CN101234826B - Sulfuration recovery processing method and device for high-acidity high-arsenic high-cadmium waste water - Google Patents
Sulfuration recovery processing method and device for high-acidity high-arsenic high-cadmium waste water Download PDFInfo
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Abstract
The invention discloses a method and a device for reclaiming and treating wastewater with high acidity, high arsenic and high cadmium, and relates to a method for reclaiming arsenic and cadmium in the wastewater with high acidity. The following steps are adopted: SO2 in the wastewater is removed; a certain quantity of lime is added into desulfated wastewater, and is filtered; filtrate is separated and led in a treatment device, wherein the treatment device is a uniform reactor with a plurality of heads of immersion type; vulcanizing agent is led in a medicine distributing chamber from a feeding pipe, evenly distributed, and added into the separated filtrate; As2S3 is generated by As3+ after a reaction, and CdS is generated by Cd2+ after a reaction, wherein the As2S3 and the CdS are filtered to reclaim the arsenic, cadmium and other metal sulfides; the filtrate without slag is led into a lime neutralization and aeration for neutralization and aeration; pH value is adjusted; the treated water is discharged after a standard is met. The method and the device for reclaiming and treating wastewater with high acidity, high arsenic and high cadmium has the advantages that a sulfuration reaction of the wastewater is carried out according to chemical amount; consumption of vulcanizing agent is little; the best sulfuration effect is attained with the lowest medicine consumption; the reclaiming rate of the arsenic is close to 100 percent; the reclaiming rate of the cadmium is over 99.7 percent; the arsenic content in sulfuration slag is high, thus beneficial to a deep processing and utilization of the arsenic and changing harm to advantages; reclamation and commercialization of the arsenic are realized; water is discharged after reaching the standard.
Description
Technical field
The present invention relates to a kind of arsenic in the dirty acid, method of cadmium of reclaiming.
Background technology
Arsenic is a kind of carcinogenic substance to human body and the toxic effect of other biological body, and the lethal quantity of its acute poisoning is 0.2～0.6g.The arsenic majority of occurring in nature is normal and nonferrous metals ore association, and gets into smelting system with concentrate.Arsenic state with sulfide or salt in the smelting process of non-ferrous metal gets in flue gas, waste water and the waste residue to some extent, and in utilizing the process of flue gas acid preparing, they transfer to again in " the dirty acid " of washing flue gas.Arsenic in the dirty acid of efficient recovery comprises being actually the toxic heavy metal of cadmium and having clutched most important source of pollution in the nonferrous smelting.How to administer produce in the colored metallurgical industrial contain the dirty acid of arsenic cadmium, make its qualified discharge and fully utilize its waste, be the research topic that must face directly.
The non-ferrous metal metallurgy system is basic at present to adopt the processing of two class methods to contain the dirty acid of arsenic cadmium:
Method one, lime one iron salt method, this method can guarantee dirty sour discharged wastewater met the national standard, and the molysite consumption significantly reduces; But the iron salt method process result is that arsenic is transferred in the iron oxygen slag, and the huge and arsenic content of the quantity of slag is less than 5%; Further enriching and recovering is difficult, has the secondary pollution risk;
Method two, sulfuration method; Use sodium sulphite, the vulcanizing agent of Sulfothiorine and so on arsenic, cadmium with the form fix of sulfide precipitation in the sulfuration slag, reach the purpose of removing arsenic, cadmium; Because arsenic (cadmium) percentage composition increases substantially in the sulfuration slag; Reach more than 30%, might realize the recycling of arsenic (cadmium) on planning strategies for from commerce, thereby be expected to eliminate the secondary pollution risk.
Present following three problems of sulfuration method ubiquity:
One, the arsenic percentage composition is on the low side in the sulfuration slag, and generally below 30%, the market circulation that has reduced the sulfuration slag is worth, and is unfavorable for recycling;
Two, arsenic content is higher in the water of sulfuration back; How more than 100mg/L, cadmium content is higher, and the sulfuration method can only be as the preprocessing means of arsenic (cadmium); The higher gypsum quality that influences of arsenic content in the gypsum that follow-up lime neutralizing treatment reclaims is unfavorable for recycling equally;
Three, vulcanizing agent (like sodium sulphite) consumption is considerably beyond theoretical amount, and hydrogen sulfide is escaped in a large number, not only causes processing cost to raise, and also can increase machine utilization and increase, and also can influence the production plant environment.
