CN104147810A - Adsorption separation method for removing iron ions in cobalt or nickel ion water solution - Google Patents
Adsorption separation method for removing iron ions in cobalt or nickel ion water solution Download PDFInfo
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- CN104147810A CN104147810A CN201410374407.0A CN201410374407A CN104147810A CN 104147810 A CN104147810 A CN 104147810A CN 201410374407 A CN201410374407 A CN 201410374407A CN 104147810 A CN104147810 A CN 104147810A
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Abstract
The invention discloses an adsorption separation method for removing iron ions in a cobalt or nickel ion water solution. The method can selectively remove ferric ions in the solution by using a carbon nanotube/poly(sodium-p-styrenesulfonate) composite material as an adsorbent. The carbon nanotube/poly(sodium-p-styrenesulfonate) composite material is a stable nanocomposite material formed by winding poly(sodium-p-styrenesulfonate) on the wall of a carbon nanotube. The solution is one of a Co<2+>/Fe<3+>water solution, a Ni<2>+/Fe<3+>water solution or a Co<2+>/ Ni<2+>/Fe<3+>water solution. The method adopts the carbon nanotube/poly(sodium-p-styrenesulfonate) composite material as the adsorbent so as to realize selective adsorption of Fe<3+>. The method is easy and convenient to operate, is less in cobalt nickel loss and does not have environmental pollution.
Description
Technical field
The invention belongs to the separating and purifying technology field of valuable metal, be specifically related to a kind of adsorption separating method of removing ferric ion in cobalt or the nickel ion aqueous solution, and the application using carbon nano-tube/poly SSS composite as selective absorbent.
Background technology
Iron, cobalt and nickel are three kinds of elements adjacent in the periodic table of elements, and physicochemical properties are close, in occurring in nature symbiosis, association.For example, in the process of the hydrometallurgy of cobalt, nickel minerals, a large amount of iron tramps can leach with cobalt and nickel.Optionally remove Co
2+or Ni
2+fe in the aqueous solution
3+it is a difficult point always.
At present, remove Co
2+or Ni
2+fe in the aqueous solution
3+mainly contain two kinds of methods: chemical precipitation method and solvent extraction.Chemical precipitation method is optionally to precipitate Fe by controlling the acid-base value of solution
3+, the Fe (OH) generating
3in solution, conventionally with colloidal state, exist, can not be thoroughly separated from solution, cause clearance low.Solvent extraction is to utilize extractant by Fe
3+from Co
2+or Ni
2+transfer in Aqueous Solution move on in organic phase.Select suitable extractant can reach high deironing rate, but in separation process, produce a large amount of organic phase waste liquids, contaminated environment.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the adsorption separating method of selectively removing iron ion that a kind of clearance is high, do not produce pollutant, convenient operation is provided.
The present invention proposed first a kind of utilize carbon nano-tube/poly SSS composite as adsorbent, optionally remove the adsorption separating method of the ferric ion impurity in cobalt ions or the nickel ion aqueous solution.The present invention proposes that a kind of to take carbon nano-tube/poly SSS composite be adsorbent, optionally remove the ferric ion in solution; Described carbon nano-tube/poly SSS composite is that kayexalate is wrapped in the stable nano composite material forming on the tube wall of CNT; Described solution is Co
2+/ Fe
3+the aqueous solution, Ni
2+/ Fe
3+the aqueous solution or Co
2+/ Ni
2+/ Fe
3+the aqueous solution any.
Adsorption separating method of the present invention, comprises the steps: that (1) regulates the pH containing ferric cobalt ions or the nickel ion aqueous solution is 1.0～2.0; (2) in the metal ion aqueous solution, drop into enough carbon nano-tube/poly SSS composites; (3) Separation of Solid and Liquid after absorption certain hour.
In adsorption separating method of the present invention, described carbon nano-tube/poly SSS composite as adsorbent is to obtain by following preparation method: CNT is added in hydrochloric acid solution to thermal agitation to remove the metal impurities in CNT, CNT after purifying is ultrasonic dispersion in the aqueous solution of kayexalate, then add thermal agitation, filtration washing is dried.
In adsorption separating method of the present invention, before adsorbing separation, the pH of described metallic cobalt ion or the nickel ion aqueous solution is adjusted to 1.0～2.0, then, described adsorbent is dropped into wherein, Separation of Solid and Liquid after absorption, separated removal iron ion, thereby the highly purified cobalt of the iron ion that is removed or the nickel ion aqueous solution.
In adsorption separating method of the present invention, carbon nano-tube/poly SSS composite is as selective absorbent, and alternative is adsorbed Fe
3+, Co
2+, Ni
2+fe in mixed liquor
3+.Mainly utilized the difference of sulfonic group and different metal ion species affinity under strong acidic condition, with Fe
3+affinity be significantly better than Co
2+and Ni
2+.CNT provides the carrier of nanoscale on the one hand for avtive spot sulfonic group, be conducive to metal ion and sulfonic interaction, makes on the other hand adsorbent separated from solution after absorption.
