CN106057263B - A kind of process for adsorbing palladium from high activity liquid waste - Google Patents
A kind of process for adsorbing palladium from high activity liquid waste Download PDFInfo
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- CN106057263B CN106057263B CN201610371028.5A CN201610371028A CN106057263B CN 106057263 B CN106057263 B CN 106057263B CN 201610371028 A CN201610371028 A CN 201610371028A CN 106057263 B CN106057263 B CN 106057263B
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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
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- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- C22B11/00—Obtaining noble metals
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Abstract
The object of the present invention is to provide the processes that palladium is adsorbed from high activity liquid waste, adsorbent is made using novel preparation method in the technique, by the way that adsorbent is added into high activity liquid waste, after ultrasonic 10min, temperature is controlled at 25 DEG C, with the velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbs palladium after adsorbent filtering is taken out from high activity liquid waste.This method uses novel sorbent preparation method, can effectively adsorb the Metal Palladium in high activity liquid waste, and the absorption to reach palladium metal utilizes.
Description
Technical field
The present invention relates to waste post-processing technology fields, more particularly to a kind of technique side for adsorbing palladium from high activity liquid waste
Method.
Background technology
In nuclear reactor, nuclear fuel can generate a large amount of Metal Palladium during fission, and the content of Metal Palladium can be because
It is different for the type of reactor and the difference of burnup.Such as the fast breeder reactor that burnup is 80GWd/t, it will produce about
The palladium of 4.34Kg, and the presurized water reactor that burnup is 33GWd/t will produce the palladium of about 1.33Kg.After spentnuclear fuel is post-treated, greatly
Partial palladium can enter in high activity liquid waste.
Palladium is a kind of noble metal, is played in modern high technology industry, modern industry and military industry important
Effect.In addition palladium is a kind of catalyst efficiently, multi-purpose, and indispensable role is played in chemical reaction.But the earth
On palladium resource it is very limited, the content in the earth's crust is only 10-8, and be unevenly distributed, extraction difficulty is larger, so seeking one
The new palladium resource acquisition mode of kind is a problem to be solved.
The palladium majority extracted from high activity liquid waste is existed with stable isotope form, and only minority is same with radioactivity
Existing for the element of position, often half-life period is very short or very long for these radioactive isotopes.Therefore, the palladium extracted from high activity liquid waste is
It can be used in the industrial production as stable palladium.So the extraction absorption palladium metal from high activity liquid waste, existing for alleviating
The palladium resource scarcity in stage has more important meaning.
Adsorbing metal palladium can encounter the problem of strong nitric acid, strong irradiation and a variety of sliver Interference between nuclei from high activity liquid waste.
Currently used extracting method is solvent extraction.Since the sixties in last century, researcher both domestic and external has carried out largely
Research, it is proposed that many new processes, but at present for majority be directed to hydrochloric acid system palladium extract, for nitric acid body
The report of the palladium extraction of system is relatively fewer.Also, there are some disadvantages in the extractant system used mostly so that the suction of Metal Palladium
Attached treatment effeciency is relatively low, and impurity content is higher.Therefore, it develops a kind of resistance to strong acid and there is good selection separation property to palladium
Palladium absorbing process be great challenge research work and a significantly scientific research.
Invention content
The object of the present invention is to provide the process for adsorbing palladium from high activity liquid waste, this method uses novel adsorbent
Preparation method can effectively adsorb the Metal Palladium in high activity liquid waste, and the absorption to reach palladium metal utilizes.
To achieve the above object, the present invention uses following technical scheme：
A kind of process for adsorbing palladium from high activity liquid waste, which is characterized in that comprise the steps of：
(1) preparation of adsorbent：Under nitrogen protection, aza macrocyclic ligands, potassium iodide and potassium carbonate have been dissolved in
It in solvent, stirs evenly, adds the mesoporous silicon oxide containing end chloro structure, continue stirring and back flow reaction 36-
48h after the completion of reaction, is cooled to room temperature, and is separated by filtration product, and dry 12-18h, must both be modified mesoporous silicon oxide after washing
Adsorbent；
(2) the palladium absorption in high activity liquid waste：It is added adsorbent into high activity liquid waste, after ultrasonic 10min, control temperature is 25
DEG C, with the velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out；
(3) the palladium desorption in adsorbent：The adsorbent of palladium will be adsorbed, has been put into desorption in the salpeter solution of thiocarbamide,
Both palladium-containing solution is obtained, adsorbent is recyclable after processing recycles.
