CN102382981A - Method for purifying iron solution by adopting extraction chromatography - Google Patents
Method for purifying iron solution by adopting extraction chromatography Download PDFInfo
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- CN102382981A CN102382981A CN2011103395201A CN201110339520A CN102382981A CN 102382981 A CN102382981 A CN 102382981A CN 2011103395201 A CN2011103395201 A CN 2011103395201A CN 201110339520 A CN201110339520 A CN 201110339520A CN 102382981 A CN102382981 A CN 102382981A
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Abstract
The invention relates to a method for purifying an iron solution by adopting extraction chromatography. The method comprises the following steps of: (1) extracting the iron solution by using a chromatographic column, namely adsorbing a P204 extracting agent to macroporous absorption resin in a saponification adsorption mode, obtaining P204 extracted resin, performing wet column filling, adding the iron solution, and leaching the P204 extracted resin chromatographic column; (2) leaching with a leaching solution, namely leaching the iron-carrying P204 extracted resin chromatographic column by using an acid solution as the leaching solution; and (3) leaching with a back extraction solution and concentrating, namely leaching with the acid back extraction solution, back extracting the iron in the P204 extracted resin chromatographic column to the aqueous phase, obtaining a high-purity iron salt solution, concentrating the high-purity iron salt solution, performing electrolytic deposition, and performing vacuum smelting on the electrolytic deposition iron obtained at the cathode to obtain a high-purity iron ingot, wherein the purity of the iron is over 4N by glow discharge mass spectrometry. The method is simple in process flow, easy in operation, high in equipment capacity, low in investment and low in consumption of chemical materials.
Description
Technical field
The present invention relates to a kind of method of extraction chromatography isolation of purified ferrous solution, be specially a kind of with 2-ethylhexyl phosphoric acid (D
2EHPA, P204) for adopting the extraction chromatography partition method, extraction agent purifies ferrous solution, produce the process method of high purity iron solution.
Background technology
The key of preparation high purity iron is the deep purifying of ferrous solution; The content that particularly will make multiple metallic impurity such as nickel in the ferrous solution, copper, manganese is all less than 10ppm; Ferrous solution after the purification obtains high-purity electrolytic iron through electrodeposition, more high-purity electrolytic iron is obtained the high-purity ingot iron of purity greater than 4N through vacuum melting.
The purifying method of ferrous solution mainly contains chemical precipitation method, ion exchange method and solvent extration.But these methods are difficult to prepare the high purity iron solution of metals content impurities such as Mg, Al, Cr, Mn, Cu, Zn, Ni less than 10ppm, are difficult to also realize that iron separates with the degree of depth of these impurity even carry out the separation of multistage number.
Chromes have the high selectivity of extraction agent in the liquid-liquid extraction, have the multistage property of ion exchange method again, on the approaching element of separating property, good performance are arranged, and therefore in hydrometallurgy, receive increasing attention.
The present invention adopts chromes to purify ferrous solution and obtains high purity ferric oxide, obtains the high purity iron of purity greater than 4N through reduction, refining and high vacuum melting.
Summary of the invention
The purpose of this invention is to provide a kind of process method of extraction chromatography isolation of purified ferrous solution, it is simple, easy to operate that this technology has flow process; Invest little characteristics, this handicraft product quality is high, stable, and the purity of the finished product metallic iron is greater than 4N.
For reaching above-mentioned goal of the invention, the present invention adopts following technical scheme:
A kind of method of extraction chromatography isolation of purified ferrous solution may further comprise the steps:
(1) chromatograph column extracting ferrous solution: adopt the mode of saponification absorption to be adsorbed on the macroporous adsorbent resin P204 extraction agent, prepare the P204 extration resin, the resin that has adsorbed extraction agent carries out wet method dress post; Add iron charge liquid then, P204 extration resin chromatograph post is carried out drip washing;
(2) leacheate drip washing: adopt the P204 extration resin chromatograph post of acid solution as leacheate drip washing load iron;
(3) strip liquor drip washing-concentrate: adopt sour strip liquor drip washing, the iron back extraction in the P204 extration resin chromatograph post to aqueous phase, is obtained the high purity iron salts solution; After the high purity iron salts solution concentrated, carry out electrolytic deposition, the electrodeposition iron that negative electrode obtains obtains high-purity ingot iron through vacuum melting, and the purity of iron is more than the 4N through the glow discharge mass spectrometry analysis.