Why the problems referred to above can occur, reason is that sodium sulphite and arsenic, cadmium are according to following reaction equation generation precipitin reaction:
2As
3++3S
2-＝As
2S
3 (1)
Cd
2++S
2-＝CdS (2)
(1), (2) formula shows: positively charged ion arsenic (As
3+) and Cd
2+With sulphur negative ion (S
2-) combination generation red arsenic (As
2S
3) and Cadmium Sulfide (CdS) deposition.
Make in the dirty acid arsenic reaction precipitation complete, the one, must make the arsenic in the dirty acid can change into arsenic cation A s
3+, the 2nd, enough sulphur negative ion S must be provided
2-React with arsenic.
Arsenic has multiple body to exist in the aqueous solution, can transform each other between the various bodies, how to transform more As
3Then depend on external conditions---the acidity of solution.As
3+Generate according to following reaction:
AsO
3 3-+6H
+＝As
3+＝3H
2O (3)
(3) formula explanation, only As under acidic conditions
3+Ion could produce, and the deposition that also just helps arsenic is complete, also can not obtain the red arsenic deposition even if under alkaline condition, add a large amount of sodium sulphite.
Two kinds of situation are arranged in the time of in the sodium sulphite pass into solution
One, solution is for acid: following reaction can take place:
Na
2S+H
2SO
4＝NaSO
4+H
2S↑ (4)
H
2S＝2H
++S
2- (5)
How to prevent H
2How a large amount of generations and the effusion of S make to keep certain density S in the solution
2-, be the problem that promotes that vulcanization reaction must be thought deeply fully.Theory and practice proves, even if in the dirty acid of 10% sulfuric acid concentration, as long as in the solution an amount of H is arranged
2S just can dissociate the enough S that ensure that precipitin reaction is carried out
2-, therefore under acidic conditions, prevent H
2S overflows just becomes the key that vulcanization reaction is quantitatively accomplished.
Two, solution is neutral or alkaline
The tendency of following reaction (6) can take place when being neutral and alkaline in solution:
As
2S
3+3S
2-＝2AsS
3 3- (6)
Thioarseniate is water-soluble, and the generation meeting of this tendency has a negative impact to arsenic precipitation.
Summary of the invention
The objective of the invention is to above-mentioned present situation; It is few to aim to provide a kind of vulcanizing agent consumption; Arsenic recovery convergence 100%, the cadmium recovery is stabilized in more than 99.7%, and the percentage composition of arsenic reaches a kind of high-acidity high-arsenic high-cadmium waste water sulfuration recovery processing method more than 30% in the sulfuration slag.
The implementation of the object of the invention does, a kind of high-acidity high-arsenic high-cadmium waste water sulfuration recovery processing method adopts following steps:
Remove the SO in the waste water earlier
2,
Analyze the acidity and remaining SO of waste water
2, As, Cu, Cd and Sb, Sn, Pb content, and according to remaining SO
2, As, Cu, Cd and Sb, Sn, the cubage sodium sulphite of Pb or the theoretical add-on of other vulcanizing agents; Actual add-on is generally 105～110% of theoretical amount; Add the fashionable sulfuric acid that should consume or other acid amounts according to what the actual add-on of sodium sulphite or other vulcanizing agents was calculated sodium sulphite or other vulcanizing agents, the sulfuric acid that deduction should consume or other acid amounts are confirmed the add-on of lime, and settling the standard is; When vulcanization reaction finished, waste water acidity was counted 15g/L>=H with sulfuric acid
2SO
4G/L>=0.5g/L,
True quantitative lime and desulfurization wastewater are added fully stirring in the lime neutralizing well, and centrifugal or cripling separates, and reclaims gypsum,
Separating filtrate gets into the immersion bull from opening for feed 7 and is uniformly distributed with reaction unit; Turn on agitator 2; Vulcanizing agent gets into medicament distributing chamber 4 from feed-pipe 6, flows into and is uniformly distributed with chemical feed pipe 9, flows out with given pace from a plurality of dosings hole 10 that is uniformly distributed with chemical feed pipe 9 bottoms; Vulcanizing agent is uniformly distributed with and disperses to join in the filtrating, the As under fully stirring in the filtrating
3+Reaction generates As
2S
3, Cd
2+Reaction generates CdS, separates, and reclaims As
2S
3, CdS and other metallic sulfides the sulfuration slag, micro-H
2S gas is discharged from venting port 8,
The filtrating of removing slag is introduced in the lime and in the aerator tank, is added and H
2SO
4The milk of lime of reaction aequum, neutralization and aeration about adjustment pH to 8.5, separate, and reclaim gypsum, the treated water qualified discharge.