Preferably, in the step 1 aza macrocyclic ligands be Isosorbide-5-Nitrae, 8,12- tetraazacyclododecane pentadecanes (14-N-4), Isosorbide-5-Nitrae,
7,10,13- five-nitrogen heterocyclic pentadecanes (15-N-5) or Isosorbide-5-Nitrae, 8,11- tetraazacyclododecane tetradecanes (14-N-4).
Preferably, in the step 1 organic solvent be anhydrous tetrahydro furan, dry toluene or anhydrous acetonitrile in one kind or
A variety of mixtures.
Preferably, aza macrocyclic ligands, potassium iodide, potassium carbonate and Jie containing end chloro structure in the step 1
The input mass ratio of hole silica is (1.5-2):(3-4):(6-10):1.
Preferably, the body of the quality and organic solvent of the mesoporous silicon oxide containing end chloro structure in the step 1
Product is than being 5-10g/L.
Preferably, the use ratio of adsorbent and high activity liquid waste is 7-10g/L in the step 2.
Preferably, the mass fraction of thiocarbamide is 1% in the salpeter solution of thiocarbamide in the step 3.
The invention has the advantages that multiple N atoms in salpeter solution in the ring skeleton of aza macrocyclic ligands
Palladium can be made to form highly stable complex compound, have very strong adsorption capacity to palladium；Simultaneously for the coordination meeting of other metal ions
It is influenced by the limitation of cavity size and the protonation of N atoms, it is difficult to adsorbed to other metal ions, to ensure that pair
The high-selectivity adsorption of palladium.
The adsorbent prepared in the invention has orderly pore passage structure, shorter mesoporous channel and larger aperture,
With very strong adsorption capacity, efficient space structure is provided for the absorption of palladium metal.
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.
The preparation of simulated high-level radioactive waste, wherein nitric acid acidity are 1mol/L, and contain each dvielement：0.35g/L K,
1.15g/L Na, 0.55g/L Cs, 0.17g/L Sr, 0.45g/L Ba, 0.05g/L Cd, 0.05g/L Ni, 0.255g/L
Nd, 0.075g/L Cr, 0.1g/L Ru, 0.09g/L Fe, 0.7g/L Mo, 0.15g/L Zr, 0.35g/L Pd.
Embodiment 1
Under nitrogen protection, by Isosorbide-5-Nitrae, 8,12- tetraazacyclododecane pentadecane (14-N-4) 160g, potassium iodide 350g and carbonic acid
Potassium 600g is dissolved in organic solvent, is stirred evenly, and the mesoporous silicon oxide 100g containing end chloro structure is added, and is continued
Simultaneously back flow reaction 36-48h is stirred, after the completion of reaction, is cooled to room temperature, is separated by filtration product, dry 12-18h after washing, both
Modified mesoporous silicon oxide adsorbent；7-10g adsorbents are added into 1L simulated high-level radioactive wastes, after ultrasonic 10min, control temperature
At 25 DEG C, with the velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out.
Palladium content is obtained with Atomic Absorption Spectrometry residue clear liquid, adsorbent is calculated to palladium according to adsorption equilibrium formula
Adsorption rate is 81.3%
Embodiment 2
Under nitrogen protection, by Isosorbide-5-Nitrae, 8,12- tetraazacyclododecane pentadecane (14-N-4) 150g, potassium iodide 380g and carbonic acid
Potassium 800g is dissolved in organic solvent, is stirred evenly, and the mesoporous silicon oxide 100g containing end chloro structure is added, and is continued
Simultaneously back flow reaction 42h is stirred, after the completion of reaction, is cooled to room temperature, is separated by filtration product, dry 16h, must both be modified Jie after washing
Hole silica adsorbent；10g adsorbents are added into 1L high activity liquid wastes, after ultrasonic 10min, control temperature at 25 DEG C, with
The velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out；The adsorbent of palladium will be adsorbed, has been put into 1% sulphur
Desorption in urea salpeter solution both obtains palladium-containing solution, and adsorbent is recyclable after processing recycles.
