CN103894155A - Ion sieve for extracting uranium from water body and preparation method thereof - Google Patents
Ion sieve for extracting uranium from water body and preparation method thereof Download PDFInfo
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- CN103894155A CN103894155A CN201410160788.2A CN201410160788A CN103894155A CN 103894155 A CN103894155 A CN 103894155A CN 201410160788 A CN201410160788 A CN 201410160788A CN 103894155 A CN103894155 A CN 103894155A
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Abstract
The invention provides an ion sieve for extracting uranium from a water body and a preparation method thereof. The ion sieve is prepared from pyrophosphate, molybdate, zirconium oxychloride, hexadecyl trimethyl ammonium bromide, acrylonitrile, and hydroxylamine hydrochloride. The preparation method comprises the steps: preparing a hydrogen ion exchanger of zirconyl-molybdopyrophosphate polyoxometalate by using zirconium oxychloride, the molybdate and the pyrophosphate, introducing a defined amount of uranium ions to the hydrogen ion exchanger, extracting through immobilizing the uranium ions, and baking for forming; then radiating and activating, making a product obtained by radiating and activating react with hexadecyl trimethyl ammonium bromide for performing organic modification, and then adding acrylonitrile and hydroxylamine hydrochloride for performing amine oximation; finally, performing solid-liquid separation, and then performing steps of high-temperature sintering, cooling and grinding, and the like to obtain the ion sieve for extracting uranium from the water body. The prepared ion sieve has a most suitable crystal structure of receiving the uranium ions, shows an efficient selective effect, and has a chelation function and a good selectivity to the uranium ions.
Description
Technical field
The present invention relates to uranium-containing waste water processing technology field, be specifically related to a kind of ion sieve extracting for water body uranium and preparation method thereof.
Background technology
International Energy Agency prediction, will increase by 65% to the year two thousand twenty world energy sources demand, and when the time comes, world energy supplies is by wretched insufficiency, and traditional energy cannot meet human wants, and nuclear energy will play an important role making up in energy breach.Along with the development of the Nuclear Power cause, the processing of uranium-containing waste water also becomes a difficult problem that countries in the world face, uranium mining, and nuclear power station operation, the elimination of nuclear facilities, core original paper production etc. all can produce a large amount of uranium-containing waste waters.Therefore, research and develop a kind of ion sieve extracting for water body uranium of relating to uranium-containing waste water processing technology field and preparation method thereof and there is important using value and strategic importance.
The method of carrying out the extraction of uranium at present from uranium-containing waste water mainly contains ion-exchange, coprecipitation, biological treatment, floatation, superconducting magnetic partition method, absorption method etc., and they respectively have pluses and minuses.As ion-exchange selectively poor, adsorption capacity is lower, easily poisoning and cost is higher, the bioanalysis processing time is long, efficiency is lower, coprecipitation needs the complicated aftertreatment technology such as evaporation and concentration, ion-exchange, counter-infiltration, has increased its industrialization difficulty and cost.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of ion sieve extracting for water body uranium and preparation method thereof.
The ion sieve extracting for water body uranium of the present invention, is characterized in: described ion sieve comprises the raw material of following percent concentration:
Pyrophosphate solution 5% ~ 25%
Molybdate solution 10% ~ 15%
Zirconium oxychloride 5% ~ 20%
Cetyl front three ammonium bromide 10% ~ 25%
Acrylonitrile 15% ~ 30%
Hydroxylamine hydrochloride 15% ~ 20%.
Wherein the content of pyrophosphate is 10% ~ 20%.
Wherein the content of zirconium oxychloride is 5% ~ 15%.
Wherein the content of acrylonitrile is 10% ~ 25%.
Wherein pyrophosphate is potassium pyrophosphate or sodium pyrophosphate.
Wherein molybdate is sodium molybdate or potassium molybdate.
