CN1400322A - Method for separating platinum, palladium and iridium - Google Patents
Method for separating platinum, palladium and iridium Download PDFInfo
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Abstract
A method for separating platinum, palladium and iridium gold is used for separating noble metal elements from metal materials. It is characterized by that it uses weak base styrene series tertiary amine type anion exchange resin as fixed phase, uses hydrochloric acid medium as mobile phase to implement component separation of platinum, palladium, iridium and gold and base metal, adopts dilute hydrochloric acid, water and EDTA to elute base metal, uses thiocyanate + ascorbic acid solution and methyl isobutyl ketone and NH balanced by hydrochloric acid4Cl+NH3·H2And (3) selectively leaching iridium, gold, palladium and platinum by using an O solution, HCl + thiourea and a methanol solution, and regenerating the chromatographic column by using hydrochloric acid. The separation degree is good, and the baseline separation is achieved; the recovery rate is over 95 percent; simple operation, low cost, repeated use of resin and wide application range.
Description
Affiliated technical field
A kind of method of separating platinum palladium iraurita, relate to a kind of from contain noble metal materials during the above-mentioned precious metal of separation and Extraction, be used for precious metal and base metal separate and precious metal element between the method that is separated from each other.
Background technology
Particularly platinum metals physics, chemical property are very similar owing to precious metal, and valence state is changeable, and nature difference is very big between the different valence state, and therefore, the precious metal separation is the difficult problem in hydrometallurgy and the chemical analysis always.At present, domestic and international separation for precious metal has the precipitator method, solvent extration, liquid-film method, extration resin method, ion-exchange and absorption method.These methods respectively have its characteristics:
(1) precipitator method are to utilize the institute of various precious metals inherent physics own, chemical property and the separation and Extraction of carrying out, this method research the earliest, thereby become the traditional method of widespread use, but owing to adopt periodical operation, repeated multiple times crystallization, process is tediously long, yield is low, cost is high, troublesome poeration, labour intensity are big.
(2) solvent extration has advantages such as selectivity is good, the rate of recovery is high, operation is continuous, the precious metal smelting factory that has part has adopted the extracting and separating flow process, but it is expensive mostly that the shortcoming of this technology is employed extraction agent price, organic solvent is more volatile, environmental pollution is serious, and another ubiquitous problem is to need to adjust feed liquid to form before each precious metal of extraction in the precious metal extraction, and the multi-stage solvent extraction process is also more loaded down with trivial details, sometimes also easily form third phase, back extraction difficulty.
(3) liquid membrane separation method melts extraction, back extraction in one, has higher mass transfer velocity and flux, selectivity and separation efficiency preferably, and bigger cycles of concentration, characteristics such as simple to operate are specially adapted to the processing of low concentration solution.The research of liquid film technology in precious metal separates is subject to people's attention day by day with application.But this technology practical application is less, and is used for multiple element and is separated from each other difficulty simultaneously.
(4) the extration resin method combines easy, the high efficiency of solvent-extracted highly selective and ion-exchange, synthetic simpler than ion exchange resin, cost is low, environmental pollution is littler than solvent extraction, and therefore, this technology also is one of more promising efficient separation method of precious metal Separation Research.But this technology should solve problems such as mechanical strength of resin, extraction agent loss, and practical application at present seldom.
