CN109385525B - Method for separating platinum and rhodium from alkaline cyanide solution by using polystyrene-tributyl quaternary phosphine resin - Google Patents
Method for separating platinum and rhodium from alkaline cyanide solution by using polystyrene-tributyl quaternary phosphine resin Download PDFInfo
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Abstract
The invention disclosesThe invention discloses a method for separating platinum and rhodium from alkaline cyanide solution by using polystyrene-tributyl quaternary phosphine resin (PS-BQP for short), belonging to the technical field of platinum group metal separation and comprising the steps of using PS-BQP as an adsorbent, and adsorbing Pt (CN) in an alkaline cyanide solution medium with pH of 9.0-11.0 together according to a solid-to-liquid ratio of 1:100(g/mL)4 2‑And Rh (CN)6 3‑By a two-step elution method, adsorbed Pt (CN)4 2‑And Rh (CN)6 3‑Performing fractional elution, desorbing Rh (CN) adsorbed on PS-BQP by using 0.5-1 mol/L KCI solution6 3‑Then 1.0-1.5 mol/L NH is adopted4SCN solution, desorption of Pt (CN) adsorbed on PS-BQP4 2‑Thereby realizing Pt (CN)4 2‑And Rh (CN)6 3‑Separation of (4). The method has the advantages of simple operation flow, short separation period, platinum recovery rate of more than 96.0 percent, rhodium recovery rate of more than 95.0 percent, large adsorption capacity of the PS-BQP adsorbent, good stability, and repeated use of the PS-BQP adsorbent after regeneration treatment of saturated KCI solution.
Description
Technical Field
The invention relates to a method for separating platinum and rhodium from alkaline cyanide solution by using polystyrene-tributyl quaternary phosphine resin (PS-BQP for short), belonging to the technical field of platinum group metal separation.
Background
Platinum and rhodium belong to the same platinum group metal, belong to the strategic resource which is in short supply in China, and need to be imported in large quantity every year, the platinum and rhodium binary catalyst is widely applied to the chemical industry, and the content of platinum and rhodium in glass fiber industrial waste is far higher than that of platinum and rhodium concentrateThe method for leaching platinum and rhodium from secondary resources is a chlorination leaching method and a pressure cyanidation leaching method, platinum and rhodium leachate obtained by the two methods respectively belong to a hydrochloric acid medium and an alkaline cyanide solution medium, the separation and extraction process of platinum and rhodium in the hydrochloric acid medium realizes industrial production at home and abroad, the adopted process preferentially separates platinum from a platinum and rhodium mixed solution, and rhodium is kept in the solution, and finally rhodium is refined, such as Mathey-Rusterburg refinery in England, NanAfrican Tandong (Lonrho) refinery, Akton (Acton) refinery in International Nickel company, Indoma platinum industry limited company in China, and platinum and rhodium separation and extraction in Jinchuan group limited company adopt the processes. In alkaline cyanide medium, Rh and Pt are respectively reacted with CN-Formation of Stable Rh (CN)6 3-And Pt (CN)4 2-At present, the separation of platinum and rhodium from alkaline cyanide solution mainly adopts base metal replacement method and adsorption separation method, the base metal replacement method firstly destroys cyanide in the solution, which not only has many steps and high cost, but also requires Rh (CN) in the treated solution6 3-And Pt (CN)4 2-The concentration should not be too low, which is not suitable for treating low concentration feed liquid. The adsorption separation method has attracted extensive attention in the technical field of platinum group metal separation because of the advantages of simple required equipment, short separation period, small environmental pollution, suitability for treating low-concentration feed liquid and the like, but the application scale is limited because of the problems of small adsorption capacity, poor selectivity, long balance time, difficult elution and the like of the adsorbents such as activated carbon, MOFs materials, various inorganic materials and the like which are applied to the extraction of platinum group metal cyanide at present, and the adsorption method is used for separating Rh (CN) in an alkaline cyanide liquid medium6 3-And Pt (CN)4 2-No industrial scale application has been achieved to date. Therefore, the research and development of the adsorbent which has high adsorption capacity, short equilibrium time and easy elution are used for replacing the existing adsorption material, and the adsorbent is used for enriching and separating platinum and rhodium in alkaline cyanide solution and has very important practical significance and great economic value.