The preparation method of the ion sieve extracting for water body uranium of the present invention, comprises the following steps successively:
(a) make the Hydrogen ion-exchanger of the burnt phosphomolybdic acid zirconium of heteropolyacid salt with zirconium oxychloride, sodium molybdate, potassium pyrophosphate;
(b) add in 1 ~ 200ppm uranyl nitrate solution at Hydrogen ion-exchanger, introduce appropriate uranium ion, then pass through the maintenance of uranium ion, extraction, finally again through baking molding;
(c) the product thing after step b baking molding is packed in irradiation tube, adopt electron beam irradiation to carry out irradiation;
(d) product after irradiation is carried out organically-modified with cetyl front three ammonium bromide;
(e) product after organically-modified, acrylonitrile, distilled water are added in there-necked flask, heating water bath control reaction temperature, at 60 ℃ ~ 80 ℃, stirs 4h ~ 6h; After having reacted, carry out Separation of Solid and Liquid;
(f) product of step e is put into baking oven, under 70 ℃ ~ 90 ℃ temperature conditions, toast 12h ~ 24h;
(g) product of step f is ground, cross 80 order ~ 100 mesh sieves;
(h) preparation 1.5mol/L ~ 2 mol/L hydroxylamine hydrochloride solution, then the product of step g is added in solution; Add the sodium carbonate liquor adjust pH of 1mol/L ~ 1.5 mol/L to neutral; Be placed in water-bath, under 60 ℃ ~ 80 ℃ temperature conditions, stir 2h ~ 4h;
(i) Separation of Solid and Liquid, puts into baking oven by solid and toast 12h ~ 24h under 70 ℃ ~ 90 ℃ temperature conditions; After baked products is ground, cross 80 order ~ 100 mesh sieves, obtain the ion sieve extracting for water body uranium.
In above-mentioned raw materials, pyrophosphate, molybdate, zirconium oxychloride synthesize the burnt phosphomolybdate of heteropolyacid salt matrix of ion sieve by chemical reaction, and it has nonstoichiometric three-dimensional structure; Burnt phosphomolybdate is immersed in certain density uranium solution again, carries out the ion marking, last wash-out, moulding, just obtained the opening structure that is suitable for uranium ion absorption on it; Cetyl front three ammonium bromide plays the effect that connects organo-functional group and ion sieve part; Acrylonitrile and hydroxylamine hydrochloride generate amidoxime group, and it has selective absorption effect to uranium ion.Choosing and percentage range of these raw materials, definite by testing, above-mentioned raw materials and percentage range make a kind of ion sieve extracting for water body uranium of the present invention have efficient sieve effect and sequestering power, can catch efficiently uranium ion, its adsorption capacity is large, contamination resistance is strong, has major progress than prior art.
the specific embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with three specific embodiments, the present invention is described in further detail.
Embodiment 1
1. the potassium pyrophosphate solution of preparation 1.5mol/L, is placed in beaker.The sodium molybdate solution of preparation 1.0mol/L, is slowly added dropwise in potassium pyrophosphate solution with separatory funnel by a certain percentage, constantly magnetic agitation.With after sodium molybdate solution is added dropwise to complete, pH value is adjusted to 2 with 1.5 mol/L hydrochloric acid.
2. the zirconyl chloride solution of preparation 1.0mol/L, slowly drops to zirconyl chloride solution in reactant liquor with separatory funnel, continuous magnetic agitation simultaneously, until precipitate not regeneration, till reacting completely.
3. by reactant liquor ageing 12h, use centrifuge (3000r/min, 15min) by the solution Separation of Solid and Liquid after ageing, solid is washed till neutrality by distilled water.Precipitation is put into 24h under 60 ℃ of conditions of baking oven and dry, solid was ground to 80 mesh sieves.Put into 1.0mol/L nitric acid again and burst, so solid repeatedly repeatedly contacts and bursts with nitric acid.Re-use distilled water solid is washed till to neutrality, put into 16h under 60 ℃ of conditions of baking oven and dry, solid was ground to 80 mesh sieves, obtain the Hydrogen ion-exchanger of burnt phosphomolybdic acid zirconium.
4. obtain after burnt phosphomolybdic acid zirconium, burnt phosphomolybdic acid zirconium immersed in the uranium solution of 50ppm, soak 24 h, make not burnt phosphomolybdic acid zirconium (uranium ion) compound of maintenance, by it 300
oc toasts 8 h, makes the uranium type ion sieve sieve nest of maintenance, then removes uranium ion with the nitric acid wash-out of 2 mol/L, Separation of Solid and Liquid, by solid 200
oCtoast 6 h.
