CN1978679A - Ru and/or chlorination treatment method of Rh - Google Patents
Ru and/or chlorination treatment method of Rh Download PDFInfo
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- CN1978679A CN1978679A CNA2006101056584A CN200610105658A CN1978679A CN 1978679 A CN1978679 A CN 1978679A CN A2006101056584 A CNA2006101056584 A CN A2006101056584A CN 200610105658 A CN200610105658 A CN 200610105658A CN 1978679 A CN1978679 A CN 1978679A
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Abstract
The invention provides a chloridize method of Ru and/or Rh, raw material of platinum metal (Pt, Pd, Ru, Rh, Ir, Os) at least comprise Ru and/or Rh (following called platinum container) mixed with sodium chloride power with average size less than 100 mum, platinum metal changed to dissolubility salts after chlorinating with chlorine, then water leaching the treated substance to leach, recover at least more than one of Ru, Rh, Ir. Thereby, leaching and recovering platinum metal effectively from raw material of platinum metal comprise Ru and/or Rh.
Description
Technical field
The present invention relates to a kind ofly from the raw material (containing thing) that contains the platinum group metal metal (Pt, Pd, Ru, Rh, Ir, Os) that comprises Ru and/or Rh at least, Ru and/or Rh are leached hereinafter referred to as platinum group metal, and the method that reclaims.This raw material that contains the platinum group metal metal that comprises Ru and/or Rh at least is, for example, the still residue exsiccant residue of the Se distillation tower that obtains from cupric electrolysis body refuse (slime) (after by the drying and distilling device residual selenium being carried out fractionation by distillation, the material of the dry residue that contains Se, Te, platinum group metal metal that obtains (below be designated as the dry residue of Se distillation tower)); By caustic soda Te is leached and filtering residue (below be designated as Te reducing slag alkali leach residue) with having reduced the residue of Te; Automotive exhaust-gas catalysts and resistor are with material etc.
Background technology
The platinum group metal metal is very difficult to dissolving for whole mineral acids under common condition.Present inventors are in patent application 2004-251721 number (patent documentation 1) for this reason, the method of a kind of leaching, recovery platinum group metal metal is disclosed, be that the platinum group metal that will contain Se and Te contains thing, in the chlorine atmosphere, carry out chloridizing volatilization and handle, to remove Se, Te, add chloride salt to this handled thing, in the chlorine atmosphere, carry out chloridizing roasting and handle, further remove Se, Te, make the platinum group metal metal become soluble salt, then water logging goes out this handled thing, and leaches, reclaims the platinum group metal metal.
In chloridizing volatilization is handled, be main purpose to remove Se, Te, but the part of platinum group metal metal and chlorine reaction convert MCl to
n(M is the platinum group metal element, and n is 2～4), but PtCl
2, RuCl
3Deng in water, being insoluble.For this reason, in the chloridizing volatilization handled thing, add chloride salt, in the chlorine atmosphere, carry out chloridizing roasting and handle, and convert water-soluble salt to.When for example adopting sodium-chlor, generate Na as chloride salt
6-nMCl
6Mixed chlorinated sodium in the chloridizing volatilization handled thing carries out the reaction of the processing of chloridizing roasting in the chlorine atmosphere, be shown below.
2M+(12-2n)NaCl+nCl2→2Na
6-nMCl
6
MCln+(6-n)NaCl→Na
6-nMCl
6
[patent documentation 1] spy opens 2004-251721
At this, be lower than when carrying out chloridizing roasting and handle, because platinum group metal element, MCl as 801 ℃ temperature of the melting point of sodium-chlor
nWith sodium-chlor all are solids, so platinum group metal element, MCl
nWith the reaction of sodium-chlor be solid phase-solid state reaction.For this reason, there is the partial reaction that has only particle to contact with each other, and do not have the part of contact that the residual problem of unreacted reactant is arranged easily each other at particle.
In addition, if handle carrying out chloridizing roasting as the temperature more than 801 ℃ of the melting point of sodium-chlor, then sodium-chlor fusion and cover platinum group metal element, MCl
nThe surface.Make the platinum group metal element become the Na of solubility
6-nMCl
6Reaction in, need chlorine, but because the sodium-chlor covering surfaces of fusion hinders passing through of gas, so reaction will be difficult to carry out, unreacted reactant is residual easily.In addition, if dissolved sodium-chlor blocking chlorine, then inner chlorine dividing potential drop reduces, and has the Na that generates
6-nMCl
6Easy problem of decomposing.
