CN108273473A - A method of detaching caesium using carbon-based calixarenes crown ether hybrid material - Google Patents
A method of detaching caesium using carbon-based calixarenes crown ether hybrid material Download PDFInfo
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- CN108273473A CN108273473A CN201810054652.1A CN201810054652A CN108273473A CN 108273473 A CN108273473 A CN 108273473A CN 201810054652 A CN201810054652 A CN 201810054652A CN 108273473 A CN108273473 A CN 108273473A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D323/00—Heterocyclic compounds containing more than two oxygen atoms as the only ring hetero atoms
Abstract
The invention discloses a kind of methods detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that including:The carbon-based calixarenes crown ether hybrid material is mixed with the nitrate solution containing various metals ion, the cesium ion in nitrate solution is by adsorbing separation.The method of the present invention is suitable for highly acidity system, easy to operate without adding other organic compounds or carrier, and selectivity is good, and separative efficiency is high, is easy to carry out industrial application.
Description
Technical field
The present invention relates to cesium element separation technology fields, and in particular to a kind of to utilize carbon-based calixarenes crown ether hybrid material point
Method from caesium.
Background technology
Being widely used in for nuclear energy also brings huge health threat while bringing various convenient to the mankind, using
A large amount of radioactive wastes are often generated during nuclear energy, these waste degradation times are long, easily cause serious environment
How pollution safely and effectively handles these radioactive wastes and has become the key factor for restricting nuclear energy sustainable development.
Nuclear power will not discharge since energy density is big, pollution is few and cause greenhouse gases and vigorously be sent out in recent years
Exhibition, however can be inevitably generated spentnuclear fuel in nuclear power operation.High activity liquid waste (HLLW) caused by spentnuclear fuel post-processing,
It is a kind of peracidity, high radioactivity and highly toxic mixed solution.
The degradation time of these high activity liquid wastes is long, easily causes serious environmental pollution, how safely and effectively to handle this
A little radioactive wastes have become the key factor for restricting nuclear energy sustainable development, and the method for common processing high activity liquid waste has suction
Attached method, ion-exchange and membrane separation process, the number of devices involved by these methods is numerous, and treatment process steps are complicated;Due to
When handling high activity liquid waste, waste liquid can all cause radioactive pollution when often passing through a kind of equipment or structures, therefore in processing procedure
Number of devices is more, and processing step is more complicated, caused by pollute more serious, therefore number of devices should be reduced to the greatest extent, shortening processing
Technological process.
137Cs is one of hot main source in high heat release nucleic and high activity liquid waste, to glass solidified body and water
Mud firming body stability has potential for adverse effects, long-term existence that can lead to firming body aging, radionuclide is caused to leak, not only
It is unfavorable for high activity liquid waste storage, and groundwater environment is polluted.If they are effectively divided before high activity liquid waste eventually disposition
From, to extend storage the time limit, save disposal costs and promoted disposal technology be all advantageous;137Efficiently separating for Cs can also be notable
High activity liquid waste radioactive intensity is reduced, is provided convenience to further detaching Minor actinides.
Invention content
For the problem that in the prior art, being difficult to Selective Separation caesium in highly acidity system, the present invention provides a kind of profits
The method for detaching caesium with carbon-based calixarenes crown ether hybrid material is suitable for highly acidity system, and easy to operate, selectivity is good, separation
It is efficient, it is easy to carry out industrial application.
The technical solution adopted by the present invention is as follows:
A method of caesium being detached using carbon-based calixarenes crown ether hybrid material, including:By the carbon-based calixarenes crown ether
Hybrid material is mixed with the nitrate solution containing various metals ion, and the cesium ion in nitrate solution is by adsorbing separation;
The structure of the carbon-based calixarenes crown ether hybrid material is shown in formula I:
Represent porous carbon ball, the integer that n is 1~4.
Contain Cs (I) and other metal ions in the nitrate solution, other metal ions include Na (I), K (I), Sr
(II), at least one of Ba (II), Ru (III) and Fe (III).
In nitrate solution, the concentration of metal ion and the concentration of nitric acid can influence separating effect, it is preferable that nitric acid
In salting liquid, a concentration of 5.0 × 10 per metal ion species-4~1.0 × 10-2M.In nitrate solution, nitric acid it is a concentration of
0.5~6M.Further preferably, in nitrate solution, a concentration of 2~4M of nitric acid, under the acid condition, carbon-based calixarenes hat
Ether hybrid material is best to the absorption property of caesium.
