CN102021333A - 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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Abstract
本发明公开了一种利用功能化介孔分子筛从金矿石中提纯贵金属的方法，包括如下步骤：首先将金矿石制成矿浆液，先调节矿浆液的pH值到1左右，功能化介孔分子筛放入矿浆液选择性吸附钯和铂；然后调节矿浆液pH值为2.5左右，利用功能性分子筛选择性吸附金；用3～6M盐酸分别清洗载有钯离子和铂离子的分子筛和载金分子筛，即可使贵金属脱附进入溶液中，同时分子筛重新活化。所述的功能化介孔分子筛为嫁接有胺基或巯基的硅系介孔分子筛。本发明所述的提纯方法工艺简单，贵金属吸附率高，同时具有环保优势。The invention discloses a method for purifying precious metals from gold ore by using functionalized mesoporous molecular sieves. Put in the ore slurry to selectively adsorb palladium and platinum; then adjust the pH value of the ore slurry to about 2.5, and use functional molecular sieves to selectively adsorb gold; use 3-6M hydrochloric acid to wash the molecular sieves and gold-loaded molecular sieves loaded with palladium ions and platinum ions respectively , that is, the noble metal can be desorbed into the solution, and the molecular sieve can be reactivated at the same time. The functionalized mesoporous molecular sieve is a silicon-based mesoporous molecular sieve grafted with amino groups or mercapto groups. The purification method of the invention has the advantages of simple process, high adsorption rate of precious metals and environmental protection advantages.
Description
One, technical field:
The present invention is specifically related to a kind of method of the precious metals such as gold, palladium, platinum of purifying from gold mine.
Three, background technology:
In general, bullion content is lower in the precious metal ore, and with other a large amount of metal associations.Reaching 3～5% as the content of gold in the ore, just can be called be high-quality rich gold mine, and different mines and other contained metal ingredient differences, mineral substance such as platinum, palladium, silver, molybdenum, copper, lead, zinc, tungsten in addition except that gold.Therefore, how effectively precious metal being leached from ore, to get up with other metal separation and enrichment, is the prerequisite of purifying noble metal, also is to reduce the key that precious metal refines cost.
With regard to the purification of gold, at present the most ripe the and high efficiency method in the world is a carbon slurry therapy extracting gold technology.This technology is to adopt the charcoal absorption gold when oxidation is leached.Its flow process mainly comprises: ore is through two sections closed circuit crushings, and two stage grinding is drawn stream device overflow mineral to 200 order; Enter thickener then, ore pulp is concentrated to about 45%; Enter the leaching adsorption tank through dashpot again and leach operation, the gac that adopts Exocarpium cocois (Cocos nucifera L) to make comes ADSORPTION OF GOLD, finally draws and carries a golden charcoal.After mine tailing sieves the gold that reclaims in the broken gac fully with high frequency, contain the cyanogen tail washings with the liquid chlorine processing.Methods such as parsing, electrolysis, pickling are then adopted in the recovery of gold.Resolve with high density prussiate, high basicity, carry out the gold that High Temperature High Pressure will carry in the golden charcoal and resolve, send electrolytic recovery with the solution of resolving then.Electrolyzer is that negative electrode, stainless steel are anode with the steel wool, and gold is adsorbed on the steel wool, the gac of resolving salt acid elution, and attached charcoal acid calcium and other impurity of going is regenerated in returning 600 ℃ rotary kiln at last.
Clearly, above-mentioned gold extraction technology further improves part in addition: the one, and the organic efficiency problem of gold.Adopt carbon slurry therapy extracting gold technology,, have quite a few gold to remain in mine tailing and the leach liquor because the adsorptive power of gac is not high; The 2nd, problem of environmental pollution.The carbon slurry therapy extracting gold process using hypertoxic prussiate leach and resolve, environment and human survival are brought harm; The 3rd, the simplification problem of technological process is carried golden charcoal and is resolved under High Temperature High Pressure, has improved the cost of golden purification.
Therefore, seek 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 wherein is how precious metal is separated and enrichment from other metals.
