CN110330155A - A kind of method of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery chromium - Google Patents
A kind of method of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery chromium Download PDFInfo
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- CN110330155A CN110330155A CN201910742171.4A CN201910742171A CN110330155A CN 110330155 A CN110330155 A CN 110330155A CN 201910742171 A CN201910742171 A CN 201910742171A CN 110330155 A CN110330155 A CN 110330155A
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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
- C02F1/26—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
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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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
- 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
Abstract
The invention belongs to field of industrial waste water treatment, and in particular to a kind of method of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery chromium, comprising the following steps: (1) the preprocessed concentration that is placed on of stereotype is 1.5molL‑1In the 100mL H-type electrolytic cell of sulfuric acid solution, using 6V as constant voltage, the electrolysis of 3h is carried out, anode electrode plate can be prepared；(2) after electrolytic cell is connected and fixed by anionic membrane, anode electrode plate and cathode stereotype are respectively placed in the electrolytic cell for filling sulfuric acid pickling waste liquid to be electrolysed, and cathode is put into a small amount of KSCN solution, after connecting power supply, it is electrolysed with fixed current density, until cathode pool red disappears；(3) excessive KSCN solution is added to cathode pool to be complexed, be electrolysed, 30min is complexed after stop；(4) cathode solution is taken out, addition is extracted by the extract liquor of extractant of tri-n-octyl amine, detects Cr (III), Fe concentration in extract liquor, and spreading calculates Cr (III), Fe recovery of extraction.The present invention have the characteristics that resource reclaim, it is without secondary pollution, save reagent, efficiently it is convenient.
Description
Technical field
The invention belongs to field of industrial waste water treatment, and in particular to a kind of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery
The method of chromium.
Background technique
China is the maximum country of iron and steel output, and crude steel yield in 2018 is 9.28 hundred million tons, accounts for world's crude steel total output
51.3%.Steel before processing, will be usually immersed in the acid of certain temperature, or spray certain density acid on its surface,
Purpose is the oxide layer in order to remove steel surface, which is known as acid cleaning process.Acid cleaning process can remove on steel surface
Oxide and rust, be clean metal surface a kind of method, the property of steel surface can be improved.With acid cleaning process
Continuous progress, pickling efficiency with the rising of iron concentration and hydrogen ion concentration in clear liquid decline, for guarantee pickling effect
Rate needs to change new pickling clear liquid, and the acid solution being discharged outside is known as pickle liquor.According to incompletely statistics, the annual discharge in the whole nation is super
Cross 2Mt.According to the difference of acid used, pickle liquor can be divided into hydrochloric acid pickling waste liquor, sulfuric acid pickling waste liquid, nitric acid acidwashing waste liquid
With mixing pickle liquor etc..Since pickle liquor has acidity strong, volume is big, and molysite class content is high, heavy metal ion content
The features such as high, if not dealing carefully with, direct emission can then be caused great harm environment.
The one kind of sulfuric acid pickling waste liquid as pickle liquor equally has harmfulness.It is the characteristics of because of its highly acid, easily rotten
Lose sewer pipe；Molysite class and heavy metal ion content are high, pollute natural environment, endanger animals and plants, or even jeopardize human health,
Sulfuric acid pickling waste liquid has been put into the catalogue of danger wastes, belongs to danger wastes, therefore, it is necessary to sulfuric acid pickling waste liquid
It pays close attention and processing appropriate in time.
