CN108554365A - A kind of uranium absorption agent and preparation method thereof - Google Patents
A kind of uranium absorption agent and preparation method thereof Download PDFInfo
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- CN108554365A CN108554365A CN201810255375.0A CN201810255375A CN108554365A CN 108554365 A CN108554365 A CN 108554365A CN 201810255375 A CN201810255375 A CN 201810255375A CN 108554365 A CN108554365 A CN 108554365A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic 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
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- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a kind of uranium absorption agent and preparation method thereof, the preparation method of the uranium absorption agent includes the following steps：(1) the dry red mud to constant weight is dispersed in water, obtains solid-liquid system, the solid-to-liquid ratio of the red mud and water is 1~20g/L；(2) solid-liquid system obtained to step (1) is stirred to pH stable, and acidic oxidation agent is then added dropwise, until the pH value of solid-liquid system is 1~6；(3) solid-liquid system that step (2) obtains is sealed, and is aged under room temperature, then filtered, retain filter residue；(4) filter residue for obtaining step (3) at 35~120 DEG C is dried, and obtains the uranium absorption agent.The present invention is using cheap nitric acid, ferric nitrate or aluminum nitrate as acidic oxidation agent, Bayer process red mud is aoxidized, impregnate and dealkalize it is series modified, preparation process is simple and fast, manufacturing cost is low, the adsorbent large specific surface area of gained, with excellent uranyl ion absorption property, maximal absorptive capacity can reach 34.69mg/g~84.48mg/g.
Description
Technical field
The present invention relates to acid uranium-containing waste water process field more particularly to a kind of uranium suctions for handling acid uranium-containing waste water
Attached dose and preparation method thereof.
Background technology
With the rise of nuclear energy, the extensive development of nuclear power station, uranium is as a kind of important nuclear fuel, in energy industry
In occupation of increasingly consequence.However, will produce a large amount of acid uranium-bearing radiation in uranium mining and nucleic extractive process
Property waste water.In acid condition, the radioactive element in mine tailings and other harmful substances are easily dissolved release, and with waste water
Discharge migration.If by untreated uranium-containing waste water direct emission, water resource for the survival of mankind and soil can be caused
Serious pollution, destroys ecological environment, seriously endangers human health.If showing human body contact, sucking or food accidentally according to correlative study
Enter uranium and its compounds, can damage or destroy tissue and organ, alopecia, skin disease, hematologic disease and cancer etc. can be caused
A series of diseases.It is generated in the energy causing death when human body excess intake uranium, such as the processing of careless short-time contact nuclear fuel
High-level radioactive liquid waste, human body will be dead by serious radiation injury.Therefore, to the processing of uranium-bearing radioactive wastewater
And control, develop the real needs that uranium-containing waste water purification techniques is very urgent.
Uranium in an acidic solution, exists generally in the form of the uranyl ion of positive sexavalence.Absorption method is processing radioactive wastewater
One of effective means, it is the key that effectively to be adsorbed and removed uranyl ion to develop efficient, reliable radionuclide adsorbent.It is red
Mud has particle tiny and the porous physical property of short texture.Red mud by Multimetal oxide (such as iron oxide, aluminium oxide,
Silica, ferrous oxide, manganese oxide etc.) it cementing forms.Wherein, iron oxide and alumina component is often considered and radionuclide
There is good binding performance.The excellent reactivity worth of these oxides is the basis that red mud is applied as superior adsorbent, displaying
Potential of the red mud in terms of Spent Radioactive Water warfare.The mud adsorbent of prior art preparation is often neutral or alkalinity, by it
Applied to that solution will be caused to cross alkali in uranium-containing waste water processing, causes uranyl ion that hydrolytic precipitation or desorption occurs, be unfavorable for uranyl
The absorption and enrichment of ion.And existing metal ion itself can be precipitated in acidic environment in the adsorbent of meta-alkalescence, cause
The restraining function of coexisting ion inhibits adsorption effect of the adsorbent to uranium, and easily causes secondary pollution.Publication No.
