CN106847357B - The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water - Google Patents
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water Download PDFInfo
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- CN106847357B CN106847357B CN201710075990.9A CN201710075990A CN106847357B CN 106847357 B CN106847357 B CN 106847357B CN 201710075990 A CN201710075990 A CN 201710075990A CN 106847357 B CN106847357 B CN 106847357B
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- G—PHYSICS
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- 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
- G21F9/10—Processing by flocculation
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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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Abstract
The invention discloses the methods of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, include the following steps：Basic treatment walnut shell powder first, then under certain conditions, the walnut shell powder of alkalization is handled with fulvic acid, hydroxyl in fulvic acid and the hydroxyl on walnut shell powder surface are reacted, it is modified walnut shell powder to which fulvic acid be made, its good dispersion in water, the uranium in waste water can more effectively be removed, on the other hand, carbon dots/meso-porous titanium dioxide silicon composite is made using one-step method in the present invention, and manufacturing cost is low, has very strong suction-operated to uranium, and fluorescence property is good, is conducive to except the monitoring during uranium.This method is easy to operate, at low cost, may be adapted to the scale processing of uranium-containing waste water.
Description
Technical field
The present invention relates to field of waste water treatment, are specifically related to coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-bearing
The method of waste water.
Background technology
The element that the atomic number of uranium (Uranium) is 92, the symbol of element is U, can be found most in nature
Heavy element.There are three kinds of isotopes in nature, carry radioactivity, possess very long half-life period (hundreds of millions of years~tens of
100000000 years).In addition there are 12 kinds of man-made isotopes (uranium -226~uranium -240).Uranium is in 1789 by Martin's Heinrich carat
General rood (Martin Heinrich Klaproth) finds.Uranium compound early stage is used for the coloring of porcelain, in nuclear fission phenomenon
Nuclear fuel is used as after being found.Its chemistry is active, can be with all nonmetallic effects (except inert gas), can be with a variety of gold
Category forms alloy.It is oxidizable in air, generate the oxidation film of one layer of obfuscation.Metallic uranium is slowly dissolved in sulfuric acid and phosphoric acid, there is oxidation
It can accelerate to dissolve in the presence of agent, uranium is soluble in nitric acid, and uranium is inert to alkaline solution, but in the presence of having oxidant, and uranium can be made molten
Solution.
Uranium is recycled from uranium-containing waste water has the double meaning of environmental protection and resource regeneration, recycles in waste water at present
The method of uranium mainly has chemical precipitation method, ion-exchange, evaporation concentration method, extraction and absorption method etc..Chemical precipitation method：Place
Manage simple for process, cost is relatively low, and treatment effect is preferable；But aqueous concentration is not often up to standard, must be for further processing；Precipitation production
Object needs after-treatment；In the presence of molten problem is returned, manipulation strength is larger.Ion-exchange：It is high to remove coefficient, comprehensive removal effect is good,
Discharge standard is can reach through processing；But this method cost is higher, when regeneration, generates waste water, can only handle nucleic into ionic state
, the waste water of non-alkaline.Evaporation concentration method：Method is simple, effective, reliable, and detersive efficiency is high；But its cost is higher, concentrates mud
Cured barrier is needed to handle.Extraction：Soil removal efficiency is high, but the waste water containing pollutant obtained after handling has higher radiation
Property.Absorption method：Simple for process, method is effective, and uranium removal rate is high.But currently used adsorbent additive amount is big, it is expensive,
When wastewater flow rate is big, it is not easy to be applicable in.
Chinese patent (201410246540.8) discloses a kind of magnetic mesoporous silica material of difunctional functionalization charcoal base
The preparation and application of material.It is specifically biological macropore template with saccharomyces cerevisiae, is mesoporous phase mould with triblock polymer P123
Plate prepares mesoporous SBA-15 using double-template method.Again using mesoporous SBA-15 as template, skill is poured using nanometer
Art be respectively filled in hard template different quality than source of iron and carbon source as predecessor, by home position polymerization reaction, prepare and close
At the orderly magnetic charcoal base mesopore silicon oxide of meso-hole structure, [3- (trimethoxy silane) propyl] three ethoxy of urea and aminopropyl is used
Base silane organic reagent is grafted after being carried out to the Si-OH on its surface and is modified, and absorption and complexation reaction dual function are made it have.It should
Invention material obtained can be used for uranium-containing waste water processing.But the material preparation is complicated, process is cumbersome, and at uranium-containing waste water
The monitoring of absorption situation is not easy to when reason.