In order to ensure separating effect, it is preferable that carbon-based calixarenes crown ether hybrid material and nitrate solution room temperature (25 ±
5 DEG C) under mixing and absorption, adsorption time be 20~120min.Mixing and absorption carries out under oscillating condition, oscillation rate be 120~
150rpm。
The usage amount of carbon-based calixarenes crown ether hybrid material can be adjusted according to demand, it is preferable that every gram of carbon-based cup virtue
Hydrocarbon crown ether hybrid material is mixed with 80~200mL nitrate solutions, and in the range, carbon-based calixarenes crown ether hybrid material is to caesium
Selectivity it is good, separative efficiency is high.
The preparation method of the carbon-based calixarenes crown ether hybrid material is as follows:
(1) concentrated nitric acid is added in porous carbon ball and carries out hydro-thermal reaction, dry carboxylated carbon ball after washed;
(2) amino cup [4]-crown- 6 as shown in formula II is dissolved in organic solvent, addition N, N- carbonyl dimidazoles,
Carboxylated carbon ball is added after 0.5~1.5h of stirring and continues 8~20h of stirring, post-treated carbon-based calixarenes crown ether that must be described is miscellaneous
Change material;
The integer that n is 1~4.
Preferably, in step (1), 8~15mL concentrated nitric acids are added in every gram of porous carbon ball;Nitric acid dosage is very few, then porous
The carboxyl that carbon ball surface generates is less;Nitric acid dosage is excessive, then can cause porous carbon ball structural instability.
Preferably, in step (1), the concentrated nitric acid is contacted by nitric acid vapor with porous carbon ball, it is ensured that inside and outside carbon ball
Surface can be contacted with nitric acid, and exposure level is uniform.
The porous carbon ball is prepared by conventional means in the prior art, is such as by carbon source, F127 of phenolic resin
Template is prepared.
The temperature of the hydro-thermal reaction is 100~150 DEG C, and the time of hydro-thermal reaction is 4~6 hours.
Preferably, in step (2), the organic solvent is dimethylformamide (DMF) or acetonitrile.
Preferably, in step (2), amino cup [4]-crown- 6, N, N- carbonyl dimidazoles, carboxylated carbon ball and organic solvent
Amount ratio is 1mol:1.1~1.5mol:30~35g:4.5~6L.
Amino cup [the 4]-crown- 6 is prepared by conventional means in the prior art.
In step (2), N, N- carbonyl dimidazoles are added portionwise in system, after ensureing that raw material can be sufficiently mixed uniformly
Reaction, reacts the CO of generation2It can escape in time.
The higher product of purity in order to obtain, it is preferable that the post-processing in step (2) includes:Reaction product was carried out
Filter, sediment wash away amino cup [4] crown- 6, the excessive N for not participating in reaction with DMF successively, and N- carbonyl dimidazoles and part are secondary
Product, ethyl alcohol wash away the DMF being mingled in porous carbon ball, ether washes away ethyl alcohol in favor of drying, it is vacuum dried obtain it is described
Carbon-based calixarenes crown ether hybrid material.
Compared with prior art, the invention has the advantages that:The present invention for the first time passes through amino cup [4]-crown- 6
The method of chemical modification is fixed in porous carbon ball, structure novel, preparation method simple possible, in energy Selective Separation water phase
Caesium.In general, the extremely similar alkali metal element association of the properties such as caesium and potassium, sodium, strontium exists, caused to the separating-purifying of caesium very big
Difficulty, for carbon-based cup [4] -6 hybrid material of crown- of the present invention for detaching caesium in water phase, which has acidproof, alkaline-resisting, high Cs
The advantages that selectivity and identity, is suitable for highly acidity system, easy to operate without adding other organic compounds or carrier,
Selectivity is good, and separative efficiency is high, is easy to carry out industrial application.
Description of the drawings
Fig. 1 is the FT- of porous carbon ball, carboxylated carbon ball, amino cup [4]-crown- 6 and carbon-based calixarenes crown ether hybrid material
IR infrared spectrums;
Fig. 2 is the SEM figures for the carbon-based calixarenes crown ether hybrid material that embodiment 1 is prepared;
Fig. 3 is the isothermal adsorption desorption curve of carbon ball, carboxylated carbon ball and carbon-based calixarenes crown ether hybrid material;
Fig. 4 is carbon ball, the graph of pore diameter distribution of carboxylated carbon ball and carbon-based calixarenes crown ether hybrid material;
Fig. 5 is to utilize the carbon-based calixarenes crown ether hybrid material prepared separating element caesium from nitrate solution of the invention
The relational graph that adsorption isothermequation changes with concentration of nitric acid;
Fig. 6 is to utilize the carbon-based calixarenes crown ether hybrid material prepared separating element caesium from nitrate solution of the invention
The relational graph that adsorption isothermequation changes with adsorption time.
