CN106630313A - Reduction circulation process method for recycling zinc elements in iron-containing waste acid - Google Patents
Reduction circulation process method for recycling zinc elements in iron-containing waste acid Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/203—Iron or iron compound
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a reduction circulation process method for recycling zinc elements in iron-containing waste acid. The reduction circulation process method includes the steps: pretreatment; extracted iron and zinc separation; extractant regeneration; back-extractant adjustment; back-extractant regeneration. The reduction circulation process method has the advantages that the removal rate of the treated zinc elements can reach 99%-99.5%, the recycled iron-containing waste acid can be widely applied to preparation of high-quality water purifying agents PFS or FeCl3 and the like, efficient fluorine removal agents obtained by back-extraction treatment can be used for efficiently purifying photovoltaic wastewater, an extractant has high efficiency and selectivity and can be regenerated and reused after back-extraction treatment, back-extractant water can be also regenerated and reused, the process is simple to operate, safe, clean and environmentally friendly and runs to form complete closed circulation, zero pollution and zero emission are realized, the iron-containing waste acid is thoroughly treated and recycled, and the method has double benefits of economical efficiency and environmental protection.
Description
Technical field
The invention belongs to endanger useless disposal, resource regeneration and technical field of developing a circular economy, are related to a kind of iron content and give up
Acid treatment and the process of recycling, and in particular to a kind of decrement circulation technology of the zinc element in recovery ferrous waste acid
Method.
Background technology
Steel members blank electroplating surface, spray it is previous as will through pickling, to remove the oxide on surface, thus
Produce a large amount of pickle liquors and pickling waste waterss.High concentration acidity and ferrum are typically contained in such waste liquid, according to statistics, sulfuric acid washing gives up
Contain 100～150g/L of sulphuric acid, FeSO in liquid4200～250g/L, typically contains FeCl in hydrochloric acid pickling waste liquor2150～280g/L,
10～50g/L of hydrochloric acid, therefore with good value and application prospect.But it is high due to the particularity of process treatment process
The inevitable resource that seriously govern ferrous waste acid of the introducing of content zinc element is recycled.
Early stage adopts neutralization precipitation method for the process of pickle liquor, i.e., directly add toward pickle liquor alkali solid or
Alkali liquor, improves its pH, heavy metal ion contained in pickle liquor is precipitated and is separated from water, so as to realize waste liquid row up to standard
The purpose put.The method is fairly simple, is easier to be received by blowdown enterprise.But the shortcoming of the method is that not only solid slag amount is big,
It is difficult to process, easily causes secondary pollution, and the precious resources in waste liquid can not be made full use of, thus protection ring can be reached far away
Border and the dual purpose of Resource recovery.With regard to the comprehensive utilization of resources of ferrous waste acid, lot of domestic and foreign scientific research institution and high
Universities and colleges are made that substantial amounts of research work, and such as Wang Xingyao locates in patent application CN201610084122.2 by the way that reduction is pre-
The multi-step process steps such as reason, double purification process, the preparation of iron oxide yellow crystal seed, and air oxidation drying is passed through by ferrous ion
It is converted into iron oxide yellow to be reclaimed, but the detached problem of heavy metal zinc in ferrous waste acid is not directed in its processing procedure,
Therefore its iron oxide yellow product for reclaiming is difficult to reach standard requirement used in connection with.Xiao Jin is preferably waited in patent application
In CN201610018595.2, pickle liquor containing zinc reduced using iron filings or iron plate, consume acid treatment and obtain ferrous chloride
Feed liquid, then by N235 extract and separate zinc and ferrum, it is many finally by dilute sulfuric acid back extraction organic faciess, strip liquor segmentation alkaline cleaning etc.