5. then, packed in irradiation tube, be placed in electron beam irradiation irradiation.Solid after irradiation is taken out, be scattered in distilled water, under the condition constantly stirring, slowly drip cetyl front three ammonium bromide with separatory funnel, be added dropwise to complete rear continuation and stir 2h, after this ageing 12h.Centrifuge Separation of Solid and Liquid (3000r/min, 10min), separation to solid be washed till and there is no Br with distillation
-till ion.80 ℃ of baking oven 24h of solid are dried to constant weight, and the solid after oven dry ground 80 mesh sieves, obtained organically-modified burnt phosphomolybdic acid zirconium.
6. by a certain percentage organically-modified burnt phosphomolybdic acid zirconium, acrylonitrile, distilled water are added in there-necked flask, under 60 ℃ of conditions of water-bath, stir 6h.Reacted rear use centrifuge Separation of Solid and Liquid, solid is put into 12h under 70 ℃ of conditions of baking oven dries to constant weight.By the solid abrasive after drying, cross 80 mesh sieves.Preparation 1.5mol/L hydroxylamine hydrochloride solution, adds aforementioned pressed powder wherein, by extremely neutrality of pH value, is placed in water-bath with the sodium carbonate liquor of 1.5 mol/L, stirs 4h at 60 ℃.After this use centrifuge (3000r/min, 10min) by Separation of Solid and Liquid, in baking oven, under 70 ℃ of conditions, 12h is dried to constant weight, will be after solid abrasive crosses 80 mesh sieves, both a kind of ion sieve for the extraction of water body uranium.
Embodiment 2
1. the sodium pyrophosphate solution of preparation 1.5mol/L, is placed in beaker.The potassium molybdate solution of preparation 1.0mol/L, is slowly added dropwise in sodium pyrophosphate solution with separatory funnel by a certain percentage, constantly magnetic agitation.With after sodium molybdate solution is added dropwise to complete, pH value is adjusted to 2 with 1.5 mol/L hydrochloric acid.
2. the zirconyl chloride solution of preparation 1.0mol/L, slowly drops to zirconyl chloride solution in reactant liquor with separatory funnel, continuous magnetic agitation simultaneously, until precipitate not regeneration, till reacting completely.
3. by reactant liquor ageing 12h, use centrifuge (3000r/min, 15min) by the solution Separation of Solid and Liquid after ageing, solid is washed till neutrality by distilled water.Precipitation is put into 24h under 60 ℃ of conditions of baking oven and dry, solid was ground to 80 mesh sieves.Put into 1.0mol/L nitric acid again and burst, so nitric acid repeatedly repeatedly contacts and bursts with solid.Re-use distilled water solid is washed till to neutrality, put into 16h under 60 ℃ of conditions of baking oven and dry, solid was ground to 80 mesh sieves, obtain the Hydrogen ion-exchanger of burnt phosphomolybdic acid zirconium.
4. obtain after burnt phosphomolybdic acid zirconium, burnt phosphomolybdic acid zirconium immersed in the uranium solution of 100ppm, soak 24 h, make not burnt phosphomolybdic acid zirconium (uranium ion) compound of maintenance, by it 300
oc toasts 8 h, makes the uranium type ion sieve sieve nest of maintenance, then removes uranium ion with the nitric acid wash-out of 2 mol/L, Separation of Solid and Liquid, by solid 200
oCtoast 6 h.
5. then, packed in irradiation tube, be placed in electron beam irradiation irradiation.Solid after irradiation is taken out, be scattered in distilled water, under the condition constantly stirring, slowly drip cetyl front three ammonium bromide with separatory funnel, be added dropwise to complete rear continuation and stir 2h, after this ageing 12h.Centrifuge Separation of Solid and Liquid (3000r/min, 10min), separation to solid be washed till and there is no Br with distillation
-till ion.80 ℃ of baking oven 24h of solid are dried to constant weight, and the solid after oven dry ground 80 mesh sieves, obtained organically-modified burnt phosphomolybdic acid zirconium.