Currently, the processing method of sulfuric acid pickling waste liquid is mainly harmless treatment and recycling treatment.Traditional neutralisation
Mainly to be closed in lime stone, in sodium hydroxide pellets and based on waiting.The advantages of this method is that simple process is convenient, treatment effeciency
It is high.The disadvantage is that largely consuming base reagent, generating precipitating sludge, it is difficult to will have the sulfuric acid of utility value in sulfuric acid pickling waste liquid
It is utilized with the sulfate resource utilization of metal class.In contrast, the recycling treatment of sulfuric acid pickling waste liquid is more conducive to resource height
The green sustainable development of effect comprehensive utilization and environment, recycling object is mainly sulfuric acid and metallic element.The recycling side of sulfuric acid
Method is mainly membrane separation process and extracting-back extraction method etc..In addition, many scholars are using neutralisation, sulphate of iron method, organic solution extraction
It follows the example of, the metals such as Fe, Cr, Zn and Ca in the recycling sulfuric acid pickling waste liquid such as dialysis, ion-exchange, and majority is with molysite
Based on recycling.Leaching agent of such as Wang using stainless steel acid-washing waste liquid as useless circuit board, not only to metal member in useless circuit board
Element is recycled, and the rate of recovery of iron is more than 50%.Special Steel Co. of Shougang Group uses concentration-filtering-spontaneous nucleation method technique
Acid wash waste liquid of rolled steel is handled, after centrifuge dripping, raffinate is 0.5% containing acid concentration, and ferrous sulfate is 150~170gL-1。
Although many scholars of state have achieved some achievements to the research of stainless steel acid-washing waste liquid, since Fe, Cr are in member
Position is close in plain periodic table, and chemical property is similar, causes the rate of recovery of molysite unsatisfactory.Therefore, in order to reduce in sulfuric acid
The influence that Fe is recycled in the presence of Cr in pickle liquor, the invention discloses combine recycling sulfuric acid washing useless using electrolysis-extraction
The method of Cr in liquid, is compared with the traditional method, although electrolysis method energy consumption is larger, electric energy replaces chemical energy, greatly reduces
The waste of secondary pollution and water resource.In addition, extraction has the characteristics that the extraction equilibrium time is short, easy to operate.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery chromium
Method develops a kind of method for metal recovery Cr in sulfuric acid pickling waste liquid, solves the low Problems Existing of the Fe salt rate of recovery, should
Method has the characteristics that economize on resources, beneficial to environmental protection, efficiently convenient.
Specific technical solution is as follows:
A kind of method of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery chromium, follows the steps below:
(1) specification 2mm × 30mm × 50mm stereotype is cut, sanding and polishing processing is carried out to stereotype surface using sand paper；
(2) it is washed using deionized water and acetone, its surface blot is cleaned using alkaline mixed solution；
(3) with 5% HNO3Cleaning after boiling 10min in 15% oxalic acid solution, is thoroughly cleaned with deionized water,
Complete the pretreatment of electrode plate；
(4) at room temperature, pretreated stereotype is placed in concentration is 1.5molL-1The 100mL H-type of sulfuric acid solution is electrolysed
Chi Zhong carries out the electrolysis of 3h using 6V as constant voltage, can prepare anode electrode plate；
(5) clamping fixed by flat mouth after connecting 100mL H-type electrolytic cell by the anionic membrane that diameter is about 2cm；
(6) 50ml sulfuric acid pickling waste liquid to be electrolysed is respectively placed in the anode slot and cathode can of electrolytic cell, by cathode
The pH value of solution is adjusted to 0.2,0.5,0.8,1.1,1.4 in slot, and it is 2gL that 1mL concentration, which is added,-1KSCN solution as referring to
Show agent；
(7) anode electrode plate prepared is placed in anode pool, takes out after fixed, is soaked according to anode electrode plate by solution
Wet area and preset current density calculate the current value by electrode plate, pretreated stereotype are placed in cathode
As cathode electrode plate；
(8) electrode fingers are separately connected yin, yang pole plate, are electrolysed under the current density of (7), and electrolysis to cathode is nothing
Color, it is 30.2gL that concentration, which is added, to cathode-1KSCN solution be complexed with trivalent chromium, after 30min stop electrolysis, complexing,
It takes a small amount of catholyte to detect the concentration of its Fe (II) by ultra-violet and visible spectrophotometer, calculates the mass ratio of Fe (II)；
(9) cathode solution after taking (8) to be electrolysed is placed in conical flask, and certain density tri-n-octyl amine liquid is first added thereto
Afterwards, it is placed in water bath chader and carries out extraction experiments；
(10) stratification after shaking takes raffinate respectively by atomic absorption photometer detection Cr (III), Fe
Concentration calculates separately its recovery of extraction.
Alkaline mixed solution in the step (2) is the Na for being 10% with mass fraction2CO3, 10% NaPO4With
What 15% NaOH was formulated.
Sulfuric acid pickling waste liquid major metal component is Cr (III) 2gL in the step (6)-1, Quan Tie 2gL-1。
Current density range in the step (7) is 100Am-2。
The mass ratio of Fe (II) in the step (8) is calculated according to the following formula:
In formula: α is mass ratio, %；The concentration gL that c is Fe (II) in solution after being electrolysed-1；c0For in sulfuric acid pickling waste liquid
The concentration of Fe, gL-1。
The revolving speed of water bath chader in the step (8) is 250rpm, time 10min.