In adsorption separating method of the present invention, adsorbent carbon nano-tube/poly SSS composite obtains by following preparation method:
(1) CNT is added in hydrochloric acid solution to thermal agitation, to remove the metal impurities in CNT;
(2) above-mentioned product ultrasonic agitation in the aqueous solution of kayexalate, the black dispersion liquid of gained adds thermal agitation, and filtration washing is also dried, and obtains carbon nano-tube/poly SSS compound adsorbent.
In adsorption separating method of the present invention, the carbon nano-tube/poly SSS composite of take is adsorbent, removes Co
2+or Ni
2+fe in solution
3+time, first regulate metal ion mixed liquor for pH is 1.0～2.0, then drop into enough adsorbents, absorption after Separation of Solid and Liquid, the highly purified cobalt ions of the iron ion that is removed or the nickel ion aqueous solution.
In adsorption separating method of the present invention, metal ion mixed aqueous solution can be Co
2+/ Fe
3+mixed aqueous solution, Ni
2+/ Fe
3+mixed aqueous solution or Co
2+/ Ni
2+/ Fe
3+any in mixed aqueous solution.
In adsorption separating method of the present invention, further, when adsorbing separation, to adsorbent ultrasonic dispersion in advance, adsorption effect is better.In a specific embodiments, can be by direct ultrasonic being dispersed in metal ion mixed aqueous solution of adsorbent, the dispersion liquid that adsorbent can also be obtained in deionized water for ultrasonic adds in metal ion mixed aqueous solution.
In adsorption separating method of the present invention, the adsorbent carbon nano-tube/poly SSS of dispersion can precipitate in adsorption process in spontaneous reunion, can be conveniently separated from solution after absorption.
The present invention also proposes carbon nano-tube/poly SSS composite to be used as the application of selective absorbent.
The invention allows for a kind of Fe
3+selective absorbent, is carbon nano-tube/poly SSS composite, is that kayexalate is wrapped in the stable nano composite material forming on the tube wall of CNT.
The present invention has proposed the Fe for selective absorption solution by carbon nano-tube/poly SSS composite first
3+application.Described carbon nano-tube/poly SSS composite is that kayexalate is wrapped in the stable nano composite material forming on the tube wall of CNT.Described solution is Co
2+/ Fe
3+the aqueous solution, Ni
2+/ Fe
3+the aqueous solution or Co
2+/ Ni
2+/ Fe
3+the aqueous solution any.
The present invention discloses first carbon nano-tube/poly SSS composite has been used as to adsorbent, realizes Fe
3+selective absorption, its beneficial effect also comprises: the raw material of preparing adsorbent is simple, and preparation process is easy, environmentally safe can scale manufacture in enormous quantities; In adsorption separation process, consumption of chemical agent is few, environmentally safe.Research experiment of the present invention shows, this adsorbent is optionally removed Co
2+or Ni
2+fe in solution
3+, and substantially there is no the loss of cobalt nickel.
The specific embodiment
In conjunction with following specific embodiment, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Do not deviating under the spirit and scope of inventive concept, variation and advantage that those skilled in the art can expect are all included in the present invention, and take appending claims as protection domain.Implement process of the present invention, condition, reagent, experimental technique etc., except the content of mentioning specially below, be universal knowledege and the common practise of this area, the present invention is not particularly limited content.
Embodiment 1
The preparation of adsorbent: 1g CNT (many walls, average caliber 15nm) put in the hydrochloric acid solution of 400mL6mol/L, in 100 ℃ of oil baths, add thermal agitation 6 hours, naturally cool to room temperature, then centrifugal, and extremely neutral with a large amount of deionized water centrifuge washings, 60 ℃ of products are dried 12 hours, obtain the CNT of purifying.The ultrasonic dispersion in kayexalate (molecular weight 70000) aqueous solution of 200mL1wt% of the CNT of 0.2g purifying, until can't see suspended particulate substance, then 50 ℃ of the dispersion liquids of black are stirred 15 hours, cooling, with aperture, it is 0.22 μ m acetyl cellulose film suction filtration black dispersion liquid, and wash by a large amount of deionized waters, filtering medium is dried 12 hours at 60 ℃, obtain the CNT that kayexalate macromolecular chain is wound around, i.e. carbon nano-tube/poly SSS compound adsorbent.