Process steps realize that extractant is reused with the regeneration of strip liquor, and so as to reclaim pure solution of ferrous chloride is obtained, but
It is that its technique is complex, condition is harsh, operation requirement is higher, and a large amount of hydrogen can be produced during iron reduction, there is one
Determine secondary pollution and the security risk of degree.Cui Shihai etc. is successively pungent by three in patent application CN201110211812.7
Amine extraction separation of Zinc, sodium sulfide precipitation remove zinc and lead element in ferrous chloride acidic waste water except lead two-step process, while sharp
Regenerated with inorganic alkali solution back extraction load organic phases, finally reclaim and obtain solution of ferrous chloride, but its technique is simply single
One, without reference to back washing agent regeneration a series of problems, such as, technique does not form whole closed cycle, and restricted application,
It is only applicable to the purified treatment of low zinc-iron-containing spent acid (Zn≤10000mg/L).
Many defects and drawback that the present invention exists for said method, by the operation of emerging multi-stage continuous extraction technique
Ferrum zinc high-purity separation in high zinc-iron-containing spent acid is realized, so as to the improvement for reaching ferrous waste acid is mutually tied with comprehensive utilization of resources
The target of conjunction.
The content of the invention
The technical problem to be solved in the present invention is：Based on the problems referred to above, the present invention is provided in a kind of recovery ferrous waste acid
The decrement circulation technology method of zinc element.
The present invention solves a technical scheme being adopted of its technical problem：A kind of zinc element in recovery ferrous waste acid
Decrement circulation technology method, comprise the following steps：
(1) pretreatment：Ferrous waste acid coarse filtration is removed into big particle suspended contamination, extraction equipment is pumped into；
(2) extract ferrum zinc to separate：Constantly injection complexing extractant carries out multi-stage continuous extraction in extraction equipment, by zinc unit
Element is extracted in organic faciess, two-phase laminated flow, obtains load organic phases zinc-iron-containing spent acid raffinate mutually low with water；
(3) extractant regeneration：Back washing agent is added to carry out back extraction regeneration in the load organic phases in step (2), after back extraction
Zinc element in load organic phases is with Zn (OH)4 2-Form be transferred in back washing agent, two-phase laminated flow obtains organic after back extraction
Acid waste water mutually and after back extraction；
(4) regulation of back washing agent：Add lime cream in the acid waste water after the back extraction in step (3), adjust pH=8～
8.5, filter after zinc hydroxide precipitation is separated out, cadmia and low containing the neutral waste water of zinc after filter；
(5) regeneration of back washing agent：The low neutrality waste water containing zinc in step (4) is pumped into into electrodialysis plant to be disposed, is obtained
High performance agent for removing fluorin and the regeneration water of reuse to back extraction operation.
Further, ferrous waste acid is pickling iron and steel industry waste hydrochloric acid containing iron or iron content Waste Sulfuric Acid, weight of iron in step (1)
Content presses Fe2O310～18% are calculated as, zinc mass content is calculated as 1000～40000mg/L by Zn.
Further, complexing extractant is by chelating agent di-(2-ethylhexyl)phosphoric acid ester (P204) in step (2) and dilutes
Agent sulfonated kerosene is constituted, and the volumetric concentration of di-(2-ethylhexyl)phosphoric acid ester is 30～50%.
Further, complexing extractant is 0.5～1 with the volume ratio and feed flow rate ratio of ferrous waste acid in step (2)：
1。
Further, the mutually low zinc-iron-containing spent acid raffinate of water for obtaining in step (2) make semi-finished product carry out it is follow-up comprehensive
Close and utilize or direct marketing.
Further, back washing agent is water in step (3), and it is with the volume ratio and feed flow rate ratio of load organic phases
1.5～2：1.
Further, the organic faciess in step (3) after back extraction are the extractant after regeneration, and being back to extraction cells circulation makes
With.
Further, acid waste water pH=2～3 in step (4) after back extraction, the dosage of lime cream is the acid after back extraction
The 4～5% of property wastewater quality.
Further, cadmia is recycled as zinc mud after filter in step (4).