Disclosure of Invention
The invention aims to provide a novel method which has the advantages of short separation period, high recovery rate of platinum and rhodium, large adsorption capacity and good stability, can realize the high-efficiency separation of platinum and rhodium in an alkaline cyanide solution medium and has obvious practical value aiming at the defects of the existing platinum and rhodium adsorption material used for separating the alkaline cyanide solution medium.
The method is implemented by the following technical scheme and is characterized in that polystyrene-tributyl quaternary phosphine resin (PS-BQP for short) is used as an adsorbent, and Pt (CN) in an alkaline cyanide solution medium with pH of 9.0-11.0 is adsorbed according to a solid-to-liquid ratio of 1:100(g/mL)4 2-And Rh (CN)6 3-Firstly, 0.5 to 1mol/L KCI solution is used to desorb Rh (CN) adsorbed on PS-BQP6 3-Then 1.0-1.5 mol/L NH is adopted4SCN solution, desorption of Pt (CN) adsorbed on PS-BQP4 2-Thereby realizing Pt (CN)4 2-And Rh (CN)6 3-Separation of (1);
in the above step, PS-BQP has the structural formula:
the technical scheme comprises the following specific steps:
(1) preparing a water phase: mixing Pt (CN)4 2-And Rh (CN)6 3-Adjusting the pH value of the mixed feed liquid to be within 9.0-11.0;
(2) adding PS-BQP into Pt (CN) according to a solid-to-liquid ratio of 1:100(g/mL)4 2-And Rh (CN)6 3-In the mixed solution of (4), shaking is carried out for 30min, and the loaded Pt (CN) is filtered off4 2-And Rh (CN)6 3-PS-BQP resin of (1);
(3) taking the adsorption load Pt (CN) in the step (2)4 2-And Rh (CN)6 3-The PS-BQP resin is shaken for 10-15 min by 0.5-1.0 mol/L KCI solution according to the solid-to-liquid ratio of 1:50(g/mL), Rh (CN) adsorbed on the PS-BQP resin is desorbed6 3-；
(4) Taking the above steps (3)Desorption Rh (CN)6 3-The subsequent PS-BQP is treated with 1.0-1.5 mol/L NH4Shaking the SCN solution for 10-20 min according to the solid-to-liquid ratio of 1:50(g/mL), desorbing Pt (CN) adsorbed on PS-BQP4 2-；
(5) Taking the step (4) to desorb Pt (CN)4 2-Washing the PS-BQP with distilled water for 2 times, shaking with saturated KCI solution at a solid-to-liquid ratio of 1:30(g/mL) for 10min, filtering to obtain regenerated PS-BQP resin, returning to step (2), adsorbing again the same Pt (CN)4 2-And Rh (CN)6 3-The mixed material liquid realizes the reutilization of PS-BQP.
Said step (2) is Pt (CN)4 2-And Rh (CN)6 3-The concentration of Pt (II) and Rh (III) in the mixed feed liquid is 10-200 mg/L, and the concentration of Rh (III) is 25-150 mg/L.
In the step (2), the concentrations of Pt (II) and Rh (III) in the aqueous phase are measured, the amounts of Pt (II) and Rh (III) adsorbed on PS-BQP are determined by subtraction, and the adsorption rates of Pt (II) and Rh (III) are calculated respectively.
The step (3) is further to determine the concentration of Pt (II) and Rh (III) in the desorption solution and calculate the recovery rate of Rh (III).
The step (4) is further to determine the concentration of Pt (II) in the desorption solution and calculate the recovery rate of Pt (II).
The invention has the following advantages
1. The separation period is short, adsorption equilibrium can be achieved within 30min, and elution can be completed at room temperature.
