CN110016555B - Method for separating and purifying noble metal in solution - Google Patents

Method for separating and purifying noble metal in solution Download PDF

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CN110016555B
CN110016555B CN201910398478.7A CN201910398478A CN110016555B CN 110016555 B CN110016555 B CN 110016555B CN 201910398478 A CN201910398478 A CN 201910398478A CN 110016555 B CN110016555 B CN 110016555B
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adsorption
rhodium
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noble metal
platinum
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吴喜龙
贺小塘
王欢
赵雨
李勇
刘�文
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Sino Platinum Metals Resources Yimen Co ltd
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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
    • 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
    • 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
    • Y02P10/00—Technologies related to metal processing
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Abstract

The invention relates to the field of comprehensive utilization of secondary resources of precious metals, in particular to a method for separating and purifying precious metals in a solution. The method for separating and purifying the noble metal in the solution comprises the following steps in sequence: A. pretreating the noble metal solution; B. adsorption; C. cleaning an adsorption column; D. rhodium elution and refining; E. separating platinum and palladium; F. and (4) regenerating the adsorption material. The method has the advantages of high recovery rate of noble metal, short production period of rhodium, no interference of rhodium after rhodium is preferentially separated, simple separation of platinum and palladium, short production flow, high production efficiency and improvement of economic benefit.