Palladium content is obtained with Atomic Absorption Spectrometry residue clear liquid, adsorbent is calculated to palladium according to adsorption equilibrium formula
Adsorption rate is 82.8%
Embodiment 3
Under nitrogen protection, by Isosorbide-5-Nitrae, 7,10,13- five-nitrogen heterocyclic pentadecane (15-N-5) 170g, potassium iodide 360g and
Potassium carbonate 700g is dissolved in organic solvent, is stirred evenly, and the mesoporous silicon oxide 100g containing end chloro structure is added,
Continue stirring and back flow reaction 48h, after the completion of reaction, be cooled to room temperature, be separated by filtration product, dry 18h, must both change after washing
Property mesoporous silicon oxide adsorbent；10g adsorbents are added into 1L high activity liquid wastes, after ultrasonic 10min, control temperature at 25 DEG C,
With the velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out；The adsorbent of palladium will be adsorbed, has been put into 1%
Desorption in thiocarbamide salpeter solution both obtains palladium-containing solution, and adsorbent is recyclable after processing recycles.
Palladium content is obtained with Atomic Absorption Spectrometry residue clear liquid, adsorbent is calculated to palladium according to adsorption equilibrium formula
Adsorption rate is 87.4%
Embodiment 4
Under nitrogen protection, by Isosorbide-5-Nitrae, 7,10,13- five-nitrogen heterocyclic pentadecane (15-N-5) 180g, potassium iodide 340g and
Potassium carbonate 1000g is dissolved in organic solvent, is stirred evenly, and the mesoporous silicon oxide containing end chloro structure is added
100g continues stirring and back flow reaction 36h, after the completion of reaction, is cooled to room temperature, is separated by filtration product, dry 16h after washing,
Both mesoporous silicon oxide adsorbent must be modified；10g adsorbents are added into 1L high activity liquid wastes, after ultrasonic 10min, control temperature exists
25 DEG C, with the velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out；The adsorbent of palladium will be adsorbed, has been put into
Desorption in 1% thiocarbamide salpeter solution both obtains palladium-containing solution, and adsorbent is recyclable after processing recycles.
Palladium content is obtained with Atomic Absorption Spectrometry residue clear liquid, adsorbent is calculated to palladium according to adsorption equilibrium formula
Adsorption rate is 86.9%
Embodiment 5
Under nitrogen protection, by Isosorbide-5-Nitrae, 8,11- tetraazacyclododecane tetradecanes (14-N-4) 190g, potassium iodide 320g and carbonic acid
Potassium 900g is dissolved in organic solvent, is stirred evenly, and the mesoporous silicon oxide 100g containing end chloro structure is added, and is continued
Simultaneously back flow reaction 42h is stirred, after the completion of reaction, is cooled to room temperature, is separated by filtration product, dry 18h, must both be modified Jie after washing
Hole silica adsorbent；10g adsorbents are added into 1L high activity liquid wastes, after ultrasonic 10min, control temperature at 25 DEG C, with
The velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out；The adsorbent of palladium will be adsorbed, has been put into 1% sulphur
Desorption in urea salpeter solution both obtains palladium-containing solution, and adsorbent is recyclable after processing recycles.
