CN104436755A - Method for separating and respectively purifying and enriching nickel and cobalt through heavy metal adsorption material - Google Patents
Method for separating and respectively purifying and enriching nickel and cobalt through heavy metal adsorption material Download PDFInfo
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- CN104436755A CN104436755A CN201310437987.9A CN201310437987A CN104436755A CN 104436755 A CN104436755 A CN 104436755A CN 201310437987 A CN201310437987 A CN 201310437987A CN 104436755 A CN104436755 A CN 104436755A
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Abstract
The invention provides a method for separating and respectively purifying and enriching nickel and cobalt through a heavy metal adsorption material. The method comprises the following steps: S1, filling heavy metal adsorption materials into adsorption columns of continuous adsorption exchange equipment, wherein the continuous adsorption exchange equipment is composed of a first adsorption column and a second adsorption column, which are connected in series; S2, regulating the pH of liquid to be treated containing nickel ions and cobalt ions to 0.5-5.0 to obtain an acid solution, and injecting the acid solution into the continuous adsorption exchange equipment after the operation in S1; and S3, separating and enriching the pickle liquor by use of the continuous adsorption exchange equipment, regulating the pH of the liquid flowing out from the liquid outlet of the first adsorption column to 1.0-6.5, and injecting the liquid into the liquid inlet of the second adsorption column, wherein the first adsorption column is used for adsorbing and enriching the nickel ions in the pickle liquor and the second adsorption column is used for adsorbing and enriching the cobalt ions in the pickle liquor. Experiments prove that the nickel ions and the cobalt ions can be separated. The method provided by the invention can be used for separating and recycling nickel and cobalt in the liquid and can be used in such fields as separation and recycle of nickel and cobalt recourses in nickel and cobalt pickle liquor of mines.
Description
Technical field
The invention belongs to heavy metal separation technology field, be specifically related to a kind ofly to realize nickel by heavy-metal adsorption material, cobalt is separated and distinguishes the method for purification enrichment.
Background technology
Along with the develop rapidly of World Economics and the continuous increase of the size of population, relative inadequacy of resources and the weak important bottleneck having become world development of environmental carrying capacity.Resources for construction economizing type and friendly environment society, advance Ecological Civilization Construction, become the theme that world is paid close attention to.
At present, for the various industrial wastewaters containing heavy metal ion, sanitary sewage and nuclear industry waste water, generally adopt the methods such as chemical precipitation method, oxidation-reduction method or ion-exchange to process it, thus reduce content of beary metal in water resource, reduce the harm of heavy metal pollution.But, there is the defect that removal efficiency is low and cost is high of heavy metal ions in wastewater in the processing method of all kinds of heavy metal wastewater therebies adopted at present.
At present, use extraction to carry out technical barriers numerous in processing procedure to nickel and cobalt containing associated minerals, as technological process is complicated, require higher to Steep cencentration, the nickel magnesium separation of raffinate, the cobalt magnesium of back extraction cobalt liquid are separated, the problems such as wastewater discharge is large.
Summary of the invention
For the defect that prior art exists, the invention provides and a kind ofly realize nickel by heavy-metal adsorption material, cobalt is separated and distinguishes the method for purification enrichment, there is the advantage strong to the selective absorption of nickel ion.
