CN103752262A - Method for preparing magnetic uranium adsorbent - Google Patents
Method for preparing magnetic uranium adsorbent Download PDFInfo
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- CN103752262A CN103752262A CN201410052120.6A CN201410052120A CN103752262A CN 103752262 A CN103752262 A CN 103752262A CN 201410052120 A CN201410052120 A CN 201410052120A CN 103752262 A CN103752262 A CN 103752262A
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Abstract
The invention provides a method for preparing a magnetic uranium adsorbent and belongs to the technical field of methods for preparing uranium adsorbing materials. The method comprises the following steps: (1) adding 0.2 g of Fe3O4 (40-80 emu/g) into ionized water and absolute ethanol, and adding ammonium hydroxide and ethyl orthosilicate under ultrasonic and agitating conditions to obtain an intermediate; (2) after adding Ca (NO3)2 and NaOH into the intermediate A under ultrasonic and agitating conditions, adding ethyl orthosilicate within 20-200 mins to obtain a magnetic adsorbent; (3) freeze-drying the magnetic adsorbent. The prepared adsorbing material is easily separated from a solution, the adsorbing performance is excellent, and the advantages of high adsorbing speed and large adsorbing capacity are represented in a wider temperature range, at different original initial concentrations and in different acid-base environments.
Description
Technical field
The present invention relates to uranium sorbing material preparation method, specifically a kind of preparation method of magnetic afwillite class uranium sorbing material.
Background technology
Nuclear energy is that the world today solves energy starved important channel, yet along with the fast development of nuclear industry, the uranium-bearing radioactive wastewater of generation is more and more.Due to half-life, high radioactivity and the bio-toxicity of uranium, uranium-bearing industrial wastewater has become a kind of long-term potential environmental hazard thing.Hydrated calcium silicate is the important uranium-bearing Industrial Wastewater Treatment raw material of a class, such material has extraordinary uranium and adsorbs under neutral and alkali condition, it is reported (Radiochim.Acta92 (2004) 645): hydrated calcium silicate for the Sorption ratio (sorption distribution ratio) of uranium between 30000-150000L/kg.Recently, the compound microballoon of preparing of afwillite and shitosan, specific area is large, for heavy metal, has suction-operated (Journal of Colloid and Interface Science418 (2014) 208-215) rapidly and efficiently.
These researchs show: afwillite has advantages of that as uranium sorbing material adsorption rate is fast, adsorption capacity is large.Yet after such adsorbent absorption, the problem of adsorbent and separated from solvent is not well solved for a long time.Along with going deep into of material structure performance study in recent years, the increase of specific area, particle diameter reduces, although adsorption rate and adsorption capacity are further improved, after absorption, the difficulty of adsorbent and separated from solvent further improves.Adding wherein magnetic material is the effective way addressing this problem.Preparation magnetic afwillite class adsorbent is not only for the removal of Uranium in Waste Water, and for the removal of other heavy metal and to realize the researchs such as slow controlled release of medicine all significant.Yet there is magnetic particle skewness in the method by simple doped magnetic medium, and the magnetic particle problems such as affecting afwillite structure and pattern that combines with silicon source.Therefore,, although magnetic separation technique has been widely used in adsorbent and separated from solvent aspect, we not yet find the report of magnetic afwillite class uranium adsorbent so far.
For above problem, the invention provides a kind of method of preparing magnetic afwillite class uranium sorbing material, it is large that this adsorbent has adsorption capacity, and adsorption rate is fast, is easy to separated advantage.
Summary of the invention
The concrete research approach of the present invention is as follows:
(1) 0.2g average grain diameter is less than to the Fe of 300nm
3o
4(40-80emu/g) put into 0.080-0.095M80mL HCl ultrasonic (20-40KHz) 15-30min, magnet is placed on to container bottom to be held applied magnetic Fe3O4 and pours out solution (Magnetic Isolation), extremely neutral by washed with de-ionized water, pour out deionized water, add 40mL deionized water and 160mL absolute ethyl alcohol, under ultrasonic (20-40KHz) and stirring condition, add 2mL28% Ammonia, further drip 0.28-0.30mmol ethyl orthosilicate, stir 7-10h, Magnetic Isolation, 50-100mL washed with de-ionized water 3-5 time, obtains intermediate;
(2) this step preparation process completes under ultrasonic (20-40KHz) and stirring condition, to the Ca (NO that adds 200mL15-30mmol/L in intermediate
3)
2solution, 10-30min, adds 1M NaOH solution 1mL, drips 4.00-4.50mmol ethyl orthosilicate in 20-200min, reaction 30min, Magnetic Isolation, 50-100mL washed with de-ionized water 3-5 time, obtains magnetic adsorbent;
(3) sample is placed in to refrigerator, at-4080 freezing 4-8h, freeze drying 24-48h;
(4) at 293-343K, pH=4-12, adsorption capacity is greater than 500mg/g, for initial concentration, is 10-500mg/L, and 30min clearance is greater than 85%.
