CN102814058B - Method for implementing nickel-magnesium separation, enrichment and purification by using heavy metal adsorbing material - Google Patents
Method for implementing nickel-magnesium separation, enrichment and purification by using heavy metal adsorbing material Download PDFInfo
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- CN102814058B CN102814058B CN201210344744.6A CN201210344744A CN102814058B CN 102814058 B CN102814058 B CN 102814058B CN 201210344744 A CN201210344744 A CN 201210344744A CN 102814058 B CN102814058 B CN 102814058B
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 108
- 239000000463 material Substances 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 238000000746 purification Methods 0.000 title claims abstract description 28
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 claims abstract description 268
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 163
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 82
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 75
- 239000007788 liquid Substances 0.000 claims abstract description 52
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 66
- 235000021110 pickles Nutrition 0.000 claims description 60
- 238000010521 absorption reaction Methods 0.000 claims description 51
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 48
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 34
- 239000003153 chemical reaction reagent Substances 0.000 claims description 34
- 238000001291 vacuum drying Methods 0.000 claims description 32
- 239000000741 silica gel Substances 0.000 claims description 31
- 229910002027 silica gel Inorganic materials 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 26
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 24
- 239000012065 filter cake Substances 0.000 claims description 24
- 150000002500 ions Chemical class 0.000 claims description 22
- 238000010992 reflux Methods 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 10
- 229920006395 saturated elastomer Polymers 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000012141 concentrate Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000004070 electrodeposition Methods 0.000 claims description 8
- 238000005363 electrowinning Methods 0.000 claims description 8
- 230000008030 elimination Effects 0.000 claims description 8
- 238000003379 elimination reaction Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- 159000000003 magnesium salts Chemical class 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000008096 xylene Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000000693 micelle Substances 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052749 magnesium Inorganic materials 0.000 abstract description 13
- 239000011777 magnesium Substances 0.000 abstract description 13
- 238000002386 leaching Methods 0.000 abstract 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000001994 activation Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a method for implementing nickel-magnesium separation, enrichment and purification by using a heavy metal adsorbing material, which comprises the following steps: S1. filling a heavy metal adsorbing material into an adsorption column of continuous adsorption exchange equipment; S2. regulating the pH value of a solution to be treated containing nickel ions and magnesium ions to 1.0-5.5, thereby obtaining an acid leaching solution; S3. injecting the acid leaching solution into the continuous adsorption exchange equipment after the operation of S1; and S4. carrying out separation, enrichment and purification on the acid leaching solution by using the continuous adsorption exchange equipment. The experiment proves that the accurate control on the temperature and flow rate of the treatment solution can implement separation of nickel and magnesium; and therefore, the method provided by the invention can be used for separating and recovering slight or trace amounts of nickel and magnesium in the liquid.
Description
Technical field
The invention belongs to heavy metal separation technology field, be specifically related to a kind of method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material.
Background technology
Along with the develop rapidly of World Economics and the continuous increase of the size of population, a little less than relative inadequacy of resources and environmental carrying capacity, become the important bottleneck of world development.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 that contain 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, thereby reduce content of beary metal in water resource, reduce the harm of heavy metal pollution.
But, there is the low and high defect of cost of the removal efficiency of heavy metal ions in wastewater in the processing method of all kinds of heavy metal wastewater therebies that adopt at present.
Summary of the invention
The defect existing for prior art, the invention provides a kind of method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material, has advantages of the selective absorption of nickel ion strong.
The technical solution used in the present invention is as follows:
The invention provides a kind of method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material, comprise the following steps:
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion is 1.0-5.5, 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 at 25-40 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 1.0-5.5 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
S5, the sulfuric acid that is 5-30% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained.
Preferably, described heavy metal adsorption material is prepared by the following method:
Pretreatment: under ultrasonic field, raw material silica gel is scattered in to the hydrochloric acid solution of 7-10mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 4-6: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 110-140 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent in reaction vessel, stir silylating reagent is dissolved in anhydrous dimethyl benzole soln, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 5-8: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 5-10: 1; Silylating reagent and activated silica gel mass ratio are 2-4: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 10-20 hour; Filtering reacting liquid after being down to 20-30 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material.