A kind of " lanthanum changed red mud removes the preparation method of chromium adsorbent " of CN106622109A, lanthanum changed red mud is used except chromium adsorbent
It is prepared after lanthana and red mud stirring and drying, grinding, calcining, sieving, 17.35mg/ is reached to the adsorbance of cadmium wastewater
G, lanthana used in the technology are rare earth oxide, expensive and have trace-level activity, are not suitable for promoting and applying.It is open
Number be CN101898128A " preparation of aluminum modified red mud defluorinating absorbent and application process " and Publication No. CN101176840
" application process of iron modified red mud arsenic-removing adsorption agent " red mud is modified using aluminium chloride, iron chloride respectively, gained
The adsorbance of mud adsorbent is small and application conditions are limited.Therefore, to develop a kind of manufacturing cost using red mud cheap and to uranium
The good adsorbent of acyl ionic adsorption effect is the hot spot studied now.
Invention content
It is an object of the invention to solve above-mentioned shortcoming and defect of the existing technology, provide a kind of for handling acidity
Uranium absorption agent of uranium-containing waste water and preparation method thereof.The present invention is using cheap nitric acid, ferric nitrate or aluminum nitrate as acidity
Oxidant, Bayer process red mud is aoxidized, impregnate and dealkalize it is series modified, preparation process is simple and fast, and manufacturing cost is low,
There is the adsorbent large specific surface area of gained excellent uranyl ion absorption property, maximal absorptive capacity can reach 34.69mg/g
~84.48mg/g.
To solve its technical problem, the technical solution adopted in the present invention is：A kind of preparation method of uranium absorption agent, including
Following steps：
(1) the dry red mud to constant weight is dispersed in water, obtains solid-liquid system, the solid-to-liquid ratio of the red mud and water is 1
~20g/L；
(2) the solid-liquid system obtained to step (1) is stirred to pH stable, and acidic oxidation agent is then added dropwise,
PH value to solid-liquid system is 1~6；
(3) the solid-liquid system that step (2) obtains is sealed, and is aged under room temperature, then filtered, retain filter residue；
(4) filter residue for obtaining step (3) at 35~120 DEG C is dried, and obtains the uranium absorption agent.
Uranium absorption agent made from preparation method of the present invention be acidity, and prepare uranium absorption agent during solid-liquid system most
The pH value that whole pH value refines the acid uranium-bearing radioactive wastewater generated with uranium mining or nucleic is close.In application process, uranium
The amount of precipitation for the metal ion that red mud itself contains in adsorbent is effectively controlled, and effectively reduces coexisting ion to uranium absorption
The inhibiting effect of agent absorption property.Meanwhile adding for uranium absorption agent of the present invention will not cause uranyl ion in acid uranium-containing waste water
Hydrolytic precipitation or desorption are conducive to adsorb and be enriched with uranyl ion.
The preferred embodiment of preparation method as uranium absorption agent of the present invention, the acidic oxidation agent are nitric acid, nitric acid
Iron or aluminum nitrate.It is highly preferred that the acidic oxidation agent is ferric nitrate.In acid condition, the acidic oxidation agent has one
Fixed oxidizing property can effectively remove the organic composition in red mud, increase the degree of crushing of red mud particle, and exposure red mud has
Oxide component is imitated, so that the surface of uranium absorption agent obtained is formed flakes nano particle, effectively increases uranium absorption agent
Specific surface area and reaction site.
The preferred embodiment of preparation method as uranium absorption agent of the present invention, the red mud are Bayer process red mud.Bayer
Method is established according to the higher gibbsite Smelting Characteristics of grade, and 90% or more aluminum ore smelting process of the whole world is all using visiing at present
Ear method produces.Sintering process and joint rule are for middle-low grade aluminum ore and the smelting process developed.With red mud from sintering process and
Combination method red mud is compared, and Bayer process red mud is because its mineral has the characteristics that high ferro high-aluminum low-silicon, so show higher activity
Oxide content, so having better sorption potential and broader application prospect.