Beneficial effect
1. step (1) is by Fe
3o
4particle surface superscribes SiO
2, it act as: parcel Fe
3o
4can avoid it for afwillite is synthetic, to exert an influence; Next this part SiO
2for unformed SiO
2, there is activity, can be used as the part silicon source that generates afwillite; Ion surface after parcel, with elecrtonegativity, can adsorb calcium ion again, makes afwillite in magnetic ion superficial growth.
2. ultrasonication is conducive to teos hydrolysis product and calcium ion generation afwillite, gets final product fast reaction speed, can avoid agglomeration again, increases specific surface, is conducive to absorption; But overcome for magnetic ion the effect deficiency that Action of Gravity Field impact fully disperses.In building-up process ultrasonic and stir under acting in conjunction condition and complete, further fast reaction speed, and realize the abundant dispersion of magnetic particle.
3. the present invention all adopts Magnetic Isolation in preparation process, and prepares pilot process and there is no suction filtration and drying steps, finally adopts freeze-dry process dry, has kept the original lamellar structure of afwillite, has increased its specific area up to 160-210m
2/ g.
4. the sorbing material of preparation is easy to the advantage separated with solution except having, and good adsorption performance, under wider temperature range, different original initial concentration and different acid or alkali environment, all shows adsorption rate fast, the advantage that adsorption capacity is large.Solid foundation has been established in the extensive use that these performances are this adsorbent.
Accompanying drawing explanation
The SEM figure of the material of accompanying drawing 1 embodiment 5 preparations, can clearly find that Fe, Ca, Si element are evenly distributed.
The TEM figure of the material of accompanying drawing 2 embodiment 5 preparations, can clearly find Fe
3o
4for spherical, at water and the calcium silicates of its outside growth sheet.
The specific embodiment
Embodiment 1:
(1) 0.2g average grain diameter is less than to the Fe of 300nm
3o
4(50-80emu/g) put into 0.080-0.095M80mL HCl ultrasonic (20-40KHz) 15-30min, Magnetic Isolation, to neutral, pours out deionized water by washed with de-ionized water, add 40mL deionized water and 160mL absolute ethyl alcohol, under ultrasonic (20-40KHz) and stirring condition, add 2mL28% Ammonia, further drip 0.28-0.30mmol ethyl orthosilicate, stir 7-10h, Magnetic Isolation, 50-100mL deionized water disappears and washes 3-5 time, obtains intermediate.
(2) this step preparation process completes under ultrasonic (20-40KHz) and stirring condition, to the Ca (NO that adds 200mL15-30mmol/L in intermediate
3)
2solution, 10-30min, adds 1M NaOH solution 1mL, drips 4.00-4.50mmol ethyl orthosilicate in 20-200min, reaction 30min, Magnetic Isolation, 50-100mL washed with de-ionized water 3-5 time, obtains magnetic adsorbent.
(3) sample is placed in to refrigerator ,-40--80 ℃ freezing 4-8h, freeze drying 24-48h.
(4) prepare adsorbent intensity of magnetization 15-40emu/g, at 293-343K, pH=4-12, is 10-500mg/L for initial concentration, and adsorption capacity is greater than 500mg/g, and 30min clearance is greater than 85%.
Embodiment 2:
The uranium absorbent preparation method of embodiment 2 is substantially the same manner as Example 1, and difference is: step (1) is less than 0.2g average grain diameter the Fe of 300nm
3o
4(40-80emu/g) put into 0.095M80mL HCl ultrasonic (20KHz) 15-30min, Magnetic Isolation, to neutral, pours out deionized water by washed with de-ionized water, add 40mL deionized water and 160mL absolute ethyl alcohol, under ultrasonic (20KHz) and stirring condition, add 2mL28% Ammonia, further drip 0.29mmol ethyl orthosilicate, stir 7h, Magnetic Isolation, 50mL washed with de-ionized water 5 times, obtains intermediate.