6. by a certain percentage organically-modified burnt phosphomolybdic acid zirconium, acrylonitrile, distilled water are added in there-necked flask, under 80 ℃ of conditions of water-bath, stir 5h.Reacted rear use centrifuge Separation of Solid and Liquid, solid is put into 16h under 80 ℃ of conditions of baking oven dries to constant weight.By the solid abrasive after drying, cross 90 mesh sieves.Preparation 2mol/L hydroxylamine hydrochloride solution, adds aforementioned pressed powder wherein, by extremely neutrality of pH value, is placed in water-bath with the sodium carbonate liquor of 1.5 mol/L, stirs 4h at 70 ℃.After this use centrifuge (3000r/min, 10min) by Separation of Solid and Liquid, in baking oven, under 80 ℃ of conditions, 12h is dried to constant weight, will be after solid abrasive crosses 90 mesh sieves, both a kind of ion sieve for the extraction of water body uranium.
Embodiment 3
1. the sodium pyrophosphate solution of preparation 1.5mol/L, is placed in beaker.The sodium molybdate solution of preparation 1.0mol/L, is slowly added dropwise in sodium pyrophosphate solution with separatory funnel by a certain percentage, constantly magnetic agitation.With after sodium molybdate solution is added dropwise to complete, pH value is adjusted to 2 with 1.5 mol/L hydrochloric acid.
2. the zirconyl chloride solution of preparation 1.0mol/L, slowly drops to zirconyl chloride solution in reactant liquor with separatory funnel, continuous magnetic agitation simultaneously, until precipitate not regeneration, till reacting completely.
3. by reactant liquor ageing 12h, use centrifuge (3000r/min, 15min) by the solution Separation of Solid and Liquid after ageing, solid is washed till neutrality by distilled water.Precipitation is put into 24h under 60 ℃ of conditions of baking oven and dry, solid was ground to 80 mesh sieves.Put into 1.0mol/L nitric acid again and burst, so nitric acid repeatedly repeatedly contacts and bursts with solid.Re-use distilled water solid is washed till to neutrality, put into 16h under 60 ℃ of conditions of baking oven and dry, solid was ground to 80 mesh sieves, obtain the Hydrogen ion-exchanger of burnt phosphomolybdic acid zirconium.
4. obtain after burnt phosphomolybdic acid zirconium, burnt phosphomolybdic acid zirconium immersed in the uranium solution of 100ppm, soak 24 h, make not burnt phosphomolybdic acid zirconium (uranium ion) compound of maintenance, by it 300
oc toasts 8 h, makes the uranium type ion sieve sieve nest of maintenance, then removes uranium ion with the nitric acid wash-out of 10ppm, Separation of Solid and Liquid, by solid 200
oCtoast 6 h.
5. then, packed in irradiation tube, be placed in electron beam irradiation irradiation.Solid after irradiation is taken out, be scattered in distilled water, under the condition constantly stirring, slowly drip cetyl front three ammonium bromide with separatory funnel, be added dropwise to complete rear continuation and stir 2h, after this ageing 12h.Centrifuge Separation of Solid and Liquid (3000r/min, 10min), separation to solid be washed till and there is no Br with distillation
-till ion.80 ℃ of baking oven 24h of solid are dried to constant weight, and the solid after oven dry ground 80 mesh sieves, obtained organically-modified burnt phosphomolybdic acid zirconium.
6. by a certain percentage organically-modified burnt phosphomolybdic acid zirconium, acrylonitrile, distilled water are added in there-necked flask, under 70 ℃ of conditions of water-bath, stir 5h.Reacted rear use centrifuge Separation of Solid and Liquid, solid is put into 16h under 80 ℃ of conditions of baking oven dries to constant weight.By the solid abrasive after drying, cross 100 mesh sieves.Preparation 1.8mol/L hydroxylamine hydrochloride solution, adds aforementioned pressed powder wherein, by extremely neutrality of pH value, is placed in water-bath with the sodium carbonate liquor of 1.5 mol/L, stirs 4h at 90 ℃.After this use centrifuge (3000r/min, 10min) by Separation of Solid and Liquid, in baking oven, under 80 ℃ of conditions, 12h is dried to constant weight, will be after solid abrasive crosses 90 mesh sieves, both a kind of ion sieve for the extraction of water body uranium.
