CN1280433C - Chlorination treatment process of Se contg. substance - Google Patents
Chlorination treatment process of Se contg. substance Download PDFInfo
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- CN1280433C CN1280433C CNB2004100817220A CN200410081722A CN1280433C CN 1280433 C CN1280433 C CN 1280433C CN B2004100817220 A CNB2004100817220 A CN B2004100817220A CN 200410081722 A CN200410081722 A CN 200410081722A CN 1280433 C CN1280433 C CN 1280433C
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- 238000011282 treatment Methods 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000005660 chlorination reaction Methods 0.000 title claims description 118
- 239000000126 substance Substances 0.000 title claims description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 146
- 239000002184 metal Substances 0.000 claims abstract description 146
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 76
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 75
- -1 platinum group metals Chemical class 0.000 claims abstract description 65
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000460 chlorine Substances 0.000 claims abstract description 39
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 39
- 238000002386 leaching Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 150000003839 salts Chemical class 0.000 claims abstract description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 95
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 55
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 46
- 239000011780 sodium chloride Substances 0.000 claims description 23
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 150000003841 chloride salts Chemical class 0.000 claims description 5
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 31
- 238000001035 drying Methods 0.000 abstract description 21
- 238000004821 distillation Methods 0.000 abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 10
- 239000011669 selenium Substances 0.000 description 104
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 36
- 239000010453 quartz Substances 0.000 description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 229910001873 dinitrogen Inorganic materials 0.000 description 16
- 238000001704 evaporation Methods 0.000 description 16
- 230000008020 evaporation Effects 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 238000001816 cooling Methods 0.000 description 14
- 229910052763 palladium Inorganic materials 0.000 description 14
- 229910052703 rhodium Inorganic materials 0.000 description 14
- 238000001914 filtration Methods 0.000 description 12
- 229910052741 iridium Inorganic materials 0.000 description 12
- 230000002829 reductive effect Effects 0.000 description 12
- 229910052707 ruthenium Inorganic materials 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 238000010304 firing Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 238000001354 calcination Methods 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 239000002893 slag Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 150000001805 chlorine compounds Chemical class 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005192 partition Methods 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052762 osmium Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- VIEXQFHKRAHTQS-UHFFFAOYSA-N chloroselanyl selenohypochlorite Chemical compound Cl[Se][Se]Cl VIEXQFHKRAHTQS-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 150000003498 tellurium compounds Chemical class 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The purpose of this invention is to efficiently remove Se and Te from a raw material containing Se, Te and platinum group metals, and to leach/recover platinum group metals. In the chloridizing treatment method for an Se-containing material, a raw material containing Se, Te and platinum group metals (e.g., residue after drying in an Se distillation tower) is subjected to chloridizing volatilizing treatment in a chlorine atmosphere to remove Se and Te; a chloride is added to the treated material, and chloridizing roasting treatment is performed in a chlorine atmosphere to further remove Se and Te, thus platinum group metals are made into soluble salts; and next, the treated material is subjected to water leaching to leach/recover platinum group metals.
Description
Technical Field
The present invention relates to a method for recovering a platinum group metal (Pt, Pd, Ru, Rh, Ir, Os) by efficiently removing Se and Te from a raw material (hereinafter referred to as Se-containing material) containing Se, Te and the platinum group metal, for example, from a residue obtained by drying a bottom residue of a Se distillation column (a dry residue containing Se, Te, and the platinum group metal obtained after distilling and separating residual selenium in a dry distillation apparatus (hereinafter referred to as Se distillation column dry residue)).
Background
Platinum group metals are very insoluble in all mineral acids under normal conditions. Conventionally, the following methods have been used to dissolve these elements: a method of treating with an alkali-soluble inorganic acid in the presence of oxygen or an oxidizing agent for dissolving these elements; mixing and melting metals such as Zn, Sn, Pb, Cu, etc., dissolving zinc, etc. with hydrochloric acid or sulfuric acid to obtain active fine powder, and dissolving the active fine powder with aqua regia; conversion of platinum group metals to Na as indicatedmMCl6(M is a platinum group element, and M is 2 or 3).
Japanese patent laid-open No. 2003-268457 (patent document 1) discloses a method in which a mixture of sodium hydroxide and sodium nitrate is added to a raw material containing Se and a platinum group metal, and the mixture is melted and leached with water to separate a Se-containing liquid component and a platinum group metal-containing residue. However, since Te is not contained in the raw material, a separation method for Te is not specifically disclosed.
Further, japanese patent laying-open No. 2-205635 (patent document 2) discloses a method in which a treated product containing Ru or an oxide thereof is mixed with a chloride complex salt forming agent, and a chlorine gas is flown out while heating to convert Ru or an oxide thereof into a chloride, and the chloride complex salt forming agent reacts with Ru or an oxide thereof to form a Ru complex salt, and thereafter Ru is recovered by dissolution separation.
Further, japanese patent No. 2505492 (patent document 3) discloses an Ir dissolving method in which a mixture of Ir monomer and metal chloride is heated in a stream of chlorine gas to convert into a metal salt of iridium chloride acid, wherein carbon is added to the mixture to perform the conversion.
However, there is no specific disclosure of a method of separating Se and Te from a raw material containing Se, Te and platinum group metals and simultaneously recovering all the platinum group metals to which Pt, Pd, Rh and Os are added.