The preferred embodiment of preparation method as uranium absorption agent of the present invention, the solid-liquid system that the step (3) obtains
PH value be 2~5；It is highly preferred that the pH value for the solid-liquid system that the step (3) obtains is 2.5~3.5；Most preferably, institute
The pH value for stating the solid-liquid system that step (3) obtains is 3.The present inventor by obtained by a large amount of creative experiments, when it is described it is solid-
When the pH value of liquid system is 3, on the one hand it is more conducive to reduce the modification cost of this preparation method, is on the other hand more conducive to uranium absorption agent
Absorption to Uranium in Waste Water acyl ion improves the reaction efficiency of adsorbent and adsorbate.
The preferred embodiment of preparation method as uranium absorption agent of the present invention, red mud and water consolidates in the step (1)
Liquor ratio is 5~15g/L；It is highly preferred that the solid-to-liquid ratio of red mud and water is 9~11g/L in the step (1)；Most preferably, described
The solid-to-liquid ratio of red mud and water is 10g/L in step (1).The present inventor is by a large amount of creative experiments gained, when the red mud
When solid-to-liquid ratio with water is 10g/L, more conducively effectively red mud particle is homogeneously dispersed in water, forms uniform muddy water
Solid-liquid system.
The preferred embodiment of preparation method as uranium absorption agent of the present invention, acidic oxidation agent in the step (3)
A concentration of 0.1~3mol/L；Preferably, in the step (3) acidic oxidation agent a concentration of 0.2~2mol/L；It is highly preferred that
A concentration of 0.5~1.5mol/L of acidic oxidation agent in the step (3)；Most preferably, acidic oxidation agent in the step (3)
A concentration of 1mol/L.The present inventor is by a large amount of creative experiments gained, as a concentration of 1mol/ of the acidic oxidation agent
When L, more conducively quickly, pH that is easy and accurately adjusting the solid-liquid system that solid-to-liquid ratio is 10g/L.
The time of the preferred embodiment of preparation method as uranium absorption agent of the present invention, step (4) ageing is 3
It.
The temperature of the preferred embodiment of preparation method as uranium absorption agent of the present invention, step (5) drying is 55
~100 DEG C；It is highly preferred that the temperature of step (5) drying is 75~90 DEG C；Most preferably, the temperature of step (5) drying
Degree is 85 DEG C.The present inventor is by obtained by a large amount of creative experiments, when the temperature of the drying is 85 DEG C, more conducively shortening
The present invention prepares uranium absorption agent in the process to the modification duration of red mud, and uranium absorption agent obtained is made to keep good physical
Matter.
The present invention also provides a kind of uranium absorption agent, are made by the preparation method of uranium absorption agent of the present invention.The uranium
Adsorbent is applied to acid uranium-containing waste water process field, and the acid uranium-bearing generated is refined particularly for purification uranium mining and nucleic
Radioactive wastewater.
Compared with prior art, beneficial effects of the present invention are：
The uranium absorption agent of the present invention is acidity, when being applied to acid uranium-containing waste water processing, metal present in uranium absorption agent
The precipitation of ion is effectively controlled, and effectively reduces inhibiting effect of the coexisting ion to uranium absorption agent absorption property.Meanwhile this
The agent of invention uranium absorption will not cause uranyl ion hydrolytic precipitation or desorption in acid uranium-containing waste water, be conducive to adsorb and enrichment uranyl from
Son.The surface of uranium absorption agent of the present invention forms flakes nano particle, has high-specific surface area and excellent uranium absorption performance, right
The maximal absorptive capacity of uranyl ion can reach 34.69mg/g~84.48mg/g, have in radioactive pollution prevention and control field wide
Application prospect.
The uranium absorption agent of the present invention can be used for the Tl in water removal3+And Th4+Equal radionuclides, Cr6+And Cd2+Deng weight
The dyestuffs such as metal ion and Congo red and methyl blue.