The concentration of tri-n-octyl amine in the step (9) is 1-8 times of Cr (III)；Three in the step (9) are just pungent
The diluent of amine is n-amyl alcohol.
The recovery of extraction of Cr (III), Fe in the step (10) are calculated according to the following formula:
In formula, E (%) is recovery of extraction c0、cεThe respectively preceding quality with Cr (III), Fe in water phase after extraction of electrolysis
Concentration, gL-1。
Compared with prior art, the present invention has following advantageous effects:
(1) found by the concentration that atomic absorption photometer detects Cr (III) in raffinate: the concentration of Cr (III) is less than
Concentration before electrolysis shows to use electrolysis method reduction Fe (III), can recycle Cr in sulfuric acid pickling waste liquid by extractant of TOA
(III)。
(2) electrolysis of the invention is with the principle for being combined recycling Cr (III) is extracted: the chloride plate electrode surface shape of preparation
At PbO2, so that Fe (III) is reduced to Fe (II) in cathode acid solution, reaction to be restored terminates, and is added into cathode solution
Excessive KSCN solution is that it is sufficiently complexed with Cr (III), is formed Cr (SCN)6 3-, make Cr (III) with the presence of negative valency state；It utilizes
Cathode systems acidity feature, uses TOA for extractant, makes itself and H+Complexing, shows positive valence state, due to electrostatic interaction, with Cr
(SCN)6 3Complexometric extraction is carried out, thus achieve the purpose that separation and recovery, extraction mechanism are as follows:
Cr3++6SCN-→Cr(SCN)6 3-
R3N+H+→R3NH+
Cr(SCN)6 3-+3R3NH+→(R3NH+)3Cr(SCN)6。
(3) present invention, which has, keeps stoste system, without secondary pollution, rate of extraction to extract back fastly, under peracid harsh conditions
It receives Cr (III).
(4) operating method of the invention is simple, does not need to add each precipitation reagent, greatly reduces the consumption of reagent, real
Existing save the cost.
(5) electrolysis of the invention and extraction good reproducibility and stability, can with the Cr (III) in sulfuric acid pickling waste liquid
Recycling.
Detailed description of the invention
Influence of the Fig. 1 for the electrolysis time in the embodiment of the present invention 1 to the mass ratio of Fe (II)；
Fig. 2 is the influence of the concentration on extraction rate of tri-n-octyl amine in the embodiment of the present invention 2.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing, but protection scope of the present invention is not limited by embodiment.
It is the anionic membrane that diameter is about 2cm used in embodiment, sulfuric acid pickling waste liquid contains 2gL-1Cr (III) and
2 gL-1Quan Tie.
Embodiment 1
A kind of method of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery chromium, which is characterized in that according to the following steps into
Row:
(1) specification 2mm × 30mm × 50mm stereotype is cut, sanding and polishing processing is carried out to stereotype surface using sand paper；
(2) it is washed using deionized water and acetone, its surface blot is cleaned using alkaline mixed solution；
(3) with 5% HNO3Cleaning after boiling 10min in 15% oxalic acid solution, is thoroughly cleaned with deionized water,
Complete the pretreatment of electrode plate；
(4) at room temperature, pretreated stereotype is placed in concentration is 1.5molL-1The 100mL H-type of sulfuric acid solution is electrolysed
Chi Zhong carries out the electrolysis of 3h using 6V as constant voltage, can prepare anode electrode plate；
(5) clamping fixed by flat mouth after connecting 100mL H-type electrolytic cell by the anionic membrane that diameter is about 2cm；
(6) 50ml sulfuric acid pickling waste liquid to be electrolysed is respectively placed in the anode slot and cathode can of electrolytic cell, by cathode
The pH value of solution is adjusted to 0.2 in slot, and it is 2gL that 1mL concentration, which is added,-1KSCN solution as indicator；
(7) anode electrode plate prepared is placed in anode pool, takes out after fixed, is soaked according to anode electrode plate by solution
Wet area and preset current density calculate the current value by electrode plate, pretreated stereotype are placed in cathode
As cathode electrode plate；
(8) electrode fingers are separately connected yin, yang pole plate, are electrolysed under the current density of (7), and electrolysis to cathode is nothing
Color, it is 30.2gL that concentration, which is added, to cathode-1KSCN solution be complexed with trivalent chromium, after 30min stop electrolysis, complexing,
It takes a small amount of catholyte to detect the concentration of its Fe (II) by ultra-violet and visible spectrophotometer, calculates the mass ratio of Fe (II)；
(9) cathode solution after taking (8) to be electrolysed is placed in conical flask, and certain density tri-n-octyl amine liquid is first added thereto
Afterwards, it is placed in water bath chader and carries out extraction experiments；
(10) stratification after shaking takes raffinate respectively by atomic absorption photometer detection Cr (III), Fe
Concentration calculates separately its recovery of extraction.