[ patent document 1]Japanese patent application laid-open No. 2003-268457
[ patent document 2]Japanese patent application laid-open No. Hei 2-205635
[ patent document 3]Japanese patent application No. 2505492
Disclosure of Invention
In view of the above circumstances, an object of the present invention is to provide a method for efficiently separating Se and Te from a raw material containing Se, Te and platinum group metals and leaching and recovering all the platinum group metals.
Namely, the invention is as follows:
(1) a method for chlorinating a Se-containing material, comprising: performing a chlorination volatilization process on a raw material (hereinafter referred to as a Se-containing material) containing Se, Te and a platinum group metal in a chlorine gas atmosphere to remove Se and Te; a chloride salt is added to the treated product, and the treated product is subjected to a chloridizing roasting treatment in a chlorine atmosphere to further remove Se and Te to convert the platinum group metal into a soluble salt, and then the treated product is leached with water.
(2) The method for chlorinating a Se-containing material according to (1), wherein the amount of chlorine used in the chlorination volatilization treatment is 0.8 to 4 times the amount necessary for the chlorination reaction of Se, Te, and a platinum group metal, and the heating temperature is 600 to 900 ℃.
(3) The method for chlorinating a Se-containing material according to (1), wherein a reducing agent is added during the chlorinating/calcining treatment.
(4) The method for chlorinating a Se-containing material according to any one of (1) to (3), wherein sodium chloride is used as a chloride salt used in the chlorination baking treatment, and carbon powder is used as a reducing agent.
(5) The method for chlorinating a Se-containing material as recited in any one of (1) to (4), wherein the amount of sodium chloride used in the chlorination roasting treatment is 1 to 7 times the amount necessary for the soluble chlorination reaction of the platinum group metal, and the amount of carbon powder is 0.5 to 12 times the amount necessary for the soluble chlorination reaction of the platinum group metal.
(6) The method for chlorinating a Se-containing material according to any one of (1) to (5), wherein the amount of chlorine used in the chlorinating/calcining treatment is 0.8 to 4 times the amount required for the chlorination reaction of Se and Te and the soluble chlorination reaction of a platinum group metal, and the heating temperature is 700 to 900 ℃.
(7) The method for chlorinating a Se-containing material according to any one of (1) to (6), wherein a carbon container is used as a reducing agent in the chlorination baking treatment, or carbon molded into a plate or rod shape is placed in a boiler instead of adding carbon powder.
(8) The method for chlorinating a Se-containing material as recited in any one of (1) to (7), wherein a leaching treatment is performed with warm water or dilute hydrochloric acid instead of the water leaching treatment.
(9) The method for chlorinating a Se-containing material according to any one of (1) to (8), wherein the raw material is sufficiently dried in advance in the chlorination volatilizing treatment and the chlorination calcining treatment.
(10) The method for chlorinating a Se-containing material according to any one of (1) to (9), wherein the Se-containing material is kept at 150 to 217 ℃ for 30 minutes to 3 hours before reaching the heating temperature in the chlorination evaporation treatment.
(11) The method for chlorinating a Se-containing material according to any one of (1) to (10), wherein the Se-containing material is maintained at 400 to 450 ℃ for 30 minutes to 3 hours before reaching the heating temperature in the chlorination evaporation treatment.
(12) The method for chlorinating a Se-containing material according to any one of (1) to (11), wherein a chlorine gas atmosphere of 550 ℃ or higher is set during the temperature raising, the temperature maintaining, and the temperature lowering in the chlorination volatilizing and chlorination firing treatments.
According to the invention as above:
(1) se and Te can be effectively removed from a raw material containing Se, Te and platinum group metals, and the platinum group metals can be leached and recovered.
(2) Platinum group metals such as Pt, Pd, Ru, Rh, Ir, Os can be obtained with a high recovery rate of 90% or more.
Drawings
FIG. 1 is a flow chart illustrating an embodiment of the present invention.
FIG. 2 is a schematic view showing the temperature mode and the gas ventilation mode of the chlorination vaporization treatment in example 1 of the present invention.
FIG. 3 is a diagram showing a method of carrying out embodiment 2 of the present invention.
FIG. 4 is a flowchart of comparative example 1 of the present invention.
Detailed Description
The present invention is described in detail below.
The object of the present invention is to remove Se and Te from a raw material containing Se, Te and platinum group metals, and leach and recover the platinum group metals.
For example, after decoppering the copper electrolytic slime (slime) by a usual method, Au is recovered by extraction with a solvent by chlorination leaching, and then with SO2Se was reduced and isolated from the solution by filtration. In order to improve the purity of the filtered Se, distillation purification is performed, but some platinum group metals mixed in Se are recovered as dry residue (mainly Se, Pt, Pd, Ru, Rh and Ir) of a Se distillation tower. Or after Se reduction, the same Te is reduced, the residue obtained by leaching Te from the reducing slag with sodium hydroxide and filtering is used as the residue of alkaline leaching of the Te reducing slag containing undissolved Se, Te and platinum group metalsThe slag (mainly Se, Te, Ru, Rh, Ir) is recovered.
In the invention, the dry solid residue of the Se distillation tower or the alkaline leaching residue of the Te reducing slag is used as a raw material. If the starting material contains moisture, it is preferably dried sufficiently beforehand, since water vapor is released during heating in a chlorine gas stream, thereby temporarily reducing the chlorine partial pressure or possibly generating oxides. The drying conditions are not particularly limited, and may be 100 to 120 ℃ for 6 to 15 hours. When a raw material having a very small amount of water is used, the drying step can be omitted.
