CN102021333B - Method to purify precious metals from gold ore using functional mesoporous molecular sieve - Google Patents
Method to purify precious metals from gold ore using functional mesoporous molecular sieve Download PDFInfo
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 103
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 51
- 239000010931 gold Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000010970 precious metal Substances 0.000 title abstract description 45
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title abstract description 36
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 36
- -1 palladium ions Chemical class 0.000 claims abstract description 31
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 claims description 17
- 239000013055 pulp slurry Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 125000003368 amide group Chemical group 0.000 claims description 7
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 7
- 229910000510 noble metal Inorganic materials 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 4
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- SUVIGLJNEAMWEG-UHFFFAOYSA-N propane-1-thiol Chemical compound CCCS SUVIGLJNEAMWEG-UHFFFAOYSA-N 0.000 claims description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 17
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- 229910052763 palladium Inorganic materials 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 4
- 239000002002 slurry Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract 1
- 125000003396 thiol group Chemical class [H]S* 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 35
- 238000001179 sorption measurement Methods 0.000 description 26
- 229910021645 metal ion Inorganic materials 0.000 description 22
- 125000000524 functional group Chemical group 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 3
- 230000000274 adsorptive effect Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910003803 Gold(III) chloride Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 101150003085 Pdcl gene Proteins 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical compound Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 2
- 229940076131 gold trichloride Drugs 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc 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
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method to purify precious metals from gold ore using functional mesoporous molecular sieve, including the following steps: slurrying the gold ore, adjusting pH value of the slurry to about 1, adding functional mesoporous molecular sieve into the slurry to selectively adsorb palladium and platinum; adjusting the pH value of the slurry to about 2.5 to allow the functional mesoporous molecular sieve to selectively absorb gold; washing the molecular sieve carrying palladium ions and platinum ions, and molecular sieve carrying gold ions with hydrochloric acid, the concentration of which is in the range of from 3 to 6 M, thus making the precious metals desorbed into the solution and molecular sieves reactivated simultaneously. The functional mesoporous molecular sieve is a silicon mesoporous sieve grafted with amino or thiol. The purification method in the invention is characterized by simple process, high absorption rate of precious metals and environmental protection.
Description
One, technical field:
The present invention be specifically related to a kind of from gold mine the method for the precious metal such as purifying gold, palladium, platinum.
Three, background technology:
In general, in precious metal ore, bullion content is lower, and with a large amount of other metal associations.As the content of Gold in Ores reaches 3～5%, just can be called be the rich gold mine of high-quality, and different mine and other contained metal ingredient differences also have the mineral substance such as platinum, palladium, silver, molybdenum, copper, lead, zinc, tungsten except gold.Therefore, how effectively precious metal being leached, to be got up with other metal separation and enrichment from ore, is the prerequisite of purifying noble metal, is also the key that reduces precious metal refinement cost.
With regard to golden purification, at present the most ripe the and high efficiency method in the world is gold extraction by CIP process.This technique is in Oxidation Leaching, to adopt activated carbon adsorption of gold.Its flow process mainly comprises: ore is through two sections of closed circuit crushings, and two stage grinding, draws stream device overflow mineral to 200 order; Then enter thickener, by slurry concentrating to 45% left and right; Enter leaching adsorption tank through dashpot again and leach operation, the gac that adopts Exocarpium cocois (Cocos nucifera L) to make carrys out ADSORPTION OF GOLD, finally draws gold loaded carbon.Mine tailing sieves completely with high frequency after the gold reclaiming in broken gac, processes and contains cyanogen tail washings with liquid chlorine.The recovery of gold adopts the methods such as parsing, electrolysis, pickling.Resolve with high density prussiate, high alkalinity, carry out High Temperature High Pressure the gold in gold loaded carbon is resolved, then send electrolytic recovery by the solution of resolving.Electrolyzer take steel wool as negative electrode, stainless steel is anode, and gold is adsorbed on steel wool, the gac of resolving salt acid elution, attached charcoal acid calcium and other impurity of going is finally regenerated in the rotary kiln that returns 600 ℃.
