CN104451166A - Method and device for recovering zinc and chrome in heavy metal sludge - Google Patents
Method and device for recovering zinc and chrome in heavy metal sludge Download PDFInfo
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Abstract
The invention provides a method and device for recovering zinc and chrome in heavy metal sludge. The method for recovering zinc and chrome in heavy metal sludge includes the following steps of pretreatment, immersion, neutralization, evaporation and electrolysis. The device for recovering zinc and chrome in heavy metal sludge comprises a multi-stage immersion system, an acid-base neutralization system, an evaporative crystallization system, an electrolysis system and a medicine adding system. According to the method and device, zinc and chrome in the heavy metal sludge can be successfully separated, waste reclamation is achieved, the recovery rates of zinc and chrome are higher than 95% and 90% respectively, obtained product gains are larger than operation cost, and actual application value is achieved.
Description
Technical field
The invention belongs to municipal solid wastes disposal and resource utilization field, particularly a kind of method and apparatus reclaiming zinc and chromium in heavy metal sewage sludge.
Background technology
Heavy metal sewage sludge is of a great variety.In China, the main source industry containing solid waste of heavy metal is attached most importance to the five large industries such as nonferrous metals ore selecting and purchasing, smelting, lead storage battery, leather and leather products, chemical feedstocks and goods thereof, and often belongs to Hazardous wastes.By 2007, leaded, mercury, pot, chromium, arsenic the Hazardous wastes generation listing " National Hazard refuse register " in was 1690.55 ten thousand tons; Five industries such as metal product industry, leather and leather products industry, non-ferrous metal metallurgy and rolling processing industry, chemical feedstocks and chemical product manufacturing and nonferrous metals ore selecting and purchasing industry account for 95.24% of whole industrial total release containing the quantity discharged of heavy metal waste.If the not treated just discharge of heavy metal sewage sludge, can cause the severe contamination of soil and water, heavy metal, by food chain enrichment layer by layer, produces chronic/cumulative toxicity, causes serious harm to human health and species diversity.
In a lot of industrial solid wastes, heavy metal content is relatively high, and the content of a lot of heavy metal has exceeded its grade in metallic ore.Heavy metal in heavy metal mud reclaims, and not only can realize changing waste into resources and utilize, can also reduce refuse toxicity, thus reduce disposal costs, be kill two birds with one stone.The comprehensive utilization technique of heavy metal waste comprises dry method and the large class of wet method two, and just reclaims with regard to elemental chromium and zinc, or wet method is more.Hydrometallurgic recovery technology mainly comprises leaching and is separated.Modal wet recycling process has acidleach and ammonia leaching.The leaching yield of acidic leaching method is very high, but selectivity is not strong; Ammonia leaching process is comparatively strong to the selectivity of copper, nickel, cobalt, less to the recycle of other metal.Later separation method after leaching has extraction process and chemical precipitation method.Adopt suitable extraction separation method, the rate of recovery of metal target is very high, and the purity of the metallic salt product obtained is also very high; Extraction process is technique the most frequently used at present, but extraction process is complicated, and organic solvent consumption is large, and investment and the operation cost of extraction equipment are higher, and the process of Discarded organic solvent is also a problem.
Summary of the invention
The present invention proposes a kind of method and apparatus reclaiming zinc and chromium in heavy metal sewage sludge, zinc and chromium can be separated and realized purifying from mud.
Reclaim a method for zinc and chromium in heavy metal sewage sludge, it is made up of following steps:
(1) pre-treatment: carried out successively by block heavy metal sewage sludge pulverizing, grinding, obtains powder;
(2) leach: solid waste powder and leaching agent, conditioning agent are carried out mixing leaching; Leaching reaction after leave standstill, after solid-liquid separation, neutralization waited until by supernatant liquor, heavy mud after filtration, washing after, as Ordinary solid waste process;
(3) neutralize: in the leaching liquid that step (2) obtains, add neutralizing agent carry out acid-base neutralisation; Neutralizer waits until evaporative crystallization after filtering; Filter residue waits until dissolving;
(4) evaporation and electrolysis: the filtrate obtained in step (3) is carried out evaporative crystallization, obtains chromic salt; The filter residue obtained in step (3) is added acid dissolve, and lysate carries out electrolysis treatment, and negative plate obtains electrolytic zinc.
Wherein, preferably, the pre-treatment of described solid waste, the particle diameter of the pressed powder obtained after grinding is 0.5-2mm.