When the raw material is heated, chlorinated and volatilized in a stream of chlorine gas, chlorides of Se and Te having high vapor pressure are removed, leaving platinum group metals. Se has a melting point of 217 ℃ and Te has a melting point of 450 ℃, and when melted during the temperature rise, the raw material particles are closely adhered to each other and chlorine gas does not smoothly flow through the particles, so that most of Se and Te should be removed as chlorides while keeping the temperature at or below the respective melting point values. The Se removal is carried out under the conditions that the temperature is 150-217 ℃ and the holding time is 30 minutes-3 hours. The Te removal iscarried out under the conditions that the temperature is 400-450 ℃ and the holding time is 30 minutes-3 hours. Since some of Se and Te generate selenium and tellurium compounds, they are difficult to be converted into chlorides for removal. To remove Se and Te sufficiently, the mixture is heated to a high temperature. The heating temperature is preferably 600 to 900 ℃, more preferably 700 to 800 ℃.
The reason for limiting the temperature range is described below. The sublimation temperature of selenium chloride is 196 ℃ and the sublimation temperature of tellurium chloride is 414 ℃, and if the treatment temperature is lower than 600 ℃, the removal rate of Se and Te is reduced. On the other hand, if the temperature exceeds 900 ℃, the vapor pressure of the chloride of the platinum group metal is high and the chloride is partially volatilized, and on the other hand, the chloride is dissociated to become a metal which is difficult to leach out by water, and therefore the recovery rate is lowered.
The treatment time is not particularly limited, but is preferably 1 to 10 hours, more preferably 3 to 6 hours.
The amount of chlorine is preferably 0.8 to 4 times the amount necessary for the chlorination reaction of Se, Te and platinum group metal. Since the same effect can be obtained in the chlorination roasting step, the removal effect of Se and Te is sufficient if the raw material and chlorine are easily brought into contact with each other, and the consumption of chlorine is increased only by 4 times or more while the required amount is 0.8 times that required. Since the chlorination reaction of Se and Te is gradually increased from a low temperature around room temperature, it is necessary to maintain a chlorine gas atmosphere during heating and holding. In addition, since chlorides of platinum group elements dissociate at 550 ℃ or higher to release chlorine, it is necessary to maintain a chlorine gas atmosphere. Since chlorine gas is not consumed at the time of temperature reduction, the minimum amount of chlorine gas necessary for maintaining a chlorine gas atmosphere can be used. When the temperature is reduced to 500 ℃ or lower, inert gas such as nitrogen or argon may be used instead. Further, if air is mixed in the chlorine gas atmosphere, the platinum group metal surface is oxidized, and even if carbon is mixed, the reduction of the oxide layer is not caused, and the recovery rate is lowered, so that it is preferable to maintain strict airtightness.
The main reaction of the chlorination volatilization treatment is as follows.
( )
Next, sodium chloride and carbon powder are added to the treated product, and the treated product is heated under a condition of flowing a chlorine gas flow to perform a chlorination firing treatment, so that Se and Te remaining in the chlorination volatilization treatment are removed again as chlorides, and the platinum group metal becomes a soluble salt. The heating temperature is preferably 700 to 900 ℃, more preferably 750 to 850 ℃.
If the treatment temperature is lower than 700 ℃, not only the removal rate of Se and Te is reduced, but also the soluble chlorination reaction of the platinum group metal is not sufficiently carried out and the yield is reduced; if the temperature exceeds 900 ℃, a part of the volatile matter is removed, and the recovery rate is lowered.
The treatment time is not particularly limited, but is preferably 1 to 10 hours, more preferably 3 to 6 hours.
The amount of chlorine is preferably 0.8 to 4 times the amount necessary for the chlorination reaction of Se or Te or the soluble chlorination reaction of a platinum group metal. In addition, since chlorination is also performed in the chlorination volatilization step, it is sufficient to use 0.8 times the amount necessary for easy contact between the raw material and chlorine.
The amount of sodium chloride added is preferably 1 to 7 times the amount necessary for the soluble chlorination reaction of the platinum group metal. Further, if the amount of sodium chloride added is increased, the ratio of the volatile substances to be chlorinated to the total amount charged into the furnace is decreased, and the treatment efficiency is lowered, and therefore, the range of 3 to 5 times is more preferable. Since commercially available sodium chloride contains water, it is preferably used after being sufficiently dried. The drying conditions are not particularly limited, and may be 100 to 150 ℃ for 6 to 15 hours.
The amount of carbon powder added is preferably 0.5 to 12 times the amount necessary for inhibiting oxidation of the platinum group metal. The carbon powder can reduce an oxide layer on the surface of the platinum group metal to promote a soluble chlorination reaction and suppress the formation of an oxide layer during the temperature rise, but the addition of the carbon powder in an amount exceeding 12 times hardly changes the effect. Further, as the reducing agent, a carbon container may be used, or carbon molded into a plate shape or a rod shape may be put into a boiler instead of adding carbon powder, so that the same effect as that obtained when carbon powder is added can be obtained. In addition, if the amount of oxygen mixed in the furnace is reduced in the chloridizing/baking treatment, it is needless to say that the amount of the carbon powder to be added can be reduced. Since commercially available sodium chloride and carbon powder contain water, it is preferable to sufficiently dry them before mixing them with a volatile chloride and roasting them. The drying conditions are not particularly limited, and may be 100 to 120 ℃ for 6 to 15 hours. Further, by using sodium chloride or carbon powder which originally contained little water and mixing the chlorinated volatile matter in a state where no water is mixed, the drying step can be omitted.
