CN101367568B - Process for the separation of strong-acid cation exchange fibre of indium and cadmium - Google Patents
Process for the separation of strong-acid cation exchange fibre of indium and cadmium Download PDFInfo
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- CN101367568B CN101367568B CN2008100737934A CN200810073793A CN101367568B CN 101367568 B CN101367568 B CN 101367568B CN 2008100737934 A CN2008100737934 A CN 2008100737934A CN 200810073793 A CN200810073793 A CN 200810073793A CN 101367568 B CN101367568 B CN 101367568B
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Abstract
The invention provides a strong-acid cation exchange fibre separation method of indium and cadmium. The feed solution is strong-acid mixed solution which comprises the indium and the cadmium. A strong-acid cation exchange fibre column is used to separate the indium and the cadmium in the solution. The separation method has simple technology, is easy to be understood, consumes low energy, has small environmental pollution, can one hundred percent separate the indium and the cadmium, has respectively more than 96 percent and 99 percent recovery rates after separation, and can recycle the second-hand strong-acid cation exchange fibre after being regenerated.
Description
Technical field
The invention belongs to the strong-acid cation exchange fibre separation method of wet separation indium cadmium, particularly indium and cadmium.
Background technology
Indium and cadmium all belong to rare elements, and they often are present in the zink sulphide with the form of low levels sulfide, and both are some similarity on chemical, thereby bring certain difficulty for their separation.And be present in cadmium in the indium, and not only can influence the quality of indium product, deal with improperly also and pollute the environment.Now the comprehensive indium product that obtains that reclaims in each smeltery generally also will be purified through electrorefining.Differ bigger impurity element for oxidizing potential and indium, adopt the method separating effect of CONTROLLED POTENTIAL better, but for the cadmium element close with the oxidizing potential of indium, separating effect is just poor.Also the someone utilizes the difference of metal saturated vapor pressure, take under the certain vacuum degree, to make the indium fusing to remove cadmium in the thick indium, reach the purpose that thick indium is purified, but not only to the equipment requirements height, energy consumption is big for this method, and the separating effect when cadmium content is low is undesirable.Indium and cadmium all are the very high heavy metal element of added value, especially high purity indium.So, separate the purification indium, rationally reclaiming cadmium is the problem that will solve of present technique.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of with polypropylene-base strong-acid cation exchange fibre post method separate and the thick indium of purifying in indium, reclaim the method that obtains the high purity cadmium simultaneously.
The present invention solves the problems of the technologies described above with following technical scheme:
Processing step is:
1, feed liquid preparation
Get the indium cadmium mixed solution that contains 0.5mol/L sulfuric acid or 1.0mol/L hydrochloric acid or nitric acid in right amount, the concentration that makes indium in the solution is 8-12mg/L.
2, ion-exchange fiber post separation condition control
1. polypropylene-base strong-acid cation exchange fibre pre-treatment
With deionized water with original polypropylene-base strong-acid cation exchange fibre washes clean after, extract, deionized water with 3～5 times of fiber volumes soaked 24 hours, extract, soaked 20 minutes with the hydrochloric acid stirring of 2mol/L, extremely neutral with deionized water wash, extract, stir with the 2mol/L sodium hydroxide solution again and soaked 20 minutes, to neutral, extract with deionized water wash.Above-mentioned acid-alkali washing process three times repeatedly.With soaked in absolute ethyl alcohol 7-9 hour, clean with deionized water wash, extract, 40 ℃ of dryings, stand-by.
2. the preparation of fibre columns
Get cleaning and, inject a certain amount of deionized water with the glass chromatography column of piston and core partition.Take by weighing predetermined amount 1. through pretreated polypropylene-base strong-acid cation exchange fibre, stirred 20 minutes with the 1mol/L soaking with sodium hydroxide that is equivalent to 3～5 times of fiber volumes, suction filtration, with washed with de-ionized water to neutrality, wet method dress post, cover one deck glass wool or absorbent cotton on the layer of fibers that installs, the fiber that loads is depressed into highly no longer variation, and keep liquid level to be higher than glass wool or degreasing cotton layer 1mm that the fibre columns upper strata covers with glass stick.With standby after the acid solution drip washing of the pH=1.5 identical and the balance fibre columns with feed liquid.
3. feed liquid upper prop
Under the room temperature (25～35 ℃), get feed liquid in container, transfer its pH=1.5, then with 1.2～0.6mL/min flow velocity 2. by fibre columns with solution with the 1mol/L sodium hydroxide solution, treat that liquid level drops to when the about 1mm of glass wool that covers the dilute nitric acid solution drip washing fibre columns of usefulness pH=1.5.