Wherein, preferably, the leaching in described step (1), control mixeding liquid temperature is 40-90 DEG C; Leaching time is 20-120min.
Wherein, preferably, described leaching agent is containing any one or a few the aqueous solution in hydrogen peroxide, dioxide peroxide, clorox; Conditioning agent is sodium hydroxide.
Wherein, preferably, the add-on of described leaching agent, in the solute in leaching agent solution, is 1-5 times of chromium content (quality) in solid waste; After in described step (2), conditioning agent adds, manipulation condition is control ph > 12.
Wherein, preferably, in described step (2), what heavy mud filtered employing is press filtration; The mud cake obtained after heavy mud press filtration adopts the alkali liquid washing of 1-10%.
Wherein, preferably, the leaching in described step (2) is multilevel leaching, and the operational path of multilevel leaching is, by the rear solid-liquid separation of pressed powder leaching obtained in pretreatment process, neutralization sent to by supernatant liquor; Lower floor's mud wouldn't be discharged; Now carry out second time leaching with the leaching liquid of new configuration to described lower floor's mud, leave standstill after leaching, supernatant liquor pumps storage, and the first time for next batch charging leaches; Add leaching agent and conditioning agent in the filtrate obtained to press filtration and mud cake washings, configure new leaching liquid, the second time for next batch charging leaches; So repeatedly.
Wherein, preferably, the supernatant liquor obtained after leaching in described step (3), in and front need to filter, the neutralizing agent of use is sulfuric acid or hydrochloric acid, and the control terminal of neutralization reaction is pH value 7.0-8.2, and the filter method of neutralizer is press filtration; Before neutralizer enters vapo(u)rization system after press filtration is separated, need to carry out secondary filter, filtering accuracy is 5-25 μm.
Wherein, preferably, the electrolysis treatment in described step (4), negative plate material is aluminium sheet or stainless steel plate; Positive plate is graphite cake or lead alloy plate.
Reclaim a device for zinc and chromium in heavy metal sewage sludge, it is characterized in that: comprise multilevel leaching system, acid-base neutralisation system, evaporation and crystallization system, electrolytic system and medicine system;
Described multilevel leaching system comprises pulper, No. 1 leaching flow container, No. 2 leaching flow containers, No. 3 leaching flow containers and No. 1 pressure filter, No. 1 leaching flow container and No. 2 leaching flow containers are bi-directionally connected with pulper respectively, the outlet of pulper is connected with the 3rd leaching can, the slurry outlet of pulper is connected with No. 1 pressure filter, and No. 1 filter press filtrate outlet is connected with the import of No. 2 leaching cans;
Described acid-base neutralisation system, comprise and connect No. 1 strainer, neutralization tank, No. 2 pressure filter and filtrate tanks successively, No. 1 strainer is connected with the 3rd leaching can;
Described evaporation and crystallization system comprises No. 2 strainers and evaporation and crystallization system, and feed liquor strainer is connected with filtrate tanks;
Described electrolytic system comprises dissolving vessel and electrolyzer, and dissolving tank is connected with No. 2 pressure filter;
Described medicine system comprises acid storage tank, alkali storage tank and leaching agent storage tank, and acid storage tank is connected with neutralization tank and dissolving vessel respectively, and alkali storage tank and leaching agent storage tank leach flow container with No. 2 respectively and be connected.
Beneficial effect of the present invention:
1. adopt in the present invention the technique proposed and device can zinc in successful separating beavy metal mud and chromium, achieve changing waste into resources, the rate of recovery of zinc and chromium be greater than 95% and 90% respectively; The product income obtained is greater than running cost, has actual application value;
2. filter residue remaining after leaching, as general refuse process, can greatly reduce disposal costs;
3. leaching technology of the present invention is multilevel leaching, achieves the sealing and circulating of medicament;
4. electrolysis process of the present invention, the acid solution that electrolytic process produces is back to neutralizing well and utilizes; By the way, avoid the discharge of residual pharmacy to greatest extent, reduce reagent cost.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, put after not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the schematic flow sheet of zinc and chromium method in recovery heavy metal sewage sludge of the present invention;
Fig. 2 is the schematic diagram of zinc and chromium device in the recovery heavy metal sewage sludge that proposes of the present invention.
