CN113026147A - Preparation method of calcium hydrophosphate nanofiber for efficiently separating uranium - Google Patents
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Abstract
The invention discloses a preparation method for constructing nano fibrous calcium hydrophosphate, belonging to the field of synthesis of nano functional materials. The invention adopts a simple nano microemulsion method to prepare the calcium hydrophosphate. Different nanotopography can be obtained by the method. And the fibrous calcium hydrophosphate shows better performance of adsorbing uranium in extracting uranium from seawater. Compared with the prior amidoxime material and other materials, the invention has the advantages of relatively simple preparation method, mass production and large-scale popularization. The uranium adsorbent can be used as a cheap and efficient uranium adsorbent and can also be used as a subsequent good adsorption carrier.
Description
The invention belongs to preparation of a uranium extraction adsorbent from seawater, and particularly relates to a method for preparing nano fibers by coordination through a soft template self-assembly method. The method realizes the high-efficiency adsorption of uranyl ions through the chelation of phosphate radicals.
Background
The nuclear energy is a green pollution-free energy source, is widely applied to top-end nuclear weapons of various countries, and is also a majority of electric energy sources of the masses. Nuclear power generation is a high percentage, particularly in many developed countries. The key element of nuclear energy is uranium, which is widely sourced from crusta, seawater and nuclear waste. However, because the storage amount of uranium on land is limited, only one of the uranium content of seawater is a few thousand, and the emission pollution of nuclear waste is serious, the search for an efficient adsorbent for extracting uranium from seawater is very necessary.
Common adsorption methods include physical chemical adsorption, photoelectrochemical adsorption, ion exchange, and the like. Chemisorption is a relatively simple, efficient, and widespread process, but the amount and rate of adsorption are limited. Most of common adsorbents are amidoxime group materials, the preparation process is complex, and the whole process is not environment-friendly. Recently, phosphate group polymer materials have attracted attention, and uranyl ions are chelated by phosphate groups to achieve efficient adsorption. Different from the high molecular phosphoric acid-based material, the natural phosphoric acid-based inorganic material such as calcium hydrophosphate, calcium phosphate and hydroxyl calcium phosphate has low price, relatively environment-friendly preparation process and relatively good adsorption performance.
The preparation of nano materials by a soft template nano emulsion method is a good method for controlling the appearance, a series of nano sheets, nano fibers and other materials with good appearance can be prepared by self-assembly of inorganic ions at an interface and ordered nucleation growth, and the materials with good appearance have higher adsorption area and are better beneficial to adsorption. Therefore, the prepared inorganic material with low price and special nano-morphology realizes rapid green adsorption, is further used as an adsorption matrix material, and has important significance and practical application value.
Disclosure of Invention
[ problem to be solved ]
The invention aims to prepare calcium hydrophosphate nano-materials with different shapes by using a micro-emulsion method and realize efficient uranium extraction from seawater. The method has mild synthesis conditions and simple synthesis process, is easy to realize rapid and efficient mass production, and has extremely high adsorption capacity of uranyl, which is two to three times of that of commercialized powder.
[ solution ]
The invention adopts the following technical scheme:
the invention utilizes the self-assembly strategy of microemulsion and inorganic salt precursor, adds surfactant in an ethanol water system, forms micelle and pore-forming agent mesitylene to form nano microemulsion by utilizing the amphiprotic characteristic of the surfactant, then supplies soluble calcium salt and phosphoric acid into the microemulsion system, has coordination action between calcium ions and the surfactant, adjusts the pH value of the solution by ammonia water, slowly precipitates out materials, the precursor can well grow special nano flaky and fibrous shape on a soft template, and removes the surfactant and mesitylene by washing and extracting for many times, thereby preparing the calcium hydrophosphate with various nano shapes. The prepared adsorbent has good adsorption effect, and has high adsorption capacity, adsorption rate and adsorption saturation value in different pH ranges and different uranyl concentrations.
A. Preparation of microemulsions
Preparing a uniform system with the volume of water/ethanol being 1:1, adding a surfactant (polyethylene oxide-polypropylene oxide-polyethylene oxide), and ultrasonically dispersing or stirring to completely dissolve the surfactant to obtain a colorless, clear and transparent solution. Then, the mesitylene is added drop by drop and stirred to obtain the stable and uniform oil-in-water microemulsion.