2. The adsorption capacity is large, the maximum static adsorption capacity of Pt (II) and Rh (III) respectively reaches 115.8mg/g and 108.6mg/g, and the method has large-scale application value.
3. The two-step desorption realizes the separation of platinum and rhodium, the recovery rate of Pt is higher than 96.0 percent, and the recovery rate of rhodium is more than 95.0 percent.
4, the pH value is in a wider alkaline range of 9.0-11.0, the adsorption effect is better, and the adsorption and separation conditions are easy to control.
And 5, the PS-BQP adsorbent has good stability, can be recycled and has low cost.
Detailed Description
The process of the present invention is further illustrated by the following examples.
Example 1
Immobilization of Rh (CN) at different pH conditions at room temperature6 3-The concentration of Rh (III) in the solution is 2.5g/L, the amount of stationary phase PS-BQP is 1.0g, the solid-to-liquid ratio is 1:100(g/mL), the solution is oscillated for 30min, and the loaded PS-BQP is filtered out; determining Rh (III) adsorption quantity, pH value adsorbing Rh (CN) to PS-BQP6 3-The effect of (c) is shown in table 1.
TABLE 1 pH vs. PS-BQP adsorption of Rh (CN)6 3-Influence of (2)
Example 2
Immobilization of Pt (CN) at different pH conditions at room temperature4 2-The concentration of Pt (II) in the solution is 3.0g/L, the amount of the stationary phase PS-BQP is 1.0g, the solid-to-liquid ratio is 1:100(g/mL), the oscillation is carried out for 30min, and the loaded PS-BQP is filtered out; measuring Pt (II) adsorption quantity, pH value and PS-BQP adsorption Pt (CN)4 2-The effect of (c) is shown in table 2.
TABLE 2 pH vs PS-BQP adsorption of Pt (CN)4 2-Influence of (2)
| pH value | 9.0 | 10.0 | 10.5 | 11.0 | 11.5 | 12.0 |
| Static adsorption Capacity (mg/g) | 114.6 | 115.5 | 115.8 | 114.2 | 96.7 | 87.2 |
As can be seen from tables 1 and 2, the PS-BQP adsorbent was resistant to Pt (CN) in a wide alkaline range at pH 9.0-11.04 2-And Rh (CN)6 3-All have better adsorption effect.
Example 3
At room temperature, 1.0g of resin was weighed out as the stationary phase and added to 100mL of Rh (CN) at pH 10.56 3-In the solution, Rh (III) with the concentration of 2.5g/L is oscillated for 30min, and the loaded PS-BQP is filtered out; measuring Rh (III) adsorption amount, adding filtered resin loaded with Rh (III) into 50mL of 1.0mol/L KCI solution, shaking for 15min, filtering to obtain PS-BQP, washing PS-BQP with distilled water for 2 times, and adsorbing the same Rh (CN)6 3-The results of the solution, 6 cycles of static adsorption capacity measurement are shown in Table 3.
TABLE 3 determination of Rh (III) Cyclic static adsorption Capacity
| Number of cycles | 1 | 2 | 3 | 4 | 5 | 6 |
| Static adsorption Capacity (mg/g) | 108.6 | 108.1 | 107.2 | 106.7 | 105.9 | 104.1 |
Example 4
At room temperature, 1.0g of resin was weighed out as the stationary phase and added to 100mL of Pt (CN) at pH 10.54 2-In the solution, the concentration of Pt (II) is 3.0/L, oscillation is carried out for 30min, and the loaded PS-BQP is filtered out; measuring the amount of Pt (II) adsorbed, adding 50mL of 1.5mol/L NH to the filtered Pt (II) -loaded resin4Shaking for 20min in SCN solution, filtering to remove PS-BQP from the desorption solution, washing with distilled water for 2 times, adding PS-BQP resin into 30mL saturated KCI solution, shaking for 10min, filtering to remove PS-BQP, adsorbing the same Pt (CN) again4 2-The results of the solution, 6 cycles of static adsorption capacity measurement are shown in Table 4.