The selective adsorption precious metal, and realize that under certain conditions precious metal and separating of common metal are the effective ways that address these problems.Common molecular sieve (as SBA-15, MCM-41) is to have a novel nano functional materials that is arranged with ordered meso-porous structure, and its duct size homogeneous, the aperture is adjustable in the 2-50nm scope, and higher specific surface area is arranged, and its BET specific surface area generally can reach 1000m
2About/g.These characteristics make mesopore molecular sieve in fields such as macromole absorption, catalyzed reaction, medicament transport good application prospects be arranged.But these molecular sieves do not have adsorption to precious metal ion in the aqueous solution.
Therefore, a kind of molecular sieve that in the aqueous solution, precious metal ion is had a selective adsorption effect of design with realize precious metal separate with common metal with enrichment highly significant.
Three, summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of purify method of precious metals such as gold, palladium, platinum of functional mesoporous molecular sieve of utilizing from Gold Ore.
At above-mentioned technical problem, research thinking of the present invention is: making full use of silicon such as SBA-15, MCM-41 is the big advantage of mesopore molecular sieve specific surface area, by some absorption precious metal ion functional groups in grafting on the meso-hole structure (as-NH
2Or-SH), thus make it have the function of selective adsorption precious metal.The functional group that utilizes grafting to have to adsorb precious metal ion (as-NH
2Or-SH) mesopore molecular sieve optionally adsorbs precious metal ion, do not adsorb the characteristics of other metal ions under certain condition, effectively with precious metal ion and common metal ion isolation in acidic solution; By the pH value of regulator solution, make the precious metal ion desorption that is adsorbed on the molecular sieve simultaneously, realize the enrichment of precious metal ion and reactivating of molecular sieve.
Technical scheme of separating purifying noble metal gold, platinum, palladium from Gold Ore of the present invention is specific as follows:
Described separating and purifying method comprises the following steps:
(1) Gold Ore is carried out pre-treatment to obtain containing the pulp slurry of gold ion, platinum ion and palladium ion, regulate about the pH value to 1 of pulp slurry earlier, functional mesoporous molecular sieve is put into pulp slurry, at room temperature stirred 8～12 hours, and filtered the molecular sieve and the filtrate A that obtain being loaded with platinum ion and palladium ion; Described functional mesoporous molecular sieve is that the silicon of amido or sulfydryl is arranged is mesopore molecular sieve in grafting;
(2) clean the molecular sieve that is loaded with platinum ion and palladium ion with 3～6M hydrochloric acid, filter and obtain platinum chloride and Palladous chloride mixing solutions and the functional mesoporous molecular sieve that reactivates;
(3) the pH value of filtrate A is adjusted to about 2.5, functional mesoporous molecular sieve is put into filtrate, at room temperature stirred 8～12 hours, filter then and obtain carrying golden molecular sieve, clean a year golden molecular sieve with 3～6M hydrochloric acid, 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: with silicon is that mesopore molecular sieve places the dry toluene that contains 0.1～0.5mol/L aminopropane or propylmercaptan to reflux 12～24 hours in 100～120 ℃, filtration and dry with evaporation toluene under 150～180 ℃ of temperature then, 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 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 separation of above-mentioned gold is purified, conventional steps such as the pre-treatment of Gold Ore comprises the steps: fragmentation, ball milling, concentrate; After the pre-treatment in the gained pulp slurry except that gold ion, platinum ion, palladium ion are arranged, generally also include other metal ions such as iron, copper, nickel.When the pH value of pulp slurry is transferred to 1 left and right sides, platinum ion and palladium ion in the functional mesoporous molecular sieve energy selective adsorption pulp slurry, gold ion and other metal ions then continue to stay among the filtrate A; When the pH value of filtrate A is transferred to 2.5 left and right sides, the gold ion among the functional mesoporous molecular sieve energy selective adsorption filtrate A, thus realize that precious metal ion separates with other general ionic.Handle by 3～6M hydrochloric acid soln and be loaded with the molecular sieve of platinum ion and palladium ion and carry golden molecular sieve, preferably handle, can make to be adsorbed on precious metal desorption on the molecular sieve, enter in the solution by the 5M hydrochloric acid soln, molecular sieve reactivates simultaneously, and is reusable.As for Palladous chloride that obtains and platinum chloride mixing solutions, then can make platinum and palladium by existing technologies such as electrolysis, generally can obtain palladium and platinum respectively by the difference of CONTROLLED POTENTIAL in electrolytic process; And chlorogold solution can adopt the hydrometallurgical technology electrolysis to obtain purity is 99.99% gold.