When the soluble chlorination reaction of the platinum group metal is not sufficiently performed, the yield is lowered, and the recovery rate in water leaching is low, the recovery rate can be improved by pulverizing the treated product subjected to the chlorination roasting treatment and repeating the heating operation in the chlorine gas flow several times.
Hereinafter, the main reaction in the chloridizing calcination treatment will be described with respect to the case of using sodium chloride as an example of the chloride salt.
( )
Thereafter, the treated material is water-leached to leach out soluble salts of platinum group metals. The conditions in this case are not particularly limited, but warm water or dilute hydrochloric acid is preferred.
The temperature of the warm water is preferably 50-90 ℃.
The concentration of dilute hydrochloric acid may be changed to hydrochloric acid by free chlorine even when only the treated product is subjected to water leaching. Therefore, it is preferably adjusted to 0.5 to 1.5N as necessary.
Filtering the residue containing excessive sodium chloride, unreacted carbon powder, and unreacted platinum group metal to obtain a platinum group metal leaching solution. The platinum group metal is recovered as a sponge from a leachate of the platinum group metal by a conventional method. By returning the filtration residue to the chloridizing/calcining treatment step, the recovery rate of the platinum group metal not recovered can be improved, and the amount of the chemical used can be reduced.
(example 1)
This example was carried out according to the procedure shown in FIG. 1. The following specifically describes the present invention based on table 1 and fig. 2.
150g of the Se distillation column dry residue after drying in a drier set at 100 ℃ for 12 hours was put into an evaporation pan made of quartz, and kept at 200 ℃ and 440 ℃ for 1 hour while flowing chlorine gas in a tubular furnace made of quartz as shown in FIG. 2, and then heated to 700 ℃ and chlorine in an amount 2 times the amount required for the chlorination reaction of Se, Te and platinum group metal was flowed for 5 hours to perform chlorination volatilization treatment. In addition, nitrogen gas was substituted at 500 ℃ during cooling. 83% of Se and 99% of Te are removed.
Subsequently, 170g of sodium chloride, which is 3 times the amount required for the soluble chlorination reaction of the platinum group metal, and 3.2g of carbon powder, which is the amount required for suppressing the oxidation of the platinum group metal, were added to the treatment substance, and sufficiently mixed. This material was dried in a drier set at 100 ℃ for 12 hours. After drying, the mixture was placed in an evaporation pan made of quartz, heated to 850 ℃ while flowing chlorine gas in a tubular furnace made of quartz, and chlorine was flowed in an amount 2 times as large as that required for chlorination reaction of Se and Te and soluble chlorination reaction of platinum group metals, and subjected to chlorination firing treatment for 3 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Thereafter, the treated material was leached out at a temperature of 80 ℃ of 420mL to leach out soluble salts of platinum group metals. Filtering the residue to obtain a leaching solution of the platinum group metals. As shown in Table 1, Se in the leachate was 19mg/L, Te of 0.1mg/L or less, and 99% or more of Se was removed from the dry residue in the Se distillation column.
As shown in table 1, the partition ratios of the platinum group metals were Pt 92%, Pd 90%, Ru 90%, Rh 93%, and Ir 95%. The raw material does not contain Os, but since it has very similar properties to Ru, it can be recovered in the same manner.
TABLE 1
(example 2)
Example 2 is explained below. The same procedure as in example 1 was repeated, except that the amount of chlorine used in the chlorination volatilization treatment was the amount necessary for the chlorination reaction of Se, Te and the platinumgroup metal, and the amount and method of addition of carbon powder in the chlorination calcination treatment were changed as shown in FIG. 3.
6000g of the Se distillation column dry residue after drying in a drier set at 100 ℃ for 12 hours was placed in an evaporation pan made of quartz, kept at 200 ℃ and 440 ℃ for 1 hour in a tubular furnace made of quartz with a core tube made of quartz while passing chlorine gas therethrough, heated to 700 ℃ and passed with chlorine in an amount necessary for chlorination reaction of Se, Te and platinum group metal for 5 hours to perform chlorination volatilization treatment. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Then, 104g of sodium chloride in an amount 5 times as large as that required for the soluble chlorination reaction of the platinum group metal was added to 30g of the treated product, and the mixture was thoroughly mixed. The material was dried in a drier set at 100 ℃ for 12 hours. Here, 1 times the amount of carbon powder necessary for inhibiting oxidation of platinum group metals was added; (2) adding 10 times of carbon powder; (3) filling into a carbon plate; (4) a sample loaded into a quartz crucible as a carbon-made lid; (5) a sample loaded into the carbon crucible; then, the furnace core tube was heated to 850 ℃ while flowing chlorine gas through the quartz tube furnace, and chlorine was flowed in an amount 2 times as large as that required for the chlorination reaction of Se and Te and the soluble chlorination reaction of platinum group metals, and the chlorination firing treatment was performed for 5 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Thereafter, the treated product was leached with warm water at 80 ℃ to leach out soluble salts of platinum group metals.