Palladium content is obtained with Atomic Absorption Spectrometry residue clear liquid, adsorbent is calculated to palladium according to adsorption equilibrium formula
Adsorption rate is 88.1%
Embodiment 6
Under nitrogen protection, by Isosorbide-5-Nitrae, 8,11- tetraazacyclododecane tetradecanes (14-N-4) 200g, potassium iodide 300g and carbonic acid
Potassium 800g is dissolved in organic solvent, is stirred evenly, and the mesoporous silicon oxide 100g containing end chloro structure is added, and is continued
Simultaneously back flow reaction 48h is stirred, after the completion of reaction, is cooled to room temperature, is separated by filtration product, dry 12h, must both be modified Jie after washing
Hole silica adsorbent；10g adsorbents are added into 1L high activity liquid wastes, after ultrasonic 10min, control temperature at 25 DEG C, with
The velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out；The adsorbent of palladium will be adsorbed, has been put into 1% sulphur
Desorption in urea salpeter solution both obtains palladium-containing solution, and adsorbent is recyclable after processing recycles.
Palladium content is obtained with Atomic Absorption Spectrometry residue clear liquid, adsorbent is calculated to palladium according to adsorption equilibrium formula
Adsorption rate is 90.2%.
Claims (6)
1. a kind of process for adsorbing palladium from high activity liquid waste, which is characterized in that comprise the steps of：
(1) preparation of adsorbent：Under nitrogen protection, aza macrocyclic ligands, potassium iodide and potassium carbonate are dissolved in organic molten
It in agent, stirs evenly, adds the mesoporous silicon oxide containing end chloro structure, continue stirring and back flow reaction 36-48h,
It after the completion of reaction, is cooled to room temperature, is separated by filtration product, dry 12-18h after washing must both be modified mesoporous silicon oxide absorption
Agent, wherein aza macrocyclic ligands are Isosorbide-5-Nitrae, 8,12- tetraazacyclododecane pentadecanes (14-N-4), Isosorbide-5-Nitrae, 7,10,13- five-nitrogen heterocyclics 15
Alkane (15-N-5) or 1,4,8,11- tetraazacyclododecane tetradecanes (14-N-4)；
(2) the palladium absorption in high activity liquid waste：Be added adsorbent into high activity liquid waste, after ultrasonic 10min, control temperature at 25 DEG C,
With the velocity fluctuation of 200r/min, until adsorption equilibrium, adsorbent is filtered and is taken out；
(3) the palladium desorption in adsorbent：The adsorbent of palladium will be adsorbed, has been put into desorption in the salpeter solution of thiocarbamide, both
Palladium-containing solution, adsorbent is recyclable after processing recycles.
2. the process according to claim 1 for adsorbing palladium from high activity liquid waste, which is characterized in that in the step 1
Organic solvent is one or more mixtures in anhydrous tetrahydro furan, dry toluene or anhydrous acetonitrile.
3. the process according to claim 1 for adsorbing palladium from high activity liquid waste, which is characterized in that in the step 1
Aza macrocyclic ligands, potassium iodide, potassium carbonate and the mesoporous silicon oxide containing end chloro structure input mass ratio be
(1.5-2):(3-4):(6-10):1。
4. the process according to claim 1 for adsorbing palladium from high activity liquid waste, which is characterized in that in the step 1
The quality of mesoporous silicon oxide containing end chloro structure and the volume ratio of organic solvent are 5-10g/L.
5. the process according to claim 1 for adsorbing palladium from high activity liquid waste, which is characterized in that in the step 2
The use ratio of adsorbent and high activity liquid waste is 7-10g/L.
6. the process according to claim 1 for adsorbing palladium from high activity liquid waste, which is characterized in that in the step 3
The mass fraction of thiocarbamide is 1% in the salpeter solution of thiocarbamide.
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| Mesoporous Silica Functionalized by Cyclam–Metal Groups Spectroscopic Studies and Numerical Modeling;M.Makowska-Janusik,et.al.;《Journal of Inorganic & Organometallic Polymers & Materials》;20101231;第761-773页 * |
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Effective date of registration: 20191114 Address after: 313000 1-B, building 1, No. 656, Qixing Road, high tech Zone, Wuxing District, Huzhou City, Zhejiang Province Patentee after: Huzhou Qiqi Electromechanical Technology Co.,Ltd. Address before: 523000 Guangdong province Dongguan City Songshan Lake high tech Industrial Zone Building 406 industrial development productivity Patentee before: Dongguan Lianzhou Intellectual Property Operation Management Co.,Ltd. |
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