Chinese patent (201410453596.0) discloses a kind of preparation method of mesoporous silicon fluorescent nano material.This method
Include the following steps：The carbon quantum dot of organosilan modification is made by high-temperature cracking method first；Then material ethyl orthosilicate
With the carbon dots after modification in the hydrolytie polycondensation of alkaline condition, one-step method obtains the order mesoporous organosilicon fluorescence nano material
Expect, material carbon quantum dot is entrained in mesoporous wall rather than in duct made from the invention；It conveys in traceable drug, is mostly logical
The fields such as road silver photo-biological imaging have broad application prospects.But organic solvent use is more in its preparation process, energy consumption is big,
There is certain pollution to environment.
Invention content
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of processing method of radioactivity uranium-containing waste water,
Using coagulant sedimentation and absorption method Combined Treatment, and process conditions are rationally controlled, uranium removal rate is high, to water body without secondary dirt
Dye, at low cost, monitoring that can effectively to uranium absorption processing procedure.
To achieve the above object, the present invention uses following technical scheme：
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, includes the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 30-50min, filtering, precipitation deionized water first
To neutrality, vacuum drying obtains modified walnut shell powder for washing, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene,
It is uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 120-150 DEG C 1-3h, is cooled to room temperature after reaction,
Filtering, precipitation is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, into solution
Mesoporous silicon oxide is added, ultrasound 15-35min under the power of 500W obtains stable dispersion liquid；Dispersion liquid is placed in reactor
In, atmospheric pressure plasma discharge processing is carried out, keeps electric current to stablize in processing procedure, after treatment centrifuges dispersion liquid, from
Gains in depth of comprehension to solid adopt and be washed with deionized 2-3 times, be dried in vacuo, obtain carbon dots/meso-porous titanium dioxide silicon composite；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and trichlorine is added
Change the mixture of iron, stir process 5-10min staticly settles 30-40min, filters, lime is added into filtered supernatant
Newborn clarified solution, the pH for adjusting waste water are 10-11, are filtered, supernatant is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/mesoporous two
Silica composite material filters after adsorption treatment, filtered water can direct emission, filtered precipitation desorbed with hydrochloric acid
Attached, the adsorbent after desorption re-uses.
As a preferred embodiment of the above technical solution, in step (1), the fulvic acid is modified walnut shell powder, to benzene methanesulfonic acid
Mass ratio is (2-7)：3：0.5.
As a preferred embodiment of the above technical solution, in step (2), a concentration of 2- of the dispersion liquid intermediary hole silica
8mg/ml。
As a preferred embodiment of the above technical solution, in step (2), the molar ratio of citric acid and ethylenediamine is 1：(0.3-11).
As a preferred embodiment of the above technical solution, in step (2), the gross mass and mesoporous silicon oxide of citric acid and ethylenediamine
Mass ratio be (30-100)：1.
As a preferred embodiment of the above technical solution, in step (2), when atmospheric pressure plasma jet treatment, the output current of electric discharge is
5-20mA, stable discharge duration are 10-40min.
As a preferred embodiment of the above technical solution, in step (3), the additive amount of the mixture of aluminum phosphate and ferric trichloride is
0.4-0.75g/L。
As a preferred embodiment of the above technical solution, the mass ratio of aluminum phosphate and ferric trichloride is 1:1.5.
As a preferred embodiment of the above technical solution, in step (4), the fulvic acid is modified walnut shell powder, carbon dots/mesoporous dioxy
The additive amount of SiClx composite material is respectively 0.33-0.45g/L, 0.15-0.2g/L.