The present invention prepares the simple for process, quick of uranium absorption agent, to equipment and process conditions without rigors, is easy behaviour
Make, favorable reproducibility.It is abundant and cheap to prepare the raw material resources such as acidic oxidation agent used and Bayer process red mud, effectively drops
The low manufacturing cost of uranium absorption agent, is suitble to produce in enormous quantities and application.The present invention solves red mud and uranium-bearing waste material simultaneously
Emission pollution problem and problem of resource waste are dexterously modified red mud using acidic oxidation agent, are constructed to purification uranium-bearing
The uranium absorption agent of waste material, realizes the treatment of wastes with processes of wastes against one another and the recycling of resource, environmental protection and economy.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure of the present invention by uranium absorption agent made from acidic oxidation agent of ferric nitrate；
Fig. 2 is scanning electron microscope (SEM) figure of the present invention by uranium absorption agent made from acidic oxidation agent of aluminum nitrate；
Fig. 3 is scanning electron microscope (SEM) figure of the present invention by uranium absorption agent made from acidic oxidation agent of nitric acid；
Fig. 4 is the process flow diagram of the preparation method of uranium absorption agent of the present invention；
Fig. 5 is the fractions distribution figure of uranyl ion in water；
Fig. 6 is the testing result of the embodiment of the present invention 12.
Specific implementation mode
Embodiment 1
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 1g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) ferric nitrate of a concentration of 0.1mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid body
The pH value of system is 1；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
35℃。
Embodiment 2
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 10g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) ferric nitrate of a concentration of 1mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid system
PH value be 3；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
85℃。
Embodiment 3
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 20g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) ferric nitrate of a concentration of 3mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid system
PH value be 6；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
120℃。
Embodiment 4
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 1g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) aluminum nitrate of a concentration of 0.1mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid body
The pH value of system is 1；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
35℃。
Embodiment 5
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 10g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) aluminum nitrate of a concentration of 1mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid system
PH value be 3；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
85℃。
Embodiment 6
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 20g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) aluminum nitrate of a concentration of 3mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid system
PH value be 6；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
120℃。
Embodiment 7
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 1g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) nitric acid of a concentration of 0.1mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid system
PH value be 1；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
35℃。
Embodiment 8
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 10g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) nitric acid of a concentration of 1mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid system
PH value is 3；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
85℃。
Embodiment 9
A kind of preparation method of uranium absorption agent, includes the following steps：
(1) water is poured into beaker, is subsequently poured into the dry Bayer process red mud to constant weight, it is made to be dispersed in water, consolidate-
Liquid system；The solid-to-liquid ratio of Bayer process red mud and water is 20g/L；
(2) the solid-liquid system obtained with magnetic stirrer step (1) is to pH stable, the rotating speed of magnetic stirring apparatus
For 200rpm/min；
(3) nitric acid of a concentration of 3mol/L is added dropwise in the solid-liquid system obtained to step (2), until solid-liquid system
PH value is 6；
(4) it is sealed with the solid-liquid system for obtaining step (3) with tinfoil sealed beaker mouth, 3 is aged under room temperature
It, then filters, and retains filter residue；
(5) filter residue for being obtained step (4) with vacuum drying chamber is dried to get the uranium absorption agent；The temperature of drying is
120℃。
Embodiment 10
Using uranium absorption agent made from embodiment 2, embodiment 5 and embodiment 8 as sample, uranium absorption performance is measured respectively.
Configuration concentration gradient be 5,10,20,40,80mg/L, initial pH=3 contain uranium solution, by 3g/L samples addition contain
In uranium solution, 30min is shaken with the rotating speed of 150rpm/min at 35 DEG C, acquired results use Langmuir (Lang Gemiaoer) heat
Mechanical equation formula carries out curve fitting to it.Gained fitting result is as follows：
The thermodynamics fitting maximum adsorption capacity of 2 uranium absorption agent of embodiment reaches 84.48mg/g, and the rate of adsorption is
0.0045L/mg, related coefficient is up to 0.99；
The thermodynamics fitting maximum adsorption capacity of 5 uranium absorption agent of embodiment reaches 34.69mg/g, and the rate of adsorption is
0.014L/mg, related coefficient is up to 0.91；
The thermodynamics fitting maximum adsorption capacity of 8 uranium absorption agent of embodiment reaches 44.45mg/g, and the rate of adsorption is
0.012L/mg, related coefficient is up to 0.93.