TABLE 4 determination of the circulating static adsorption Capacity of Pt (II)
As can be seen from tables 3 and 4, after 6 cycles of use at pH 10.5, PS-BQP has no significant decrease in the static adsorption capacity of the single component rh (iii) or pt (ii) in the alkaline cyanide solution medium, and PS-BQP has high stability and can be recycled many times.
Example 5
At room temperature, 1.0g of PS-BQP was weighed out as the stationary phase and added to a solution of pH 9.0 containing Pt (CN)4 2-And Rh (CN)6 3-The content of Pt (II) and Rh (III) in the mixed feed liquid is respectively 10.0mg/L and 25.0mg/L, the mixed feed liquid is oscillated for 30min, the loaded PS-BQP is filtered out, 50mL of 0.5mol/L KCI desorption liquid is added, the oscillation is carried out for 10min, the content of Pt (II) and Rh (III) in the desorption liquid is measured, the PS-BQP in the desorption liquid is filtered out, and 1.0mol/L NH is added4Shaking SCN desorption solution 50mL for 10min, filtering to remove PS-BQP in the desorption solution, measuring Pt (II) content in the desorption solution, and calculating Rh (III) and Pt (II) recovery rates (specific data are shown in Table 5).
Example 6
At room temperature, 1.0g of PS-BQP was weighed out as the stationary phase and added to a solution of pH 10.0 containing Pt (CN)4 2-And Rh (CN)6 3-The content of Pt (II) and Rh (III) in the mixed feed liquid is respectively 30.0mg/L and 50.0mg/L, the mixed feed liquid is oscillated for 30min, the loaded PS-BQP is filtered out, 50mL of 0.5mol/L KCI desorption liquid is added, the oscillation is carried out for 10min, the content of Pt (II) and Rh (III) in the desorption liquid is measured, the PS-BQP in the desorption liquid is filtered out, and 1.0mol/L NH is added4Shaking SCN desorption solution 50mL for 12min, filtering to remove PS-BQP, measuring Pt (II) content in the desorption solution, and calculating Rh (III) and Pt (II) recovery rates (see Table 5).
Example 7
At room temperature, 1.0g of PS-BQP was weighed out as the stationary phase and added to a solution of pH 11.0 containing Pt (CN)4 2-And Rh (CN)6 3-The content of Pt (II) and Rh (III) in the mixed feed liquid of 100mL is respectively 60.0mg/L and 85.0mg/L, oscillation is carried out for 30min, the loaded PS-BQP is filtered out, 50mL of KCI desorption liquid of 0.6mol/L is added, oscillation is carried out for 10min, the content of Pt (II) and Rh (III) in the desorption liquid is measured, and P in the desorption liquid is filtered outS-BQP, adding 1.0mol/L NH4Shaking SCN desorption solution 50mL for 15min, filtering to remove PS-BQP in the desorption solution, measuring the content of Pt (II) in the desorption solution, and calculating Rh (III) and Pt (II) recovery rates respectively (specific data are shown in Table 5).
Example 8
At room temperature, 1.5g of PS-BQP was weighed out as the stationary phase and added to a solution of pH 10.5 containing Pt (CN)4 2-And Rh (CN)6 3-In 150mL of mixed feed liquid, the content of the mixed feed liquid Pt (II) and Rh (III) is 110.0mg/L and 100.0mg/L respectively, oscillating for 30min, filtering out the loaded PS-BQP, adding 75mL of 0.8mol/L KCI desorption liquid, oscillating for 12min, measuring the content of Pt (II) and Rh (III) in the desorption liquid, filtering out the PS-BQP in the desorption liquid, adding 1.2mol/L NH4Shaking SCN desorption solution 75mL for 15min, filtering to remove PS-BQP in the desorption solution, measuring the content of Pt (II) in the desorption solution, and calculating Rh (III) and Pt (II) recovery rates respectively (specific data are shown in Table 5).
