CN110055416A - A kind of method of zinc hydrometallurgy industrial sulphuric acid hydrochloric acid separating and recovering - Google Patents
A kind of method of zinc hydrometallurgy industrial sulphuric acid hydrochloric acid separating and recovering Download PDFInfo
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- CN110055416A CN110055416A CN201910439574.1A CN201910439574A CN110055416A CN 110055416 A CN110055416 A CN 110055416A CN 201910439574 A CN201910439574 A CN 201910439574A CN 110055416 A CN110055416 A CN 110055416A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The present invention relates to a kind of methods of zinc hydrometallurgy industrial sulphuric acid hydrochloric acid separating and recovering.The sulfate acid-mixed acid generated for the chloride ion in zinc hydrometallurgy industrial ionic exchange process removal solution of zinc sulfate, in conjunction with zinc hydrometallurgy production process, the acidity of nitration mixture is improved by way of adding sulfuric acid, then the hydrochloric acid in nitration mixture is largely steamed by the method for vacuum distillation, remaining sulfuric acid contains the hydrochloric acid of low concentration, a portion is used for the acidleach process of the miscellaneous secondary zinc-containing raw materials of Zinc Hydrometallurgy Process, dilute sulfuric acid is obtained after another part water supplement, strippant as ion-exchange removing chloride process, to realize the reuse of sulfuric acid, the hydrochloric acid of recycling can be used for producing zinc chloride product, it eliminates sulfate acid-mixed acid and calcium sulfate slag and calcium chloride wastewater is led to the problem of using the processing of lime neutralization precipitation method.
Description
Technical field
The invention belongs to technical field of chemistry, it is related to the sulfate acid-mixed generated in a kind of zinc hydrometallurgy industrial processes
The method that acid separation and recovery utilizes.
Background technique
Mainly using zinc concentrate as raw material, other miscellaneous secondary raw materials containing zinc are also important raw material sources for zinc hydrometallurgy industry.Contain
The miscellaneous secondary raw material of zinc is mainly zinc dross, the Zinc smelting ingot casting of the zinc smoke of pyrometallurgical smelting process generation, hot galvanizing process generation
The oxidation zinc dross that process generates, these miscellaneous secondary zinc-containing raw materials usually contain the chlorine element of 0.2-8%, in Zinc Hydrometallurgy Process
Dissolution enters solution of zinc sulfate, and chloride ion content in zinc liquid is caused to be up to every liter several grams, significantly beyond general enterprises control
The index of 0.1g/L.Contain chloride ion in solution of zinc sulfate, hydrochloric acid and salt acid mist, electrolyte will be generated during DC electrolysis
The hydrochloric acid of middle generation will corrode cathode-anode plate, reduce the pole plate service life, influence electrolytic zinc quality, and salt acid mist will deteriorate potroom ring
Border air and labour health condition.
Zinc hydrometallurgy enterprise generallys use ion-exchange dechlorination aiming at the problem that above-mentioned chloride ion superelevation at present.First
Resin anion (R.A.) is transformed into-SO by dilute sulfuric acid4 2-Type, then sulfuric chlorohydrin zinc solution will be contained and pass through ion exchange resin layer, zinc liquid
In Cl-With the SO in resin4 2-It swaps and enters in resin, to realize the removal of chloride ion in zinc liquid.Ion exchange
Resin is by Cl-After saturation, zinc sulfate solution stops input, then dilute sulfuric acid, the Cl in resin are passed through into ion exchange resin layer-
By the SO in dilute sulfuric acid4 2-To realize that the regeneration of resin makes the transition, resin enters back into the subsequent work period for exchange.In resin
Cl-By the SO in dilute sulfuric acid4 2-Enter in dilute sulfuric acid after exchange, so that a kind of sulfate acid-mixed acid is generated, because chlorine therein is wet
The harmful element of method zinc metallurgy process causes the nitration mixture to cannot be directly used to zinc metallurgy process and become industrial wastewater.For this kind of acid
Property industrial wastewater, zinc hydrometallurgy enterprise generally uses lime neutralization precipitation method to handle at present, and sulfuric acid and lime reaction generate sulfuric acid
Calcium precipitate, and hydrochloric acid and lime reaction generate water-soluble calcium chloride, waste water is in neutrality alkalinity on the weak side outlet again after neutralization.
The technical problem that the sulfate acid-mixed acid recycles is the influence of wherein hydrochloric acid, and how sulfuric acid and hydrochloric acid divide in other words
From.At present for the separation of dilute hydrochloric acid, the method industrially used includes roasting method, extraction, evaporation and electrolysis method.