Interpretation of result：Under the premise of being tested according to the fitting of above-mentioned Lang Gemiaoer thermodynamics it is found that other preparation conditions are identical, use
It is latent that three kinds of uranium absorption agent made from ferric nitrate, aluminum nitrate or Nitric Acid Modified red mud show uranium different maximum adsorptions respectively
The maximum adsorption capacity value of power, wherein 2 uranium absorption agent of embodiment is maximum, illustrates the uranium absorption agent made from Ferric nitrate modified red mud
With superior uranium absorption performance.
Embodiment 11
According to Fig. 5 (the existing forms distribution map of uranyl ion in water) it is found that after the pH ＞ 3.5 of water, uranyl in water
The concentration of ion falls sharply, it follows that the suitable existence condition of uranyl ion is pH ＜ 3.5, is conducive to adsorb and be enriched with water at this time
In uranyl ion.
Influence for detection architecture pH to absorption uranyl ion, the present embodiment are more of the invention using pH=3.5 as separation
In the preparation method of uranium absorption agent, solid-liquid system is added dropwise after acidic oxidation agent (hereinafter referred to as " modified solid-liquid system "), pH
When ＞ 3.5 and pH ＜ 3.5, the uranium absorption performance of uranium absorption agent obtained.
Experiments verify that uranium absorption agent obtained and the pH ＜ 3 for being modified solid-liquid system when the pH=3 of modified solid-liquid system
When uranium absorption agent obtained absorption property it is close, and while being modified the pH=3 of solid-liquid system, prepares the modification cost of uranium absorption agent
Relatively low, therefore, most preferably scheme of the invention is that the pH value for being modified solid-liquid system is adjusted to 3.
The present embodiment is using uranium absorption agent made from embodiment 2, embodiment 5 and embodiment 8 as modified solid-liquid system pH ＜
Representative when 3.5.Simultaneously using uranium absorption agent made from comparative example 1, comparative example 2 and comparative example 3 as modified solid-liquid system pH ＞
Representative when 3.5.Its uranium absorption performance is detected respectively.
Comparative example 1：Uranium absorption agent is prepared according to the method for embodiment 2, but the pH value of modified solid-liquid system is adjusted to 5,
Remaining condition is constant.
Comparative example 2：Uranium absorption agent is prepared according to the method for embodiment 5, but the pH value of modified solid-liquid system is adjusted to 5,
Remaining condition is constant.
Comparative example 3：Uranium absorption agent is prepared according to the method for embodiment 8, but the pH value of modified solid-liquid system is adjusted to 5,
Remaining condition is constant.
Detection method：Configuration concentration gradient be 5,10,20,40,80mg/L, initial pH=3 contain uranium solution, by 3g/L's
It detects sample to be added containing in uranium solution, 30min is shaken with the rotating speed of 150rpm/min at 35 DEG C.Testing result is as shown in table 1：
Table 1
As can be known from the results of Table 1, the adsorbent prepared as the pH ＞ 3.5 of modified solid-liquid system and modified solid-liquid system
PH ＜ 3.5 when the adsorbent for preparing when comparing, the former adsorption capacity significantly reduces.The experimental results showed that pH ＜ 3.5 change
Property system under changed red mud adsorb uranyl ion, it is preferable to the adsorption effect of uranyl ion, as pH=3, exist for uranyl ion
Modified adsorbent pH is set as 3 by most suitable existence condition, the present invention in water, is had more excellent absorption property to uranium and optimal is modified to
This.
Embodiment 12
Bayer process red mud to be modified without acidic oxidation agent is made with embodiment 2, embodiment 5 and embodiment 8 as a contrast
The uranium absorption agent obtained compares, and detects its uranium absorption performance, the performance improvement effect of red mud after comparison before modified.Detection method is joined
According to the detection method in embodiment 11, testing result is as shown in Figure 6.