The technical solution used in the present invention is as follows:
The invention provides and a kind ofly realize nickel by heavy-metal adsorption material, cobalt is separated and distinguishes the method for purification enrichment, comprise the following steps:
S1, fills heavy-metal adsorption material respectively in each adsorption column of continuous adsorption switching equipment; Wherein, described continuous adsorption switching equipment is composed in series by the first adsorption column and the second adsorption column;
S2, the pH that adjustment contains the pending liquid of nickel ion and cobalt ions is 0.5-5.0, obtains pickle liquor;
S3, injects the described continuous adsorption switching equipment after S1 operation by described pickle liquor;
S4, described continuous adsorption switching equipment carries out separation and concentration purification to described pickle liquor, specifically comprises: be the inlet that described continuous adsorption switching equipment is injected in the described pickle liquor of 0.5-5.0 by pH; Nickel ion in pickle liquor described in described first adsorption column adsorption and enrichment; The liquid flowed out from described first adsorption column liquid outlet adjusts pH to be the inlet injecting described second adsorption column after 1.0-6.5, the cobalt ions in pickle liquor described in described second adsorption column adsorption and enrichment;
S5, rinses described first adsorption column and described second adsorption column respectively with dilute acid soln; Described heavy-metal adsorption material in described first adsorption column carries out desorption operations, obtains containing nickel ion stripping liquid and the described heavy-metal adsorption material be desorbed after desorption operations; Described heavy-metal adsorption material in described second adsorption column carries out desorption operations, obtains containing cobalt ions stripping liquid and the described heavy-metal adsorption material be desorbed after desorption operations;
S6, carries out electrodeposition operation containing nickel ion stripping liquid by direct electrowinning equipment described in being obtained by S5, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy-metal adsorption material be desorbed in the first adsorption column recovers absorption property after rinsing process;
Carry out electrodeposition operation by direct electrowinning equipment after concentrated containing cobalt ions stripping liquid described in being obtained by S5, obtain cobalt metallic plate or cobalt metal powder; Meanwhile, the described heavy-metal adsorption material be desorbed in the second adsorption column recovers absorption property after rinsing process.
Preferably, the synthetic method of described heavy-metal adsorption material.
Preferably, the method for nickel, cobalt separation is realized by heavy-metal adsorption material.
Below the present invention is described further:
Novelty of the present invention prepare a kind of heavy-metal adsorption material, the experiment proved that, this heavy-metal adsorption material all has adsorptivity to nickel and cobalt ions, the impurity such as calcium, magnesium, silicon are not adsorbed, and to the adsorption activity of nickel ion higher than the adsorption activity to cobalt ions, for this feature, for realizing being separated nickel ion and cobalt ions, inventor has carried out test of many times to the technique using adsorption column to cross post, find by the series connection to mistake post, can realize being separated of good nickel ion and cobalt ions, nickel and cobalt ions is separated with foreign ion.Therefore, the method being realized Separation of nickel and cobalt by heavy-metal adsorption material provided by the invention, can be applied to being separated and recovery of nickel and cobalt in liquid, can be applied to separation and the recovery of nickel minerals, cobalt in nickeliferous, cobalt ore.
Accompanying drawing explanation
Fig. 1 is heavy-metal adsorption material figure.
Fig. 2 is the methods experiment installation drawing being realized Separation of nickel and cobalt by heavy-metal adsorption material.
Fig. 3 is the process route chart of the method being realized Separation of nickel and cobalt by heavy-metal adsorption material
detailed description of the invention
Below the method realizing Separation of nickel and cobalt by heavy-metal adsorption material provided by the invention is described in detail:
heavy-metal adsorption material preparation method embodiment
1), by former silica gel add in the reactor of corrosion resistant band stirring, then add the acid of an equivalent of silica gel weight more than 1.5 times from elevated dosing vessel, carry out heating and boil and slowly stir, in order to avoid damage silica gel; Stirring and pickling under bubble point temperature, washes away the greasy dirt of silica gel and the metal ion of surface attachment; Then the chuck to reactor leads to cooling water temperature, releases silica gel when making temperature of charge in still drop to normal temperature; The silica gel of releasing is in filtration washing device, and elimination acid solution, then washs silica gel by deionized water, stops washing when washings display is neutral, carries out being separated of silica gel and water, then dries silica gel; Take out when silica gel reaches constant weight, enter next procedure; Through pickling and the silica gel being dried to constant weight is put in a water vapour saturator, start the humid air that air compressor bromizates sodium/KBr saturated solution reactor and enter in water vapour saturator, make Silica Surface generate hydrone individual layer; To recording the moisture content of hydrated silica gel between 2.0-5.0%, hydration completes; Hydrated silica gel is put into the reactor that another corrosion resistant band stirs, hexane elevated dosing vessel above