After tested, the highest peak of fluorescence intensity of carbon dots/mesoporous silicon oxide produced by the present invention is in 360nm excitation waves
Under length, in 450nm or so, fluorescence property is good for peak position.
There are the functional groups such as carboxyl, hydroxyl in fulvic acid, it can be with the uranium in the formation and waste water of bidentate shape ligand
Very strong complexing occurs, forms stable complex compound, to effectively remove the uranium in waste water；
Walnut shell powder, it is cheap to be easy to get, have stable microcellular structure, adsorption capacity big；Fulvic acid is modified
The good dispersion of walnut shell powder in water not only may be implemented the absorption of Uranium in Waste Water, but also can form ligand with uranium, from
And precipitate, more effectively accelerate the removal speed of uranium.
Compared with prior art, the invention has the advantages that：
(1) present invention uses the method for coagulating sedimentation to pre-process uranium-containing waste water first；Using substep when pretreatment
Method is precipitated, and solves the problems, such as a large amount of body refuses containing radionuclide generated when one-step method coagulating kinetics, and
In coagulating sedimentation using the mixture of aluminum phosphate and ferric trichloride as precipitating reagent, which can be solidifying with the uranium in waste water
Be polymerized to tiny precipitable particle, and loose suede grain be combined into the suspended matter in water, reach it is preliminary remove the impurities in water that gives up,
The purpose of suspended matter and uranium；
(2) waste water after coagulating kinetics is handled using absorption method, is changed using homemade fulvic acid after adsorption treatment
Property walnut shell powder and carbon dots/meso-porous titanium dioxide silicon composite as adsorbent, fulvic acid is modified point of walnut shell powder in water
It is good to dissipate property, can be come into full contact with waste water, the uranium in waste water, carbon dots/Jie are removed by absorption and complexation reaction double action
Hole silicon dioxide composite material has good photoluminescent property, and adsorption capacity is big, and speed is fast, may be implemented to adsorbing uranyl ion
Visualization；
(3) uranium-containing waste water processing method provided by the invention, efficient, effect is good, at low cost, to water body and environment without two
Secondary pollution, and suitable for the extensive processing of uranium-containing waste water.
Specific implementation mode
In order to better understand the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, includes the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 30min, filtering first, precipitation is washed with deionized water
It washs to neutrality, vacuum drying obtains modified walnut shell powder, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene, stirred
It mixes uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 120 DEG C 1h, is cooled to room temperature after reaction, filters, and sinks
Shallow lake is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；Wherein, fulvic acid, modified walnut shell powder,
Mass ratio to benzene methanesulfonic acid is 2：3：0.5；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, into solution
Mesoporous silicon oxide is added, ultrasound 15min under the power of 500W obtains stable dispersion liquid；Dispersion liquid intermediary hole silica
A concentration of 2mg/ml；Dispersion liquid is placed in reactor, atmospheric pressure plasma discharge processing is carried out, electricity is kept in processing procedure
Stream is stablized, and after treatment centrifuges dispersion liquid, and the solid centrifuged, which is adopted, to be washed with deionized 2-3 times, and vacuum drying obtains
To carbon dots/meso-porous titanium dioxide silicon composite；Wherein, the molar ratio of citric acid and ethylenediamine is 1：0.3；Citric acid and ethylenediamine
Gross mass and mesoporous silicon oxide mass ratio be 30：1；When atmospheric pressure plasma jet treatment, the output current of electric discharge is 5mA,
The stable discharge duration is 40min；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and trichlorine is added
The additive amount of the mixture of the mixture of change iron, aluminum phosphate and ferric trichloride is 0.4g/L, and stir process 5min is staticly settled
Milk of lime clarified solution is added into filtered supernatant for 30min, filtering, and the pH for adjusting waste water is 10-11, filtering, supernatant
It is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/mesoporous two
Silica composite material filters after adsorption treatment, filtered water can direct emission, filtered precipitation desorbed with hydrochloric acid
Attached, the adsorbent after desorption re-uses；Wherein, fulvic acid is modified walnut shell powder, carbon dots/meso-porous titanium dioxide silicon composite
Additive amount be respectively 0.33g/L, 0.15g/L.
