
Outlet at stage pump 5 utilizes pipe connection nanofiltration membrane concentrating and separating device 6, and electroplating wastewater is carried out concentrating and separating with nanofiltration membrane; Divalent ion concentration is set on nanofiltration membrane concentrating and separating device 6 is less than or equal to exporting of 3mg/L through liquid, and divalent ion concentration exporting greater than 3mg/L through liquid, and utilize pipeline to be connected with concentrated liquid bath 3 in the liquid outlet that sees through that divalent ion concentration is less than or equal to 3mg/L, utilize pipeline and be connected in of the liquid outlet that sees through of divalent ion concentration, and on described pipeline, under meter 8 is set respectively through liquid bath 7 greater than 3mg/L.
Waste water enters pretreater 2 through water pump and carries out pre-treatment, after pre-treatment, enter and concentrate in the liquid bath 3, deliver to nanofiltration membrane concentrating and separating device 6 through topping-up pump 4 and stage pump 5 again and carry out nanofiltration and handle, the liquid that sees through after the processing enters through in the liquid bath 7, and the concentrated solution after the processing is back to and concentrates in the liquid bath 3.
The present invention is based on the application of nanofiltration, its theoretical foundation is: sieve effect is held back or held back to (1) physics, can hold back less dissolved constituent effectively; (2) charge, promptly selectivity is held back, and to the rejection lower (40%～80%) of univalent ion, thereby can reduce the enrichment of univalent ion in plating tank, and the reuse that improves concentrated solution is worth.To the rejection of divalence and polyvalent ion then higher (more than 98%),, realize the enrichment of metal ion so can hold back most of heavy metal ion.
Technical scheme of the present invention is as follows:
1), the pre-treatment of electroplating wastewater
To can not causing the electroplating wastewater of the comparison cleaning that nanofiltration membrane pollutes, need not pre-treatment, directly carry out nanofiltration and handle; To the electroplating wastewater that causes nanofiltration membrane to pollute easily, for example contain the anode sludge, debris particle impurity or turbidity greater than the waste water of 4NTU with pretreater 2 (comprising deep bed filter, fabric filter, micro-filtration, sand filtration etc.) the filtering anode sludge and debris particle impurity; To containing the organism in the organic waste water usefulness activated carbon adsorption filtered wastewater; With the suspended substance in the ultra-filtration membrane filtering waste water.With in the strainer, activated carbon adsorption, ultra-filtration membrane one or more, remove one or more materials in the anode sludge, debris particle impurity, suspended substance and the organism in the waste water according to water quality characteristics.
2), nanofiltration membrane concentrating and separating
To be used for concentrating and separating with the nanofiltration membrane of holding back relative molecular mass 80Da～200Da through pretreated waste water, working pressure is 0.8MPa～2.4MPa, the liquid that sees through that is less than or equal to 3mg/L for divalent ion concentration can be used as the rinse water reuse, is mixed into nanofiltration processing greater than the liquid that sees through of 3mg/L with feed liquid for divalent ion concentration; Concentrated solution is got back to plating tank and is used; To bivalent ions rejection greater than 98%.
3), concentrated solution reuse
But nanofiltration membrane concentrated solution direct reuse is in plating tank or through one or more methods in purifying with acid solution again after activated carbon, weak current electrolysis and the alkali solution precipitate, removes impurity and is back in the plating tank and uses.
Below in conjunction with accompanying drawing the specific embodiment of the present invention is elaborated.
Figure 1 shows that the technical process of the embodiment of the invention, as shown in Figure 1, comprise pre-treatment, nanofiltration membrane separation, concentrated solution and see through the liquid reuse.
Handle to electroplate and contain Ni
2+Waste water
1, pre-treatment
At first with Ni
2+Concentration be that the electronickelling waste water of 4000mg/L is through 5 μ m cloth envelop collectors, with the big suspended impurity elimination of the anode sludge in the waste water, fragment etc.; Then adopt the most of organism in the active carbon adsorption absorption waste water, alleviate the pollution of organism membrane module; Pass through ultra-filtration equipment again, under 0.1MPa, waste water is further separated, remove suspended substance tiny in the waste water, thus the effect of playing the protective membrane element, prolonging its work-ing life.