this reactor and silane coupler elevated dosing vessel, in reactor, put the hexane of quite former silica gel weight more than two times, the silane coupler of more than 0.5 times respectively into, be then slowly uniformly mixed; Silica gel carries out the Silanization reaction under normal temperature in a kettle., and the reaction time should ensure more than 10 hours; Carry out being separated of silica gel and raffinate after having reacted, then silanized silica gel is washed; Washed silanized silica gel is dried, and to when the rate of body weight gain recording silanized silica gel is between 15-22%, this is silanized silica gel; Silanized silica gel is added in the reactor of a corrosion resistant band stirring, then to reactor, add epomine and deionized water from elevated dosing vessel respectively, be slowly uniformly mixed; When reaction temperature drops to below 40 DEG C, add quite former silica gel weight 0.5-1.5 methyl alcohol doubly again, add in backward reacting kettle jacketing and pass into hot water and carry out heating and maintain reacting kettle jacketing water temperature and be less than 69 DEG C and slowly stir, to when to record the silica gel after grafting be more than 1.5 times of former silica gel weight, grafting completes; After graft reaction terminates, wash after grafting silica gel is separated with solution; Wherein, the addition of epomine requires at least equal with former silica gel weight, and it is more than the twice of former silica gel weight that deionized water addition requires; Dry to record moisture content below 10% time discharging, obtain low concentration heavy metal water inorganic agent material of the present invention;
2), the low concentration heavy metal water inorganic agent of above-mentioned acquisition and sodium chloroacetate generate toxic heavy metal waste water treating agent of the present invention; Its process is as follows: reactor sodium chloroacetate being put into a corrosion resistant band stirring, in this reactor, deionized water is added slowly by elevated dosing vessel, and till stirring sodium chloroacetate being dissolved completely, 0.5 times of the addition >=above-mentioned low concentration heavy metal water inorganic agent weight of sodium chloroacetate; Again the low concentration heavy metal water inorganic agent that above step obtains is added in reactor, soaked completely by sodium chloroacetate solution; At this moment, start vavuum pump, extract the methane gas of emerging in dereaction still through vacuum pipeline; Above-mentioned low concentration heavy metal water inorganic agent is through stirring and sodium chloroacetate complete reaction at leisure, now starting heat-exchanger pump is sent in the chuck of reactor by the hot water in tank, it is made to heat below 69 DEG C, and making its pH value remain between 8-10, reaction is carried out after more than 20 hours, stops stirring, open valve, solution is connected material from reactor, puts into sink, elimination solution, puts into storage tank; Material in sink is washed, then dries, to stopping when moisture content is below 10% drying and discharging; Obtain toxic heavy metal wastewater treatment agent material of the present invention;
separation of nickel and cobalt methods experiment example 1
the heavy-metal adsorption material that this experimental example adopts heavy-metal adsorption material preparation method embodiment to prepare.
S1, fills heavy-metal adsorption material respectively in each adsorption column of continuous adsorption switching equipment; Wherein, described continuous adsorption switching equipment is composed in series by the first adsorption column and the second adsorption column;
S2, the pH that adjustment contains the pending liquid of nickel ion and cobalt ions is 3.5, obtains pickle liquor;
S3, injects the described continuous adsorption switching equipment after S1 operation by described pickle liquor;
S4, described continuous adsorption switching equipment carries out separation and concentration purification to described pickle liquor, specifically comprises: by pH be 3.5 described pickle liquor pump into the inlet of described continuous adsorption switching equipment; Nickel ion in pickle liquor described in described first adsorption column adsorption and enrichment; The liquid flowed out from described first adsorption column liquid outlet adjusts pH to be the inlet pumping into described second adsorption column after 5.0, the cobalt ions in pickle liquor described in described second adsorption column adsorption and enrichment;
Mass fraction is that the sulfuric acid of 20% rinses described first adsorption column and described second adsorption column respectively by S5; Described heavy-metal adsorption material in described first adsorption column carries out desorption operations, obtains containing nickel ion stripping liquid and the described heavy-metal adsorption material be desorbed after desorption operations; Described heavy-metal adsorption material in described second adsorption column carries out desorption operations, obtains containing cobalt ions stripping liquid and the described heavy-metal adsorption material be desorbed after desorption operations;
S6, carries out electrodeposition operation by direct electrowinning equipment after concentrated containing nickel ion stripping liquid described in being obtained by S5, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy-metal adsorption material be desorbed in the first adsorption column recovers absorption property after pure water rinsing process;
Carry out electrodeposition operation by direct electrowinning equipment after concentrated containing cobalt ions stripping liquid described in being obtained by S5, obtain cobalt metallic plate or cobalt metal powder; Meanwhile, the described heavy-metal adsorption material be desorbed in the second adsorption column recovers absorption property after rinsing process.