Example 9
2.0g of PS-BQP were weighed out at room temperature as the stationary phase and added to a solution of pH 10.5 containing Pt (CN)4 2-And Rh (CN)6 3-The content of the mixed feed liquid Pt (II) and Rh (III) is respectively 150.0mg/L and 130.0mg/L, the shaking is carried out for 30min, the loaded PS-BQP is filtered out, 100mL of KCI desorption liquid with the concentration of 1.0mol/L is added, the shaking is carried out for 15min, the content of Pt (II) and Rh (III) in the desorption liquid is measured, the PS-BQP in the desorption liquid is filtered out, and NH with the concentration of 1.5mol/L is added4Shaking SCN desorption solution 100mL for 20min, filtering to remove PS-BQP, measuring Pt (II) content in the desorption solution, and calculating Rh (III) and Pt (II) recovery rates (see Table 5).
Example 10
2.0g of PS-BQP were weighed out at room temperature as the stationary phase and added to a solution of pH 10.5 containing Pt (CN)4 2-And Rh (CN)6 3-200mL of the mixed feed liquid, wherein the contents of Pt (II) and Rh (III) in the mixed feed liquid are respectively 200.0mg/L and 150.0mg/L, oscillating for 30min, filtering out the loaded PS-BQP, adding 100mL of 1.0mol/L KCI desorption liquid, oscillating for 15min, measuring the contents of Pt (II) and Rh (III) in the desorption liquid, filtering out PS-BQP in the desorption liquid, adding 1.5mol/L NH4Shaking 100mL of SCN desorption solution for 20min, and filtering out PS-BQ in the desorption solutionAnd P, measuring the content of Pt (II) in the desorption solution, and respectively calculating the recovery rate of Rh (III) and Pt (II) (the specific data are shown in Table 5).
TABLE 5 Pt (CN)4 2-And Rh (CN)6 3-Effect of PS-BQP in separating Rh (III), Pt (II)
As can be seen from table 5: PS-BQP for Pt (CN) in alkaline cyanide solution medium with pH of 9.0-11.04 2-And Rh (CN)6 3-Has good adsorption effect, and desorbs Pt (CN) adsorbed on PS-BQP by a two-step method4 2-And Rh (CN)6 3-In the first step, KCI solution is used for desorbing Rh (CN) adsorbed on PS-BQP6 3-(ii) a Second step with NH4SCN solution desorption of Pt (CN) adsorbed on PS-BQP4 2-. Thereby realizing Pt (CN)4 2-And Rh (CN)6 3-The recovery rate of platinum is more than 96.0 percent, and the recovery rate of rhodium is more than 95.0 percent.
Claims (6)
1. A method for separating platinum and rhodium from alkaline cyanide solution by using polystyrene-tributyl quaternary phosphine resin is characterized in that PS-BQP is used as an adsorbent, and Pt (CN) in alkaline cyanide solution medium is adsorbed according to a solid-to-liquid ratio of 1:100(g/mL)4 2-And Rh (CN)6 3-Two step desorption of Pt (CN)4 2-And Rh (CN)6 3-In the first step, KCL solution is adopted to desorb Rh (CN) adsorbed on PS-BQP6 3-(ii) a Second step with NH4SCN solution desorption of Pt (CN) adsorbed on PS-BQP4 2-；
PS-BQP has the structural formula:
the PS-BQP is short for polystyrene-tributyl quaternary phosphine resin.