Summary of the invention
Problem of the present invention is to find out a kind ofly from the raw material that contains the platinum group metal metal, leaches, reclaims the method for Ru and/or Rh efficiently.
Promptly, (1) the present invention is the chlorination processing method of a kind of Ru and/or Rh: in the raw material (containing thing hereinafter referred to as platinum group metal) that contains the platinum group metal element (Pt, Pd, Ru, Rh, Ir, Os) that comprises Ru and/or Rh at least, mixing median size is the following sodium-chlor powder of 100 μ m, carrying out chloridizing roasting in the chlorine atmosphere handles, make the platinum group metal metal become soluble salt, then this handled thing is carried out water logging and go out, thereby leach, reclaim among Ru, Rh, the Ir more than one.
(2) according to the chlorination processing method of (1) described Ru and/or Rh, it is the following powder of 500 μ m that platinum group metal contains thing.
(3) according to each described Ru in above-mentioned (1) to (2) and/or the chlorination processing method of Rh, contain in the thing, when containing Se and/or Te, carry out chloridizing volatilization in advance and handle, remove Se and/or Te at platinum group metal.
(4) according to each described Ru in above-mentioned (1) to (3) and/or the chlorination processing method of Rh, in chloridizing roasting is handled, after 520～570 ℃ of maintenances, again with 700～800 ℃ of maintenances.
According to foregoing invention,
(1) can leach, reclaim Ru and/or Rh with the high-recovery more than 95%.
(2) by with below sodium-chlor efflorescence to the 100 μ m, use as the chlorizating agent of chloridizing roasting, can under the high-recovery more than 95%, handle Ru and/or Rh.
(3) can leach the residue from the dry residue of Se distillation tower or Te reducing slag alkali and reclaim Ru and/or Rh effectively.
(4) can use the material from automotive exhaust-gas catalysts or resistor, reclaim Ru and/or Rh effectively.
Description of drawings
Fig. 1 is the schema of embodiments of the invention 1.
Fig. 2 is the schema of embodiments of the invention 2.
Fig. 3 is the mode chart of the gas curve of the temperature curve of chloridizing roasting correct principle of embodiments of the invention 1 and ventilation.
Embodiment
Below explain the present invention.
The objective of the invention is to, from the raw material that contains the platinum group metal element that comprises Ru and/or Rh at least, leach, reclaim Ru and/or Rh.
For example, with usual method with cupric electrolysis body refuse decopper(ing) after, chlorination is leached, by solvent extract reclaim Au after, use SO
2Reduction Se filters from solution.Distill purification in order to make filtering Se improve purity, but a part of platinum group metal metal that is mixing is recovered as the dry residue of Se distillation tower (mainly being Se, Pt, Pd, Ru, Rh, Ir) among Se.
Perhaps after the Se reduction, similarly reduce Te, but this reducing slag is leached Te and filtering residue by caustic soda, leach residue (mainly being Se, Te, Ru, Rh) and reclaim as the Te reducing slag alkali of the undissolved Se of containing, Te, platinum group metal metal.
In addition in recent years, used the automotive exhaust-gas catalysts (mainly being aluminum oxide, Pt, Rh, Pd) and the resistor of platinum group metal metal to be widely used with material (mainly being glass, Ru, Pd), but, in order to utilize the platinum group metal metal again, and need to reclaim, purify.
In the present invention, when the dry residue of described Se distillation tower or Te reducing slag alkali are leached residue as initial feed, preferably in cl gas flow, raw material is heated up, heating, carry out chloridizing volatilization and handle, remove the muriate of the high Se of vapour pressure, Te thus, concentrate Ru and/or Rh.With material (mainly being glass, Ru, Pd) during as initial feed, preferably the method for flotation etc. concentrates Ru and/or Rh with pulverizing with automotive exhaust-gas catalysts (mainly being aluminum oxide, Pt, Rh, Pd) and resistor.If contain moisture, emit water vapour during then because of heating in cl gas flow at this, the chlorine dividing potential drop is temporarily reduced, or the possibility that oxide compound is generated, so preferably dry fully in advance.Drying conditions does not limit especially, but can be in 100～150 ℃, 6～15 hours.Also have, when using the few raw material of moisture, can certainly omit drying process.