The quantity of medicament pipe of the present invention and medicine outlet hole number confirm through experiment that according to reactor volume and cross-sectional area advancing dose and advancing medicine speed of drug-feeding tube controlled by volume pump.
The present invention has following advantage:
1, set up the theoretical basis of arsenic in the dirty acid, cadmium sulfuration recycling; Establish efficient sulfuration and reclaimed the condition of arsenic, cadmium; Reformed the vulcanization reaction device, it is controlled that the basic realization of reaction is reclaimed in sulfuration, carries out according to stoichiometry basically; The consumption rate of vulcanizing agent is lower than domestic level of the same trade, obtains the highest cure efficiency with minimum reagent consumption;
2, adopt the method for the degassing or aeration before the dirty acid sulfuration, can effectively reduce SO
2Content, this can not only reduce the consumption of sodium sulphite, the SO that the while aeration comes out
2Acid making system can be returned to, pollution can be do not produced;
3, with immersion bull uniformly distributing device; Adopt " immersion bull uniformly distributing method " to vulcanize recovery; Effectively prevented " escape " of " local overrich phenomenon " and hydrogen sulfide; Be to improve sulfuration efficient; Reduce vulcanizing agent consumption; Improve the percentage composition of arsenic in the sulfuration slag, reduce the key equipment and the technology of hydrogen sulfide contamination;
4, adopt the present invention, the recovery convergence 100% of arsenic in the dirty acid, the recovery of cadmium is stabilized in more than 99.7%, and arsenic, cadmium concentration are below 1mg/L in the filtrating, and both significantly are superior to the level of domestic sulfuration process;
5, the arsenic percentage composition can reach more than 30% in the sulfuration slag that is produced, and is significantly higher than domestic level of the same trade, helps the deep processing and utilization of arsenic, realizes the resource utilization and the commercialization of arsenic, turns bane into boon, and helps the sustainable development of enterprise;
6, through in the latter stage and oxide treatment, treated water can stably reaching standard discharging; Needn't add the ferrous sulfate arsenic removing agent again with the traditional method comparison.
Description of drawings
Fig. 1 is a treatment scheme synoptic diagram of the present invention
Fig. 2 is that the immersion bull is uniformly distributed with the reaction unit structural representation
Fig. 3 is a substep device structural representation
Embodiment
Treatment scheme of the present invention is as shown in Figure 1, removes the SO in the waste water earlier
2, a large amount of waste water adopts degassing tower, and the water yield hour can adopt aerating apparatus.
Calculate the acidity of waste water, analyze wherein remaining SO
2, As, Cu, Cd and Sb, Sn, Pb content, and according to remaining SO
2, As, Cu, Cd and Sb, Sn, the cubage sodium sulphite of Pb or the theoretical add-on of other vulcanizing agents; Actual add-on is generally 105～110% of theoretical amount; Add the fashionable sulfuric acid that should consume or other acid amounts according to what the actual add-on of sodium sulphite or other vulcanizing agents was calculated sodium sulphite or other vulcanizing agents, the sulfuric acid that deduction should consume or other acid amounts are confirmed the add-on of lime, and settling the standard is; When vulcanization reaction finished, waste water acidity was counted 15g/L>=H with sulfuric acid
2SO
4G/L>=0.5g/L.
True quantitative lime and desulfurization wastewater are added fully stirring in the lime neutralizing well, and centrifugal or cripling separates, and reclaims gypsum.