B. Preparation of inorganic salt solution
Weighing a certain amount of calcium source and a certain amount of phosphorus source, respectively placing the calcium source and the phosphorus source in a beaker, and adding a certain amount of ethanol water (volume ratio is 1: 1). Ultrasonic dispersion is convenient for dissolving and stirring to promote the salt solution to be uniform, and a colorless, clear and transparent solution is obtained.
C. Inorganic ion coordination polymerization assembly
And C, slowly adding the inorganic salt solution in the step B into the microemulsion in the step A, so that the inorganic ions and the microemulsion are self-assembled, and stirring for a period of time.
D. Adjusting pH to precipitate the product
Dispersing a certain amount of ammonia water into a beaker, and adding a certain amount of ethanol water (volume ratio is 1: 1). Ultrasonic separation is carried out to facilitate dispersion, and the solution in C is added. After reacting for a period of time, centrifuging, extracting, washing, and freeze-drying to obtain the product.
According to a further technical scheme of the invention, in the step A, the volume of the ethanol water is 50 ml; the surfactant is Pluronic F-127, and the mass of the P123 surfactant is 0 g-2 g; the volume of the mesitylene is 0-4 ml.
According to a further technical scheme of the invention, in the step B, the metal salt is calcium chloride, calcium nitrate, calcium acetate and calcium sulfate; the mass of the calcium source is 1 mmol-3 mmol; the anion salt comprises phosphoric acid, sodium dihydrogen phosphate and disodium hydrogen phosphate, wherein the volume of (85 wt%) is 0.1-1ml, and the mass of the phosphate is 1 mmol-3 mmol; the volume of the corresponding mixture is 30ml-50 ml.
According to a further technical scheme, in the step C, the stirring time is 10-30 min.
According to a further technical scheme, in the step D, the corresponding volume of ammonia water is 0-2ml, the amount of ethanol water is 30-50ml, and the selected centrifugal speed is 8000 rpm; the extractant can be ethanol and acetone, and the detergent can be water and ethanol.
The calcium hydrophosphate nanofiber obtained by the preparation method is adsorbed to be saturated in a short time under a certain uranyl ion concentration, and the adsorption efficiency of the calcium hydrophosphate nanofiber is twice that of an amidoxime material which is researched more before and is three times that of commercialized powder.
The present invention will be described in detail below.
A preparation method of calcium hydrophosphate nanofiber for efficiently separating uranium comprises the following steps:
A. preparation of microemulsions
Firstly preparing a uniform 50ml system of water/ethanol, adding a surfactant Pluronic F-127(PEO polyethylene oxide-PPO polypropylene oxide-PEO polyethylene oxide), and performing ultrasonic dispersion or stirring to completely dissolve the mixture to obtain a colorless, clear and transparent solution. Then, the mesitylene is added drop by drop and stirred to obtain the stable and uniform oil-in-water microemulsion.
In the invention, as PPO-PEO is added into ethanol water, and PPO has one more methyl group than PEO, the hydrophilic and hydrophobic difference forms reverse micelles, but the hydrophilic and hydrophobic difference is not large, and the formed reverse micelles are not stable, so that the non-polar TMB added into the oil phase can stabilize TMB liquid drops, not only can enhance the hydrophilic and hydrophobic difference at two ends of F127 to form microemulsion, but also can be used as a pore-forming agent.
B. Preparation of inorganic salt solution
Weighing a certain amount of calcium source and a certain amount of phosphorus source, respectively placing the calcium source and the phosphorus source in a beaker, and adding a certain amount of ethanol water (volume ratio is 1: 1). Ultrasonic dispersion is convenient for dissolving and stirring to promote the salt solution to be uniform, and a colorless, clear and transparent solution is obtained.
In the present invention, the dielectric constant of the calcium source and phosphate in ethanolic water will be reduced, which makes them less susceptible to ionization than water, which effectively slows down the nucleation rate, allowing for the construction of specific nanotopography.
C. Inorganic ion coordination-assisted polymerization assembly
And C, slowly adding the inorganic salt solution in the step B into the microemulsion in the step A, so that the inorganic ions and the microemulsion are self-assembled, and stirring for a period of time.
In the invention, a plurality of ether bonds of PEO and PPO of the surfactant F127 can not only form coordination with metal calcium ions to effectively control the nucleation of calcium hydrophosphate, but also form coordination with the metal calcium ions, and the micelle linear structure of the surfactant in water creates conditions for preparing the precursor of the nanofiber. The addition of the oil phase molecule mesitylene forms holes in the fiber winding growth process, which is beneficial to expanding the adsorption area.