The platinum group metal that so obtains is contained thing pulverize, preferred screening is that particle diameter is below 500 μ m.This is that then reaction is difficult to arrive the inside of particle because surpass 500 μ m if platinum group metal contains the particle diameter of thing.
Pulverize, can utilize the method for hammer mill, jaw crusher, roller crusher etc., but not be specially limited.
Sodium-chlor adopts the few purified salt of impurity.If adopt the ordinary salt comprise impurity in a large number, then because dissolve simultaneously at the impurity that leaches Shi Mei etc., the purification of platinum group metal metal is bothersome and be not preferred.In addition because the sodium-chlor of market sale contains moisture, so preferred thorough drying and using.Drying conditions is not particularly limited, but can be in 100～150 ℃, 6～15 hours.
The purified salt particle diameter of market sale is about 200～500 μ m.For this reason, sodium-chlor be pulverized median size is become below the 100 μ m, contain thing with above-mentioned platinum group metal and mix fully.Pulverizing can utilize the method for hammer mill, needle mill, ball mill etc., but is not particularly limited.Median size is disperseed in the ethanol that does not dissolve sodium-chlor, with mensuration such as laser diffractometries.Because the easy moisture absorption caking of the sodium-chlor of pulverizing, thus be preferably at once with platinum group metal contain thing mixes before pulverizing.Also have, pulverize and mixed the mixture that platinum group metal contains thing and sodium-chlor and also can access same effect, still, if pulverize the different material of hardness, the then soft bed course (cushion) that becomes is difficult to obtain crushing effect.
The addition of sodium-chlor, in the solubility chlorination reaction of preferred platinum group metal metal 1～7 times of needed amount.Also have, if the addition of sodium-chlor increases, then because for the total amount in the stove of can packing into, the ratio that is chlorinated the volatilization handled thing diminishes, and the processing efficiency variation is so be preferably 2～5 times scope especially.
If contain aerobic in raw material and chloridized atmosphere, then Ru, Rh generate insoluble oxide compound, rate of recovery step-down.For this reason,, add a spot of carbon dust earlier by when mixing platinum group metal and contain thing and sodium-chlor, thus generation that can the inhibited oxidation thing.
The mixture that method thus obtains is put into furnace pot, in the chlorine atmosphere, carry out chloridizing roasting and handle.The material of furnace pot is preferably quartz, aluminum oxide, graphite etc.The time that chloridizing roasting is handled is not particularly limited, but, by 520～570 ℃ keep 30 minutes～3 hours after, kept 1～10 hour with 700～800 ℃, thereby the platinum group metal metal becomes soluble salt.Also can suppress the decomposition of resultant in order to lower the temperature, preferably keep chlorination atmosphere at least to the temperature below 550 ℃ till.
Preferably 520～570 ℃ of reasons that kept 30 minutes～3 hours be because, the reaction in this stage by platinum group metal element and chlorine, muriate generates, but will be suitable for to the supply of the chlorine of handled thing inside and two aspects of muriatic formation reaction.What table 1 showed is platinum group metal to be contained thing put into quartz crucible, the reactive result when investigation keeps 3 hours in cl gas flow.
From then on the result generates muriatic reaction in the temperature that is lower than 520 ℃ and does not fully carry out.On the other hand, if surpass 570 ℃, then this handled thing shrinks, and the bottom of crucible has unreacted reactant to produce.
In this stage, the chlorine that need supply with requirement early arrives the inside of handled thing, but if surpass 570 ℃, then this handled thing shrinks, and pass through of chlorine worsens, and can't fully supply with chlorine and arrive inside.
700～800 ℃ of preferred reasons that kept 1～10 hour is because in this stage, the reaction of muriate and sodium-chlor by the platinum group metal element generates the Na of solubility
6-nMCl
6, but when being lower than 700 ℃, reaction can't fully be carried out.In addition, if surpass 800 ℃, then because the sodium-chlor of fusion interdicts chlorine, so inner chlorine dividing potential drop reduces the Na of generation
6-nMCl
6Decompose, the rate of recovery reduces.