Embodiment 2
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, includes the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 50min, filtering first, precipitation is washed with deionized water
It washs to neutrality, vacuum drying obtains modified walnut shell powder, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene, stirred
It mixes uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 150 DEG C 3h, is cooled to room temperature after reaction, filters, and sinks
Shallow lake is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；Wherein, fulvic acid, modified walnut shell powder,
Mass ratio to benzene methanesulfonic acid is 2：3：0.5；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, into solution
Mesoporous silicon oxide is added, ultrasound 35min under the power of 500W obtains stable dispersion liquid；Dispersion liquid intermediary hole silica
A concentration of 8mg/ml；Dispersion liquid is placed in reactor, atmospheric pressure plasma discharge processing is carried out, electricity is kept in processing procedure
Stream is stablized, and after treatment centrifuges dispersion liquid, and the solid centrifuged, which is adopted, to be washed with deionized 2-3 times, and vacuum drying obtains
To carbon dots/meso-porous titanium dioxide silicon composite；Wherein, the molar ratio of citric acid and ethylenediamine is 1：11；Citric acid and ethylenediamine
Gross mass and mesoporous silicon oxide mass ratio be 100：1；When atmospheric pressure plasma jet treatment, the output current of electric discharge is
20mA, stable discharge duration are 10min；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and trichlorine is added
The additive amount of the mixture of the mixture of change iron, aluminum phosphate and ferric trichloride is 0.75g/L, and stir process 10min is staticly settled
Milk of lime clarified solution is added into filtered supernatant for 40min, filtering, and the pH for adjusting waste water is 10-11, filtering, supernatant
It is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/mesoporous two
Silica composite material filters after adsorption treatment, filtered water can direct emission, filtered precipitation desorbed with hydrochloric acid
Attached, the adsorbent after desorption re-uses；Wherein, fulvic acid is modified walnut shell powder, carbon dots/meso-porous titanium dioxide silicon composite
Additive amount be respectively 0.45g/L, 0.2g/L.
Embodiment 3
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, includes the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 35min, filtering first, precipitation is washed with deionized water
It washs to neutrality, vacuum drying obtains modified walnut shell powder, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene, stirred
It mixes uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 130 DEG C 1h, is cooled to room temperature after reaction, filters, and sinks
Shallow lake is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；Wherein, fulvic acid, modified walnut shell powder,
Mass ratio to benzene methanesulfonic acid is 3：3：0.5；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, into solution
Mesoporous silicon oxide is added, ultrasound 20min under the power of 500W obtains stable dispersion liquid；Dispersion liquid intermediary hole silica
A concentration of 3mg/ml；Dispersion liquid is placed in reactor, atmospheric pressure plasma discharge processing is carried out, electricity is kept in processing procedure
Stream is stablized, and after treatment centrifuges dispersion liquid, and the solid centrifuged, which is adopted, to be washed with deionized 2-3 times, and vacuum drying obtains
To carbon dots/meso-porous titanium dioxide silicon composite；Wherein, the molar ratio of citric acid and ethylenediamine is 1：2；Citric acid and ethylenediamine
The mass ratio of gross mass and mesoporous silicon oxide is 50：1；When atmospheric pressure plasma jet treatment, the output current of electric discharge is 10mA, is put
Electricity stablizes the duration as 40min；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and trichlorine is added
The additive amount of the mixture of the mixture of change iron, aluminum phosphate and ferric trichloride is 0.45g/L, and stir process 6min is staticly settled
Milk of lime clarified solution is added into filtered supernatant for 30min, filtering, and the pH for adjusting waste water is 10-11, filtering, supernatant
It is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/mesoporous two
Silica composite material filters after adsorption treatment, filtered water can direct emission, filtered precipitation desorbed with hydrochloric acid
Attached, the adsorbent after desorption re-uses；Wherein, fulvic acid is modified walnut shell powder, carbon dots/meso-porous titanium dioxide silicon composite
Additive amount be respectively 0.35g/L, 0.16g/L.