In addition, because the functional mesoporous molecular sieve that the present invention makes all has its loading capacity for precious metal ion under different condition, those skilled in the art can determine both usage ratio according to the loading capacity of precious metal ion content in the pulp slurry and functional mesoporous molecular sieve in actual mechanical process.
Compared with prior art, the present invention adopts the functional mesoporous molecular sieve of energy selective adsorption precious metal to purify and reclaims precious metal, and technology is simple, and the acidity of only adjusting solution simply can reach the purpose of precious metal ion separation, parsing and enrichment; The adsorption efficiency height of functional mesoporous molecular sieve, its ADSORPTION OF GOLD ionic efficient reaches more than 98%, and the efficient of absorption palladium ion and platinum ion is also more than 90%; Purification of the present invention and removal process do not relate to 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 thereto:
Embodiment one: utilize MCM-41 molecular sieve grafting functional group and the application in SEPARATION OF GOLD and palladium
1, the grafting of functional group
2.5g MCM-41 powder is placed in contains 0.1mol/L aminopropane (C
3H
7NH
2) in 250 milliliters the dry toluene, under 120 ℃ of temperature, refluxed 18 hours grafting functional group-NH on molecular sieve
2, filter then and mention the MCM-41 powder, and this powder drying under 110 ℃ of temperature was obtained NH to evaporate complete toluene in 12 hours
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 that makes
2The physical and chemical performance of-MCM-41, SH-MCM-41 sees Table 1.
2, the selective adsorption of precious metal and desorption
With 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 the molecular sieve that 2 hours after-filtration go out to be loaded with precious metal ion, measure the content of GOLD FROM PLATING SOLUTION, palladium ion.Clean the molecular sieve that is loaded with precious metal ion with 5M HCl solution then, only contained PdCl
3The solution and the molecular sieve of resolving.Again functional molecular sieve is put into the solution that contains after last the filtration, the pH value of solution is adjusted to 2.5, equally at room temperature stir the molecular sieve that 2 hours after-filtration are loaded with gold ion, the content of mensuration GOLD FROM PLATING SOLUTION, palladium ion.And clean the molecular sieve be 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 sees Table 1.
Table 1: physics, chemistry and the absorption property of mesopore molecular sieve before and after the 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
2The cryogenic absorption test-results can be seen ,-NH
2Or-in the grafting, also successful grafting on the mesoporous inwall of molecular sieve makes the internal diameter of mesopore molecular sieve diminish to the SH group on the molecular sieve surface, as in the grafting-NH
2Behind the group, internal diameter reduces to 2.92nm from 3.09nm, and like this, the specific surface area of molecular sieve reduces to some extent before and after the grafting functional group, and the 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, have the ability of the strong efficient absorption precious metal of selectivity.Can see NH from the adsorption test result
2-MCM-41 molecular sieve almost can adsorbent solution in all precious metal ions, 100% gold ion and 99.2% palladium ion are adsorbed in the solution; And simply the pH of solution is adjusted to 2.5 from 1.0, just can realize separating of gold and palladium ion preferably.With NH
2-MCM-41 molecular sieve is compared, and the adsorptive power of SH-MCM-41 molecular sieve is a bit weaker.Adopt the SH-MCM-41 molecular sieve, 99.3% gold ion can be adsorbed and separate effectively with 91.9% palladium ion in the solution.