(1) roasting method.The method is applied to the processing of steel plant's acid-washing waste acid, and under high temperature, dilute hydrochloric acid and moisture evaporate to obtain
Hydrochloric acid is recycled, obtains iron oxide byproduct after the ferrous ion high-temperature oxydation in pickling solution.The method is in the condition of high temperature, and acid mist produces
Raw amount is big, and energy consumption is high, is not suitable for the separation of above-mentioned nitration mixture；
(2) extraction.Extraction and separation are carried out to hydrochloric acid as extractant using tributyl phosphate, primary amine etc., but are existed in sulfuric acid
Under conditions of, the effect of extracting of hydrochloric acid significantly reduces；
(3) evaporation.Utilize the hydrochloric acid boiling point feature low compared with sulfuric acid, by nitration mixture ebuillition of heated, hydrochloric acid and water evaporation, to realize
The separation of sulfuric acid and hydrochloric acid, but the method is formed azeotropic solution with water by hydrochloric acid and is limited, when the mass fraction of hydrochloric acid in liquid
Form azeotropic mixture when reaching 20.24%, continue ebuillition of heated, the content of hydrochloric acid in liquid will be reduced no longer, thus influence sulfuric acid with
The final effect of hydrochloric acid separation；
(4) electrolysis method.By DC electrolysis, the hydrochloric acid in nitration mixture is subjected to electrolytic separation in the form of chlorine.Existing for the method
Problem is power consumption height, and the chlorine of generation needs mating processing unit.
Summary of the invention
In order to solve above-mentioned zinc hydrometallurgy industry due to leading to chloride ion content in solution of zinc sulfate using raw material containing chlorine
Superelevation, and the method for using ion exchange dechlorination, in solution of zinc sulfate is effectively reduced while chloride ion content, but generate one
Kind of sulfate acid-mixed acid, and the nitration mixture cannot be directly used to zinc metallurgy process and become the prior art problem of industrial wastewater.This hair
It is bright to provide a kind of method of zinc hydrometallurgy industrial sulphuric acid hydrochloric acid separation and recovery, it is by the separation of the nitration mixture and zinc hydrometallurgy industry
The method that process combines.
To realize the present invention, as follows using technical solution:
(1) anion exchange resin in exchange column is after the desorption transition of the dilute sulfuric acid of mass ratio 5-15%, by chloride ion-containing
The zinc sulfate solution of 0.5-5g/L is passed through in exchange column, and the chloride ion in zinc sulfate solution is adsorbed into resin, detects efflux
Middle chloride ion average content is less than 0.1g/L and stops feed liquor, and ion exchange resin adsorbing chloride ions are in a saturated state.Outflow
Zinc sulfate solution send to zinc hydrometallurgy electrowinning process；
(2) ion exchange resin of adsorption saturation is desorbed by dilute sulfuric acid and is made the transition, and dilute sulfuric acid comes from the sulfate acid-mixed of process (4)
Sour vacuum distillation process, nitration mixture are reduced by content of hydrochloric acid after vacuum distillation, are 5-15% with sulfuric acid mass ratio is added water to, wherein
Remaining chloride ion content is 0.1-0.5g/L, makes it through ion exchange resin column, resin desorption is simultaneously transformed into-SO4 2-Type is again
Into the adsorption process of process (1), desorbs transformation process and generate sulfate acid-mixed acid, wherein sulfur acid mass ratio is 5-10%, is contained
Chloride ion 2.5-20g/L；
(3) sulfate acid-mixed acid is evaporated under reduced pressure separation process.It is less than the characteristic of sulfuric acid using the boiling point of hydrochloric acid, in ebuillition of heated shape
Under state, hydrochloric acid, which is preferentially distilled, leaves solution in gaseous state to realizing sulfuric acid and a degree of separation of hydrochloric acid, and gaseous hydrochloric acid is cold
It coagulates for dilute hydrochloric acid, gaseous state condensation volume sharply reduces thus System forming negative pressure.Due to chloride ion content only 2.5- in the nitration mixture
20g/L, a large amount of water will be evaporated by directly heating distillation, therefore increase acidity by way of adding sulfuric acid in advance, and control is mixed
Sulfuric acid mass ratio is 30-40% in acid, with this condition heating distillation, and hydrochloric acid will steam preferentially, at the end of distillation in nitration mixture chlorine from
Sub- content is 0.5-4g/L, and sulfuric acid mass ratio is 37-50%, is equivalent to hydrochloric acid and is separated off 65-85% from nitration mixture, isolates
Dilute hydrochloric acid is used for zinc chloride production process；
(4) the nitration mixture a part for obtaining process (3) be used for the miscellaneous secondary zinc-containing raw materials acidleach process of zinc hydrometallurgy, another part with addition of
Water is 5-15% to sulfuric acid mass ratio, and the ion exchange resin as process (1) desorbs transition dilute sulfuric acid, is hereafter repeated
Subsequent process realizes the dechlorination purpose of chloride ion and the purpose of sulfate acid-mixed acid separating and recovering in solution of zinc sulfate.
