CN104587982A - Material capable of enriching and separating uranium in water solution and preparation method of material - Google Patents
Material capable of enriching and separating uranium in water solution and preparation method of material Download PDFInfo
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- CN104587982A CN104587982A CN201510022179.5A CN201510022179A CN104587982A CN 104587982 A CN104587982 A CN 104587982A CN 201510022179 A CN201510022179 A CN 201510022179A CN 104587982 A CN104587982 A CN 104587982A
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- uranium
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- aqueous solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a material capable of enriching and separating uranium in a water solution and a preparation method of the material. The material capable of enriching and separating the uranium in the water solution is polyacrylic acid modified hydroxyapatite. The material is a uranium separation agent which is easily available in raw materials and relatively good in performance; the preparation method is simple and feasible, and the desorption and absorption conditions of the material are moderate, and no a large amount of strong acid and no a large quantity of toxin harmful substances are not emitted; no secondary pollution is generated and the material is a green novel material; and the material has strong specificity, and elements of a first main group and a second main group have no obvious influences on a separation system.
Description
Technical field
The present invention relates to a kind of can the material of uranium and the preparation method of this material in the concentration and separation aqueous solution.
Background technology
Along with the peaceful use of nuclear energy and the development of nuclear power, the efficiency of Radwastes treatment method and security thereof are the key issues affecting current nuclear energy sustainable development.Thorium is different in nature and role mode etc. as the special metal of a class and common heavy metal element, so will while with reference to original processing method in processing method, and the processing method more wanting positive exploitation new and technique.The method of common process radioactive liquid waste has: ion-exchange-resin process, chemical precipitation method, membrane separation process, extraction and biological adsorption method etc.Efficient with it, the cheap and practical feature of absorption method is one of method of most study in these methods, and adsorbent mainly concentrates on oxide, clay mineral, soil, granite and natural plants and microorganism etc.But these natural adsorbent elements are complicated, in research adsorption mechanism, there is certain difficulty, and workload is also larger.
In recent years, containing can chelating functional group high-molecular gel, the attention simple with its structure, absorption property is excellent, the feature such as reusable causes some researchers.Why this type of material has desirable adsorption effect, its reason is exactly that gel-type high molecular polymer can be swelling in water, form water-fast tridimensional network, by introducing different functional groups on macromolecular chain, such as carboxyl, amino or sulfonic group etc. make it have well and the performance of metallic ion coordination.Owing to its macromolecular chain having hydrophilic radical and hydrophobic group simultaneously, when the environment changes, the hydrogen bonding interaction of the parent of these groups/between hydrophobic effect and macromolecular chain is affected, thus destroy the balance of gel rubber system, gel structure is changed, there is volume phase transition, thus realize the controlled combination of gel to metal ion.But the shortcoming that its radiation-resistant property is not good enough limits it and is processing the application in radioactive metal ion.
While the organic adsorption material development such as high-molecular gel, hydroxyapatite (Hydroxyapatite is called for short HAP), started the attention causing scientist as a kind of inorganic adsorbing material, its chemical composition is Ca
10(PO
4)
6(OH)
2, hexagonal crystal system, has special crystal structure feature, is rich in PO on the surface
4 3-, Ca
2+, OH
-plasma, has good ion-exchange performance, and nanoscale HAP has the performances such as Surface porous structure, specific area are large, high adsorption capacity, is commonly used for the functional material of the depollution of environment such as drinking water and industrial wastewater process field.Simon research group find HAP can from underground water enrichment U (VI) (F.G. Simon, V. Biermann, B. Peplinski, Uranium removal from groundwater using hydroxyapatite,
applied Geochemistry, 2008,23 (8): 2137 – 2145).Cortina research group
[12]synthesize nano-HAP, be successfully used in removing the Cd in the aqueous solution
2+, Cu
2+, Ni
2+, Co
2+, Hg
2+metal ion (J. Oliva, J.D. Pablo, J.L. Cortina, et al, Removal of cadmium, copper, nickel, cobalt and mercury from water by Apatite II
tM: Column experiments,
journal of Hazardous Materials, 2011,194:312 – 323).The radioactive tracer technical research discovery nano-HAP process 1 × 10 of Rosskopfova group
-4the Ni of mol/L
2+during the aqueous solution, in 30 min, clearance can reach 98%.(O. Rosskopfova, M. Galambos, L. Pivarciova, M. Caplovicova, P. Rajec, Adsorption of nickel on synthetic hydroxyapatite from aqueous solutions,
J Radioanal Nucl Chem, 2013, 295(1 ): 459–465 )。Although HAP has excellent absorption property, the preparation cost of HAP is higher, and fragility is large, not easily machine-shaping, and HAP powder is easily reunited simultaneously, reclaims more difficult, and this also just limits its practical ranges as sorbing material.