Separating filtrate gets into the immersion bull from opening for feed 7 and is uniformly distributed with reaction unit; Vulcanizing agent gets into medicament distributing chamber 4 from feed-pipe 6; Flow into again and be uniformly distributed with chemical feed pipe 9; Flow out with given pace from a plurality of dosings hole 10 that is uniformly distributed with chemical feed pipe 9 bottoms, vulcanizing agent is uniformly distributed with and disperses to join in the filtrating, the As under fully stirring in the filtrating
3+Reaction generates As
2S
3, Cd
2+Reaction generates CdS, filters, and reclaims As
2S
3, CdS and other metallic sulfides the arsenic slag, micro-H
2S gas is discharged from venting port 8, is sent to the tower of removing the evil through induced exhaust and absorbs.
The filtrating of removing slag is introduced in the lime and in the aerator tank, is added and H
2SO
4The milk of lime of reaction aequum, neutralization and aeration about adjustment pH to 8.5, separate, and reclaim gypsum, the treated water qualified discharge.
Treatment unit of the present invention adopts and is uniformly distributed with reaction unit like Fig. 2, the intermittent type immersion bull shown in 3; Manhole 1, vapor pipe 8 are arranged at top; Opening for feed 7, discharge opening 5 are arranged on the wall, in baffle plate 3, whisking appliance 2 are arranged, medicament distributing chamber 4 is arranged at the bottom; There is the feed-pipe 6 that communicates with it in medicament distributing chamber 4, is uniformly distributed with chemical feed pipe 9, and being uniformly distributed with the chemical feed pipe bottom has a plurality of dosings hole 10.
Enumerate the specific embodiment of the invention below:
250 liters of instance 1, waste water, testing program: adopt the immersion bull to be uniformly distributed with reaction unit, the reinforced and reaction times: 30 minutes, sodium sulphite was excessive 10%, and result is seen table 1,
Table 1
| Composition | H 2SO 4(g/L) | As(mg/L) | Cu(mg/L) | Cd(mg/L) | Temperature |
| Content before handling | 25 | 3420 | 459 | 158.7 | 30℃ |
| Handle content in the rear filtrate | 16.7 | 0.15 | Do not pick | Do not pick | ? |
| Handle content (%) in the postcure slag | ? | 43.38 | ? | ? | ? |
| The arsenic recovery (%) | ? | ∝100％ | ? | ∝100％ | ? |
Example 2,250 liters of waste water, testing program: adopt intermittent type immersion bull to be uniformly distributed with reaction unit, the reinforced and reaction times: 30 minutes, sodium sulphite was excessive 10%, and result is seen table 2,
Table 2
| Composition | H 2SO 4(g/L) | As(mg/L) | Cu(mg/L) | Cd(mg/L) | Temperature |
| Content before handling | 24 (neutralization backs) | 4900 | 108.5 | 291.4 | 30℃ |
| Handle content in the rear filtrate | 12.98 | 0.62 | Do not pick | Do not pick | ? |
| Handle content (%) in the postcure slag | ? | 35.94 | ? | ? | ? |
| The arsenic recovery (%) | ? | ∝100％ | ? | ∝100％ | ? |
Instance 3,22 cubic metres of waste water (technical scale)
Testing program: adopt the immersion bull to be uniformly distributed with reaction unit, the reinforced and reaction times: 120 minutes, sodium sulphite was excessive 10%, and result is seen table 3,
Table 3
| Composition | H 2SO 4(g/L) | As(mg/L) | Cu(mg/L) | Cd(mg/L) | Temperature |
| Content before handling | 42.17 | 4.14 | 350 | 180 | 30℃ |
| Handle content in the rear filtrate | 11.56 | 0.13 | / | 0.6 | ? |
| Handle content (%) in the postcure slag | ? | 30.09％ | / | ? | ? |
| The recovery (%) | ? | ∝100％ | ? | 99.7％ | ? |
Visible from above test-results, adopt the present invention, effectively prevented " escape " of " local overrich phenomenon " and hydrogen sulfide; This is to improve sulfuration efficient; Reduce vulcanizing agent consumption, improve the percentage composition of arsenic in the sulfuration slag, reduce the key equipment and the technology of hydrogen sulfide contamination; The recovery convergence 100% of arsenic, the recovery of cadmium is stabilized in more than 99.7%.