Further, high performance agent for removing fluorin contains the calcium chloride of mass content 25～30% in step (5), for photovoltaic wastewater
Purified treatment.
The invention has the beneficial effects as follows：(1) the inventive method is separated in ferrous waste acid using multi-stage continuous extraction technique
Zinc element, the clearance of the zinc element Jing after processing is up to more than 99%～99.5%；(2) after the inventive method is processed and reclaimed
Ferrous waste acid can be widely applied to high-quality water purification agent PFS or FeCl3Deng preparation, the high-effective defluorination that obtains Jing after back extraction is processed
Agent can be used for the high-efficient purification of photovoltaic wastewater and process；(3) extractant that the present invention is used has high efficiency and high selectivity, and Jing is anti-
Renewable recycling after extraction process, the similarly renewable circulating and recovering of back washing agent water；(4) present invention process it is simple to operate, peace
Entirely, cleaning, environmental protection, process operation forms a whole set of closed cycle, no pollution zero-emission, thoroughly realize the improvement of ferrous waste acid with
Recycling, with the economic double benefit with environmental protection.
Description of the drawings
Below in conjunction with the accompanying drawings the present invention is further described.
Fig. 1 is the process chart of the present invention.
Specific embodiment
Presently in connection with specific embodiment, the invention will be further described, and following examples are intended to illustrate rather than
Limitation of the invention further.
The zinc element in steel industry pickle liquor is removed using the process of the present invention, the ferrous waste acid derives from certain
High salt concentration acid waste liquid after steel plate factory pickling process, its typical water quality index is shown in Table 1：
The waste hydrochloric acid containing iron of table 1 typical case's water quality index
Embodiment 1
The amount of taking fully P204 is the complexing extractant of 30% volumetric concentration, controls the waste hydrochloric acid containing iron after coarse filtration and complexation extraction
The volume ratio and feed flow rate ratio for taking agent is 1：0.5, cross extraction in multi-stage continuous extraction system, after discharge simultaneously,
The residual concentration of zinc element in the mutually low zinc-iron-containing spent acid raffinate of water is determined, and detects the loss of iron content and acidity；Take fully
Amount back washing agent water, controls it and is 1.5 with the volume ratio and feed flow rate ratio of load organic phases：1, in multistage continuous back extraction system
Cross back extraction in system, after discharge simultaneously, determines the concentration of zinc element, iron content and acidity in the acid waste water after back extraction；To
4% lime cream is added in acid waste water after back extraction, pH8.0 is adjusted, is stirred to precipitation and filtered after all separating out, determined low containing zinc
The concentration of zinc element, iron content and acidity in neutral waste water；The low neutrality waste water containing zinc is pumped into into electrodialysis plant to be disposed, is obtained
To a kind of high performance agent for removing fluorin and the regeneration water of reuse to back extraction operation, effective ingredient CaCl in high performance agent for removing fluorin is determined2Contain
Amount.
Embodiment 2
The amount of taking fully P204 is the complexing extractant of 40% volumetric concentration, controls the waste hydrochloric acid containing iron after coarse filtration and complexation extraction
The volume ratio and feed flow rate ratio for taking agent is 1：0.75, cross extraction in multi-stage continuous extraction system, after discharge simultaneously,
The residual concentration of zinc element in the mutually low zinc-iron-containing spent acid raffinate of water is determined, and detects the loss of iron content and acidity；Take fully
Amount back washing agent water, controls it and is 1.75 with the volume ratio and feed flow rate ratio of load organic phases：1, in multistage continuous back extraction
Cross back extraction in system, after discharge simultaneously, determines the concentration of zinc element, iron content and acidity in the acid waste water after back extraction；
4% lime cream is added in the acid waste water after back extraction, pH8.0 is adjusted, is stirred to precipitation and filtered after all separating out, determine clear liquid
The concentration of zinc element, iron content and acidity in the low neutrality waste water containing zinc；The low neutrality waste water containing zinc is pumped into into electrodialysis plant is carried out
Dispose, obtain the regeneration water of a kind of high performance agent for removing fluorin and reuse to back extraction operation, determine effective ingredient in high performance agent for removing fluorin
CaCl2Content.