(5) ion-exchange and absorption method since separation efficiency height, equipment with simple to operate, resin and sorbent material is renewable and use repeatedly, and environmental pollution is little, it is a kind of " the green extraction " technology, therefore it is a kind of important method for separating and concentrating, and the application in hydrometallurgy is separated more and more is subject to people's attention.But this technology exists following defective: a. that the ion of oppositely charged in the feed liquid is had higher selectivity, but ion for like charges, separation selectivity is poor, for the very similar precious metal element of physics, chemical property, realizes that the multielement separating difficulty is big simultaneously; B. exchange or adsorptive power are strong more, selectivity is poor more, adsorb firm more, resin or sorbent material that precious metal is arranged in conjunction with firm load, leaching regeneration is difficulty relatively, and having to of having adopts the method for burning resin to reclaim wherein precious metal, and then lost repeatedly used superiority, increase tooling cost, restricted the practical application of this technology.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists in the above-mentioned prior art in order to overcome, and a kind of easy and simple to handle, separation efficiency is high, environmental pollution is little, cost is low precious metal separation method is provided.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method of separating platinum palladium iraurita comprises that precious metal and base metal are separated from each other from, precious metal, is characterized in that:
A. material is made the feed liquid that the hydrochloric acid medium total concn is 0.5mol/L～3mol/L, with weakly alkaline polystyrene tertiary amine-type anionite-exchange resin is the chromatographic stationary phase, with above-mentioned feed liquid is the moving phase sample introduction, moving phase linear rate of flow≤15cm/min during sample introduction, gold, platinum, palladium, iridium, bismuth and part are plumbous, zinc, antimony is kept by resin, most of base metal flows out, replace the lead that drip washing is retained with 0.1mol/L～0.5mol/L dilute hydrochloric acid and water, zinc, elements such as antimony, with slightly acidic EDTA solution drip washing bismuth, moving phase linear rate of flow≤10cm/min during drip washing, through above-mentioned sample introduction and drip washing step, Precious Metals-Gold, platinum, palladium, iridium separates with base metal;
B. for the precious metal that is adsorbed, the control phase line flow velocity≤6cm/min that flows, adopt selectively eluent by following order stepwise elution: iridium is with being selected from 0.5mol/L～2mol/L NH
4A kind of solution drip washing in SCN and KSCN+5g/L～40g/L xitix; The mibk drip washing that gold is crossed with the salt acid balance, mibk and concentrated hydrochloric acid volume ratio are 10/1～3/1 during balance; Palladium 0.5mol/L～2mol/L NH
4Cl+1mol～3mol/L NH
3H
2The drip washing of O solution; Platinum 0.2mol/L～0.8mol/L HCl+40g/L～70g/L thiocarbamide+40%～60% methanol solution drip washing; Chromatographic column 2mol/L～6mol/L regeneration of hydrochloric acid.
According to claims 1 described method, it is characterized in that: material is made the feed liquid that the hydrochloric acid medium total concn is 1mol/L, the chromatographic column stationary phase is a weakly alkaline polystyrene tertiary amine-type anionite-exchange resin, and expensive, base metal is finished when replacing drip washing and the drip washing of 0.12mol/L HCl+1g/L EDTA solution at sample introduction with 0.1mol/～0.5mol/L dilute hydrochloric acid, water.
According to claims 1 described method, it is characterized in that: precious metal iridium, gold, palladium, platinum are separated from each other by stepwise elution and finish, and tool optionally eluent is: 1mol/L NH
4SCN or KSCN+20g/L xitix drip washing iridium; With the mibk drip washing gold that the salt acid balance is crossed, during balance, mibk and concentrated hydrochloric acid volume ratio are 5/1; 1mol/LNH
4Cl+2mol/L NH
3H
2O drip washing palladium; 0.5mol/L HCl+50g/L thiocarbamide+50% methyl alcohol drip washing platinum; 3mol/L hydrochloric acid makes chromatographic column regeneration.
Method of the present invention, characteristics according to noble metal materials, adopt diverse ways to handle respectively, platinum palladium concentrate, the anode sludge adopt chloroazotic acid to decompose, blister copper, precious metal alloys adopt rare nitric acid to decompose then and handle with chloroazotic acid, preparation precious metal feed liquid, and this feed liquid is after method of the present invention is separated, realize that gold, platinum, palladium, iridium separate with base metal, are separated from each other between the precious metal.
This method resolution is good, all reaches baseline separation; Rate of recovery height is all more than 95%; Required time is short, can finish a separation process in the 10h; Easy and simple to handle, cost is low, resin can use repeatedly; Applied widely, can be used for the separation and Extraction of precious metal in the multiple resources such as platinum palladium concentrate, the anode sludge, blister copper, precious metal alloys.
Description of drawings
Fig. 1 is the process flow sheet of method of the present invention.
Fig. 2 is the separating platinum palladium concentrate principal element elution curve of embodiment 1.