D. Adjusting pH to precipitate the product
Dispersing a certain amount of ammonia water into a beaker, and adding a certain amount of ethanol water (volume ratio is 1: 1). Ultrasonic separation is carried out to facilitate dispersion, and the solution in C is added. After reacting for a period of time, centrifuging, extracting, washing, and freeze-drying to obtain the product.
In the invention, most of the phosphoric acid source and calcium source solution in the solution C is acidic, so that the whole precursor is difficult to precipitate, and the ammonia water is dissolved in the ethanol water, so that the pH of the solution can be regulated and controlled, the precursor of the calcium hydrophosphate can be precipitated, and in addition, compared with the method of directly dripping the ammonia water, the method is favorable for slow nucleation. The ethanol water extraction can remove most of the surfactant and pore-forming agent, and after freeze drying, the water is sublimated, and the powder becomes fluffy.
The calcium hydrophosphate nanofiber prepared by the preparation method is about more than 250mg, and is saturated by adsorption for three hours under a certain uranyl ion concentration, the adsorption capacity is close to 3000mg-U/g, and the adsorption efficiency of the calcium hydrophosphate nanofiber is greatly higher than that of an amidoxime material which is researched more before.
[ advantageous effects ]
Compared with the prior art, the invention has the following beneficial effects:
compared with the prior art, the synthesis process of the nano fibrous inorganic compound powder prepared by the invention is simpler. The calcium hydrophosphate nanofiber is prepared by using micelle as a template through the coordination of a commercialized surfactant and inorganic cations. The preparation method has the advantages of easily available raw materials, simple preparation process, low price and mass production.
The calcium hydrogen phosphate adsorbent prepared by the invention has better advantages when being used for adsorbing uranyl, the fibrous nanometer morphology improves the adsorption area, and the surface protonated anions are beneficial to fully coordinating uranyl ions, so that the rapid and efficient adsorption is realized. The adsorbent can be used as a good adsorption matrix and loaded on fibers, hydrogel and sponge, and large-area commercial uranium extraction from seawater is realized.
Drawings
FIG. 1 is a scanning electron microscope image of fibrous calcium hydrogen phosphate produced by the method;
FIG. 2 shows the comparison of the adsorption performance of calcium hydrogen phosphate fiber on different metal ions in 700L natural seawater;
Detailed Description
The invention will be further elucidated and described with reference to the embodiments of the invention described hereinafter.
1g of F127 was added to 50ml of ethanol water (volume ratio 1:1) and stirred to form a clear solution, 2ml of TMB was added and stirred to form a microemulsion. Adding 2mmol of CaCl2With 0.5ml H3PO4Respectively dissolved in 30ml of ethanol water (volume ratio is 1: 1). Adding into the microemulsion in sequence, stirring and reacting for 0.5h, and dissolving 1ml of ammonia water in 30ml of ethanol water (volume ratio is 1:1) respectively. Adding into the solution successively, stirring for reaction for 10 hr, centrifuging, extracting, washing to remove surfactant and trimethylbenzene, and freeze drying to obtain powder.
Claims (5)
1. A preparation method of calcium hydrophosphate nanofiber for efficiently separating uranium comprises the following steps:
A. preparation of microemulsions
Preparing a uniform system with the volume of water/ethanol being 1:1, adding a surfactant (polyethylene oxide-polypropylene oxide-polyethylene oxide), and ultrasonically dispersing or stirring to completely dissolve the surfactant to obtain a colorless, clear and transparent solution. Then, the mesitylene is added drop by drop and stirred to obtain the stable and uniform oil-in-water microemulsion.
B. Preparation of inorganic salt solution
Weighing a certain amount of calcium source and a certain amount of phosphoric acid source, respectively placing the calcium source and the phosphoric acid source in a beaker, and adding a certain amount of ethanol water (volume ratio is 1: 1). Ultrasonic dispersion is convenient for dissolving and stirring to promote the salt solution to be uniform, and a colorless, clear and transparent solution is obtained.
C. Inorganic ion coordination-assisted polymerization assembly
And C, slowly adding the inorganic salt solution in the step B into the microemulsion in the step A, so that the inorganic ions and the microemulsion are self-assembled, and stirring for a period of time.
