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Ordered lamellar polyamidoxime-based graphene oxide composite material for extracting uranium from seawater and preparation method thereof

A technology of polyamidoxime and composite materials, applied in chemical instruments and methods, alkali metal compounds, alkali metal oxides/hydroxides, etc., can solve the problem of limited uranium extraction effect, slow adsorption rate of uranyl ions, and poor adsorption rate. Slow and other problems, to achieve ultra-high hydrophilicity and water permeability, good uranium adsorption performance, the effect of simple process

Active Publication Date: 2021-11-26
HAINAN UNIVERSITY
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Problems solved by technology

Adsorption method is one of the most researched methods at present, but some adsorption materials such as metal-organic frameworks and nano-carbon materials have problems such as low adsorption efficiency, poor water stability, high cost, and difficult recovery. Therefore, the preparation is efficient, cheap, and has high selectivity. And durable uranium adsorption material is the key to realize the industrialization of seawater uranium extraction
[0003]Amidoxime-based materials have a strong affinity for uranyl ions, and even under the condition of extremely low uranyl ion concentration, they still have a strong affinity for uranyl ions. Strong complexation, but due to the shortcomings of amidoxime-based materials such as poor ion selectivity and slow adsorption rate
Chinese patent CN202010304846.X discloses a polyamide oxime / graphene nanoribbon composite aerogel, which first uses potassium permanganate oxidation to axially cut multi-walled carbon nanotubes to make graphene oxide nanoribbons; In the mixture of fully mixed acrylonitrile and ammonium persulfate, the polyacrylonitrile / graphene nanoribbon composite hydrogel was preliminarily prepared by solvothermal polymerization; The reaction converts the cyano group into an amidoxime group to obtain a polyamide oxime / graphene nanoribbon composite hydrogel, which is finally made into a polyamide oxime / graphene nanoribbon composite aerogel after low-temperature freeze-drying. Has a certain effect of extracting uranium, but the slow adsorption rate of uranyl ions leads to limited effect of extracting uranium

Method used

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  • Ordered lamellar polyamidoxime-based graphene oxide composite material for extracting uranium from seawater and preparation method thereof
  • Ordered lamellar polyamidoxime-based graphene oxide composite material for extracting uranium from seawater and preparation method thereof
  • Ordered lamellar polyamidoxime-based graphene oxide composite material for extracting uranium from seawater and preparation method thereof

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Embodiment 1

[0021] Embodiment 1: A method for preparing an ordered lamellar polyamidoxime-based graphene oxide composite material for extracting uranium from seawater, comprising the following steps:

[0022] S101: Preparation of amidoxime-based polyacrylonitrile powder

[0023] Add 5.5g of hydroxylamine hydrochloride to a flask containing 60mL of N-N dimethylformamide, heat to 45°C, stir magnetically until completely dissolved, then add 3.8g of sodium bicarbonate and 1g of sodium hydroxide, stir for at least 3h, then add 4.2 g polyacrylonitrile powder, fully dissolved, heated to 65°C for 24 hours, then added 1.9g sodium bicarbonate and 0.5g sodium hydroxide to react for 12 hours, cooled and centrifuged at 10000rpm / min to obtain amidoximated polyacrylonitrile solution , the solution was dropped into deionized water to obtain a white precipitate, and finally vacuum-dried at 60° C. to obtain amidoximated polyacrylonitrile powder.

[0024] S102: Preparation of amidoxime-based polyacrylonitr...

Embodiment 2

[0033] Embodiment two: the difference between embodiment two and embodiment one is that the mass ratios of graphene oxide and polyamidoxime used in step S103 are respectively 25:75, 20:80, 15:85, 10:90, 5: 95 and 0:100, uranium adsorption test was carried out at room temperature (25°C), 1L, 8ppm uranium spiked simulated seawater (pH=8).

[0034] Table 1 Effect of different polyamidoxime concentrations on the properties of polyamidoxime graphene oxide composites

[0035]

[0036]It can be seen from Table 1 that with the increase of polyamidoxime concentration, the uranyl ion adsorption capacity of the prepared ordered lamellar polyamidoxime graphene oxide composite material first gradually increased and then decreased, and at 85% When the mass ratio of polyamide oxime is 75%, the uranium adsorption capacity of the material is significantly lower than that of 85%, the main reason is that the structure gradually changes from disorder to order, and the order structure is optima...

Embodiment 3

[0037] Embodiments three to four: The difference between embodiment three and embodiment one is that in step (3), the molds are respectively immersed in liquid nitrogen for freezing, and at room temperature (25° C.), 1 L, 8 ppm uranium spiked simulated seawater (pH =8) for uranium adsorption test. The difference between Example 3 and Example 1 is that it was directly frozen at -60°C for 24 hours and formed without undergoing rapid freezing in a liquid nitrogen environment.

[0038] Table 2 Effects of different freezing conditions on the properties of polyamide oxime graphene oxide composites

[0039]

[0040] It can be seen from Table 2 that different freezing methods will directly affect the forming structure of the material, and the uranium adsorption effect of the ordered lamellar structure is better than that of the disordered structure, because the specific surface area and adsorption property of the ordered structure are better. in a disordered structure.

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Abstract

The invention discloses a preparation method of an ordered lamellar polyamidoxime-based graphene oxide composite material for extracting uranium from seawater. The preparation method comprises the following steps of mixing a polyamidoxime alkaline solution and a graphene oxide aqueous solution, and uniformly stirring at room temperature to obtain a polyamidoxime-graphene oxide mixed solution, injecting the polyamidoxime-graphene oxide mixed solution into a mold, enabling the liquid level of the mixed solution to be positioned above the liquid nitrogen, carrying out primary freezing, putting the mixed solution into a cold trap of a freeze dryer, carrying out secondary freezing, and finally drying to obtain the ordered lamellar polyamidoxime-based graphene oxide composite material. The mass ratio of the graphene oxide to the polyamidoxime is (5-15): (85-95). According to the method disclosed by the invention, a lamellar ordered macroporous structure is formed by self-assembly under the supramolecular action between the graphene oxide and the amidoxime, so that the composite material has ultrahigh hydrophilicity and water permeability, thereby having excellent uranium adsorption efficiency and uranium adsorption selectivity.

Description

technical field [0001] The invention relates to the field of preparation of new materials, in particular to an ordered lamellar polyamidoxime-based graphene oxide composite material for extracting uranium from seawater and a preparation method thereof. Background technique [0002] Seawater contains a large amount of uranium resources, with a total reserve of 4.29 billion tons of uranium, which is nearly 1,000 times that of land reserves. However, due to the extremely low concentration of uranium in seawater (3.3 μg / L), uranium usually exists as very stable uranyl carbonate ions, and the concentration of other metal ions in seawater is much higher than the concentration of uranyl ions, so from It is very difficult to extract uranium from seawater for nuclear fuel. Adsorption method is one of the most researched methods at present, but some adsorption materials such as metal-organic frameworks and nano-carbon materials have problems such as low adsorption efficiency, poor wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C22B3/24C22B60/02
CPCB01J20/20B01J20/265B01J20/28033C22B60/0265C22B3/24Y02P10/20
Inventor 刘涛张若倩王宁陈梦伟
Owner HAINAN UNIVERSITY
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