Summary of the invention
The invention provides a kind of overcome prior art deficiency can the material of uranium in the concentration and separation aqueous solution, and the preparation method of this material.
Of the present invention can the material of uranium be the hydroxyapatite that a kind of polyacrylic acid is modified in the concentration and separation aqueous solution.
Of the present invention can the material preparation method of uranium in the concentration and separation aqueous solution; phosphoric acid is added drop-wise in calcium hydroxide to react under strong agitation condition; acrylic acid and crosslinking agent is added wherein again after reaction terminates; initator is added again after intensification; thermal response is added under inert gas shielding; reaction isolates solid after stopping, then obtains object through cleaning-drying process.
Of the present inventionly can in the concentration and separation aqueous solution a concrete preparation method of the material of uranium be, under vigorous stirring by the H of 0.3M 25mL
3pO
4the Ca (OH) of 50mL 0.25M is added dropwise to the speed of 1mL/min
2in, reaction remains on 55 DEG C, after phosphoric acid is added dropwise to complete, and logical N
2, then add the acrylic acid 1 ± 0.0010g of 1 ± 0.0010g wherein, then add 0.2g N, N-methylene acrylamide, raised temperature controls at 80 DEG C, treats that temperature adds potassium peroxydisulfate 0.5 mg through heating for dissolving after reaching, continues at N
2add thermal response under protection, after 8 hours reaction time, finally product is centrifugal, with washed with de-ionized water, centrifugal, dry process.
The present invention modifies HAP with macromolecular material polyacrylic acid, synthesize the organic/inorganic sorbing material that a class is novel, while keeping it to have excellent concentration and separation ability, the deficiency that can also overcome homogenous material to a certain extent expands its range of application, for the green process realizing radioactive wastewater provides Data support.
The present invention is that a kind of raw material is easy to get, the uranium release agent of better performances, and used is adamantine main component, is actually a kind of novelty teabag of Common materials.
Acrylic acid used in the present invention is cheap and easy to get, macromolecule modifiedly completes with synthesis one step of hydroxyapatite, and method is simple.
Desorption mild condition of the present invention, discharge without a large amount of strong acid and poisonous and harmful substance, the generation of non-secondary pollution thing is a kind of environmental type new material.
High specificity of the present invention, the first main group and the second major element have no significant effect this separation system.In nuke rubbish uranium fission product in be just rich in the first main group and the second major element, such as monovalence Cs, and divalence Sr, by the uranium concentration and separation that success is selected from mixed solution, the further process for mixed solution is provided convenience.Meanwhile, uranium, as its recyclable performance of center energy and material of nuclear energy, will save the energy greatly.
Accompanying drawing explanation
Accompanying drawing 1 is material IR Characterization curve of the present invention.
Accompanying drawing 2 is scanning of materials Electronic Speculum of the present invention.
Accompanying drawing 3 is the influence curve of concussion time to materials adsorption of the present invention.
Accompanying drawing 4 is the influence curve of pH value to the absorption percentage of materials adsorption U (VI) of the present invention.
Accompanying drawing 5 is Na
+ionic strength is to the influence curve of materials adsorption U (VI) of the present invention.
Accompanying drawing 6 is that the initial concentration of U (VI) is to the influence curve of adsorption capacities of materials of the present invention.
Accompanying drawing 7 is the change of temperature on the impact of materials adsorption U (VI) of the present invention.
Accompanying drawing 8 is the material desorption efficiency change of the present invention under different concentration of nitric acid.
Accompanying drawing 9 is material of the present invention multiple adsorb-desorption performance figure.
Detailed description of the invention
The present invention is below in conjunction with embodiment explanation.
One, the preparation of material of the present invention
Under vigorous stirring by the H of 0.3M25mL
3pO
450mL is added dropwise to, the Ca (OH) of 0.25M with the speed of 1mL/min
2in, reaction remains on 55 DEG C, after phosphoric acid is added dropwise to complete, and logical N
2a period of time, then add acrylic acid 1 ± 0.0010g(1:1) or 0.5 ± 0.0010g(2:1), then adding 0.2g crosslinking agent (N, N-methylene acrylamide (TEMED)), raised temperature controls at about 80 DEG C.Treat that temperature is incorporated in initator (potassium peroxydisulfate) 0.5mg of heating for dissolving in small beaker after reaching, continue at N
2add thermal response under protection, amount to 8 hours reaction time.Reaction stop after, product is centrifugal, with washed with de-ionized water repeatedly, centrifugal, dry.