D. Adjusting pH to precipitate the product
Adding a certain amount of ammonia water into a beaker, and adding a certain amount of ethanol water (volume ratio is 1: 1). Ultrasonic separation is convenient for complete dispersion, and the solution in C is added. After reacting for a period of time, centrifuging, extracting, washing, and freeze-drying to obtain the product.
2. The production method according to claim 1, wherein in step a, the ethanol water has a volume of 50 ml; the surfactant is Pluronic F-127, and the mass of the P123 surfactant is 0 g-2 g; the volume of the mesitylene is 0-4 ml.
3. The preparation method according to claim 1, wherein in the step B, the metal salt is calcium chloride, calcium nitrate, calcium acetate, calcium sulfate; the mass of the calcium source is 1 mmol-3 mmol; the anion salt comprises phosphoric acid, sodium dihydrogen phosphate and disodium hydrogen phosphate, wherein the volume of the phosphoric acid (85 wt%) is 0.1-0.5 ml, and the mass of the phosphate is 1-3 mmol; the volume of the corresponding mixture is 30ml-50 ml.
4. The method according to claim 1, wherein in the step C, the stirring time is 10 to 30 min.
5. The preparation method according to claim 1, in the step D, the ammonia water corresponds to a volume of 0-1ml, the amount of ethanol water is 30-50ml, and the selected centrifugation speed is 8000 rpm; the extractant is ethanol or acetone, and the detergent is water and ethanol.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB799627A (en) * | 1955-12-29 | 1958-08-13 | Exxon Research Engineering Co | Recovery of uranium from aqueous solutions |
| US4311676A (en) * | 1978-09-08 | 1982-01-19 | Minemet Recherche | Process for the recovery of uranium contained in phosphated compounds |
| US4410497A (en) * | 1982-01-26 | 1983-10-18 | Mobil Oil Corporation | Separation of uranium from carbonate containing solutions thereof by direct precipitation |
| US20080220233A1 (en) * | 2004-06-15 | 2008-09-11 | Promimic Ab | Synthetic Nano-Sized Crystalline Calcium Phosphate and Method of Production |
| US20090061284A1 (en) * | 2007-08-31 | 2009-03-05 | Peter Blennow | Ceria and strontium titanate based electrodes |
| CN105688828A (en) * | 2016-02-05 | 2016-06-22 | 南华大学 | Method for preparing plant-inorganic composite adsorbents from phosphoric-acid-modified folium cycas for extracting uranium from seawater |
| CN110330004A (en) * | 2019-08-06 | 2019-10-15 | 山东交通学院 | A method of regulating and controlling hydroxyapatite micro Nano material pattern using phosphorus source |
| CN111384407A (en) * | 2020-02-25 | 2020-07-07 | 电子科技大学 | Preparation method of metal monoatomic-dispersed ordered mesoporous carbon spheres |
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2021
- 2021-03-17 CN CN202110283716.7A patent/CN113026147B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB799627A (en) * | 1955-12-29 | 1958-08-13 | Exxon Research Engineering Co | Recovery of uranium from aqueous solutions |
| US4311676A (en) * | 1978-09-08 | 1982-01-19 | Minemet Recherche | Process for the recovery of uranium contained in phosphated compounds |
| US4410497A (en) * | 1982-01-26 | 1983-10-18 | Mobil Oil Corporation | Separation of uranium from carbonate containing solutions thereof by direct precipitation |
| US20080220233A1 (en) * | 2004-06-15 | 2008-09-11 | Promimic Ab | Synthetic Nano-Sized Crystalline Calcium Phosphate and Method of Production |
| US20090061284A1 (en) * | 2007-08-31 | 2009-03-05 | Peter Blennow | Ceria and strontium titanate based electrodes |
| CN105688828A (en) * | 2016-02-05 | 2016-06-22 | 南华大学 | Method for preparing plant-inorganic composite adsorbents from phosphoric-acid-modified folium cycas for extracting uranium from seawater |
| CN110330004A (en) * | 2019-08-06 | 2019-10-15 | 山东交通学院 | A method of regulating and controlling hydroxyapatite micro Nano material pattern using phosphorus source |
| CN111384407A (en) * | 2020-02-25 | 2020-07-07 | 电子科技大学 | Preparation method of metal monoatomic-dispersed ordered mesoporous carbon spheres |
Non-Patent Citations (1)
| Title |
|---|
| LIANG PENG ET AL.: "Versatile Nanoemulsion Assembly Approach to Synthesize Functional Mesoporous Carbon Nanospheres with Tunable Pore Sizes and Architectures", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
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