4. the separation of indium cadmium and wash-out
Under the room temperature (25～35 ℃), when rare nitric acid leacheate liquid level of pH=1.5 is near the glass wool on fibre columns upper strata in treating 3., 1.2mol/L nitric acid with pre-determined volume, with 1.2～0.6mL/min flow velocity wash-out and collect cadmium, after treating that cadmium flows out fully, use the 0.5mol/L metabisulfite solution instead, with same flow velocity wash-out and collect indium.
The renovation process of fibre columns: with 3mol/L sodium-chlor with the flow velocity of 1.2～0.6mL/min by the fibre columns behind the wash-out indium cadmium, to effluent liquid, do not contain CI with deionized water wash then
-, use the acid solution drip washing and the balance fibre columns of pH=1～2 again.
Present method employing strong-acid cation exchange fibre post separates indium and the cadmium in the acid indium cadmium mixed solution.The separation method that the present invention proposes, technology is simple, easily grasp, energy consumption is low, environmental pollution is little, indium and reach 100% separating of cadmium, yield after the separation can reach respectively more than 96% and 99%, and the exhausted strong-acid cation exchange fibre can be reused once more through after regenerating.
Embodiment
The feed liquid that present method is used is the low acid leaching liquor of zinc baking sand in the Guangxi Hua Xi group electrolytic zinc production technique, and handles through certain separation and concentration, and that removes coexistence elements such as dezincify, iron, copper, manganese, calcium and magnesium contains indium and cadmium enrichment solution.
Embodiment 1
The feed liquid preparation: get 10mL and contain 0.5mol/L vitriolic indium cadmium mixed solution, diluting soln makes indium concentration wherein be 10mg/L, and is stand-by.
Polypropylene-base strong-acid cation exchange fibre pre-treatment: take by weighing the original polypropylene-base strong-acid cation exchange fibre of 100g, with deionized water with washes clean after, extract, soaked 24 hours, extract with the deionized water of 5 times of fiber volumes, stir with the hydrochloric acid of the 2mol/L of 3 times of fiber volumes and to soak 20 minutes,, extract to neutral with deionized water wash, the 2mol/L sodium hydroxide solution with 3 times of fiber volumes stirs immersion 20 minutes again,, extract to neutral with deionized water wash.Above-mentioned acid-alkali washing process three times repeatedly.With the soaked in absolute ethyl alcohol of 3 times of fiber volumes 7 hours, clean with deionized water wash, extract, 40 ℃ of dryings, stand-by.
The preparation of fibre columns: get cleaning and, inject a certain amount of deionized water with the glass chromatography column of piston and core partition.Take by weighing 10.0g through pretreated polypropylene-base strong-acid cation exchange fibre, stirred 20 minutes with the 1mol/L soaking with sodium hydroxide that is equivalent to 3 times of fiber volumes, suction filtration, with washed with de-ionized water to neutrality, wet method dress post, cover one deck glass wool or absorbent cotton on the layer of fibers that installs, with glass stick the fiber that loads is depressed into highly no longer variation, and keep liquid level to be higher than glass wool or degreasing cotton layer 1mm that the fibre columns upper strata covers, standby after the sulfuric acid liquid drip washing of usefulness pH=1.5 and the balance fibre columns.
The feed liquid upper prop: regulate with the 1mol/L sodium hydroxide solution under material liquid pH=1.5,35 ℃ of preparation, with solution with the 1.2mL/min flow velocity by fibre columns, treat that liquid level drops to when the about 1mm of glass wool that covers, uses the dilute nitric acid solution drip washing fibre columns of pH=1.5.
The separation of indium cadmium and wash-out: under the said temperature, rare nitric acid leacheate liquid level for the treatment of above-mentioned pH=1.5 is during near the glass wool on fibre columns upper strata, with 1.2mol/L nitric acid eluent, carry out wash-out with the 1.2mL/min flow velocity, collect the effusive cadmium of 30～50mL section, use the 0.5mol/L metabisulfite solution then instead,, collect the indium in 25～40mL effluent liquid after this with the flow velocity wash-out indium of 1.2mL/min.The separation of indium cadmium reaches 100%, and the rate of recovery of indium reaches 97.5%, and the rate of recovery of cadmium reaches 100%.