In the methods of the invention, the length-to-diameter ratio of described chromatograph post is 11/1 ~ 5/1.
The particle diameter of said macroporous adsorbent resin is 70 ~ 150 orders.Preferably oily matter there is higher optionally macroporous adsorbent resin.
The P204 that contains 30% ~ 70% (weight percentage, down together) in the said P204 extration resin.
Muriate or sulfate liquor that described iron charge liquid is iron, wherein the total concn of iron is 5 ~ 30 grams per liters.Described leacheate is the hydrochloric acid soln of 1 mol, and described strip liquor is that free acidity is the sulphuric acid soln or the hydrochloric acid soln of 6 mol.After said high purity iron salts solution concentrates, obtain the iron(ic)chloride or the ferrum sulfuricum oxydatum solutum of iron content 50 ~ 120 grams per liters.
The P204 extration resin that will pass through after the strip liquor drip washing carries out manipulation of regeneration.
Said manipulation of regeneration is that the hydrochloric acid soln of 1 mol carries out drip washing for adopting regenerated liquid.
The method of extraction chromatography isolation of purified ferrous solution of the present invention, whole process is mainly passed through three phases, [1] chromatograph column extracting ferrous solution, [2] leacheate drip washing removal of impurities [3] back extraction obtains high purity iron solution, also can further carry out the regeneration of [4] extration resin.The purification that the isolating method of P204 extraction chromatography is carried out ferrous solution particularly in the degree of depth sepn process of iron nickel, iron copper, through extraction-drip washing-back extraction process, obtains qualified high purity iron solution.This solution obtains high-purity negative electrode iron (electrodeposition iron) through electrodeposition, and electrodeposition iron carries out vacuum melting more further purifies, and obtains the high pure metal iron of purity greater than 4N.
With P204 is extraction agent, and macroporous adsorbent resin is a support, and this technology adopts the regeneration of P204 extraction agent absorption preparation P204 extration resin, drip washing, back extraction iron, extration resin successively.
Adopt the mode of saponification absorption to be adsorbed on the macroporous adsorbent resin P204 extraction agent, prepare 30% ~ 70% (weight percentage, down together) P204 extration resin.The preparation method that chromes purify the P204 extration resin in the ferrous solution process is to use macroporous adsorbent resin; Preferably oily matter there is higher optionally macroporous adsorbent resin (commercially available); Under stirring condition, the P204 extraction agent is carried out saponification absorption, prepare the P204 extration resin of desired content.
Iron charge liquid is the muriate or the sulfate liquor of iron, and wherein the total concn of iron is 5 ~ 30 grams per liters.The preparation method of chromes isolation of purified ferrous solution raw material is that those skilled in the art are total to knowledge.First method is that technical grade or reagent of sulfuric acid iron or iron(ic)chloride are dissolved in the water, adds hydrochloric acid or sulfuric acid adjustment pH value; Second method is with metallic iron or iron powder adds quantitative hydrochloric acid or sulfuric acid dissolution obtains iron charge liquid; The third method is to be that main metal or alloy adds quantitative hydrochloric acid or sulfuric acid dissolution obtains iron charge liquid with iron content.Ferric sulfate that the feed liquid that obtains is or ferric chloride Solution(38, the solution iron level that obtains is 5 ~ 30 grams per liters, solution acidity is 1 mol.
The factor that influences iron such as iron nickel, iron copper, iron zinc and other separation of metal ions in the system of chromes isolation of purified ferrous solution in the present invention is a lot; They are the length-to-diameter ratio of extracting chromatographic column, the particle diameter and the porosity size of support, the pH value and the efflux volume of leacheate; The concentration of P204 extraction agent; Factors such as the concentration of iron and other metals ion and acidity in the feed liquid.
When other factors are fixed, along with the increase of extraction agent P204 concentration, extracting and separating factor beta value also increases, if the concentration of extraction agent P204 is less than 30%, loading capacity is little, and production capacity is low; The concentration of extraction agent P204 is greater than 70%, and the support adsorptive capacity is near saturated, so the concentration of extraction agent P204 is 30 ~ 70% scope.