Fig. 3 is the separating copper anode principal element elution curve (I) of embodiment 2.
Fig. 4 is the separating copper anode principal element elution curve (II) of embodiment 2.
Fig. 5 is the separation blister copper principal element elution curve (I) of embodiment 3.
Fig. 6 is the separation blister copper principal element elution curve (II) of embodiment 3.
Fig. 7 is the separate precious metal alloy principal element elution curve (I) of embodiment 4.
Fig. 8 is the separate precious metal alloy principal element elution curve (II) of embodiment 4.
Embodiment
Below in conjunction with example method of the present invention is described further.
Characteristics according to noble metal materials, adopt diverse ways to handle respectively according to the material composition, platinum palladium concentrate, the anode sludge adopts chloroazotic acid to decompose, blister copper, precious metal alloys adopt rare nitric acid to decompose and handle with chloroazotic acid then, preparation precious metal feed liquid, a. material is made the feed liquid that the hydrochloric acid medium total concn is 0.5mol/L～3mol/L, with weakly alkaline polystyrene tertiary amine-type anionite-exchange resin is the chromatographic stationary phase, with above-mentioned feed liquid is the moving phase sample introduction, moving phase linear rate of flow≤15cm/min during sample introduction, gold, platinum, palladium, iridium, bismuth and part are plumbous, zinc, antimony is kept by resin, most of base metal flows out, replace the lead that drip washing is retained with 0.1mol/L～0.5mol/L dilute hydrochloric acid and water, zinc, elements such as antimony, with slightly acidic EDTA solution drip washing bismuth, moving phase linear rate of flow≤10cm/min during drip washing is through above-mentioned sample introduction and drip washing step, Precious Metals-Gold, platinum, palladium, iridium separates with base metal; B. for the precious metal that is adsorbed, the control phase line flow velocity≤6cm/min that flows, adopt selectively eluent by following order stepwise elution: iridium is with 0.5mol/L～2mol/L NH
4SCN or KSCN+5g/L～40g/L ascorbic acid solution drip washing; The mibk drip washing that gold is crossed with the salt acid balance, mibk and concentrated hydrochloric acid volume ratio are 10/1～3/1 during balance; Palladium 0.5mol/L～2mol/L NH
4Cl+1mol/L～3mol/L NH
3H
2The drip washing of O solution; Platinum 0.2mol/L～0.8mol/L HCl+40g/L～70g/L thiocarbamide+40%～60% methanol solution drip washing; Chromatographic column 2mol/L～6mol/L regeneration of hydrochloric acid.C. sample introduction feed liquid hydrochloric acid medium optimum concn is 1mol/L; Slightly acidic EDTA solution top condition is 0.12mol/L HCl+1g/L EDTA; Iridium, gold, palladium, platinum stepwise elution and chromatographic column regeneration top condition are respectively: 1mol/L NH
4SCN or KSCN+20g/L xitix, with the mibk that the salt acid balance is crossed, mibk and concentrated hydrochloric acid volume ratio are 5/1 during balance, 1mol/L NH
4Cl+2mol/L NH
3H
2O, 0.5mol/L HCl+50g/L thiocarbamide+50% methyl alcohol, 3mol/L hydrochloric acid; Sample introduction and rate of flow in rinse are good more more slowly, and sample introduction linear rate of flow≤15cm/min, base metal drip washing linear rate of flow≤10cm/min, precious metal drip washing linear rate of flow≤6cm/min all obtain better separating effect.
Method resolution height of the present invention all reaches baseline separation; Rate of recovery height is all more than 90%; Required time is short, can finish a separation process in the 10h; Easy and simple to handle, cost is low, resin can use repeatedly; Applied widely, can be used for the separation and Extraction of precious metal in the multiple resources such as platinum palladium concentrate, the anode sludge, blister copper, lead bullion, precious metal alloys.
