CN110016555A - Precious metal separation method of purification in solution - Google Patents
Precious metal separation method of purification in solution Download PDFInfo
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- CN110016555A CN110016555A CN201910398478.7A CN201910398478A CN110016555A CN 110016555 A CN110016555 A CN 110016555A CN 201910398478 A CN201910398478 A CN 201910398478A CN 110016555 A CN110016555 A CN 110016555A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention relates to noble metal secondary resource field of comprehensive utilization, and in particular to precious metal separation method of purification in solution.Precious metal separation method of purification in solution successively carries out: the A, pre-treatment of precious metal solution as follows；B, it adsorbs；C, the cleaning of adsorption column；D, rhodium elution and refining；E, platinum palladium separates；F, the regeneration of adsorbent material.The noble metal rate of recovery of the present invention is high, and the production cycle of rhodium shortens, and after preferential separate rhodium, the interference of no rhodium, platinum, the separation of palladium are simple, and production procedure is short, and high production efficiency is increased economic efficiency.
Description
Technical field
The present invention relates to noble metal secondary resource field of comprehensive utilization, and in particular to precious metal separation purification side in solution
Method.
Background technique
Noble metal has gold, silver and platinum group metal totally 8 elements, and wherein platinum family gold includes platinum, palladium, rhodium, iridium, ruthenium and osmium 6
Element.Platinum group metal chemical property is similar, and hydrochloric acid medium platinum group metal aqueous solution existence is extremely complex, and platinum family element chlorine is matched
Object, hydrate quantity are very more, thermodynamic instability, cause in solution platinum group metal to be separated from each other extremely difficult.Utilize platinum family
The different oxidation state of element and kinetics carry out being separated from each other between platinum group metal, hand over frequently with oxidation distillation, ion
It changes, solution extraction, the methods of chemical precipitation are separated.
Precious metal separation sequence in solution: palladium-platinum-rhodium or platinum-palladium-rhodium, since the chemical property of rhodium is special, the refining of rhodium
Be normally placed at process finally, separating-purifying rhodium long flow path, complex process, return period are long, the rate of recovery of rhodium are reduced, due to rhodium
Price fluctuation it is big, commercial risks is also larger.The advanced preferential separating-purifying of rhodium adsorbent material high selection is used in hydrochloric acid solution
Rhodium reduces the dispersion of rhodium, improves the rate of recovery of rhodium, substantially reduces overstocking for rhodium in production process, reduces risk.Separate rhodium
Afterwards, the interference of rhodium is reduced, the separation of platinum palladium is simpler, improves the rate of recovery of platinum palladium.
Chinese patent 201510797487.5 is related to precious metal smelting technical field, discloses a kind of molten from platinum group metal
The method that platinum group metal is separated in liquid, the solution of platinum group metal is first added in reactor after concentration, is diluted with water to molten by it
The acidity of liquid is 1.5-3mol/L；The temperature of solution is adjusted to 60-70 DEG C again, is slowly introducing SO2Gas adjusts reactor
Reduction potential is 210-230mv, and constant potential reacts 0.5-1h, carries out reduction reaction, solution after reaction to platinum group metallic solution
In Pt, Pd be reduced into simple substance and be precipitated from solution, Rh, Ir are present in after reduction in liquid；The present invention passes through control solution acid
The factors such as degree, reaction temperature and end time current potential carry out Reduced separating to platinum group metal in golden extraction raffinate is extracted.By SO2Reduction,
The rate of deposition of Pt, Pd are up to 98% or more, and the rate of deposition of Rh, Ir are less than 8%.This method has process flow short, easy to operate,
The advantages that production cost is low, and environmental pollution is small.
Summary of the invention
It is an object of the invention to overcome the deficiency of the above-mentioned prior art, using the preferential separate rhodium-warp of advanced adsorbent material
The method of allusion quotation platinum precipitation palladium technology separating-purifying noble metal from solution, this method noble metal rate of recovery is high, the production cycle of rhodium
Shorten, after preferential separate rhodium, the interference of no rhodium, platinum, the separation of palladium are simple, and production procedure is short, high production efficiency, improve economic effect
Benefit.