The invention has the beneficial effects as follows, for how to extract uranium from uranium-containing waste water, the present invention has researched and developed directly adsorbs uranium ion, selectively strong, a kind of ion sieve that adsorbance is large and preparation method thereof.It has the optimum crystal structure of accepting uranium ion, show efficient selection sieve effect, introduce amidoxime group by irradiation grafting means carrying uranium ion sieve surface simultaneously, made this ion sieve extracting for water body uranium there is sequestering power and better selective to uranium ion.A kind of ion sieve extracting for water body uranium is a kind of have firm three-dimensional bone, nonstoichiometric novel inorganic-organic double compound, uranium ion is had to direct adsorption capacity, can catch efficiently uranium ion, its adsorption capacity is large, contamination resistance is strong, has major progress than prior art.
Claims (7)
1. the ion sieve extracting for water body uranium, is characterized in that: described ion sieve comprises the raw material of following percent concentration:
Pyrophosphate solution 5% ~ 25%
Molybdate solution 10% ~ 15%
Zirconium oxychloride 5% ~ 20%
Cetyl front three ammonium bromide 10% ~ 25%
Acrylonitrile 15% ~ 30%
Hydroxylamine hydrochloride 15% ~ 20%.
2. the ion sieve extracting for water body uranium according to claim 1, is characterized in that: wherein the content of pyrophosphate is 10% ~ 20%.
3. the ion sieve extracting for water body uranium according to claim 1, is characterized in that: wherein the content of zirconium oxychloride is 5% ~ 15%.
4. the ion sieve extracting for water body uranium according to claim 1, is characterized in that: wherein the content of acrylonitrile is 10% ~ 25%.
5. the ion sieve extracting for water body uranium according to claim 1, is characterized in that: wherein pyrophosphate is potassium pyrophosphate or sodium pyrophosphate.
6. the ion sieve extracting for water body uranium according to claim 1, is characterized in that: wherein molybdate is sodium molybdate or potassium molybdate.
7. for the preparation method of the ion sieve extracting for water body uranium claimed in claim 1, it is characterized in that, described method comprises the following steps successively:
(a) make the Hydrogen ion-exchanger of the burnt phosphomolybdic acid zirconium of heteropolyacid salt with zirconium oxychloride, sodium molybdate, potassium pyrophosphate;
(b) add in 1 ~ 200ppm uranyl nitrate solution at Hydrogen ion-exchanger, introduce appropriate uranium ion, then pass through the maintenance of uranium ion, extraction, finally again through baking molding;
(c) the product thing after step b baking molding is packed in irradiation tube, adopt electron beam irradiation to carry out irradiation;
(d) product after irradiation is carried out organically-modified with cetyl front three ammonium bromide;
(e) product after organically-modified, acrylonitrile, distilled water are added in there-necked flask, heating water bath control reaction temperature, at 60 ℃ ~ 80 ℃, stirs 4h ~ 6h; After having reacted, carry out Separation of Solid and Liquid;
(f) product of step e is put into baking oven, under 70 ℃ ~ 90 ℃ temperature conditions, toast 12h ~ 24h;
(g) product of step f is ground, cross 80 order ~ 100 mesh sieves;
(h) preparation 1.5mol/L ~ 2 mol/L hydroxylamine hydrochloride solution, then the product of step g is added in solution; Add the sodium carbonate liquor adjust pH of 1mol/L ~ 1.5 mol/L to neutral; Be placed in water-bath, under 60 ℃ ~ 80 ℃ temperature conditions, stir 2h ~ 4h;
(i) Separation of Solid and Liquid, puts into baking oven by solid and toast 12h ~ 24h under 70 ℃ ~ 90 ℃ temperature conditions; After baked products is ground, cross 80 order ~ 100 mesh sieves, obtain the ion sieve extracting for water body uranium.
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