CN102614842B - Chelate fiber adsorbent for extracting uranium from seawater and preparation method thereof - Google Patents
Chelate fiber adsorbent for extracting uranium from seawater and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method for chelate fiber adsorbent for extracting uranium from seawater. The preparation method includes following steps that (1) ultra-high molecular weight polyethylene fibers are in irradiation treatment, and an irradiation source is a cobalt source or an electron beam; (2) the irradiated ultra-high molecular weight polyethylene fibers are mixed with solution containing graft monomers, graft polyacrylonitrile modified fibers are obtained via graft polymerization, the graft monomers are pure crylonitrile or mixed monomers including crylic acid and crylonitrile, and molar content ratio of the acrylic acid to the crylonitrile in the mixed monomers is smaller than or equal to 1:2; and (3) the graft polyacrylonitrile fibers are in amidoximation reaction, so that cyanogroup is converted into amidoxime group, and accordingly the chelate fiber adsorbent is prepared. The invention further provides the chelate fiber adsorbent obtained by the preparation method, and the adsorbent not only has excellent mechanical properties of the ultra-high molecular weight polyethylene fibers, but also has a fine effect of adsorbing the uranium, and can be reused for extracting the uranium from the seawater for a long time.
Description
Technical field
The present invention relates to adsorbent and preparation method thereof for a kind of extraction of uranium from seawater, relate in particular to chelate fibre adsorbent and preparation method thereof for a kind of extraction of uranium from seawater.
Background technology
Nuclear energy power generation fast development in world wide in recent years, increase fast to the demand of nuclear fuel uranium, and the uranium ore that is applicable to exploitation according to present depletion rate land is enough decades only.The URANIUM IN SEAWATER reserves are huge, approximately have 4,000,000,000 tons, are 4000 times of land reserves.But the concentration of URANIUM IN SEAWATER is very low, only has 3ppb, must carries out enrichment to uranium with sorbing material and could realize " extraction of uranium from seawater ".The extraction of uranium from seawater is a lot of with sorbing material, what application potential was arranged most is polymer-based sorbing material, and they contain the chelating groups such as amidoxim usually, can select the uranyl ion in adsorbing seawater, the Large ratio surface such as macromolecular fibre, film macromolecular material, most suitable as the function sorbing material.
While with adsorbent, carrying out the extraction of uranium from seawater, at first adsorbent is placed into to suitable marine site and adsorbs for a long time (being generally some months), then adsorbent collected from seawater and carried out a series of chemical desorption programs, with acquisition, being rich in uranium enrichment liquid reduction adsorption agent.Desirable adsorbent not only has the adsorbance of good adsorption uranium with selective, also should have mechanical strength preferably, can stand the adsorption and desorption processing procedure, and can reuse repeatedly.High-molecule chelated adsorbent commonly used often has adsorption and desorption performance preferably, but mechanical strength is inadequate, and can not be for a long time, Reusability repeatedly.
Summary of the invention
The present invention, in order to solve extraction of uranium from seawater adsorbent poor mechanical property, the poor problem of repeat performance in prior art, provides chelate fibre adsorbent and preparation method thereof for a kind of extraction of uranium from seawater, specifically by the following technical solutions:
The invention provides a kind of extraction of uranium from seawater preparation method with the chelate fibre adsorbent, comprise the steps: that (1) carry out radiation treatment by superhigh molecular weight polyethylene fibers, described irradiation bomb is cobalt source or electron beam; (2) superhigh molecular weight polyethylene fibers after irradiation is mixed by graft polymerization reaction and obtains graft polypropylene nitrile modified fibre with the solution that contains grafted monomers, described grafted monomers is pure acrylonitrile, or the mix monomer of acrylic acid and acrylonitrile, in the mix monomer of described acrylic acid and acrylonitrile, acrylic acid is less than or equal to 1: 2 with the molar content ratio of acrylonitrile; (3) graft polypropylene nitrile fiber is carried out to amidoximation, make cyano group be converted into amidoxime group, make the chelate fibre adsorbent.
Because the difficult reaction of acrylonitrile, acrylic acid easily reacts, and acrylic acid ratio is too large, will be difficult to effectively introduce acrylonitrile.In the mix monomer of described acrylic acid and acrylonitrile acrylic acid with the molar content of acrylonitrile than preferably being less than or equal to 1: 4.