To achieve the goals above, the technical solution of the present invention is as follows:
Precious metal separation method of purification in solution successively carries out as follows:
A, the pre-treatment of precious metal solution:
It is 4-6mol/L with the pure hydrochloric acid adjustment solubilized precious metal liquid acidity of chemistry, adjusts precious metal solution current potential with current potential regulator
For 500-900mV, it is then heated to 80-95 DEG C, soaking time 60-240 minutes, keeps the rhodium Chloro complex in precious metal solution to be
RhCl6 3-, the concentration control of rhodium is 1-5g/L in precious metal solution；
B, it adsorbs:
Adsorbent material is that silica gel is loaded with active function groups, and active function groups are 1- ethyl pyridinium chloride, active function groups load
Amount is 1.0-1.2mmol/g, and rhodium in active function groups energy high-selectivity adsorption filtrate, functional silicon material particle size is 140-500 μm,
Aperture is 100-200；3 glass adsorption column series connection, every absorption column volume are 100ml, are equipped with 80-100 grams in splitter
Adsorbent material；The precious metal solution room temperature of pre-treatment is flowed through into adsorption column, control adsorption flow rate is 10-30ml/min, adsorbs rhodium
Tail washings afterwards is put into platinum, in palladium separation vessel；
C, the cleaning of adsorption column:
Adsorption column is washed with 6 mol/L hydrochloric acid solutions, and the liquid-to-solid ratio (ml/g) of hydrochloric acid and adsorbent material is 3-5:1, washing lotion and is inhaled
Attached platinum palladium tail washings merges；Then adsorption column is washed with clear water, the liquid-to-solid ratio (ml/g) of clear water and adsorbent material is 1-2:1, is removed
Extra hydrochloric acid；
D, rhodium elution and refining:
With the KCl solution elution adsorption column of 3-5 mol/L, the liquid-to-solid ratio (ml/g) of KCl solution and adsorbent material is 4-6:1；So
Afterwards with the pH to 10-12 of NaOH solution adjustment rhodium eluent, Rh is generated2O3.xH2O, clear water washing is dry, leads to hydrogen reduction, obtains
The rate of recovery of 99.95% sponge rhodium powder, rhodium is greater than 92%；
E, platinum palladium separates:
Tail washings after adsorbing rhodium, using classical ammonium salt sedimentation separating-purifying platinum, palladium, obtaining purity is 99.95% sponge
Platinum, palladium product, the rate of recovery of platinum are greater than 98%, and the rate of recovery of palladium is greater than 99%；
F, the regeneration of adsorbent material:
Adsorption column is washed with clear water, and the liquid-to-solid ratio (ml/g) of clear water and adsorbent material is 3-5:1, then molten with 6 mol/L hydrochloric acid
The liquid-to-solid ratio (ml/g) of liquid equilibrium adsorption column, hydrochloric acid solution and adsorbent material is 1-2:1；The adsorbent material regenerated is for next time
Separating-purifying noble metal in precious metal solution.
The current potential regulator is Cl2、H2O2, one of NaClO.
Beneficial effects of the present invention:
1, active group of the present invention has high selection absorption to the rhodium in precious metal solution, and adsorption rate is high, and adsorption capacity is big etc.
Characteristic.
2, the noble metal rate of recovery of the present invention is high, and the rate of recovery of platinum is greater than 98%, and the rate of recovery of palladium is greater than 99%, the rate of recovery of rhodium
Greater than 92%.
3, the production cycle of rhodium of the present invention shortens, and reduces rhodium price fluctuation risk.
4, after the preferential separate rhodium of the present invention, the interference of no rhodium, platinum, the separation of palladium are simple, and production procedure is short, production efficiency
Height is increased economic efficiency.