Filtering the residue to obtain a leaching solution of the platinum group metals. As shown in table 2, extremely high distribution ratios were shown for all of Pt, Pd, Ru, Rh, and Ir. Particularly, when the carbon crucible of (5) is used, the distribution ratio of all metals is 99% or more.
The effect hardly changed when the carbon powder was added in an amount exceeding 12 times. Further, by using a carbon container as the reducing agent or putting carbon molded into a plate-like or rod-like shape into the boiler instead of adding carbon powder, the same or more effects as those in the case of adding carbon powder can be obtained.
TABLE 2
(example 3)
Example 3 will be specifically described below based on table 3. The Te reducing slag alkali leaching residue is used as a raw material.
6000g of alkaline leaching residue of Te reducing slag after drying in a drier set at 100 ℃ for 12 hours was put into an evaporation pan made of quartz, kept at 200 ℃ and 440 ℃ for 1 hour in a tubular furnace made of quartz with a furnace core tube filled with chlorine gas, heated to 780 ℃ and supplied with chlorine in an amount 2 times the amount required for chlorination reaction of Se, Te and platinum group metals, and subjected to chlorination volatilization for 5 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling. More than 99% of Se and Te are removed.
Next, 2650g of the treatment substance was added with 7500g of sodium chloride in an amount 5 times as large as that required for soluble chlorination of platinum group metals and 204g of carbon powder in an amount 2 times as large as that required for suppressing oxidation of platinum group metals, and sufficiently mixed. The material was dried in a drier set at 100 ℃ for 12 hours. After drying, the resultant was placed in an evaporation pan made of quartz, heated to 780 ℃ in a tubular furnace made of quartz with a muffle tube filled with chlorine gas, and subjected to a chlorinating/baking treatment for 5 hours with chlorine gas being supplied in an amount of 1.9 times as large as that required for the chlorination reaction of Se and Te and the soluble chlorination reaction of a platinum group metal. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Thereafter, the treated product was leached with warm water 22L at 80 ℃ to leach out soluble salts of platinum group metals. The residue was filtered to obtain 21.7L of a leaching solution of platinum group metals. As shown in Table 3, Se in the leachate was 22mg/L, Te of 34mg/L or less, and 99.9% or more of Se was removed from the alkaline leaching residue of Te-reducing slag.
As shown in table 3, the partition ratios of the platinum group metals were Pt 98%, Pd 95%, Ru 96%, Rh 99%, and Ir 92%. Se and Te can be separated even if the characteristics of the raw materials are different, and the platinum group metal in the leachate can be recovered with an efficiency of 90% or more.
TABLE 3
Comparative example 1
Comparative example 1 is described below based on table 4 and fig. 4. In the case of not performing chlorination volatilization treatment, sodium chloride and carbon powder are added to the dry residue of the Se distillation tower, and the leaching solution of platinum group metals is obtained only by chlorination roasting treatment.
To 150g of the dry solid residue of the Se distillation column, 750g of sodium chloride in an amount 10 times as large as that required for the soluble chlorination reaction of the platinum group metal and 2.8g of carbon powder in an amount necessary for suppressing the oxidation of the platinum group metal were added and sufficiently mixed. This material was dried in a drier set at 100 ℃ for 12 hours. After drying, the mixture was placed in an evaporation pan made of quartz, heated to 850 ℃ while flowing chlorine gas in a tubular furnace made of quartz, and chlorine was flowed in an amount 2 times as large as that required for chlorination reaction of Se and Te and soluble chlorination reaction of platinum group metals, and subjected to chlorination firing treatment for 3 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Thereafter, soluble salts of platinum group metals were leached with 825mL of warm water at 80 ℃. Filtering the residue to obtain a leaching solution of the platinum group metals.
As shown in Table 4, Se in the leachate was 13mg/L, Te which was less than 0.1mg/L, and was removed from the dry residue of the Se distillation column by at least 99%.
As shown in table 4, the partition ratios of the platinum group metals were Pt 84%, Pd 93%, Ru 59%, Rh 80%, and Ir 70%. As is clear from comparison with examples, the distribution ratio of the platinum group metal is lowered, which is not preferable. Since the chlorination volatilization treatment is not performed, the chlorination reaction of Se and Te is preferentially performed, and the soluble chlorination reaction of the platinum group metal does not proceed sufficiently, and the yield is lowered.
TABLE 4
Comparative example 2
Comparative example 2 is described below based on table 5. The same procedure as in example 1 was repeated, except that the temperature of the chlorination evaporation treatment was changed to 500 ℃.
150g of the Se distillation column dry residue after drying for 12 hours in a drier set at 100 ℃ was put into an evaporation pan made of quartz, kept at 200 ℃ and 440 ℃ for 1 hour in a tubular furnace made of quartz with a furnace core tube filled with chlorine gas, heated to 500 ℃ and supplied with chlorine in an amount 2 times the amount required for the chlorination reaction of Se, Te and platinum group metals, and subjected to chlorination volatilization for 5 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling. As shown in Table 5, it was not preferable to remove 43% of Se and 27% of Te at a lower removal rate than in the examples.