In step (2), described graft polymerization reaction is so that fiber reaches certain percent grafting is purpose, and the percent grafting of polyacrylonitrile component is 5～200%, and for the adsorption conditions of chelate fibre, preferably scope is 20～100%.
Wherein, the reaction purpose described in step (3) is to make to be grafted on cyano group in the polyacrylonitrile on the UHMWPE fiber (CN) to transfer from a team to another as far as possible fully as amidoxime group (C (NH
2)=N-OH).Method commonly used is as follows: the fiber after grafting is placed in the aqueous solution of hydroxylamine hydrochloride and natrium carbonicum calcinatum, the mol ratio of hydroxylamine hydrochloride and natrium carbonicum calcinatum is 1: 0.5, keep the molar fraction of hydroxylamine hydrochloride excessive than the molar fraction of cyano group in fiber, regulate pH value 6～7 with aqueous sodium carbonate, be 60～80 ℃ in temperature and carry out the hydroxamamide reaction 3～5 hours, take out after reaction, with distilled water, wash and dry, condition and method that washing and the condition of drying and method are this area routine.
Irradiation described in step (1) is undertaken by following any mode: 1., when described radiation source is the cobalt source, described superhigh molecular weight polyethylene fibers is placed in the cobalt source and carries out radiation treatment; The close rate of described irradiation is 0.01～10kGy/h, and the dosage of described irradiation is 0.1～100kGy; 2. when described radiation source is electron beam, described superhigh molecular weight polyethylene fibers is carried out to radiation treatment by electron beam; The close rate of described irradiation is 1～100kGy/s, and the dosage of described irradiation is 5～100kGy.
Conventional irradiation temperature and atmosphere that the temperature of described irradiation and atmosphere are this area; Described irradiation temperature is room temperature; The atmosphere of described irradiation is any in air atmosphere, inert atmosphere, oxygen and vacuum.
At described predose, described superhigh molecular weight polyethylene fibers is carried out to cleaning treatment, purpose is to remove the slurry of fiber surface, promotes graft polymerization reaction.The step of described cleaning is: described superhigh molecular weight polyethylene fibers is placed in to normal heptane and soaks 1～8 hour, then use acetone rinsing, dry.
By this area general knowledge, the superhigh molecular weight polyethylene fibers after described irradiation can store certain hour as required, when to be used, take out and carries out described graft polymerization reaction.
For realizing the percent grafting requirement, the grafted monomers concentration described in step (2) in solution is 20～100wt%; The temperature of described graft polymerization reaction is 30～80 ℃, is preferably 40～70 ℃.
The time of described graft polymerization reaction is 2～24 hours, and preferably the graft polymerization reaction time is 3～6 hours.The solvent of described solution is one or more in methyl alcohol, water, DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO).
Also can contain polymerization inhibitor in described solution, described polymerization inhibitor is preferably 1.0 * 10
-4～2.0 * 10
-3the Mohr's salt of mol/L.
The present invention also provides a kind of extraction of uranium from seawater chelate fibre adsorbent obtained by above-mentioned preparation method.
Superhigh molecular weight polyethylene fibers is to take ultra-high molecular weight polyethylene (english abbreviation UHMWPE) as a kind of high strength, high modulus fibre prepared through special process by raw material, has that density is little, intensity is high, an excellent properties such as corrosion-resistant, shock resistance, anti-cutting, biologically inert.
On the basis that meets this area general knowledge, above-mentioned each optimum condition, but any combination obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material be commercially available obtaining all.
Positive progressive effect of the present invention is:
Adopt method of the present invention to prepare containing together with the chelate fibre of hydroxamamide group, both having inherited preferably the good mechanical property of superhigh molecular weight polyethylene fibers, there is again the performance of higher adsorption uranium, can be prolonged and repeated for the extraction of uranium from seawater.
The specific embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, according to conventional method and condition, or select according to catalogue.
In following embodiment, superhigh molecular weight polyethylene fibers is purchased from Beijing TongYiZhong special fiber Technology Development Co., Ltd's product, trade mark FT-103, molecular weight 3,000,000,3.6 dawn of monofilament linear density.
