CN102432123A - Reproducible heavy metal complexing agent and application method thereof - Google Patents
Reproducible heavy metal complexing agent and application method thereof Download PDFInfo
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- CN102432123A CN102432123A CN2011103437153A CN201110343715A CN102432123A CN 102432123 A CN102432123 A CN 102432123A CN 2011103437153 A CN2011103437153 A CN 2011103437153A CN 201110343715 A CN201110343715 A CN 201110343715A CN 102432123 A CN102432123 A CN 102432123A
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Abstract
The invention aims to provide a reproducible heavy metal complexing agent and an application method thereof. In the method, hydrolyzed collagen serving as a complexing agent is applied to a membrane separating process, and heavy metal copper-containing waste water is integrally treated by performing membrane separation-electrolysis. The method mainly comprises the following steps of: enriching; filtering; concentrating; decomplexing; electrodepositing; refluxing and the like to realize efficient recovery of heavy metal copper-containing waste water.
Description
Technical field
The invention belongs to water-treatment technology field, relate in particular to a kind of process for treating industrial waste water, specifically relate to contain the heavy metal copper wastewater treatment method.
Background technology
Heavy metal wastewater thereby is that environmental pollution is serious and to one of great trade effluent of human health risk.The heavy metal wastewater thereby wide material sources mainly result from industries such as plating, mining and metallurgy, electronics, machinofacture and chemical industry.Along with the fast development of these industries, heavy metal wastewater thereby discharges in a large number, paid more and more attention.According to the different sources and the component of waste water, the treatment process that heavy metal wastewater thereby is taked is different.In general, the main method of processing heavy metal wastewater thereby has: chemical precipitation method, absorption method, ion exchange method, electrochemical process and membrane separation process etc.Chemical precipitation method is subject to the influence of precipitation agent and envrionment conditions, and the precipitator method often go out water concentration and do not reach requirement, need be for further processing.Simple to operate, metals ion removal efficient advantages of higher that absorption method has; But adsorbents adsorb still exist the aftertreatment problem after the heavy metal; Await further handling through the elutriant that contains the high density heavy metal of enrichment and could realize the resource recovery, limited the industrial applications of absorption method.The IX subtraction unit costs an arm and a leg, and processing cost is higher, resin pollution or oxidation deactivation.Electrodip process can be reduced to simple substance with heavy metal ion, and electrodeposition process can be peeled off the metal simple-substance on the pole plate after finishing, and easily realizes the recovery of resource, produces certain economic benefits.But electrodip process only is fit to the heavy metal wastewater thereby of treatment of high concentration, and processing low concentration heavy metal water power consumption is big, cost of investment is high.
Membrane separation technique is to utilize a kind of special semi-permeable membranes that solution is separated, and is motivating force with pressure, and when waste water was flowed through face, pollutent wherein was trapped, and water molecules sees through film, and waste water is purified.Membrane technique has low consumption, advantage such as efficient, easy to operate as a kind of novel water technology; Generally receive domestic and international water treatment person's concern; Particularly can when realizing the water reuse, improve the heavy metal content in the dense water, help the further recycling of heavy metal.Used membrane separation technique mainly is micro-filtration technology, ultra-filtration technique, nanofiltration and reverse osmosis technology at present.Still fenestra is little for the metal removal rate height for nanofiltration and r-o-, and membrane flux is low, and the working pressure that needs is high, generally is used for the purifying treatment of tap water.Ultra-filtration membrane and microfiltration membrane flux are big; Working pressure is low, but because membrane pore size is far longer than the metals ion diameter, can't be with its direct interception; Need to add tensio-active agent and form micella or add high molecular weight water soluble polymer and metal complex, its volume is increased and be trapped.Just formed thus and contained high density metal and organic liquid concentrator, directly be not discharged in the environment, can cause secondary pollution if further do not handle.On the other hand, the trade effluent water yield is big, need in treating processes, constantly add tensio-active agent or complexing agent, has increased running cost.