Table 1
| The maintenance temperature (℃) | Estimate | The state of the test portion after the heating |
| 500 | × | Whole unreacted |
| 520 | ○ | Reaction equably |
| 550 | ○ | Reaction equably |
| 570 | ○ | Reaction equably |
| 575 | × | Shrink the bottom unreacted |
| 600 | × | Shrink the bottom unreacted |
After this, this handled thing is put into water or dilute hydrochloric acid, leach the platinum group metal metal soluble salt.Be not particularly limited as at this moment condition, but be preferably 50～90 ℃ warm water or dilute hydrochloric acid.The concentration of dilute hydrochloric acid also has when water logging goes out this handled thing, becomes hydrochloric acid tart situation by free chlorine.For this reason, as required, more preferably be adjusted into 0.5～1.5N.
Superfluous filtrations such as sodium-chlor, unreacted carbon dust and unreacted platinum group metal metal, can access the aqueous solution of platinum group metal metal.
[embodiment]
(embodiment 1)
Below specifically describe embodiment.Embodiment 1 is by flow implementation shown in Figure 1.That is, will become the Te reducing slag that contains Ru and Rh of raw material and alkali and leach residue 8235g, be set at 100 ℃ drying machine inner drying 12 hours.
After this, the quartz system of packing into furnace pot, in the stove core barrel is the tube furnace of quartzy system, chlorine on one side circulates when beginning from heating up, kept 1 hour at 200 ℃ and 440 ℃ respectively on one side, reheat to 820 ℃, the doubling dose that makes chlorine dose become the needed amount of chlorination reaction of Se, Te, platinum group metal metal circulates, and the chloridizing volatilization of carrying out 5 hours is handled.
Also have, during cooling with 500 ℃ by nitrogen replacement.Remove Se and Te, Ru is condensed into 48wt%, Rh is condensed into 12wt%.
The chloridizing volatilization residue was pulverized 20 minutes by ball mill, by the sieve screening of mesh 500 μ m, but will allow whole amounts sieve.Also have, it is finely particulate that the Te reducing slag alkali of raw material leaches residue, handles the back particles aggregate in chloridizing volatilization, but can easily decompose pulverizing.
The sodium-chlor of market sale (purified salt, median size 350 μ m) 7800g was pulverized 1 hour by ball mill respectively with the chloridizing volatilization residue.Median size after the pulverizing is scattered in that the result with mensuration such as laser diffractometries is 80 μ m in the ethanol.The sodium-chlor amount is reacted 3 times of amounts of needed amount with respect to this handled thing for the solubility chlorination of platinum group metal metal.
Secondly, in chloridizing volatilization residue of pulverizing and sodium-chlor, interpolation is as the carbon dust of the 350g of the needed amount of inhibition of oxidation of platinum group metal metal, thorough mixing.
With the furnace pot of its quartzy system of packing into, in the stove core barrel is the tube furnace of quartzy system, as shown in Figure 3, kept 1 hour at 300 ℃ while the chlorine that circulates, remove residual moisture after, kept 2 hours with 550 ℃, reheat to 780 ℃, the chloridizing roasting of carrying out 5 hours is handled.
Also have, during cooling with 500 ℃ by nitrogen replacement.During by this handled thing of observation by light microscope, do not observe unreacted sodium-chlor particle substantially, roughly total amount is all reacted equably.
After this, this processing was stirred 1 hour in 80 ℃ warm water 30L, leach the platinum group metal metal soluble salt.Filtration residue, and obtain the leach liquor 29.5L of platinum group metal metal.
As shown in table 2, for the rate of recovery in water-leach liquor of Te reducing slag alkali leaching residue, Ru is up to more than 99%, and Rh is up to 98%.Can obtain the platinum group metal leach liquor of Ru and Rh effectively with this method.
Table 2
Te reducing slag alkali leaches residue 8235 (g)
(embodiment 2)
Embodiment 2 is by flow implementation shown in Figure 2.
That is, the resistor that contains the Ru that becomes raw material is pulverized by mortar with material waste (scrap), until the sieve that all can pass through mesh 500 μ m.In being set at 100 ℃ drying machine, be dried 12 hours.
Sodium-chlor adopts method similarly to Example 1 to pulverize.Median size after the pulverizing is scattered in the ethanol, is 80 μ m with the result of mensuration such as laser diffractometry.The sodium-chlor amount is to react 3 times of amounts of needed amount for the solubility chlorination of this handled thing platinum group metal metal.
