CN115571931B - Method for preparing chloroiridic acid from pure iridium powder - Google Patents
Method for preparing chloroiridic acid from pure iridium powder Download PDFInfo
- Publication number
- CN115571931B CN115571931B CN202211380379.4A CN202211380379A CN115571931B CN 115571931 B CN115571931 B CN 115571931B CN 202211380379 A CN202211380379 A CN 202211380379A CN 115571931 B CN115571931 B CN 115571931B
- Authority
- CN
- China
- Prior art keywords
- iridium
- solution
- exchange resin
- acid
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002253 acid Substances 0.000 title claims abstract description 69
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 28
- YNJJJJLQPVLIEW-UHFFFAOYSA-M [Ir]Cl Chemical compound [Ir]Cl YNJJJJLQPVLIEW-UHFFFAOYSA-M 0.000 claims abstract description 28
- IUJMNDNTFMJNEL-UHFFFAOYSA-K iridium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Ir+3] IUJMNDNTFMJNEL-UHFFFAOYSA-K 0.000 claims abstract description 26
- 239000002244 precipitate Substances 0.000 claims abstract description 22
- 239000007800 oxidant agent Substances 0.000 claims abstract description 21
- 230000001590 oxidative effect Effects 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000457 iridium oxide Inorganic materials 0.000 claims abstract description 17
- 239000002893 slag Substances 0.000 claims abstract description 16
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 14
- 230000001105 regulatory effect Effects 0.000 claims abstract description 7
- 238000007670 refining Methods 0.000 claims abstract description 5
- 238000004537 pulping Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 13
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 235000010288 sodium nitrite Nutrition 0.000 claims description 5
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 5
- ZJRXSAYFZMGQFP-UHFFFAOYSA-N barium peroxide Chemical compound [Ba+2].[O-][O-] ZJRXSAYFZMGQFP-UHFFFAOYSA-N 0.000 claims description 4
- XUXNAKZDHHEHPC-UHFFFAOYSA-M sodium bromate Chemical compound [Na+].[O-]Br(=O)=O XUXNAKZDHHEHPC-UHFFFAOYSA-M 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 abstract description 19
- 239000000047 product Substances 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- -1 platinum group metals Chemical class 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 73
- 238000001704 evaporation Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 9
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 150000002504 iridium compounds Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000007500 overflow downdraw method Methods 0.000 description 2
- 229910000575 Ir alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- SXRIPRHXGZHSNU-UHFFFAOYSA-N iridium rhodium Chemical compound [Rh].[Ir] SXRIPRHXGZHSNU-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of platinum group metals. The invention provides a method for preparing chloroiridium acid from pure iridium powder. The method comprises the following steps: refining treatment is carried out after the pure iridium powder reacts with a strong oxidant, so as to obtain iridium oxide slag; after the iridium oxide slag, water and an oxidant react, the pH value of the solution is regulated to obtain iridium hydroxide precipitate; adding water into the iridium hydroxide precipitate for pulping, and then reacting with hydrochloric acid solution to obtain chloroiridium acid solution; and (3) passing the chloroiridic acid solution through cation exchange resin to obtain the chloroiridic acid. The invention adopts a solid oxidation process, and the single impurity introduced adopts an oxidation precipitation and resin adsorption two-step removal technology, so that the whole process flow is shortened, the dissolution efficiency of iridium is improved, and the batch processing capacity is large; the quality of the chloroiridic acid product is higher than YS/T595-2006 chloroiridic acid industry standard, and the chloroiridic acid product is stable and reliable.
Description
Technical Field
The invention relates to the technical field of platinum group metals, in particular to a method for preparing chloroiridium acid from pure iridium powder.
Background
The high melting point and high stability of iridium make it of great importance in many special applications. For example, iridium was first used as nib material, and later on, injection needles, balance blades, compass holders, electrical contacts, etc. have been proposed; the iridium crucible can work for thousands of hours at 2100-2200 ℃, and can be used for growing refractory oxide crystals; the high-temperature oxidation resistance and thermoelectric property of iridium make an iridium/iridium rhodium thermocouple be the only noble metal temperature measuring material capable of measuring the high temperature reaching 2100 ℃ in the atmosphere; iridium may be used as a containment material for radioactive heat sources; anodic iridium oxide film is also a promising electrochromic material; ir-192 is a gamma ray source, which can be used for nondestructive inspection and radiochemical treatment; iridium is also an important alloying element, and some iridium alloys can be used in certain critical departments; iridium compounds also have their particular uses.