Specific implementation mode
Porous carbon ball used in the present invention is prepared by the following method:
0.96g F127 are taken to be dissolved in 15mL deionized waters;Accurately weigh 0.6g phenol, 2.1mL formaldehyde, 15mL
0.1mol·L-1NaOH is uniformly mixed, with 340rmin at a temperature of 70 DEG C-10.5h synthesis low molecules are at the uniform velocity stirred under rotating speed
The phenolic resin of amount;Then the F127 of dissolving is poured into phenolic resin, temperature is changed to 66 DEG C, continues to stir, is added after 2h
50mL deionized waters persistently stir 16~18h, have seen whether that precipitation generates, and stop reaction after generating precipitation;When standing one section
Between precipitation dissolving after, take the dissolved liquid of 17.7mL with 56mL deionized waters uniformly dilution after be transferred into autoclave;In
Hydro-thermal reaction is taken out afterwards for 24 hours at 130 DEG C, and centrifugation is cleaned up with deionized water, and drying is put into after milling in tube furnace, nitrogen
Gas shielded calcines 3h at 700 DEG C, it is burned after black solid fully ground up to the porous carbon in shape planetary ball mill
Ball.
Embodiment 1
The synthesis signal route of the carbon-based calixarenes crown ether hybrid material of the present embodiment is as follows:
The preparation method of the present embodiment includes:
(1) 0.2g porous carbon balls are weighed, are put into 20mL inner liner of reaction kettle, the 20mL liners equipped with porous carbon ball are put into
The inner liner of reaction kettle of 100mL takes 2mL concentrated nitric acids to be added in 100mL inner liner of reaction kettle, is reacted 5 hours in 120 DEG C after sealing, the phase
Between, concentrated nitric acid, with porous carbon ball haptoreaction, it is clear to take out product deionized water in the form of nitric acid vapor after being cooled to room temperature
It is washed till drying carboxylated carbon ball after neutrality.
(2) in Ar protects gas, 3.382g (4.75mmol) amino cup as shown in formula II I is added to 25ml DMF
[4]-crown- 6, makes it dissolve, then 0.923g (5.7mmol) N, N- carbonyl dimidazoles are added thereto, and CDI points of several aliquots are added,
The CO of generation2It is escaped in 5min, 1h is stirred at room temperature in mixture.0.166g carboxylated carbon balls are added in the mixture,
Stirring 18 hours.Filtering mixture obtains sediment after reaction, and sediment is washed twice with 20mlDMF, the washing of 20ml ethyl alcohol
Twice, 20ml ether washes twice, and 8h is dried in vacuo at 50 DEG C, the carbon-based calixarenes crown ether hydridization material described in 1.47g can be obtained
Expect (i.e. carbon-based cup [4]-crown- 6), carbon-based cup [4]-crown- 6) structure as shown in formula IV, yield 65%.
Wherein, the FT- of porous carbon ball, carboxylated carbon ball, amino cup [4]-crown- 6 and carbon-based calixarenes crown ether hybrid material
IR infrared spectrums are as shown in Figure 1.Carbon-based cup [4]-crown- 6 is by the amino in the carboxyl and amino cup [4]-crown- 6 in carbon ball
It carries out amidation process to be made, therefore carbon-based cup [4]-crown- 6 can retain carbon ball and 6 infrared signature peak of cup [4]-crown-.In amino
In cup 6 spectrogram of [4]-crown-, 3365cm-1Do not go out in carbon-based cup [the 4]-crown- 6 obtained after amide reaction for amino peak, the peak
Show, at the same time the 1612cm in carbon-based cup [4] -6 spectrogram of crown--1There is the peaks N-H, 1712cm in place-1There are the peaks C=O in place, shows
Amido bond is formed.Infrared spectrum confirms that carbon-based cup [4]-crown- 6 is successfully prepared.
The SEM figures for the carbon-based calixarenes crown ether hybrid material that the present embodiment is prepared are as shown in Figure 2.