Embodiment 4
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, includes the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 40min, filtering first, precipitation is washed with deionized water
It washs to neutrality, vacuum drying obtains modified walnut shell powder, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene, stirred
It mixes uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 135 DEG C 1.5h, is cooled to room temperature after reaction, filtering,
Precipitation is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；Wherein, fulvic acid, modified walnut shell
Powder is 4 to the mass ratio of benzene methanesulfonic acid：3：0.5；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, into solution
Mesoporous silicon oxide is added, ultrasound 15min under the power of 500W obtains stable dispersion liquid；Dispersion liquid intermediary hole silica
A concentration of 4mg/ml；Dispersion liquid is placed in reactor, atmospheric pressure plasma discharge processing is carried out, electricity is kept in processing procedure
Stream is stablized, and after treatment centrifuges dispersion liquid, and the solid centrifuged, which is adopted, to be washed with deionized 2-3 times, and vacuum drying obtains
To carbon dots/meso-porous titanium dioxide silicon composite；Wherein, the molar ratio of citric acid and ethylenediamine is 1：4；Citric acid and ethylenediamine
The mass ratio of gross mass and mesoporous silicon oxide is 60：1；When atmospheric pressure plasma jet treatment, the output current of electric discharge is 10mA, is put
Electricity stablizes the duration as 30min；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and trichlorine is added
The additive amount of the mixture of the mixture of change iron, aluminum phosphate and ferric trichloride is 0.5g/L, and stir process 7min is staticly settled
Milk of lime clarified solution is added into filtered supernatant for 35min, filtering, and the pH for adjusting waste water is 10-11, filtering, supernatant
It is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/mesoporous two
Silica composite material filters after adsorption treatment, filtered water can direct emission, filtered precipitation desorbed with hydrochloric acid
Attached, the adsorbent after desorption re-uses；Wherein, fulvic acid is modified walnut shell powder, carbon dots/meso-porous titanium dioxide silicon composite
Additive amount be respectively 0.37g/L, 0.17g/L.
Embodiment 5
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, includes the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 45min, filtering first, precipitation is washed with deionized water
It washs to neutrality, vacuum drying obtains modified walnut shell powder, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene, stirred
It mixes uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 140 DEG C 1.5h, is cooled to room temperature after reaction, filtering,
Precipitation is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；Wherein, fulvic acid, modified walnut shell
Powder is 5 to the mass ratio of benzene methanesulfonic acid：3：0.5；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, into solution
Mesoporous silicon oxide is added, ultrasound 25min under the power of 500W obtains stable dispersion liquid；Dispersion liquid intermediary hole silica
A concentration of 5mg/ml；Dispersion liquid is placed in reactor, atmospheric pressure plasma discharge processing is carried out, electricity is kept in processing procedure
Stream is stablized, and after treatment centrifuges dispersion liquid, and the solid centrifuged, which is adopted, to be washed with deionized 2-3 times, and vacuum drying obtains
To carbon dots/meso-porous titanium dioxide silicon composite；Wherein, the molar ratio of citric acid and ethylenediamine is 1：8；Citric acid and ethylenediamine
The mass ratio of gross mass and mesoporous silicon oxide is 70：1；When atmospheric pressure plasma jet treatment, the output current of electric discharge is 45mA, is put
Electricity stablizes the duration as 20min；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and trichlorine is added
The additive amount of the mixture of the mixture of change iron, aluminum phosphate and ferric trichloride is 0.5g/L, and stir process 8min is staticly settled
Milk of lime clarified solution is added into filtered supernatant for 30min, filtering, and the pH for adjusting waste water is 10-11, filtering, supernatant
It is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/mesoporous two
Silica composite material filters after adsorption treatment, filtered water can direct emission, filtered precipitation desorbed with hydrochloric acid
Attached, the adsorbent after desorption re-uses；Wherein, fulvic acid is modified walnut shell powder, carbon dots/meso-porous titanium dioxide silicon composite
Additive amount be respectively 0.41g/L, 0.18g/L.