Platinum palladium concentrate separates
It is higher to contain palladium, gold, platinum in the platinum palladium concentrate, tests with the sample that contains palladium 38009g/t, golden 37611g/t, platinum 3821g/t.In the test, the concentrate treatment capacity is 1g because rhodium, iridium, cobalt, nickel, zinc content are lower, for the investigation method to the separating effect between expensive, base metal and the precious metal, in feed liquid, added 5mg iridium, 2mg rhodium, 5mg cobalt, 5mg nickel, 5mg zinc; Chromatographic column is φ 11mm * 150mm; Sampling volume is 200mL, and medium hydrochloric acid total concn is 0.5mol/L, sample introduction moving phase linear rate of flow 10cm/min; First group of leacheate is 300mL 0.2mol/L hydrochloric acid, 50mL water, 50mL0.1mol/L hydrochloric acid, 50mL water, 100mL0.05mol/L HCl+1g/L EDTA, moving phase linear rate of flow 5cm/min; Second group of leacheate is 150mL0.5mol/L KSCN+40g/L xitix, moving phase linear rate of flow 2cm/min; The 3rd group of leacheate is the MIBK that 300mL crosses with the salt acid balance, and MIBK and concentrated hydrochloric acid volume ratio are 5/1 during balance, moving phase linear rate of flow 6cm/min; The 4th group of leacheate is 25mL ethanol, 25mL water, moving phase linear rate of flow 2cm/min; The 5th group of leacheate is 200mL1mol/L NH
4Cl+2mol/L NH
3H
2O, moving phase linear rate of flow 3cm/min; The 6th group of leacheate is 200mL0.2mol/L HCl+70g/L thiocarbamide+50% methyl alcohol, moving phase linear rate of flow 4.5cm/min.Chromatographic column 500mL2mol/L regeneration of hydrochloric acid.
1 ( ％ ) ,μg Pt 3821 99.00 0.75 1.07 1.16 0.09 1.00 96.80 100.87 100.86 95.83Pd 38009 99.93 0.17 0.01 0.06 0.01 100.44 0.43 101.12 101.12 100.37Ir 5000 99.00 0.70 98.90 0.04 0.00 0.13 0.82 100.59 100.58 97.91Au 37611 99.66 0.19 0.11 100.69 0.01 0.08 0.10 101.18 101.18 100.35Rh 2000 12.40 82.20 2.40 0.00 0.00 1.55 0.36 86.50 98.32Fe 2745 16.40 92.10 3.64 6.10 0.79 2.66 5.86 111.14 101.83Co 5000 4.20 113.00 0.00 0.30 0.00 0.00 0.00 112.80 100.54Ni 5851 7.76 87.00 5.10 4.99 0.00 0.00 0.00 97.06 99.77Cu 266660 5.97 88.42 0.18 0.81 0.14 0.59 0.52 90.66 99.44Pb 65272 63.11 99.04 0.00 0.05 0.02 0.04 0.04 99.19 99.49Zn 5910 62.60 98.40 0.02 0.04 0.00 0.91 0.07 99.41 99.63As 1254 18.70 51.00 9.00 7.79 3.84 1.17 31.50 104.26 100.80Sb 621 16.40 79.80 1.79 3.98 5.51 2.76 24.20 117.99 102.94Bi 788 100.00 98.80 3.31 0.00 0.13 0.53 1.45 104.23 104.23Se 29850 5.33 114.76 0.22 0.00 0.00 0.00 0.00 114.98 100.80Te 1433 9.58 59.13 0.00 1.00 0.00 2.17 3.80 66.10 96.75Sn 275 83.33 72.13 0.35 2.20 0.00 14.67 17.23 106.58 105.48
The result shows, precious metal and base metal good separating effect, and resolution height between the precious metal all reaches baseline separation; Precious metal rate of recovery height, platinum, palladium, iridium, gold recovery are respectively 95.83%, 100.37%, 97.91%, 100.35%; Velocity of separation is fast, and whole separation process is finished in 10h.
Among Fig. 2 in the platinum palladium concentrate principal element elution curve 0～200mL be the sample introduction elution curve, 200～500mL is a 0.2mol/L hydrochloric acid wash-out, 500～550mL is a water elution, 550～600mL is a 0.1mol/L hydrochloric acid wash-out, 600～650mL is a water elution, 650～750mL is a 0.05mol/L HCl+1g/L EDTA wash-out, 750～900mL is a 0.5mol/L KSCN+40g/L xitix wash-out, 900～1200mL is the MIBK wash-out, 1200～1250mL is ethanol and water elution, and 1250～1450mL is 1mol/L NH
4Cl+2mol/L NH
3H
2O wash-out, 1450～1650mL are 0.2mol/L HCl+70g/L thiocarbamide+50% methanol-eluted fractions.
