CN107162276A - A kind of method for removing chromium of ferric trichloride etching waste liquor - Google Patents
A kind of method for removing chromium of ferric trichloride etching waste liquor Download PDFInfo
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- CN107162276A CN107162276A CN201710554984.1A CN201710554984A CN107162276A CN 107162276 A CN107162276 A CN 107162276A CN 201710554984 A CN201710554984 A CN 201710554984A CN 107162276 A CN107162276 A CN 107162276A
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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
- 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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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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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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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Hydrology & Water Resources (AREA)
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Abstract
The present invention discloses a kind of method for removing chromium of ferric trichloride etching waste liquor, ferric ion and hydrogen ion in ferric trichloride etching waste liquor is reduced by iron plate, reduce ferric ion and hydrogen ion in solution, avoid that alkaline precipitating agent subsequently is lost, it is simple to operate, it is with low cost, and other metal impurities are not introduced, chromium ion in solution is separated out by alkaline precipitating agent, the chrome content of chromium slag is improved；By the ferrous ion in chlorine oxidation filtrate, liquor ferri trichloridi finished product is obtained；Chromium slag and iron and steel pickling waste liquid are dissolved again, alkaline precipitating agent is added again, while separating out the chromium in iron and steel pickling waste liquid in the lump, the content of chromium is improved, the two comprehensive utilization is turned waste into wealth, increased economic efficiency.
Description
Technical field
The present invention relates to etching waste liquor processing technology field, in particular it relates to which a kind of ferric trichloride etching waste liquor removes chromium
Method.
Background technology
In the finishing process such as stainless steel stamp, engraving, liquor ferri trichloridi has obtained extensively should as etchant
With.Liquor ferri trichloridi with stainless steel etching process, by it is lasting generation dark brown ferric trichloride etching waste liquor, its is main
Composition is ferric ion, and mass fraction is about 8%, and ferrous ion mass fraction is about 4%, and hydrogen chloride mass fraction is about
3%, chromium content is more than 5000mg/L.The conventional treatment method of this etching waste liquor, which is generally, directly neutralizes discharge, is adjusted using lime
PH value of solution is saved, will be filtered to remove, wherein consuming substantial amounts of alkali, also produced after heavy metal ion formation hydroxide precipitation in solution
The sludge of many metals containing siderochrome, not only causes environmental hazard, and greatly waste, and processing cost expense is caused to resource
It is high.If prepared by etching waste liquor recovery into molysite water treatment agent, because chromium content is higher in solution, it have impact on molysite water treatment agent and exist
Application in terms of sludge dewatering, and excessive chromium metal discharge can have certain harm to the mankind and environment, and it must be carried out
Effectively processing.
Mainly have on chromate waste water minimizing technology at present：Physical, chemical method, bioanalysis.Physical is mainly：(1)
Membrane separation process.At present, the more ripe technique industrially applied has electrodialysis, counter-infiltration, ultrafiltration, liquid film.Membrane separation process has
Selective good, device is simple, operation is easy, low power consumption and other advantages, has the disadvantage that investment and operation and maintenance cost are high, and film
Quality need to be improved.(2) absorption method, is to be adsorbed one or several kinds of components in water sample using porous solid absorbent
Prediction group decomposition is inhaled in surface, then with methods such as suitable solvent, heating or air blowings, the purpose for reaching separation and enrichment (is such as lived
Property charcoal etc.).
Chemical method：(1) the electronation precipitation method, add reducing agent, by Cr to waste water in acid condition6+It is reduced to Cr3 +, alkali (lime or sodium hydroxide) is then added, it is generated chromium hydroxide precipitation in the basic conditions, is gone by precipitation and separation
Except chromium ion.Reducing agent has：FeSO4、NaSO3、NaH2SO3, Fe etc..Reduction precipitation method has one-time investment small, operating cost
The easy advantage of low, high treating effect, operational administrative, relatively broad application.(2) electrolytic reduction is iron anode in direct current
Under effect, constantly dissolving produces ferrous ion, in acid condition, by Cr6+It is reduced to Cr3+.Due to the hydrogen ion in waste water not
Break and reduce, therefore pH value will constantly rise, and form chromium hydroxide (III) precipitation, so as to suppress pH value rising, make the chromium in waste water
Separate.Electrolytic Theatment of Chrome Containing Wastewater effect stability, operational administrative is easy, but consumption electricity, steel plate, running expense compared with
It is high；This method is in application process, and iron filings channel, caking and passivation phenomenon, reduction treatment effect easily occur, it is necessary to periodically punching
Wash, operating cost is significantly greatly increased, technique adjustment pH is relatively complicated, the actual control of inconvenience, the technique uses not quite varied.