The percent grafting of pure acrylonitrile monemer calculates according to following formula by weight method:
Fibre weight * 100% before percent grafting=(the front fibre weight of fibre weight-grafting after grafting)/grafting
While in graft polymers, containing acrylic acid, the percent grafting sum that the percent grafting obtained by above-mentioned weight method is graft acrylic acid and acrylonitrile, need to be proofreaied and correct with infra-red sepectrometry, infra-red sepectrometry test: first fiber is shredded, use again pressing potassium bromide troche, survey infared spectrum.
Filament properties test: adopt LLY-06E type electronic mono-fiber strong force instrument, by GB GB9997-88 test ultimate fibre tensile property, each sample in measurement is averaged for 50 times, and strength of filament means the value of thrust of the fracture needs of a fiber, and unit is a li ox (cN).
The experiment of adsorption/desorption uranium: the fiber of the accurate a certain amount of amidoxim of weighing, be placed in certain density uranium solution, adsorb certain hour in 30 ℃ of constant temperature oscillators, leach, measure the concentration of uranium in the rear solution of absorption.Adsorbance is calculated with following formula:
Q＝(C
0-C)V/W
In formula, Q is adsorbance (mg/g); C
0for adsorbing the uranium concentration (mg/L) in front solution; C is the uranium concentration (mg/L) in the rear solution of absorption; V is liquor capacity (L); W is dry adsorbent (g).The carbonate aqueous solution drip washing of fiber after absorption, uranyl ion and carbonate generate stable complex compound, after desorption, fiber washing are dried and are proceeded the adsorption/desorption experiment.
Uranium concentration is measured: the concentration of uranium adopts arsenazo by Spectrophotometry.Get the uranium titer in the 25mL colorimetric cylinder, add 0.4mL arsenazo (III) solution, with the salpeter solution constant volume of pH=2, with reagent blank, make reference, with ultraviolet-uisible spectrophotometer, measure absorption spectrum, select to measure under the 650nm wavelength concentration of uranium.Under selected experiment condition, draw the working curve of uranium content and absorbance, in unknown solution, the concentration of uranium obtains from working curve according to absorbance.
Embodiment 1
(1) pre-irradiation.Accurately take 10.0 gram UHMWPE fibers and be placed in a glass radiation pipe, with sealing after the nitrogen replacement inner air tube.Irradiation tube is put into to the cobalt source, irradiation 15 hours, the irradiation accumulated dose is 50kGy, close rate is 3.3kGy/h.
(2) graft polymerization reaction.Fiber sample after taking-up irradiation, put into rapidly the preprepared graft copolymer solution, and under nitrogen protection, 60 ℃ are reacted 3 hours.Graft copolymer solution is totally 150 grams, consists of: acrylonitrile 60wt%, and acrylic acid 20wt% (acrylic acid and acrylonitrile mol ratio are 1: 4), DMF 20wt%, separately containing H
2sO
40.1mol/L, Mohr's salt 2 * 10
-4mol/L.Take out fiber sample after graft polymerization reaction finishes, clean with DMF, distilled water successively, then dry to constant weight for 60 ℃, weight is 18.5 grams, and percent grafting is 85%, with infrared method, proofreaies and correct, in graft, the polyacrylonitrile percent grafting is 48%, and polyacrylic acid grafted rate is 37%.
(3) amidoximation.By the fiber after grafting in (2), be placed in the 250ml aqueous solution that contains 14 gram hydroxylamine hydrochlorides and 10.6 gram natrium carbonicum calcinatums, regulate pH value 7 left and right with dense sodium carbonate liquor, then be heated to 70 ℃, reaction 3h, take out fiber, washing, dry, obtain the amidoxime group fiber, chelate fibre 20.9 grams of weighing to obtain.
(4) get chelate fibre 0.50 gram, the simulated seawater that to be placed in the 5L uranium concentration be 1.00mg/L carries out adsorption experiment, and adsorption temp is 30 ℃, and adsorption time is 1 week, and in solution, uranium concentration is reduced to 0.72mg/L, and the adsorbance of calculating chelate fibre is 2.8mg/g.