Copper anode mud separates
In the test, the copper anode mud treatment capacity is 5g, and sampling volume is 200mL, and the hydrochloric acid medium total concn is 1.0mol/L, sample introduction moving phase linear rate of flow 5cm/min; Chromatographic column is φ 11mm * 125mm; First group of leacheate is 400mL0.5mol/L hydrochloric acid, 50mL0.1mol/L hydrochloric acid, 50mL water, 50mL0.1mol/L hydrochloric acid, 50mL water, 300mL 0.2mol/L HCl+0.5g/L EDTA, moving phase linear rate of flow 10cm/min; Second group of leacheate is 100mL1.0mol/L KSCN+20g/L xitix, moving phase linear rate of flow 4cm/min; The 3rd group of leacheate is the MIBK that 200mL crosses with the salt acid balance, and MIBK and concentrated hydrochloric acid volume ratio are 7/1 during balance, moving phase linear rate of flow 4.5cm/min; The 4th group of leacheate is 25mL ethanol, 25mL water, moving phase linear rate of flow 3cm/min; The 5th group of leacheate is 150mL2mol/L NH
4Cl+3mol/L NH
3H
2O, moving phase linear rate of flow 4.5cm/min; The 6th group of leacheate is 150mL0.6mol/L HCl+60g/L thiocarbamide+60% methyl alcohol moving phase linear rate of flow 6cm/min.Chromatographic column 500mL 3mol/L regeneration of hydrochloric acid.
Fig. 3 of test-results and Fig. 4 are copper anode mud principal element elution curve,) 0～200mL is the sample introduction elution curve among the figure, 200～600mL is a 0.5mol/L hydrochloric acid wash-out, 600～800mL is that 0.1mol/L hydrochloric acid and water replace wash-out, 800～1100mL is a 0.2mol/L HCl+0.5g/L EDTA wash-out, 1100～1200mL is a 1.0mol/L KSCN+20g/L xitix wash-out, 1200～1400mL is the MIBK wash-out, 1400～1450mL is ethanol and water elution, and 1450～1600mL is 2mol/L NH
4Cl+3mol/L NH
3H
2O wash-out, 1600～1750mL are 0.6mol/L HCl+60g/L thiocarbamide+60% methanol-eluted fractions.
Table 2 copper anode mud separation test result (%) element sample solution sample introduction adsorbs first group to be washed second group the 3rd group the 4th group the 5th group the 6th group and always washes total stream precious metal and return
,μg Pt 86 100.00 2.62 1.54 1.31 0.22 0.65 95.93 102.27 102.27 95.93Pd 1071 98.51 0.10 0.08 0.02 0.15 96.91 3.89 101.15 101.13 95.47Au 3542 99.38 0.47 0.10 99.77 0.57 1.25 1.43 103.59 103.57 99.15Fe 864 8.76 73.82 10.46 23.19 8.31 23.03 27.30 166.11 105 79Co 350 11.93 96.67 0.00 0.00 0.00 0.00 0.00 96.67 99.60Ni 100097 4.97 95.05 0.00 0.00 0.00 0.00 0.00 95.05 99.75Cu 249745 5.18 98.93 0.01 0.10 0.01 0.33 0.27 99.65 99.98Pb 2189 17.55 101.13 0.45 1.86 2.96 2.30 2.98 111.68 102.05Zn 21094 27.74 101.66 0.00 0.44 0.07 0.72 0.26 103.15 100.87As 7880 9.60 99.12 1.65 0.53 0.16 2.40 2.51 106.37 100.61Sb 5333 11.19 86.91 0.53 0.85 0.00 3.54 1.24 93.07 99.22Bi 28 100.00 90.36 1.34 5.13 0.00 3.13 4.06 104.02 104.02Se 601 24.17 90.55 6.46 6.76 0.00 8.65 3.04 115.46 103.74Te 127 21.88 95.89 7.23 4.15 0.00 4.96 5.30 117.53 103.84Sn 235 58.47 97.75 0.00 5.47 4.57 0.00 6.15 113.94 108.15
Test shows, platinum, palladium, gold and base metal good separating effect in the copper anode mud, and resolution height between the precious metal all reaches baseline separation; Precious metal rate of recovery height, the rate of recovery of platinum, palladium, gold is respectively 95.93%, 95.47%, 99.15%; Velocity of separation is fast, and whole separation process is finished in 10h.