Specific embodiment
Embodiment 1
Precious metal separation method of purification in solution successively carries out as follows:
A, the pre-treatment of precious metal solution:
Solubilized precious metal liquid acidity is adjusted with the pure hydrochloric acid of chemistry, leads to Cl2Oxidation 4 hours, then heat precious metal solution to 80 DEG C,
Soaking time 60 minutes；The acidity of precious metal solution is 4mol/L after processing, and the concentration of noble metal is Pt4.5g/L, Pd12.7g/
L, Rh1.0g/L, the current potential of precious metal solution are 500mV, volume 1000ml；
B, it adsorbs:
Adsorbent material is that silica gel is loaded with active function groups, and active function groups are 1- ethyl pyridinium chloride, active function groups load
Amount is 1.0mmol/g, and rhodium in active function groups energy high-selectivity adsorption filtrate, functional silicon material particle size is 140-500 μm, aperture
For 100-200；3 glass adsorption column series connection, every absorption column volume are 100ml, and 80 grams of adsorbent materials are housed in splitter；
The precious metal solution room temperature of pre-treatment is flowed through into adsorption column, control adsorption flow rate is 10ml/min, and the tail washings after adsorbing rhodium is put into
In platinum, palladium separation vessel；
C, the cleaning of adsorption column:
Adsorption column is washed with the 6 mol/L hydrochloric acid solutions of 240ml, washing lotion merges with absorption platinum palladium tail washings；Then clear with 80ml
Water washing adsorption column removes extra hydrochloric acid；
D, rhodium elution and refining:
Adsorption column is eluted with the KCl solution of the 3mol/L of 320ml, it is raw then with the pH to 10 of NaOH solution adjustment rhodium eluent
At Rh2O3.xH2O, clear water washing is dry, leads to hydrogen reduction, obtains 99.95% 0.93 gram of sponge rhodium powder, the rate of recovery 93. of rhodium
00%；
E, platinum palladium separates:
Tail washings after adsorbing rhodium, using classical ammonium salt sedimentation separating-purifying platinum, palladium, obtaining purity is 99.95% spongy platinum
4.42 grams, the rate of recovery of platinum is 98.22%, and obtaining purity is 12.59 grams of 99.95% palladium sponge, the rate of recovery 99.13% of palladium；
F, the regeneration of adsorbent material:
Adsorption column is washed with the clear water of 240ml, then the use 6mol/L hydrochloric acid solution equilibrium adsorption column of 80ml, the absorption regenerated
Material is used for separating-purifying noble metal in next precious metal solution.
Embodiment 2
Precious metal separation method of purification in solution successively carries out as follows:
A, the pre-treatment of precious metal solution:
Solubilized precious metal liquid acidity is adjusted with the pure hydrochloric acid of chemistry, H is added2O2Then oxidation is heated precious metal solution to 90 DEG C, is protected
150 minutes warm time；The acidity of precious metal solution is 5mol/L after processing, and the concentration of noble metal is Pt5.4g/L, Pd13.4g/
L, Rh3.0g/L, the current potential of precious metal solution are 700mV, volume 1000ml；
B, it adsorbs:
Adsorbent material is that silica gel is loaded with active function groups, and active function groups are 1- ethyl pyridinium chloride, active function groups load
Amount is 1.1mmol/g, and rhodium in active function groups energy high-selectivity adsorption filtrate, functional silicon material particle size is 140-500 μm, aperture
For 100-200；3 glass adsorption column series connection, every absorption column volume are 100ml, and 90 grams of adsorbent materials are housed in splitter；
The precious metal solution room temperature of pre-treatment is flowed through into adsorption column, control adsorption flow rate is 20ml/min, and the tail washings after adsorbing rhodium is put into
In platinum, palladium separation vessel；
C, the cleaning of adsorption column:
Adsorption column is washed with the 6 mol/L hydrochloric acid solutions of 360ml, washing lotion merges with absorption platinum palladium tail washings；Then clear with 135ml
Water washing adsorption column removes extra hydrochloric acid；
D, rhodium elution and refining:
Adsorption column is eluted with the KCl solution of the 4mol/L of 450ml, it is raw then with the pH to 11 of NaOH solution adjustment rhodium eluent
At Rh2O3.xH2O, clear water washing is dry, leads to hydrogen reduction, obtains 99.95% 2.8 grams of sponge rhodium powder, the rate of recovery 93. 33% of rhodium；
E, platinum palladium separates:
Tail washings after adsorbing rhodium, using classical ammonium salt sedimentation separating-purifying platinum, palladium, obtaining purity is 99.95% spongy platinum
5.31 grams, the rate of recovery of platinum is 98.33%, and obtaining purity is 13.29 grams of 99.95% palladium sponge, the rate of recovery 99.18% of palladium；
F, the regeneration of adsorbent material:
Adsorption column is washed with the clear water of 360ml, then the use 6mol/L hydrochloric acid solution equilibrium adsorption column of 135ml, the suction regenerated
Enclosure material is used for separating-purifying noble metal in next precious metal solution.