Embodiment 2
Feed liquid preparation: except the acid medium of solution is the 1.0mol/L hydrochloric acid, other are with embodiment 1.
Regenerated fibre post: use 80mL3mol/L sodium-chlor to pass through used exchange fiber column among the embodiment 1 with the flow velocity of 0.6mL/min.To effluent liquid, do not contain Cl with deionized water wash then
-, use dilute hydrochloric acid solution drip washing and the balance fibre columns of pH1.5 again, standby.
The feed liquid upper prop: regulate under material liquid pH=1.5,30 ℃ with the 1mol/L sodium hydroxide solution, with solution with the 1.0mL/min flow velocity by fibre columns, treat that liquid level drops to when the about 1mm of glass wool that covers, uses the dilute nitric acid solution drip washing fibre columns of pH=1.5.
The separation of indium cadmium and wash-out: under 30 ℃, rare nitric acid leacheate liquid level for the treatment of above-mentioned pH=1.5 is during near the glass wool on fibre columns upper strata, with 1.2mol/L nitric acid eluent, carry out wash-out with the 0.8mL/min flow velocity, collect the effusive cadmium of 30～50mL section, use the 0.5mol/L metabisulfite solution then instead,, collect the indium in 25～40mL effluent liquid after this with the flow velocity wash-out indium of 1.2mL/min.The separation of indium cadmium reaches 100%, and the rate of recovery of indium reaches 96.6%, and the rate of recovery of cadmium reaches 99.5%.
Embodiment 3
Feed liquid preparation: get the indium cadmium mixed solution that 8.0mL contains 1mol/L hydrochloric acid, the regulator solution volume makes wherein indium concentration about 12mg/L, and is stand-by.
Regenerated fibre post: use 80mL3mol/L sodium-chlor to pass through used exchange fiber column among the embodiment 1 with the flow velocity of 0.6mL/min.To effluent liquid, do not contain Cl with deionized water wash then
-, use dilute hydrochloric acid liquid drip washing and the balance fibre columns of pH=1.5 again, standby.
The feed liquid upper prop: with 1mol/L sodium hydroxide solution flavouring liquid pH=1.5, under 25 ℃, with solution with the 0.8mL/min flow velocity by fibre columns, treat that liquid level drops to when the about 1mm of glass wool that covers the dilute nitric acid solution drip washing fibre columns of usefulness pH=1.5.
The separation of indium cadmium and wash-out: under 25 ℃, rare nitric acid leacheate liquid level for the treatment of above-mentioned pH=1.5 is during near the glass wool on fiber upper strata, with 1.2mol/L nitric acid eluent, carry out wash-out with the 0.6mL/min flow velocity, collect the effusive cadmium of 30～50mL section, use the 0.5mol/L metabisulfite solution then instead,, collect the indium in 25～40mL effluent liquid after this with the flow velocity wash-out indium of 1.2mL/min.The separation of indium cadmium reaches 100%, and the rate of recovery of indium reaches 98.0%, and the rate of recovery of cadmium reaches 100%.
Embodiment 4
The feed liquid preparation: get the indium cadmium mixed solution that 9.0mL contains 1.0mol/L nitric acid, diluting soln makes indium concentration wherein be 8mg/L, and is stand-by.
Polypropylene-base strong-acid cation exchange fibre pre-treatment: with embodiment 1.
The preparation of fibre columns: with the nitric acid liquid drip washing and balance fibre columns of pH=1.5, other are with embodiment 1 except last.
Feed liquid upper prop: under 35 ℃, get feed liquid in container, transfer its pH=1.5, then solution is passed through fibre columns with the 1.2mL/min flow velocity with the 1mol/L sodium hydroxide solution, treat that liquid level drops to when the about 1mm of glass wool that covers the dilute nitric acid solution drip washing fibre columns of usefulness pH=1.5.
The separation of indium cadmium and wash-out: under 35 ℃, rare nitric acid leacheate liquid level for the treatment of above-mentioned pH=1.5 is during near the glass wool on fiber upper strata, with 1.2mol/L nitric acid eluent, carry out wash-out with the 1.2mL/min flow velocity, collect the effusive cadmium of 30～50mL section, use the 0.5mol/L metabisulfite solution then instead,, collect the indium in 25～40mL effluent liquid after this with the flow velocity wash-out indium of 1.2mL/min.The separation of indium cadmium reaches 100%, and the rate of recovery of indium reaches 97.8%, and the rate of recovery of cadmium reaches 100%.
Claims (2)
1. the strong-acid cation exchange fibre separation method of indium and cadmium is characterized in that processing step is:
A, feed liquid preparation
Get the indium cadmium mixed solution that contains 0.5mol/L sulfuric acid or 1.0mol/L hydrochloric acid or nitric acid in right amount, the concentration that makes indium in the solution is 8-12mg/L;
B, the control of ion-exchange fiber post separation condition
1. polypropylene-base strong-acid cation exchange fibre pre-treatment
After washing original polypropylene-base strong-acid cation exchange fibre only with deionized water, extract, deionized water with 3～5 times of fiber volumes soaked 24 hours, extract, soaked 20 minutes with the hydrochloric acid stirring of 2mol/L, extremely neutral with deionized water wash, extract, stir with the 2mol/L sodium hydroxide solution again and soaked 20 minutes, to neutral, extract with deionized water wash; Above-mentioned acid-alkali washing process three times repeatedly, more than 7 hours, clean with soaked in absolute ethyl alcohol with deionized water wash, extract, 40 ℃ of dryings, stand-by;
2. the preparation of fibre columns
Get cleaning and, inject a certain amount of deionized water with the glass chromatography column of piston and core partition; Take by weighing predetermined amount 1. through pretreated polypropylene-base strong-acid cation exchange fibre, stirred 20 minutes with the 1mol/L soaking with sodium hydroxide that is equivalent to 3～5 times of fiber volumes, suction filtration, with washed with de-ionized water to neutrality, wet method dress post, cover one deck glass wool on the layer of fibers that installs, the fiber that loads is depressed into highly no longer variation, and keep liquid level to be higher than the glass wool layer 1mm that the fibre columns upper strata covers with glass stick; With standby after the acid solution drip washing of the pH=1.5 identical and the balance fibre columns with feed liquid;
3. feed liquid upper prop
Under the room temperature 25～35 ℃, get feed liquid in container, transfer its pH=1.5, then with 1.2～0.6mL/min flow velocity 2. by fibre columns with solution with the 1mol/L sodium hydroxide solution, treat that liquid level drops to when the glass wool 1mm that covers, with the dilute nitric acid solution drip washing fibre columns of pH=1.5;
4. the separation of indium cadmium and wash-out
Under the room temperature 25～35 ℃, when rare nitric acid leacheate liquid level of pH=1.5 is near the glass wool on fibre columns upper strata in treating 3., 1.2mol/L nitric acid with pre-determined volume, with 1.2～0.6mL/min flow velocity wash-out and collect cadmium, after treating that cadmium flows out fully, use the 0.5mol/L metabisulfite solution instead, with same flow velocity wash-out and collect indium.
2. the strong-acid cation exchange fibre separation method of indium as claimed in claim 1 and cadmium, the renovation process that it is characterized in that fibre columns are with through the fibre columns behind separation of indium cadmium and the wash-out, pass through with the flow velocity of 3mol/L sodium-chlor with 1.2～0.6mL/min; To effluent liquid, do not contain Cl with the deionized water wash fibre columns then
-, use the acid solution drip washing and the balance fibre columns of pH=1～2 again.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100737934A CN101367568B (en) | 2008-09-19 | 2008-09-19 | Process for the separation of strong-acid cation exchange fibre of indium and cadmium |
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| CN2008100737934A CN101367568B (en) | 2008-09-19 | 2008-09-19 | Process for the separation of strong-acid cation exchange fibre of indium and cadmium |
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| CN101367568B true CN101367568B (en) | 2010-08-04 |
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| CN102895877B (en) * | 2011-07-29 | 2014-08-13 | 北京有色金属研究总院 | Anion exchange purifying method for cadmium condensation isotopes |
| CN103693711B (en) * | 2013-11-12 | 2015-11-04 | 郑州大学 | Utilize weak acidic ion-exchange fiber process nickeliferous/method of copper-contained electroplating waste water |
| CN105645514B (en) * | 2016-01-20 | 2017-06-16 | 西北大学 | The isolation and purification method of ammonium sulfate and sodium sulphate mixed solution in a kind of fume desulfurizing agent regenerative process |
| CN105600805B (en) * | 2016-01-20 | 2017-06-16 | 西北大学 | A kind of method that ammonium sulfate is isolated and purified in the regenerative process by-product solution from fume desulfurizing agent |
| CN109402402B (en) * | 2018-12-11 | 2020-08-18 | 西安诺博尔稀贵金属材料股份有限公司 | Method for recovering gold and silver from gold-silver-copper alloy waste |
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