Summary of the invention
The objective of the invention is to overcome the problem that the liquid concentrator that exists in the prior art is difficult to handle, running cost is high; And a kind of reproducible heavy metal complexing agent and method of use thereof are provided; Because the complexing of this complexing agent and metal and in galvanic deposit, be difficult for oxidized reductive character can apply to this complexing agent in ultrafiltration-galvanic deposit combined method liquid concentrator to be effectively addressed; Reduce the danger of secondary pollution; And complexing agent can in electrodeposition process, obtain regeneration, the recycling through complexing agent effectively reduces running cost.
For realizing above-mentioned purpose, the technical scheme that the present invention adopted is:
In to the treating processes of heavy metal wastewater thereby, use a kind of reproducible heavy metal complexing agent, through the combined treatment of membrane sepn, two steps of galvanic deposit.In the step of said combined treatment, comprise complexing agent and cupric ion complexing and solution concentration, complexing agent regeneration and reuse.
Realize complexing agent and cupric ion complexing in the membrane sepn process; Realize solution concentration, complexing agent regeneration and reuse in the electrodeposition step.
Concrete scheme is:
(1) the pending waste water that contains heavy metal copper is put into an equalizing tank that has whisking appliance.
(2) in equalizing tank-1, add Collagen Hydrolysate as complexing agent; And add NaOH, and the pH that control adds back waste water remains between the 5.5-7.0, and the rotating speed of whisking appliance remains between the 400-600rpm; Reacted at normal temperatures 1-2 hour, with guarantee cupric ion all with the Collagen Hydrolysate complexing.
(3) under the effect of lift pump-1, the waste water in the equalizing tank-1 gets into more medium filter, ultrafiltration membrane system, and water molecules becomes through ultra-filtration membrane under pressure purifies waste water, and the cupric ion rejection reaches more than 90% in the filtrating, can be back to production technique.Cupric ion and Collagen Hydrolysate complex compound form liquid concentrator owing to held back by ultra-filtration membrane greater than the micropore size of ultra-filtration membrane.
(4) liquid concentrator of membrane sepn acquisition is got back in the equalizing tank-1; After the liquid concentrator in the equalizing tank-1 reaches 2-4 concentration rate doubly; Close the lift pump-1 of equalizing tank to ultrafiltration membrane system; Open the lift pump-2 between equalizing tank-1 and the equalizing tank-2, the feed liquid in the equalizing tank-1 is squeezed in the equalizing tank-2.
(5) in equalizing tank-2, add sulfuric acid, control adds the pH of back waste water between 2-4, makes Collagen Hydrolysate and cupric ion decomplexing.
(6) open the lift pump-3 of equalizing tank-2 between the dull and stereotyped electric deposition device, solution is squeezed into carried out electrolysis in the electrolyzer, copper is separated out on negative plate, Collagen Hydrolysate is stayed in the electrolytic solution, has realized separating of metals ion and complexing agent.
(7) after electrodeposition process finishes, open the valve between electrolyzer and the equalizing tank-1, the Collagen Hydrolysate after the regeneration is back in the equalizing tank-1 and recycles.
