CN102258884A - Method for extracting metal ions by utilizing two-phase system through sugar separation induction - Google Patents
Method for extracting metal ions by utilizing two-phase system through sugar separation induction Download PDFInfo
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Abstract
The invention relates to the field of metal ion extraction and particularly relates to a method for extracting metal ions by utilizing a two-phase system through sugar separation induction. The method provided by the invention comprises the following steps: 1) adding polarity organic solvents which are mutually soluble with water to an aqueous solution containing target metal ions and obtaining a mixed solution; 2) adding sugar to the mixed solution in the step 1), enabling the concentration of the sugar in the mixed solution to be 40-150g/L and fully oscillating and mixing at 0-25 DEG C to obtain the mixed solution containing the sugar; 3) carrying out centrifugation and phase splitting on the mixed solution containing the sugar in the step 2) to obtain a two-layer liquid phase coexisting system containing a water phase and an organic phase; and 4) taking the organic phase in the step 3) and eliminating the polarity organic solvents to obtain the target metal ions. The method provided by the invention has the advantages that the sugar is used to substitute salt so as to avoid a series of problems caused by a high salt concentration which is needed by a conventional separation phase extraction method.
Description
Technical field
The present invention relates to metal ion extraction field, particularly, the present invention relates to the method that a kind of sugar is analysed the two-phase system extracting metals ion of inducing.
Background technology
Solvent extraction is the separation of metal ions and the most important method of purifying.At present, the two-phase extraction system that is used for the metal ion extract and separate mainly comprises two big classes: traditional organic solvent-water two-phase system and phase separation extraction system.The former is containing target artificial another the immiscible with it organic solution that adds in the aqueous solution of thing of waiting to come together, and utilizes target wait the to come together difference of thing distribution coefficient in two immiscible liquid phases to realize its extract and separate; The phase separation extraction generally is the strong electrolyte salt that adds high concentration in extraction system, utilize salting-out effect to cause single phase soln system of script homogeneous to split the liquid phase that is divided into two-layer coexistence, the utilization difference on two cenotype physico-chemical properties that produce of saltouing realizes that the target thing of waiting to come together distributes in the difference of two-phase.Phase separation extraction based on this principle is called the extraction of saltouing again, high molecular weight water soluble polymer double-aqueous phase system that can be divided into saltouts induces and the polar organic solvent-water two-phase system two big classes of saltouing and inducing.In addition, the phase separation extraction process also can be by the temperature of control extraction system, cause the aqueous solution of the high molecular polymer aqueous solution or polar organic solvent to be split into the liquid phase that two macroscopic views coexist, utilize the physicochemical properties difference of two-layer liquid medium to realize that two of target extract is separated.Phase separation extraction based on this principle is called warm separation extracting method again.
The technology that traditional organic solvent-water two-phase system is used for the extract and separate metal ion is very ripe, for example the extract and separate of copper, nickel, cobalt, gold and platinum family ion etc.; But because the one-tenth phase behavior that extraction process can't the artificial adjustment two-phase and being separated very easily produces emulsification, interphase precipitate thing or third phase, the metal target ion that causes being come together is wayward in two alternate mass transfer and distribution behaviors, extract and separate index instability.
Studies show that in recent years, the strong electrolyte salt (as chlorate, nitrate or the sulfate of alkali metal or alkaline-earth metal) that in the high molecular polymer aqueous solution that dissolves each other with water, adds certain mass, the control proper reaction conditions also can obtain a two-phase system.The water content of two-phase is all very high, is called double-aqueous phase system.Because can being implemented in the two-phase differences, the physicochemical properties difference of two-layer water, target extract distribute.The characteristics of this two-phase system maximum are the one-tenth phase behavior of its two-phase and the easily control that is separated, and can utilize its minute phase behavior to realize the come together controlled separation of thing of target.But, owing to form the salt that the stable polymer double-aqueous phase system needs higher concentration, tend to cause taking place some unpredictable side reactions in the extraction process in the high salt concentration medium, the final form of extraction product is restive, and how from load to reclaim metal and regenerated polymer the polymer phase of metal ion cost-effectively also be one of difficulty of usually facing of this method practical application.
In the presence of strong electrolyte salt, the polar organic solvent that dissolves each other with water also can be under certain condition with moisture from the two-phase system that forms two-layer coexistence, this is another phase separation extraction system.For example, in the mixed solution of acetonitrile and water, add a kind of strong electrolyte salt, or control certain mixed phase temperature, single phase soln that the script homogeneous dissolves each other can split and be divided into two immiscible liquid phases, and the target in the initial aqueous solution is come together thing along with the two-phase division can produce the selective difference distribution in two-phase.This two-phase system was having a lot of reports aspect the metal ion extract and separate.But this individual system exists needs to use the problem of higher concentration salt equally, and higher salinity is one of widely used difficulty of this extraction system of influence for the corrosion of equipment.
Therefore, the invention provides a kind of sugar and analyse the method for the two-phase system extracting metals ion of inducing, need use high concentration strong electrolyte salt in the hope of solving existing phase separation extraction extracting metals ion process, easily cause equipment corrosion, and use the high molecular polymer cost higher, be difficult to difficulties such as regeneration.
Summary of the invention
The method of the two-phase system extracting metals ion that the object of the present invention is to provide a kind of sugar to analyse to induce.
The method that sugar of the present invention is analysed the two-phase system extracting metals ion of inducing may further comprise the steps:
1) will join in the aqueous solution that contains metal ion with the polar organic solvent that water dissolves each other, obtain mixed solution;
2) add sugar in the mixed solution of step 1), making the concentration of sugar in mixed solution is 40～150g/L, mixes 0 ℃～25 ℃ abundant down vibrations, obtains containing sugared mixed solution;
3) with step 2) in the sugared mixed solution that contains carry out centrifugal, phase-splitting, obtain the two-layer liquid phase of water and organic facies coexistence system;
4) get organic facies in the step 3), remove polar organic solvent, obtain metal ion.
Sugar according to the present invention is analysed the method for the two-phase system extracting metals ion of inducing, the described metal ion of step 1) comprises VIII family, in IB family and the IIB family one or more, be selected from platinum, palladium, rhodium, copper, nickel, cobalt, one or more of iron and chromium, the described aqueous solution that contains metal ion can dissolve the compound of respective metal with the aqueous solution of pH 1～7, can with concentration the hydrochloric acid of 0.1mol/L～10mol/L also, nitric acid, or the compound of aqueous sulfuric acid dissolving respective metal, preferably use the chloride preparation of the aqueous hydrochloric acid solution dissolving respective metal of 1mol/L～3mol/L.The compound of respective metal includes but not limited to its chloride, oxide, hydrochloride, nitrate, sulfate or carbonate.
Sugar according to the present invention is analysed the method for the two-phase system extracting metals ion of inducing, and the pure acetonitrile volume of the described adding of step 1) is 0.5～4: 1 with the volume ratio that contains the aqueous solution of metal ion, is preferably 1～3: 1.
Sugar according to the present invention is analysed the method for the two-phase system extracting metals ion of inducing, and the described sugar of step (2) is monose, for being selected from any monose of glucose, maltose, sucrose, galactolipin or fructose.
Sugar according to the present invention is analysed the method for the two-phase system extracting metals ion of inducing, step 2) described in contain the sugar that adds certain mass in the aqueous solution of metal ion, the concentration of sugar in the aqueous solution is 40g/L～150g/L, is preferably 80g/L～100g/L.
Sugar according to the present invention is analysed the method for the two-phase system extracting metals ion of inducing, step 2) to mix the control temperature be 0 ℃～25 ℃ for described vibration, is preferably 5 ℃～15 ℃.
Sugar according to the present invention is analysed the method for the two-phase system extracting metals ion of inducing, the described distillation under vacuum of step 4) ties up to and allows the system environmental pressure remain on below the atmospheric pressure in the still-process, vapo(u)rizing temperature is 30 ℃～60 ℃, preferably, environmental pressure is 0MPa～0.05MPa, and vapo(u)rizing temperature is 40 ℃～50 ℃.
Sugar according to the present invention is analysed the method for the two-phase system extracting metals ion of inducing, and the described method that obtains metal from steam raffinate of step 4) is a conventional method, includes but not limited to reagent reducing process, electrodeposition process etc.
According to one embodiment of the invention, what this method was concrete may further comprise the steps:
(1) the pure acetonitrile with certain volume is dissolved in the aqueous solution that contains metal ion;
(2) sugar of adding certain mass in the mixed solution of step (1), fully vibration mixing at a certain temperature then;
(3) mixture that step (2) is obtained carries out centrifugal treating, obtains up and down two-layer two immiscible liquid phases coexistence system;
(4) get the last phase of step (3) after centrifugal, remove lower boiling acetonitrile, from steam raffinate, obtain metal with distillation under vacuum.
A kind of sugar of the present invention is analysed the method for the two-phase system extracting metals ion of inducing, and the concentration of metal ion in initial aqueous solution of being come together does not limit.In addition, contain that high acid concentration can not cause the degraded of sugar to destroy in the aqueous solution of metal ion, the present invention can be used for extract and separate metal target ion from the aqueous solution that contains one or more metal ions.
Principle of the present invention is: use sugar to replace salt, add sugar in the single_phase system that dissolves each other of polar organic solvent and water, can cause separating of induced electrical polarity organic solvent and water equally, form two-phase system.For example, when adding a certain amount of sugar in the mixture that dissolves each other of acetonitrile and water, under suitable temperature, the mixture that the script homogeneous dissolves each other can split and be divided into two immiscible liquid phases.Therefore, need the concentration and the concussion of sugar in the strict control mixed solution in the present invention, static temperature, the concentration of having only sugar is at 40～150g/L, this mixed solution just can be divided into two-phase fast and effectively when temperature was 0～25 ℃, the two-phase separating effect is bad when the concentration of sugar is lower than 40g/L, but when the concentration of sugar is higher than 150g/L, the viscosity of solution is too big, be not easy layering equally, simultaneously, also can cause the partial miscibility of water and acetonitrile after adding sugar when temperature is too high, thereby divide phase effect to be affected, therefore, in order to reach good branch phase effect, needing the concentration of control sugar is 40～150g/L, temperature is 0～25 ℃.
The invention has the advantages that, use sugar to replace salt, can avoid common phase separation extraction to require the too high a series of problems brought of salinity.
Description of drawings
Fig. 1 analyses the method flow diagram of the two-phase system extracting metals ion of inducing for sugar.
The specific embodiment
The present invention is described in detail by the following examples, but all embodiment do not constitute any restriction to the present invention.
Embodiment 1
With 5mL concentration is the aqueous hydrochloric acid solution dissolving platinum chloride of 2mol/L, platinum ion concentration is 100mg/L, add the pure acetonitrile of 10mL, the volume ratio of the acetonitrile and the metal ion aqueous solution is 2: 1, fully mixing adds 0.6g glucose then again in this mixed liquor, and the concentration of glucose in mixed liquor is 40g/L, 10 ℃ of temperature controls, fully vibration mixes.Carry out centrifugal treating then, obtain the two-phase system of two-layer up and down immiscible clarification phase-splitting.Get the concentration that detects platinum through spectroscopic methodology, the platinum extraction yield is 85.36%.With load platinum ion on separate separately with separatory funnel, carry out decompression distillation with Rotary Evaporators and remove lower boiling acetonitrile, the pressure of distillation procedure is 0.05MPa, vapo(u)rizing temperature is 45 ℃, revolve the acetonitrile that steams and to return and recycle, and the platinum ion that steams in the raffinate reclaims with chloride precipitation.
Embodiment 2
With 5mL concentration is the aqueous hydrochloric acid solution dissolving palladium metal chloride of 3mol/L, and palladium ion concentration is 100mg/L, adds the pure acetonitrile of 15mL, and the volume ratio of the acetonitrile and the metal ion aqueous solution is 3: 1, fully mixing.Add 0.96g maltose then in this mixed liquor again, the concentration of maltose in mixed liquor is 48g/L, 5 ℃ of temperature controls, and fully vibration mixes.Carry out centrifugal treating then, obtain the two-phase system of two-layer up and down immiscible clarification phase-splitting.Get the concentration that detects palladium through spectroscopic methodology, the palladium extraction yield is 90.35%.With load palladium ion on separate separately with separatory funnel, carry out decompression distillation with Rotary Evaporators and remove lower boiling acetonitrile, the pressure of distillation procedure is 0.02MPa, vapo(u)rizing temperature is 40 ℃, revolve the acetonitrile that steams and to return and recycle, and the palladium metal ion that steams in the raffinate reclaims with chloride precipitation.
Embodiment 3
With 5mL concentration is the aqueous hydrochloric acid solution dissolving platinum chloride of 1mol/L, and platinum ion concentration is 100mg/L, adds the pure acetonitrile of 10mL, and the volume ratio of the acetonitrile and the metal ion aqueous solution is 2: 1, fully mixing.Add the 0.75g galactolipin then in this mixed liquor again, the concentration of galactolipin in mixed liquor is 50g/L, 10 ℃ of temperature controls, and fully vibration mixes.Carry out centrifugal treating then, obtain the two-phase system of two-layer up and down immiscible clarification phase-splitting.Get the concentration that detects platinum through spectroscopic methodology, the platinum extraction yield is 93.5%.With load platinum ion on separate separately with separatory funnel, carry out decompression distillation with Rotary Evaporators and remove lower boiling acetonitrile, the pressure of distillation procedure is 0.01MPa, vapo(u)rizing temperature is 50 ℃, revolve the acetonitrile that steams and to return and recycle, and the platinum ion that steams in the raffinate reclaims with chloride precipitation.
Embodiment 4
With 5mL concentration is the metal chloride that the aqueous hydrochloric acid solution of 1mol/L dissolves platinum and rhodium respectively, then together with the aqueous solution of two metal ion species, platinum, the rhodium ion concentration in mixed liquor is 100mg/L, add the pure acetonitrile of 15mL then, the volume ratio of the acetonitrile and the metal ion aqueous solution is 3: 1, fully mixing.Add 0.96g glucose in this mixed liquor again, the concentration of galactolipin in mixed liquor is 48g/L, 15 ℃ of temperature controls, and fully vibration mixes.Carry out centrifugal treating then, obtain the two-phase system of two-layer up and down immiscible clarification phase-splitting.Get the concentration that detects platinum, rhodium through spectroscopic methodology, the platinum extraction yield is 93.5%, and the extraction yield of rhodium is 2.45%.Platinum is enriched in phase, and rhodium is enriched in down phase.With enrichment platinum ion on separate with separatory funnel, carry out decompression distillation with Rotary Evaporators and remove lower boiling acetonitrile, the operating pressure of decompression distillation is 0.05MPa, vapo(u)rizing temperature is 45 ℃, revolving the acetonitrile that steams can return and recycle, steam enrichment platinum ion in the raffinate, further purify with chloride precipitation.The following middle mutually enrichment rhodium that obtains after the centrifugal phase-splitting can add and go back original reagent, reclaims with chemical reduction method.
Embodiment 5
With 5mL concentration is the metal chloride that the aqueous hydrochloric acid solution of 1mol/L dissolves palladium and rhodium respectively, then together with the aqueous solution of two metal ion species, palladium, the rhodium ion concentration in mixed liquor is 100mg/L, add the pure acetonitrile of 15mL then, the volume ratio of the acetonitrile and the metal ion aqueous solution is 3: 1, fully mixing.Add the 2.0g galactolipin in this mixed liquor again, the concentration of galactolipin in mixed liquor is 100g/L, 15 ℃ of temperature controls, and fully vibration mixes.Carry out centrifugal treating then, obtain the two-phase system of two-layer up and down immiscible clarification phase-splitting.Get the concentration that detects palladium, rhodium through spectroscopic methodology, the palladium extraction yield is 96.25%, and the extraction yield of rhodium is 5.35%.Palladium is enriched in phase, and rhodium is enriched in down phase.With enrichment palladium ion on separate with separatory funnel, carry out decompression distillation with Rotary Evaporators and remove lower boiling acetonitrile, the operating pressure of decompression distillation is 0.01MPa, vapo(u)rizing temperature is 45 ℃, revolving the acetonitrile that steams can return and recycle, steam enriched palladium ion in the raffinate, further purify with chloride precipitation.The following middle mutually enrichment rhodium that obtains after the centrifugal phase-splitting can add and go back original reagent, reclaims with chemical reduction method.
The present inventor has investigated the embodiment that each metal ion species is extracted under the different condition, its leaching process reference example 1, and the result is as shown in table 1.
The experimental result of under table 1 different experimental conditions each metal ion species being extracted
By table 1 as seen, the concentration of the sugar that adds in the mixed solution of strictness control acetonitrile and metal ion is at 40～150g/L, and the temperature of control concussion, mixed phase is when being 0～25 ℃, can realize that acetonitrile-metallic ion mixed liquor fast hierarchical becomes two not miscible liquid phases, extraction yield during the branch phase effect of this mixed solution has determined on the acetonitrile that metal ion obtains after phase-splitting mutually, to different metal ion in VIII family, IB family and the IIB family, all can realize sugared efficiently separation extracting.
Claims (10)
1. a sugar is analysed the method for the two-phase system extracting metals ion of inducing, and it is characterized in that, said method comprising the steps of:
1) will join in the aqueous solution that contains metal ion with the polar organic solvent that water dissolves each other, obtain mixed solution;
2) add sugar in the mixed solution of step 1), making the concentration of sugar in mixed solution is 40～150g/L, mixes 0 ℃～25 ℃ abundant down vibrations, obtains containing sugared mixed solution;
3) with step 2) in the sugared mixed solution that contains carry out centrifugal, phase-splitting, obtain the two-layer liquid phase of water and organic facies coexistence system;
4) get organic facies in the step 3), remove polar organic solvent, obtain metal ion.
2. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, it is characterized in that the aqueous solution that contains metal ion in the described step 1) is that dissolving of 1～7 aqueous solution or the dissolving with hydrochloric acid corresponding metal chloride by 1mol/L～3mol/L obtain by pH.
3. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, it is characterized in that, metal ion described in the described step 1) comprises one or more in VIII family, IB family and the IIB family, is selected from one or more of platinum, palladium, rhodium, copper, nickel, cobalt, iron, chromium.
4. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, it is characterized in that, described step 1) Semi-polarity organic solvent is for being selected from acetonitrile, acetone, 1, one or more of 4-dioxane, oxolane, 1-propyl alcohol and/or 2-propyl alcohol.
5. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, and it is characterized in that, the volume ratio of the described step 1) Semi-polarity organic solvent and the metal ion aqueous solution is 0.5～4: 1.
6. sugar according to claim 5 is analysed the method for the two-phase system extracting metals ion of inducing, and it is characterized in that, the volume ratio of the described step 1) Semi-polarity organic solvent and the metal ion aqueous solution is 1～3: 1.
7. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, and it is characterized in that described step 2) in sugar be monose, be selected from a kind of of glucose, maltose, sucrose, galactolipin and fructose.
8. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, and it is characterized in that described step 2) in sugar concentration be 80～100g/L.
9. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, and it is characterized in that described step 2) in the vibration mixing temperature be 5 ℃～15 ℃.
10. sugar according to claim 1 is analysed the method for the two-phase system extracting metals ion of inducing, and it is characterized in that, the method that removes polar organic solvent in the described step 4) is decompression distillation, the pressure≤0.05MPa of distillation under vacuum.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966267A (en) * | 2014-05-23 | 2014-08-06 | 大连理工大学 | Method for separating ethanol from fermentation liquor in extracting and fermenting coupled manner |
| CN109913666A (en) * | 2019-03-12 | 2019-06-21 | 滨州学院 | The sugar analysis three-phase system and method for a kind of extraction and separation Fe (III), Cr (III) and Ni (II) |
| CN111001184A (en) * | 2019-12-25 | 2020-04-14 | 中国科学院长春应用化学研究所 | Method for efficiently inducing water-organic solvent mixed solution phase separation by inorganic salt |
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| US20090090894A1 (en) * | 2007-10-05 | 2009-04-09 | Bin Wang | Separation and extraction system |
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| US20090090894A1 (en) * | 2007-10-05 | 2009-04-09 | Bin Wang | Separation and extraction system |
Non-Patent Citations (1)
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| 刘蓓蕾等: "糖析-HPLC法测定几种重金属离子", 《广州化工》, no. 06, 30 March 2011 (2011-03-30) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966267A (en) * | 2014-05-23 | 2014-08-06 | 大连理工大学 | Method for separating ethanol from fermentation liquor in extracting and fermenting coupled manner |
| CN103966267B (en) * | 2014-05-23 | 2016-07-06 | 大连理工大学 | Extract and the method for ethanol in fermentation coupling separation and fermentation liquid |
| CN109913666A (en) * | 2019-03-12 | 2019-06-21 | 滨州学院 | The sugar analysis three-phase system and method for a kind of extraction and separation Fe (III), Cr (III) and Ni (II) |
| CN111001184A (en) * | 2019-12-25 | 2020-04-14 | 中国科学院长春应用化学研究所 | Method for efficiently inducing water-organic solvent mixed solution phase separation by inorganic salt |
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Application publication date: 20111130 |