2. The method for separating platinum and rhodium from alkaline cyanide solution by using polystyrene-tributyl quaternary phosphine resin according to claim 1, comprising the following steps:
(1) preparing a water phase: mixing Pt (CN)4 2-And Rh (CN)6 3-Adjusting the pH value of the mixed feed liquid to be within 9.0-11.0;
(2) adding PS-BQP into Pt (CN) according to a solid-to-liquid ratio of 1:100(g/mL)4 2-And Rh (CN)6 3-Of (2) a mixture
In the solution, the mixture was shaken for 30min, and the Pt (CN) supported thereon was filtered off4 2-And Rh (CN)6 3-PS-BQP resin of (1);
(3) taking the adsorption load Pt (CN) in the step (2)4 2-And Rh (CN)6 3-The PS-BQP resin (2) is shaken for 10-15 min by using a 0.5-1.0 mol/LKCL solution according to a solid-to-liquid ratio of 1:50(g/mL), and Rh (CN) adsorbed on the PS-BQP resin is desorbed6 3-；
(4) Taking the step (3) to desorb Rh (CN)6 3-The subsequent PS-BQP is treated with 1.0-1.5 mol/L NH4SCN solution in solid-liquid form
Oscillating for 10-20 min at a ratio of 1:50(g/mL), desorbing Pt (CN) adsorbed on PS-BQP4 2-；
(5) Taking the step (4) to desorb Pt (CN)4 2-Washing the PS-BQP with distilled water for 2 times, shaking with saturated KCL solution at solid-to-liquid ratio of 1:30(g/mL) for 10min, filtering out regenerated PS-BQP resin, returning to step (2), adsorbing again the same Pt (CN)4 2-And Rh (CN)6 3-The mixed material liquid realizes the reutilization of PS-BQP.
3. The process according to claim 2, wherein the step (2) of Pt (CN)4 2-And Rh (CN)6 3-The concentration of Pt (II) in the mixed feed liquid is 10-200 mg/L,the concentration of Rh (III) is 25-150 mg/L.
4. The method according to claim 2, wherein the step (2) further comprises measuring the concentrations of Pt (II) and Rh (III) in the aqueous phase, and the amounts of Pt (II) and Rh (III) adsorbed on PS-BQP are determined by subtraction, and the adsorption rates of Pt (II) and Rh (III) are calculated respectively.
5. The method of claim 2, wherein step (3) further comprises determining the concentration of Pt (II) and Rh (III) in the desorption solution, and calculating the recovery of Rh (III).
6. The method according to claim 2, wherein the step (4) is further a step of determining Pt (II) in the desorption solution
And calculating the recovery of Pt (II).
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| CN101603123A (en) * | 2009-06-26 | 2009-12-16 | 云南大学 | Method with macroporous adsorbent resin solid-phase extraction of gold from alkaline cyanide liquid |
| RU2479651C1 (en) * | 2012-01-11 | 2013-04-20 | Федеральное Государственное Автономное Образовательное Учреждение Высшего Профессионального Образования "Сибирский Федеральный Университет" | Method for extraction and separation of platinum and rhodium in sulphate solutions |
| CN107488790A (en) * | 2017-08-11 | 2017-12-19 | 云南大学 | With the copolymer adsorbing separation palladium of aniline and the methoxy benzoic acid of 2 amino 6, platinum, rhodium method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB848555A (en) * | 1958-02-18 | 1960-09-21 | Nat Res Dev | Treatment of aqueous solutions of complex metallic cyanides |
| JPH0533071A (en) * | 1991-07-31 | 1993-02-09 | Sumitomo Metal Mining Co Ltd | Method for separating and refining rhodium from aqueous solution |
| CN101603123A (en) * | 2009-06-26 | 2009-12-16 | 云南大学 | Method with macroporous adsorbent resin solid-phase extraction of gold from alkaline cyanide liquid |
| RU2479651C1 (en) * | 2012-01-11 | 2013-04-20 | Федеральное Государственное Автономное Образовательное Учреждение Высшего Профессионального Образования "Сибирский Федеральный Университет" | Method for extraction and separation of platinum and rhodium in sulphate solutions |
| CN107488790A (en) * | 2017-08-11 | 2017-12-19 | 云南大学 | With the copolymer adsorbing separation palladium of aniline and the methoxy benzoic acid of 2 amino 6, platinum, rhodium method |
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