The processing condition of following each parts of stated and function:
Equalizing tank-1: be positioned at before the ultrafiltration membrane system, the complexing agent of adding is a Collagen Hydrolysate, is that protein is through ordinary method hydrolysis gained in ox, pig and the fish fur, and its molecular weight is 2000-3000.Those skilled in the art can obtain through technological method commonly used, for example: CN101948900A, CN1903918A etc.Foreign glitin factory (CompanyAddress: the north side is located for 78.2 kilometers in Wu Qian road, ancient city town, Fucheng County, Hebei province) is learned for Hebei in the Collagen Hydrolysate source among the present invention, and name of product is the Collagen Hydrolysate powder, and CAS number is 9007-34-5.The Collagen Hydrolysate mass ratio of heavy metal copper and adding in the waste water is 1: 10-1: 25.Regulating pH is 5.5～7.0, and the rotating speed of whisking appliance remains between the 400-600rpm, reacts at normal temperatures 1-2 hour;
More medium filter: remove the suspended substance in the water, reduce the turbidity of water, satisfy the ultrafiltration water inlet and require (turbidity is less than 1.0NTU); Existing commercialization on the market, sophisticated strainer all can be realized this technique effect, like JX-010 type quartz sand filtration device (model JHD-18, the JHD-22 of Qinhuangdao good meeting environmental protection equipment ltd production; JHD-36), YLSS series Guartz filter (YLSS-500, YLSS-750, the YLSS-1000 of the production of source, Beijing Lay Water Management Equipment Ltd.; YLSS-1200), ZWJ29-JDL-3 type quartz sand filtration device (the model JDL-3 that provides of Beijing (Tai'an, Chinese and Western) Technology Service Co., Ltd; JDL-6, JDL-10, JDL-15) etc.What the present invention was used is the quartz sand filtration device in the more medium filter.In the said ultrafiltration membrane system sepn process, hyperfiltration membrane assembly is a plate and frame, and mould material adopts poly (ether sulfone) film, and molecular weight cut-off is 1000 dalton.In the ultra-filtration and separation process, the working pressure that uses is 0.4-0.6Mpa, 25 ℃～35 ℃ of waste water working temperatures, and the average rejection of cupric ion is 90%-92%, effluent quality reaches the industrial circulating water water quality standard, can be back to the industrial cycle water system.Existing commercialization on the market, sophisticated assembly all can be realized this technique effect; For example: small-sized micro-filtration, ultrafiltration flat sheet membrane separation system (SY-MU2010, SY-MU2050, SY-MU-2-500) that Shanghai generation biological plant far away Engineering Co., Ltd produces, the ultrafiltration of pilot scale type, nanofiltration, reverse osmosis membrane separation system (SY-UNR-D3-4040); The Millipore ultrafiltration system of U.S. Millipore Corp. (the small-sized cross-flow ultrafiltration of labscale TFF system, Congent-M ultrafiltration system, Pellicon ultrafiltration system).Hyperfiltration membrane assembly: the liter LH3 series ultrafiltration membrane assembly (LH3-1060-V, LH3-0680-V, LH3-0660-V, LH3-0650-V, LH3-0450-V) of modification polysulfones (PS) hollow fiber film assembly (HQM-4040PS, HQM-6040PS) of Hangzhou Hong Quan membrane technique ltd development and production, upright Noboru enterprise production.Mould material: polysulfones (PS) film (PS-20) that U.S. Sepro company produces, pvdf (PVDF) film (PVDF-200, PVDF-350; PVDF-400, PVDF-700), polyacrylonitrile (PAN) film (PAN-50; PAN-200; PAN-350, PAN-400), polyethersulfone (PES) film (PES-5, PES-10, PES-20, PES-900C/D); Polyethersulfone (PES) ultra-filtration membrane (PES-1, PES-3, PES-5, PES-8, PES-10, PES-20, PES-30, PES-50) that Ande Membrane Separation Technology & Engineering (Beijing) Co., Ltd. produces; Polysulfones (PS) ultra-filtration membrane (PS-20, PS-50); Pvdf (PVDF) film (PVDF-50; PVDF-100), polyacrylonitrile (PAN) film (PAN-100).Above-mentioned ultrafiltration membrane system sepn process, through ultrafiltration membrane treatment, fully heavy metal in the concentrating spent liquor makes the concentration of metal ions in the liquid concentrator obtain bigger raising, is applicable to galvanic deposit recovery heavy metal.Ultra-filtration process finished when concentration ratio reached 2-4 times.
Equalizing tank-2: be positioned at before the two-dimensional flat plate electric deposition device, adjusting pH is 2-4, and the rotating speed of whisking appliance remains between the 400-600rpm, makes the complex compound of Collagen Hydrolysate and cupric ion separate the complexing reaction.The device that is adopted also all is that those skilled in the art can obtain; The electrochemical processing cell announced of CN03820055.4 for example; Bipolar electrolysis and unit electrolytic bath thereof that CN86107225 announces, the electrolyzer that is used for electrochemical process that CN1930325 announces, a kind of noble electrode aluminium cell that CN1986898 announces; The diaphragm electrolyzer with metal anodes that CN1995461 announces, the negative electrode that CN2173247 announces rotates the cellular-type electrolyzer.