Clearly, above-mentioned gold extraction technology further improves part in addition: the one, and golden organic efficiency problem.Adopt gold extraction by CIP process, because the adsorptive power of gac is not high, have quite a few gold to remain in mine tailing and leach liquor; The 2nd, problem of environmental pollution.Gold extraction by CIP process has adopted hypertoxic prussiate to leach and resolve, and environment and human survival are brought to harm; The 3rd, the simplification problem of technological process, gold loaded carbon is resolved under High Temperature High Pressure, has improved the cost of golden purification.
Therefore, find a kind of simple, environmental protection, precious metal is purified and recovery method is those skilled in the art's problem demanding prompt solutions efficiently, and key is wherein how precious metal to be separated from other metals and enrichment.
Selective adsorption precious metal, and to realize under certain conditions precious metal be the effective ways that address these problems with separating of common metal.Common molecular sieve (as SBA-15, MCM-41) has the Nano-function thin films that is arranged with ordered meso-porous structure, its duct size homogeneous, aperture is adjustable within the scope of 2-50nm, have higher specific surface area, its BET specific surface area generally can reach 1000m
2/ g left and right.These characteristics make mesopore molecular sieve have good application prospect in fields such as macromolecules adsorption, catalyzed reaction, medicament transport.But these molecular sieves do not have adsorption to precious metal ion in the aqueous solution.
Therefore, design a kind of molecular sieve that in the aqueous solution, precious metal ion is had to a selective adsorption effect with realize precious metal and separate with common metal and enrichment highly significant.
Three, summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of method of utilizing functional mesoporous molecular sieve precious metal such as purifying gold, palladium, platinum from Gold Ore.
For above-mentioned technical problem, Research Thinking of the present invention is: making full use of the silicon such as SBA-15, MCM-41 is the advantage that mesopore molecular sieve specific surface area is large, by some absorption precious metal ion functional groups in grafting on meso-hole structure (as-NH
2or-SH), thereby make it have the function of selective adsorption precious metal.Utilize grafting to have to adsorb the functional group of precious metal ion (as-NH
2or-SH) mesopore molecular sieve in acidic solution, optionally adsorb precious metal ion, the feature of not adsorbing other metal ions under certain condition, effectively by precious metal ion and common metal ion isolation; By the pH value of regulator solution, make to be adsorbed on the precious metal ion desorption on molecular sieve simultaneously, realize the enrichment of precious metal ion and reactivating of molecular sieve.
Of the present invention from Gold Ore the technical scheme of separating-purifying Precious Metals-Gold, platinum, palladium specific as follows:
Described separating and purifying method comprises the following steps:
(1) Gold Ore is carried out to the pulp slurry of pre-treatment to obtain containing gold ion, platinum ion and palladium ion, first regulate the pH value of pulp slurry to 1 left and right, functional mesoporous molecular sieve is put into pulp slurry, at room temperature stir 8～12 hours, filter the molecular sieve and the filtrate A that obtain being loaded with platinum ion and palladium ion; Described functional mesoporous molecular sieve is that to have the silicon of amido or sulfydryl be mesopore molecular sieve in grafting;
(2) be loaded with the molecular sieve of platinum ion and palladium ion with 3～6M hydrochloric acid cleaning, filter the functional mesoporous molecular sieve that obtains platinum chloride and Palladous chloride mixing solutions and reactivate;
(3) the pH value of filtrate A is adjusted to 2.5 left and right, functional mesoporous molecular sieve is put into filtrate, at room temperature stir 8～12 hours, then filter and obtain carrying golden molecular sieve, carry golden molecular sieve with 3～6M hydrochloric acid cleaning, filter the functional mesoporous molecular sieve that obtains chlorogold solution and reactivate.