Secondly, in the sodium-chlor 42g of the resistor of pulverizing with material waste 35g and pulverizing, interpolation is as the carbon dust of the 1.8g of the needed amount of inhibition of oxidation of platinum group metal metal, thorough mixing.With the crucible of its quartzy system of packing into, in the stove core barrel is the tube furnace of quartzy system, Yi Bian the chlorine that circulates similarly to Example 1, kept 1 hour on one side at 300 ℃, remove residual moisture after, kept 2 hours with 550 ℃, reheat to 780 ℃, the chloridizing roasting of carrying out 4 hours is handled.
This handled thing is leached the platinum group metal metal soluble salt in 80 ℃ warm water.Filtration residue obtains the leach liquor 460mL of platinum group metal metal.
As shown in table 3, for resistor with the rate of recovery of the Ru in water-leach liquor of material waste up to 98%.Can obtain the leach liquor of Ru effectively with this method.
Table 3
Resistor material waste 35 (g)
(comparative example 1)
Below comparative example is described.Comparative example 1 leaches residue 8000g except changing to Te reducing slag alkali, with 200 ℃ and 440 ℃ temperature curve was kept 1 hour respectively, beyond reheat to 800 ℃ kept two hours, carry out chloridizing volatilization by the method identical and handle, obtain chloridizing volatilization residue 3170g with embodiment 1.Remove Se and Te, Ru is concentrated into 50wt%, and Rh is concentrated into 13wt%.
The sodium-chlor 6600g of used market sale does not pulverize, screens among chloridizing volatilization residue 3170g and the embodiment 1, and directly adds carbon dust 297g, thorough mixing.With its quartzy system furnace pot of packing into, in the stove core barrel is the tube furnace of quartzy system, as shown in Figure 2, kept 1 hour at 300 ℃ while the chlorine that circulates, remove residual moisture after, kept 2 hours with 600 ℃, reheat to 780 ℃, the chloridizing roasting of carrying out 5 hours is handled.Also have, during cooling with 500 ℃ by nitrogen replacement.
During with this handled thing of observation by light microscope, observe unreacted sodium-chlor particle, observe and be unfavorable for the sodium-chlor particle that reacts.
After this, this handled thing was stirred 1 hour in 80 ℃ warm water 27L, leach the platinum group metal metal soluble salt after, filtration residue obtains the leach liquor 26.7L of platinum group metal metal.As shown in table 4, to the rate of recovery in the water-leach liquor, Ru is 86%, and Rh is 90%.With embodiment 1 relatively, low and be not preferred to the rate of recovery of the Ru in the water-leach liquor, Rh.
The result who goes out residue by the water logging of X-ray diffraction determination and analysis detects a large amount of RuCl
3And RhCl
3Because the median size of sodium-chlor is greatly to 350 μ m, so the platinum group metal metal does not fully contact with the sodium-chlor particle, the reaction that becomes the sodium salt of solubility can't be carried out.
Table 4
Te reducing slag alkali leaches residue 8000 (g)
(comparative example 2)
Comparative example 2 will be as the resistor that contains Ru of raw material with material waste (median size 2mm), at the drying machine inner drying 12 hours that is set at 100 ℃.The exsiccant resistor is not pulverized with material waste 31g, and directly added sodium-chlor 50g and the carbon dust 1.7g that pulverizes by method similarly to Example 1, thorough mixing.With its quartzy system crucible of packing into, in the stove core barrel is the tube furnace of quartzy system, Yi Bian the chlorine that circulates similarly to Example 2, kept 1 hour on one side at 300 ℃, remove residual moisture after, kept 2 hours with 550 ℃, reheat to 780 ℃, the chloridizing roasting of carrying out 4 hours is handled.
This handled thing is leached the platinum group metal metal soluble salt in 80 ℃ warm water.Filtration residue obtains the leach liquor 480mL of platinum group metal metal.As shown in table 5, be low to moderate 74% for resistor with the rate of recovery of the Ru in water-leach liquor of material waste.Because do not pulverize the resistor material waste, so can not leach the interior Ru of particle effectively.
Table 5
Resistor material waste 31 (g)
(comparative example 3)
Comparative example 3 is that Te reducing slag alkali is leached residue 8000g, carries out chloridizing volatilization by method similarly to Example 1 and handles, and obtains chloridizing volatilization residue 2954g.Remove Se and Te, Ru is concentrated into 49wt%, and Rh is concentrated into 13wt%.The chloridizing volatilization residue was pulverized 20 minutes with ball mill, and the sieve screening by mesh 500 μ m is sieved full dose.