2, nanofiltration membrane separation
Enter nanofiltration membrane concentrating and separating device 6 through pretreated waste water by topping-up pump 4, stage pump 5 under 2.0MPa pressure and separate, this nanofiltration membrane is that U.S. KOCH company produces
It is 80 (dalton) that-S type nanofiltration membrane, its relative molecular mass are held back scope, and nanofiltration membrane surface lotus positive electricity has different Donnan current potentials to the ion of different electric charges and different valence state, and surface characteristic that nanofiltration membrane is exclusive and aperture have determined its particular performances.It is lower to the monovalent ion rejection, and divalent ion is had higher rejection, promptly the metal ion of different valence state is had selectivity and holds back.The nanofiltration membrane that native system adopts is at 2.0MPa pressure, and is lower to the rejection of sodium-chlor, have only about 20%, and can be up to more than 99% to bivalent ions rejection.Most sodium-chlor sees through membrane element, and Ni
2+Be trapped concentratedly, the solution after concentrating can make to produce usefulness to light nickel plating tank by direct reuse; Concentrated solution NaOH solution-treated produces throw out, throw out is separated from solution, to throw out H
2SO
4After solution-treated and the purification, obtain highly purified single nickel salt, can be back to plating tanks such as mute nickel; Throw out with the HCl solution-treated and after purifying, is obtained highly purified nickelous chloride, can be back to the chemical nickel plating tank.In order to alleviate the pollution of face, prolong the work-ing life of film, clear water regularly washes device, and the flux recovery is good.After the process nanofiltration system concentrates, Ni
2+Concentration reaches 22000mg/L, to Ni
2+Rejection can be greater than 99%.
The method of the embodiment of the invention has certain for property.Electroplating wastewater for other divalence or trivalent metal ion can directly be suitable for, as electroplating Zn
2+, Cu
2+Or Cr
3+Waste water.
Claims (6)
1, a kind of clean preparation method for the treatment of electroplating waste water by nano filtering process is characterized in that:
A, nanofiltration membrane concentrating and separating: electroplating wastewater is carried out concentrating and separating with nanofiltration membrane, and working pressure is 0.8MPa～2.4Mpa; See through liquid as the rinse water reuse for what electroplating wastewater divalent ion concentration after nanofiltration membrane treatment was less than or equal to 3mg/L, for divalent ion concentration seeing through liquid and entering nanofiltration membrane treatment again after the charging electroplating wastewater mixes greater than 3mg/L; To bivalent ions rejection greater than 98%;
B, concentrated solution reuse: the liquid direct reuse that sees through that divalent ion concentration is less than or equal to 3mg/L uses in plating tank; Or handle through one or more processing modes in the following step, remove to be back in the plating tank again behind the impurity and use; Described processing mode comprises: activated carbon, weak current electrolysis or with purifying with acid solution after the alkali solution precipitate again;
2, the clean preparation method for the treatment of electroplating waste water by nano filtering process according to claim 1, it is characterized in that: before the nanofiltration membrane concentrating and separating, earlier electroplating wastewater is carried out pre-treatment: cause electroplating wastewater that nanofiltration membrane pollutes with in strainer, activated carbon adsorption, the ultra-filtration membrane one or more to meeting, remove the anode sludge, debris particle impurity, suspended substance and organism in the electroplating wastewater.
3, method according to claim 1 is characterized in that: handled electroplating wastewater is the electroplating wastewater that contains divalence or trivalent metal ion.
4, method according to claim 1 is characterized in that: it is 80Da～200Da that nanofiltration membrane characterizes trapped molecular weight.
5, method according to claim 1 is characterized in that: described alkaline solution is one or more solution in sodium hydroxide, potassium hydroxide, yellow soda ash and the salt of wormwood; Described acid solution is one or more solution in sulfuric acid, hydrochloric acid, the nitric acid.
6, according to the equipment that uses in the described method of claim 1, it is characterized in that: the water outlet at water pump utilizes the pipe connection pretreater; The electroplating wastewater that causes nanofiltration membrane to pollute to meeting is removed the anode sludge, debris particle impurity, suspended substance and organism in the electroplating wastewater with pretreater;
Outlet at pretreater utilizes pipe connection to concentrate liquid bath;
Connect topping-up pump and stage pump in the outlet that concentrates liquid bath;
Utilize pipe connection nanofiltration membrane concentrating and separating device at multistage pump outlet, electroplating wastewater is carried out concentrating and separating with nanofiltration membrane; Divalent ion concentration is set on the nanofiltration membrane concentrating and separating device is less than or equal to exporting of 3mg/L through liquid, and divalent ion concentration exporting greater than 3mg/L through liquid, and utilize pipeline to be connected with concentrated liquid bath in the liquid outlet that sees through that divalent ion concentration is less than or equal to 3mg/L, export and utilize pipeline and be connected at the liquid that sees through of divalent ion concentration through liquid bath greater than 3mg/L.
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| CN103253798B (en) * | 2013-06-08 | 2014-09-10 | 国家海洋局天津海水淡化与综合利用研究所 | Zero discharge treatment and recycling method for chromium ions in electroplating wastewater and device of method |
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