CN106710659B - A kind of method using silicon dioxide composite material absorption Uranium in Waste Water acyl - Google Patents

A kind of method using silicon dioxide composite material absorption Uranium in Waste Water acyl Download PDF

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CN106710659B
CN106710659B CN201710021145.3A CN201710021145A CN106710659B CN 106710659 B CN106710659 B CN 106710659B CN 201710021145 A CN201710021145 A CN 201710021145A CN 106710659 B CN106710659 B CN 106710659B
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waste water
composite material
silicon dioxide
dioxide composite
acyl
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CN106710659A (en
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李风浪
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Jiangxi Chenghong Industrial Co., Ltd.
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04Treating liquids
    • G21F9/06Processing
    • G21F9/12Processing by absorption; by adsorption; by ion-exchange

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  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
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Abstract

The invention discloses a kind of method using silicon dioxide composite material absorption Uranium in Waste Water acyl, comprises the following steps (1) and carries out the processing of normal pressure microplasma discharge using earth silicon material so as to prepare adsorbent;(2) it is 4 6.8 to adjust the waste water containing uranyl to pH, is added an adsorbent into wherein, 36 48h of stirring and adsorbing, and after filtering, filtrate centrifugal treating is further separated to the solid in waste water, collects solid particle.This method is easy to operate, and adsorption efficiency is high, good waste water treatment effect;And adsorption effect can be monitored in real time, there is good industrialization practical prospect.