In the cobalt powder prepared, cobalt mass fraction is 99.998%, and nickel mass fraction is 0.002%;
In the nickel powder prepared, nickel mass fraction is 99.997%, and cobalt mass fraction is 0.003%.
separation of nickel and cobalt methods experiment example 2
This experimental example, for testing the absorption property of heavy-metal adsorption material to nickel ion and cobalt ions, specifically comprises: pH on the impact of adsorbance and temperature on the impact of adsorbance.
Experimental technique: compound concentration is the nickel ion solution of 0.02mol/L, utilizes acidometer to regulate the pH of nickel ion solution; The solution 50ml mixing up pH is placed in the wide-mouth bottle that 1g heavy-metal adsorption material is housed, wide-mouth bottle is placed in the water bath with thermostatic control of 25 degrees Celsius 36 hours, take out and filter, measure the concentration of nickel ion in filtrate.Adsorbance is calculated according to formula ();
Q=(C
0-C) * V/m formula ()
Wherein, Q is adsorbance (mmol/g); C
0for adsorbing front nickel ion concentration (mol/L); C is nickel ion concentration (mol/L) after absorption; V is the volume (ml) of solution; M is the quality (g) of heavy-metal adsorption material.
Identical with the above-mentioned experimental technique to nickel ion to the experimental technique of cobalt ions.
(1) pH tests the impact of adsorbance
Change the pH of above-mentioned experimental technique, carry out adsorption experiment to nickel ion with to cobalt ions respectively, experimental result is in table 1.
Table 1
| Nickel adsorbance (mmol/g) | Cobalt adsorbance (mmol/g) | |
| pH=1 | 0.22 | 0.05 |
| pH=2 | 0.31 | 0.07 |
| pH=2.5 | 0.37 | 0.10 |
| pH=3.0 | 0.42 | 0.16 |
| pH=3.5 | 0.51 | 0.15 |
| pH=4.0 | 0.55 | 0.24 |
| pH=5.0 | 0.53 | 0.27 |
| pH=5.5 | 0.38 | 0.41 |
| pH=6.0 | 0.24 | 0.45 |
| pH=6.5 | 0.16 | 0.44 |
As can be seen from Table 1, the heavy-metal adsorption material that the present invention prepares all has certain adsorption capacity to nickel ion and cobalt ions, and is better than the absorption property to cobalt ions to the absorption property of nickel ion.So, by the heavy-metal adsorption material adopting the present invention to prepare, after separating technology is optimized, the effect that nickel ion is separated with cobalt ions can be realized.
In addition, for the adsorption experiment to nickel ion, along with the increase of pH, heavy-metal adsorption material increases rapidly the adsorbance of nickel ion, and when pH reaches 4.0, adsorbance reaches maximum; Then along with the increase of pH, adsorbance slowly reduces, and therefore, the Optimal pH of nickel ion absorption is 3.5-5.0.
To the adsorption experiment of cobalt ions, along with the increase of pH, the adsorbance of heavy-metal adsorption material to cobalt ions increases gradually, and pH is when 5.5-6.5, and adsorbance is larger; Therefore, the Optimal pH of cobalt ions absorption is 5.5-6.5.
(2) temperature is tested the impact of adsorbance
Nickel ion adsorption experiment gets pH 4.0, and cobalt ions adsorption experiment gets pH 5.5; Change the bath temperature of experimental technique, carry out adsorption experiment to nickel ion with to cobalt ions respectively, experimental result is in table 2.
Table 2
| Nickel adsorbance (mmol/g) | Cobalt adsorbance (mmol/g) | |
| 10 | 0.10 | 0.05 |
| 15 | 0.26 | 0.15 |
| 20 | 0.38 | 0.22 |
| 25 | 0.52 | 0.30 |
| 30 | 0.51 | 0.32 |
| 35 | 0.53 | 0.38 |
| 40 | 0.50 | 0.40 |
| 45 | 0.55 | 0.41 |
| 50 | 0.56 | 0.41 |
As can be seen from Table 2, along with the increase of temperature, heavy-metal adsorption material increases rapidly the adsorbance of nickel ion, and when temperature reaches 25 DEG C, adsorbance is larger; Then along with the continuation of temperature increases, adsorbance increasing degree is slow.The adsorbance impact of temperature on cobalt ions is similar to on the impact of nickel.So can determine, in the process of carrying out Separation of nickel and cobalt, optimum temperature is 25 DEG C.