(3) photocatalytic method, is catalyst using conductor oxidate (ZnO/TiO2), waste electroplating liquor containing chromium is subject to using solar source
Processing, through 90min solar irradiations (1182.5W/m2), makes hexavalent chrome reduction trivalent chromium, then remove trivalent in chromium hydroxide form
Chromium.Bioanalysis：By the function bacterium manually cultivated, acted on, be complexed by the catalyzed conversion of electrostatic adsorption, enzyme, flocculated, altogether
Precipitation and the cushioning effect to pH value, utilize microbiological treatment inorganic heavy metal waste water.With microorganism remove chromium efficiency high,
The characteristics of non-secondary pollution, still, culture microorganism, usually require that operating condition (temperature, the pH value, the control of dissolved oxygen of harshness
And prevent living contaminants etc.), with high content of technology, operation requires strict.
In addition, it is necessary to be cleaned with hydrochloric acid solution to steel and iron parts surface, to remove its surface in steel processing industry
Iron rust.In acid cleaning process, the hydrochloric acid in hydrochloric acid solution is constantly consumed, while ferrous ion is continuously increased, until the salt
Acid is exhausted, and the waste liquid now produced is exactly iron and steel pickling waste liquid.The main component of the iron and steel pickling waste liquid is water, protochloride
Iron, free acid and a small amount of impurity.Because it is big containing sour salt content, it is impossible to directly discharge, if to neutralize discharge, need a large amount of
Alkali, and produce high-concentration salt-containing wastewater and a large amount of saliferous sludge；If reclaiming hydrochloric acid therein, high energy consumption, investment is big, corrosion
It is serious and operating environment is poor.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of method for removing chromium of iron chloride etching waste liquor.
A kind of method for removing chromium of iron chloride etching waste liquor disclosed by the invention, it comprises the following steps：
(1) iron plate, reduction ferric ion and hydrogen ion are added into ferric trichloride etching waste liquor, formation contains protochloride
The solution of iron；
(2) alkaline precipitating agent is added into above-mentioned solution and is stirred, hydroxide sediment is produced, separation of solid and liquid is obtained
Filter residue containing chromium and and the clear liquid containing frerrous chloride；
(3) chlorine is added into clear liquid, ferric trichloride finished product is obtained；
(4) filter residue and iron and steel pickling waste liquid are pressed 2:1 ratio in reactor in being mixed and stirred for, the steel acid
The hydrogen chloride mass fraction for washing waste liquid is 13%~30%, reacts 1~3H, dissolved hydrogen oxide precipitation thing, until in solution
Hydrogen chloride mass fraction is down to 2%, adds the excessive iron plate, reduces the ferric ion and hydrogen ion of residual；
(5) solution into step (4) adds alkaline precipitating agent, by the chromium ion Precipitation in solution.
According to an embodiment of the present invention, the reaction temperature in above-mentioned steps (1) is 40~80 DEG C, and the reaction time is 1
~3H, the content of ferrous ion is 10%~16%.
According to an embodiment of the present invention, the mixing speed of above-mentioned steps (2) is 50~100r/min, adds alkalescence heavy
The speed of shallow lake agent is 1.5~3.0kg/min, and the pH value of solution is adjusted to 3.0~4.0, and the reaction time is 90min.
According to an embodiment of the present invention, above-mentioned steps (2) also include extracting clear liquid, then press filtration filter residue, by press filtration
Residual night afterwards merges with clear liquid.
According to an embodiment of the present invention, above-mentioned alkaline precipitating agent is calcium oxide, calcium hydroxide, sodium hydroxide or carbonic acid
Sodium.
Compared with prior art, the present invention can be obtained including following technique effect：
The present invention reduces the ferric ion and hydrogen ion in ferric trichloride etching waste liquor by iron plate first, reduces solution
Middle ferric ion and hydrogen ion, it is to avoid alkaline precipitating agent is subsequently lost, it is simple to operate, it is with low cost, and other gold are not introduced
Belong to impurity, the chromium ion in solution is separated out by alkaline precipitating agent, improve the chrome content of chromium slag；By in chlorine oxidation filtrate
Ferrous ion, obtains liquor ferri trichloridi finished product；Chromium slag and iron and steel pickling waste liquid are dissolved again, alkaline precipitating agent is added again,
Separate out the chromium in iron and steel pickling waste liquid in the lump simultaneously, improve the content of chromium, the two comprehensive utilization is turned waste into wealth, and improves economic effect
Benefit.
