CN107376850A - A kind of sorbing material to uranyl ion under highly acidity with good adsorption properties - Google Patents
A kind of sorbing material to uranyl ion under highly acidity with good adsorption properties Download PDFInfo
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- CN107376850A CN107376850A CN201710722240.6A CN201710722240A CN107376850A CN 107376850 A CN107376850 A CN 107376850A CN 201710722240 A CN201710722240 A CN 201710722240A CN 107376850 A CN107376850 A CN 107376850A
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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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/106—Selenium compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention relates to a kind of sorbing material to uranyl ion under highly acidity with good adsorption properties, is using silica as shell, the nano particle composite material that ASAIII (arsenazo III) is core.The material is obtained by the following manner：By saturation ASAIII aqueous solution 15mL, hexamethylene 150mL, the μ L of Tween 80 30~200, through ultrasound, stir, be 8 with ammoniacal liquor regulation pH；100~600 μ L TEOS are taken, 40mL is diluted to hexamethylene, TEOS cyclohexane solutions are made；The container for filling mixed solution is placed on magnetic stirring apparatus, under the conditions of rotating speed is 400 turns/min, TEOS cyclohexane solutions made from dropwise addition, 200~500 μ L are added dropwise every 15~20min, stopping stirring being added dropwise, liquid is poured out, centrifugation, supernatant is removed, is dried after ethanol washing at 80 DEG C.The material is under highly acidity (pH=1), show preferably to the absorption property of uranyl ion, adsorption rate is up to 65%, hence it is evident that higher than activated carbon ball and the absorbent charcoal material of ASAIII processing, and reusable, the processing especially suitable for low concentration uranium-bearing wastewater under the conditions of highly acidity.
Description
Technical field
The present invention relates to a kind of sorbing material to uranyl ion under highly acidity with good adsorption properties and its preparation
Method, the sorbing material can be used for the removal of highly acidity Uranium in Waste Water acyl ion.
Background technology
Nuclear energy power generation has turned into a trend of energy development, and it has the advantages that, and pollution is small, generated energy is big, efficiency high,
It is a kind of new energy for having development potentiality under the background of current global low-carbon environment-friendly.It can both avoid a large amount of fuel transport and
Consumption, can reduce the pollution to environment again.In addition, nuclear energy as peaceful use important energy source, have been widely used for medical treatment,
Other fields such as industry, agricultural.Wherein uranium and its compoundses are one of indispensable important source materials in nuclear industry, and nuclear reaction
Caused nuclear radiation line and the uranium isotope manually produced are even more effective research tool in many scientific research fields.In recent years, core
The fast development of energy to human society while great economic benefit and social benefit is brought, because of the discharge of its radioactive wastewater
Measure increasing, serious pollution is also result in environment.Low concentration uranium-bearing wastewater source is a lot, in nuclear fuel cycle process
In, exploitation from uranium ore, select smelting and refined waste water, waste water to the manufacture of nuclear fuel original paper, in the operation waste water of reactor all
Containing substantial amounts of uranium, waste water liquid acidity is very high.The experiment of various big hospital, research department and institution of higher learning laboratory in research uranium
Cheng Zhonghui produces a certain amount of uranium-bearing acid waste water, and the pollution to environment also can not be ignored.Uranium is that have natural radioactive member
Element, it is widely used in the various fields such as industry, agricultural and national defence, but it has very big toxicity, radioactive nucleus to organism
After plain uranium enters environment, ecological environment and human health can be damaged, therefore people increasingly pay attention to going for Uranium in Waste Water
Remove and reclaim.
Do not only have heavy metal ion and a variety of soda acid salts in uranium-containing waste water, also containing radioactive elements such as radium, thoriums[4]。
The valence state of uranium in aqueous includes：Trivalent, tetravalence, pentavalent and sexavalence.Trivalent uranium ion is strong reductant, is easily oxidized to four
Valency and sexavalence.Uranous can slowly be oxidized to sexavalence by the oxygen in solution.It is anti-that disproportionation can occur in an acidic solution for pentavalent uranium
Should, a part is reduced to tetravalence, and a part is oxidized to sexavalence.Under normal circumstances, the uranium in the aqueous solution is sexavalence, i.e., with uranium
Acyl ion (UO2 2+) form presence, it is migrated, pH is influenceed on it very greatly, when pH is raised, as uranium sulfate exists in disperse process
pH>Begin to intense hydrolysis when 3, can precipitate completely during pH=5~6, so at low ph conditions, uranium be easier disperse,
Migration, it is soluble preferably to be not easy to remove, except uranium generally refers to removal U (VI) and its compound in water body, i.e., micro uranyl from
Son.