Preferably, the power of described ultrasonic field is 150-250 watt;
Described vacuum drying in silica gel bonded reaction specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think the be refrigerated to-50--45 DEG C of speed cooling of 5-8 DEG C/min, the time of maintain-50--45 DEG C is 4-5 hour;
Second stage, be warming up to-10--5 DEG C of the speed of 3-6 DEG C/min, the time of maintain-10--5 DEG C is 5-7 hour;
Phase III, in putting fast and being the vacuum drying chamber of 160 DEG C-170 DEG C to temperature, obtain described heavy metal adsorption material 13-17 hour drying time.
Preferably, described silylating reagent is 3-ethylenediamine base propyl trimethoxy silicane or 3-Diethylenetriamine base propyl trimethoxy silicane.
Preferably, the aperture of described heavy metal adsorption material is 5.25-7.38nm, the pore volume of described heavy metal adsorption material be 1.0-1.4 cubic centimetre/gram.
Preferably, described raw silicon micelle degree is 300-400 order silica gel.
Preferably, S4 specifically comprises following three phases:
First stage: the pickle liquor that is 1.0-5.5 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 2-4ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 7-9ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
Preferably, S4 specifically comprises following three phases:
First stage: the pickle liquor that is 3.5-4.0 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 3ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 8ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
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 has stronger adsorptivity to nickel ion, adsorb hardly magnesium ion, for this feature, for realizing separating nickel ion and magnesium ion, inventor has carried out test of many times to the technique that uses adsorption column to cross post, unexpected discovery, by to crossing the temperature of post and the accurate control of flow velocity, can realize separating of good nickel ion and magnesium ion, and, in the preparation process of heavy metal adsorption material, as well known to those skilled in the art, silica gel is the porous mass being formed by the intermolecular dehydration of poly silica gel, water in silica gel structure formula comprises constitution water and adsorbed water, wherein, constitution water is connected with silicon atom with OH-form, be covered in Silica Surface.The inventor, silica gel is carried out in activation process, introduces ultrasonic technology, and has taked to add with concentrated hydrochloric acid the violent condition of hot reflux.Carry out, in dry process, having taked special temperature controlled processes at the heavy metal adsorption material to the hygrometric state finally obtaining, the heavy metal adsorption material of preparing thus the experiment proved that, can extraordinary realization separating nickel ion and magnesium ion.Therefore, the method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material provided by the invention, can be applied to separating and recovery of trace in liquid or Determination of Trace Nickel and magnesium.
Detailed description of the invention
Below the method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material provided by the invention is described in detail:
Heavy metal adsorption material preparation method embodiment 1
Pretreatment: under 150 watts of ultrasonic fields, raw material silica gel is scattered in to the hydrochloric acid solution of 10mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 4: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 140 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent 3-ethylenediamine base propyl trimethoxy silicane in reaction vessel, stirring is dissolved in anhydrous dimethyl benzole soln silylating reagent, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 5: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 10: 1; Silylating reagent and activated silica gel mass ratio are 3.5: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 12 hours; Filtering reacting liquid after being down to 24 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material.In this step, vacuum drying specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think that the speed cooling of 5 DEG C/min is refrigerated to-50 DEG C, the time that maintains-50 DEG C is 4 hours;
Second stage, is warming up to-7 DEG C with the speed of 5 DEG C/min, and the time that maintains-7 DEG C is 5.5 hours;
Phase III, puts fast to the temperature vacuum drying chamber that is 160 DEG C DEG C, obtains described heavy metal adsorption material 13 hours drying times.
Making aperture is that 6.85nm, pore volume are the heavy metal adsorption material of 1.3 cubic centimetres/gram.