Description

Method for separating and purifying noble metal in solution
Technical Field
The invention relates to the field of comprehensive utilization of secondary resources of precious metals, in particular to a method for separating and purifying precious metals in a solution.
Background
The noble metal comprises 8 elements including gold, silver and platinum group metals, wherein the platinum group gold comprises 6 elements including platinum, palladium, rhodium, iridium, ruthenium and osmium. The chemical properties of the platinum group metals are similar, the existing state of the hydrochloric acid medium platinum group metal aqueous solution is very complicated, the chlorine complexes and hydrates of the platinum group metals are very large in amount, and the thermodynamic instability is caused, so that the separation of the platinum group metals in the solution is very difficult. The mutual separation of platinum group metals is carried out by utilizing different oxidation states and reaction kinetics of the platinum group elements, and the separation is usually carried out by adopting methods such as oxidation distillation, ion exchange, solution extraction, chemical precipitation and the like.
Separation sequence of noble metals in solution: the palladium-platinum-rhodium or the platinum-palladium-rhodium has the advantages that due to the special chemical property of rhodium, the rhodium is usually refined at the end of the process, the rhodium is separated and purified, the process is long, the process is complex, the recovery period is long, the recovery rate of rhodium is reduced, and due to the large price fluctuation of rhodium, the commercial risk is also large. The rhodium is separated and purified in the hydrochloric acid solution by adopting an advanced rhodium adsorption material with high selectivity and priority, so that the dispersion of the rhodium is reduced, the recovery rate of the rhodium is improved, the backlog of the rhodium in the production process is greatly reduced, and the risk is reduced. After rhodium is separated, the interference of rhodium is reduced, the platinum-palladium separation is simpler, and the recovery rate of platinum-palladium is improved.
Chinese patent 201510797487.5 relates to the technical field of precious metal smelting and discloses a method for separating platinum group metals from platinum group metal-containing solution, which comprises the steps of firstly adding the platinum group metal-containing solution into a reactor for concentration, and then adding water for dilution until the acidity of the solution is 1.5-3 mol/L; then the temperature of the solution is adjusted to 60-70 DEG CSlowly introducing SO2Gas, the reduction potential of the reactor is adjusted to 210-230mv, the constant potential reaction is carried out for 0.5-1h, the reduction reaction is carried out on the platinum group-containing metal solution, Pt and Pd in the solution after the reaction are reduced into simple substances to be separated out from the solution, and Rh and Ir exist in the solution after the reduction; the invention reduces and separates the platinum group metal in the gold extraction raffinate by controlling the factors such as the acidity of the solution, the reaction temperature, the time end point potential and the like. Through SO2And reduction is carried out, the precipitation rate of Pt and Pd can reach more than 98%, and the precipitation rate of Rh and Ir is less than 8%. The method has the advantages of short process flow, simple operation, low production cost, little environmental pollution and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, adopts the technology of preferentially separating rhodium by an advanced adsorbing material and classically precipitating platinum and palladium to separate and purify noble metal from solution, has high recovery rate of noble metal, shortens the production period of rhodium, has no interference of rhodium after preferentially separating rhodium, has simple separation of platinum and palladium, short production flow and high production efficiency, and improves economic benefit.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the method for separating and purifying the noble metal in the solution comprises the following steps in sequence:
A. pretreatment of the noble metal solution:
adjusting the acidity of the noble metal solution to 4-6mol/L by using chemically pure hydrochloric acid, adjusting the potential of the noble metal solution to 500-900mV by using a potential adjusting agent, heating to 80-95 ℃, keeping the temperature for 60-240 minutes, and keeping the rhodium-chlorine complex in the noble metal solution as RhCl6 3-Controlling the concentration of rhodium in the noble metal solution to be 1-5 g/L;
B. adsorption:
the adsorption material is silica gel loaded with active functional groups, the active functional groups are 1-ethylpyridine chloride, the loading capacity of the active functional groups is 1.0-1.2mmol/g, the active functional groups can adsorb rhodium in the filtrate with high selectivity, the particle diameter of the silicon functional material is 140-500 mu m, and the pore diameter is 100-200A; 3 glass adsorption columns are connected in series, the volume of each adsorption column is 100ml, and 80-100 g of adsorption material is filled in the adsorption columns; allowing the pretreated precious metal solution to flow through an adsorption column at a temperature of 10-30ml/min, and putting the rhodium-adsorbed tail solution into a platinum-palladium separation container;
C. cleaning an adsorption column:
washing the adsorption column by using 6mol/L hydrochloric acid solution, wherein the liquid-material ratio ml/g of hydrochloric acid to the adsorption material is 3-5: 1, combining a washing liquid with tail liquid after rhodium adsorption; then washing the adsorption column with clear water, wherein the liquid-material ratio ml/g of the clear water to the adsorption material is 1-2: 1, removing redundant hydrochloric acid;
D. rhodium elution and refining:
eluting the adsorption column by using 3-5 mol/L KCl solution, wherein the liquid-material ratio ml/g of the KCl solution to the adsorption material is 4-6: 1; then adjusting the pH value of the rhodium eluent to 10-12 by using NaOH solution to generate Rh2O3.xH2O, washing with clean water, drying, introducing hydrogen for reduction to obtain 99.95% of sponge rhodium powder, wherein the recovery rate of rhodium is more than 92%;
E. separating platinum and palladium:
separating and purifying platinum and palladium from the tail liquid after rhodium adsorption by adopting a classical ammonium salt precipitation technology to obtain sponge platinum and palladium products with the purity of 99.95 percent, wherein the recovery rate of platinum is more than 98 percent, and the recovery rate of palladium is more than 99 percent;
F. regeneration of the adsorption material:
washing the adsorption column with clear water, wherein the liquid-material ratio ml/g of the clear water to the adsorption material is 3-5: 1, then balancing the adsorption column by using 6mol/L hydrochloric acid solution, wherein the liquid-material ratio ml/g of the hydrochloric acid solution to the adsorption material is 1-2: 1; the regenerated adsorbing material is used for separating and purifying the noble metal in the next noble metal solution.
The potential regulator is Cl2、H2O2And NaClO.
The invention has the beneficial effects that:
1. the active group has the characteristics of high selective adsorption on rhodium in noble metal solution, high adsorption rate, large adsorption capacity and the like.
2. The method has the advantages of high recovery rate of noble metals, platinum recovery rate of more than 98%, palladium recovery rate of more than 99% and rhodium recovery rate of more than 92%.
3. The production period of rhodium is shortened, and the price fluctuation risk of rhodium is reduced.
4. The method has the advantages of no rhodium interference after the rhodium is preferentially separated, simple separation of the platinum and the palladium, short production flow, high production efficiency and improvement of economic benefit.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
The method for separating and purifying the noble metal in the solution comprises the following steps in sequence:
A. pretreatment of the noble metal solution:
adjusting the acidity of the noble metal solution with chemically pure hydrochloric acid, introducing Cl2Oxidizing for 4 hours, then heating the noble metal solution to 80 ℃, and keeping the temperature for 60 minutes; the acidity of the treated noble metal solution is 4mol/L, the concentration of the noble metal is Pt4.5g/L, Pd12.7g/L and Rh1.0g/L, the potential of the noble metal solution is 500mV, and the volume is 1000 ml;
B. adsorption:
the adsorption material is silica gel loaded with active functional groups, the active functional groups are 1-ethylpyridine chloride, the loading capacity of the active functional groups is 1.0mmol/g, the active functional groups can adsorb rhodium in the filtrate with high selectivity, the particle diameter of the silicon functional material is 140-200 < u > m, and the pore diameter is 100-200 < u > a-; 3 glass adsorption columns are connected in series, the volume of each adsorption column is 100ml, and 80 g of adsorption material is filled in the adsorption columns; allowing the pretreated precious metal solution to flow through an adsorption column at a temperature, controlling the adsorption flow rate to be 10ml/min, and putting the rhodium-adsorbed tail solution into a platinum-palladium separation container;
C. cleaning an adsorption column:
washing the adsorption column with 240ml of 6mol/L hydrochloric acid solution, and combining the washing solution with the tail solution after rhodium adsorption; then washing the adsorption column with 80ml of clear water to remove redundant hydrochloric acid;
D. rhodium elution and refining:
eluting the adsorption column with 320ml of 3mol/L KCl solution, and then adjusting the pH of the rhodium eluate to 10 with NaOH solution to generate Rh2O3.xH2O, washing with clean water, drying, introducing hydrogen for reduction to obtain 0.93 g of 99.95% sponge rhodium powder, wherein the recovery rate of rhodium is 93.00%;
E. separating platinum and palladium:
separating and purifying platinum and palladium by adopting a classical ammonium salt precipitation technology to obtain 4.42 g of sponge platinum with the purity of 99.95 percent, the recovery rate of the platinum is 98.22 percent, the recovery rate of the sponge palladium with the purity of 99.95 percent is 12.59 g, and the recovery rate of the palladium is 99.13 percent;
F. regeneration of the adsorption material:
the adsorption column is washed by 240ml of clean water, then 80ml of the adsorption column is balanced by 6mol/L hydrochloric acid solution, and the regenerated adsorption material is used for separating and purifying noble metals in next noble metal solution.
Example 2
The method for separating and purifying the noble metal in the solution comprises the following steps in sequence:
A. pretreatment of the noble metal solution:
adjusting the acidity of the noble metal solution with chemically pure hydrochloric acid, adding H2O2Oxidizing, heating the noble metal solution to 90 ℃, and keeping the temperature for 150 minutes; the acidity of the treated noble metal solution is 5mol/L, the concentration of the noble metal is Pt5.4g/L, Pd13.4g/L and Rh3.0g/L, the potential of the noble metal solution is 700mV, and the volume is 1000 ml;
B. adsorption:
the adsorption material is silica gel loaded with active functional groups, the active functional groups are 1-ethylpyridine chloride, the loading capacity of the active functional groups is 1.1mmol/g, the active functional groups can adsorb rhodium in the filtrate with high selectivity, the particle diameter of the silicon functional material is 140-200 < u > m, and the pore diameter is 100-200 < u > a-; 3 glass adsorption columns are connected in series, the volume of each adsorption column is 100ml, and 90 g of adsorption material is filled in the adsorption columns; allowing the pretreated precious metal solution to flow through an adsorption column at a temperature, controlling the adsorption flow rate to be 20ml/min, and putting the rhodium-adsorbed tail solution into a platinum-palladium separation container;
C. cleaning an adsorption column:
washing the adsorption column with 360ml of 6mol/L hydrochloric acid solution, and combining the washing solution with the tail solution after rhodium adsorption; then washing the adsorption column with 135ml of clear water to remove the redundant hydrochloric acid;
D. rhodium elution and refining:
eluting the adsorption column with 450ml of 4mol/L KCl solution, and adjusting the rhodium eluate with NaOH solutionpH to 11 to form Rh2O3.xH2O, washing with clean water, drying, introducing hydrogen for reduction to obtain 2.8 g of 99.95% sponge rhodium powder, wherein the recovery rate of rhodium is 93.33%;
E. separating platinum and palladium:
separating and purifying platinum and palladium from the tail liquid after rhodium adsorption by adopting a classical ammonium salt precipitation technology to obtain 5.31 g of sponge platinum with the purity of 99.95 percent, the recovery rate of the platinum is 98.33 percent, 13.29 g of sponge palladium with the purity of 99.95 percent is obtained, and the recovery rate of the palladium is 99.18 percent;
F. regeneration of the adsorption material:
the adsorption column is washed by 360ml of clean water, 135ml of the adsorption column is balanced by 6mol/L hydrochloric acid solution, and the regenerated adsorption material is used for separating and purifying the noble metal in the next noble metal solution.
Example 3
The method for separating and purifying the noble metal in the solution comprises the following steps in sequence:
A. pretreatment of the noble metal solution:
adjusting the acidity of the noble metal solution by using chemically pure hydrochloric acid, adding NaClO for oxidation, heating the noble metal solution to 95 ℃, and keeping the temperature for 240 minutes; the acidity of the treated noble metal solution is 6mol/L, the concentration of the noble metal is Pt6.3g/L, Pd15.1g/L and Rh5.0g/L, the potential of the noble metal solution is 900mV, and the volume is 1000 ml;
B. adsorption:
the adsorption material is characterized in that active functional groups are loaded on silica gel, the active functional groups are 1-ethylpyridine chloride, the loading capacity of the active functional groups is 1.2mmol/g, the active functional groups can adsorb rhodium in the filtrate with high selectivity, the particle diameter of the silicon functional material is 140-200 < u > m, and the pore diameter is 100-200 < u > a-; 3 glass adsorption columns are connected in series, the volume of each adsorption column is 100ml, and 100 g of adsorption material is filled in the adsorption columns; allowing the pretreated precious metal solution to flow through an adsorption column at a warm temperature, controlling the adsorption flow rate to be 30ml/min, and putting the rhodium-adsorbed tail solution into a platinum-palladium separation container;
C. cleaning an adsorption column:
washing the adsorption column with 500ml of 6mol/L hydrochloric acid solution, and combining the washing solution with the tail solution after rhodium adsorption; then washing the adsorption column with 200ml of clear water to remove redundant hydrochloric acid;
D. rhodium elution and refining:
eluting the adsorption column with 600ml of 5mol/L KCl solution, and adjusting the pH of the rhodium eluate to 12 with NaOH solution to obtain Rh2O3.xH2O, washing with clean water, drying, introducing hydrogen for reduction to obtain 4.67 g of 99.95% sponge rhodium powder, wherein the recovery rate of rhodium is 93.40%;
E. separating platinum and palladium:
separating and purifying platinum and palladium from the tail liquid after rhodium adsorption by adopting a classical ammonium salt precipitation technology to obtain sponge platinum with the purity of 99.95% 3.21 g, the recovery rate of the platinum is 98.57%, the recovery rate of the sponge palladium with the purity of 99.95% 14.98 g and the recovery rate of the palladium is 99.21%;
F. regeneration of the adsorption material:
washing the adsorption column with 500ml of clean water, then balancing the adsorption column with 200ml of 6mol/L hydrochloric acid solution, and using the regenerated adsorption material for next separation and purification of noble metals from noble metal solution.