Embodiment 3
Precious metal separation method of purification in solution successively carries out as follows:
A, the pre-treatment of precious metal solution:
Solubilized precious metal liquid acidity is adjusted with the pure hydrochloric acid of chemistry, NaClO oxidation is added, then heats precious metal solution to 95 DEG C,
Soaking time 240 minutes；The acidity of precious metal solution is 6mol/L after processing, and the concentration of noble metal is Pt6.3g/L,
Pd15.1g/L, Rh5.0g/L, the current potential of precious metal solution are 900mV, volume 1000ml；
B, it adsorbs:
Adsorbent material is that silica gel is loaded with active function groups, and active function groups are 1- ethyl pyridinium chloride, active function groups load
Amount is 1.2mmol/g, and rhodium in active function groups energy high-selectivity adsorption filtrate, functional silicon material particle size is 140-500 μm, aperture
For 100-200；3 glass adsorption column series connection, every absorption column volume are 100ml, and 100 grams of adsorbent materials are housed in splitter；
The precious metal solution room temperature of pre-treatment is flowed through into adsorption column, control adsorption flow rate is 30ml/min, and the tail washings after adsorbing rhodium is put into
In platinum, palladium separation vessel；
C, the cleaning of adsorption column:
Adsorption column is washed with the 6mol/L hydrochloric acid solution of 500ml, washing lotion merges with absorption platinum palladium tail washings；Then clear with 200ml
Water washing adsorption column removes extra hydrochloric acid；
D, rhodium elution and refining:
Adsorption column is eluted with the KCl solution of the 5mol/L of 600ml, it is raw then with the pH to 12 of NaOH solution adjustment rhodium eluent
At Rh2O3.xH2O, clear water washing is dry, leads to hydrogen reduction, obtains 99.95% 4.67 grams of sponge rhodium powder, the rate of recovery 93.40% of rhodium；
E, platinum palladium separates:
Tail washings after adsorbing rhodium, using classical ammonium salt sedimentation separating-purifying platinum, palladium, obtaining purity is 99.95% spongy platinum
3.21 grams, the rate of recovery of platinum is 98.57%, and obtaining purity is 14.98 grams of 99.95% palladium sponge, the rate of recovery 99.21% of palladium；
F, the regeneration of adsorbent material:
Adsorption column is washed with the clear water of 500ml, then the use 6mol/L hydrochloric acid solution equilibrium adsorption column of 200ml, the suction regenerated
Enclosure material is used for separating-purifying noble metal in next precious metal solution.