Blister copper separates
Carry out separation test with the 5g blister copper, sampling volume is 200mL, and the hydrochloric acid medium total concn is 2.0mol/L, sample introduction moving phase linear rate of flow 10cm/min; Chromatographic column is φ 11mm * 130mm; First group of leacheate is 300mL0.2mol/L hydrochloric acid, 50mL water, 50mL0.1mol/L hydrochloric acid, 50mL water, 200mL0.12mol/L HCl+1g/L EDTA, moving phase linear rate of flow 15cm/min; Second group of leacheate is 100mL 1.0mol/L NH
4The SCN+20g/L xitix, moving phase linear rate of flow 4cm/min; The 3rd group of leacheate is the MIBK that 200mL crosses with the salt acid balance, and MIBK and concentrated hydrochloric acid volume ratio are 10/1 during balance, moving phase linear rate of flow 3cm/min; The 4th group of leacheate is 25mL ethanol, 25mL water, moving phase linear rate of flow 6cm/min; The 5th group of leacheate is 100mL0.5mol/L NH
4Cl+1.0mol/L NH
3H
2O, moving phase linear rate of flow 6cm/min; The 6th group of leacheate is 100mL 0.8mol/L HCl+40g/L thiocarbamide+40% methyl alcohol, moving phase linear rate of flow 2cm/min.Chromatographic column 500mL4.5mol/L regeneration of hydrochloric acid.Test-results is seen Fig. 5,6, table 3.
Test shows, blister copper platinum, palladium, gold and base metal good separating effect, and resolution height between the precious metal all reaches baseline separation; Precious metal rate of recovery height, the rate of recovery of platinum, palladium, gold is respectively 95.72%, 95.25%, 95.38%; Velocity of separation is fast, and whole separation process is finished in 10h.
0～200mL is the sample introduction elution curve among Fig. 5 of experimental result and Fig. 6,200～500mL is a 0.2mol/L hydrochloric acid wash-out, 500～550mL is a water elution, 550～600mL is a 0.1mol/L hydrochloric acid wash-out, 600～650mL is a water elution, 650～850mL is a 0.12mol/L HCl+1g/L EDTA wash-out, and 850～950mL is 1.0mol/L NH
4SCN+20g/L xitix wash-out, 950～1150mL are the MIBK wash-out, and 1150～1200mL is ethanol and water elution, and 1200～1300mL is 0.5mol/L NH
4Cl+1.0mol/L NH
3H
2O wash-out, 1300～1400mL are 0.8mol/LHCl+40g/L thiocarbamide+40% methanol-eluted fractions; Cu concentration is one of percentage of actual concentrations among Fig. 5.