Embodiment
Multiple embodiments of the application will be disclosed below, as clearly stated, details in many practices will with
Illustrate in the lump in lower narration.It should be appreciated, however, that the details in these practices is not applied to limit the application.That is,
In some embodiments of the application, the details in these practices is non-essential.
Technical scheme between each embodiment can be combined with each other, but must be with those of ordinary skill in the art's energy
Based on enough realizations, when the combination appearance of technical scheme is conflicting or can not realize it will be understood that the knot of this technical scheme
Conjunction is not present, also not within the protection domain of application claims.
The ferric ion and hydrogen ion of ferric trichloride etching waste liquor are reduced first.Ferric trichloride etching waste liquor is collected in ground
Chi Zhong, be put into excessive iron plate soaked in ground pond reaction 2H, reaction temperature be 50 DEG C, by reduction reaction by ferric ion also
Originally it was ferrous ion, reducing hydrogen ions are hydrogen, and obtained solution of ferrous chloride, the content of ferrous ion is 13%~16%.Again
Add alkaline precipitating agent into ground pond, charging rate is 1.5~3.0kg/min, and mixing speed is 50r/min, by one side plus
Material is while stirring, control charging rate and mixing speed, so as to be sufficiently mixed alkaline precipitating agent and solution of ferrous chloride, prevent office
Alkali is crossed in portion, and partial over-alkali can cause ferrous ion Precipitation, improve iron loss rate.Preferably, alkaline precipitating agent is hydroxide
Calcium, can also be replaced with calcium oxide, sodium hydroxide or calcium carbonate, be reacted by the chromium ion in alkaline precipitating agent and solution, generation
Chromium hydroxide precipitation thing, also produces a small amount of hydroxide iron precipitate in addition；After testing, ferro element now in solution and chromium member
The content of element is compared with the original amount in solution, and the loss late of iron ion is 3.8%, and the clearance of chromium ion is 96.56%,
Chromium content in solution is down to 100ppm.
, it is necessary to carry out separation of solid and liquid after generation solid sediment.Neutralized through above-mentioned alkaline precipitating agent, now in solution
Acidity is low.Because the particle diameter that hydroxide precipitates particulate matter is small, therefore 4H is first settled, treats that solid sediment falls to ground bottom of pond portion,
Form supernatant, it is preferable that extract supernatant into holding vessel, then the liquid pressure for being remained solid sediment by filter press
Go out, retain filter residue, supernatant is mixed with the liquid being press-filtered out, for preparing ferric trichloride water treatment agent.To supernatant and press filtration
Chlorine is added in the liquid gone out, ferrous ions are ferric ion by chlorine, because part metals impurity is in previous step
Precipitated through alkaline precipitating agent, the impurity metal ion contained in solution now is few, the purity of the liquor ferri trichloridi of generation is high.
Filter residue and the iron and steel pickling waste liquid mixing retained after above-mentioned separation of solid and liquid, the quality of the hydrogen chloride of iron and steel pickling waste liquid
Fraction is about 14.5%, and the mass ratio of filter residue and iron and steel pickling waste liquid presses 2:1 mixes in reactor, and this solid-liquid mass ratio can
Hydroxide precipitation is completely dissolved, also ensures that the hydrogen cloride concentration of solution residual is low, is easy to subsequently use.At the same time, stir
Mixing is mixed, now the temperature of mixture is risen to after 40~80 DEG C, 1~3H of reaction, hydroxide sediment and chlorine in filter residue
Change hydracid alkali and occur neutralization reaction, hydroxide sediment fully dissolves ferrous ion, trivalent chromic ion and a small amount of ferric iron
Ion.After completion of the reaction, the mass fraction of hydrogen chloride is 2%.Excessive iron plate is now added, by remained in solution a small amount of three
Valency iron ion and hydrogen ion are fully reduced, and ferrous ion and chromium ion are now contained in solution.Alkaline precipitating agent is added again, will
Chromium ion Precipitation, so as to obtain the chromium slag of high-purity.
In summary, the ferric ion and hydrogen ion in ferric trichloride etching waste liquor are reduced by iron plate first, reduced
Ferric ion and hydrogen ion in solution, it is to avoid alkaline precipitating agent is subsequently lost, it is simple to operate, it is with low cost, and it is not introduced
Its metal impurities, the chromium ion in solution is separated out by alkaline precipitating agent, improves the chrome content of chromium slag；Pass through chlorine oxidation filtrate
In ferrous ion, obtain liquor ferri trichloridi finished product；Chromium slag and iron and steel pickling waste liquid are dissolved again, alkaline sedimentation is added again
Agent, while separating out the chromium in iron and steel pickling waste liquid in the lump, improves the content of chromium, and the two comprehensive utilization is turned waste into wealth, and improves economical
Benefit.