The particle diameter of support isolation of purified to ferrous solution in 70 ~ 150 purpose scopes does not significantly influence.When particle diameter during less than 70 orders, the flow velocity of extracting chromatographic column is fast, the flow of solution state of wayward post; When particle diameter during greater than 150 orders, the flow velocity of extracting chromatographic column is slow, and sepn process is long.Therefore the particle diameter of support is advisable in 70 ~ 150 purpose scopes.
When the total concn of iron was lower than 5 grams per liters in the feed liquid, the feed liquid treatment capacity was bigger, and it is big to consume total acid content; When the total concn of iron is higher than 30 grams per liters in the feed liquid; Iron and other foreign metal ionic separation factor are reduced; In order to guarantee ferrous solution isolation of purified effect preferably; The concentration of iron is at 5 ~ 30 grams per liters in the feed liquid, and feed acidity is 1 mol, and other foreign metal total ion concentration is good less than 1 grams per liter.
Leacheate is the hydrochloric acid soln of 1 mol, and the flow velocity of leacheate is 1.0 ~ 1.5 times/h of chromatograph column void volume.Used strip liquor is 6 mol hydrochloric acid or sulphuric acid solns in back extraction iron liquid.
The invention has the advantages that: P204 extraction chromatography method of the present invention has combined the highly selective of liquid-liquid extraction method and the multistage property of ion exchange method, has strengthened the detergent power of ferrous solution and to have a technical process simple, easy to operate; Equipment capacity is big, invest little, the characteristics that the consumption of chemical materials is little; Chromes make the equipment of whole extraction and separation technology be easy to sealing simultaneously, reduce the irritating smell of the hydrochloric acid soln generation of high density, have improved Working environment.
Following indefiniteness embodiment is just in order to further specify the present invention, rather than as the qualification to the scope of the invention, protection scope of the present invention is determined by claim.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
As shown in Figure 1, be process flow sheet of the present invention.When chromes extracting and separating of the present invention purified ferrous solution, at first, macroporous adsorbent resin carried out saponification absorption to the P204 extraction agent under stirring condition, prepares the P204 extration resin of desired content, packed the P204 extration resin in the extracting chromatographic column into; P204 extration resin post is reinforced with ferrous solution then, makes extraction agent P204 and iron carry out extractive reaction; Secondly; P204 extration resin post to extraction iron carries out drip washing, arrives the leacheate aqueous phase to drip washing such as the metallic impurity in the P204 extration resin post such as nickel, cobalt, copper, zinc, manganese with leacheate, and iron is still stayed in the extraction agent of P204 extration resin; Arrive aqueous phase to the iron back extraction in the P204 extration resin post with sour strip liquor again; Obtain the high purity iron salts solution, carry out drip washing, regeneration to the P204 extration resin post of containing metal impurity with 1N hydrochloric acid at last, the resin after the regeneration continues to recycle.The temperature of carrying out above-mentioned all operations is between 10 ~ 40 degrees centigrade.
The high purity iron salts solution that obtains after the extraction chromatography purification separation is through concentrating iron(ic)chloride or the ferrum sulfuricum oxydatum solutum that obtains iron content 50 ~ 120 grams per liters, and the pH value is 2 ~ 4.Through current density is 15A/dm
2Constant-current electrolysis, 40 ~ 50 ℃ of temperature, titanium is coated with the ruthenium plate and does anode, the titanium plate is done negative electrode, electrolytic deposition obtains negative electrode iron on negative electrode.Negative electrode iron obtains the high-purity ingot iron of purity greater than 4N through vacuum melting, and smelting temperature is greater than 1536 ℃, vacuum tightness 10
-3~ 10Pa.
Embodiment 1
Adopt 10 kilograms of aqueous macroporous adsorbent resins (buying trade mark HPD-100 from market), its correlation parameter:
1, granularity: particle diameter is 70 ~ 150 orders (0.1-0.2mm) >=90%.
2, mean pore size: 85-90 ° A; Specific surface 650-700m
2/ g; Absorption flow velocity: 1-4BV/h; Desorb flow velocity: 0.6-2BV/h; Strippant: ethanol or aqueous ethanolic solution; Strippant consumption: 2-3 BV.
