CN103831090B - A kind of caesium selective absorbent and preparation method thereof - Google Patents
A kind of caesium selective absorbent and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to material preparation and radioactive liquid waste process field, a kind of caesium selective absorbent and preparation method thereof is provided, described caesium selective absorbent is shaped as spherical particle, formed by mass fraction by inorganic ion exchanger and the polyacrylonitrile caesium to high selectivity: 50 ~ 90 parts of inorganic ion exchangers, 10 ~ 50 parts of polyacrylonitrile. The spherical caesium selective absorbent of class of the present invention, both retained the high selectivity of inorganic ion exchanger to caesium, the well-regulated shape of tool again, the spherical profile of its class can make it evenly be seated in fixed bed, solved the difficult problem that former inorganic ion exchanger is unsuitable for fixed-bed operation, prepared adsorbent can be used for the radioactive liquid waste of fixed bed processing nuclear industry and nuclear power station generation. Preparation method's uniqueness of the present invention, have the advantages such as simple to operate, synthesis condition gentleness, and the prilling granulator equipment using is simple, and easy operating is reproducible.
Description
Technical field
The invention belongs to material preparation and radioactive liquid waste process field, be specifically related to a kind of caesium selective absorbent andPreparation method, this sorbing material can be removed caesium from solution, particularly removes in radioactive liquid waste137Cs。
Background technology
Nuclear power station and some other nuclear facilities are in operation, maintenance, retired and can produce a large amount of radioactivity while having an accidentWaste liquid,137Cs is one of main radionuclide in this class waste liquid, and it is a kind of long-life (t1/2=30.17a) high heat releaseFission product, its radioactivity brings long-term impact can to the mankind's living environment. Before the further processing of radioactive wastewater,If first by radioactivity137Cs removes, and both can reduce the time limit of waste water storage and the quality requirement to storage material, again canTo save storage cost.
At present, contain137The processing method of Cs waste liquid mainly contains evaporation, precipitation, ion-exchange etc. Wherein ion-exchangeBe widely used in radioactive wastewater137The removal of Cs, the material that ion-exchange adopts can be divided into two large class, i.e. ion-exchangesResin and inorganic ion exchanger. Conventional ion exchange resin non-refractory and anti-radiation performance are poor, at high temperature, radiation parameterLower can decomposition, causes secondary pollution, increases the difficulty of refuse subsequent treatment, thereby application in Spent Radioactive water treatment is subject toCertain limitation. With Ion Exchange Resin Phase ratio, inorganic ion exchanger advantages, as selective high in caesium, heat endurance andAnti-radiation performance is strong etc., therefore in radioactive wastewater137In the removal material of Cs, the development of inorganic ion exchanger is the most fastSpeed.
In recent years, both at home and abroad for the exploitation of the inorganic ion exchanger of caesium mainly concentrate on alumino-silicate, heteropolyacid salt,The ferrocyanide of transition metal, insoluble polyvalent metal ackd salt, insoluble polyvalent metal hydrous oxide, titan silicate etc.Aspect. These materials have different advantages and disadvantages parts separately, and out-of-shape or particle are too thin mostly, inner mass transfer barPart and bad mechanical strength, be not suitable for fixed-bed operation. For improving the mass transfer dynamics condition of inorganic ion exchanger, oftenBe carried on porous material carrier and make composite, conventional carrier comprises silica gel, titanium dioxide, amberliteFat, polyvinyl alcohol, polyacrylonitrile etc., but the synthetic selective composite of caesium existed inorganic ion exchanger load capacity low in the pastOr the defect such as out-of-shape. Therefore, exploitation is applicable to fixed-bed operation, has homo-ion exchanger resin shape, big or small similarCaesium selective absorbent and preparation method thereof very necessary.
Summary of the invention
The object of the invention is to overcome the selective inorganic ion exchanger of some caesiums at present and be not suitable for fixed-bed operationShortcoming, is ensureing high-adsorption-capacity and optionally under prerequisite, and providing a kind of has compared with strong selectivity to caesium in radioactive wastewaterCaesium selective absorbent and preparation method thereof.