Heavy metal adsorption material preparation method embodiment 2
Pretreatment: under 250 watts of ultrasonic fields, raw material silica gel is scattered in to the hydrochloric acid solution of 7mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 6: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 110 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent 3-Diethylenetriamine base propyl trimethoxy silicane in reaction vessel, stirring is dissolved in anhydrous dimethyl benzole soln silylating reagent, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 8: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 10: 1; Silylating reagent and activated silica gel mass ratio are 4: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 18 hours; Filtering reacting liquid after being down to 27 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material.In this step, vacuum drying specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think that the speed cooling of 8 DEG C/min is refrigerated to-45 DEG C, the time that maintains-45 DEG C is 5 hours;
Second stage, is warming up to-9 DEG C with the speed of 5 DEG C/min, and the time that maintains-9 DEG C is 5.5 hours;
Phase III, in putting fast and being the vacuum drying chamber of 170 DEG C to temperature, obtain described heavy metal adsorption material 13 hours drying times.
Making aperture is that 6.32nm, pore volume are the heavy metal adsorption material of 1.1 cubic centimetres/gram.
Heavy metal adsorption material preparation method embodiment 3
Pretreatment: under 200 watts of ultrasonic fields, raw material silica gel is scattered in to the hydrochloric acid solution of 8mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 5: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 120 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent 3-ethylenediamine base propyl trimethoxy silicane in reaction vessel, stirring is dissolved in anhydrous dimethyl benzole soln silylating reagent, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 6: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 6: 1; Silylating reagent and activated silica gel mass ratio are 3.2: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 18 hours; Filtering reacting liquid after being down to 25 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material.In this step, vacuum drying specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think that the speed cooling of 7 DEG C/min is refrigerated to-47 DEG C, the time that maintains-47 DEG C is 4.5 hours;
Second stage, is warming up to-6 DEG C with the speed of 5 DEG C/min, and the time that maintains-6 DEG C is 6 hours;
Phase III, in putting fast and being the vacuum drying chamber of 162 DEG C to temperature, obtain described heavy metal adsorption material 14 hours drying times.
Making aperture is that 7.12nm, pore volume are the heavy metal adsorption material of 1.3 cubic centimetres/gram.
Heavy metal adsorption material preparation method embodiment 4
Pretreatment: under 220 watts of ultrasonic fields, raw material silica gel is scattered in to the hydrochloric acid solution of 9mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 5: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 120 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent 3-Diethylenetriamine base propyl trimethoxy silicane in reaction vessel, stirring is dissolved in anhydrous dimethyl benzole soln silylating reagent, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 7: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 6: 1; Silylating reagent and activated silica gel mass ratio are 3.7: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 15 hours; Filtering reacting liquid after being down to 22 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material.In this step, vacuum drying specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think that the speed cooling of 7 DEG C/min is refrigerated to-46 DEG C, the time that maintains-46 DEG C is 4.2 hours;
Second stage, is warming up to-8 DEG C with the speed of 4 DEG C/min, and the time that maintains-8 DEG C is 6 hours;
Phase III, in putting fast and being the vacuum drying chamber of 165 DEG C to temperature, obtain described heavy metal adsorption material 15 hours drying times.
Making aperture is that 6.32nm, pore volume are the heavy metal adsorption material of 1.2 cubic centimetres/gram.
Heavy metal adsorption material preparation method embodiment 5
Pretreatment: under 220 watts of ultrasonic fields, raw material silica gel is scattered in to the hydrochloric acid solution of 9mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 5.5: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 130 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent 3-Diethylenetriamine base propyl trimethoxy silicane in reaction vessel, stirring is dissolved in anhydrous dimethyl benzole soln silylating reagent, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 7: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 8: 1; Silylating reagent and activated silica gel mass ratio are 3.8: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 20 hours; Filtering reacting liquid after being down to 20 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material.In this step, vacuum drying specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think that the speed cooling of 7.5 DEG C/min is refrigerated to-48 DEG C, the time that maintains-48 DEG C is 4.8 hours;
Second stage, is warming up to-10 DEG C with the speed of 6 DEG C/min, and the time that maintains-10 DEG C is 7 hours;
Phase III, in putting fast and being the vacuum drying chamber of 166 DEG C to temperature, obtain described heavy metal adsorption material 136 hours drying times.
Making aperture is that 7.38nm, pore volume are the heavy metal adsorption material of 1.4 cubic centimetres/gram.