Alkaline mixed solution in the step (2) is the Na for being 10% with mass fraction2CO3, 10% NaPO4With
What 15% NaOH was formulated.
Sulfuric acid pickling waste liquid major metal component is Cr (III) 2gL in the step (6)-1, Quan Tie 2gL-1。
Current density range in the step (7) is 100Am-2。
The mass ratio of Fe (II) in the step (8) is calculated according to the following formula:
In formula: α mass ratio, %；The concentration gL that c is Fe (II) in solution after being electrolysed-1；c0For Fe in sulfuric acid pickling waste liquid
Concentration, gL-1。
The revolving speed of water bath chader in the step (8) is 250rpm, time 10min.
The concentration of tri-n-octyl amine in the step (9) is 0.5 times of Cr (III)；Tri-n-octyl amine in the step (9)
Diluent be n-amyl alcohol.
The recovery of extraction of Cr (III), Fe in the step (10) are calculated according to the following formula:
In formula, E (%) is recovery of extraction c0、cεThe respectively preceding quality with Cr (III), Fe in water phase after extraction of electrolysis
Concentration, gL-1。
Cr (III) in water phase before electrolysis and after extraction, Fe mass concentration be respectively 2.03gL-1、1.98g·L-1；Extraction
Take Cr (III) in rear water phase, the mass concentration of Fe is respectively 1.32gL-11.82g·L-1.The extraction and recovery of Cr (III), Fe
The calculated result of rate is respectively 34.875%, 8.081%.
Embodiment 2
Difference from Example 1 is:
The pH value of catholyte is 0.8 in (6) in step；
The concentration of tri-n-octyl amine in step (9) is 3 times of Cr (III)；
Cr (III) in water phase before electrolysis and after extraction, Fe mass concentration be respectively 2.01gL-1、1.99g·L-1；Extraction
Take Cr (III) in rear water phase, the mass concentration of Fe is respectively 1.18gL-1、1.06g·L-1.The extraction and recovery of Cr (III), Fe
The calculated result of rate is respectively 41.294%, 46.734%.
Embodiment 3
Difference from Example 1 is:
The pH of catholyte is 1.4 in (6) in step.
The concentration of tri-n-octyl amine in step (9) is 5 times of Cr (III)；
Cr (III) in water phase before electrolysis and after extraction, Fe mass concentration be respectively 1.97gL-1、2.02g·L-1；Extraction
Take Cr (III) in rear water phase, the mass concentration of Fe is respectively 1.27gL-1、0.92g·L-1.The extraction and recovery of Cr (III), Fe
The calculated result of rate is respectively 35.533%, 54.554%.
Since the concentration of Fe (III) seriously affects Cr (III) and SCN-Effect is complexed, it is thus determined that electrolysis Fe (III) is also
The former time is particularly important.The dense of Fe (II) is detected when electrolysis time is 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, pH value are 0.2
Degree, as a result as shown in Fig. 1.By attached drawing 1 it is found that when electrolysis time is 5h, the concentration of Fe (II) is maximum, i.e. the matter of Fe (II)
Amount is most energy saving at this time than maximum.
Tri-n-octyl amine extracts the mechanism of Cr (III) are as follows:
Cr(SCN)6 3-+3R3NH+→(R3NH+)3Cr(SCN)6
Due to extraction system H+Concentration is higher, influences its complexing, therefore has investigated the pass of tri-n-octyl amine concentration and extraction yield
System, as shown in Fig. 2.As seen from the figure, be in range when the extraction yield of Cr (III) is 61.111% is tri-n-octyl amine investigating
Concentration is four times of Cr (III).