3 ( ％ ) ,μg Pt 76 100.00 1.12 0.10 0.49 0.00 3.76 95.72 101.19 101.19 95.72Pd 46 100.00 0.43 0.54 2.11 0.41 95.25 8.48 107.22 107.22 95.25Au 107 99.52 2.10 1.55 95.84 0.82 2.51 3.93 109.85 106.75 95.38Fe 175 27.27 57.29 5.73 7.76 11.72 8.23 11.72 102.45 100.67Co 53 9.70 101.92 0.00 3.01 0.00 6.01 1.81 112.75 101.24Ni 20298 5.20 111.62 0.00 0.00 0.00 0.02 0.00 111.64 100.61Cu 4930225 5.65 100.15 0.00 0.04 0.004 0.02 0.02 100.23 100.01Pb 16975 41.38 100.67 0.29 0.08 0.00 0.14 0.04 101.22 100.50Zn 6388 6.23 98.04 0.31 2.17 0.00 2.67 3.30 106.49 100.40As 1532 7.53 98.92 2.38 2.44 1.28 3.13 0.75 108.90 100.67Sb 3104 7.69 100.04 1.25 0.18 0.00 0.47 1.54 103.48 100.27Bi 352 100.00 101.88 1.15 0.14 0.00 0.11 0.11 103.39 103.39Se 183 6.52 99.25 4.46 2.33 0.52 2.60 3.81 112.97 100.85Te 101 35.29 75.42 7.71 6.46 1.04 2.08 0.00 92.71 97.43Sn 80 42.50 44.56 3.75 21.54 8.64 4.78 9.38 92.65 96.88
Precious metal alloys separate
Carry out separation test with the 50g precious metal alloys, add iridium, each 5mg of rhodium in the feed liquid, sampling volume is 500mL, and the hydrochloric acid medium total concn is 3.0mol/L, sample introduction moving phase linear rate of flow 15cm/min; Chromatographic column is φ 40mm * 600mm.In the test, first group of leacheate is 600mL0.3mol/L hydrochloric acid, 200mL water, 200mL0.1mol/L hydrochloric acid, 200mL water, 400mL0.12mol/L HCl+1g/L EDTA, moving phase linear rate of flow 10cm/min; Second group of leacheate is 1500mL2.0mol/L NH
4The SCN+5g/L xitix, moving phase linear rate of flow 6cm/min; The 3rd group of leacheate is the MIBK that 1500mL crosses with the salt acid balance, and MIBK and concentrated hydrochloric acid volume ratio are 3/1 during balance, moving phase linear rate of flow 2cm/min; The 4th group of leacheate is 100mL ethanol, 100mL water, moving phase linear rate of flow 4.5cm/min; The 5th group of leacheate is 1500mL1mol/L NH
4Cl+2mol/L NH
3H
2O, 200mL water, moving phase linear rate of flow 2cm/min; The 6th group of leacheate is 1500mL0.5mol/L HCl+50g/L thiocarbamide+50% methyl alcohol, moving phase linear rate of flow 3cm/min.Chromatographic column 2000mL6mol/L regeneration of hydrochloric acid.
4 ( ％ ) ,μg Pt 32600 100.00 0.09 0.30 0.16 0.05 0.41 100.16 101.17 101.17 100.90Pd 21600 100.00 0.30 0.10 0.08 0.05 99.19 0.41 100.13 100.13 99.17Ir 6600 100.00 0.12 99.33 0.38 0.00 0.91 0.22 100.96 100.96 99.33Au 13000 100.00 0.06 0.02 98.37 0.19 0.54 0.66 99.84 99.84 98.37Rh 6000 67.83 95.62 1.17 0.37 0.02 0.78 0.65 98.61 99.06Fe 3530000 78.19 99.09 0.00 0.00 0.00. 0.00 0.00 99.09 99.29Co 675000 46.81 101.79 0.00 0.00 0.00 0.00 0.00 101.79 100.84Ni 33050000 42.51 98.2 0.00 0.00 0.00 0.00 0.00 98.2 99.23Cu 7150000 66.5 98.69 0.00 0.00 0.00 0.00 0.00 98.69 99.13Pb 7750 73.68 100.14 0.12 0.17 0.00 0.00 0.13 100.56 100.41Zn 65000 74.46 99.98 0.00 0.09 0.04 0.04 0.02 100.17 100.13As 19000 59.47 99.2 0.00 0.00 0.00 0.14 0.11 99.45 99.67Se 4200 60.36 99.35 0.22 0.00 0.00 0.36 0.23 100.16 100.10Te 6250 64.96 99.16 0.00 0.22 0.00 0.37 0.02 99.77 99.85
Test shows, precious metal rate of recovery height, and platinum, palladium, iridium, rhodium, gold recovery are respectively 100.16%, 99.19%, 99.33%, 97.00%, 98.37%; With the base metal good separating effect, although the base metal amount is big, as nickel up to 33g, but 98.20%～101.79% base metal all in the first step drip washing by wash-out, thereby separate with platinum, palladium, iridium, gold, method of proof can be from a large amount of base metals enriching noble metals: the resolution height all reaches baseline separation; Velocity of separation is fast, and whole flow process is finished in 10h.Calculating by to platinum, palladium, iridium, golden pregnant solution foreign matter content obtains product purity and is respectively: 97.04%, 98.28%, 97.14%, 98.67%, and the product purity height.