The object of the invention is to be achieved by the following technical measures.
A kind of caesium selective absorbent, described caesium selective absorbent is shaped as spherical particle, by caesium is had to Gao XuanInorganic ion exchanger and the polyacrylonitrile of selecting property form by mass fraction: 50 ~ 90 parts of inorganic ion exchangers, polyacrylonitrile 10~ 50 parts. The diameter of described spherical particle is in the scope of 0.1 to 2.0 millimeter, and preferably diameter is within the scope of 0.5 ~ 0.9 millimeter.
In technique scheme, the inorganic ion exchanger that caesium is had to a high selectivity can be following in any one or severalThe mixture of planting:
(a) ferrocyanide of transition metal: as potassium ferrocyanide cobalt, potassium ferrocyanide nickel, potassium ferrocyanide titanium, ferrous ironPotassium cyanide copper, potassium ferrocyanide cadmium etc.;
(b) alumino-silicate: as zeolite, vermiculite, clay, imvite etc.;
(c) heteropolyacid salt: as ammonium phosphomolybdate, ammonium phosphotungstate, burnt phosphomolybdic acid zirconium, burnt phosphotungstic acid titanium etc.;
(d) insoluble polyvalent metal ackd salt: as titanium phosphate, basic zirconium phosphate etc.;
(e) insoluble polyvalent metal hydrous oxide: as hydrous titanium oxide, hydrated manganese oxide, aqua oxidation tin etc.;
(f) titan silicate: as titanium sodium metasilicate etc.
The present invention also provides a kind of preparation method of above-mentioned caesium selective absorbent, and the method comprises the following steps:
(1) polyacrylonitrile is dissolved in solvent, is mixed with content and is 2 ~ 20% polyacrylonitrile solution;
(2) inorganic ion exchanger powder is added in polyacrylonitrile solution, addition is 1 ~ 9 of polyacrylonitrile dry weightDoubly, under 40 ~ 60 C, fully stir afterwards 2 ~ 3h, slurries are mixed;
(3) slurries that step (2) obtained add prilling granulator, after the ejection of grit blast hole, enter coagulating bath coagulation forming,Make spherical particle caesium selective absorbent through cleaning, being dried.
Wherein, solvent described in step (1) be a kind of of dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO) orSeveral mixtures.
Wherein, described in step (3), coagulating bath is deionized water.
Wherein, in step (3), coagulation bath temperature is 20 ~ 100 C.
Wherein, in step (3), baking temperature is 40 ~ 80 C.
Wherein, the prilling granulator described in step (3) is by admission gear, gas drier structure, gas flow regulating valve, gasFlowmeter body, feed liquor mechanism, prilling spry, solidify mechanism composition, described prilling spry is respectively equipped with air inlet and inlet, instituteState prilling spry and comprise two independently passages, one of them is gas channel, and another is slurry channels, and slurry channels is positioned atWithin gas channel, the centre of the outlet of slurry channels in gas channel outlet, this prilling granulator carries out the flow process of granulationFor, first, the gas that admission gear provides enters gas drier structure, and dried gas enters through gas flow regulating valveGas flowmeter, finally enters the air inlet of prilling spry, and feed liquor mechanism is transported to slurries the inlet of prilling spry, is makingGrain shower nozzle exit, slurries are separated into symmetrical liquid drop under gas effect, and drop splashes into and solidifies mechanism's coagulation forming.
Wherein, the admission gear of described prilling granulator is air compressor, nitrogen cylinder, oxygen cylinder or dioxide bottle;Described drier is filled with drier, and drier is anhydrous calcium chloride or the concentrated sulfuric acid; Described feed liquor mechanism is lead channel, wrigglingPump or plunger displacement pump; Described gas flow flow is counted the mass air flow sensor corresponding with admission gear, nitrogen flow meter, Oxygen FlowAmount meter or carbon dioxide flow meter; Gas flow is 200 ~ 440L/h, and slurry feed flow is 0.2 ~ 5mL/min.