Prepared material characterizes: IR infrared spectrometer (Fourier transform infrared spectrometer, FTIR, Spectrum 100) is analyzed sample infrared absorption characteristic, and infrared figure is shown in Fig. 1.Hitachi S-4800 type field emission scanning electron microscope (scanning electron microscope, SEM) is utilized to obtain the surface topography (see figure 2) of composite.
Two, the adsorption test of material of the present invention
1) preparation of uranium standard liquid: take 0.2824 g U
3o
8in 25ml beaker, drip a small amount of red fuming nitric acid (RFNA) heating for dissolving and be evaporated near dry, after then adding one or two red fuming nitric acid (RFNA), with deionized water constant volume in 1000 mL volumetric flasks.
2) concentration and separation test: static method is used in this experiment, research U (VI) absorption on functional hydroxy apatite.A certain amount of adsorbent solution, deionized water and functional hydroxy apatite is added, with NaOH and HCl (HNO in the polyethylene tool plug test tube of 10 mL
3) be adjusted to certain pH, keep cumulative volume to be 5 mL, shake in isothermal vibration device under 25 ± 0.1 DEG C of conditions.Reach after balance until system, centrifuging and taking supernatant 1 mL is placed in 25 mL volumetric flasks, then adds 0.5 mol/L HNO
3solution 1 mL, 0.1% arsenazo Ⅲ is settled to scale 2 mL, and develop the color 20 min, measures U (VI) content.Relevant test and result as follows:
(1) equilibration time tested
Fig. 3 is shown in the impact of concussion time on the absorption of uranyl.Result shows that at uranyl initial concentration be 2.0012 × 10
-4mol/L, solid-to-liquid ratio is 0.08 g/L, pH is 4 ± 0.05, when temperature is 25 ± 0.1 DEG C, reaches balance very soon, and absorption percentage is higher.As can be seen from Figure, equilibration time is about 10 min, and therefore material of the present invention is the material of a Fast-Balance.
(2) impact of pH value
Fig. 4 is shown in the impact of pH value on functional hydroxy apatite absorption U (VI).As can be seen from Figure, the adsorbance impact of pH on U (VI) is very large, when pH value is less than 3.5, adsorbance increases along with the increase of pH value: as 3.5<pH<5.5, adsorbance is substantially constant: and when pH value is greater than 5.5, then adsorbance reduces along with the increase of pH value.
(3) impact of ionic strength
Na
+fig. 5 is shown in the impact of ionic strength on functional hydroxy apatite absorption U (VI).As can be seen from Figure, Na
+from in the scope of 0 ~ 1 mol/L, in acid medium, the absorption percentage of functional hydroxy apatite to U (VI) is substantially constant, i.e. Na
+intensity does not almost affect absorption behavior.
(4) impact of initial concentration
Fig. 6 is shown in the impact of initial concentration on adsorbance of U (VI).By to scheme and data show, pH in 3.0 ± 0.01(adsorption rate now between 60% to 70%) under condition, functional hydroxy apatite to U (VI) though adsorbance U (VI) concentration increase and increase, when reaching certain value, adsorbance is tending towards saturated.
(5) impact of system temperature
Fig. 7 is shown in the impact of temperature on absorption U (VI) adsorbance, and by finding out, along with the rising of asking, adsorbance increases to some extent, and therefore this reaction is the endothermic reaction.But as a whole, the impact of temperature on adsorbance is little.
3) desorb
Condition during absorption is: by absorption time uranyl nitrtate initial concentration be 1.3412 × 10
-3mol/L, solid-to-liquid ratio is 0.08 g/L, and temperature is 25 ± 0.1 DEG C, and pH value is 4.00 ± 0.05, and the concussion time is 20 min, under 650 nm wavelength condition, survey its absorbance, centrifugally to be washed out by supernatant dropper afterwards, then dries at 50 DEG C.Get 5 polyethylene tool plug test tubes, after above condition process, add the salpeter solution of different concentration respectively, after centrifugal after shaking 20 min, under the wavelength of 650nm, survey its absorbance.Calculate desorption efficiency as Fig. 8.Find that salpeter solution concentration just can be resolved completely at 0.01M.