TABLE 5
Comparative example 3
Comparative example 3 is explained below. The same procedure as in example 2 was repeated, except that the amount of chlorine used in the chlorination volatilization treatment was 2 times as large as the amount necessary for the chlorination reaction of Se, Te and the platinum group metal, and carbon powder was not added in the chlorination calcination treatment.
150g of dry solid residue of Se distillation tower dried in a drier set at 100 ℃ for 12 hours was put in an evaporation pan made of quartz, kept at 200 ℃ and 440 ℃ for 1 hour in a tubular furnace made of quartz with a core tube made of quartz while passing chlorine gas therethrough, heated to 700 ℃ and passed through chlorine in an amount 2 times as large as that required for chlorination reaction of Se, Te and platinum group metal, and subjected to chlorination volatilization for 5 hours.
Then, 281g of sodium chloride in an amount 7 times that required for the soluble chlorination reaction of the platinum group metal was added to the treated product, and mixed well. No carbon powder is added here. The material was dried in a drier set at 100 ℃ for 12 hours. After drying, the resultant was placed in a quartz evaporation pan, heated to 850 ℃ in a quartz tube furnace, and subjected to a chlorinating/baking treatment for 3 hours with chlorine gas flowing through the tube furnace in an amount 2 times as large as that required for the chlorination reaction of Se and Te and the soluble chlorination reaction of a platinum group metal. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Thereafter, 359mL of the treated product was leached with warm water at 80 ℃ to leach out soluble salts of platinum group metals. Filtering the residue to obtain a leaching solution of the platinum group metals. As shown in Table 6, the leaching solution contained Se at a level of less than 0.1mg/L and Te at a level of less than 0.1mg/L, and 99% or more of the solution was removed from the Se column.
As shown in table 6, the partition ratios of the platinum group metals were Pt 85%, Pd 89%, Ru 55%, Rh 82%, and Ir 80%. As is clear from comparison with the examples, the distribution ratio of the platinum group metal is lowered, which is not preferable. Since carbon powder is not added, reduction of the oxidized layer on the surface of the platinum group metal does not proceed and formation of the oxidized layer during temperature rise is not suppressed, so that the soluble chlorination reaction of the platinum group metal does not proceed sufficiently and the yield is lowered.
TABLE 6
Comparative example 4
Comparative example 4 is described below based on table 7. The same procedure as in example 2 was repeated, except that the amount of carbon powder added in the chloridizing calcination treatment was 0.1 times the amount necessary for suppressing the oxidation of the platinum group metal.
6000g of the Se distillation column dry residue after drying in a drier set at 100 ℃ for 12 hours was placed in an evaporation pan made of quartz, kept at 200 ℃ and 440 ℃ for 1 hour in a tubular furnace made of quartz with a core tube made of quartz while passing chlorine gas therethrough, heated to 700 ℃ and passed with chlorine in an amount necessary for chlorination reaction of Se, Te and platinum group metal for 5 hours to perform chlorination volatilization treatment. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Then, 104g of sodium chloride in an amount of 5 times that required for soluble chlorination of platinum group metals and 0.12g of carbon powder in an amount of 0.1 time that required for inhibition of oxidation of platinum group metals were added to 30g of the treated product, and mixed thoroughly. The material was dried in a drier set at 100 ℃ for 12 hours. After drying, the furnace core tube was heated to 850 ℃ while flowing chlorine gas through the quartz tube furnace, and chlorine was flowed in an amount 2 times as large as that required for the chlorination reaction of Se and Te and the soluble chlorination reaction of platinum group metals, and the chlorination firing treatment was carried out for 5 hours. In addition, nitrogen was replaced at 500 ℃ when the temperature was lowered.
Thereafter, the treated product was leached with warm water at 80 ℃ to leach out soluble salts of platinum group metals. Filtering the residue to obtain a leaching solution of the platinum group metals.
As shown in table 7, the partition rates of the platinum group metals were Pt 81%, Pd 68%, Ru 67%, and Rh 49%. As compared with example 2, the distribution ratio of the platinum group metal is lowered, which is not preferable. Addition of less than 0.5 times the amount of carbon powder is also hardly effective. As in the case of the case where no carbon powder is added, reduction of the oxide layer on the platinum group metal surface and suppression of the formation of the oxide layer during the temperature rise are not or cannot be sufficiently performed, so that the soluble chlorination reaction of the platinum group metal does not proceed sufficiently and the yield is lowered.
TABLE 7
Comparative example 5
Comparative example 5 is described below based on table 8. The dry starting material and sodium chloride were not used here and compared with example 2.
6000g of the undried dry residue of the Se distillation column was placed in an evaporation pan made of quartz, and the mixture was kept at 200 ℃ and 440 ℃ for 1 hour in a tubular furnace having a quartz core tube while passing chlorine gas therethrough, and then heated to 700 ℃ to pass chlorine in an amount necessary for the chlorination reaction of Se, Te and a platinum group metal therethrough, and subjected to a chlorination volatilization treatment for 5 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Next, 5780g of sodium chloride, which is commercially available and undried and 5 times the amount required for the soluble chlorination reaction of the platinum group metals, and 696g of carbon powder, which is 10 times the amount necessary for suppressing the oxidation of the platinum group metals, were added to 1730g of the above-mentioned treatment substance and mixed thoroughly. The material was heated to 850 ℃ without drying, while passing chlorine gas through a quartz tube furnace, and chlorine was passed through the furnace in an amount 2 times as large as that required for the chlorination reaction of Se and Te and the soluble chlorination reaction of a platinum group metal, and the chlorination firing treatment was carried out for 5 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Thereafter, the treated product was leached with warm water at 80 ℃ to leach out soluble salts of platinum group metals. Filtering the residue to obtain a leaching solution of the platinum group metals.