The BET characterization results of porous carbon ball, carboxylated carbon ball and carbon-based calixarenes crown ether hybrid material as shown in figs. 34,
BET data is as shown in table 1,
Table 1
Embodiment 2
The preparation method of the present embodiment includes:
(1) 0.2g porous carbon balls are weighed, are put into 20mL inner liner of reaction kettle, the 20mL liners equipped with porous carbon ball are put into
The inner liner of reaction kettle of 100mL takes 2mL concentrated nitric acids to be added in 100mL inner liner of reaction kettle, is reacted 5 hours in 120 DEG C after sealing, the phase
Between, concentrated nitric acid, with porous carbon ball haptoreaction, it is clear to take out product deionized water in the form of nitric acid vapor after being cooled to room temperature
It is washed till drying carboxylated carbon ball after neutrality.
(2) in Ar protects gas, 3.382g (4.75mmol) amino cups [4]-crown- 6 is added to 25ml DMF, keeps its molten
Solution, then 0.923g (5.7mmol) N, N- carbonyl dimidazoles are added thereto, CDI points of several aliquots are added, the CO of generation2In 5min
1h is stirred at room temperature in mixture by interior effusion.0.143g carboxylated carbon balls are added in the mixture, stir 12 hours.Reaction
After filter mixture obtain sediment, sediment is washed twice with 20ml DMF, and 20ml ethyl alcohol washes twice, and 20ml ether is washed
It washs twice, 8h is dried in vacuo at 50 DEG C, the carbon-based calixarenes crown ether hybrid material described in 1.52g, yield 73% can be obtained.
Embodiment 3~9
(1) by alkali metal salt NaNO3、KNO3、CsNO3;Alkali salt Sr (NO3)2、Ba(NO3)2;Transition metal salt Fe
(NO3)3;7 kinds of metal salts such as nitrate solution of noble metal Ru are dissolved in salpeter solution addition deionized water and are configured to contain simultaneously
The nitrate solution of various metals ion, the concentration of nitric acid in nitrate solution are 4.0M, each metal ion a concentration of 2.0 ×
10-3M。
(2) concentrated nitric acid and deionized water are added in the nitrate solution that step (1) obtains, adjusts in nitrate solution
Concentration of nitric acid is respectively 0.5,1.0,2.0,3.0,4.0,5.0,6.0M, a concentration of 5.0 × 10 per metal ion species-3M。
(3) salting liquid for the different concentration of nitric acid containing 7 kinds of metallic elements for obtaining step (2) is prepared with embodiment 1
The contact mixing of carbon-based calixarenes crown ether hybrid material, amount ratio when mixing is:0.1g carbon is corresponded to per 10mL nitrate solutions
Base calixarenes crown ether hybrid material;
(4) mixed liquor obtained by step (3) is adsorbed on DHG-9073BS-III type electric heating constant-temperature blowing drying boxes
Experiment, oscillator oscillation rate are 120rpm, are operated under room temperature 298K, adsorption time 180min makes absorption reach balance, makes
Absorption reaches balance, and the content of each element in the front and back different nitric acid water phases of absorption is then measured with ICP-OES.
The absorption result of embodiment 3~9 is as shown in figure 5, abscissa is concentration of nitric acid value in Fig. 5;Ordinate is absorption point
Distribution coefficient Kd, unit cm3/ g, as seen from the figure, when concentration of nitric acid increases to 3.0M by 0.5M, the absorption distribution system of caesium
Number is by 51.2cm3/ g increases to 75.2cm3/ g, when concentration of nitric acid continues to increase to 6.0M by 3.0M, the adsorption isothermequation of caesium
By 75.2cm3/ g drops to 45.4cm3/g.The result illustrates that under the highly acidity of 1.0M~6.0M, carbon-based cup [4]-crown- 6 is still
Performance with Separation of Cs;Optimum acidity is 3.0M, this acidity is consistent with the acidity of common high activity liquid waste, it was demonstrated that the material has directly
Scoop out the potentiality for high-level liquid waste partitioning Cs.Meanwhile the material has higher selectivity to Cs, other metal ions are not
It is adsorbed.
Embodiment 10~17
Experiment condition and step are same as Example 3, the difference is that, by nitrate solution, concentration of nitric acid is solid
Be set to 3.0M, successively change time of contact be, 1,5,10,20,30,60,90,120min, gained separating resulting as shown in fig. 6,
Abscissa is adsorption time in Fig. 6, and ordinate is adsorption isothermequation Kd, unit cm3/g.Before 30min, the absorption point of caesium
Distribution coefficient Kd(Cs)Quickly increase increase with time, when 30min, Kd(Cs)For 75.1cm3/ g, later Kd(Cs)It is basically unchanged, shows to inhale
The attached time for reaching balance is 30min.The K of Na (I), K (I), Sr (II), Ba (II), Ru (III) and Fe (III)dValue compared with
It is small, show not adsorbed.