Functional mesoporous molecular sieve of the present invention, can make by the following method: be that mesopore molecular sieve is placed in the dry toluene that contains 0.1～0.5mol/L aminopropane or propylmercaptan in 100～120 ℃ of backflows 12～24 hours by silicon, then filter and be dried at 150～180 ℃ of temperature with evaporation toluene, obtain amido or mercapto-functionalized mesopore molecular sieve, i.e. it is mesopore molecular sieve that grafting has the silicon of amido or sulfydryl.
Described silicon is the preferred SBA-15 of mesopore molecular sieve or MCM-41 mesopore molecular sieve, more preferably MCM-41 mesopore molecular sieve.
Functional mesoporous molecular sieve of the present invention, energy highly selective ADSORPTION OF GOLD ion, platinum ion and palladium ion under acidic conditions, and the adsorptive power of functional amido mesopore molecular sieve is more better compared to mercapto-functionalized mesopore molecular sieve.
In the separating-purifying of above-mentioned gold, the pre-treatment of Gold Ore comprises the steps: fragmentation, ball milling, the conventional steps such as concentrated; After pre-treatment in gained pulp slurry apart from beyond gold ion, platinum ion, palladium ion, generally also include other metal ions such as iron, copper, nickel.In the time that the pH value of pulp slurry is transferred to 1 left and right, platinum ion and palladium ion in functional mesoporous molecular sieve energy selective adsorption pulp slurry, gold ion and other metal ions continue to stay in filtrate A; In the time that the pH value of filtrate A is transferred to 2.5 left and right, the gold ion in functional mesoporous molecular sieve energy selective adsorption filtrate A, thus realize separating of precious metal ion and other general ions.And be loaded with the molecular sieve of platinum ion and palladium ion and carry golden molecular sieve by the processing of 3～6M hydrochloric acid soln, preferably, by the processing of 5M hydrochloric acid soln, can make to be adsorbed on the precious metal desorption on molecular sieve, enter in solution, molecular sieve reactivates simultaneously, reusable.As for the Palladous chloride obtaining and platinum chloride mixing solutions, can make platinum and palladium by existing techniques such as electrolysis, generally can obtain respectively palladium and platinum by the difference of controlling current potential in electrolytic process; Be 99.99% gold and chlorogold solution can adopt hydrometallurgical technology electrolysis to obtain purity.
In addition, the functional mesoporous molecular sieve making due to the present invention all has its loading capacity for precious metal ion under different condition, those skilled in the art, in actual mechanical process, can determine according to the loading capacity of the precious metal ion content in pulp slurry and functional mesoporous molecular sieve both usage ratio.
Compared with prior art, the present invention adopts the functional mesoporous molecular sieve of energy selective adsorption precious metal purify and reclaim precious metal, and technique is simple, and the acidity of only adjusting simply solution can reach the object of precious metal ion separation, parsing and enrichment; The adsorption efficiency of functional mesoporous molecular sieve is high, and the efficiency of its ADSORPTION OF GOLD ion reaches more than 98%, and the efficiency of absorption palladium ion and platinum ion is also more than 90%; Purification of the present invention and removal process do not relate to the highly toxic substances such as prussiate, have environment-friendly advantage.
Four, embodiment
With specific embodiment, technical scheme of the present invention is described further below, but protection scope of the present invention is not limited to this:
Embodiment mono-: utilize MCM-41 molecular sieve grafting functional group the application in SEPARATION OF GOLD and palladium
1, the grafting of functional group
2.5g MCM-41 powder is placed in and contains 0.1mol/L aminopropane (C
3h
7nH
2) in the dry toluene of 250 milliliters, at 120 ℃ of temperature, reflux 18 hours, grafting functional group-NH on molecular sieve
2, then filter and mention MCM-41 powder, and this powder is dried to 12 hours to evaporate complete toluene at 110 ℃ of temperature, obtain NH
2-MCM-41 selective adsorption precious metal functional molecular sieve.Adopt the grafting functional group-SH that uses the same method, obtain SH-MCM-41 selective adsorption precious metal functional molecular sieve.The NH making
2the physical and chemical performance of-MCM-41, SH-MCM-41 is in table 1.