Either recycling uranium resource with improve resource utilization, reduce uranium resource supply and demand gap, or reduce contain
Pollution, reduction injury to human body of the uranium waste water to environment, separating enriched uranium is all necessary from waste water.Handle uranium-containing waste water
Method can be divided into physics, physical chemistry, bioremediation.Have in Physical natural subsidence, filtering, dilution, evaporation and concentration,
Film process etc.；Physical chemistry processing method has chemical precipitation, ion exchange, electrodialysis, absorption etc.；Bioanalysis has bacterium or micro- life
Thing purification etc..At present processing uranium-containing waste water main method have evaporation and concentration, film process, chemical precipitation, ion exchange, absorption and
Biological treatment etc..Wherein absorption method is known as the adsorbent of adsorptivity by selection to radioactive nucleus, solidifies radionuclide, from
And remove Uranium in Waste Water.It has the advantages that material source is abundant, simple, with strong points, is the recovery uranium from uranium-containing waste water
Most popular method.The dominant mechanism of adsorption method for purifying Uranium in Waste Water includes：Ion exchange, surface recombination, surface precipitation and surface
Precipitate reduction etc., key are to select suitable adsorbent.
Common uranium absorption agent has several classes such as clay mineral, biological material, natural polymer, carbon material, but these
The problems such as adsorption efficiency is not high, selectivity is not strong, the production cycle is long, cost is high, recovery is difficult be present in sorbing material.And composite wood
Expect that the adsorbance of made adsorbent is relatively bigger, and composite can select different matrix form to be answered according to different purposes
Close, there is the characteristics of matrix form of diverse.Even more important is a bit, the functional group of composite be it is programmable, can
Adsorptive selectivity of the adsorbent to special metal ion is improved with this.Therefore composite sorbing material is as uranium in recent years
The study hotspot of concentration and separation.Matrices of composite material for absorption requires physics, chemical stability is good, specific surface area is big, hole
Gap rate is high and mainly has resin, fiber, chitosan, carbon material, porous silicon containing the strong functional group of grafting ability, matrix
Deng.But existing sorbing material is also difficult to effectively adsorb uranyl ion under highly acidity at present.Composite
In nuclear shell structured nano material be a fast-developing field in current investigation of materials, it passes through core particle and shell
The ordered fabrication of molecule can realize the joint of the respective characteristic of two kinds of compositions, and wherein silicon covering material has been widely used in many
Among research.Silicon covering material is a kind of porous nano composite with nucleocapsid structure, and the cladding of silica gel can passing through
The modes such as effect, electrostatic attraction, surface deposition, Supramolecular Assembling are realized.Due to its have larger surface area, height it is more
The property of permeability and size adjustable, the reaction such as it can be applied to adsorb, separate, be catalyzed, having been obtained for more and more closing
Note.
The content of the invention
It is an object of the invention to propose a kind of adsorption material to uranyl ion under highly acidity with good adsorption properties
Material, the processing for uranium-containing waste water under highly acidity provide performance more excellent new material.
A kind of sorbing material to uranyl ion under highly acidity with good adsorption properties prepared by the present invention, is with oxygen
The nano particle composite material that SiClx is shell, ASAIII (arsenazo III) is core.
Sorbing material of the present invention is prepared using reverse micro emulsion technology, is comprised the following steps：
A. it is equal through ultrasound, stirring by saturation ASAIII aqueous solution 15mL, hexamethylene 150mL, the μ L of Tween 80 30~200
It is even, it is 8 with ammoniacal liquor regulation pH；
B. 100~600 μ L TEOS are taken, 40mL is diluted to hexamethylene, TEOS- cyclohexane solutions are made；
C. the container for filling step a mixed solutions is placed on magnetic stirring apparatus, under the conditions of rotating speed is 400 turns/min,
TEOS- cyclohexane solutions made from step b are added dropwise, 200~500 μ L are added dropwise every 15~20min, are added dropwise afterwards several times,
Stop stirring, liquid is poured out, centrifuge, remove supernatant, after ethanol washing, sample is dried for 80 DEG C, i.e., contained described in acquisition
ASAIII core shell structure sorbing material.
