CN104645946A - Method for adsorbing uranium by using macroporous poly-N-isopropylacrylamide/chitosan semi-interpenetrating network temperature-sensitive hydrogel - Google Patents
Method for adsorbing uranium by using macroporous poly-N-isopropylacrylamide/chitosan semi-interpenetrating network temperature-sensitive hydrogel Download PDFInfo
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Abstract
The invention relates to a method for adsorbing uranium by using macroporous poly-N-isopropylacrylamide/chitosan semi-interpenetrating network temperature-sensitive hydrogel. The method comprises the following steps: by utilizing emulsion polymerization means, taking Span-80 as an emulsifier, taking N,N'-methylene bisacrylamide (MBA) as a cross-linking agent, taking ammonium persulfate (APS) as an initiator, and taking N,N,N',N'-tetramethylethylenediamine (TEMED) as an accelerant, preparing the macroporous poly-N-isopropylacrylamide/chitosan semi-interpenetrating network temperature-sensitive hydrogel under certain conditions, and researching and measuring the adsorption performance of the hydrogel on uranium. Compared with the traditional gel and pore-free gel, the hydrogel disclosed by the invention has the characteristics of high mechanical strength, good swelling properties, large adsorption surface area, controllable adsorption and desorption processes, high uranium adsorption quantity and the like.
Description
Technical field
The invention belongs to the technical field to uranium absorption, relate to a kind of method carrying out adsorption uranium with macropore poly-N-isopropyl acrylamide/shitosan (being called for short macropore PNIPAAm/CS, lower same) semi-intercrossing network temperature-sensitive hydrogel.
Background technology
Uranium (uranium is called for short U) is a kind of very important energy goods and materials, all significant in industry, agricultural, national defence and science and technology.Uranium, as a kind of nuclear fuel, can discharge huge energy in nuclear reactor.In light-water reactor, the natural uranium of 1 ton is equivalent to 15 ~ 17 kiloton coals, can reach 45 ~ 50,000,000 degree for generating; In fast breeder reactor, about 1 ton of natural uranium is equivalent to 1,000,000 tons of coals, about 3,000,000,000 degree can be generated electricity.Nuclear fuel is also widely used in thrust power aspect in transport facility simultaneously.The nuclear power reactor that nuclear fuel produces can be used for submarine, ocean-going freighter, nuclear fuel load and flying power, is that general fuel is incomparable.Uranium also as nuclear explosive, can be used as the charging of nuclear weapon.Can produce more than 300 kind of nucleic during uranium fission, these nucleic and the peaceful use being applied as nuclear energy in every respect of generation ray thereof open another wide field.Simultaneously, uranium also can be used as the detonator of thermonuclear weapon hydrogen bomb, more than the 200 kind of radio isotope produced during uranium fission, each department of national economy is widely used in after being separated, as agriculturally for radioactive breeding, food industry is used for food fresh keeping sterilizing, pharmaceutically for radiotherapy, industrial for nondestructive inspection, geological prospecting, archaeology of cultural relic etc.Making full use of of uranium resource is that national economy is healthy, the Strategic Demand of steady development.Thus, carrying out the new industrial research adopted in uranium, while improving Utilization Rate of Mineral Resources, must focus on adopting the radioactive wastewater of smelting generation from uranium extracting uranium, to improve the comprehensive utilization ratio of uranium.Meanwhile, the contaminated wastewater produced in uranium mining process not only can affect the water quality of surrounding area, and produces irreversible pollution to mining area surrounding plants, farmland and soil, the health of the existence that impact is biological and the public.
Separation conventional at present, the method for enriched uranium have chemical precipitation, ion-exchange, solvent extraction, filtration and inverse osmosis etc., but these methods also exist produce new chemical contamination, energy consumption high, operate the shortcomings such as loaded down with trivial details and with high costs, limit their application.Compared with these methods, absorption method has the advantages such as the fast and capacity of sorbing material wide material sources, with low cost, selective height, speed is large.Absorption method is a kind of physical chemistry isolation technics to dissolved pollutant, waste water is mainly allowed to contact with the solid absorbent with absorption property, thus make the poisonous and hazardous material in waste water be attached on adsorbent surface, and then by poisonous and harmful substance removing in waste water.The key of absorption method is the absorption property of adsorbent, commonly mainly contains organic polymer, clay class, living beings class and rock etc. for the adsorbent of uranium in the Adsorption aqueous solution.But generally all there is high adsorption capacity but the deficiencies such as desorption is more difficult, mechanical strength is poor, the more difficult control of adsorption and desorption process, therefore, develop a kind of new adsorbent, make it have that larger adsorption surface area, mechanical strength are good, adsorption and desorption process control, high to uranium adsorbance, not only there is important theory significance, and there is actual application value.