In the said electrodeposition process, solution is carried out stirring at normal temperature, stirring velocity is 300-500rpm, can promote the mass transfer process of copper and reduce the absorption of Collagen Hydrolysate on pole plate; Electrode materials is selected graphite anode/stainless steel cathode counter-electrodes for use, and bath voltage is 6.0V-16.0V, and electrolysis time is 90min-180min, the Cu after electrodeposition process
2+Minimum concentration is less than 20mg/L, and the recovery of copper on pole plate reaches as high as 89%.The regeneration rate of Collagen Hydrolysate is 84%-86%.
Above-mentioned electrodeposition process obtains contains the proteic liquid concentrator of regeneration collagen and is back in the equalizing tank and reuses; Mix and fully reaction with initiate cupric heavy metal wastewater thereby; Under the effect of lift pump, get into more medium filter, ultrafiltration membrane system again; Under no new collagen protein supplementary information, reach more than 70% for the clearance of heavy metal copper.
The present invention compared with prior art has following advantage:
First; Collagen Hydrolysate is applied in polymer reinforced ultrafiltration process and the galvanic deposit combined method; Given full play to the advantage of Collagen Hydrolysate: both easy and cupric ion forms complex compound; Improve the clearance of copper in the ultra-filtration process, separate complexing through ad hoc approach easily again and regenerate, and in electrolytic process, can not destroyed in pole plate generation redox reaction.
The second, Collagen Hydrolysate is a kind of crude substance, and nontoxicity is separated the middle tensio-active agent that uses with ultra-filtration membrane and compared, and is littler to the harm of environment.
The 3rd, realized that the Collagen Hydrolysate after the regeneration can reuse in ultra-filtration process, effectively reduce running cost.
Description of drawings
Fig. 1 is the method for use schema of this renewable heavy metal complexing agent.
Embodiment
Embodiment 1:
Adopting the inventive method concentration of treatment is the cupric heavy metal wastewater thereby of 100mg/L; Water inlet pH value is 4.6; 25 ℃ of water temperatures are complexing agent with the Collagen Hydrolysate, through ultrafiltration membrane system water quality are purified; Liquid concentrator is handled through electrodip process, realizes the recovery of copper, the regeneration and the recycle of Collagen Hydrolysate. and employed Collagen Hydrolysate, more medium filter, ultrafiltration membrane system, two-dimensional flat plate electric deposition device etc. all are conventional waste-water recovering treater in this process.Collagen Hydrolysate used in the present invention is that molecular weight 2000～3000 is the enzymolysis process gained.Be specially: the method according to CN101948900A is a raw material with fresh ox-hide, after handling with sodium hydroxide solution, adds papoid, Sumizyme MP stage by stage; Add the complex enzyme hydrolysis protective material simultaneously; The enzyme that goes out that behind twice enzymolysis, heats up again through oxidative decoloration, filters ultrafiltration; Collect trapped fluid, obtain molecular weight after the spraying drying and be 2000～3000 Collagen Hydrolysate.Or directly purchase and learn foreign glitin factory, CAS:9007-34-5 in Hebei.More medium filter is the ZWJ29-JDL-3 type quartz sand filtration device that Beijing (Tai'an, Chinese and Western) Technology Service Co., Ltd provides; Ultrafiltration membrane system designs the UF-2319 pilot experiment machine of producing for Ande Membrane Separation Technology & Engineering (Beijing) Co., Ltd.; Two-dimensional flat plate electric deposition device electrolyzer is a PP polypropylene high molecular material electrolyzer, and anode and cathode is respectively stainless steel plate and graphite cake.Concrete technical process is following: step 1: the pending waste water that contains heavy metal copper is put into an equalizing tank-1 that has whisking appliance.
Step 2: in equalizing tank-1, add Collagen Hydrolysate as complexing agent, the mass ratio of Collagen Hydrolysate and copper is 10: 1-25: 1.Add NaOH, regulating the pH that adds back waste water is 5.5-7.0, and the rotating speed of whisking appliance is 400rpm, reacted at normal temperatures 1 hour, with guarantee cupric ion all with the Collagen Hydrolysate complexing.