Claims (9)
1. a kind of method detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that including:By the carbon-based cup
Aromatic hydrocarbons crown ether hybrid material is mixed with the nitrate solution containing various metals ion, and the cesium ion in nitrate solution is adsorbed
Separation;
The structure of the carbon-based calixarenes crown ether hybrid material is shown in formula I:
Represent porous carbon ball, the integer that n is 1~4.
2. the method according to claim 1 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that institute
It states and contains Cs (I) and other metal ions in nitrate solution, other metal ions include Na (I), K (I), Sr (II), Ba
(II), at least one of Ru (III) and Fe (III).
3. the method according to claim 1 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that institute
It states in nitrate solution, a concentration of 5.0 × 10 per metal ion species-4~1.0 × 10-2M, nitric acid a concentration of 0.5~
6.0M。
4. the method according to claim 1 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that every
Gram carbon-based calixarenes crown ether hybrid material is mixed with 80~200mL nitrate solutions.
5. the method according to claim 1 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that institute
The preparation method for the carbon-based calixarenes crown ether hybrid material stated is as follows:
(1) concentrated nitric acid is added in porous carbon ball and carries out hydro-thermal reaction, dry carboxylated carbon ball after washed;
(2) amino cup [4]-crown- 6 as shown in formula II is dissolved in organic solvent, N, N- carbonyl dimidazoles, stirring is added
Carboxylated carbon ball is added after 0.5~1.5h and continues 8~20h of stirring, post-treated carbon-based calixarenes crown ether hydridization material that must be described
Material;
The integer that n is 1~4.
6. the method according to claim 5 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that step
Suddenly in (1), 8~15mL concentrated nitric acids are added in every gram of porous carbon ball.
7. the method according to claim 5 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that step
Suddenly in (1), the temperature of the hydro-thermal reaction is 100~150 DEG C, and the time of hydro-thermal reaction is 4~6 hours.
8. the method according to claim 5 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that step
Suddenly in (2), the amount ratio of amino cup [4]-crown- 6, N, N- carbonyl dimidazoles, carboxylated carbon ball and organic solvent are 1mol:1.1
~1.5mol:30~35g:4.5~6L.
9. the method according to claim 5 for detaching caesium using carbon-based calixarenes crown ether hybrid material, which is characterized in that step
Suddenly the post-processing in (2) includes:Reaction product is filtered, sediment is washed with DMF, ethyl alcohol and ether successively, through vacuum
It is dried to obtain the carbon-based calixarenes crown ether hybrid material.
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---|---|---|---|---|
CN111285880A (en) * | 2019-08-28 | 2020-06-16 | 中南大学 | Preparation and application of switch compound containing bisprown ether |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1295861A2 (en) * | 2001-09-24 | 2003-03-26 | Synaptec GmbH | Calix(6)arenes, process for their preparation and their application |
CN102935355A (en) * | 2012-11-06 | 2013-02-20 | 浙江大学 | Adsorbent for separating heating element Cs and preparation method and application thereof |
CN105363425A (en) * | 2015-12-03 | 2016-03-02 | 中国科学院青海盐湖研究所 | Magnetic cesium ion adsorbent and preparation method therefor |
-
2018
- 2018-01-19 CN CN201810054652.1A patent/CN108273473A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1295861A2 (en) * | 2001-09-24 | 2003-03-26 | Synaptec GmbH | Calix(6)arenes, process for their preparation and their application |
CN102935355A (en) * | 2012-11-06 | 2013-02-20 | 浙江大学 | Adsorbent for separating heating element Cs and preparation method and application thereof |
CN105363425A (en) * | 2015-12-03 | 2016-03-02 | 中国科学院青海盐湖研究所 | Magnetic cesium ion adsorbent and preparation method therefor |
Non-Patent Citations (1)
Title |
---|
ANYUN ZHANG ET AL.: ""Extraction behavior of cesium and some typical fission and non-fission products with a new 1,3-di(1-decyloxy)-2,4- crown-6-calix[4]arene"", 《RADIOCHIM. ACTA》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111285880A (en) * | 2019-08-28 | 2020-06-16 | 中南大学 | Preparation and application of switch compound containing bisprown ether |
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