Utilize caesium selective absorbent of the present invention to the method for processing of radioactive liquid waste with ion-exchangePost, static state or alternate manner carry out.
The spherical caesium selective absorbent of class of the present invention, had both retained the high selectivity of inorganic ion exchanger to caesium, againThe well-regulated shape of tool, the spherical profile of its class can make it evenly be seated in fixed bed, has solved former inorganic ion exchangerBe unsuitable for a difficult problem for fixed-bed operation, prepared adsorbent can be used for the radiation of fixed bed processing nuclear industry and nuclear power station generationProperty waste liquid. Preparation method's uniqueness of the present invention, has the advantages such as simple to operate, synthesis condition gentleness, and usePrilling granulator equipment is simple, and easy operating is reproducible.
Brief description of the drawings
Fig. 1 is the structural representation of prilling granulator in the present invention.
Wherein: 1. admission gear, 2. gas drier structure, 3. gas flow regulating valve, 4. gas flowmeter, 5. feed liquorMechanism, 6. prilling spry, 7. solidifies mechanism.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described, but embodiment does not limit the present invention.
Embodiment 1
(1) polyacrylonitrile is dissolved in dimethyl sulfoxide (DMSO), is mixed with content and is 4% polyacrylonitrile solution;
(2) be the potassium ferrocyanide nickel by powder of 4 times of polyacrylonitrile dry weights by quality, particle diameter is less than 160 orders, on adding toState in polyacrylonitrile solution, under 50 C, fully stir afterwards 2h, slurries are mixed;
(3) slurries that step (2) obtained add prilling granulator, after the ejection of grit blast hole, enter coagulating bath coagulation forming,Conventional operation spherical particle polyacrylonitrile/potassium ferrocyanide processed nickel caesium selective absorbents such as cleaning, be dried in process. Institute adoptsPrilling granulator in inlet duct be air compressor machine, feeding device is the lead channel of capacity 10mL, is filled with dense sulphur in drying deviceAcid, gas flow is 380L/h, coagulating bath is deionized water, setting temperature 30 C, spherical particle baking temperature 60 C, gainedGrain diameter is 0.5 ~ 0.9mm.
(4) replace the potassium ferrocyanide nickel powder in step (2) with potassium ferrocyanide cobalt, potassium ferrocyanide titanium powder respectivelyEnd, making particle diameter is polyacrylonitrile/potassium ferrocyanide cobalt, the selection of polyacrylonitrile/potassium ferrocyanide titanium caesium of 0.5 ~ 0.9mmProperty adsorbent.
Embodiment 2
(1) polyacrylonitrile is dissolved in dimethyl sulfoxide (DMSO), is mixed with content and is 2% polyacrylonitrile solution;
(2) be the potassium ferrocyanide cobalt dust of 9 times of polyacrylonitrile dry weights by quality, particle diameter is less than 160 orders, on adding toState in polyacrylonitrile solution, under 40 C, fully stir afterwards 2h, slurries are mixed;
(3) slurries that step (2) obtained add prilling granulator, after the ejection of grit blast hole, enter coagulating bath coagulation forming,Conventional operation spherical particle polyacrylonitrile/potassium ferrocyanide processed cobalt caesium selective absorbents such as cleaning, be dried in process. Institute adoptsPrilling granulator in inlet duct be air compressor machine, feeding device is the lead channel of capacity 10mL, is filled with dense sulphur in drying deviceAcid, gas flow is 380L/h, coagulating bath is deionized water, setting temperature 30 C, spherical particle baking temperature 60 C, gainedGrain diameter is 0.5 ~ 0.9mm.