Description

A kind of method using silicon dioxide composite material absorption Uranium in Waste Water acyl
Technical field
The present invention relates to field of waste water treatment, and silicon dioxide composite material absorption Uranium in Waste Water is utilized more particularly to one kind The method of acyl.
Background technology
Uranium is a kind of natural radioactive element, and important nuclear power source fuel, has very strong radiotoxicity.With core Can it is growing, uranium-containing waste water is more and more, these waste water such as deal with improperly directly discharge the health of the mankind can be produced Raw greatly harm.Uranium is extracted from the waste water of uranium-bearing can be effectively reduced the pollution of uranium, can also improve the profit of uranium resource With rate.So from the angle of environmental protection and the double angle of raising uranium utilization rate, the uranium extraction in waste water is separated simultaneously It is used with great practical value.
The processing method of more common processing uranium-containing waste water is chemical precipitation method, ion-exchange, evaporation and concentration at present Method and absorption method.Wherein chemical precipitation method has the advantages that treatment process is simple, cost is low, but there is aqueous concentration easily not The shortcomings that up to standard;The advantages of ion-exchange has that removing coefficient is high, and comprehensive removal effect is good, but processing procedure cost compared with It is high;Evaporation concentration method equally has the shortcomings that of high cost.Absorption method processing uranium-bearing sewage is simple with technique, and removal efficiency is high Advantage, selects the key that suitable adsorbent is whole adsorption process.The clay pit species such as attapulgite, montmorillonite, montmorillonite It is the composite material such as common sorbing material, resin, chitosan, carbon material that material, which has loose structure and larger specific surface area, Different functional groups can be introduced in the composite by design, the effective choosing for improving adsorbent to some specific ions Selecting property, so as to improve the adsorption efficiency of material.
The method that Chinese patent CN201410657254.0 discloses uranyl ion in a kind of high efficiency extraction water, it is included such as Lower step:Uranyl ion is adsorbed in advance on sorbing material surface;The sorbing material for being adsorbed with uranyl ion in advance input is contained In the waste water of uranyl ion, after stirring, filtered, collect filter residue.The invention is simple with method, easy to operate under room temperature, no Other impurity and environmentally protective are introduced, the advantages that economical and effective;But adsorption rate need to be improved.
The content of the invention
The object of the present invention is to provide a kind of method using silicon dioxide composite material absorption Uranium in Waste Water acyl, this method Easy to operate, adsorption efficiency is high, good waste water treatment effect;And adsorption effect can be monitored in real time, there is good industrialization reality Use prospect.
To achieve the above object, the present invention uses following technical scheme:
A kind of method using silicon dioxide composite material absorption Uranium in Waste Water acyl, comprises the following steps:
(1) earth silicon material is distributed in the mixed solution of ethamine and oxalic acid, adds dispersant, add ultrasonic disperse 1-2h, is made suspension, suspension is placed in reactor, carries out normal pressure microplasma discharge processing, adjusts output current For 11-15mA, output voltage 2500V-3000V, 30min is reacted, after reaction, filters and by solid particle centrifuge clearly Wash repeatedly, then with after washes of absolute alcohol 3 times, vacuumize drying, prepare adsorbent;
(2) it is 4-6.8 to adjust the waste water containing uranyl to pH, is added an adsorbent into wherein, stirring and adsorbing 36-48h, filtering Afterwards, filtrate centrifugal treating is further separated to the solid in waste water, collects solid particle.
Preferably, the earth silicon material is ordered mesoporous silicon-dioxide material.
Preferably, the earth silicon material is SBA-15 types, MCM-41 types or MSU-H type ordered mesoporous silica dioxide materials One or more mixtures in material.
Preferably, concentration of the earth silicon material in mixed solution is 3-8g/L.
Preferably, the molar ratio of the ethamine and oxalic acid is 1:(2-5), concentration of the ethamine in mixed solution are 40- 70g/L。
Preferably, the dispersant is lauryl sodium sulfate, methyl anyl alcohol, polyacrylamide or fatty acid polyglycol ethylene glycol One or more mixtures in ester.
Preferably, the mass ratio of the dispersant and earth silicon material is (1-2):10.
Preferably, the amount ratio of adsorbent and waste water is 0.6-1g/L in the adsorption process.
Wherein, in normal pressure microplasma discharge processing operation, air-flow selection argon stream, gas velocity 60-90mL/ Min, anode use tunger tube, and cathode uses platinum electrode.
The invention has the advantages that by the way of carbon dots modifies earth silicon material, composite material is added While to the adsorption effect of uranyl, the fluorescence property of carbon dots can be utilized so that earth silicon material adsorbs the process of uranyl Visualization, can preferably control adsorption process and have more intuitive research to its adsorption dynamics adsorption kinetics.The preparation of adsorbent During prepared using normal pressure microplasma auxiliary one-step method and have the silicon dioxide composite material of carbon dots, this method operation letter It is single, it is swift in response, energy consumption is low, is easy to mass produce.The adsorbent uranyl ion, is easier to be eluted, so that Be conducive to the recycling of uranyl, effectively raise the service efficiency of uranium.
Embodiment
In order to be better understood from 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 formed to the present invention.
Embodiment 1
(1) 100mgSBA-15 type ordered mesoporous silicon-dioxide materials are distributed to the mixed solution of 13mL ethamine and oxalic acid In, 10mg lauryl sodium sulfate is added, adds ultrasonic disperse 1h, suspension is made, suspension is placed in reactor, is carried out The processing of normal pressure microplasma discharge, adjusting output current are 11mA, output voltage 2500V, react 30min, reaction terminates Afterwards, filter that solid particle carried out eccentric cleaning is multiple, then with drying after washes of absolute alcohol 3 times, is vacuumized, prepare absorption Agent;