Claims (2)
1. precious metal separation method of purification in solution, which is characterized in that successively carry out as follows:
A, the pre-treatment of precious metal solution:
It is 4-6mol/L with the pure hydrochloric acid adjustment solubilized precious metal liquid acidity of chemistry, adjusts precious metal solution current potential with current potential regulator
For 500-900mV, it is then heated to 80-95 DEG C, soaking time 60-240 minutes, keeps the rhodium Chloro complex in precious metal solution to be
RhCl6 3-, the concentration control of rhodium is 1-5g/L in precious metal solution；
B, it adsorbs:
Adsorbent material is that silica gel is loaded with active function groups, and active function groups are 1- ethyl pyridinium chloride, active function groups load
Amount is 1.0-1.2mmol/g, and rhodium in active function groups energy high-selectivity adsorption filtrate, functional silicon material particle size is 140-500 μm,
Aperture is 100-200；3 glass adsorption column series connection, every absorption column volume are 100ml, are equipped with 80-100 grams in splitter
Adsorbent material；The precious metal solution room temperature of pre-treatment is flowed through into adsorption column, control adsorption flow rate is 10-30ml/min, adsorbs rhodium
Tail washings afterwards is put into platinum, in palladium separation vessel；
C, the cleaning of adsorption column:
Adsorption column is washed with 6 mol/L hydrochloric acid solutions, and the liquid-to-solid ratio (ml/g) of hydrochloric acid and adsorbent material is 3-5:1, washing lotion and is inhaled
Attached platinum palladium tail washings merges；Then adsorption column is washed with clear water, the liquid-to-solid ratio (ml/g) of clear water and adsorbent material is 1-2:1, is removed
Extra hydrochloric acid；
D, rhodium elution and refining:
With the KCl solution elution adsorption column of 3-5 mol/L, the liquid-to-solid ratio (ml/g) of KCl solution and adsorbent material is 4-6:1；So
Afterwards with the pH to 10-12 of NaOH solution adjustment rhodium eluent, Rh is generated2O3.xH2O, clear water washing is dry, leads to hydrogen reduction, obtains
The rate of recovery of 99.95% sponge rhodium powder, rhodium is greater than 92%；
E, platinum palladium separates:
Tail washings after adsorbing rhodium, using classical ammonium salt sedimentation separating-purifying platinum, palladium, obtaining purity is 99.95% sponge
Platinum, palladium product, the rate of recovery of platinum are greater than 98%, and the rate of recovery of palladium is greater than 99%；
F, the regeneration of adsorbent material:
Adsorption column is washed with clear water, and the liquid-to-solid ratio (ml/g) of clear water and adsorbent material is 3-5:1, then molten with 6 mol/L hydrochloric acid
The liquid-to-solid ratio (ml/g) of liquid equilibrium adsorption column, hydrochloric acid solution and adsorbent material is 1-2:1；The adsorbent material regenerated is for next time
Separating-purifying noble metal in precious metal solution.
2. precious metal separation method of purification in solution according to claim 1, which is characterized in that the current potential regulator is
Cl2、H2O2, one of NaClO.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430376A (en) * | 2021-07-06 | 2021-09-24 | 湖南省南铂新材料有限公司 | Method for efficiently separating noble metals in solution and preparing high-purity noble metals |
| CN115418490A (en) * | 2022-09-16 | 2022-12-02 | 贵研资源（易门）有限公司 | Method for recovering platinum and palladium from waste liquid containing trace precious metals |
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| CN1493706A (en) * | 2002-10-08 | 2004-05-05 | ס�ѽ�����ɽ��ʽ���� | Method for separating/ recovering platinum family metal |
| CN104831073A (en) * | 2015-05-04 | 2015-08-12 | 昆明正江工贸有限责任公司 | Technology for recovering platinum, palladium and rhodium from spent auto-catalyst |
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2019
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| CN1385545A (en) * | 2002-05-24 | 2002-12-18 | 张方宇 | Method for recovering platinum, palladium and rhodium from waste catalyst in car tail gas |
| CN1493706A (en) * | 2002-10-08 | 2004-05-05 | ס�ѽ�����ɽ��ʽ���� | Method for separating/ recovering platinum family metal |
| CN104831073A (en) * | 2015-05-04 | 2015-08-12 | 昆明正江工贸有限责任公司 | Technology for recovering platinum, palladium and rhodium from spent auto-catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430376A (en) * | 2021-07-06 | 2021-09-24 | 湖南省南铂新材料有限公司 | Method for efficiently separating noble metals in solution and preparing high-purity noble metals |
| CN115418490A (en) * | 2022-09-16 | 2022-12-02 | 贵研资源（易门）有限公司 | Method for recovering platinum and palladium from waste liquid containing trace precious metals |
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