Chloroiridic acid is an important raw material for preparing other iridium compounds, and the preparation method mainly comprises a high-temperature chlorination method, an alkali fusion method and an electrolysis method. In the patent documents of patent numbers 201510847873.0 and 201510846643.2, an alkali fusion method is adopted to prepare chloroiridic acid, an iron crucible and a nickel crucible are adopted in the process, and as iron and nickel are corroded in the alkali fusion process, metal impurities are brought to pure iridium powder, and subsequent impurity removal is difficult; patent No. 201711042141.X, patent name "a method for preparing chloroiridic acid" adopts high temperature chlorination method to prepare chloroiridic acid, because chlorine in quartz tube only contacts with iridium powder on surface layer, so make internal iridium powder unable to react with chlorine fully, thus cause smelting effect of iridium powder bad, leaching efficiency of iridium powder is low; the patent number is 201010290275.5, the patent name is an electrochemical dissolution method of iridium powder, an electrolytic method is adopted to prepare chloroiridium acid, iridium powder is added into the anode region of a U-shaped electrolytic cell, hydrochloric acid solution is added into the electrolytic cell, the iridium powder is dissolved into the hydrochloric acid solution after electrification, the chloroiridium acid aqueous solution is filtered and distilled, and chloroiridium acid concentrate is obtained.
Therefore, research and development of the method for preparing the chloroiridic acid from the pure iridium powder, which can improve the dissolution efficiency of iridium and the quality of chloroiridic acid products and has simple process, has important significance.
Disclosure of Invention
The invention aims to provide a method for preparing chloroiridium acid from pure iridium powder aiming at the defects of the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing chloroiridium acid from pure iridium powder, which comprises the following steps:
1) Refining treatment is carried out after the pure iridium powder reacts with a strong oxidant, so as to obtain iridium oxide slag;
2) After the iridium oxide slag, water and an oxidant react, the pH value of the solution is regulated to obtain iridium hydroxide precipitate;
3) Adding water into the iridium hydroxide precipitate for pulping, and then reacting with hydrochloric acid solution to obtain chloroiridium acid solution;
4) And (3) passing the chloroiridic acid solution through cation exchange resin to obtain the chloroiridic acid.
Preferably, the strong oxidant in the step 1) is one or more of sodium chlorate, sodium bromate, sodium peroxide, barium peroxide and sodium nitrite; the mass ratio of the pure iridium powder to the strong oxidant is 1:0.5 to 5.
Preferably, the temperature of the reaction in the step 1) is 450-750 ℃, and the reaction time is 30-120 min.
Preferably, the mass ratio of the water in the step 2) to the pure iridium powder in the step 1) is 1-10: 1.
Preferably, the temperature of the reaction in the step 2) is 40-80 ℃, and the reaction time is 30-120 min.
Preferably, the oxidant in the step 2) is nitric acid, hydrogen peroxide, chlorine, sodium chlorate solution or sodium hypochlorite solution; the mass concentration of the nitric acid is 60-70%, the mass concentration of the hydrogen peroxide is 25-35%, and the mass concentrations of the sodium chlorate solution and the sodium hypochlorite solution are 5-15% independently; the mass ratio of the oxidant to the pure iridium powder in the step 1) is 0.1-5: 1.
Preferably, in the step 2), the pH value of the solution is adjusted to 6-8 by adopting a sodium hydroxide solution with the mass fraction of 18-22%.
Preferably, the volume ratio of iridium hydroxide precipitate to water in step 3) is 1:1 to 2; the mass fraction of the hydrochloric acid solution is 14-16%; the pH value of the solution is regulated to 0.5-2.
Preferably, the cation exchange resin in the step 4) is one or two of CH-90Na exchange resin, T-IRR exchange resin, 732 exchange resin, T-62MP exchange resin and T-42H exchange resin; the volume mass ratio of the cation exchange resin to the pure iridium powder in the step 1) is 1-3 mL:1g.
Preferably, the flow rate of the chloroiridium acid solution passing through the cation exchange resin in the step 4) is 100-500 mL/min.
The beneficial effects of the invention include the following points:
1) The invention adopts a solid oxidation process, and the single impurity introduced adopts an oxidation precipitation and resin adsorption two-step removal technology, so that the whole process flow is shortened, the dissolution efficiency of iridium is improved, and the batch processing capacity is large.
2) The quality of the chloroiridic acid product is higher than the YS/T595-2006 chloroiridic acid industry standard, and the chloroiridic acid product is stable and reliable.