Embodiment 6
The method of coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, includes the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 45min, filtering first, precipitation is washed with deionized water
It washs to neutrality, vacuum drying obtains modified walnut shell powder, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene, stirred
It mixes uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 140 DEG C 2h, is cooled to room temperature after reaction, filters, and sinks
Shallow lake is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；Wherein, fulvic acid, modified walnut shell powder,
Mass ratio to benzene methanesulfonic acid is 6：3：0.5；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, into solution
Mesoporous silicon oxide is added, ultrasound 30min under the power of 500W obtains stable dispersion liquid；Dispersion liquid intermediary hole silica
A concentration of 7mg/ml；Dispersion liquid is placed in reactor, atmospheric pressure plasma discharge processing is carried out, electricity is kept in processing procedure
Stream is stablized, and after treatment centrifuges dispersion liquid, and the solid centrifuged, which is adopted, to be washed with deionized 2-3 times, and vacuum drying obtains
To carbon dots/meso-porous titanium dioxide silicon composite；Wherein, the molar ratio of citric acid and ethylenediamine is 1：9；Citric acid and ethylenediamine
The mass ratio of gross mass and mesoporous silicon oxide is 80：1；When atmospheric pressure plasma jet treatment, the output current of electric discharge is 10mA, is put
Electricity stablizes the duration as 10min；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and trichlorine is added
The additive amount of the mixture of the mixture of change iron, aluminum phosphate and ferric trichloride is 0.6g/L, and stir process 8min is staticly settled
Milk of lime clarified solution is added into filtered supernatant for 40min, filtering, and the pH for adjusting waste water is 10-11, filtering, supernatant
It is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/mesoporous two
Silica composite material filters after adsorption treatment, filtered water can direct emission, filtered precipitation desorbed with hydrochloric acid
Attached, the adsorbent after desorption re-uses；Wherein, fulvic acid is modified walnut shell powder, carbon dots/meso-porous titanium dioxide silicon composite
Additive amount be respectively 0.43g/L, 0.19g/L.
Comparative example 1
Adsorption treatment process is identical as embodiment, does not include the process of coagulating sedimentation.
Comparative example 2
Uranium-containing waste water is handled only with coagulating kinetics method, condition and embodiment 1 are identical.
Comparative example 3
Using coagulating kinetics method and adsorption treatment method Combined Treatment uranium-containing waste water, when adsorption treatment, only with
Fulvic acid is modified walnut shell powder as adsorbent, remaining condition and embodiment 1 are identical.
Comparative example 4
Using coagulating kinetics method and adsorption treatment method Combined Treatment uranium-containing waste water, when adsorption treatment, only with
For carbon dots/meso-porous titanium dioxide silicon composite as adsorbent, remaining condition and embodiment 1 are identical.
Comparative example 5
Using coagulating kinetics method and adsorption treatment method Combined Treatment uranium-containing waste water, when adsorption treatment, using Huang
Rotten acid is modified walnut shell powder and mesoporous silicon oxide as adsorbent, remaining condition is same as Example 1.
Comparative example 6
Using coagulating kinetics method and adsorption treatment method Combined Treatment uranium-containing waste water, when adsorption treatment, using Huang
Rotten acid is modified the mesoporous silicon oxide of walnut shell powder and atmospheric pressure plasma jet treatment as adsorbent, remaining condition and embodiment 1
It is identical.
A concentration of 200mg/L for the uranium-containing waste water that above-described embodiment and comparative example use, pH value 3.
The uranium of the different disposal method of above-mentioned uranium-containing waste water removing effect is detected below.
When detection, the clear solution 10ml that takes that treated, with the concentration of the Uranium in Waste Water after ICP-AES analyzing processings.