The sulfate acid-mixed acid that Zinc Hydrometallurgy Process generates is separated by this method, the hydrochloric acid of recycling can be used for giving birth to
Zinc chloride product is produced, and sulfuric acid is for the acidleach process of the miscellaneous secondary zinc-containing raw materials of zinc hydrometallurgy industry and dilute sulphur of ion exchange dechlorination
Acidolysis vapor.
Compared with prior art, beneficial effects of the present invention also reside in:
(1) compared with the existing sulfate acid-mixed acid lime neutralization precipitation facture of zinc hydrometallurgy factory, sulfuric acid and hydrochloric acid can be with
Realization is separated and recovered from utilization；
(2) compared with the existing sulfate acid-mixed acid lime neutralization precipitation facture of zinc hydrometallurgy factory, treatment process is not consumed
The alkaline matters such as lime, advantageously reduce processing cost；
(3) compared with the existing sulfate acid-mixed acid lime neutralization precipitation facture of zinc hydrometallurgy factory, treatment process is not generated
Calcium sulfate precipitation does not generate the efflux wastewater of chloride containing calcium；
(4) addition sulfuric acid can be such that hydrochloric acid preferentially steams in advance to improve solution acidity before the vacuum distillation of sulfate acid-mixed acid, can be with
Distillation cost is reduced, and the sulfuric acid of pre-add is used for miscellaneous secondary zinc-containing raw materials acidleach process hereafter, does not increase sulfuric acid consumption, realizes sulphur
The combination of the hydrochlorate separation process of acid-mixed acid and zinc hydrometallurgy production technology.
Detailed description of the invention
Fig. 1 is the process drawing of zinc hydrometallurgy industrial sulphuric acid hydrochloric acid separating and recovering method of the present invention.
Specific embodiment
Technical solution of the present invention is further illustrated with reference to the accompanying drawings and examples.
Referring to Fig.1, zinc hydrometallurgy industrial sulphuric acid hydrochloric acid separating and recovering method, comprising the following steps:
(1) after anion exchange resin is packed into exchange column, the dilute sulfuric acid desorption for being passed through mass ratio 5-15% is transformed into rear-SO4 2-Type.
Then the sulfuric acid zinc purification fluid of the chloride ion-containing 0.5-5g/L obtained after miscellaneous secondary zinc-containing raw materials acidleach is flowed into certain flow velocity
Ion exchange column, the Cl in solution of zinc sulfate-- SO in ion and resin4 2-It swaps and enters in resin, detection outflow
It is in a saturated state to be less than 0.1g/L i.e. stopping feed liquor, ion exchange resin adsorbing chloride ions for chloride ion average content in liquid.Stream
Zinc sulfate solution out is sent to zinc hydrometallurgy electrowinning process；
(2) ion exchange resin of adsorption saturation desorbs transition by dilute sulfuric acid again, and dilute sulfuric acid comes from the sulfate of process (4)
Acid-mixed acid vacuum distillation process, nitration mixture is reduced by content of hydrochloric acid after vacuum distillation, sulfuric acid content increases, with adding water to sulfuric acid matter
Amount makes it through ion exchange resin column, resin desorption wherein remaining chloride ion content is 0.1-0.5g/L than being 5-15%
Chloride ion and it is transformed into-SO out4 2-Type enters the adsorption process of process (1) again, and desorption transformation process generates sulfate acid-mixed acid,
Wherein sulfur acid mass ratio is 5-10%, chloride ion-containing 2.5-20g/L；
(3) sulfate acid-mixed acid is evaporated under reduced pressure separation process.Under normal pressure, 20.2% hydrochloric acid boiling point is 110 DEG C, concentrated sulfuric acid boiling point
It is 337 DEG C, the characteristic of sulfuric acid is less than using the boiling point of hydrochloric acid, under ebuillition of heated state, hydrochloric acid is preferentially distilled to be left in gaseous state
Solution is condensed into dilute hydrochloric acid to realize sulfuric acid and a degree of separation of hydrochloric acid, by gaseous hydrochloric acid, and volume is anxious after gaseous state condensation
Play is reduced to System forming negative pressure, and negative pressure advantageously reduces the boiling point of solution.Due to chloride ion content only 2.5- in the nitration mixture
20g/L, a large amount of water will be evaporated by directly heating distillation, therefore increase acidity by way of adding sulfuric acid in advance, and control is mixed
Sulfuric acid mass ratio is 30-40% in acid, with this condition heating distillation, and hydrochloric acid will steam preferentially, at the end of distillation in nitration mixture chlorine from
Sub- content is 0.5-4g/L, and sulfuric acid mass ratio is 37-50%, is equivalent to hydrochloric acid and is separated off 65-85% from nitration mixture, isolates
Dilute hydrochloric acid is used for zinc chloride production process；
(4) the nitration mixture a part for obtaining process (3) is for the miscellaneous secondary zinc-containing raw materials acidleach process of zinc hydrometallurgy industry, another part
It is 5-15% with addition of water to sulfuric acid mass ratio, the ion exchange resin as process (1) desorbs transition dilute sulfuric acid, hereafter repeats
Subsequent process is carried out, realizes the mesh of the separating and recovering of the dechlorination purpose and sulfate acid-mixed acid of chloride ion in solution of zinc sulfate
's.