Embodiment two: utilize SBA-15 molecular sieve grafting functional group and the application in SEPARATION OF GOLD and platinum
1, the grafting of functional group
2.5g SBA-15 powder is placed in contains 0.1mol/L aminopropane (C
3H
7NH
2) in 250 milliliters the dry toluene, under 120 ℃ of temperature, refluxed 18 hours grafting functional group-NH on molecular sieve
2, filter then and mention the SBA-15 powder, and this powder drying under 110 ℃ of temperature was obtained NH to evaporate complete toluene in 12 hours
2-SBA-15 selective adsorption precious metal functional molecular sieve.
2, the gold, platinum selective adsorption with separate
With 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 the functional molecular sieve that 2 hours after-filtration go out to be loaded with gold and platinum ion, the content of mensuration GOLD FROM PLATING SOLUTION, platinum ion.Clean the molecular sieve that is loaded with precious metal ion with 5M HCl solution then, only contained PtCl
3The solution and the molecular sieve of resolving.Again the functional molecular sieve is put into the solution that contains after the last time filters, the pH value of solution is adjusted to 2.5, equally at room temperature stir the molecular sieve that 2 hours after-filtration are loaded with gold ion, measure the content of GOLD FROM PLATING SOLUTION, platinum ion, and clean the molecular sieve be loaded with gold ion with 5M HCl solution, obtain AuCl
3Solution and molecular sieve, absorption result sees Table 2.The result shows, by the pH value of regulator solution, NH
2-SBA-15 reaches the purpose of separation and enrichment gold and platinum.The molecular sieve that 5M HCl solution washes down can utilize again.
Table 2: physicals and the fractionation by adsorption of SBA-15 before and after the grafting functional group
Claims (4)
1. the method for a purifying noble metal from Gold Ore comprises the steps:
(1) Gold Ore is carried out pre-treatment to obtain containing the pulp slurry of gold ion, platinum ion and palladium ion, regulate about the pH value to 1 of pulp slurry earlier, functional mesoporous molecular sieve is put into pulp slurry, at room temperature stirred 8～12 hours, and filtered the molecular sieve and the filtrate A that obtain being loaded with platinum ion and palladium ion; Described functional mesoporous molecular sieve is that the silicon of amido or sulfydryl is arranged is mesopore molecular sieve in grafting;
(2) clean the molecular sieve that is loaded with platinum ion and palladium ion with 3～6M hydrochloric acid, filter and obtain platinum chloride and Palladous chloride mixing solutions and the functional mesoporous molecular sieve that reactivates;
(3) the pH value of filtrate A is adjusted to about 2.5, functional mesoporous molecular sieve is put into filtrate, at room temperature stirred 8～12 hours, filter then and obtain carrying golden molecular sieve, clean a year golden molecular sieve with 3～6M hydrochloric acid, filter the functional mesoporous molecular sieve that obtains chlorogold solution and reactivate.
2. 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: with silicon is that mesopore molecular sieve places the dry toluene that contains 0.1～0.5mol/L aminopropane or propylmercaptan to reflux 12～24 hours in 100～120 ℃, filter then and drying under 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.
3. 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.
4. as claimed in claim 1 from Gold Ore the method for purifying noble metal, the molecular sieve that it is characterized in that using 5M hydrochloric acid to clean and be loaded with platinum ion, palladium ion and carry golden molecular sieve.
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| 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 |
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| CN1635168A (en) * | 2003-12-30 | 2005-07-06 | 邹贵田 | Process for extracting gold, platinum and palladium from goldmine |
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| CN103526021A (en) * | 2013-10-11 | 2014-01-22 | 南丹县吉朗铟业有限公司 | Cleansing and cobalt-removing method for zinc smelting leachate and scavenging agent used therein |
| CN103526021B (en) * | 2013-10-11 | 2015-08-12 | 南丹县吉朗铟业有限公司 | A kind of zinc abstraction purification of leaching liquor is except cobalt method and scavenging agent used thereof |
| CN103611625A (en) * | 2013-12-06 | 2014-03-05 | 林平生 | Flotation tailing retreatment system |
| CN103981368A (en) * | 2014-05-22 | 2014-08-13 | 陕西省环境科学研究院 | Method for separating and recycling lithium in waste lithium ion battery by using mesoporous molecular sieve |
| 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 preparation method and product thereof for adsorbing palladium ions |
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