Detailed Description
The invention provides a method for preparing chloroiridium acid from pure iridium powder, which comprises the following steps:
1) Refining treatment is carried out after the pure iridium powder reacts with a strong oxidant, so as to obtain iridium oxide slag;
2) After the iridium oxide slag, water and an oxidant react, the pH value of the solution is regulated to obtain iridium hydroxide precipitate;
3) Adding water into the iridium hydroxide precipitate for pulping, and then reacting with hydrochloric acid solution to obtain chloroiridium acid solution;
4) And (3) passing the chloroiridic acid solution through cation exchange resin to obtain the chloroiridic acid.
In the invention, the strong oxidant in the step 1) is one or more of sodium chlorate, sodium bromate, sodium peroxide, barium peroxide and sodium nitrite; the mass ratio of the pure iridium powder to the strong oxidant is 1:0.5 to 5, preferably 1:1.5 to 4, more preferably 1:2 to 3.5, more preferably 1:3.
In the invention, the pure iridium powder and the strong oxidant in the step 1) are uniformly mixed and then are put into an evaporation dish to react in a muffle furnace.
In the present invention, the temperature of the reaction in step 1) is 450 to 750 ℃, preferably 500 to 700 ℃, further preferably 550 to 650 ℃, and more preferably 600 ℃; the reaction time is 30 to 120 minutes, preferably 50 to 100 minutes, more preferably 70 to 80 minutes, and still more preferably 75 minutes.
In the invention, the refining treatment in the step 1) is to take out the evaporating dish, cool the evaporating dish and then crush the evaporating dish.
In the invention, the mass ratio of the water in the step 2) to the pure iridium powder in the step 1) is 1-10: 1, preferably 3 to 8:1, more preferably 5 to 7:1, more preferably 6:1.
In the present invention, the water of step 2) is preferably deionized water.
In the present invention, the temperature of the reaction in step 2) is 40 to 80 ℃, preferably 50 to 70 ℃, further preferably 55 to 65 ℃, and more preferably 60 ℃; the reaction time is 30 to 120 minutes, preferably 50 to 100 minutes, more preferably 70 to 80 minutes, and still more preferably 75 minutes.
In the invention, the oxidant in the step 2) is nitric acid, hydrogen peroxide, chlorine, sodium chlorate solution or sodium hypochlorite solution; the mass concentration of the nitric acid is 60 to 70%, preferably 62 to 68%, more preferably 64 to 66%, and even more preferably 65%; the mass concentration of the hydrogen peroxide is 25-35%, preferably 28-32%, and more preferably 30%; the mass concentration of the sodium chlorate solution and the sodium hypochlorite solution is independently 5-15%, preferably 8-12%, more preferably 10-12%, and even more preferably 10%; the mass ratio of the oxidant to the pure iridium powder in the step 1) is 0.1-5: 1, preferably 1.1 to 4:1, more preferably 2.1 to 3:1, more preferably 2.5:1.
In the step 2), the pH value of the solution is adjusted to 6-8 by adopting a sodium hydroxide solution with the mass fraction of 18-22%, and the mass fraction of the sodium hydroxide solution is preferably 19-21%, and more preferably 20%; the pH of the solution is preferably 6 to 7, more preferably 7.
In the invention, the step 2) is carried out after the pH value of the solution is regulated, and the solution is also filtered and washed.
In the invention, the volume ratio of the iridium hydroxide precipitate to the water in the step 3) is 1:1 to 2, preferably 1:1 to 1.5, more preferably 1:1, a step of; the mass fraction of the hydrochloric acid solution is 14-16%, preferably 14-15%, and more preferably 15%; the pH of the solution is adjusted to 0.5 to 2, preferably 1 to 1.5, and more preferably 1.
In the invention, the hydrochloric acid solution in the step 3) can dissolve iridium hydroxide precipitate and can also adjust the pH value of the solution.
In the invention, the cation exchange resin in the step 4) is one or two of CH-90Na exchange resin, T-IRR exchange resin, 732 exchange resin, T-62MP exchange resin and T-42H exchange resin; the volume mass ratio of the cation exchange resin to the pure iridium powder in the step 1) is 1-3 mL:1g, preferably 1.5 to 2.5mL:1g, more preferably 2mL:1g.
In the present invention, the flow rate of the chloroiridium acid solution passing through the cation exchange resin in the step 4) is 100 to 500mL/min, preferably 200 to 400mL/min, more preferably 250 to 350mL/min, and even more preferably 300mL/min.