(2) it is 4 to adjust waste water of the 100mL containing uranyl to pH, by 60mg adsorbents input wherein, stirring and adsorbing 36h, mistake After filter, filtrate centrifugal treating is further separated to the solid in waste water, collects solid particle.
Wherein the molar ratio of ethamine and oxalic acid is 1:2, concentration of the ethamine in mixed solution is 40g/L.The micro- grade of normal pressure from In the operation of daughter discharge treatment, air-flow selects argon stream, gas velocity 60mL/min, and anode uses tunger tube, and cathode is adopted Use platinum electrode.
In the adsorption process, the adsorption efficiency of uranyl is 60%.
Embodiment 2
(1) 100mgMCM-41 type ordered mesoporous silicon-dioxide materials are distributed to the mixed solution of 33mL ethamine and oxalic acid In, 20mg methyl anyl alcohols are added, add ultrasonic disperse 2h, suspension is made, suspension is placed in reactor, it is micro- to carry out normal pressure Plasma discharge processing, adjusting output current are 15mA, output voltage 3000V, react 30min, after reaction, filtering Solid particle progress eccentric cleaning is multiple, then with after washes of absolute alcohol 3 times, vacuumize drying, prepare adsorbent;
(2) it is 6.8 to adjust waste water of the 100mL containing uranyl to pH, by 100mg adsorbents input wherein, stirring and adsorbing Filtrate centrifugal treating, after filtering, is further separated the solid in waste water, collects solid particle by 48h.
Wherein the molar ratio of ethamine and oxalic acid is 1:5, concentration of the ethamine in mixed solution is 70g/L.The micro- grade of normal pressure from In the operation of daughter discharge treatment, air-flow selects argon stream, gas velocity 90mL/min, and anode uses tunger tube, and cathode is adopted Use platinum electrode.
In the adsorption process, the adsorption efficiency of uranyl is 72%.
Embodiment 3
(1) 100mg MSU-H type ordered mesoporous silicon-dioxide materials are distributed to the mixed solution of 13mL ethamine and oxalic acid In, 20mg polyacrylamides are added, add ultrasonic disperse 1h, suspension is made, suspension is placed in reactor, carry out normal pressure Microplasma discharge processing, adjusting output current are 15mA, output voltage 2500VV, react 30min, after reaction, Filtering is multiple by solid particle progress eccentric cleaning, then with after washes of absolute alcohol 3 times, vacuumizes drying, prepare adsorbent;
(2) it is 6.8 to adjust waste water of the 100mL containing uranyl to pH, by 60mg adsorbents input wherein, stirring and adsorbing 48h, After filtering, filtrate centrifugal treating is further separated to the solid in waste water, collects solid particle.
Wherein the molar ratio of ethamine and oxalic acid is 1:2, concentration of the ethamine in mixed solution is 70g/L.The micro- grade of normal pressure from In the operation of daughter discharge treatment, air-flow selects argon stream, gas velocity 60mL/min, and anode uses tunger tube, and cathode is adopted Use platinum electrode.
In the adsorption process, the adsorption efficiency of uranyl is 67%.
Embodiment 4
(1) 100mg MSU-H type ordered mesoporous silicon-dioxide materials are distributed to the mixed solution of 33mL ethamine and oxalic acid In, 10mg fatty acid polyethylene glycol esters are added, add ultrasonic disperse 2h, suspension is made, suspension is placed in reactor, into The processing of row normal pressure microplasma discharge, adjusting output current are 11mA, output voltage 3000V, react 30min, reaction knot Shu Hou, filters that solid particle carried out eccentric cleaning is multiple, then with drying after washes of absolute alcohol 3 times, is vacuumized, prepares absorption Agent;
(2) it is 4 to adjust waste water of the 100mL containing uranyl to pH, by 100mg adsorbents input wherein, stirring and adsorbing 36h, After filtering, filtrate centrifugal treating is further separated to the solid in waste water, collects solid particle.
Wherein the molar ratio of ethamine and oxalic acid is 1:5, concentration of the ethamine in mixed solution is 40g/L.The micro- grade of normal pressure from In the operation of daughter discharge treatment, air-flow selects argon stream, gas velocity 90mL/min, and anode uses tunger tube, and cathode is adopted Use platinum electrode.
In the adsorption process, the adsorption efficiency of uranyl is 78%.
Embodiment 5
(1) 100mgSBA-15 type ordered mesoporous silicon-dioxide materials are distributed to the mixed solution of 21mL ethamine and oxalic acid In, 15mg polyacrylamides are added, add ultrasonic disperse 2h, suspension is made, suspension is placed in reactor, carry out normal pressure Microplasma discharge processing, adjusting output current are 12mA, output voltage 2800V, react 30min, after reaction, mistake Filter is multiple by solid particle progress eccentric cleaning, then with after washes of absolute alcohol 3 times, vacuumizes drying, prepare adsorbent;
(2) it is 5 to adjust waste water of the 100mL containing uranyl to pH, by 80mg adsorbents input wherein, stirring and adsorbing 48h, mistake After filter, filtrate centrifugal treating is further separated to the solid in waste water, collects solid particle.
Wherein the molar ratio of ethamine and oxalic acid is 1:3, concentration of the ethamine in mixed solution is 60g/L.The micro- grade of normal pressure from In the operation of daughter discharge treatment, air-flow selects argon stream, gas velocity 72mL/min, and anode uses tunger tube, and cathode is adopted Use platinum electrode.
In the adsorption process, the adsorption efficiency of uranyl is 68%.
Embodiment 6
(1) 100mgMCM-41 type ordered mesoporous silicon-dioxide materials are distributed to the mixed solution of 29mL ethamine and oxalic acid In, 12mg methyl anyl alcohols are added, add ultrasonic disperse 1h, suspension is made, suspension is placed in reactor, it is micro- to carry out normal pressure Plasma discharge processing, adjusting output current are 12mA, output voltage 2900V, react 30min, after reaction, filtering Solid particle progress eccentric cleaning is multiple, then with after washes of absolute alcohol 3 times, vacuumize drying, prepare adsorbent;
(2) it is 6 to adjust waste water of the 100mL containing uranyl to pH, by 60-100mg adsorbents input wherein, stirring and adsorbing Filtrate centrifugal treating, after filtering, is further separated the solid in waste water, collects solid particle by 36h.
Wherein the molar ratio of ethamine and oxalic acid is 1:4, concentration of the ethamine in mixed solution is 60g/L.The micro- grade of normal pressure from In the operation of daughter discharge treatment, air-flow selects argon stream, gas velocity 80mL/min, and anode uses tunger tube, and cathode is adopted Use platinum electrode.
In the adsorption process, the adsorption efficiency of uranyl is 72%.