The technical economic analysis of this invention:
The sulfuric acid that invention progress sulfuric acid hydrochloric acid separating and recovering process is added is eventually for the miscellaneous secondary zinc-containing raw materials of zinc hydrometallurgy industry
Acidleach process, do not cause consumption of raw materials additionally, only need in the process consumption distillation process heating steam.Through calculating, with
For one ton of electrolytic zinc of every production, 1.2-2.0 cubic metres of the sulfate acid-mixed acid of above-mentioned composition need to be handled, 0.15- need to be distilled
0.25 cubic metre of liquid need to consume steam 0.2-0.3 tons of heating, value about 52-78 member.Under square one, zinc hydrometallurgy work
The existing sulfate acid-mixed acid lime neutralization precipitation facture of factory need to consume 0.08-0.2 tons of quick lime, and value about 32-80 is first, together
When generate 0.25-0.61 tons of calcium sulfate (anhydrous) waste residues, the calcium chloride containing 4.0-31g/L in furthermore treated waste water.It is comprehensive
Composition and division in a proportion is compared with the expense of two kinds of processing methods is close, but in view of existing lime neutralization precipitation method cannot be real by sulfuric acid and hydrochloric acid
It is now separated and recovered from utilization, and generates calcium sulfate waste residues and calcium chloride wastewater, zinc hydrometallurgy industrial sulphuric acid hydrochloric acid of the invention
Separating and recovering method has significant techno-economic effect, and the hydrochloric acid of recycling can be used for producing zinc chloride product, and sulfuric acid is used for
The acidleach process of the miscellaneous secondary zinc-containing raw materials of zinc hydrometallurgy industry and the dilute sulfuric acid strippant of ion exchange dechlorination.
The above, only best mode for carrying out the invention, anyone skilled in the art is in the present invention
In the technical scope of disclosure, the simple change or equivalence replacement for the technical solution that can be become apparent to each fall within of the invention
In protection scope.
Claims (1)
1. a kind of method of zinc hydrometallurgy industrial sulphuric acid hydrochloric acid separating and recovering, it is characterised in that the following steps are included:
(1) anion exchange resin in exchange column is after the dilute sulfuric acid desorption transition that mass ratio is 5-15%, by chloride ion-containing
The zinc sulfate solution of 0.5-5g/L is passed through in exchange column, and the chloride ion in zinc sulfate solution is adsorbed into resin, detects efflux
Middle chloride ion average content is less than 0.1g/L and stops feed liquor, and ion exchange resin adsorbing chloride ions are in a saturated state, outflow
Zinc sulfate solution send to zinc hydrometallurgy electrowinning process；
(2) ion exchange resin of adsorption saturation is desorbed by dilute sulfuric acid and is made the transition, and dilute sulfuric acid comes from the sulfate acid-mixed of process (4)
Sour vacuum distillation process, nitration mixture are reduced by content of hydrochloric acid after vacuum distillation, are 5-15% with sulfuric acid mass ratio is added water to, wherein
Remaining chloride ion content is 0.1-0.5g/L, makes it through ion exchange resin column, resin desorption is simultaneously transformed into-SO4 2-Type is again
Into the adsorption process of process (1), desorbs transformation process and generate sulfate acid-mixed acid, wherein sulfur acid mass ratio is 5-10%, is contained
Chloride ion 2.5-20g/L；
(3) the vacuum distillation separation of sulfate acid-mixed acid: it is less than the characteristic of sulfuric acid using the boiling point of hydrochloric acid, in ebuillition of heated state
Under, hydrochloric acid, which is preferentially distilled, leaves solution in gaseous state to realize sulfuric acid and a degree of separation of hydrochloric acid, and gaseous hydrochloric acid is condensed