Test result indicates that the Tween 80 addition described in step a is 50 μ L, the TEOS dosages described in step b are 400 μ
L, when the TEOS- cyclohexane solutions dosage being added dropwise every time after dilution is 400 μ L, the silicon obtained coats ASAIII sorbing materials
Microscopic appearance is optimal, and adsorption effect is also most preferable.
Arsenazo Ⅲ (ASAIII) is a kind of chromotropic acid bisazo class developer, has very strong complexing to make to uranyl ion
With can be with uranyl ion (UO in highly acidity (pH=1~3) medium2 2+)1：1 coordination, because it is dissolved in water, it is impossible to directly use
Make adsorbent, so needing it and water segregation, be encapsulated using core shell structure in silica shell, so as to realize that silica is dredged
The combination of water-based, chemical stability, heat endurance and the strong complexings of ASAIII, prepare a kind of NEW TYPE OF COMPOSITE sorbing material.
There is the microenvironment of particular characteristic using reverse micro emulsion Technology design, prepare the nano particle of various particular characteristics
It is a kind of simple, quick, effective method, is opened up a new way for the preparation synthesis of new material.The preparation of microemulsion
Method has mechanical emulsion process, phase conversion emulsifying and natural emulsification method, and mainly Natural Emulsification is used during nano particle is prepared
Method.Hexamethylene, the saturation ASAIII aqueous solution are well mixed according to a certain percentage with surface active agent tween 80, dripped into system
Solubilization has the hexamethylene of silester, and microemulsion can be formed in certain ratio range.In this microenvironment, pass through catalyst
Catalytic action, TEOS occur hydrolysis, polycondensation, generation silica simultaneously be coated on the outside of ASAIII surfaces drop, preparation is provided
There is nano adsorption material of the core shell structure containing ASAIII.Shell silica can form multiple ducts by specially treated, turn into uranium
The passage of acyl Ion transfer.It is shell with silica, its internal ASAIII is core, has good adsorptivity to uranyl ion
Energy.After the silicon poly aluminum chloride centrifugal filtration for having adsorbed uranyl ion is separated, ion is desorbed by changing pH, is made
Regneration of adsorbent material, the uranium of absorption are also recycled.
Prepared by the inventive method has sorbing material of the core shell structure containing ASAIII under highly acidity (pH=1), performance
Go out preferably to the absorption property of uranyl ion, adsorption rate is up to 65%, hence it is evident that higher than activated carbon ball and the activity of ASAIII processing
Carbon Materials.Illustrate this new sorbing material containing ASAIII with core shell structure to uranyl ion with stronger energy of adsorption
Power, it is a kind of new uranyl ion sorbing material, suitable for the processing of low concentration uranium-bearing wastewater under the conditions of highly acidity, will shows
Go out good application prospect.
Brief description of the drawings
Fig. 1 is the SEM figures (a for the silicon cladding ASAIII sorbing materials that the inventive method obtains：Tween 80 dosage is 50 μ L,
b：Tween 80 dosage is 200 μ L)；
Fig. 2 is the TEM figures for the silicon cladding ASAIII sorbing materials that the inventive method obtains；
Fig. 3 is the IR design sketch for the silicon cladding ASAIII sorbing materials that the inventive method obtains；
Fig. 4 is the influence for the silicon cladding ASAIII sorbing material adsorption capacities that pH obtains to the inventive method；
Fig. 5 is that the silicon that the inventive method obtains coats design sketch of the ASAIII sorbing materials to uranyl ion absorption property；
Fig. 6 is the silicon cladding ASAIII sorbing materials and absorption of other Carbon Materials to uranyl ion that the inventive method obtains
Performance comparison figure (a:Activated carbon ball；b:Impregnate ASAIII silicon cladding activated carbon ball；c:Silicon cladding ASAIII sorbing materials).
Embodiment
The present invention is described in further detail by following examples.
Embodiment 1
Silicon coats the preparation of arsenazo sorbing material.
Configure the saturation ASAIII aqueous solution, concentration 1.4mmol/L.Take saturation ASAIII solution 15mL, hexamethylene 150mL
And 50 μ L Tween 80s, through ultrasound, stir, add about 8mL ammoniacal liquor, regulation pH is 8, is poured into single necked round bottom flask, is placed
On magnetic stirring apparatus, rotating speed is 400 turns/min；400 μ L TEOS are taken, 40mL is diluted to hexamethylene；At room temperature by several times
TEOS- hexamethylene dilute solutions are added dropwise, 400 μ L TEOS- hexamethylene dilute solutions are added dropwise every 15~20min, are stirred when being added dropwise
Mix.Stop stirring after being added dropwise several times, liquid is poured out, centrifuged, remove supernatant, after ethanol washing, by sample
Dried, that is, obtain the 460mg nano particle composite materials of the present invention using silica as shell, ASAIII for core.