Claims (1)
1. high-acidity high-arsenic high-cadmium waste water sulfuration recovery processing method is characterized in that adopting following steps:
Remove the SO in the waste water earlier
2,
Analyze the acidity and remaining SO of waste water
2, As, Cu, Cd and Sb, Sn, Pb content, and according to remaining SO
2, As, Cu, Cd and Sb, Sn, the cubage sodium sulphite of Pb or the theoretical add-on of other vulcanizing agents; Actual add-on is 105～110% of a theoretical amount; Add the fashionable sulfuric acid that should consume or other acid amounts according to what the actual add-on of sodium sulphite or other vulcanizing agents was calculated sodium sulphite or other vulcanizing agents, the sulfuric acid that deduction should consume or other acid amounts are confirmed the add-on of lime, and settling the standard is; When vulcanization reaction finished, waste water acidity was counted 15g/L>=H with sulfuric acid
2SO
4G/L>=0.5g/L,
True quantitative lime and desulfurization wastewater are added fully stirring in the lime neutralizing well, and centrifugal or cripling separates, and reclaims gypsum,
Separating filtrate gets into the immersion bull from opening for feed (7) and is uniformly distributed with reaction unit; Turn on agitator (2); Vulcanizing agent gets into medicament distributing chamber (4) from feed-pipe (6), flows into and is uniformly distributed with chemical feed pipe (9), flows out with given pace from a plurality of dosings hole (10) that is uniformly distributed with chemical feed pipe (9) bottom; Vulcanizing agent is uniformly distributed with and disperses to join in the filtrating, the As under fully stirring in the filtrating
3+Reaction generates As
2S
3, Cd
2+Reaction generates CdS, separates, and reclaims As
2S
3, CdS and other metallic sulfides the sulfuration slag, micro-H
2S gas is discharged from vapor pipe (8),
The filtrating of removing slag is introduced in the lime and in the aerator tank, is added and H
2SO
4The milk of lime of reaction aequum, neutralization and aeration, adjustment pH to 8.5 separates, and reclaims gypsum, the treated water qualified discharge.
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| CN102030439A (en) * | 2010-11-22 | 2011-04-27 | 浙江双屿实业有限公司 | Sewage and waste acid treatment device and treatment process thereof |
| CN102249450B (en) * | 2011-05-11 | 2012-08-29 | 天津理工大学 | Method for removing trace cadmium from aqueous solution |
| CN102978397A (en) * | 2012-10-12 | 2013-03-20 | 金川集团股份有限公司 | Removal method of arsenic from arsenic-containing waste liquid with high acidity |
| CN102897885B (en) * | 2012-10-26 | 2016-04-27 | 广西南宁东和新赢环保技术有限公司 | The method of sulfuric acid industry Two-way Cycle jet-type arsenic removal |
| CN103112974B (en) * | 2013-01-22 | 2014-07-23 | 长沙创享环保科技有限公司 | Treatment method of arsenic wastewater |
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| JP7031207B2 (en) * | 2017-10-05 | 2022-03-08 | 住友金属鉱山株式会社 | Treatment method of waste acid generated in copper smelting |
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| CN108467133B (en) * | 2018-04-11 | 2021-04-20 | 赛恩斯环保股份有限公司 | Treatment method for recycling arsenic and cadmium separation resources in precious metal smelting wastewater |
| CN109055780A (en) * | 2018-07-18 | 2018-12-21 | 河南中原黄金冶炼厂有限责任公司 | A kind of method of iron sulfonium processing pyrometallurgical smelting acid making system spent acid containing arsenic |
| CN110054322B (en) * | 2019-05-22 | 2021-05-11 | 海洲环保集团有限公司 | Hazardous waste residue reduction treatment system and process for heavy metal-containing acidic wastewater |
| CN111875087A (en) * | 2020-06-12 | 2020-11-03 | 金川集团股份有限公司 | Method for removing copper and arsenic from complex precious metal wastewater |
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