Heavy metal adsorption material preparation method embodiment 6
Pretreatment: under 160 watts of ultrasonic fields, raw material silica gel is scattered in to the hydrochloric acid solution of 8mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 4.3: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 130 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent 3-Diethylenetriamine base propyl trimethoxy silicane in reaction vessel, stirring is dissolved in anhydrous dimethyl benzole soln silylating reagent, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 5.5: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 7: 1; Silylating reagent and activated silica gel mass ratio are 3.2: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 10 hours; Filtering reacting liquid after being down to 30 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material.In this step, vacuum drying specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think that the speed cooling of 7.8 DEG C/min is refrigerated to-48 DEG C, the time that maintains-48 DEG C is 4.3 hours;
Second stage, is warming up to-5 DEG C with the speed of 3 DEG C/min, and the time that maintains-5 DEG C is 5 hours;
Phase III, in putting fast and being the vacuum drying chamber of 168 DEG C to temperature, obtain described heavy metal adsorption material 15 hours drying times.
Making aperture is that 5.25nm, pore volume are the heavy metal adsorption material of 1.0 cubic centimetres/gram.
The separation of nickel magnesium, enrichment, method of purification experimental example 1
The heavy metal adsorption material that this experimental example adopts heavy metal adsorption material preparation method embodiment 1 to prepare.
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion 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 at 25 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 3.5 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
Wherein, specifically comprise following three phases:
First stage: the pickle liquor that is 3.5 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 2ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 8.5ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
S5, the sulfuric acid that is 29% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained.
In the nickel powder preparing, nickel mass fraction is 99.999%, and magnesium mass fraction is 0.001%.
The separation of nickel magnesium, enrichment, method of purification experimental example 2
The heavy metal adsorption material that this experimental example adopts heavy metal adsorption material preparation method embodiment 1 to prepare.
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion is 4.0, 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 at 40 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 4.0 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
Wherein, specifically comprise following three phases:
First stage: the pickle liquor that is 4.0 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 4ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 8.2ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
S5, the sulfuric acid that is 25% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained.
In the nickel powder preparing, nickel mass fraction is 99.997%, and magnesium mass fraction is 0.003%.
The separation of nickel magnesium, enrichment, method of purification experimental example 3
The heavy metal adsorption material that this experimental example adopts heavy metal adsorption material preparation method embodiment 1 to prepare.
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion is 5.5, 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 at 35 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 5.5 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
Wherein, specifically comprise following three phases:
First stage: the pickle liquor that is 5.5 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 3ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 7.5ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
S5, the sulfuric acid that is 30% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained.
In the nickel powder preparing, nickel mass fraction is 99.998%, and magnesium mass fraction is 0.002%.
The separation of nickel magnesium, enrichment, method of purification experimental example 4
The heavy metal adsorption material that this experimental example adopts heavy metal adsorption material preparation method embodiment 1 to prepare.
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion is 1.0, 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 at 29 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 1.0 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
Wherein, specifically comprise following three phases:
First stage: the pickle liquor that is 1.0 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 3.5ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 8ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
S5, the sulfuric acid that is 24% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained.
In the nickel powder preparing, nickel mass fraction is 99.998%, and magnesium mass fraction is 0.002%.
The separation of nickel magnesium, enrichment, method of purification experimental example 5
The heavy metal adsorption material that this experimental example adopts heavy metal adsorption material preparation method embodiment 1 to prepare.
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion is 2.7, 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 at 38 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 2.7 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
Wherein, specifically comprise following three phases:
First stage: the pickle liquor that is 2.7 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 2.5ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 9ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
S5, the sulfuric acid that is 12% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained.
In the nickel powder preparing, nickel mass fraction is 99.998%, and magnesium mass fraction is 0.002%.
The separation of nickel magnesium, enrichment, method of purification experimental example 6
The heavy metal adsorption material that this experimental example adopts heavy metal adsorption material preparation method embodiment 1 to prepare.