Embodiment 3
The amount of taking fully P204 is the complexing extractant of 50% volumetric concentration, controls the waste hydrochloric acid containing iron after coarse filtration and complexation extraction
The volume ratio and feed flow rate ratio for taking agent is 1：1, cross extraction in multi-stage continuous extraction system, after discharge simultaneously, surveys
Determine the residual concentration of zinc element in the mutually low zinc-iron-containing spent acid raffinate of water, and detect the loss of iron content and acidity；The amount of taking fully
Back washing agent water, controls it and is 2 with the volume ratio and feed flow rate ratio of load organic phases：1, in multistage continuous back extraction system
Cross back extraction, after discharge simultaneously, determines the concentration of zinc element, iron content and acidity in the acid waste water after back extraction；To back extraction
5% lime cream is added in acid waste water afterwards, pH8.5 is adjusted, is stirred to precipitation and filtered after all separating out, determine clear liquid low containing zinc
The concentration of zinc element, iron content and acidity in neutral waste water；The low neutrality waste water containing zinc is pumped into into electrodialysis plant to be disposed, is obtained
To a kind of high performance agent for removing fluorin and the regeneration water of reuse to back extraction operation, effective ingredient CaCl in high performance agent for removing fluorin is determined2Contain
Amount.
The embodiment correlation water index of table 2
From table 2 it can be seen that the inventive method be applicable to high zinc-iron-containing spent acid except zinc purified treatment, and iron content is useless
It is sour Jing after whole multi-stage continuous extraction PROCESS FOR TREATMENT substantially without iron content and acidity lost, the clearance of zinc element is up to 99.5%
More than, extractant and back washing agent are capable of achieving 100% regeneration.
With the above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete
Entirely various change and modification can be carried out in the range of without departing from this invention technological thought.The technology of this invention
Property scope is not limited to the content in description, it is necessary to its technical scope is determined according to right.
Claims (10)
1. a kind of decrement circulation technology method for reclaiming the zinc element in ferrous waste acid, is characterized in that：Comprise the following steps：
(1) pretreatment：Ferrous waste acid coarse filtration is removed into big particle suspended contamination, extraction equipment is pumped into；
(2) extract ferrum zinc to separate：Constantly injection complexing extractant carries out multi-stage continuous extraction in extraction equipment, and zinc element is extracted
In getting organic faciess, two-phase laminated flow obtains load organic phases zinc-iron-containing spent acid raffinate mutually low with water；
(3) extractant regeneration：Back washing agent is added to carry out back extraction regeneration, back extraction back loading in the load organic phases in step (2)
Zinc element in organic faciess is with Zn (OH)4 2-Form be transferred in back washing agent, two-phase laminated flow, obtain the organic faciess after back extraction and
Acid waste water after back extraction；
(4) regulation of back washing agent：Lime cream is added in the acid waste water after the back extraction in step (3), pH=8～8.5 are adjusted,
Filter after zinc hydroxide precipitation is separated out, cadmia and low containing the neutral waste water of zinc after filter；
(5) regeneration of back washing agent：The low neutrality waste water containing zinc in step (4) is pumped into into electrodialysis plant to be disposed, is obtained efficiently
Defluorinating agent and the regeneration water of reuse to back extraction operation.
2. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：Ferrous waste acid is pickling iron and steel industry waste hydrochloric acid containing iron or iron content Waste Sulfuric Acid in described step (1), and weight of iron content is pressed
Fe2O310～18% are calculated as, zinc mass content is calculated as 1000～40000mg/L by Zn.
3. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：Complexing extractant is made up of chelating agent di-(2-ethylhexyl)phosphoric acid ester and diluent sulfonated kerosene in described step (2),
The volumetric concentration of di-(2-ethylhexyl)phosphoric acid ester is 30～50%.
4. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：Complexing extractant is 0.5～1 with the volume ratio and feed flow rate ratio of ferrous waste acid in described step (2)：1.
5. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：The mutually low zinc-iron-containing spent acid raffinate of water obtained in described step (2) make semi-finished product subsequently comprehensively utilized or
Direct marketing.
6. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：Back washing agent is water in described step (3), and it is 1.5～2 with the volume ratio and feed flow rate ratio of load organic phases：1.
7. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：Organic faciess in described step (3) after back extraction are the extractant after regeneration, are back to extraction cells recycling.
8. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：Acid waste water pH=2～3 in described step (4) after back extraction, the dosage of lime cream is the spent acidic water quality after back extraction
The 4～5% of amount.
9. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：Cadmia is recycled as zinc mud after filter in described step (4).
10. it is according to claim 1 it is a kind of reclaim ferrous waste acid in zinc element decrement circulation technology method, its feature
It is：High performance agent for removing fluorin contains the calcium chloride of mass content 25～30% in described step (5), at the purification of photovoltaic wastewater
Reason.
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Cited By (6)
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|---|---|---|---|---|
| CN107245582A (en) * | 2017-05-26 | 2017-10-13 | 金川集团股份有限公司 | It is a kind of that iron, the method for zinc are reclaimed from waste hydrochloric acid |
| CN108193052A (en) * | 2017-12-28 | 2018-06-22 | 江苏永葆环保科技有限公司 | Resource utilization prepares the method without ammonium fluxing agent using low acid waste water containing zinc |
| CN112575187A (en) * | 2020-11-24 | 2021-03-30 | 昆明理工大学 | Extraction system and extraction separation method for selective dezincification of waste pickle liquor |
| CN113479939A (en) * | 2021-06-09 | 2021-10-08 | 南京护航环保科技有限公司 | Separating treatment agent for ferrous chloride and zinc chloride in hot galvanizing waste hydrochloric acid liquid and application thereof |
| CN114807603A (en) * | 2022-05-26 | 2022-07-29 | 重庆康普化学工业股份有限公司 | Method for extracting zinc from high-hydrochloric-acid washing liquor |
| CN115231647A (en) * | 2022-07-27 | 2022-10-25 | 赣州步莱铽新资源有限公司 | Recovery method of back extraction waste acid |
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| CN107245582A (en) * | 2017-05-26 | 2017-10-13 | 金川集团股份有限公司 | It is a kind of that iron, the method for zinc are reclaimed from waste hydrochloric acid |
| CN107245582B (en) * | 2017-05-26 | 2019-01-22 | 金川集团股份有限公司 | A method of recycling iron, zinc from waste hydrochloric acid |
| CN108193052A (en) * | 2017-12-28 | 2018-06-22 | 江苏永葆环保科技有限公司 | Resource utilization prepares the method without ammonium fluxing agent using low acid waste water containing zinc |
| CN112575187A (en) * | 2020-11-24 | 2021-03-30 | 昆明理工大学 | Extraction system and extraction separation method for selective dezincification of waste pickle liquor |
| CN113479939A (en) * | 2021-06-09 | 2021-10-08 | 南京护航环保科技有限公司 | Separating treatment agent for ferrous chloride and zinc chloride in hot galvanizing waste hydrochloric acid liquid and application thereof |
| CN114807603A (en) * | 2022-05-26 | 2022-07-29 | 重庆康普化学工业股份有限公司 | Method for extracting zinc from high-hydrochloric-acid washing liquor |
| CN114807603B (en) * | 2022-05-26 | 2023-08-22 | 重庆康普化学工业股份有限公司 | Method for extracting zinc from high hydrochloric acid washing liquid |
| CN115231647A (en) * | 2022-07-27 | 2022-10-25 | 赣州步莱铽新资源有限公司 | Recovery method of back extraction waste acid |
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Application publication date: 20170510 |