Test result is as shown in table 1
Table 1
| Uranium concentration in processed waste water, mg/L | |
| Comparative example 1 | 11.32 |
| Comparative example 2 | 30.50 |
| Comparative example 3 | 10.05 |
| Comparative example 4 | 7.11 |
| Comparative example 5 | 6.09 |
| Comparative example 6 | 5.87 |
| Embodiment 1 | 2.05 |
| Embodiment 2 | 1.98 |
| Embodiment 3 | 2.00 |
| Embodiment 4 | 1.93 |
| Embodiment 5 | 1.99 |
| Embodiment 6 | 1.99 |
From the point of view of above table data, using coagulant sedimentation and absorption method Combined Treatment uranium-containing waste water, and using self-control
Fulvic acid be modified walnut shell powder, carbon dots/mesoporous silicon oxide as Joint adsorption agent when, uranium treatment effect is best.
Claims (9)
1. the method for coagulant sedimentation-absorption method Combined Treatment radioactivity uranium-containing waste water, which is characterized in that include the following steps：
(1) 15% sodium hydroxide solution of walnut shell powder is handled into 30-50min, filtering first, precipitation is washed with deionized
To neutrality, vacuum drying obtains modified walnut shell powder, and fulvic acid, modified walnut shell powder are added sequentially in hexamethylene, stirred
It is uniformly mixed, and p-methyl benzenesulfonic acid is added, then flow back at 120-150 DEG C 1-3h, is cooled to room temperature after reaction, mistake
Filter, precipitation is washed with deionized to neutrality, dry, obtains fulvic acid and is modified walnut shell powder；
(2) ethylenediamine and deionized water are uniformly mixed, citric acid is added, continued stirring to solid and dissolve, be added into solution
Mesoporous silicon oxide, ultrasound 15-35min under the power of 500W, obtains stable dispersion liquid；Dispersion liquid is placed in reactor,
Atmospheric pressure plasma discharge processing is carried out, keeps electric current to stablize in processing procedure, dispersion liquid is centrifuged, centrifuged by after treatment
To solid adopt and be washed with deionized 2-3 times, be dried in vacuo, obtain carbon dots/meso-porous titanium dioxide silicon composite；
(3) lime is added in except the uranium-containing waste water in uranium pond, adjusts the pH to 4-5 of waste water, aluminum phosphate and ferric trichloride is added
Mixture, stir process 5-10min staticly settles 30-40min, filters, and it is clear that milk of lime is added into filtered supernatant
Clear liquid, the pH for adjusting waste water are 10-11, are filtered, supernatant is transferred in adsorption tank；
(4) fulvic acid obtained above is sequentially added in the waste water into adsorption tank is modified walnut shell powder, carbon dots/meso-porous titanium dioxide
Silicon composite filters after adsorption treatment, filtered water can direct emission, filtered precipitation carries out desorption with hydrochloric acid,
Adsorbent after desorption re-uses.
2. the method for coagulant sedimentation as described in claim 1-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：In step (1), the fulvic acid, modified walnut shell powder are (2-7) to the mass ratio of benzene methanesulfonic acid：3：0.5.
3. the method for coagulant sedimentation as described in claim 1-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：In step (2), a concentration of 2-8mg/ml of the dispersion liquid intermediary hole silica.
4. the method for coagulant sedimentation as described in claim 1-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：In step (2), the molar ratio of citric acid and ethylenediamine is 1：(0.3-11).
5. the method for coagulant sedimentation as described in claim 1-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：In step (2), the mass ratio of the gross mass and mesoporous silicon oxide of citric acid and ethylenediamine is (30-100)：1.
6. the method for coagulant sedimentation as described in claim 1-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：In step (2), when atmospheric pressure plasma jet treatment, the output current of electric discharge is 5-20mA, and the stable discharge duration is 10-
40min。
7. the method for coagulant sedimentation as described in claim 1-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：In step (3), the additive amount of the mixture of aluminum phosphate and ferric trichloride is 0.4-0.75g/L.
8. the method for coagulant sedimentation as claimed in claim 7-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：The mass ratio of aluminum phosphate and ferric trichloride is 1:1.5.
9. the method for coagulant sedimentation as described in claim 1-absorption method Combined Treatment radioactivity uranium-containing waste water, feature exist
In：In step (4), the fulvic acid is modified walnut shell powder, the additive amount of carbon dots/meso-porous titanium dioxide silicon composite is respectively
0.33-0.45g/L、0.15-0.2g/L。
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