As shown in table 8, the results were Pt 9%, Pd 99% or more, Ru 51%, Rh 94%, and Ir 53%, and the distribution ratios of Pt, Ru, and Ir were lowered as compared with example 2, which was not preferable. The leaching residue was measured by X-ray diffraction, and the platinum group metal oxide was detected. Since the raw material contains a large amount of water, oxides formed during the temperature rise process are not sufficiently reduced by the carbon powder, and as a result, the soluble chlorination reaction of the platinum group metal does not proceed sufficiently, and the yield is lowered.
TABLE 8
Comparative example 6
Comparative example 6 is described below based on table 9. In the chloridizing and baking step, the heating temperature was continuously raised to 700 ℃.
6000g of the Se distillation column dry residue after drying in a drier set at 100 ℃ for 12 hours was put into a quartz evaporation pan, and chlorinated volatilization treatment was carried out for 5 hours by passing chlorine gas through a quartz tubular furnace having a furnace core tube and continuously raising the temperature to 700 ℃ while passing chlorine gas therethrough, and passing chlorine in an amount necessary for the chlorination reaction of Se, Te and a platinum group metal therethrough. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Next, 5770g of sodium chloride in an amount 5 times as large as that required for the soluble chlorination reaction of the platinum group metal and 70g of carbon powder in an amount necessary for suppressing the oxidation of the platinum group metal were added to 1741g of the treatment substance, and sufficiently mixed. The material was dried in a drier set at 100 ℃ for 12 hours. After drying, the furnace core tube was heated to 850 ℃ while flowing chlorine gas through the quartz tube furnace, and chlorine was flowed in an amount 2 times as large as that required for the chlorination reaction of Se and Te and the soluble chlorination reaction of platinum group metals, and the chlorination firing treatment was carried out for 5 hours. In addition, nitrogen gas was substituted at 500 ℃ during cooling.
Thereafter, the treated product was leached with warm water at 80 ℃ to leach out soluble salts of platinum group metals. Filtering the residue to obtain a leaching solution of the platinum group metals.
As shown in table 9, the results were Pt 71%, Pd 81% or more, Ru 99%, Rh 99% or more, and Ir 97%, and it was found that the distribution ratio of Pt and Pd was lowered as compared with example 2, which was not preferable. As a result of X-ray diffraction measurement of the leaching residue, platinum group metals in a metallic state were detected. This is because Se contained in a large amount in the raw material is melted during the temperaturerise, and the raw material particles are closely adhered to each other, so that the chlorine gas cannot smoothly flow, and as a result, the soluble chlorination reaction of the platinum group metal does not proceed sufficiently, and the yield is lowered.
TABLE 9
Comparative example 7
Comparative example 7 is described below based on table 10. In the chlorination volatilizing step and the chlorination firing step, the atmosphere gas was replaced with nitrogen from chlorine immediately after the start of temperature reduction after the heating temperature was maintained for a predetermined time, and comparison was made.
6000g of dry residue of the Se distillation tower dried in a drier set at 100 ℃ for 12 hours was put in an evaporation pan made of quartz, and while flowing chlorine gas, the temperature was continuously raised to 700 ℃ in a tubular furnace made of quartz as a furnace core tube, chlorine in an amount necessary for the chlorination reaction of Se, Te and platinum group metals was flowed, and chlorination volatilization treatment was performed for 5 hours, and immediately after the temperature was lowered.
Next, to 1741g of the treatment, 4360g of sodium chloride in an amount of 5 times as large as that required for the soluble chlorination reaction of the platinum group metal and 525g of carbon powder in an amount of 10 times as large as that required for suppressing the oxidation of the platinum group metal were added and mixed thoroughly. The material was dried in a drier set at 100 ℃ for 12 hours. After drying, the furnace core tube was a quartz tubular furnace, heated to 820 ℃ while flowing chlorine gas, and chlorine was flowed in an amount 2 times as large as that required for the chlorination reaction of Se and Te and the soluble chlorination reaction of platinum group metals, and subjected to the chlorination roasting treatment for 5 hours, and immediately after the temperature reduction was started, nitrogen gas was flowed.
Thereafter, the treated product was leached with warm water at 80 ℃ to leach out soluble salts of platinum group metals. Filtering the residue to obtain a leaching solution of the platinum group metals.
As shown in table 10, the results were Pt 52%, Pd 57%, Ru 68%, Rh 72%, and Ir 64%, and it was found that the partition rate of the platinum group metal was lowered as compared with example 2, which was not preferable. As a result of X-ray diffraction measurement of the leaching residue, platinum group metals in a metallic state were detected. This is because chlorides of platinum group elements dissociate at a temperature of 550 ℃ or higher to release chlorine, and nitrogen gas is directly passed through at a high temperature during the temperature reduction process, and the partial pressure of chlorine is reduced, thereby decomposing into platinum group metals in a metallic state. As a result, the soluble chloride of the platinum group metal is reduced, and the yield is lowered.