Embodiment 2
The ESEM of silicon cladding arsenazo III sorbing material and infrared spectrum analysis.
By SEM electron microscopic pictures, well dispersed microballoon is filtered out, the adsorption material that Tween 80 addition is 50 μ L in Fig. 1 a
Expect, Tween 80 addition is 200 μ L sorbing material in Fig. 1 b, it can be seen that, Tween 80 addition is the nanometer that 50 μ L are obtained
Core shell structure microballoon composite dispersive property is preferable, is also adhered without any, silicon cladding ASAIII sorbing material approximation balls
Shape, surface is smooth, and size is homogeneous, and dispersion effect is preferable, is shown in shell and coats one layer of uniform silicon layer.
Fig. 2 provides the TEM projection electron microscopic pictures of this material, shows silicon cladding ASAIII sorbing materials clearly nucleocapsid knot
Structure.Fig. 3 is the IR spectrograms that silicon coats ASAIII sorbing materials.In 1700cm-1C=O stretching vibration peaks νC=O, this is coupling agent
On carbonyl and SiO2The silicone hydroxyl of ball surface forms the reason of hydrogen bond, illustrates in SiO2Ball surface, which is modified, has connected C=C pairs
Key functional group, in 3000~3700cm-1Between with the presence of-OH vibration peaks, 3 446cm of appearance-1Absorption band is SiO2Surface
Because absorption vapor forms the O-H ... O-H of dimerization νO–H, illustrate not all SiO2The silicone hydroxyl of ball surface all with participation
Si-O-Si keys are formed, the silicone hydroxyl of also part remains in SiO2On the surface of spheroid, 1102cm-1Bands of a spectrum are νSi–OIt is flexible
Vibration.In 1634cm-1, 1080cm-1, 446cm-1Represent to contain ASAIII in sorbing material.806cm-1Absworption peak is Si-O-Si
Symmetrical stretching vibration, 1080cm-1Absworption peak be Si-O-Si antisymmetric stretching vibration, 970cm-1Absworption peak is end group Si-
OH symmetrical stretching vibration.
Embodiment 3
Silicon coats influences of the arsenazo sorbing material pH to uranyl ion absorption property.
ASAIII could be complexed under relatively low pH to uranyl ion, so pH influences to have selected in the experiment of absorption
PH scopes are 0.5~6, and as a result as shown in figure 4, when acidity is very big, silicon coats arsenazo sorbing material to uranyl ion
Hardly adsorb, because substantial amounts of H+Ion and uranyl ion are at war with absorption, cause adsorption rate small, with pH increasing
Add, H in solution+Ion is reduced, and Competition reduces, and has more amino functional groups to be complexed with uranyl ion, so inhaling
Attached rate increase, if pH continues to increase, it would be possible to there is precipitation to generate, but this patent requires that the silicon cladding ASAIII prepared inhales
Enclosure material be used for highly acidity radioactive wastewater in uranium absorption, so selection pH be 1 in the case of progress uranium absorption experiment.
Embodiment 4
Silicon coats absorption property of the arsenazo III sorbing material to uranyl ion equilibrium concentration.
Prepare the uranium solution of ten concentration：1mg/mL uranium standard items take 50 μ L, 100 μ L, 200 μ L, 400 μ L, 800 respectively
μ L, 10mg/mL uranium standard items take 100 μ L, 200 μ L, 400 μ L, 800 μ L, 1000 μ L respectively, supplement water and diluted acid extremely respectively
1mL, PH are 1 or so, and numbering is 1~10.Take silicon to coat each 10mg of ASAIII sorbing materials, be added in ten pipes, ultrasound
5min, standing adsorption 2h, every half an hour concussion once, 3000r/min centrifuges 3min afterwards.Supernatant is taken out respectively, and use is micro-
Measure uranium analysis-e/or determining.Fig. 5 shows absorption property of the silicon cladding ASAIII sorbing materials to uranyl ion equilibrium concentration.As a result
Show, the reduction change of the either increase of adsorbance or adsorption rate is all from fast to slow, because with absorption
Carry out, the adsorption site of material surface is reduced, and progressivelyes reach balance, therefore the change of adsorption rate and adsorbance tends to be steady
It is fixed.