(5) by the carbonate solution drip washing of 0.5mol/L for the chelate fibre of adsorption uranium in (4) step, measure uranium-bearing 1.4mg in leacheate, the uranium of adsorbing fiber is described, and desorption is complete.
(6) circulate as an adsorption desorption by (4), (5) step, repeat 4 times, measure respectively strength of filament, the calculating adsorbance of each fiber, data are listed in table 1.
Known according to the experimental data of embodiment 1, prepared chelate fibre after repeating to use for 5 times to the adsorbance of uranium still up to 2.4mg/g, the adsorbance 2.8mg/g that its adsorption capacity is used has relatively for the first time reduced by 14%, filament strength is reduced to 68cN from 74cN, but still within spendable scope.Therefore, the prepared chelate fibre of the present embodiment can guarantee good absorption property as the extraction of uranium from seawater with adsorbent, can meet the requirement be repeatedly used again.
When described radiation source is the cobalt source, the close rate scope of described irradiation is preferably 0.01～10kGy/h, and dosage range is preferably 0.1～100kGy.Above-mentioned graft polymerization reaction all can carry out under 30～80 ℃, is preferably 40～70 ℃.The graft polymerization reaction time all can carry out at 2～24 hours, and preferably the graft polymerization reaction time is 3～6 hours, and the time is longer, and percent grafting is higher, and the time is shorter, and percent grafting is lower.The temperature range of hydroxamamide reaction is 60～80 ℃ carries out, and reaction time range is 3～5 hours.The percent grafting of polyacrylonitrile component is preferably 5～200%, and preferably scope is 20～100%.
Embodiment 2
(1) pre-irradiation.The UHMWPE fiber is wrapped with aluminium foil, used electron beam irradiation 20kGy, close rate is 50kGy/s, and irradiation atmosphere is air.
(2) graft polymerization reaction.Accurately take the fiber sample after 10.0 gram irradiation, put into the preprepared graft copolymer solution, under nitrogen protection, 60 ℃ of reactions 3 hours.Graft copolymer solution is totally 150 grams, forms: acrylonitrile 60wt%, distilled water 20wt%, DMF 20wt%, Mohr's salt 2 * 10
-4mol/L.Take out sample after graft polymerization reaction finishes, clean with DMF, distilled water successively, then dry to constant weight for 60 ℃, weight is 13.5 grams, and percent grafting is 35%.
(3) amidoximation.By the fiber after grafting in step (2), be placed in the 250ml aqueous solution that contains 14 gram hydroxylamine hydrochlorides and 10.6g gram natrium carbonicum calcinatum, regulate pH value 7 left and right with dense sodium carbonate liquor, then be heated to 70 ℃, reaction 3h, take out fiber, washing, dry, obtain the amidoxime group fiber, chelate fibre 14.9 grams of weighing to obtain.
(4) get chelate fibre 0.50 gram, the simulated seawater that to be placed in the 5L uranium concentration be 1.00mg/L carries out adsorption experiment, and adsorption temp is 30 ℃, and adsorption time is 1 week, and in solution, uranium concentration is reduced to 0.81mg/L, and the adsorbance of calculating chelate fibre is 1.9mg/g.
(5) by the carbonate solution drip washing of 0.5mol/L for the chelate fibre of adsorption uranium in (4) step, measure uranium-bearing 0.94mg in leacheate, the uranium of adsorbing fiber is described, and desorption is complete substantially.
(6) by (4), (5) step is operating as an adsorption desorption circulation, repeats 4 times, measure respectively each fiber strength of filament, calculate adsorbance, data are listed in table 1.
Table 1
Known according to the experimental data of embodiment 2, prepared chelate fibre adsorbance to uranium after repeating 5 uses still reaches 1.7mg/g, the adsorbance 1.9mg/g that its adsorption capacity is used has relatively for the first time reduced by 11%, filament strength is reduced to 85cN from 95cN, but still within spendable scope.The prepared chelate fibre of the present embodiment can guarantee good absorption property as the extraction of uranium from seawater with adsorbent, can meet the requirement be repeatedly used again.
When described radiation source is electron beam, the close rate scope of described irradiation is preferably 1～100kGy/s, and the dosage range of described irradiation is preferably 5～100kGy.