Embodiment 3
(1) polyacrylonitrile is dissolved in dimethyl sulfoxide (DMSO), is mixed with content and is 20% polyacrylonitrile solution;
(2) be the potassium ferrocyanide cobalt dust of 1 times of polyacrylonitrile dry weight by quality, particle diameter is less than 160 orders, on adding toState in polyacrylonitrile solution, under 60 C, fully stir afterwards 2h, slurries are mixed;
(3) slurries that step (2) obtained add prilling granulator, after the ejection of grit blast hole, enter coagulating bath coagulation forming,Conventional operation spherical particle polyacrylonitrile/potassium ferrocyanide processed cobalt caesium selective absorbents such as cleaning, be dried in process. Institute adoptsPrilling granulator in inlet duct be air compressor machine, feeding device is the lead channel of capacity 10mL, is filled with dense sulphur in drying deviceAcid, gas flow is 380L/h, coagulating bath is deionized water, setting temperature 30 C, spherical particle baking temperature 60 C, gainedGrain diameter is 0.5 ~ 0.9mm.
Embodiment 4
Polyacrylonitrile/potassium ferrocyanide nickel caesium selective absorbent the 0.75g, the 3.45mL that get embodiment 1 gained, be filled inInternal diameter is 6.5mm, long for the glass column of absorbent cotton as supporting layer arranged at 410mm and bottom, contains137Cs concentration is 1.16 ×106The radioactive wastewater that Bq/L, total salinity are 5.62mg/g under the effect of constant flow pump with 2.3mL/min (40BV/h) flowThe glass column of flowing through, wherein BV refers to the packing volume of polyacrylonitrile/potassium ferrocyanide nickel caesium selective absorbent. What table 1 was caesium wearsRate and decontamination factor are with the variation of effluent volume, the penetrance C/C of caesium thoroughly0Represent, wherein C represents that in efflux, caesium is denseDegree, C0Represent initial caesium concentration, decontamination factor represents with DF.
Table 1 polyacrylonitrile/potassium ferrocyanide nickel is processed radioactive wastewater experimental result
Table 1 data show, processing in the process of 2122BV radioactive wastewater, and C/C0Value remains on 0.151 ~ 0.199%,Decontamination factor DF value remains on 500 ~ 665, and polyacrylonitrile/potassium ferrocyanide nickel caesium selective absorbent pair is described137Cs has veryHigh is selective, and adsorption capacity is large.
Embodiment 5
Get polyacrylonitrile/potassium ferrocyanide cobalt caesium selective absorbent 0.75g of embodiment 1 gained, 3.45mL, adopt withThe method that embodiment 4 is identical is processed the aqueous solution containing caesium 20mg/L, and experimental result is as shown in table 2.
Table 2 polyacrylonitrile/potassium ferrocyanide cobalt is processed the aqueous solution experimental result containing caesium 20mg/L
The data of table 2 show, polyacrylonitrile/potassium ferrocyanide cobalt caesium selective absorbent can effectively be removed in the aqueous solutionCesium ion, is 50% place in the penetrance of caesium, processes the caesium solution of about 875.98BV20mg/L.
Embodiment 6
Get polyacrylonitrile/potassium ferrocyanide titanium caesium selective absorbent 0.75g of embodiment 1 gained, 3.45mL, adopt withThe method that embodiment 4 is identical is processed the aqueous solution containing caesium 20mg/L, and experimental result is as shown in table 3.
Table 3 polyacrylonitrile/potassium ferrocyanide titanium is processed the aqueous solution experimental result containing caesium 20mg/L
The data of table 3 show, polyacrylonitrile/potassium ferrocyanide titanium caesium selective absorbent can effectively be removed in the aqueous solutionCesium ion, is 50% place in the penetrance of caesium, processes the caesium solution of about 2311.28BV20mg/L.
Above-described embodiment is only that the present invention is not limited only to above-mentioned example for the ease of illustrating in detail the present invention, onlyIn the scope that will require at this letter of authorization, or those skilled in the art are not departing from the scope of the invention and spiritual carry out eachKind modifications and variations all belong to the protection category of this patent.