In the invention, the step 4) of the chloroiridium acid solution is performed with cation exchange resin to obtain the high-purity chloroiridium acid solution.
In the invention, the mode of obtaining the chloroiridic acid in the step 4) is to concentrate or decompress and distill the chloroiridic acid solution with high purity.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Uniformly mixing 500g of pure iridium powder, 300g of sodium chlorate, 500g of sodium bromate and 200g of sodium peroxide, putting into an evaporation pan, then reacting in a muffle furnace at 500 ℃ for 60min, taking out the evaporation pan, cooling, and crushing reactants to obtain iridium oxide slag; adding iridium oxide slag, 3000g deionized water and 1000g hydrogen peroxide with mass concentration of 30% into a 10L reaction kettle, reacting for 30min at 80 ℃, adjusting the pH value of the solution to 7 by adopting a sodium hydroxide solution with mass fraction of 18% after the reaction is finished, and then sequentially filtering and washing by deionized water to obtain iridium hydroxide precipitate.
The volume ratio of iridium hydroxide sediment to water is 1:1, adding water into iridium hydroxide precipitate to slurry, adding hydrochloric acid solution with the mass fraction of 14% to dissolve, and simultaneously adjusting the pH value of the solution to 0.5 to obtain chloroiridium acid solution; the chloroiridium acid solution was passed through 1000mL732 exchange resin at a flow rate of 100mL/min to obtain a high purity iridium chloride solution.
And (3) carrying out reduced pressure distillation on the high-purity iridium chloride solution to obtain chloroiridic acid.
1426.13G of chloroiridic acid with 34.86% iridium content is prepared in the embodiment, the direct yield of iridium is 99.43%, and the quality of the chloroiridic acid product is superior to YS/T595-2006 chloroiridic acid industry standard.
Example 2
Uniformly mixing 1000g of pure iridium powder, 500g of sodium chlorate and 500g of barium peroxide, putting the mixture into an evaporation pan, then reacting for 80min in a muffle furnace at 650 ℃, taking out the evaporation pan, cooling, crushing reactants, and obtaining iridium oxide slag; adding iridium oxide slag, 8000g of deionized water and 1000g of sodium hypochlorite solution with the mass concentration of 10% into a 20L reaction kettle, reacting for 100min at 40 ℃, adjusting the pH value of the solution to 6 by adopting a sodium hydroxide solution with the mass fraction of 22% after the reaction is finished, and then sequentially filtering and washing by using deionized water to obtain iridium hydroxide precipitate.
The volume ratio of iridium hydroxide sediment to water is 1:1.5, adding water into the iridium hydroxide precipitate to slurry, adding hydrochloric acid solution with the mass fraction of 16% to dissolve, and simultaneously adjusting the pH value of the solution to 2 to obtain chloroiridium acid solution; the chloroiridium acid solution is passed through 3000mLCH-90Na exchange resin at a flow rate of 200mL/min to obtain high-purity iridium chloride solution.
And (3) carrying out reduced pressure distillation on the high-purity iridium chloride solution to obtain chloroiridic acid.
2834.52G of chloroiridic acid with the iridium content of 35.11% is prepared in the embodiment, the direct yield of iridium is 99.52%, and the quality of the chloroiridic acid product is superior to YS/T595-2006 chloroiridic acid industry standard.
Example 3
100G of pure iridium powder, 100g of sodium chlorate and 200g of sodium nitrite are uniformly mixed and then put into an evaporation pan, then reacted in a muffle furnace at 450 ℃ for 40min, the evaporation pan is taken out for cooling, and reactants are crushed to obtain iridium oxide slag; adding iridium oxide slag, 1000g of deionized water and 300g of nitric acid with the mass concentration of 65% into a 5L reaction kettle, reacting for 80min at 50 ℃, adjusting the pH value of the solution to 8 by adopting a sodium hydroxide solution with the mass fraction of 20% after the reaction is finished, and then sequentially filtering and washing by using deionized water to obtain iridium hydroxide precipitate.
The volume ratio of iridium hydroxide sediment to water is 1:2, adding water into the iridium hydroxide precipitate to slurry, adding hydrochloric acid solution with the mass fraction of 15% to dissolve the iridium hydroxide precipitate, and simultaneously adjusting the pH value of the solution to be 1 to obtain chloroiridium acid solution; the chloroiridium acid solution is passed through 100mL of T-IRR exchange resin at a flow rate of 400mL/min, and then the high-purity iridium chloride solution is obtained.