More known by two embodiment, to the graft modification effect difference of superhigh molecular weight polyethylene fibers, also must affect it and finally make the adsorption capacity of chelate fibre to uranium.
Embodiment 3
(1) pre-irradiation.Accurately take 10.0 gram UHMWPE fibers and be placed in a glass radiation pipe, irradiation tube is put into to the cobalt source, irradiation 6 hours, the irradiation accumulated dose is 5kGy, close rate is 0.8kGy/h.
(2) graft polymerization reaction.Fiber sample after taking-up irradiation, put into the preprepared graft copolymer solution, and under nitrogen protection, 40 ℃ are reacted 8 hours.Graft copolymer solution is totally 150 grams, consists of: acrylonitrile 60wt%, and acrylic acid 10wt% (acrylic acid and acrylonitrile mol ratio are 1: 8), DMF 30wt%, separately containing H
2sO
40.1mol/L, Mohr's salt 2 * 10
-4mol/L.Take out fiber sample after graft polymerization reaction finishes, clean with DMF, distilled water successively, then dry to constant weight for 60 ℃, weight is 13.5 grams, and percent grafting is 35%, with infrared method, proofreaies and correct, in graft, the polyacrylonitrile percent grafting is 18%, and polyacrylic acid grafted rate is 17%.
(3) amidoximation.With embodiment 1, obtain chelate fibre 14.4 grams.
(4) get chelate fibre 0.50 gram, the simulated seawater that to be placed in the 5L uranium concentration be 1.00mg/L carries out adsorption experiment, and adsorption temp is 30 ℃, and adsorption time is 1 week, and in solution, uranium concentration is reduced to 0.84mg/L, and the adsorbance of calculating chelate fibre is 1.6mg/g.Data are listed in table 2.
Embodiment 4
1) pre-irradiation.Accurately take 10.0 gram UHMWPE fibers and be placed in a glass radiation pipe, seal after the nitrogen replacement inner air tube, irradiation tube is put into to the cobalt source, irradiation 24 hours, the irradiation accumulated dose is 100kGy, close rate is 4.2kGy/h.
(2) graft polymerization reaction.By sample after irradiation, put into rapidly the preprepared graft copolymer solution, under nitrogen protection, 60 ℃ are reacted 3 hours.Graft copolymer solution is totally 150 grams, forms: acrylonitrile 60wt%, distilled water 20wt%, DMF 20wt%, Mohr's salt 2 * 10
-4mol/L.Take out sample after graft polymerization reaction finishes, clean with DMF, distilled water successively, then dry to constant weight for 60 ℃, weight is 17.5 grams, and percent grafting is 75%.
(3) amidoximation.With embodiment 1, obtain chelate fibre 21.4 grams.
(4) get chelate fibre 0.50 gram, the simulated seawater that to be placed in the 5L uranium concentration be 1.00mg/L carries out adsorption experiment, and adsorption temp is 30 ℃, and adsorption time is 1 week, and in solution, uranium concentration is reduced to 0.78mg/L, and the adsorbance of calculating chelate fibre is 2.2mg/g.Data are listed in table 2.
Embodiment 5
(1) pre-irradiation.The UHMWPE fiber is wrapped with aluminium foil, used electron beam irradiation 100kGy, close rate is 10kGy/s, and irradiation atmosphere is air.
(2) graft polymerization reaction.After radiation treatment sample 2 days, accurately take the fiber sample after 10.0 gram irradiation, put into the preprepared graft copolymer solution, under nitrogen protection, 70 ℃ of reactions 3 hours.Graft copolymer solution is totally 150 grams, consists of: acrylonitrile 60wt%, and acrylic acid 20wt% (acrylic acid and acrylonitrile mol ratio are 1: 4), DMF 20wt%, separately containing H
2sO
40.1mol/L, Mohr's salt 2 * 10
-4mol/L.Take out fiber sample after graft polymerization reaction finishes, clean with DMF, distilled water successively, then dry to constant weight for 60 ℃, weight is 22.5 grams, and percent grafting is 125%, with infrared method, proofreaies and correct, in graft, the polyacrylonitrile percent grafting is 78%, and polyacrylic acid grafted rate is 47%.