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion is 3.8, 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 at 32 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 3.8 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
Wherein, specifically comprise following three phases:
First stage: the pickle liquor that is 3.8 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 2.9ml/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 7ml/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
S5, the sulfuric acid that is 6% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained.
In the nickel powder preparing, nickel mass fraction is 99.998%, and magnesium mass fraction is 0.002%.
Test example 1
This test example, for testing the absorption property of heavy metal adsorption material to nickel and magnesium, specifically comprises: impact and the temperature impact on adsorbance of pH on adsorbance.
Experimental technique: the nickel ion solution that compound concentration is 0.02mol/L, utilizes acidometer to regulate the pH of nickel ion solution; The solution 50ml that mixes 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 to 36 hours, take out and filter, measure the concentration of nickel ion in filtrate.
Calculate adsorbance according to formula ();
Q＝(C
0-C)*V/m
Wherein, Q is adsorbance (mmol/g); C
0for adsorbing front nickel ion concentration (mol/L); C is the rear nickel ion concentration (mol/L) of absorption; V is the volume (ml) of solution; The attach most importance to quality (g) of metal-adsorbing material of m.
Identical with the above-mentioned experimental technique to nickel ion to the experimental technique of magnesium ion.
(1) the impact experiment of pH on adsorbance
Change the pH of above-mentioned experimental technique, carry out adsorption experiment respectively to nickel ion with to magnesium ion, experimental result is in table 1.
Table 1
| Nickel adsorbance (mmol/g) | Magnesium adsorbance (mmol/g) | |
| pH＝1 | 0.16 | 0.00 |
| pH＝2 | 0.23 | 0.00 |
| pH＝3 | 0.48 | 0.00 |
| pH＝3.5 | 0.83 | 0.00 |
| pH＝4 | 0.95 | 0.00 |
| pH＝4.5 | 0.65 | 0.00 |
| pH＝5 | 0.35 | 0.00 |
| pH＝5.5 | 0.29 | 0.00 |
As can be seen from Table 1, the heavy metal adsorption material that the present invention prepares has certain adsorption capacity to nickel, to magnesium without any adsorption activity.So, by the heavy metal adsorption material that adopts the present invention to prepare, after separating technology is optimized, can realize the effect that nickel ion is separated with magnesium ion.
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 in the time that pH reaches 4.0, adsorbance reaches maximum; Then along with the increase of pH, adsorbance slowly reduces.So, can determine, carrying out in the process that nickel ion separates with magnesium ion, best pH is 4.0.
(2) the impact experiment of temperature on adsorbance
Under the experiment condition of best pH 4.0, change the bath temperature of above-mentioned experimental technique, carry out adsorption experiment to nickel ion with to magnesium ion respectively, experimental result is in table 2.
Table 2
| Nickel adsorbance (mmol/g) | Magnesium adsorbance (mmol/g) | |
| 10 | 0.20 | 0.00 |
| 15 | 0.42 | 0.00 |
| 20 | 0.63 | 0.00 |
| 28 | 0.95 | 0.00 |
| 30 | 0.96 | 0.00 |
| 35 | 0.96 | 0.00 |
| 40 | 0.97 | 0.00 |
| 45 | 0.63 | 0.00 |
| 50 | 0.42 | 0.00 |
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 in the time that temperature reaches 28 DEG C, adsorbance is larger; Then along with the continuation of temperature increases, adsorbance increasing degree is slow.So, can determine, carrying out in the process that nickel ion separates with magnesium ion, optimum temperature is 28 DEG C.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be looked protection scope of the present invention.