In figure: 1. pulper; No. 2.2 leaching flow containers; No. 3.3 leaching flow containers; No. 4.1 leaching flow containers; No. 5.1 pressure filter; No. 6.1 strainers; 7. neutralization tank; No. 8.2 pressure filter; 9. filtrate tanks; 10.2 number strainer; 11. evaporation and crystallization system; 12. dissolving vessels; 13. electrolyzers; 14. acid storage tanks; 15. leaching agent storage tanks; 16. alkali storage tanks
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art put obtained every other embodiment after not making creative work, all belong to the scope of protection of the invention.
Embodiment 1
As shown in Figure 2, the present embodiment provides a kind of device reclaiming zinc and chromium in heavy metal sewage sludge, comprises multilevel leaching system, acid-base neutralisation system, evaporation and crystallization system, electrolytic system and medicine system;
Multilevel leaching system comprises No. 1,1, pulper leaching No. 4,2, flow container leaching No. 2,3, flow container leaching flow container and No. 1 pressure filter 5, No. 1 leaching flow container 4 and No. 2 leaching flow containers 2 are bi-directionally connected with pulper 1 respectively, the outlet of pulper 1 is connected with the 3rd leaching can, the slurry outlet of pulper 1 is connected with No. 1 pressure filter 5, and No. 1 pressure filter 5 filtrate outlet is connected with the import of No. 2 leaching cans;
Acid-base neutralisation system, comprises connection No. 1 strainer 6, neutralization tank 7, No. 2 pressure filter 8 and filtrate tanks 9, No. 1 strainer 6 successively and is connected with the 3rd leaching can;
Evaporation and crystallization system comprises No. 2 strainers 10 and evaporation and crystallization system 11, and feed liquor strainer is connected with filtrate tanks 9;
Electrolytic system comprises dissolving vessel 12 and electrolyzer 13, and dissolving tank is connected with No. 2 pressure filter;
Medicine system comprises acid storage tank 14, alkali storage tank 16 and leaching agent storage tank 15, and acid storage tank 14 is connected with neutralization tank 7 and dissolving vessel 12 respectively, and alkali storage tank 16 and leaching agent storage tank 15 leach flow container 2 with No. 2 respectively and be connected.
Wherein, the mass transport between stream oriented device is led to pump and is carried out.
Embodiment 2
The present embodiment provides the technological process reclaiming zinc and chromium in heavy metal sewage sludge, employing be that embodiment 1 is arranged, its process flow sheet is as shown in Figure 1.
In the present embodiment heavy metal sewage sludge be Hubei electronic components fabrication factory produce containing chromium, containing zinc refuse, its main component is as follows:
First above-mentioned mud is sent into crusher in crushing, crusher discharging enters rod mill and pulverizes, the particle diameter of the pressed powder obtained after grinding is 0.5mm, grinding machine discharging is delivered to pulper by screw feeder, technical grade liquid caustic soda (30%), clorox (10%) and water are configured to leaching liquid by a certain percentage in No. 2 leaching flow containers, and the pH value of leaching liquid is 14.2, sends into pulper together, stir leaching, leaching temperature 40 DEG C; Leaching time is 120min, and material dosage is 0.72 ton of liquid caustic soda/ton refuse, 1.8 tons sodium/ton refuses, 0.5t water/ton refuses; After mixed solution complete for leaching is left standstill 40min in pulper, supernatant liquor is pumped into No. 3 leaching flow containers, in order to later separation; Lower floor's mud waits until second time leaching, now in No. 2 leaching flow containers, configures leaching liquid according to the above ratio, pumps into pulper, stir leaching, leaching temperature 80 DEG C; Leaching time is 20min, and this is considered as secondary leaching, is heated to 40 DEG C, leaches complete after 20min, then leaves standstill 40min, and No. 1 leaching liquid bath sent into by supernatant liquor, and the first time for next batch charging leaches.Heavy dredge pump enters pressure filter press filtration, and pressing filtering liquid enters No. 2 leaching grooves, mud cake alkali lye (5%) washing, and washings consumption is 0.5 ton of/ton of refuse, washes after alkali cleaning; Washings enters No. 2 leaching liquid baths in the lump.By the mud cake after washing according to HJ/T299-2007 " solid waste-Leaching leaching method-sulfonitric method " tissue leaching experiment, detect and find, the concentration of the heavy metals such as the copper in leach liquor, zinc, nickel, chromium, cadmium, lead is lower than the limit value specified in GB5085.3-2007 " Hazardous wastes judging standard-leaching characteristic identification "; Therefore by being transported to a brickmaking factory outside this mud cake, for brickmaking.