(3) amidoximation.Fiber by after grafting in (2), be placed in the 250ml aqueous solution that contains 21 gram hydroxylamine hydrochlorides and 15.3 gram natrium carbonicum calcinatums, with dense sodium carbonate liquor, regulates pH value 7 left and right, then be heated to 70 ℃, reaction 3h, take out fiber, washing, dry, and obtains chelating fiber containing amidoxime group 26.5 grams.
(4) get chelate fibre 0.50 gram, the simulated seawater that to be placed in the 5L uranium concentration be 1.00mg/L carries out adsorption experiment, and adsorption temp is 30 ℃, and adsorption time is 1 week, and in solution, uranium concentration is reduced to 0.66mg/L, and the adsorbance of calculating chelate fibre is 3.4mg/g.Data are listed in table 2.
Table 2
(annotate: the data of embodiment 1 and embodiment 2 are for adsorbing for the first time numerical value.)
By embodiment 1-5, can also see, the acrylonitrile grafting rate is high, and the ability of the chelate fibre adsorption uranium of modification is strong; Acrylic acid and acrylonitrile cograft are conducive to improve the percent grafting of acrylonitrile, the chelate fibre simultaneously obtained has stronger adsorption uranium ability, illustrate acrylic acid content in the mol ratio of acrylic acid and acrylonitrile at 0-1: 2 scope, the increase be preferably in the scope of 1: 4 can promote the adsorption capacity of amidoxime group to uranium.
Claims (8)
1. the preparation method of chelate fibre adsorbent for the extraction of uranium from seawater, it comprises the steps:
(1) superhigh molecular weight polyethylene fibers is carried out to radiation treatment, the irradiation bomb of described irradiation is cobalt source or electron beam;
(2) superhigh molecular weight polyethylene fibers after irradiation is mixed by graft polymerization reaction and obtains graft polypropylene nitrile fiber with the solution that contains grafted monomers, the mix monomer that described grafted monomers is acrylic acid and acrylonitrile, in described mix monomer, the molar content ratio of acrylic acid and acrylonitrile is less than or equal to 1:4 and is more than or equal to 1:8, and the percent grafting of described polyacrylonitrile component is 5～200%;
(3) graft polypropylene nitrile fiber is carried out to amidoximation, make cyano group be converted into amidoxime group, make the chelate fibre adsorbent;
In described step (3), described graft polypropylene nitrile fiber is placed in the aqueous solution of hydroxylamine hydrochloride and natrium carbonicum calcinatum, the mol ratio of hydroxylamine hydrochloride and natrium carbonicum calcinatum is 1:0.5, keep the molar fraction of hydroxylamine hydrochloride excessive than the molar fraction of cyano group in fiber, regulate pH value 6～7 with aqueous sodium carbonate, be 60～80 ℃ in temperature and carry out hydroxamamide reaction 2-5 hour.
2. preparation method as claimed in claim 1, is characterized in that, in described step (2), the percent grafting of described polyacrylonitrile component is 20～100%.
3. preparation method as claimed in claim 1, is characterized in that, described irradiation is undertaken by following any mode:
1. when described radiation source is the cobalt source, described superhigh molecular weight polyethylene fibers is placed in the cobalt source and carries out radiation treatment; The close rate of described irradiation is 0.01～10kGy/h, and the dosage of described irradiation is 0.1～100kGy;
2. when described radiation source is electron beam, described superhigh molecular weight polyethylene fibers is carried out to radiation treatment by electron beam; The close rate of described irradiation is 1～100kGy/s, and the dosage of described irradiation is 5～100kGy.
4. preparation method as described as claim 1 or 3, is characterized in that, the temperature of described irradiation is room temperature; The atmosphere of described irradiation is any in air atmosphere, inert atmosphere, oxygen and vacuum.
5. preparation method as claimed in claim 1, is characterized in that, the grafted monomers concentration in described solution is 20～100wt%; The temperature of described graft polymerization reaction is 30～80 ℃.
6. preparation method as claimed in claim 1, is characterized in that, the time of described graft polymerization reaction is 2～24 hours.
7. preparation method as claimed in claim 1, is characterized in that, the solvent of described solution is one or more in methyl alcohol, water, DMF, dimethyl sulfoxide (DMSO).
8. the chelate fibre adsorbent made by the described preparation method of any one in claim 1～7.
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