4) cycle-index
Under different acidity after desorb, one that chooses maximal solution pipette is continued repetition twice by primary condition, and as Fig. 9 shows, adsorption rate during its recycling of material of the present invention decreases, but still has good adsorption rate.
Claims (3)
1. can the material of uranium in the concentration and separation aqueous solution, it is characterized in that the hydroxyapatite that a kind of polyacrylic acid is modified.
2. according to claim 1 can uranium material preparation method in the concentration and separation aqueous solution; it is characterized in that under strong agitation condition, phosphoric acid being added drop-wise in calcium hydroxide reacting; acrylic acid and crosslinking agent is added wherein again after reaction terminates; initator is added again after intensification; thermal response is added under inert gas shielding; reaction isolates solid after stopping, then obtains object through cleaning-drying process.
3. according to claim 2 can uranium material preparation method in the concentration and separation aqueous solution, it is characterized in that under vigorous stirring by the H of 0.3M 25mL
3pO
4the Ca (OH) of 50mL 0.25M is added dropwise to the speed of 1mL/min
2in, reaction remains on 55 DEG C, after phosphoric acid is added dropwise to complete, and logical N
2, then add the acrylic acid 1 ± 0.0010g of 1 ± 0.0010g wherein, then add 0.2g N, N-methylene acrylamide, raised temperature controls at 80 DEG C, treats that temperature adds potassium peroxydisulfate 0.5mg through heating for dissolving after reaching, continues at N
2add thermal response under protection, after 8 hours reaction time, finally product is centrifugal, with washed with de-ionized water, centrifugal, dry process.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622098A (en) * | 2017-01-06 | 2017-05-10 | 大工（青岛）新能源材料技术研究院有限公司 | Method for enriching and detecting cobalt ions in water by using hydroxyapatite adsorption characteristics |
| CN107670645A (en) * | 2017-11-09 | 2018-02-09 | 中国工程物理研究院核物理与化学研究所 | Separation material of thorium and uranium and preparation method thereof in a kind of separation aqueous solution |
| CN110508232A (en) * | 2019-08-30 | 2019-11-29 | 广州大学 | The method that the preparation method and applications and hydroxyapatite of hydroxyapatite remove uranium in waste water |
| CN113842892A (en) * | 2020-06-28 | 2021-12-28 | 西南科技大学 | Method for treating uranium-containing wastewater by using amide/phosphate group modified natural fibers |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308016A (en) * | 2000-11-10 | 2001-08-15 | 中国科学院上海硅酸盐研究所 | Preparation of low temperature sinterable hydroxyapatite powder |
| CN103588187A (en) * | 2013-11-14 | 2014-02-19 | 安徽淮化股份有限公司 | Preparation method of nano bioactive material |
-
2015
- 2015-01-16 CN CN201510022179.5A patent/CN104587982B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308016A (en) * | 2000-11-10 | 2001-08-15 | 中国科学院上海硅酸盐研究所 | Preparation of low temperature sinterable hydroxyapatite powder |
| CN103588187A (en) * | 2013-11-14 | 2014-02-19 | 安徽淮化股份有限公司 | Preparation method of nano bioactive material |
Non-Patent Citations (1)
| Title |
|---|
| 王金磊等: "聚乙烯醇/聚丙烯酸/羟基磷灰石复合高吸水性树脂的制备及溶胀行为", 《高分子材料科学与工程》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622098A (en) * | 2017-01-06 | 2017-05-10 | 大工（青岛）新能源材料技术研究院有限公司 | Method for enriching and detecting cobalt ions in water by using hydroxyapatite adsorption characteristics |
| CN107670645A (en) * | 2017-11-09 | 2018-02-09 | 中国工程物理研究院核物理与化学研究所 | Separation material of thorium and uranium and preparation method thereof in a kind of separation aqueous solution |
| CN107670645B (en) * | 2017-11-09 | 2020-02-21 | 中国工程物理研究院核物理与化学研究所 | Separation material for separating thorium and uranium in aqueous solution and preparation method thereof |
| CN110508232A (en) * | 2019-08-30 | 2019-11-29 | 广州大学 | The method that the preparation method and applications and hydroxyapatite of hydroxyapatite remove uranium in waste water |
| CN113842892A (en) * | 2020-06-28 | 2021-12-28 | 西南科技大学 | Method for treating uranium-containing wastewater by using amide/phosphate group modified natural fibers |
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