Embodiment 5
Silicon coats the comparison of ASAIII sorbing materials and activated carbon series material absorption property.
The commercially available activated carbon ball 1g splendid to uranyl ion absorption property is taken, saturation ASA III after filtering is added dropwise by several times, repeatedly
Solution total amount is 9mL, is dried under the conditions of 80 DEG C, obtains impregnating ASAIII silicon cladding activated carbon ball sample.Preparing 3 concentration is
1mg/L each 1mL of uranium solution, regulation pH is 1, takes silicon cladding ASAIII sorbing materials, original activity charcoal ball and dipping ASAIII
Silicon cladding each 20mg of activated carbon ball be added thereto, ultrasonic 5min, standing adsorption 2h, every half an hour concussion once, afterwards
3000r/min centrifuges 3min.Supernatant micro-uranium analyzer, the solution uranyl ion equilibrium concentration after measure absorption are taken respectively
Ce, it is analyzed.As shown in fig. 6, in figure, a:Activated carbon ball；b:Impregnate ASAIII silicon cladding activated carbon ball；c:Silicon coats
ASAIII sorbing materials；In low concentration uranyl ion solution, impregnated of saturation ASAIII suction of the Carbon Materials to uranyl ion
Attached rate is above corresponding activated carbon ball, illustrates that the ASAIII in Carbon Materials enhances its absorption property.Under the conditions of pH is 1,
To compare be highest to the adsorption rate of silicon cladding ASAIII sorbing materials, hence it is evident that higher than activated carbon ball, illustrate this material due to
Functional group and more stable structure, good adsorption performance with selective absorption uranyl ion, it is expected to turn into a kind of good
Under the conditions of highly acidity, the sorbing material of radioactivity uranyl ion.
Claims (3)
1. a kind of sorbing material to uranyl ion under highly acidity with good adsorption properties, it is characterized in that using silica as
Shell, the nano particle composite material that ASAIII is core.
A kind of 2. method for preparing sorbing material described in claim 1, it is characterised in that comprise the following steps：
A. by saturation ASAIII aqueous solution 15mL, hexamethylene 150mL and 30~200 μ L Tween 80s, through ultrasound, stir, use
Ammoniacal liquor regulation pH is 8, and mixed solution is made；
B. 100~600 μ L TEOS are taken, 40mL is diluted to hexamethylene, TEOS- cyclohexane solutions are made；
C. the container for filling step a mixed solutions is placed on magnetic stirring apparatus, under the conditions of rotating speed is 400 turns/min, be added dropwise
TEOS- cyclohexane solutions made from step b, 200~500 μ L are added dropwise every 15~20min, are added dropwise afterwards several times, stop
Stirring, liquid is poured out, and is centrifuged, and removes supernatant, after ethanol washing, sample is dried for 80 DEG C, i.e., contained described in acquisition
ASAIII core shell structure sorbing material.
3. preparation method according to claim 2, it is characterised in that the Tween 80 addition described in step a is 50 μ L, step
TEOS dosages described in rapid b are 400 μ L, and the TEOS- cyclohexane solutions dosage being added dropwise every time after dilution is 400 μ L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62114632A (en) * | 1985-11-13 | 1987-05-26 | Osaka Soda Co Ltd | Adsorbent for mercury contained in gas |
| CN102211017A (en) * | 2011-06-11 | 2011-10-12 | 中国海洋大学 | Amidoxime group uranium extraction sorbent and preparation method thereof |
| CN106000418A (en) * | 2016-05-16 | 2016-10-12 | 中国石油大学(北京) | Hydrosilylation heterogeneous catalyst and preparation method thereof |
-
2017
- 2017-08-22 CN CN201710722240.6A patent/CN107376850A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62114632A (en) * | 1985-11-13 | 1987-05-26 | Osaka Soda Co Ltd | Adsorbent for mercury contained in gas |
| CN102211017A (en) * | 2011-06-11 | 2011-10-12 | 中国海洋大学 | Amidoxime group uranium extraction sorbent and preparation method thereof |
| CN106000418A (en) * | 2016-05-16 | 2016-10-12 | 中国石油大学(北京) | Hydrosilylation heterogeneous catalyst and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 彭维: "新型铜和铀吸附材料的制备及其吸附性能的研究", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技I辑》 * |
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Application publication date: 20171124 |