2, the selective adsorption of precious metal and desorption
By 50g NH
2-MCM-41 selective adsorption precious metal functional molecular sieve is put into 2.5 liters and is contained 276g gold trichloride (AuCl
3) and 59g Palladous chloride (PdCl
3) solution in, the pH value of solution is adjusted to 1.0, at room temperature stir after 2 hours and filter out the molecular sieve that is loaded with precious metal ion, measure the content of GOLD FROM PLATING SOLUTION, palladium ion.Then clean with 5M HCl solution the molecular sieve that is loaded with precious metal ion, obtain only containing PdCl
3solution and the molecular sieve of resolving.Again functional molecular sieve is put into the solution containing after last filtration, the pH value of solution is adjusted to 2.5, equally at room temperature stir after 2 hours and filter the molecular sieve that is loaded with gold ion, measure the content of GOLD FROM PLATING SOLUTION, palladium ion.And clean the molecular sieve that is loaded with gold ion with 5M HCl solution, obtain AuCl
3solution and molecular sieve, molecular sieve can utilize again.
Equally, to adopt SH-MCM-41 be the selective adsorption of carrying out precious metal of selective adsorption precious metal functional molecular sieve and separate.
NH
2the absorption property of-MCM-41, SH-MCM-41 is in table 1.
Table 1: physics, chemistry and the absorption property of mesopore molecular sieve before and after grafting functional group
Table 1 is the situation of physics, chemistry and the absorption precious metal ion of three kinds of differing molecular sieves.From N
2cryogenic absorption test-results can be seen ,-NH
2or-SH group is on molecular sieve surface in grafting, also successful grafting on the mesoporous inwall of molecular sieve, diminishes the internal diameter of mesopore molecular sieve, as in grafting-NH
2after group, internal diameter reduces to 2.92nm from 3.09nm, and like this, before and after grafting functional group, the specific surface area of molecular sieve reduces to some extent, and BET specific surface is from 1140m
2/ g reduces to 774m
2/ g, but do not have the molecular sieve of grafting functional group not possess the effect of absorption precious metal ion, and grafting the molecular sieve of functional group in acidic solution, there is the ability of the stronger efficient adsorption precious metal of selectivity.Can see NH from adsorption test result
2-MCM-41 molecular sieve almost can adsorbent solution in all precious metal ions, in solution, 100% gold ion and 99.2% palladium ion are adsorbed; And simply the pH of solution is adjusted to 2.5 from 1.0, just can realize preferably separating of gold and palladium ion.With NH
2-MCM-41 molecular sieve is compared, and the adsorptive power of SH-MCM-41 molecular sieve is a bit weaker.Adopt SH-MCM-41 molecular sieve, in solution, 99.3% gold ion can effectively be adsorbed and separate with 91.9% palladium ion.
Embodiment bis-: utilize SBA-15 molecular sieve grafting functional group the application in SEPARATION OF GOLD and platinum
1, the grafting of functional group
2.5g SBA-15 powder is placed in and contains 0.1mol/L aminopropane (C
3h
7nH
2) in the dry toluene of 250 milliliters, at 120 ℃ of temperature, reflux 18 hours, grafting functional group-NH on molecular sieve
2, then filter and mention SBA-15 powder, and this powder is dried to 12 hours to evaporate complete toluene at 110 ℃ of temperature, obtain NH
2-SBA-15 selective adsorption precious metal functional molecular sieve.