Claims (2)

1. The method for separating and purifying the noble metal in the solution is characterized by comprising the following steps in sequence:
A. pretreatment of the noble metal solution:
adjusting the acidity of the noble metal solution to 4-6mol/L by using chemically pure hydrochloric acid, adjusting the potential of the noble metal solution to 500-900mV by using a potential adjusting agent, heating to 80-95 ℃, keeping the temperature for 60-240 minutes, and keeping the rhodium-chlorine complex in the noble metal solution as RhCl6 3-Controlling the concentration of rhodium in the noble metal solution to be 1-5 g/L;
B. adsorption:
the adsorption material is silica gel loaded with active functional groups, the active functional groups are 1-ethylpyridine chloride, the loading capacity of the active functional groups is 1.0-1.2mmol/g, the active functional groups can adsorb rhodium in the filtrate with high selectivity, the particle diameter of the silicon functional material is 140-500 mu m, and the pore diameter is 100-200A; 3 glass adsorption columns are connected in series, the volume of each adsorption column is 100ml, and 80-100 g of adsorption material is filled in the adsorption columns; allowing the pretreated precious metal solution to flow through an adsorption column at a temperature of 10-30ml/min, and putting the rhodium-adsorbed tail solution into a platinum-palladium separation container;
C. cleaning an adsorption column:
washing the adsorption column by using 6mol/L hydrochloric acid solution, wherein the liquid-material ratio ml/g of hydrochloric acid to the adsorption material is 3-5: 1, combining a washing liquid with tail liquid after rhodium adsorption; then washing the adsorption column with clear water, wherein the liquid-material ratio ml/g of the clear water to the adsorption material is 1-2: 1, removing redundant hydrochloric acid;
D. rhodium elution and refining:
eluting the adsorption column by using 3-5 mol/L KCl solution, wherein the liquid-material ratio ml/g of the KCl solution to the adsorption material is 4-6: 1; then adjusting the pH value of the rhodium eluent to 10-12 by using NaOH solution to generate Rh2O3.xH2O, washing with clean water, drying, introducing hydrogen for reduction to obtain 99.95% of sponge rhodium powder, wherein the recovery rate of rhodium is more than 92%;
E. separating platinum and palladium:
separating and purifying platinum and palladium from the tail liquid after rhodium adsorption by adopting a classical ammonium salt precipitation technology to obtain sponge platinum and palladium products with the purity of 99.95 percent, wherein the recovery rate of platinum is more than 98 percent, and the recovery rate of palladium is more than 99 percent;
F. regeneration of the adsorption material:
washing the adsorption column with clear water, wherein the liquid-material ratio ml/g of the clear water to the adsorption material is 3-5: 1, then balancing the adsorption column by using 6mol/L hydrochloric acid solution, wherein the liquid-material ratio ml/g of the hydrochloric acid solution to the adsorption material is 1-2: 1; the regenerated adsorbing material is used for separating and purifying the noble metal in the next noble metal solution.
2. The method as claimed in claim 1, wherein the potential modifier is Cl2、H2O2And NaClO.
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