Adopt the mode of saponification absorption to be adsorbed on the macroporous adsorbent resin P204 extraction agent, concrete operations are: 10 kilograms of aqueous macroporous adsorbent resins are put into water, add 2 kilograms P204 extraction agent; Under stirring condition, carry out adsorption treatment, prepare the extration resin of 34%P204 after the filtration, the resin that has adsorbed extraction agent carries out wet method dress post; The diameter of packing into is 80mm; Length is the synthetic glass post of 850mm, is assembled into P204 extration resin post, is about about 400ml through measuring its void volume.
Add 5 liters of iron(ic)chloride feed liquids, wherein concentration of iron is 10 grams per liters, the acidity [H of feed liquid
+] be 1.0 mol, P204 extration resin chromatograph post to be carried out drip washing be about 10 grams per liters until the concentration of iron that drenches fluid, this moment, chromatograph post color was by colourless yellowing.
Use [H then
+] be the P204 extration resin of the hydrochloric acid soln of 1.0 mol as leacheate wash load iron, observe chromatograph post color by yellow become colourless after, promptly arrive the terminal point of washing.Use acidity this moment instead is the iron ion that adsorbs in the rapid wash-out chromatograph of the 6 mol hydrochloric acid solns post; Chromatograph post color is by colourless yellowing in the process; This step adopts sour strip liquor drip washing, and the iron back extraction in the P204 extration resin chromatograph post to aqueous phase, is obtained high-purity ferric chloride Solution(38.
To the drip washing of regenerating of P204 extration resin post, regenerated liquid is 1 mol hydrochloric acid soln at last, and chromatograph post color is become by yellow and finishes when colourless fully in the regenerative process.
The ferric chloride Solution(38 of collecting is concentrated to 100 grams per liters, carries out electrolytic deposition, is 15A/dm through current density
2Constant-current electrolysis, 40 ~ 50 ℃ of temperature, titanium is coated with the ruthenium plate and does anode, the titanium plate is done negative electrode, electrolytic deposition obtains negative electrode iron on negative electrode.Negative electrode iron is through vacuum melting, and smelting temperature is greater than 1536 ℃, vacuum tightness 10
-3~ 10Pa obtains the high-purity ingot iron of purity greater than 4N.
Embodiment 2
Preparation 60%P204 extration resin, experimental working technique is with embodiment 1.Add 5 liters of ferric sulfate feed liquids, wherein concentration of iron is 30 grams per liters, the acidity [H of feed liquid
+] be 1.0 mol, P204 extration resin post to be carried out drip washing be about 30 grams per liters until the concentration of iron that drenches fluid, this moment, chromatograph post color was by the colourless scarlet that becomes.
With [H
+] be the P204 extration resin of the hydrochloric acid soln of 1.0 mol as leacheate wash load iron, observe chromatograph post color by redness become colourless after, promptly arrive the terminal point of washing.Use acidity this moment instead is the iron ion that adsorbs in the rapid wash-out chromatograph of the 6 mol sulphuric acid solns post, and chromatograph post color is by the colourless redness that becomes in the process.
To the drip washing of regenerating of P204 extration resin post, regenerated liquid is 1 mol hydrochloric acid soln at last, and chromatograph post color is become by redness and finishes when colourless fully in the regenerative process.
The ferrum sulfuricum oxydatum solutum of collecting is concentrated to more than 90 grams per liters, carries out electrolytic deposition, and the negative electrode iron that negative electrode obtains obtains high-purity ingot iron through vacuum melting, and the purity of iron is more than the 4N through spectroscopic analysis.
In an embodiment of the present invention, preferably selecting has higher optionally macroporous adsorbent resin to oily matter, and the particle diameter of macroporous adsorbent resin is 70 ~ 150 orders, can make in the sepn process flow velocity suitable like this, is easy to control the flow of solution state of post.The concentration of P204 extration resin is between 30% ~ 70% (weight percentage), and the length-to-diameter ratio that adopts the chromatograph post simultaneously is between 11/1 ~ 5/1, and extracting and separating factor beta value is bigger like this, and loading capacity is moderate, and production capacity is higher, can obtain effect of the present invention preferably.
P204 extration resin through after the strip liquor drip washing can further carry out manipulation of regeneration.Adopting regenerated liquid during manipulation of regeneration is that the hydrochloric acid soln of 1 mol carries out drip washing, and the flow velocity of leacheate is 1.0 ~ 1.5 times/h of chromatograph column void volume.