Claims (7)

  1. A kind of 1. method using silicon dioxide composite material absorption Uranium in Waste Water acyl, it is characterised in that:Comprise the following steps:
    (1) earth silicon material is distributed in the mixed solution of ethamine and oxalic acid, adds dispersant, add ultrasonic disperse 1- 2h, is made suspension, suspension is placed in reactor, carries out normal pressure microplasma discharge processing, adjusts output current and is 11-15mA, output voltage 2500V-3000V, react 30min, after reaction, filter solid particle carrying out eccentric cleaning Repeatedly, then with after washes of absolute alcohol 3 times, drying is vacuumized, prepares adsorbent;
    (2) it is 4-6.8 to adjust the waste water containing uranyl to pH, is added an adsorbent into wherein, stirring and adsorbing 36-48h, after filtering, Filtrate centrifugal treating is further separated to the solid in waste water, collects solid particle;
    The earth silicon material is ordered mesoporous silicon-dioxide material.
  2. 2. the method according to claim 1 using silicon dioxide composite material absorption Uranium in Waste Water acyl, it is characterised in that: The earth silicon material is one kind or more in SBA-15 types, MCM-41 types or MSU-H type ordered mesoporous silicon-dioxide materials Kind mixture.
  3. 3. the method according to claim 1 using silicon dioxide composite material absorption Uranium in Waste Water acyl, it is characterised in that: Concentration of the earth silicon material in mixed solution is 3-8g/L.
  4. 4. the method according to claim 1 using silicon dioxide composite material absorption Uranium in Waste Water acyl, it is characterised in that: The molar ratio of the ethamine and oxalic acid is 1:(2-5), concentration of the ethamine in mixed solution are 40-70g/L.
  5. 5. the method according to claim 1 using silicon dioxide composite material absorption Uranium in Waste Water acyl, it is characterised in that: The dispersant is one kind or more in lauryl sodium sulfate, methyl anyl alcohol, polyacrylamide or fatty acid polyethylene glycol ester Kind mixture.
  6. 6. the method according to claim 1 using silicon dioxide composite material absorption Uranium in Waste Water acyl, it is characterised in that: The mass ratio of the dispersant and earth silicon material is (1-2):10.
  7. 7. the method according to claim 1 using silicon dioxide composite material absorption Uranium in Waste Water acyl, it is characterised in that: The amount ratio of adsorbent and waste water is 0.6-1g/L in the adsorption process.
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CN107589098B (en) * 2017-08-30 2019-12-06 苏州大学 Method for fluorescence detection of trace uranyl ions
CN109727695B (en) * 2017-10-30 2023-01-24 中核四0四有限公司 Cleaning and recycling method for MOX powder contaminated by grinding balls
CN112967828B (en) * 2021-02-01 2022-09-30 南华大学 Uranium-bearing wastewater treatment device and uranium-bearing wastewater treatment method

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CN105139910A (en) * 2015-09-07 2015-12-09 南京理工大学 Application of porous orderly silicon dioxide foam material to processing of radionuclide uranium in waste water
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