Claims (7)
1. realize nickel by heavy-metal adsorption material, cobalt is separated and distinguishes a method for purification enrichment, it is characterized in that, realize Separation of nickel and cobalt by heavy-metal adsorption material.
2. the method being realized the separation of nickel cobalt by heavy-metal adsorption material according to claim 1, be is characterized in that, comprise the following steps:
S1, fills heavy-metal adsorption material respectively in each adsorption column of continuous adsorption switching equipment; Wherein, described continuous adsorption switching equipment is composed in series by the first adsorption column and the second adsorption column;
S2, adjustment contains the pH of the pending liquid of cobalt ions and manganese ion to OK range, obtains pickle liquor A;
S3, injects the described continuous adsorption switching equipment after S1 operation by described pickle liquor A;
S4, described continuous adsorption switching equipment carries out separation and concentration purification to described pickle liquor A, specifically comprises: the inlet described pickle liquor A being injected described continuous adsorption switching equipment; Nickel ion in pickle liquor A described in described first adsorption column adsorption and enrichment; The liquid flowed out from described first adsorption column liquid outlet adjusts pH to OK range, obtains pickle liquor B; Described pickle liquor B is injected the inlet of described second adsorption column, the cobalt ions in pickle liquor B described in described second adsorption column adsorption and enrichment;
S5, rinses described first adsorption column and described second adsorption column respectively with dilute acid soln; Described heavy-metal adsorption material in described first adsorption column carries out desorption operations, obtains containing nickel ion stripping liquid and the described heavy-metal adsorption material be desorbed after desorption operations; Described heavy-metal adsorption material in described second adsorption column carries out desorption operations, obtains containing cobalt ions stripping liquid and the described heavy-metal adsorption material be desorbed after desorption operations;
S6, carries out electrodeposition operation containing nickel ion stripping liquid by direct electrowinning equipment described in being obtained by S5, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy-metal adsorption material be desorbed in the first adsorption column recovers absorption property after rinsing process;
Carry out electrodeposition operation by direct electrowinning equipment after concentrated containing cobalt ions stripping liquid described in being obtained by S5, obtain cobalt metallic plate or cobalt metal powder; Meanwhile, the described heavy-metal adsorption material be desorbed in the second adsorption column recovers absorption property after rinsing process.
3. the method being realized the separation of nickel cobalt by heavy-metal adsorption material according to claim 1, be is characterized in that, the synthetic method patent applied for of described heavy-metal adsorption material, and the patent No. is:
ZL 03126367.4(authorizes);
ZL 03126366.6(authorizes);
ZL 03126365.8(authorizes);
ZL 03126368.2(authorizes).
4. the method being realized Separation of nickel and cobalt by heavy-metal adsorption material according to claim 1, be is characterized in that, completes the enrichment of two kinds of metals while carrying out Separation of nickel and cobalt.
5. the method being realized Separation of nickel and cobalt by heavy-metal adsorption material according to claim 1, be is characterized in that, the nickel after the method separation and concentration and cobalt can obtain nickel metallic plate or nickel metal powder, nickel metallic plate or nickel metal powder by direct electro-deposition.
6. according to claim 1ly realize the separation of nickel cobalt and the method for respectively purifying by heavy-metal adsorption material, it is characterized in that, in described step S2, the pH of pickle liquor A adjusts to 0.5-5.5.
7. according to claim 1ly realize the separation of nickel cobalt and the method for respectively purifying by heavy-metal adsorption material, it is characterized in that, in described step S4, the pH of pickle liquor B adjusts to 1.0-6.5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219658A (en) * | 2016-08-16 | 2016-12-14 | 南昌航空大学 | The classification removal of a kind of heavy metals in industrial wastewater and recovery method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219658A (en) * | 2016-08-16 | 2016-12-14 | 南昌航空大学 | The classification removal of a kind of heavy metals in industrial wastewater and recovery method |
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