Claims (5)
1. a method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material, is characterized in that, comprises the following steps:
S1 fills heavy metal adsorption material in the adsorption column of continuous adsorption switching equipment;
S2, the pH that adjusts the pending liquid that contains nickel ion and magnesium ion is 1.0-5.5, 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 at 25-40 DEG C to described pickle liquor, specifically comprise: the described pickle liquor that is 1.0-5.5 by pH pumps into the inlet of described continuous adsorption switching equipment; Nickel ion described in described adsorption column adsorption and enrichment in pickle liquor; Then collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet;
S5, the sulfuric acid that is 5-30% by mass fraction rinses described adsorption column; Described heavy metal adsorption material in described adsorption column carries out desorb operation, obtains containing nickel ion stripping liquid and the described heavy metal adsorption material being desorbed after desorb operation;
S6, the described nickel ion stripping liquid that contains that S5 is obtained carries out electrodeposition operation by direct electrowinning equipment, obtains nickel metallic plate or nickel metal powder; Meanwhile, the described heavy metal adsorption material being desorbed in adsorption column recovers absorption property after rinsing processing;
Make magnesium salts described the containing after magnesium ion solution concentrates that S4 is obtained;
Wherein, described heavy metal adsorption material is prepared by the following method:
Pretreatment: under ultrasonic field, raw material silica gel is scattered in to the hydrochloric acid solution of 7-10mol/L, adds hot reflux 20-30 hour, wherein, the mass ratio of raw material silica gel and hydrochloric acid solution is 4-6: 1; Then filter, elimination acid solution, Washing of Filter Cake, to neutral, obtains activated silica gel after 110-140 DEG C of vacuum drying;
Silica gel bonded reaction: add anhydrous dimethyl benzole soln and silylating reagent in reaction vessel, stir silylating reagent is dissolved in anhydrous dimethyl benzole soln, obtain the first solution, wherein, the mass ratio of silylating reagent and xylene solution is 5-8: 1; In activated silica gel, add dry DMF, stir and make to mix, obtain the second solution, wherein, the mass ratio of activated silica gel and DMF is 5-10: 1; Silylating reagent and activated silica gel mass ratio are 2-4: 1;
The first flow of solution is added in the second solution of reflux state, after stream adds, continues back flow reaction 10-20 hour; Filtering reacting liquid after being down to 20-30 DEG C, filter cake is used methyl alcohol and toluene wash successively, and then vacuum drying obtains described heavy metal adsorption material;
The power of described ultrasonic field is 150-250 watt;
Described vacuum drying in silica gel bonded reaction specifically comprises following three phases:
First stage: will put into freeze drying box with the filter cake after methyl alcohol and toluene wash, think the be refrigerated to-50--45 DEG C of speed cooling of 5-8 DEG C/min, the time of maintain-50--45 DEG C is 4-5 hour;
Second stage, be warming up to-10--5 DEG C of the speed of 3-6 DEG C/min, the time of maintain-10--5 DEG C is 5-7 hour;
Phase III, in putting fast and being the vacuum drying chamber of 160 DEG C-170 DEG C to temperature, obtain described heavy metal adsorption material 13-17 hour drying time;
S4 specifically comprises following three phases:
First stage: the pickle liquor that is 1.0-5.5 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 2-4mL/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 7-9mL/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
2. the method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material according to claim 1, is characterized in that, described silylating reagent is 3-ethylenediamine base propyl trimethoxy silicane or 3-Diethylenetriamine base propyl trimethoxy silicane.
3. the method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material according to claim 1, it is characterized in that, the aperture of described heavy metal adsorption material is 5.25-7.38nm, the pore volume of described heavy metal adsorption material be 1.0-1.4 cubic centimetre/gram.
4. the method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material according to claim 1, is characterized in that, described raw silicon micelle degree is 300-400 order silica gel.
5. the method that realizes the separation of nickel magnesium, enrichment, purification by heavy metal adsorption material according to claim 1, is characterized in that, S4 specifically comprises following three phases:
First stage: the pickle liquor that is 3.5-4.0 by pH pumps into the inlet of described continuous adsorption switching equipment with the speed of 3mL/min, by described adsorption column absorbed Ni ion and magnesium ion simultaneously, until described adsorption column is saturated to nickel ion absorption;
Second stage: the inlet that pickle liquor is pumped into described continuous adsorption switching equipment with the speed of 8mL/min, the continuous absorbed Ni ion of described adsorption column, and the nickel ion of new absorption replaces the magnesium ion of former absorption, until the magnesium ion of adsorption column absorption is replaced by nickel ion completely;
After second stage is processed, collect the magnesium ion solution that contains flowing out from described adsorption column liquid outlet.
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