Summary of the invention
The object of this invention is to provide a kind of method of adsorption uranium, namely with a method for macropore PNIPAAm/CS semi-intercrossing network temperature-sensitive hydrogel adsorption uranium, the adsorbent that described method is prepared have larger adsorption surface area, mechanical strength better, adsorption and desorption process control and there is high adsorbance to uranium.
The method of adsorption uranium of the present invention is as follows: the method first utilizing emulsion polymerisation, take Span-80 as emulsifying agent, N, N '-methylene-bisacrylamide (MBA) is crosslinking agent, and ammonium persulfate (APS) is initator, N, N, N ', N '-tetramethylethylenediamine (TEMED) is promoter, prepares macropore PNIPAAm/CS semi-intercrossing network temperature sensitive type uranium adsorbent.Then obtained macropore PNIPAAm/CS semi-interpenetrating network gel is joined in conical flask after freeze drying, add certain density uranium solution again, regulate the pH value of uranium solution with NaOH solution or HNO3 solution, vibrate to adsorption equilibrium with 200 r/min on the oscillator.Sample measuring liquid is treated in taking-up, treating to add in test sample the monoxone-sodium acetate buffer of pH=2.5 and arsenazo Ⅲ and constant volume, can calculate adsorption capacity (qe) according to adsorption equilibrium formula.
Absorbent preparation step of the present invention is as follows:
1) taking 0.5-1.0g shitosan monomer is dissolved in acetic acid, adds NIPA (NIPAAm) monomer and N, N '-methylene-bisacrylamide (MBA) crosslinking agent, mixes.
2) under stirring, add polyvinyl alcohol (PVA) stabilizing agent, emulsifying agent Span-80, after stirring 5-10 min, add ammonium persulfate (APS) initator and TEMED (TEMED) promoter.
3), after leaving standstill 24 h after stirring 10-15 min, take out gel, wash away Span-80 and PVA perforating agent with ethanol, use distilled water immersion 45-48 h again, timing changes water to remove unreacted monomer, residual initiators or catalyst, and finally gel is cut into block, freeze drying is for subsequent use.At polyvinyl alcohol (PVA), Span-80, after the whole mix and blend of ammonium persulfate (APS), TEMED (TEMED), time of repose is 20-30h.
In the preparation method of adsorbent, the mass fraction of acetic acid solution is 5%-10%.
In the preparation method of adsorbent, the mass ratio of shitosan monomer, NIPA (NIPAAm) monomer, N, N '-methylene-bisacrylamide (MBA) is 1:20-50:1.
In the preparation method of adsorbent, polyvinyl alcohol (PVA) stabilizing agent addition is 0.5-0.8mL.
In the preparation method of adsorbent, Span-80 emulsifying agent addition is 0.5-1.0mL.
In the preparation method of adsorbent, ammonium persulfate (APS) initator addition is 0.01-0.05g.
In the preparation method of adsorbent, TEMED promoter addition is 50-100 μ L.
Accompanying drawing explanation
Fig. 1 is the ESEM multiplication factor of large pore gel is 5000 times of figure,
Fig. 2 is the ESEM multiplication factor of large pore gel is 25000 times of figure,
Fig. 3 is the infrared spectrogram that large pore gel did not adsorb uranium,
Fig. 4 adsorption time affects change curve to macropore PNIPAAm/CS semi-interpenetrating network aqueous gel adsorption uranium,
Fig. 5 macropore PNIPAAm/CS semi-interpenetrating network aqueous gel is to the Temp .-changing adsorption curve of uranium.
Detailed description of the invention
Following examples are of the present invention further illustrating, instead of limit the scope of the invention.
Embodiment 1
1) accurately taking 0.5g shitosan monomer, to be dissolved in mass fraction be in the acetic acid of 5 %, adds 15 gNIPAAm monomers and 0.5g crosslinking agent MBA, mix.