0～500mL is the sample introduction elution curve among Fig. 7 of experimental result and Fig. 8,500～1100mL is a 0.3mol/L hydrochloric acid wash-out, 1100～1300mL is a water elution, 1300～1500mL is a 0.1mol/L hydrochloric acid wash-out, 1500～1700mL is a water elution, 1700～2100mL is a 0.12mol/L HCl+1g/L EDTA wash-out, and 2100～3600mL is 2.0mol/LNH
4SCN+5g/L xitix wash-out, 3600～5100mL are the MIBK wash-out; 5100～5300mL is ethanol and water elution, and 5300～6800mL is 1mol/L NH
4Cl+2mol/L NH
3H
2O wash-out, 6800～7000mL are water elution, and 7000～8500mL is 0.5mol/L HCl+50g/L thiocarbamide+50% methanol-eluted fractions.
Claims (3)
1. the method for a separating platinum palladium iraurita comprises that precious metal and base metal are separated from each other from, precious metal, is characterized in that:
A. material is made the feed liquid that the hydrochloric acid medium total concn is 0.5～3mol/L, with weakly alkaline polystyrene tertiary amine-type anionite-exchange resin is the chromatographic stationary phase, with above-mentioned feed liquid is the moving phase sample introduction, moving phase linear rate of flow≤15cm/min during sample introduction, gold, platinum, palladium, iridium, bismuth and part are plumbous, zinc, antimony is kept by resin, most of base metal flows out, replace the lead that drip washing is retained with 0.1～0.5mol/L dilute hydrochloric acid and water, zinc, elements such as antimony, with slightly acidic EDTA solution drip washing bismuth, moving phase linear rate of flow≤10cm/min during drip washing, through above-mentioned sample introduction and drip washing step, Precious Metals-Gold, platinum, palladium, iridium separates with base metal;
B. for the precious metal that is adsorbed, the control phase line flow velocity≤6cm/min that flows, adopt selectively eluent by following order stepwise elution: iridium is with 0.5～2mol/L NH
4SCN or KSCN+5～40g/L ascorbic acid solution drip washing; The mibk drip washing that gold is crossed with the salt acid balance, mibk and concentrated hydrochloric acid volume ratio are 10/1～3/1 during balance; Palladium is with 0.5～2mol/L NH
4Cl+1～3mol/L NH
3H
2The drip washing of O solution; Platinum is with 0.2～0.8mol/L HCl+40～70g/L thiocarbamide+40～60% methanol solution drip washing; Chromatographic column is with 2～6mol/L regeneration of hydrochloric acid.
2. according to claims 1 described method, it is characterized in that: material is made the feed liquid that the hydrochloric acid medium total concn is 1mol/L, the chromatographic column stationary phase is a weakly alkaline polystyrene tertiary amine-type anionite-exchange resin, and expensive, base metal is finished when replacing drip washing and the drip washing of 0.12mol/L HCl+1g/L EDTA solution at sample introduction with 0.1～0.5mol/L dilute hydrochloric acid, water.
3. according to claims 1 described method, it is characterized in that: precious metal iridium, gold, palladium, platinum are separated from each other by stepwise elution and finish, and tool optionally eluent top condition is: 1mol/L NH
4SCN or KSCN+20g/L xitix drip washing iridium; With the mibk drip washing gold that the salt acid balance is crossed, during balance, mibk and concentrated hydrochloric acid volume ratio are 5/1; 1mol/L NH
4Cl+2mol/L NH
3H
2O drip washing palladium; 0.5mol/L HCl+50g/L thiocarbamide+50% methyl alcohol drip washing platinum; 3mol/L hydrochloric acid makes chromatographic column regeneration.
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