2, gold, platinum selective adsorption with separate
By 25g NH
2-SBA-15 selective adsorption precious metal functional molecular sieve is put into 2 liters and is contained 76g gold trichloride (AuCl
3) and 24g platinum chloride (PtCl
3) solution in, the pH value of solution is adjusted to 1.0, at room temperature stir and after 2 hours, filter out the functional molecular sieve that is loaded with gold and platinum ion, the content of mensuration GOLD FROM PLATING SOLUTION, platinum ion.Then clean with 5M HCl solution the molecular sieve that is loaded with precious metal ion, obtain only containing PtCl
3solution and the molecular sieve of resolving.Again functional molecular sieve is put into the solution containing after last filtration, the pH value of solution is adjusted to 2.5, equally at room temperature stir after 2 hours and to filter the molecular sieve that is loaded with gold ion, measure the content of GOLD FROM PLATING SOLUTION, platinum ion, and clean the molecular sieve that is loaded with gold ion with 5M HCl solution, obtain AuCl
3solution and molecular sieve, absorption result is in table 2.Result shows, by the pH value of regulator solution, NH
2-SBA-15 reaches the object of separation and Concentration of Gold and platinum.
The molecular sieve that 5M HCl solution washes down can recycle.
Table 2: physicals and the fractionation by adsorption of SBA-15 before and after grafting functional group
Claims (4)
1. a method for purifying noble metal from Gold Ore, comprises the steps:
(1) Gold Ore is carried out to the pulp slurry of pre-treatment to obtain containing gold ion, platinum ion and palladium ion, first regulate the pH value to 1 of pulp slurry, functional mesoporous molecular sieve is put into pulp slurry, at room temperature stir 8～12 hours, filter the molecular sieve and the filtrate A that obtain being loaded with platinum ion and palladium ion; Described functional mesoporous molecular sieve is that to have the silicon of amido or sulfydryl be mesopore molecular sieve in grafting;
(2) be loaded with the molecular sieve of platinum ion and palladium ion with 3～6M hydrochloric acid cleaning, filter the functional mesoporous molecular sieve that obtains platinum chloride and Palladous chloride mixing solutions and reactivate;
(3) the pH value of filtrate A is adjusted to 2.5, functional mesoporous molecular sieve is put into filtrate, at room temperature stir 8～12 hours, then filter and obtain carrying golden molecular sieve, carry golden molecular sieve with 3～6M hydrochloric acid cleaning, filter the functional mesoporous molecular sieve that obtains chlorogold solution and reactivate.
As claimed in claim 1 from Gold Ore the method for purifying noble metal, it is characterized in that described functional mesoporous molecular sieve makes by the following method: be that mesopore molecular sieve is placed in the dry toluene that contains 0.1～0.5mol/L aminopropane or propylmercaptan in 100～120 ℃ of backflows 12～24 hours by silicon, then filter and be dried at 150～180 ℃ of temperature, obtain amido or mercapto-functionalized mesopore molecular sieve, i.e. it is mesopore molecular sieve that grafting has the silicon of amido or sulfydryl.
As claimed in claim 1 or 2 from Gold Ore the method for purifying noble metal, it is characterized in that described silicon is that mesopore molecular sieve is SBA-15 or MCM-41 mesopore molecular sieve.
As claimed in claim 1 from Gold Ore the method for purifying noble metal, it is characterized in that the molecular sieve that uses 5M hydrochloric acid cleaning to be loaded with platinum ion, palladium ion and carry golden molecular sieve.
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| CN103981368B (en) * | 2014-05-22 | 2016-04-27 | 陕西省环境科学研究院 | A kind of method of lithium in mesopore molecular sieve separation and recovery waste and old lithium ion battery |
| CN108251656A (en) * | 2016-12-29 | 2018-07-06 | 江西瑞林稀贵金属科技有限公司 | The method for extracting gold, platinum and palladium in electronic waste copper anode mud |
| CN107226478A (en) * | 2017-06-23 | 2017-10-03 | 太仓沪试试剂有限公司 | A kind of purification process of photosensitive material silver nitrate |
| CN110394153A (en) * | 2019-07-05 | 2019-11-01 | 重庆科技学院 | A kind of composite material and preparation method thereof and products thereof for adsorbing palladium ion |
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