Embodiment 2
Co
2+/ Ni
2+/ Fe
3+fe in mixed liquor
3+removal: configuration 20mL Co
2+/ Ni
2+/ Fe
3+ar ion mixing liquid, the concentration of each ion is Fe
3+=10ppm, Co
2+=Ni
2+=100ppm, using the pH of watery hydrochloric acid and sodium hydroxide solution regulator solution is 1.3.Get 100mg adsorbent, put in mixed liquor, ultrasonic dispersion 2min, then adsorbs 5h under normal temperature.Mixed liquor is filtered, obtain mixed liquor after removal of impurities, use inductively coupled plasma atomic emission to measure the concentration of three kinds of elements, experiment obtains following result: Fe repeatedly
3+< 1ppm, Co
2+> 99ppm, Ni
2+> 99ppm.
Claims (6)
1. an adsorption separating method of removing iron ion in solution, is characterized in that, the carbon nano-tube/poly SSS composite of take is adsorbent, optionally removes the ferric ion in solution; Described carbon nano-tube/poly SSS composite is that kayexalate is wrapped in the stable nano composite material forming on the tube wall of CNT; Described solution is Co
2+/ Fe
3+the aqueous solution, Ni
2+/ Fe
3+the aqueous solution or Co
2+/ Ni
2+/ Fe
3+the aqueous solution any.
2. adsorption separating method as claimed in claim 1, is characterized in that, before adsorbing separation, the pH of described cobalt ions or the nickel ion aqueous solution is adjusted to 1.0～2.0, described adsorbent is dropped into wherein to Separation of Solid and Liquid after absorption, the cobalt of the iron ion that can be removed or the nickel ion aqueous solution.
3. adsorption separating method as claimed in claim 1, is characterized in that, when adsorbing separation, to adsorbent ultrasonic dispersion in advance.
4. adsorption separating method as claimed in claim 1, is characterized in that, described adsorbent is spontaneous reunion in adsorption process.
5. adsorption separating method as claimed in claim 1, it is characterized in that, described carbon nano-tube/poly SSS composite obtains by following preparation method: CNT is added in hydrochloric acid solution to thermal agitation to remove the metal impurities in CNT, CNT after purifying is ultrasonic dispersion in the aqueous solution of kayexalate, then add thermal agitation, filtration washing is dried.
6. the Fe of carbon nano-tube/poly SSS composite in selective absorption solution
3+application, it is characterized in that, described carbon nano-tube/poly SSS composite is that kayexalate is wrapped in the stable nano composite material forming on the tube wall of CNT; Described solution is Co
2+/ Fe
3+the aqueous solution, Ni
2+/ Fe
3+the aqueous solution or Co
2+/ Ni
2+/ Fe
3+the aqueous solution any.
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|---|---|---|---|
| CN201410374407.0A CN104147810A (en) | 2014-07-31 | 2014-07-31 | Adsorption separation method for removing iron ions in cobalt or nickel ion water solution |
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|---|---|---|---|
| CN201410374407.0A CN104147810A (en) | 2014-07-31 | 2014-07-31 | Adsorption separation method for removing iron ions in cobalt or nickel ion water solution |
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Family
ID=51873559
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110733031A (en) * | 2019-09-26 | 2020-01-31 | 广东工业大学 | quick response self-sensing polymorphic shape memory soft body driver and preparation method and application thereof |
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| CN101058417A (en) * | 2007-04-06 | 2007-10-24 | 华东理工大学 | Electric polyaniline derivative surface modified water decentralized carbon nano-tube and preparation method |
| US20080023396A1 (en) * | 2004-05-13 | 2008-01-31 | Hokkaido Technology Licensing Office Co., Ltd. | Fine Carbon Dispesion |
| CN101234341A (en) * | 2008-02-28 | 2008-08-06 | 上海交通大学 | Method for preparing functional polymer-active carbon composite material for water treatment |
| CN102500318A (en) * | 2011-09-28 | 2012-06-20 | 武汉工程大学 | Surface modification method of carbon nanotube, carbon nanotube and application thereof |
-
2014
- 2014-07-31 CN CN201410374407.0A patent/CN104147810A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080023396A1 (en) * | 2004-05-13 | 2008-01-31 | Hokkaido Technology Licensing Office Co., Ltd. | Fine Carbon Dispesion |
| CN101058417A (en) * | 2007-04-06 | 2007-10-24 | 华东理工大学 | Electric polyaniline derivative surface modified water decentralized carbon nano-tube and preparation method |
| CN101234341A (en) * | 2008-02-28 | 2008-08-06 | 上海交通大学 | Method for preparing functional polymer-active carbon composite material for water treatment |
| CN102500318A (en) * | 2011-09-28 | 2012-06-20 | 武汉工程大学 | Surface modification method of carbon nanotube, carbon nanotube and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110733031A (en) * | 2019-09-26 | 2020-01-31 | 广东工业大学 | quick response self-sensing polymorphic shape memory soft body driver and preparation method and application thereof |
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Application publication date: 20141119 |