Claims (6)
1. a caesium selective absorbent, is characterized in that: described caesium selective absorbent is shaped as diameter at 0.5 ~ 0.9mm modelSpherical particle in enclosing, is made up of by mass fraction inorganic ion exchanger and the polyacrylonitrile caesium to high selectivity,50 ~ 90 parts of inorganic ion exchangers, 10 ~ 50 parts of polyacrylonitrile, the particle diameter of described inorganic ion exchanger powder is less than 160 orders;The described inorganic ion exchanger that caesium is had to a high selectivity be following in any one or a few mixture
(a) ferrocyanide of transition metal: potassium ferrocyanide cobalt, potassium ferrocyanide nickel, potassium ferrocyanide titanium, potassium ferrocyanideCopper, potassium ferrocyanide cadmium;
(b) alumino-silicate: zeolite, vermiculite, clay, imvite;
(c) heteropolyacid salt: ammonium phosphomolybdate, ammonium phosphotungstate, burnt phosphomolybdic acid zirconium, burnt phosphotungstic acid titanium;
(d) insoluble polyvalent metal ackd salt: titanium phosphate, basic zirconium phosphate;
(e) insoluble polyvalent metal hydrous oxide: hydrous titanium oxide, hydrated manganese oxide, aqua oxidation tin;
(f) titan silicate: titanium sodium metasilicate.
2. a preparation method for caesium selective absorbent as claimed in claim 1, is characterized in that comprising the following steps:
(1) polyacrylonitrile is dissolved in solvent, is mixed with content and is 2 ~ 20% polyacrylonitrile solution;
(2) inorganic ion exchanger powder is added in polyacrylonitrile solution, addition is 1 ~ 9 times of polyacrylonitrile dry weight,Under 40 ~ 60 C, fully stir afterwards 2 ~ 3h, slurries are mixed;
(3) slurries that step (2) obtained add prilling granulator, after the ejection of grit blast hole, enter coagulating bath coagulation forming, through clearWash, the dry spherical particle caesium selective absorbent that makes; Described prilling granulator is by admission gear, gas drier structure, gasFlow control valve, gas flowmeter, feed liquor mechanism, prilling spry, solidify mechanism composition, described prilling spry is respectively equipped with air inletMouthful and inlet, described prilling spry comprises two independently passages, one of them be gas channel, another for slurries lead toRoad, within slurry channels is positioned at gas channel, the centre of the outlet of slurry channels in gas channel outlet, this prilling granulatorThe flow process of carrying out granulation is that first, the gas that admission gear provides enters gas drier structure, dried gas process gasFlow control valve enters gas flowmeter, finally enters the air inlet of prilling spry, and slurries are transported to granulation spray by feed liquor mechanismThe inlet of head, in prilling spry exit, slurries are separated into symmetrical liquid drop under gas effect, and drop splashes into that to solidify mechanism solidifyingGu moulding; The admission gear of described prilling granulator is air compressor, nitrogen cylinder, oxygen cylinder or dioxide bottle; Described dryDry mechanism is filled with drier, and drier is anhydrous calcium chloride or the concentrated sulfuric acid; Described feed liquor mechanism is lead channel, peristaltic pump or postPlug pump; Described gas flow is counted the mass air flow sensor corresponding with admission gear, nitrogen flow meter, oxygen flow meter or twoCarbonoxide flowmeter; Gas flow is 200 ~ 440L/h, and slurry feed flow is 0.2 ~ 5mL/min.
3. the preparation method of caesium selective absorbent according to claim 2, is characterized in that: solvent described in step (1)For one or more mixture of dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO).
4. the preparation method of caesium selective absorbent according to claim 2, is characterized in that: step is solidified described in (3)Bathe as deionized water.
5. the preparation method of caesium selective absorbent according to claim 2, is characterized in that: coagulating bath temperature in step (3)Degree is 20 ~ 100 C.
6. the preparation method of caesium selective absorbent according to claim 2, is characterized in that: baking temperature in step (3)Be 40 ~ 80 C.
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