The upper only embodiments of the present invention, are not intended to limit the invention.For those skilled in the art
For, the present invention can have various modifications and variations.It is all any modifications made in spirit and principles of the present invention, equivalent
Replace, improve etc., it all should be included within scope of the presently claimed invention.
Claims (5)
1. a kind of method for removing chromium of ferric trichloride etching waste liquor, it is characterised in that comprise the following steps：
(1) iron plate, reduction ferric ion and hydrogen ion are added into ferric trichloride etching waste liquor, formation contains frerrous chloride
Solution；
(2) alkaline precipitating agent is added into above-mentioned solution and is stirred, hydroxide sediment is produced, separation of solid and liquid obtains and contains chromium
Filter residue and and the clear liquid containing frerrous chloride；
(3) chlorine is added into the clear liquid, ferric trichloride finished product is obtained；
(4) filter residue and iron and steel pickling waste liquid are pressed 2:1 ratio in reactor in being mixed and stirred for, and the pickling iron and steel gives up
The hydrogen chloride mass fraction of liquid is 13%~30%, reacts 1~3H, dissolved hydrogen oxide precipitation thing, until the chlorination in solution
Hydrogen mass fraction is down to 2%, adds the excessive iron plate, reduces the ferric ion and hydrogen ion of residual；
(5) solution into step (4) adds alkaline precipitating agent, by the chromium ion Precipitation in solution.
2. method for removing chromium according to claim 1, it is characterised in that the reaction temperature in step (1) is 40~80 DEG C, instead
It is 1~3H between seasonable, the content of ferrous ion is 10%~16%.
3. method for removing chromium according to claim 2, it is characterised in that the mixing speed of step (2) is 50~100r/min,
The speed for adding the alkaline precipitating agent is 1.5~3.0kg/min, and the pH value of solution is adjusted to 3.0~4.0, during reaction
Between be 90min.
4. method for removing chromium according to claim 3, it is characterised in that step (2) also includes extracting the clear liquid, then presses
The filter residue is filtered, the residual night after press filtration is merged with the clear liquid.
5. according to any described method for removing chromium of Claims 1-4, it is characterised in that the alkaline precipitating agent is calcium oxide, hydrogen
Calcium oxide, sodium hydroxide or sodium carbonate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710554984.1A CN107162276B (en) | 2017-07-10 | 2017-07-10 | Chromium removal method for ferric trichloride etching waste liquid |
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| CN201710554984.1A CN107162276B (en) | 2017-07-10 | 2017-07-10 | Chromium removal method for ferric trichloride etching waste liquid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970441A (en) * | 2018-12-24 | 2019-07-05 | 海安南京大学高新技术研究院 | The method that stainless steel etching sludge prepares strontium ferrite |
| CN110327911A (en) * | 2019-07-19 | 2019-10-15 | 常熟理工学院 | A kind of preparation method of 1,2- dichloro benzene exhaust air removal catalyst |
| CN112250053A (en) * | 2020-09-28 | 2021-01-22 | 合肥国轩高科动力能源有限公司 | Method for preparing battery-grade iron phosphate by using ferric trichloride etching waste liquid |
| CN114195190A (en) * | 2021-12-30 | 2022-03-18 | 斯瑞尔环境科技股份有限公司 | Preparation method of chromium hydroxide easily soluble in acid |
| CN114959711A (en) * | 2022-04-29 | 2022-08-30 | 东北大学 | Comprehensive utilization method of stainless steel etching waste liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970441A (en) * | 2018-12-24 | 2019-07-05 | 海安南京大学高新技术研究院 | The method that stainless steel etching sludge prepares strontium ferrite |
| CN110327911A (en) * | 2019-07-19 | 2019-10-15 | 常熟理工学院 | A kind of preparation method of 1,2- dichloro benzene exhaust air removal catalyst |
| CN112250053A (en) * | 2020-09-28 | 2021-01-22 | 合肥国轩高科动力能源有限公司 | Method for preparing battery-grade iron phosphate by using ferric trichloride etching waste liquid |
| CN114195190A (en) * | 2021-12-30 | 2022-03-18 | 斯瑞尔环境科技股份有限公司 | Preparation method of chromium hydroxide easily soluble in acid |
| CN114195190B (en) * | 2021-12-30 | 2023-09-15 | 斯瑞尔环境科技股份有限公司 | Preparation method of easily acid-soluble chromium hydroxide |
| CN114959711A (en) * | 2022-04-29 | 2022-08-30 | 东北大学 | Comprehensive utilization method of stainless steel etching waste liquid |
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