Embodiment 3:
The uranium absorbent preparation method of embodiment 3 is substantially the same manner as Example 2, and difference is: step (2) this step preparation process completes under ultrasonic (40KHz) and stirring condition, to the Ca (NO that adds 200mL22mmol/L in intermediate
3)
2solution, 10min, adds 1M NaOH solution 1mL, drips 4.50mmol ethyl orthosilicate in 30min, reaction 30min, Magnetic Isolation, 50mL washed with de-ionized water 5 times, obtains magnetic adsorbent.
Embodiment 4:
The uranium absorbent preparation method of embodiment 4 is substantially the same manner as Example 3, and difference is: step (2) this step preparation process completes under ultrasonic (40KHz) and stirring condition, to the Ca (NO that adds 200mL18mmol/L in intermediate
3)
2solution, 10min, adds 1M NaOH solution 1mL, drips 4.50mmol ethyl orthosilicate in 30min, reaction 30min, Magnetic Isolation, 50mL washed with de-ionized water 5 times, obtains magnetic adsorbent.
Embodiment 5:
The uranium absorbent preparation method of embodiment 5 is substantially the same manner as Example 3, and difference is: step (3) is placed in refrigerator by sample, at-60 ℃ of freezing 6h, freeze drying 24h.
Embodiment 6:
The uranium absorbent preparation method of embodiment 5 is substantially the same manner as Example 4, and difference is: step (3) is placed in refrigerator by sample, at-60 ℃ of freezing 6h, freeze drying 24h.
Claims (6)
1. a preparation method for magnetic uranium adsorbent, concrete steps are as follows:
(1) 0.2g average grain diameter is less than to the Fe of 300nm
3o
4(50-80emu/g) put into 0.080-0.095M80mL HCl ultrasonic (20-40KHz) 15-30min, Magnetic Isolation, extremely neutral by washed with de-ionized water, after Magnetic Isolation, add 40mL deionized water and 160mL absolute ethyl alcohol, under ultrasonic (20-40KHz) and stirring condition, add 2mL28% Ammonia, further drip 0.28-0.30mmol ethyl orthosilicate, stir 7-10h, Magnetic Isolation, 50-100mL washed with de-ionized water 3-5 time, obtains intermediate;
(2) this step preparation process completes under ultrasonic (20-40KHz) and stirring condition, to the Ca (NO that adds 200mL15-30mmol/L in intermediate
3)
2solution, 10-30min, adds 1M NaOH solution 1mL, drips 4.00-4.50mmol ethyl orthosilicate in 20-200min, reaction 30min, Magnetic Isolation, 50-100mL washed with de-ionized water 3-5 time, obtains magnetic adsorbent;
(3) sample is placed in to refrigerator ,-40--80 ℃ freezing 4-8h, freeze drying 24-48h.
2. the preparation method of magnetic uranium adsorbent as claimed in claim 1, is characterized in that: step (1) is less than 0.2g average grain diameter the Fe of 300nm
3o
4(40-80emu/g) put into 0.095M80mL HCl ultrasonic (20KHz) 15-30min, Magnetic Isolation, to neutral, pours out deionized water by washed with de-ionized water, add 40mL deionized water and 160mL absolute ethyl alcohol, under ultrasonic (20KHz) and stirring condition, add 2mL28% Ammonia, further drip 0.29mmol ethyl orthosilicate, stir 7h, Magnetic Isolation, 50mL washed with de-ionized water 5 times, obtains intermediate A.
3. the preparation method of magnetic uranium adsorbent as claimed in claim 2, is characterized in that: step (2) this step preparation process completes under ultrasonic (40KHz) and stirring condition, to the Ca (NO that adds 200mL22mmol/L in intermediate A
3)
2solution, 10min, adds 1M NaOH solution 1mL, drips 4.50mmol ethyl orthosilicate in 30min, reaction 30min, Magnetic Isolation, 50mL washed with de-ionized water 5 times, obtains magnetic adsorbent.
4. the preparation method of magnetic uranium adsorbent as claimed in claim 2, is characterized in that: step (2) this step preparation process completes under ultrasonic (40KHz) and stirring condition, to the Ca (NO that adds 200mL18mmol/L in intermediate A
3)
2solution, 10min, adds 1M NaOH solution 1mL, drips 4.50mmol ethyl orthosilicate in 30min, reaction 30min, Magnetic Isolation, 50mL washed with de-ionized water 5 times, obtains magnetic adsorbent.