Step 3: under the effect of lift pump-1, the waste water in the equalizing tank-1 is removed the suspended substance in the water through more medium filter, reduces the turbidity of water, satisfies ultrafiltration water inlet requirement; Get into ultrafiltration membrane system afterwards, the working pressure that uses is 0.45Mpa, 25 ℃ of waste water working temperatures, and water molecules becomes through ultra-filtration membrane under pressure purifies waste water, and the cupric ion rejection is 93.1% in the filtrating, can be back to production technique.Cupric ion and Collagen Hydrolysate complex compound form liquid concentrator owing to held back by ultra-filtration membrane greater than the micropore size of ultra-filtration membrane.
Step 4: the liquid concentrator that membrane sepn obtains is got back in the equalizing tank-1; After the liquid concentrator in the equalizing tank-1 reaches 2 times concentration rate; Close the lift pump-1 of equalizing tank-1 to ultrafiltration membrane system; Open the lift pump-2 between equalizing tank-1 and the equalizing tank-2, the feed liquid in the equalizing tank-1 is squeezed in the equalizing tank-2.
Step 5: in equalizing tank-2, add sulfuric acid, the pH that control adds back waste water is 2-4, makes Collagen Hydrolysate and cupric ion decomplexing.
Step 6: open equalizing tank-2 to the lift pump between the electrolyzer-3; Solution is squeezed into through lift pump-3 and is carried out electrodeposition process in the electrolyzer; Solution is carried out stirring at normal temperature, and stirring velocity is 300rpm, can promote the mass transfer process of copper and reduce the absorption of Collagen Hydrolysate on pole plate; Electrode materials is selected graphite anode/stainless steel cathode counter-electrodes for use, and bath voltage is 6.0～16.0V, and electrolysis time is 90min～180min, and copper is separated out on negative plate, Cu in the solution after electrodeposition process
2+Concentration is 18～24mg/L, and the recovery of copper on pole plate is 88%～90%.Simultaneously, because the separating out of copper makes Collagen Hydrolysate separate with cupric ion, Collagen Hydrolysate is stayed in the electrolytic solution and is obtained regeneration, and the regeneration rate of Collagen Hydrolysate is 84%～86%.
Step 7: after electrodeposition process finishes; Open the valve between electrolyzer and the equalizing tank-1; Collagen Hydrolysate after the regeneration is back in the equalizing tank-1; Mix with the waste water that contains heavy metal copper of new entering, fully more medium filter, ultrafiltration membrane system are squeezed into by lift pump-1 in the reaction back, have begun second circulating treatment procedure.Under the situation that no new complexing agent adds, be 80% for the clearance of cupric ion.
Claims (9)
1. the method for use of a renewable heavy metal complexing agent is characterized in that this method carries out the combined treatment of membrane sepn, two steps of galvanic deposit to waste water.
2. method of use as claimed in claim 1 in said combined treatment, is applied to heavy metal containing wastewater treatment with complexing agent, and this application comprises complexing agent and cupric ion complexing and solution concentration, complexing agent regeneration and two steps of reuse.
3. according to claim 1 or claim 2 method of use, it is characterized in that: said membrane sepn step comprises:
(1) the pending waste water that contains heavy metal copper is put into an equalizing tank that has whisking appliance.
(2) in equalizing tank-1, add complexing agent, and add NaOH, the pH that control adds back waste water remains between the 5.5-7.0, and the rotating speed of whisking appliance remains between the 400-600rpm, reacted at normal temperatures 1-2 hour, with guarantee cupric ion all with the complexing agent complexing.
(3) under the effect of lift pump-1, the waste water in the equalizing tank-1 gets into more medium filter, ultrafiltration membrane system, and water molecules becomes through ultra-filtration membrane under pressure purifies waste water, and the cupric ion rejection reaches more than 90% in the filtrating, can be back to production technique.The complex compound that cupric ion and complexing agent form forms liquid concentrator owing to held back by ultra-filtration membrane greater than the micropore size of ultra-filtration membrane.