In No. 2 leaching liquid baths, add liquid caustic soda and time sodium, additional amount is 0.6 ton of liquid caustic soda/ton refuse, 1.4 tons sodium/ton refuses, and configure new leaching liquid, the second time for next batch charging leaches.After the leaching of first material, the parting liquid in No. 3 leaching cans is sent into neutralization tank, adds sulfuric acid (98%) and neutralize, it is pH=8.1 that neutralization reaction controls terminal; Mixed solution after neutralization is sent into pressure filter press filtration, and filtrate pumps into Sodium chromate tank; After mud cake washing, wash-down water sends into Sodium chromate tank in the lump; Mud cake sends into zinc sulfate dissolving vessel, adds acid dissolve.The filtrate of Sodium chromate tank is after more medium filter (filtering accuracy is 5 μm) filters, and send into two effect vapo(u)rization systems, evaporative crystallization, obtains Sodium chromate; Zinc sulfate sends into electrolyzer (graphite sheet anode+aluminium sheet negative electrode) electrolysis after dissolving, and negative plate obtains electrolytic zinc.The rate of recovery of chromium and zinc is respectively 94.4% and 90.5%.
In the present embodiment, leaching agent is the chlorine bleach liquor of 10%, also can be hydrogen peroxide or aqueous solution of chlorine dioxide, and the liquid caustic soda in the present embodiment is aqueous sodium hydroxide solution.
Wherein, electrolyzer also can be stainless steel plate negative electrode and lead alloy plate anode.
Embodiment 3
The present embodiment provides the technological process reclaiming zinc and chromium in heavy metal sewage sludge, employing be that embodiment 1 is arranged, its process flow sheet is as shown in Figure 1.
In the present embodiment heavy metal sewage sludge be Hubei tannery produce containing chromium refuse, its main component is as follows:
Because in mud, Zn content is less, therefore only reclaim chromium.
Mud is through hammering into shape broken, after rod milling, obtaining particle diameter is 2mm powder, powder is by manually delivering to pulper, technical grade liquid caustic soda (30%), secondary sodium (10%) and water are configured to leaching liquid in No. 2 leaching flow containers, pH value is 15, send into pulper together, stir leaching, leaching temperature 90 DEG C; Leaching time is 20min, and material dosage is 0.15 ton of liquid caustic soda/ton refuse, 3.9 tons sodium/ton refuses, 0.5t water/ton refuses; After mixed solution complete for leaching is left standstill 30min in pulper, supernatant liquor is pumped into No. 3 leaching flow containers, in order to later separation; Lower floor's mud waits until second time leaching, now in No. 2 leaching flow containers, configures leaching liquid according to the above ratio, pumps into pulper, stir leaching, leaching temperature 80 DEG C; Leaching time is 20min, and this is considered as secondary leaching, leaves standstill 30min after leaching, and No. 1 leaching liquid bath sent into by supernatant liquor, and the first time for next batch charging leaches.Heavy dredge pump enters pressure filter press filtration, and pressing filtering liquid enters No. 2 leaching grooves, and mud cake is washed; Washings enters No. 2 leaching liquid baths in the lump.By the mud cake after washing according to HJ/T299-2007 " solid waste-Leaching leaching method-sulfonitric method " tissue leaching experiment, detect and find, the concentration of the heavy metals such as the copper in leach liquor, zinc, nickel, chromium, cadmium, lead is lower than the limit value specified in GB5085.3-2007 " Hazardous wastes judging standard-leaching characteristic identification "; Therefore by this mud cake directly as general waste reclamation process.
In No. 2 leaching liquid baths, add liquid caustic soda and time sodium, additional amount is 0.15 ton of liquid caustic soda/ton refuse, 1.2 tons sodium/ton refuses, and configure new leaching liquid, the second time for next batch charging leaches.After the leaching of first material, the parting liquid in No. 3 leaching cans is sent into neutralization tank, adds sulfuric acid (98%) and neutralize, it is pH=7.0 that neutralization reaction controls terminal; Mixed solution after neutralization is sent into deep bed filter filter, filtrate pumps into Sodium chromate tank; After mud cake washing, wash-down water sends into Sodium chromate tank in the lump; After the mud cake method of pressing described in HJ/T299-2007 detects, as general waste reclamation process.The filtrate of Sodium chromate tank is after more medium filter (filtering accuracy is 25 μm) filters, and send into two effect vapo(u)rization systems, evaporative crystallization, obtain Sodium chromate, chromium recovery ratio is 92%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. reclaim a method for zinc and chromium in heavy metal sewage sludge, it is characterized in that it is made up of following steps:
(1) pre-treatment: block heavy metal sewage sludge is carried out successively broken, grinding, obtain powder;
(2) leach: solid waste powder and leaching agent, conditioning agent are carried out mixing leaching; Leaching reaction after leave standstill, after solid-liquid separation, neutralization waited until by supernatant liquor, heavy mud after filtration, washing after, as Ordinary solid waste process;
(3) neutralize: in the leaching liquid that step (2) obtains, add neutralizing agent carry out acid-base neutralisation; Neutralizer waits until evaporative crystallization after filtering; Filter residue waits until dissolving;
(4) evaporation and electrolysis: the filtrate obtained in step (3) is carried out evaporative crystallization, obtains chromic salt; The filter residue obtained in step (3) is added acid dissolve, and lysate carries out electrolysis treatment, and negative plate obtains electrolytic zinc.
2. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 1, is characterized in that: the pre-treatment of described solid waste, and the particle diameter of the pressed powder obtained after grinding is 0.5-2mm.
3. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 1, is characterized in that: the leaching in described step (1), and control mixeding liquid temperature is 40-90 DEG C; Leaching time is 20-120min.
4. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 1, is characterized in that: described leaching agent is containing any one or a few the aqueous solution in hydrogen peroxide, dioxide peroxide, clorox; Conditioning agent is sodium hydroxide.
5. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 4, is characterized in that: the add-on of described leaching agent, in the solute in leaching agent solution, is 1-5 times of chromium content (quality) in solid waste; After in described step (2), conditioning agent adds, manipulation condition is control ph is >12.
6. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 1, is characterized in that: in described step (2), and what heavy mud filtered employing is press filtration; The mud cake obtained after heavy mud press filtration adopts the alkali liquid washing of 1-10%.
7. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 1, it is characterized in that: the leaching in described step (2) is multilevel leaching, the operational path of multilevel leaching is, by the rear solid-liquid separation of pressed powder leaching obtained in pretreatment process, neutralization sent to by supernatant liquor; Lower floor's mud wouldn't be discharged; Now carry out second time leaching with the leaching liquid of new configuration to described lower floor's mud, leave standstill after leaching, supernatant liquor pumps storage, and the first time for next batch charging leaches; Add leaching agent and conditioning agent in the filtrate obtained to press filtration and mud cake washings, configure new leaching liquid, the second time for next batch charging leaches; So repeatedly.
8. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 1, it is characterized in that: the supernatant liquor obtained after leaching in described step (3), in and front need filter, the neutralizing agent used is sulfuric acid or hydrochloric acid, the control terminal of neutralization reaction is pH value 7.0-8.2, and the filter method of neutralizer is press filtration; Before neutralizer enters vapo(u)rization system after press filtration is separated, need to carry out secondary filter, filtering accuracy is 5-25 μm.
9. the method for zinc and chromium in the recovery heavy metal sewage sludge according to right 1, is characterized in that: the electrolysis treatment in described step (4), and negative plate material is aluminium sheet or stainless steel plate; Positive plate is graphite cake or lead alloy plate.
10. reclaim a device for zinc and chromium in heavy metal sewage sludge, it is characterized in that: comprise multilevel leaching system, acid-base neutralisation system, evaporation and crystallization system, electrolytic system and medicine system;
Described multilevel leaching system comprises pulper, No. 1 leaching flow container, No. 2 leaching flow containers, No. 3 leaching flow containers and No. 1 pressure filter, No. 1 leaching flow container and No. 2 leaching flow containers are bi-directionally connected with pulper respectively, the outlet of pulper is connected with the 3rd leaching can, the slurry outlet of pulper is connected with No. 1 pressure filter, and No. 1 filter press filtrate outlet is connected with the import of No. 2 leaching cans;
Described acid-base neutralisation system, comprise and connect No. 1 strainer, neutralization tank, No. 2 pressure filter and filtrate tanks successively, No. 1 strainer is connected with the 3rd leaching can;
Described evaporation and crystallization system comprises No. 2 strainers and evaporation and crystallization system, and feed liquor strainer is connected with filtrate tanks;
Described electrolytic system comprises dissolving vessel and electrolyzer, and dissolving tank is connected with No. 2 pressure filter;
Described medicine system comprises acid storage tank, alkali storage tank and leaching agent storage tank, and acid storage tank is connected with neutralization tank and dissolving vessel respectively, and alkali storage tank and leaching agent storage tank leach flow container with No. 2 respectively and be connected.
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