It will be appreciated from fig. 6 that using the adsorption capacity amplification of Ferric nitrate modified red mud up to 33.29%~122.31%, use nitre
The adsorption capacity amplification of sour aluminum modified red mud uses the adsorption capacity of Nitric Acid Modified red mud to increase up to 17.13%~122.72%
Width is up to 29.64%~152.66%.It can be seen that the three classes acidic oxidation agent of the present invention is good to the modification power of red mud, work as uranium-bearing
When solution concentration relatively low (being less than 20mg/L), each oxidant modification power difference is less；It is 20mg/ when uranium-bearing solution concentration increases
When L~50mg/L, Ferric nitrate modified red mud shows its more preferably modification power；When uranium-bearing solution concentration range 50mg/L~
80mg/L, Nitric Acid Modified red mud show its more preferably modification power.
The adsorption capacity for comparing unmodified Bayer process red mud is adsorbed through the modified adsorbent of acidic oxidation agent of the present invention
Capacity amplification reaches 60% or more, and wherein ferric nitrate and Nitric Acid Modified red mud is being 20mg/L~80mg/L time-divisions containing uranium solution
Its more preferably modification power is not shown.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention
The limitation of range is protected, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art should
Understand, technical scheme of the present invention can be modified or replaced equivalently, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of preparation method of uranium absorption agent, which is characterized in that include the following steps：
(1) the dry red mud to constant weight being dispersed in water, obtains solid-liquid system, the solid-to-liquid ratio of the red mud and water is 1~
20g/L；
(2) the solid-liquid system obtained to step (1) is stirred to pH stable, and acidic oxidation agent is then added dropwise, until
The pH value of solid-liquid system is 1~6；
(3) the solid-liquid system that step (2) obtains is sealed, and is aged under room temperature, then filtered, retain filter residue；
(4) filter residue for obtaining step (3) at 35~120 DEG C is dried, and obtains the uranium absorption agent.
2. the preparation method of uranium absorption agent as described in claim 1, which is characterized in that the acidic oxidation agent is nitric acid, nitre
Sour iron or aluminum nitrate.
3. the preparation method of uranium absorption agent as described in claim 1, which is characterized in that the red mud is Bayer process red mud.
4. the preparation method of uranium absorption agent as described in claim 1, which is characterized in that the solid-liquid body that the step (3) obtains
The pH value of system is 2~5；It is highly preferred that the pH value for the solid-liquid system that the step (3) obtains is 2.5~3.5；Most preferably,
The pH value for the solid-liquid system that the step (3) obtains is 3.
5. such as the preparation method of Claims 1 to 4 any one of them uranium absorption agent, which is characterized in that red in the step (1)
The solid-to-liquid ratio of mud and water is 5~15g/L；It is highly preferred that the solid-to-liquid ratio of red mud and water is 9~11g/L in the step (1)；Most
Preferably, the solid-to-liquid ratio of red mud and water is 10g/L in the step (1).
6. the preparation method of uranium absorption agent as claimed in claim 5, which is characterized in that acidic oxidation agent in the step (3)
A concentration of 0.1~3mol/L；Preferably, in the step (3) acidic oxidation agent a concentration of 0.2~2mol/L；More preferably
Ground, a concentration of 0.5~1.5mol/L of acidic oxidation agent in the step (3)；Most preferably, acid oxygen in the step (3)
A concentration of 1mol/L of agent.
7. the preparation method of uranium absorption agent as described in claim 1, which is characterized in that the time of step (4) ageing is 3
It.
8. the preparation method of uranium absorption agent as described in claim 1, which is characterized in that the temperature of the step (5) drying is
55~100 DEG C；It is highly preferred that the temperature of step (5) drying is 75~90 DEG C；Most preferably, the step (5) dries
Temperature is 85 DEG C.
9. a kind of uranium absorption agent, which is characterized in that be made by claim 1~8 any one of them preparation method.
10. uranium absorption agent as claimed in claim 9 is in the application of acid uranium-containing waste water process field.
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| CN109926032A (en) * | 2019-04-11 | 2019-06-25 | 广州大学 | A kind of uranium absorption agent and preparation method thereof based on hydroxyapatite |
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