The high-purity iridium chloride solution is concentrated to obtain the chloroiridic acid.
247.67G of chloroiridic acid with the iridium content of 40.11% is prepared in the embodiment, the direct yield of iridium is 99.34%, and the quality of the chloroiridic acid product detected by the embodiment is superior to YS/T595-2006 chloroiridic acid industry standard.
Example 4
Uniformly mixing 5000g of pure iridium powder, 3000g of sodium nitrite and 4500g of sodium peroxide, putting into an evaporation pan, then reacting for 120min in a muffle furnace at 750 ℃, taking out the evaporation pan, cooling, crushing reactants, and obtaining iridium oxide slag; adding iridium oxide slag, 8000g of deionized water and 500g of sodium chlorate solution with the mass concentration of 10% into a 20L reaction kettle, reacting for 120min at 70 ℃, adjusting the pH value of the solution to 7 by adopting a sodium hydroxide solution with the mass fraction of 19% after the reaction is finished, and then sequentially filtering and washing by using deionized water to obtain iridium hydroxide precipitate.
The volume ratio of iridium hydroxide sediment to water is 1:2, adding water into the iridium hydroxide precipitate to slurry, adding hydrochloric acid solution with the mass fraction of 15% to dissolve the iridium hydroxide precipitate, and simultaneously adjusting the pH value of the solution to 2 to obtain chloroiridium acid solution; the chloroiridium acid solution is passed through 5000mL of T-62MP exchange resin at a flow rate of 500mL/min to obtain a high-purity iridium chloride solution.
And (3) carrying out reduced pressure distillation on the high-purity iridium chloride solution to obtain chloroiridic acid.
12436.95G of chloroiridic acid with the iridium content of 40.05% is prepared in the embodiment, the direct yield of iridium is 99.62%, and the quality of the chloroiridic acid product is superior to YS/T595-2006 chloroiridic acid industry standard through detection.
As can be seen from examples 1 to 4: when the pure iridium powder is used for preparing chloroiridic acid, the direct yield of iridium exceeds 99%, and the quality of chloroiridic acid products is superior to YS/T595-2006 chloroiridic acid industry standard.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (3)
1. The method for preparing chloroiridium acid from pure iridium powder is characterized by comprising the following steps:
1) Refining treatment is carried out after the pure iridium powder reacts with a strong oxidant, so as to obtain iridium oxide slag;
2) After the iridium oxide slag, water and an oxidant react, the pH value of the solution is regulated to obtain iridium hydroxide precipitate;
3) Adding water into the iridium hydroxide precipitate for pulping, and then reacting with hydrochloric acid solution to obtain chloroiridium acid solution;
4) The chloroiridium acid solution passes through cation exchange resin to obtain chloroiridium acid;
The strong oxidant is one or more of sodium chlorate, sodium bromate, sodium peroxide, barium peroxide and sodium nitrite; the mass ratio of the pure iridium powder to the strong oxidant is 1:0.5-5;
The oxidant is nitric acid, hydrogen peroxide, chlorine, sodium chlorate solution or sodium hypochlorite solution; the mass concentration of nitric acid is 60-70%, the mass concentration of hydrogen peroxide is 25-35%, and the mass concentrations of sodium chlorate solution and sodium hypochlorite solution are 5-15% independently; the mass ratio of the oxidant to the pure iridium powder in the step 1) is 0.1-5:1;
The cation exchange resin is one or two of CH-90Na exchange resin, T-IRR exchange resin, 732 exchange resin, T-62MP exchange resin and T-42H exchange resin; the volume mass ratio of the cation exchange resin to the pure iridium powder in the step 1) is 1-3 mL/1 g;
The flow rate of the chloroiridium acid solution passing through the cation exchange resin is 100-500 mL/min;
In the step 1), the reaction temperature is 450-750 ℃ and the reaction time is 30-120 min;
In the step 2), the mass ratio of the water to the pure iridium powder in the step 1) is 1-10:1;
in the step 2), the reaction temperature is 40-80 ℃ and the reaction time is 30-120 min.
2. The method according to claim 1, wherein in the step 2), a sodium hydroxide solution with a mass fraction of 18-22% is used to adjust the pH of the solution to 6-8.