Claims (6)
1. the method for an extraction chromatography isolation of purified ferrous solution may further comprise the steps:
(1) chromatograph column extracting ferrous solution: adopt the mode of saponification absorption to be adsorbed on the macroporous adsorbent resin P204 extraction agent, prepare the P204 extration resin, carry out wet method dress post; Add iron charge liquid then, P204 extration resin chromatograph post is carried out drip washing;
(2) leacheate drip washing: adopt the P204 extration resin chromatograph post of acid solution as leacheate drip washing load iron;
(3) strip liquor drip washing-concentrate: adopt sour strip liquor drip washing, the iron back extraction in the P204 extration resin chromatograph post to aqueous phase, is obtained the high purity iron salts solution; After the high purity iron salts solution concentrated, carry out electrolytic deposition, the electrodeposition iron that negative electrode obtains obtains high-purity ingot iron through vacuum melting, and the purity of iron is more than the 4N through the glow discharge mass spectrometry analysis.
2. the method for extraction chromatography isolation of purified ferrous solution according to claim 1 is characterized in that: the length-to-diameter ratio of described chromatograph post is 11/1 ~ 5/1.
3. the method for extraction chromatography isolation of purified ferrous solution according to claim 2 is characterized in that: the particle diameter of said macroporous adsorbent resin is 70 ~ 150 orders.
4. the method for extraction chromatography isolation of purified ferrous solution according to claim 3 is characterized in that: the P204 that contains 30% ~ 70wt.% in the said P204 extration resin.
5. according to the method for each described extraction chromatography isolation of purified ferrous solution among the claim 1-4, it is characterized in that: the P204 extration resin that will pass through after the strip liquor drip washing carries out manipulation of regeneration.
6. the method for extraction chromatography isolation of purified ferrous solution according to claim 5 is characterized in that: said manipulation of regeneration is that the hydrochloric acid soln of 1 mol carries out drip washing for adopting regenerated liquid.
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| CN2011103395201A CN102382981A (en) | 2011-11-01 | 2011-11-01 | Method for purifying iron solution by adopting extraction chromatography |
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| CN2011103395201A CN102382981A (en) | 2011-11-01 | 2011-11-01 | Method for purifying iron solution by adopting extraction chromatography |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219959A (en) * | 2015-11-06 | 2016-01-06 | 武汉理工大学 | Adopt the method for Solvent-Impregnated Resins isolation of purified extracting vanadium from stone coal pickling liquor |
| CN105964228A (en) * | 2016-05-17 | 2016-09-28 | 辽宁大学 | P2O4-loaded sodium alginate composite microsphere adsorbent l as well as preparation method and application thereof |
| CN107058765A (en) * | 2017-04-26 | 2017-08-18 | 武汉理工大学 | A kind of V-extracting solvent impregnating resin and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101643859A (en) * | 2008-08-07 | 2010-02-10 | 北京有色金属研究总院 | Process method for separating and purifying cobalt solution by extraction chromatography |
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2011
- 2011-11-01 CN CN2011103395201A patent/CN102382981A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101643859A (en) * | 2008-08-07 | 2010-02-10 | 北京有色金属研究总院 | Process method for separating and purifying cobalt solution by extraction chromatography |
Non-Patent Citations (2)
| Title |
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| 孙辉等: "P204萃取色层法制备高纯三氯化铁溶液", 《湿法冶金》 * |
| 孙辉等: "高纯铁制备技术综述", 《金属功能材料》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219959A (en) * | 2015-11-06 | 2016-01-06 | 武汉理工大学 | Adopt the method for Solvent-Impregnated Resins isolation of purified extracting vanadium from stone coal pickling liquor |
| CN105964228A (en) * | 2016-05-17 | 2016-09-28 | 辽宁大学 | P2O4-loaded sodium alginate composite microsphere adsorbent l as well as preparation method and application thereof |
| CN107058765A (en) * | 2017-04-26 | 2017-08-18 | 武汉理工大学 | A kind of V-extracting solvent impregnating resin and its preparation method and application |
| CN107058765B (en) * | 2017-04-26 | 2019-03-19 | 武汉理工大学 | A kind of V-extracting solvent impregnating resin and its preparation method and application |
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Application publication date: 20120321 |