2) under stirring, add 0.6 mL emulsifying agent stabilizing agent PVA, 0.8 mL emulsifying agent Span-80, after stirring 5-10 min, add 0.03 g initiator A PS and 60 μ L acceterator TE MED.
3), after leaving standstill 24 h after stirring 10-15 min, take out gel, wash away perforating agent Span-80 and PVA with ethanol, use distilled water immersion 48 h again, timing changes water to remove unreacted monomer, residual initiators or catalyst, finally gel is cut into block, freeze drying is for subsequent use.
Fig. 1 is the scanning electron microscope (SEM) photograph of large pore gel, and multiplication factor is 5000 times, and Fig. 2 multiplication factor is 25000 times.As we can see from the figure, there is obvious pore space structure gel inside, and the diameter of hole is about about 3 μm.Result shows, the pore structure be interconnected of preparation, adds the contact area of gel with uranium solution, is conducive to macropore PNIPAAm/CS semi-interpenetrating network gel to the absorption of uranium.
Embodiment 2
The absorption property to uranium investigated by the hydrogel that utilizes embodiment 1 to prepare, accurately takes three parts of 0.03g gels, first part of sample in contrast.Second part joins in the uranium standard liquid of 70 μ g/mL, at 308.15K temperature spot vibration appropriate time, get 1 mL supernatant at regular intervals, add 2 mL cushioning liquid, 2 mL arsenazo Ⅲs, are settled to 25 mL, measure absorbance, analyze the concentration of uranium in solution before and after absorption, calculate the adsorbance of uranium.3rd part joins in the uranium standard liquid of 70 μ g/mL, at 293.15K, 323.15K two temperatures point vibration appropriate time, gets 1 mL supernatant at regular intervals, add 2 mL cushioning liquid, 2 mL arsenazo Ⅲs, are settled to 25 mL, measure absorbance, calculate the adsorbance of uranium.
Fig. 3 is the infrared spectrogram that large pore gel did not adsorb uranium, as can be seen from Figure 3, the O-H of shitosan and the stretching vibration peak of-NH2 has been there is at about 3400 cm-1 place, and belong to the symmetry of-CH2 in shitosan and asymmetric absworption peak respectively at 2972 cm-1 and 2852 cm-1 places, the stronger absworption peak of C-N key is observed at 1386 cm-1 places.Fig. 4 is the infared spectrum after gel adsorption uranium.Near 910 cm-1, have an absworption peak clearly after adsorption uranium, this is the characteristic peak of uranyl ion.Also an absworption peak has been there is at 1550 cm-1 places, this is the characteristic peak of secondary amine (-N-H), absworption peak is there is at 1625 cm-1 places, this is the characteristic peak of acid amides (-CO-NH-), illustrate that the amino of gel surface changes acid amides into, also namely with uranyl ion chelating, show that this gel has successfully adsorbed the uranyl ion in water body.
Fig. 4 adsorption time affects change curve to macropore PNIPAAm/CS semi-interpenetrating network aqueous gel adsorption uranium, and as can be seen from the figure, gel reaches adsorption equilibrium at about 2 h, and adsorption capacity is 112 mg/g, illustrates the adsorbance of uranium high.
Fig. 5 macropore PNIPAAm/CS semi-interpenetrating network aqueous gel is to the Temp .-changing adsorption curve of uranium.
When temperature changes repeatedly, the adsorbance of uranium is also changed by the change of temperature.Experimental result shows, by simply changing temperature conditions, can well control the adsorption and desorption of large pore gel, reaches the final object of experiment.
Claims (10)
1. one kind with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium, it is characterized in that: the method first utilizing emulsion polymerisation, take Span-80 as emulsifying agent, N, N '-methylene-bisacrylamide (MBA) is crosslinking agent, ammonium persulfate (APS) is initator, N, N, N ', N '-tetramethylethylenediamine (TEMED) is promoter, prepare macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature sensitive type uranium adsorbent, then obtained macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel is joined in conical flask after freeze drying, add certain density uranium solution again, the pH value of uranium solution is regulated with NaOH solution or HNO3 solution, vibrate to adsorption equilibrium with 200 r/min on the oscillator, sample measuring liquid is treated in taking-up, treating to add in test sample the monoxone-sodium acetate buffer of pH=2.5 and arsenazo Ⅲ and constant volume, utilizing the mass concentration of uranium in spectrophotometry solution, can calculate adsorption capacity (qe) according to adsorption equilibrium formula.
2. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to claim 1, the preparation method of described macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature sensitive type uranium adsorbent, comprises the steps:
1) taking 0.5-1.0g shitosan monomer is dissolved in acetic acid, adds NIPA (NIPAAm) monomer and N, N '-methylene-bisacrylamide (MBA) crosslinking agent, mixes;
2) under stirring, add polyvinyl alcohol (PVA) stabilizing agent, emulsifying agent Span-80, after stirring certain hour, add ammonium persulfate (APS) initator and TEMED (TEMED) promoter;
3) leave standstill after stirring a period of time, take out gel, wash away Span-80 and PVA perforating agent, then use distilled water immersion with ethanol, timing changes water to remove unreacted monomer, residual initiators or catalyst, and finally gel is cut into block, freeze drying is for subsequent use.
3. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, is characterized in that: the mass fraction of acetic acid solution is 5%-10%.
4. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, it is characterized in that: the mass ratio of shitosan monomer, NIPA (NIPAAm) monomer, N, N '-methylene-bisacrylamide (MBA) is 1:20-50:1.
5. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, is characterized in that: polyvinyl alcohol (PVA) stabilizing agent addition is 0.5-0.8mL.
6. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, is characterized in that: Span-80 emulsifying agent addition is 0.5-1.0mL.
7. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, is characterized in that: ammonium persulfate (APS) initator addition is 0.01-0.05g.
8. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, is characterized in that: TEMED promoter addition is 50-100 μ L.
9. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, it is characterized in that: under stirring, add polyvinyl alcohol (PVA) stabilizing agent, emulsifying agent Span-80, ammonium persulfate (APS) initator and N is added after stirring 5-10 min, N, N ', N '-tetramethylethylenediamine (TEMED) promoter.
10. a kind of with the method for macropore poly-N-isopropyl acrylamide/shitosan semi-intercrossing network temperature-sensitive hydrogel adsorption uranium according to right 1 or 2, it is characterized in that: at polyvinyl alcohol (PVA), Span-80, ammonium persulfate (APS), N, N, N ', N '-tetramethylethylenediamine (TEMED) is mixing rear stirring 10-15 min all.
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| CN105885065A (en) * | 2016-05-13 | 2016-08-24 | 西南交通大学 | Preparation method of electrical stimulation-near infrared dual response high strength hydrogel |
| CN111013550A (en) * | 2019-12-12 | 2020-04-17 | 贵州师范学院 | Preparation of magnetic chitosan semi-interpenetrating thermal expansion hydrogel and application thereof in Cr (VI) adsorption |
| CN111545182A (en) * | 2019-11-20 | 2020-08-18 | 湖南工业大学 | Spherical double-network temperature-sensitive hydrogel adsorbent and preparation method and application thereof |
| CN114716724A (en) * | 2022-03-16 | 2022-07-08 | 华南理工大学 | Bionic intelligent hydrogel based on cuttlefish bone and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104945639A (en) * | 2015-06-17 | 2015-09-30 | 华南理工大学 | Sulfur-containing modified chitosan containing aerogel as well as preparation method and application thereof |
| CN105312041A (en) * | 2015-11-13 | 2016-02-10 | 哈尔滨工程大学 | Modified loofah sponge absorbent for uranium extraction from seawater and preparation method for loofah sponge absorbent |
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| CN111545182A (en) * | 2019-11-20 | 2020-08-18 | 湖南工业大学 | Spherical double-network temperature-sensitive hydrogel adsorbent and preparation method and application thereof |
| CN111013550A (en) * | 2019-12-12 | 2020-04-17 | 贵州师范学院 | Preparation of magnetic chitosan semi-interpenetrating thermal expansion hydrogel and application thereof in Cr (VI) adsorption |
| CN111013550B (en) * | 2019-12-12 | 2022-07-08 | 贵州师范学院 | Preparation of magnetic chitosan semi-interpenetrating thermal expansion hydrogel and application thereof in Cr (VI) adsorption |
| CN114716724A (en) * | 2022-03-16 | 2022-07-08 | 华南理工大学 | Bionic intelligent hydrogel based on cuttlefish bone and preparation method thereof |
| CN114716724B (en) * | 2022-03-16 | 2023-08-22 | 华南理工大学 | Bionic intelligent hydrogel based on cuttlefish bone and preparation method thereof |
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