The chloridizing volatilization residue adds the sodium-chlor 6600g that is pulverized by method similarly to Example 1, carbon dust 350g, thorough mixing.With its quartzy system furnace pot of packing into, in the stove core barrel be the tube furnace of quartzy system, the chlorine that circulates on one side was 300 ℃ of maintenances 1 hour, remove residual moisture after, with 500 ℃ of maintenances 2 hours, reheat to 780 ℃ carried out 5 hours chloridizing roasting processing.Also have, during cooling with 500 ℃ by nitrogen replacement.
After this, this handled thing was stirred 1 hour in 80 ℃ warm water, leach the platinum group metal metal soluble salt after, filtration residue obtains the leach liquor 22.5L of platinum group metal metal.As shown in table 6, to the rate of recovery in the water-leach liquor, Ru is 57%, and Rh is 81%.With embodiment 1 relatively, low and be not preferred to the rate of recovery of the Ru in the water-leach liquor, Rh.Its reason is because keep temperature to be low to moderate 500 ℃, so the chlorination reaction of Ru, Rh can't advance.
Table 6
Te reducing slag alkali leaches residue 8000 (g)
(comparative example 4)
Comparative example 4 is that Te reducing slag alkali is leached residue 9017g, carries out chloridizing volatilization by method similarly to Example 1 and handles, and obtains chloridizing volatilization residue 3922g.Remove Se and Te, Ru is concentrated into 49wt%, and Rh is concentrated into 8.8wt%.The chloridizing volatilization residue was pulverized 20 minutes with ball mill, and the sieve screening by mesh 500 μ m is sieved full dose.
The chloridizing volatilization residue adds the sodium-chlor 6600g that is pulverized by method similarly to Example 1, carbon dust 350g, thorough mixing.With its quartzy system furnace pot of packing into, in the stove core barrel be the tube furnace of quartzy system, the chlorine that circulates on one side was 300 ℃ of maintenances 1 hour, remove residual moisture after, with 600 ℃ of maintenances 2 hours, reheat to 780 ℃ carried out 5 hours chloridizing roasting processing.Also have, during cooling with 500 ℃ by nitrogen replacement.
After this, this handled thing was stirred 1 hour in 80 ℃ warm water, leach the platinum group metal metal soluble salt after, filtration residue obtains the leach liquor 31.0L of platinum group metal metal.As shown in table 7, to the rate of recovery in the water-leach liquor, Ru is 87%, and Rh is 90%.With embodiment 1 relatively, low and be not preferred to the rate of recovery of the Ru in the water-leach liquor, Rh.Its reason is because keep temperature up to 600 ℃, so the circulation variation of chlorine, the thing that responds during the chlorination reaction of Ru, Rh is residual.
Table 7
Te reducing slag alkali leaches residue 9017 (g)
(comparative example 5)
Comparative example 5 is that Te reducing slag alkali is leached residue 8000g, carries out chloridizing volatilization by method similarly to Example 1 and handles, and obtains chloridizing volatilization residue 3405g.Remove Se and Te, Ru is concentrated into 47wt%, and Rh is concentrated into 12wt%.The chloridizing volatilization residue was pulverized 20 minutes with ball mill, and the sieve screening by mesh 500 μ m is sieved full dose.
The chloridizing volatilization residue adds the sodium-chlor 6800g that is pulverized by method similarly to Example 1, carbon dust 350g, thorough mixing.With its quartzy system furnace pot of packing into, in the stove core barrel be the tube furnace of quartzy system, the chlorine that circulates on one side was 300 ℃ of maintenances 1 hour, remove residual moisture after, with 550 ℃ of maintenances 2 hours, reheat to 680 ℃ carried out 5 hours chloridizing roasting processing.Also have, during cooling with 500 ℃ by nitrogen replacement.
After this, this handled thing was stirred 1 hour in 80 ℃ warm water, leach the platinum group metal metal soluble salt after, filtration residue obtains the leach liquor 26.0L of platinum group metal metal.As shown in table 8, to the rate of recovery in the water-leach liquor, Ru is 42%, and Rh is 58%.With embodiment 1 relatively, low and be not preferred to the rate of recovery of the Ru in the water-leach liquor, Rh.Its reason is because the chloridizing roasting temperature is low to moderate 680 ℃, thus the reaction of Ru, Rh and NaCl do not carry out, insufficient to the conversion of the salt of solubility.