4. like the described method of use of claim 1-3, it is characterized in that: said electrodeposition step comprises:
(4) liquid concentrator that obtains through membrane sepn is got back in the equalizing tank-1; After the liquid concentrator in the equalizing tank-1 reaches 2-4 concentration rate doubly; Close the lift pump-1 of equalizing tank to ultrafiltration membrane system; Open the lift pump-2 between equalizing tank-1 and the equalizing tank-2, the feed liquid in the equalizing tank-1 is squeezed in the equalizing tank-2.
(5) in equalizing tank-2, add sulfuric acid, control adds the pH of back waste water between 2-4, makes complexing agent and cupric ion decomplexing.
(6) open the lift pump-3 of equalizing tank-2 between the dull and stereotyped electric deposition device, solution is squeezed into carried out electrolysis in the electrolyzer, copper is separated out on negative plate, complexing agent is stayed in the electrolytic solution, has realized separating of metals ion and complexing agent.
(7) after electrodeposition process finishes, open the valve between electrolyzer and the equalizing tank-1, the complexing agent after the regeneration is back in the equalizing tank-1 and recycles.
5. like the described method of use of claim 1-4, it is characterized in that: described complexing agent is a Collagen Hydrolysate, is that protein is through ordinary method hydrolysis gained in ox, pig and the fish fur, and its molecular weight is 2000-3000.
6. like the described method of use of claim 3-5, in step (1), the Collagen Hydrolysate mass ratio of heavy metal copper and adding in the waste water is 1: 10-1: 25.
7. like the described method of use of claim 3-5, in step (3), in the described ultrafiltration membrane system sepn process, hyperfiltration membrane assembly is a plate and frame, and mould material adopts poly (ether sulfone) film, and molecular weight cut-off is 1000 dalton.In the ultra-filtration and separation process, the working pressure that uses is 0.4-0.6Mpa, 25 ℃～35 ℃ of waste water working temperatures.
8. like the described method of use of claim 3-5, in step (6), solution is carried out stirring at normal temperature, stirring velocity is 300-500rpm; Electrode materials is selected graphite anode/stainless steel cathode counter-electrodes for use, and bath voltage is 6.0～16.0V, and electrolysis time is 90～180min.
9. like the described method of use of claim 3-8, the regeneration rate of complexing agent is 84%-86%.
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| CN103785677A (en) * | 2014-01-26 | 2014-05-14 | 河北欧美环境工程有限公司 | Integrated device for heavy metal contaminated soil remediation and leacheate recycling and method thereof |
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| CN103084065A (en) * | 2013-01-14 | 2013-05-08 | 天津工业大学 | Ultra-filtration membrane removing method of metal ions |
| CN103785677B (en) * | 2014-01-26 | 2016-08-17 | 河北欧美环境工程有限公司 | Heavy-metal contaminated soil reparation and leacheate recycle integrated apparatus and method thereof |
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| CN105541018A (en) * | 2015-12-31 | 2016-05-04 | 朱辉 | Treatment method for removing heavy metals in industrial wastewater |
| CN107721063A (en) * | 2016-01-14 | 2018-02-23 | 张作玮 | A kind of food and drink waste water oil removal treatment system |
| CN105621815A (en) * | 2016-03-10 | 2016-06-01 | 广州聚注专利研发有限公司 | Method for treating heavy metal wastewater through fish bone dust |
| CN107539991A (en) * | 2017-09-29 | 2018-01-05 | 四川绿源聚能环保科技有限责任公司 | A kind of apparatus system for handling chlorosilane slurry raffinate |
| CN108486199A (en) * | 2018-03-27 | 2018-09-04 | 北京中科众联新能源技术服务有限公司 | Water-soluble chelator, preparation method and the process for treating heavy-metal waste water with it |
| CN108486199B (en) * | 2018-03-27 | 2020-12-22 | 北京中科众联新能源技术服务有限公司 | Water-soluble chelating agent, preparation method thereof and heavy metal wastewater treatment method using water-soluble chelating agent |
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Application publication date: 20120502 |