Claims (8)
1. a kind of electrolysis-complexing sulfuric acid pickling waste liquid extraction and recovery chromium method, which is characterized in that follow the steps below:
(1) specification 2mm × 30mm × 50mm stereotype is cut, sanding and polishing processing is carried out to stereotype surface using sand paper；
(2) it is washed using deionized water and acetone, its surface blot is cleaned using alkaline mixed solution；
(3) with 5% HNO3Cleaning after boiling 10min in 15% oxalic acid solution, is thoroughly cleaned with deionized water, that is, completed
The pretreatment of electrode plate；
(4) at room temperature, pretreated stereotype is placed in concentration is 1.5molL-1The 100mL H-type electrolytic cell of sulfuric acid solution
In, using 6V as constant voltage, the electrolysis of 3h is carried out, anode electrode plate can be prepared；
(5) clamping fixed by flat mouth after connecting 100mL H-type electrolytic cell by the anionic membrane that diameter is about 2cm；
(6) 50ml sulfuric acid pickling waste liquid to be electrolysed is respectively placed in the anode slot and cathode can of electrolytic cell, it will be in cathode can
The pH value of solution is adjusted to 0.2,0.5,0.8,1.1,1.4, and it is 2g ﹒ L that 1mL concentration, which is added,-1KSCN solution as indicator；
(7) anode electrode plate prepared is placed in anode pool, takes out after fixed, is soaked according to anode electrode plate by solution
Area and preset current density, calculate through the current value of electrode plate, using pretreated stereotype be placed in cathode as
Cathode electrode plate；
(8) electrode fingers are separately connected yin, yang pole plate, are electrolysed under the current density of (7), and it is colourless for being electrolysed to cathode, to
It is 30.2g ﹒ L that concentration, which is added, in cathode-1KSCN solution be complexed with trivalent chromium, stop electrolysis, complexing after 30min, take a small amount of
Catholyte detects the concentration of its Fe (II) by ultra-violet and visible spectrophotometer, calculates the mass ratio of Fe (II)；
(9) cathode solution after taking (8) to be electrolysed is placed in conical flask, after certain density tri-n-octyl amine liquid is first added thereto,
It is placed in water bath chader and carries out extraction experiments；
(10) shake after stratification, take raffinate respectively by atomic absorption photometer detection Cr (III), Fe it is dense
Degree, calculates separately its recovery of extraction.
2. the method for chromium in electrolytic recovery sulfuric acid pickling waste liquid as described in claim 1, which is characterized in that the step (2)
In alkaline mixed solution be with mass fraction be 10% Na2CO3, 10% NaPO4NaOH with 15% is formulated.
3. electrolysis as described in claim 1-complexing sulfuric acid pickling waste liquid extraction and recovery chromium method, which is characterized in that described
Sulfuric acid pickling waste liquid major metal component is Cr (III) 2g ﹒ L in step (6)-1, Quan Tie 2g ﹒ L-1。
4. electrolysis as described in claim 1-complexing sulfuric acid pickling waste liquid extraction and recovery chromium method, which is characterized in that described
Current density in step (7) is 100A ﹒ m-2。
5. electrolysis as described in claim 1-complexing sulfuric acid pickling waste liquid extraction and recovery chromium method, which is characterized in that described
The mass ratio of Fe (II) in step (8) is calculated according to the following formula:
In formula: α is mass ratio, %；The concentration g ﹒ L that c is Fe (II) in solution after being electrolysed-1；c0For Fe in sulfuric acid pickling waste liquid
Concentration, g ﹒ L-1。
6. electrolysis as described in claim 1-complexing sulfuric acid pickling waste liquid extraction and recovery chromium method, it is characterised in that: described
The revolving speed of water bath chader in step (8) is 250rpm, time 10min.
7. electrolysis as described in claim 1-complexing sulfuric acid pickling waste liquid extraction and recovery chromium method, it is characterised in that: described
The concentration of tri-n-octyl amine in step (9) is 0.5-5 times of Cr (III)；The diluent of tri-n-octyl amine in the step (9)
For n-amyl alcohol.
8. electrolysis as described in claim 1-complexing sulfuric acid pickling waste liquid extraction and recovery chromium method, it is characterised in that: described
The recovery of extraction of Cr (III), Fe in step (10) are calculated according to the following formula:
In formula, E (%) is recovery of extraction c0、cεThe respectively preceding mass concentration with Cr (III), Fe in water phase after extraction of electrolysis,
G ﹒ L-1。
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