5. the preparation method of magnetic uranium adsorbent as claimed in claim 3, is characterized in that: step (3) is placed in refrigerator by sample, at-60 ℃ of freezing 6h, freeze drying 24h.
6. the preparation method of magnetic uranium adsorbent as claimed in claim 4, is characterized in that: step (3) is placed in refrigerator by sample, at-60 ℃ of freezing 6h, freeze drying 24h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104741084A (en) * | 2015-03-03 | 2015-07-01 | 清华大学 | Uranium adsorbent applicable to alkaline environment and preparation method of uranium adsorbent |
| CN105236455A (en) * | 2015-09-27 | 2016-01-13 | 黑龙江科技大学 | Composite material |
| CN107570108A (en) * | 2017-09-27 | 2018-01-12 | 黑龙江科技大学 | A kind of processing method of spent acid, kerosene shale ash and white clay |
| CN114249450A (en) * | 2020-09-21 | 2022-03-29 | 西南科技大学 | Method for one-step deep purification of high-concentration organic uranium-containing low-level radioactive waste liquid by using magnetic ferrite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101856628A (en) * | 2010-04-30 | 2010-10-13 | 北京科技大学 | Conducting polymer modified magnetic photocatalyst and preparation method thereof |
| JP2012240017A (en) * | 2011-05-23 | 2012-12-10 | Nittetsu Kankyo Engineering Kk | Treating material of harmful substance, and treating method of harmful substance |
| CN102921435A (en) * | 2012-10-31 | 2013-02-13 | 湖北大学 | Magnetic Fe3O4/SiO2/TiO2/quantum dot compounded nanometer photocatalyst and preparation method and application thereof |
-
2014
- 2014-02-14 CN CN201410052120.6A patent/CN103752262B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101856628A (en) * | 2010-04-30 | 2010-10-13 | 北京科技大学 | Conducting polymer modified magnetic photocatalyst and preparation method thereof |
| JP2012240017A (en) * | 2011-05-23 | 2012-12-10 | Nittetsu Kankyo Engineering Kk | Treating material of harmful substance, and treating method of harmful substance |
| CN102921435A (en) * | 2012-10-31 | 2013-02-13 | 湖北大学 | Magnetic Fe3O4/SiO2/TiO2/quantum dot compounded nanometer photocatalyst and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| BING-QIANG LU ET.AL.: "Synthesis and application in drug delivery of hollow-core-double-shell magnetic iron oxide/silica/calcium silicate nanocomposites", 《MATERIALS LETTERS》, vol. 104, 10 April 2013 (2013-04-10), pages 53 - 56 * |
| JIN WU ET.AL.: "Hierachically Nanostructured Mesoporous Spheres of Calcium Silicate Hydrate: Surfactant-Free Sonochemical Synthesis and Drug-Delivery System with Ultrahigh Drug-Loading Capacity", 《ADV. MATER》, vol. 22, 24 November 2009 (2009-11-24), pages 749 - 753, XP007921708, DOI: doi:10.1002/adma.200903020 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104741084A (en) * | 2015-03-03 | 2015-07-01 | 清华大学 | Uranium adsorbent applicable to alkaline environment and preparation method of uranium adsorbent |
| CN104741084B (en) * | 2015-03-03 | 2017-10-17 | 清华大学 | It is a kind of suitable for uranium absorption agent of alkaline environment and preparation method thereof |
| CN105236455A (en) * | 2015-09-27 | 2016-01-13 | 黑龙江科技大学 | Composite material |
| CN107570108A (en) * | 2017-09-27 | 2018-01-12 | 黑龙江科技大学 | A kind of processing method of spent acid, kerosene shale ash and white clay |
| CN114249450A (en) * | 2020-09-21 | 2022-03-29 | 西南科技大学 | Method for one-step deep purification of high-concentration organic uranium-containing low-level radioactive waste liquid by using magnetic ferrite |
| CN114249450B (en) * | 2020-09-21 | 2024-02-02 | 西南科技大学 | Method for deep purification of high-concentration organic uranium-containing low-level waste liquid in one step by using magnetic ferrite |
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| CN103752262B (en) | 2015-08-05 |
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