Watch 10
Claims (12)
1. A method for chlorinating Se, Te and platinum group metal-containing substances, which is characterized in that:
performing chlorination volatilization treatment on a raw material containing Se, Te and platinum group metal in a chlorine atmosphere to remove Se and Te; adding chloride salt to the treated product, performing chlorination roasting treatment in a chlorine atmosphere to further remove Se and Te to convert the platinum group metal into soluble salt, and leaching the treated product with water to recover the platinum group metal.
2. The method for chlorinating Se, Te and a platinum group metal-containing substance according to claim 1, wherein:
the amount of chlorine used in the chlorination volatilization treatment is 0.8 to 4 times the amount necessary for the chlorination reaction of Se, Te and platinum group metals, and the heating temperature is 600 to 900 ℃.
3. The method for chlorinating Se, Te and a platinum group metal-containing substance according to claim 1, wherein:
in the chloridizing/baking treatment, a carbon container, carbon powder, or carbon molded into a plate or rod shape is used as a reducing agent.
4. The method for chlorinating Se, Te and a platinum group metal-containing substance according to claim 3, wherein:
sodium chloride is used as the chloride salt used in the chloridizing roasting treatment, and carbon powder is used as the reducing agent.
5. The method for chlorinating Se, Te and platinum group metal-containing substances according to claim 4, wherein:
the amount of sodium chloride used in the chlorination roasting treatment is 1 to 7 times the amount necessary for the soluble chlorination reaction of the platinum group metal, and the amount of carbon powder is 0.5 to 12 times the amount necessary for the soluble chlorination reaction of the platinum group metal.
6. The method for chlorinating a Se, Te and platinum group metal-containing substance according to any one of claims 1 to 5, wherein:
the amount of chlorine used in the chloridizing roasting treatment is 0.8 to 4 times of the amount necessary for the chlorination reaction of Se and Te and the soluble chlorination reaction of platinum group metals, and the heating temperature is 700 to 900 ℃.
7. The method for chlorinating Se, Te and platinum group metal-containing substances according to claim 5, wherein:
in the chloridizing roasting treatment, instead of adding carbon powder, a carbon container or carbon molded into a plate or rod shape is used as a reducing agent.
8. The method for chlorinating a Se, Te and platinum group metal-containing substance according to any one of claims 1 to 5, wherein:
the leaching treatment is carried out by warm water or dilute hydrochloric acid to replace the water leaching treatment.
9. The method for chlorinating a Se, Te and platinum group metal-containing substance according to any one of claims 1 to 5, wherein:
in the chlorination volatilizing treatment and the chlorination roasting treatment, the raw materials are sufficiently dried in advance.
10. The method for chlorinating Se, Te and platinum group metal-containing substances according to claim 2, wherein:
in the chlorination volatilization treatment, the temperature is kept at 150-217 ℃ for 30 minutes-3 hours before the heating temperature is reached.
11. The method for chlorinating Se, Te and platinum group metal-containing substances according to claim 2, wherein:
in the chlorination volatilization treatment, the temperature is kept at 400-450 ℃ for 30 minutes-3 hours before the heating temperature is reached.
12. The method for chlorinating a Se, Te and platinum group metal-containing substance according to any one of claims 1 to 5, wherein:
and in the temperature rising process, the temperature maintaining process and the temperature reducing process of the chlorination volatilizing process and the chlorination roasting process, setting the chlorine atmosphere at the temperature of more than 550 ℃.
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| JP4313361B2 (en) * | 2005-12-05 | 2009-08-12 | 日鉱金属株式会社 | Method of chlorinating Ru and / or Rh |
| JP4789001B2 (en) * | 2006-03-01 | 2011-10-05 | Ｊｘ日鉱日石金属株式会社 | Method for separating ruthenium and tantalum from ruthenium-tantalum alloys |
| JP5021331B2 (en) * | 2007-02-16 | 2012-09-05 | 田中貴金属工業株式会社 | Method for recovering platinum group metals from waste |
| JP5223085B2 (en) * | 2007-03-13 | 2013-06-26 | 国立大学法人秋田大学 | Separation and purification of rare metals by chloride volatilization method |
| JP2010077510A (en) * | 2008-09-29 | 2010-04-08 | Nippon Mining & Metals Co Ltd | Method of separating rhodium from platinum and/or palladium |
| JP5134607B2 (en) * | 2009-09-30 | 2013-01-30 | Ｊｘ日鉱日石金属株式会社 | Efficient operation method for Ru-Rh purification process |
| JP5560440B2 (en) * | 2010-06-03 | 2014-07-30 | 一般財団法人生産技術研究奨励会 | Method for recovering platinum group metals |
| JP5591749B2 (en) * | 2011-03-30 | 2014-09-17 | パンパシフィック・カッパー株式会社 | Method for recovering tellurium from alkaline leaching residue containing tellurium |
| JP5591748B2 (en) * | 2011-03-30 | 2014-09-17 | パンパシフィック・カッパー株式会社 | How to recover tellurium |
| CN105441691A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for extracting precious metals from low-grade gold (Au)-palladium (Pd)-platinum (Pt) materials |
| CN114737063A (en) * | 2022-03-22 | 2022-07-12 | 咸阳欧冶科技有限公司 | Platinum alloy purification process |
| CN116161629A (en) * | 2023-04-03 | 2023-05-26 | 昆明理工大学 | Method for purifying selenium |
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