3. The method according to claim 2, wherein the volume ratio of iridium hydroxide precipitate to water in step 3) is 1:1-2; the mass fraction of the hydrochloric acid solution is 14-16%; the pH value of the solution is regulated to 0.5-2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211380379.4A CN115571931B (en) | 2022-11-04 | 2022-11-04 | Method for preparing chloroiridic acid from pure iridium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211380379.4A CN115571931B (en) | 2022-11-04 | 2022-11-04 | Method for preparing chloroiridic acid from pure iridium powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115571931A CN115571931A (en) | 2023-01-06 |
| CN115571931B true CN115571931B (en) | 2024-05-28 |
Family
ID=84588154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211380379.4A Active CN115571931B (en) | 2022-11-04 | 2022-11-04 | Method for preparing chloroiridic acid from pure iridium powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115571931B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103302298A (en) * | 2013-06-03 | 2013-09-18 | 贵研资源（易门）有限公司 | Method for separating and purifying iridium |
| CN107758752A (en) * | 2017-10-31 | 2018-03-06 | 中南大学 | A kind of method for preparing chloro-iridic acid |
| CN108421986A (en) * | 2018-05-17 | 2018-08-21 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity iridium powder |
| CN112357979A (en) * | 2020-11-16 | 2021-02-12 | 沈阳有色金属研究院有限公司 | Method for directly preparing chloro-iridic acid from iridium-containing waste material |
-
2022
- 2022-11-04 CN CN202211380379.4A patent/CN115571931B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103302298A (en) * | 2013-06-03 | 2013-09-18 | 贵研资源（易门）有限公司 | Method for separating and purifying iridium |
| CN107758752A (en) * | 2017-10-31 | 2018-03-06 | 中南大学 | A kind of method for preparing chloro-iridic acid |
| CN108421986A (en) * | 2018-05-17 | 2018-08-21 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity iridium powder |
| CN112357979A (en) * | 2020-11-16 | 2021-02-12 | 沈阳有色金属研究院有限公司 | Method for directly preparing chloro-iridic acid from iridium-containing waste material |
Non-Patent Citations (2)
| Title |
|---|
| 从有机废液中回收铱的工艺;贺小塘;刘伟平;吴喜龙;常桥稳;王欢;韩守礼;;贵金属;20100515(第02期);第6-9页 * |
| 铂铱合金的分离与提纯;李富荣;中国资源综合利用;20010825(第08期);第12-14页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115571931A (en) | 2023-01-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107150128B (en) | Preparation method of high-purity platinum powder | |
| CN112705727B (en) | Preparation method of high-purity rhodium powder | |
| CN111112637A (en) | Method for preparing 5N-grade high-purity iridium powder | |
| CN114105229B (en) | Preparation method of high-purity iridium trichloride | |
| RO126480B1 (en) | Process for obtaining gold and silver | |
| CN113337723A (en) | Method for separating and extracting silver, palladium, copper and germanium from silver separating slag | |
| CN115571931B (en) | Method for preparing chloroiridic acid from pure iridium powder | |
| CN101319278A (en) | Quick dissolution method for high-purity rhodium material | |
| CN109504858B (en) | Method for preparing indium hydroxide by using ITO waste material | |
| CN111172413A (en) | Method for producing high-purity metal scandium by using low-purity scandium oxide concentrate | |
| CN108555313B (en) | Preparation method of medical high-purity platinum powder | |
| CN115536081B (en) | Method for preparing chloroiridium acid from multiple platinum group metal materials | |
| CN108658133B (en) | Rapid dissolving method of insoluble metal iridium | |
| CN114350971B (en) | Method for recovering rhodium from rhodium-containing ammonium chloroplatinate precipitation slag | |
| CN101628730B (en) | Method for preparing photographic-grade silver nitrate through one-time crystallization | |
| CN107827149B (en) | A kind of production method of the sodium stannate of low leaded antimony arsenic iron tramp | |
| US3988150A (en) | Process for extraction of gallium from sodium aluminate liquors | |
| CN116283552B (en) | Refining method of oxalic acid | |
| CN114453589B (en) | Preparation method of high-purity gold | |
| CN117206536A (en) | Preparation method of high-purity ruthenium powder | |
| CN117585687A (en) | Method for synthesizing gold potassium cyanide from gold plating waste | |
| CN114878486A (en) | Chemical analysis method for measuring chloride ion content in crude copper | |
| CN117865243A (en) | Method for directly preparing corresponding compound by extracting iridium and ruthenium from iridium ruthenium alloy ingot | |
| Baxter et al. | A REVISION OF THE ATOMIC WEIGHT OF LEAD. THE ANALYSIS OF LEAD BROMIDE AND CHLORIDE.[THIRD PAPER.] | |
| CN116445721A (en) | Reworking treatment method for unqualified rhodium product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant |