CN102179066A - Method for extracting and separating ions in two valence states of the same element in three phases - Google Patents
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Abstract
The invention relates to the technical field of extraction and separation, in particular to a method for extracting and separating ions in two valence states of the same element in three phases. The method comprises the following steps of: 1) adding water-soluble high polymer, inorganic strong polyelectrolyte salt and a coordinating agent in turn into aqueous solution containing the ions in two valence states of the same element, and fully mixing to obtain mixed solution; and 2) regulating the pH of the mixed solution in the step 1), adding an organic extracting agent immiscible with water, fully mixing, standing and centrifuging to obtain a liquid-liquid-liquid three-phase system with coexistent upper layer, middle layer and lower layer, wherein the upper layer is an organic phase, the middle layer is an aqueous phase of the high polymer and the lower layer is an aqueous phase of the inorganic strong polyelectrolyte salt, and the ions in the two valence states are respectively extracted into the upper, middle or lower layer to realize the extraction and separation of the ions in the two valence states of the same element. By the method, the same element in two valence states is finely separated, and the problem of low recovery rate in a liquid-liquid extraction process is solved.
Description
Technical field
The present invention relates to the extraction and separation technology field, particularly, the present invention relates to the method for a kind of three phase extraction separation with two kinds of valence state ions of a kind of element.
Background technology
In natural environment, a kind of element often exists two kinds of main valence states.The element of two kinds of valence states has diverse chemical behavior and toxicology behavior.For example: chromium (III) is to keep human homergy's trace elements necessary, and the complex compound of it and B2 globulin is that to keep eubolism institute indispensable, and scarce chromium can cause multiple diseases such as atherosclerotic.On the contrary, chromium (VI) has strong toxicity, and its absorption can influence the redox of cell, can combine with nucleic acid, and alimentary canal, respiratory tract are had stimulation, and carcinogenic, mutagenesis is arranged, and health is produced serious harm.Antimony (III) has high-affinity with human erythrocyte, and its toxicity is about 10 times of antimony (V), and arsenic (III) is more a lot of greatly than arsenic (V) toxicity.This shows that the morphological analysis of element all has important meaning at aspects such as environmental science, life science, physiological medical sciences.The effective way of carrying out Elemental Speciation Analysis is that the detection means of simple and reliable separation method with sensitivity combined.The separation method of existing bibliographical information mainly contains: coprecipitation, liquid-liquid extraction method, ion-exchange chromatography, absorption method, liquid film extraction method and solid phase extraction etc.
Wherein, liquid-liquid extraction is to utilize in the solution each component to distribute the difference of character to realize a kind of process of separating in two immiscible liquid phases.Liquid-liquid extraction is because separative efficiency height, energy consumption are low, easy operating, be fit to characteristics such as large-scale production, still unimportant laboratory isolation technics, and be widely used in fields such as metallurgy, pharmacy, food, oil.When using liquid-liquid extraction from matrix solution, to separate certain element, usually have only a kind of element of valence state to be extracted, reach and extract a kind of element fully, generally acknowledge that ripe method is to adopt redox method, make this element all become a kind of valence state and extract, but owing to will change ionic valence condition, the process complexity, restive, often cause separating index and descend because of the valence state control of element is bad.
Liquid-liquid-liquid three phase extraction technology is emerging in recent years extracting process, compares with traditional liquid-liquid two-phase extraction, and three phase extraction can realize that separating technology is integrated, simplifies technological process; Three components are separated from each other, all become pure component, can also realize that specific components separates, certain two kinds of interested material is separated from mixture, all the other materials still mix.Liquid-liquid-liquid three phase extraction process is immiscible to carry out in mutually at three, the composition of three-phase is not made up of separated material itself in this system, but other materials that added carrier function are phase, and promptly three-phase is made up of non-sample fraction, and sample fraction is in three alternate distribution.As phase on the organic solvent in the three-phase system, phase and salt water in the high polymer.The partition equilibrium that relates in the liquid-liquid-liquid three phase extraction process is many, separate to utilize each component of separation to realize in the difference of three alternate distribution capability.In the liquid-liquid-liquid three-phase system, the composition of phase can change in very wide scope, the variation of this phase composition must cause the variation of different material in three alternate distribution coefficient sizes, therefore can utilize the variation of phase composition to enlarge the difference of different material, thereby realize separating at three alternate distribution coefficients.The liquid-liquid-liquid three-phase system can be used for the separation of the very little material of nature difference.At present, the liquid-liquid-liquid three phase extraction has been successfully applied to the separation and concentration of target components in multi-component complex system such as biofermentation system, natural products system, multicomponent waste water system and the multi-metal system.The identity element that the liquid-liquid-liquid three phase extraction separates different valence state does not appear in the newspapers.
Summary of the invention
The objective of the invention is in order to overcome the problems referred to above, the method of a kind of three phase extraction separation with two kinds of valence state ions of a kind of element is provided, make mutually material with organic solvent, high polymer and inorganic salt solution and construct the liquid-liquid-liquid three-phase system, be implemented under the situation that does not adopt the redox means, step extraction separates the ion of two kinds of valence states of identity element simultaneously.
Three phase extraction separation according to the present invention said method comprising the steps of with the method for two kinds of valence state ions of a kind of element:
1) in the aqueous solution that contains with two kinds of valence state ions of a kind of element, add high molecular weight water soluble polymer, inorganic strong electrolyte salt and complexant successively, fully mixing obtains mixed solution;
2) regulating step 1) in the pH of mixed solution, add and the immiscible organic extractant of water then, fully mix, leave standstill, centrifugal, obtain the liquid-liquid-liquid three-phase system of three layers of coexistence of upper, middle and lower, the upper strata is an organic facies, and the middle level is the water of high molecular weight water soluble polymer, and lower floor is the water of inorganic strong electrolyte salt, the ion of two kinds of valence states is extracted into respectively, in or down mutually in, realize extract and separate with two kinds of valence state ions of a kind of element;
Wherein,
Described element is an iron, and two kinds of valence states are Fe (III) and Fe (II), and employed complexant is a phenanthroline, the mol ratio of phenanthroline and Fe (II) is 3～8: 1, regulating step 1) pH of gained iron ion mixed solution is 1～6, and organic extractant is a neutral phosphorus extractant
Described element is a chromium, and two kinds of valence states are Cr (III) and Cr (VI), regulating step 1) pH of gained chromium ion mixed solution is 3～6, organic extractant is di(2-ethylhexyl)phosphate (2-methyl hexyl) ester,
Described element is a vanadium, two kinds of valence states are V (IV) and V (V), employed complexant is 4-(2-pyridylazo)-resorcinol, the mol ratio of 4-(2-pyridylazo)-resorcinol and V (V) is 1～3: 1, regulating step 1) pH of gained vanadium ion mixed solution is 4.5～6.5, organic extractant is di(2-ethylhexyl)phosphate (2-methyl hexyl) ester
Described element is a thallium, two kinds of valence states are Tl (III) and Tl (I), employed complexant is oxine (or phenanthroline), oxine (or phenanthroline) is 3～5: 1 with the mol ratio of Tl (III), regulating step 1) pH of gained thallium ion mixed solution is 3～6.5, organic extractant is bicyclohexane-18-hat-6
Described element is an antimony, two kinds of valence states are Sb (III) and Sb (V), employed complexant is 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol, the mol ratio of 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol and Sb (III) is 2～3: 1, regulating step 1) pH of gained antimony ion mixed solution is 0～2, organic extractant is an isopropyl ether
Described element is an iridium, two kinds of valence states are Ir (III) and Ir (IV), employed complexant is 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol, the mol ratio of 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol and Ir (IV) is 1～2: 1, regulating step 1) pH of gained iridium ion mixed solution is 5～7, organic extractant is a neutral phosphorus extractant
Described element is a platinum, two kinds of valence states are Pt (II) and Pt (IV), employed complexant is oxine (or thiocarbamide), oxine (or thiocarbamide) is 3～5: 1 with the mol ratio of Pt (II), regulating step 1) pH of gained platinum ion mixed solution is 2～5, organic extractant is a neutral phosphorus extractant
Described element is an arsenic, two kinds of valence states are As (III) and As (V), employed complexant is diethylammonium diethyldithiocarbamate (or pyrrolidines two bamic acid ammoniums), diethylammonium diethyldithiocarbamate (or pyrrolidines two bamic acid ammoniums) is 2～3: 1 with the mol ratio of As (III), regulating step 1) pH of gained arsenic ion mixed solution is 1～7, organic extractant is a neutral phosphorus extractant
Described element is a selenium, two kinds of valence states are Se (IV) and Se (VI), and employed complexant is cup [4] aromatic hydrocarbons, and the mol ratio of cup [4] aromatic hydrocarbons and Se (VI) is 1～2: 1, regulating step 1) pH of gained plasma selenium mixed solution is 1～3, and organic extractant is a neutral phosphorus extractant.
Three phase extraction separation according to the present invention is with the method for two kinds of valence state ions of a kind of element, the described high molecular weight water soluble polymer of step 1), for polyethylene glycol, the molecular weight of molecular weight 500 to 6000 is polyoxyethylene-polyoxypropylene copolymer of 1000～10000, one or more in (wherein poly-ethylene oxide block account for the mass fraction of copolymer be 35～90%), the polyoxyethylene-poly-oxypropylene polyoxyethylene three close block copolymers.
Separate method with two kinds of valence state ions of a kind of element according to three phase extraction according to the present invention, the described inorganic strong electrolyte salt of step 1) is selected from ammonium sulfate, sodium sulphate, magnesium sulfate, sodium dihydrogen phosphate, dibastic sodium phosphate, potassium phosphate and the sodium phosphate one or more.
Three phase extraction separation according to the present invention is with the method for two kinds of valence state ions of a kind of element, the consumption of described high molecular polymer of step 1) and salt is: every 20mL contains in the aqueous solution of certain element of two kinds of valence states, add high molecular polymer 1.5～5.5g, inorganic strong electrolyte salt 2～5g.
Separate method with two kinds of valence state ions of a kind of element, step 2 according to three phase extraction according to the present invention) volume of organic solvent that added, with the volume ratio of the aqueous solution of the element ion that contains two kinds of valence states be 1: 1.25～6.
Three phase extraction separation according to the present invention is with the method for two kinds of valence state ions of a kind of element, and described neutral phosphorus extractant is one or more in tributyl phosphate, methyl acid phosphate diformazan heptyl ester, dioctyl octyl phosphate, trioctyl phosphine oxide and the trialkyl phosphine.
The method that one step of a kind of three phase extraction of the present invention is separated same a kind of element of two kinds of valence states, by the pH of regulator solution and the complexant of adding energy and object ion or interfering ion complexing, and control ratio between the two, realized the coupling of " oil-water " liquid-liquid two-phase extraction technology and polymer-salt aqueous two phase extraction technique, the integrated separation advantage of the two, can either adapt to the step separation of two kinds of same metallic elements of valence state in the multi-component complex system, one step that can adapt to two kinds of same nonmetalloids of valence state again separates, in separation process, effectively eliminated the interference of using Oxidizing and Reducing Agents to bring, improve the subsequent analysis measurement sensitivity greatly, avoid two kinds of valence state identity elements spectra overlapping to each other, for the content of the identity element that detects two kinds of valence states provides a kind of pre-treating method, the total amount that adds and can also obtain this element of the content of the identity element by two kinds of valence states.
The method that one step of a kind of three phase extraction of the present invention is separated same a kind of element of two kinds of valence states, the stack of loading capacity and the working in coordination with of extraction ability of organic solvent phase and polymer phase have been given full play to, promoted the extraction total amount of target substance greatly, the identity element of two kinds of valence states has all obtained catching, and is easy to further recycle respectively.
The method that one step of a kind of three phase extraction of the present invention is separated same a kind of element of two kinds of valence states, not only can realize the meticulous separation of the identity element of two kinds of valence states, and can solve and have only certain valence state element to be extracted when liquid-liquid extraction technology reclaims element and cause the low problem of the material rate of recovery, having broad application prospects aspect the pre-treatment of Analysis of environmental samples test and the resource recovery.
The specific embodiment
To be further described specifically the present invention by specific embodiment below.
Embodiment 1
1.5g molecular weight is 2000 polyethylene glycol and 5g ammonium sulfate to be dissolved in and to contain Cr (III) and Cr (VI) is in the 100 μ mol solution, transfer pH=6 with sulfuric acid and NaOH, and to be settled to volume be 20mL, then add 3.3mL30% (v/v) di(2-ethylhexyl)phosphate (2-ethylhexyl) ester/n-hexane mixed organic solvents, the volume ratio of the organic solvent and the aqueous solution is 1: 6, behind the vibration 5min, centrifugal 10min under rotating speed 3000rpm condition forms the liquid-liquid-liquid three-phase system this moment.Cr (VI) extraction yield of phase in polyethylene glycol reaches 80.2%, and Cr (III) reaches 91.5% in the extraction yield of last phase.
Embodiment 2
5.5g molecular weight is 1500 polyoxyethylene-polyoxypropylene copolymer (wherein poly-ethylene oxide block account for the mass fraction of copolymer be 40%) and 2g sodium sulphate to be dissolved in and to contain in 150 μ mol Cr (III) and 100 μ mol Cr (VI) solution, transfer pH=3 with sulfuric acid and ammoniacal liquor, and to be settled to volume be 20mL, then add 16mL 30% (v/v) di(2-ethylhexyl)phosphate (2-ethylhexyl) ester/kerosene mixed organic solvents, the volume ratio of the organic solvent and the aqueous solution is 1: 1.25, behind the vibration 15min, centrifugal 8min under rotating speed 3000rpm condition forms the liquid-liquid-liquid three-phase system this moment.Cr (VI) reaches 99.3% in the extraction yield of middle phase, and Cr (III) reaches 60.6% in the extraction yield of last phase.
Embodiment 3
1.5g molecular weight is 2000 polyethylene glycol and 5g ammonium sulfate to be dissolved in and to contain Fe (III) and Fe (II) is in the 50 μ mol solution, add 150 μ mol phenanthrolines, wherein the mol ratio of phenanthroline and Fe (II) is 3: 1, transfer pH=6 with sulfuric acid, and to be settled to volume be 20mL, then add 8mL 60% (v/v) trialkyl phosphine/n-dodecane mixed organic solvents, the volume ratio of the organic solvent and the aqueous solution is 1: 2.5, behind the vibration 30min, centrifugal 10min under rotating speed 3000rpm condition forms the liquid-liquid-liquid three-phase system this moment.Fe (II) extraction yield of phase in polyethylene glycol reaches 99.5%, and Fe (III) reaches 75.7% in the extraction yield of last phase.
Embodiment 4
5.5g molecular weight is 6000 polyethylene glycol and 2g sodium sulphate to be dissolved in and to contain in 150 μ mol Fe (III) and 100 μ mol Fe (II) solution, add 350 μ mol phenanthrolines, wherein the mol ratio of phenanthroline and Fe (II) is 8: 1, transfer pH=1 with sulfuric acid, and to be settled to volume be 20mL, then add the 5mL trioctyl phosphine oxide, the volume ratio of the organic solvent and the aqueous solution is 1: 4, behind the vibration 40min, centrifugal 15min under rotating speed 4000rpm condition forms the liquid-liquid-liquid three-phase system this moment.Fe (II) extraction yield of phase in polyethylene glycol reaches 98.1%, and Fe (III) reaches 83.5% in the extraction yield of last phase.
Embodiment 5
The 2g molecular weight is 2000 polyethylene glycol, the 1g molecular weight is 1500 polyoxyethylene-polyoxypropylene copolymer (wherein poly-ethylene oxide block account for the mass fraction of copolymer be 50%) and 2g ammonium sulfate, 1g sodium sulphate is dissolved in and contains in 100 μ mol Cr (III) and 50 μ mol Cr (VI) solution, transfer pH=4 with sulfuric acid, and to be settled to volume be 20mL, then add 10mL 50% (v/v) di(2-ethylhexyl)phosphate (2-ethylhexyl) ester/positive nonane and mix organic facies, the volume ratio of the organic solvent and the aqueous solution is 1: 2, behind the vibration 5min, centrifugal 10min under rotating speed 3000rpm condition forms the liquid-liquid-liquid three-phase system this moment.Cr (VI) reaches 92.9% in the extraction yield of middle phase, and Cr (III) reaches 95.4% in the extraction yield of last phase.
In addition, the present invention has also investigated the required condition of separation of two kinds of different valence state of ion of other elements, and its result is as shown in table 1.
The separation of two kinds of different valence state ions of table 1 identity element
Therefore, by the data in embodiment 1～5 and the form 1 as can be seen, two kinds of valence states for above-mentioned each element, as long as strict this element ion solution of control and the pH of high molecular weight water soluble polymer, inorganic strong electrolyte salt and complexant mixed solution, the kind and the proportioning of complexant, select appropriate organic solvent, can realize that fully a step three phase extraction separates two kinds of different valence state with a kind of element, and have good separating effect.
Claims (6)
1. a three phase extraction separates the method with two kinds of valence state ions of a kind of element, it is characterized in that, said method comprising the steps of:
1) in the aqueous solution that contains with two kinds of valence state ions of a kind of element, add high molecular weight water soluble polymer, inorganic strong electrolyte salt and complexant successively, fully mixing obtains mixed solution;
2) regulating step 1) in the pH of mixed solution, add and the immiscible organic extractant of water then, fully mix, leave standstill, centrifugal, obtain the liquid-liquid-liquid three-phase system of three layers of coexistence of upper, middle and lower, the upper strata is an organic facies, and the middle level is the water of high molecular weight water soluble polymer, lower floor is the water of inorganic strong electrolyte salt, the ion of two kinds of valence states is extracted into respectively, in or down mutually in, realize extract and separate with two kinds of valence state ions of a kind of element
Wherein,
Described element is an iron, and two kinds of valence states are Fe (III) and Fe (II), and employed complexant is a phenanthroline, the mol ratio of phenanthroline and Fe (II) is 3～8: 1, regulating step 1) pH of gained iron ion mixed solution is 1～6, and organic extractant is a neutral phosphorus extractant
Described element is a chromium, and two kinds of valence states are Cr (III) and Cr (VI), regulating step 1) pH of gained chromium ion mixed solution is 3～6, organic extractant is di(2-ethylhexyl)phosphate (2-methyl hexyl) ester,
Described element is a vanadium, two kinds of valence states are V (IV) and V (V), employed complexant is 4-(2-pyridylazo)-resorcinol, the mol ratio of 4-(2-pyridylazo)-resorcinol and V (V) is 1～3: 1, regulating step 1) pH of gained vanadium ion mixed solution is 4.5～6.5, organic extractant is di(2-ethylhexyl)phosphate (2-methyl hexyl) ester
Described element is a thallium, two kinds of valence states are Tl (III) and Tl (I), employed complexant is oxine or phenanthroline, the mol ratio of oxine or phenanthroline and Tl (III) is 3～5: 1, regulating step 1) pH of gained thallium ion mixed solution is 3～6.5, organic extractant is bicyclohexane-18-hat-6
Described element is an antimony, two kinds of valence states are Sb (III) and Sb (V), employed complexant is 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol, the mol ratio of 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol and Sb (III) is 2～3: 1, regulating step 1) pH of gained antimony ion mixed solution is 0～2, organic extractant is an isopropyl ether
Described element is an iridium, two kinds of valence states are Ir (III) and Ir (IV), employed complexant is 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol, the mol ratio of 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol and Ir (IV) is 1～2: 1, regulating step 1) pH of gained iridium ion mixed solution is 5～7, organic extractant is a neutral phosphorus extractant
Described element is a platinum, two kinds of valence states are Pt (II) and Pt (IV), employed complexant is oxine or thiocarbamide, the mol ratio of oxine or thiocarbamide and Pt (II) is 3～5: 1, regulating step 1) pH of gained platinum ion mixed solution is 2～5, organic extractant is a neutral phosphorus extractant
Described element is an arsenic, two kinds of valence states are As (III) and As (V), employed complexant is diethylammonium diethyldithiocarbamate or pyrrolidines two bamic acid ammoniums, the mol ratio of diethylammonium diethyldithiocarbamate or pyrrolidines two bamic acid ammoniums and As (III) is 2～3: 1, regulating step 1) pH of gained arsenic ion mixed solution is 1～7, organic extractant is a neutral phosphorus extractant
Described element is a selenium, two kinds of valence states are Se (IV) and Se (VI), and employed complexant is cup [4] aromatic hydrocarbons, and the mol ratio of cup [4] aromatic hydrocarbons and Se (VI) is 1～2: 1, regulating step 1) pH of gained plasma selenium mixed solution is 1～3, and organic extractant is a neutral phosphorus extractant.
2. three phase extraction according to claim 1 separates the method with two kinds of valence state ions of a kind of element, it is characterized in that, to be selected from molecular weight be that 500～6000 polyethylene glycol, molecular weight are 1000～10000 PEP-101 and in the polyoxyethylene-poly-oxypropylene polyoxyethylene three close block copolymers one or more to high molecular weight water soluble polymer in the described step 1), and wherein the mass fraction that poly-ethylene oxide block accounts for copolymer in the PEP-101 is 35～90%.
3. three phase extraction according to claim 1 separates the method with two kinds of valence state ions of a kind of element, it is characterized in that inorganic strong electrolyte salt is to be selected from ammonium sulfate, sodium sulphate, magnesium sulfate, sodium dihydrogen phosphate, dibastic sodium phosphate, potassium phosphate and the sodium phosphate one or more in the described step 1).
4. three phase extraction according to claim 1 separates the method with two kinds of valence state ions of a kind of element, it is characterized in that the addition of high molecular polymer is 1.5～5.5g/20mL aqueous solution in the described step 1), and the addition of salt is 2～5g/20mL aqueous solution.
5. three phase extraction according to claim 1 separates the method with two kinds of valence state ions of a kind of element, it is characterized in that described step 2) in the addition of organic solvent and the volume ratio of the mixed solution in the step 1) be 1: 1.25～6.
6. three phase extraction according to claim 1 separates the method with two kinds of valence state ions of a kind of element, it is characterized in that described neutral phosphorus extractant is one or more in tributyl phosphate, methyl acid phosphate diformazan heptyl ester, dioctyl octyl phosphate, trioctyl phosphine oxide and the trialkyl phosphine.
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| CN102503003A (en) * | 2011-10-28 | 2012-06-20 | 中国科学院过程工程研究所 | Photoreduction/liquid-liquid-liquid three-phase extraction coupled method for removing and recycling chromium |
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| CN105369036A (en) * | 2015-11-20 | 2016-03-02 | 中国科学院过程工程研究所 | Method for extracting vanadium from vanadium-containing high-concentration hydrochloric acid solution |
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