For dilute hydrochloric acid, gaseous state condensation volume sharply reduces to System forming negative pressure；Due to chloride ion content only 2.5- in the nitration mixture
20g/L, a large amount of water will be evaporated by directly heating distillation, therefore increase acidity by way of adding sulfuric acid in advance, and control is mixed
Sulfuric acid mass ratio is 30-40% in acid, with this condition heating distillation, and hydrochloric acid will steam preferentially, at the end of distillation in nitration mixture chlorine from
Sub- content is 0.5-4g/L, and sulfuric acid mass ratio is 37-50%, is equivalent to hydrochloric acid and is separated off 65-85% from nitration mixture, isolates
Dilute hydrochloric acid is used for zinc chloride production process；
(4) the nitration mixture a part for obtaining process (3) is used for miscellaneous secondary zinc-containing raw materials acidleach process, and another part is with addition of water to sulfuric acid
Mass ratio is 5-15%, and the ion exchange resin as process (1) desorbs transition dilute sulfuric acid, hereafter repeats subsequent process,
Realize the purpose of the separating and recovering of the dechlorination purpose and sulfate acid-mixed acid of chloride ion in solution of zinc sulfate.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111994872A (en) * | 2020-09-01 | 2020-11-27 | 江苏康祥实业集团有限公司 | Method for recovering sulfuric acid in benzene sulfonyl chloride production process |
| CN113292094A (en) * | 2021-06-02 | 2021-08-24 | 江西思远再生资源有限公司 | Method for removing chlorine radicals and sulfate radicals in secondary zinc oxide raw material |
| CN113694552A (en) * | 2020-05-22 | 2021-11-26 | 江西理工大学 | Method and system for removing fluorine and/or chlorine from sulfate solution by flash evaporation |
| CN114959296A (en) * | 2022-05-18 | 2022-08-30 | 陕西中创进取科技有限公司 | Process method for producing hydrochloric acid by sulfuric acid extraction through zinc hydrometallurgy ion exchange dechlorination |
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| JPH067782A (en) * | 1992-05-18 | 1994-01-18 | Nippon Parkerizing Co Ltd | Treatment of heavy metal ion-containing waste solution |
| CN101492772A (en) * | 2009-02-27 | 2009-07-29 | 宋志红 | Fluorine and chlorine removal process for zinc metallurgy industrialization ion exchange process with wet-process |
| CN105439356A (en) * | 2015-12-28 | 2016-03-30 | 中南大学 | Method and device for synchronously recycling sulfuric acid and fluorine and chlorine from polluted acid |
| CN106277514A (en) * | 2015-06-05 | 2017-01-04 | 西南大学 | The method of recycling saccharin sodium wastewater |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH067782A (en) * | 1992-05-18 | 1994-01-18 | Nippon Parkerizing Co Ltd | Treatment of heavy metal ion-containing waste solution |
| CN101492772A (en) * | 2009-02-27 | 2009-07-29 | 宋志红 | Fluorine and chlorine removal process for zinc metallurgy industrialization ion exchange process with wet-process |
| CN106277514A (en) * | 2015-06-05 | 2017-01-04 | 西南大学 | The method of recycling saccharin sodium wastewater |
| CN105439356A (en) * | 2015-12-28 | 2016-03-30 | 中南大学 | Method and device for synchronously recycling sulfuric acid and fluorine and chlorine from polluted acid |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113694552A (en) * | 2020-05-22 | 2021-11-26 | 江西理工大学 | Method and system for removing fluorine and/or chlorine from sulfate solution by flash evaporation |
| CN113694552B (en) * | 2020-05-22 | 2023-01-17 | 江西理工大学 | Method and system for removing fluorine and/or chlorine from sulfate solution by flash evaporation |
| CN111994872A (en) * | 2020-09-01 | 2020-11-27 | 江苏康祥实业集团有限公司 | Method for recovering sulfuric acid in benzene sulfonyl chloride production process |
| CN113292094A (en) * | 2021-06-02 | 2021-08-24 | 江西思远再生资源有限公司 | Method for removing chlorine radicals and sulfate radicals in secondary zinc oxide raw material |
| CN114959296A (en) * | 2022-05-18 | 2022-08-30 | 陕西中创进取科技有限公司 | Process method for producing hydrochloric acid by sulfuric acid extraction through zinc hydrometallurgy ion exchange dechlorination |
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Application publication date: 20190726 |