Table 8
Te reducing slag alkali leaches residue 8000 (g)
(comparative example 6)
Comparative example 6 is that Te reducing slag alkali is leached residue 9178g, carries out chloridizing volatilization by method similarly to Example 1 and handles, and obtains chloridizing volatilization residue 4082g.Remove Se and Te, Ru is concentrated into 42wt%, and Rh is concentrated into 15wt%.The chloridizing volatilization residue was pulverized 20 minutes with ball mill, and the sieve screening by mesh 500 μ m is sieved full dose.
The chloridizing volatilization residue adds the sodium-chlor 6200g that is pulverized by method similarly to Example 1, carbon dust 350g, thorough mixing.With its quartzy system furnace pot of packing into, in the stove core barrel be the tube furnace of quartzy system, the chlorine that circulates on one side was 300 ℃ of maintenances 1 hour, remove residual moisture after, with 550 ℃ of maintenances 2 hours, reheat to 820 ℃ carried out 5 hours chloridizing roasting processing.Also have, during cooling with 500 ℃ by nitrogen replacement.
After this, this handled thing was stirred 1 hour in 80 ℃ warm water, leach the platinum group metal metal soluble salt after, filtration residue obtains the leach liquor 25.0L of platinum group metal metal.As shown in table 9, to the rate of recovery in the water-leach liquor, Ru is 89%, and Rh is 94%.With embodiment 1 relatively, low and be not preferred to the rate of recovery of the Ru in the water-leach liquor, Rh.Its reason be because the chloridizing roasting temperature up to 820 ℃, so NaCl fusion and interdict chlorine, inner muriate decomposes.
Table 9
Te reducing slag alkali leaches residue 9178 (g)
Claims (4)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005350216A JP4313361B2 (en) | 2005-12-05 | 2005-12-05 | Method of chlorinating Ru and / or Rh |
| JP2005350216 | 2005-12-05 |
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|---|---|
| CN1978679A true CN1978679A (en) | 2007-06-13 |
| CN100410396C CN100410396C (en) | 2008-08-13 |
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| RU2385960C1 (en) * | 2008-11-20 | 2010-04-10 | Государственное образовательное учреждение высшего профессионального образования "Сибирский государственный индустриальный университет" | Processing method of silicon-containing alloys of platinum and noble metals |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AT406273B (en) * | 1997-10-23 | 2000-03-27 | Prior Eng Ag | METHOD FOR UNLOCKING MATERIALS CONTAINING PRECIOUS METALS |
| JP3943564B2 (en) * | 2004-01-30 | 2007-07-11 | 日鉱金属株式会社 | Method for chlorinating Se-containing materials |
-
2005
- 2005-12-05 JP JP2005350216A patent/JP4313361B2/en not_active Expired - Lifetime
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| TWI411581B (en) * | 2008-02-26 | 2013-10-11 | Jx Nippon Mining & Metals Corp | Method for recovering ruthenium from waste containing ruthenium |
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| CN105256145A (en) * | 2015-11-18 | 2016-01-20 | 金川集团股份有限公司 | Method for extracting noble metal from waste vehicle exhaust catalyst |
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| CN114107691A (en) * | 2021-11-05 | 2022-03-01 | 安徽元琛环保科技股份有限公司 | Method for recovering platinum from platinum-containing waste catalyst |
| CN114107691B (en) * | 2021-11-05 | 2024-01-19 | 安徽元琛环保科技股份有限公司 | Method for recovering platinum from waste catalyst containing platinum |
| CN115011808A (en) * | 2022-06-22 | 2022-09-06 | 广东先导稀材股份有限公司 | Method for separating and recovering ruthenium and iridium from ruthenium and iridium-containing materials |
| CN115011808B (en) * | 2022-06-22 | 2023-10-24 | 广东先导稀材股份有限公司 | Method for separating and recovering ruthenium and iridium from ruthenium and iridium-containing material |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2007154250A (en) | 2007-06-21 |
| JP4313361B2 (en) | 2009-08-12 |
| CN100410396C (en) | 2008-08-13 |
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