CN107349919B - Synthetic method and application of uranyl adsorbing material - Google Patents
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Abstract
The invention belongs to the field of adsorption materials, and particularly relates to a synthetic method and application of a uranyl adsorption material. The synthesis method provided by the invention comprises the following steps: a) mixing the fiber, the polymer, the double bond monomer and water, and performing electron beam irradiation to obtain gel; the polymer comprises one or more of polyvinyl alcohol, polyvinylpyrrolidone, polystyrene and polyacrylonitrile; the double-bond monomer comprises one or more of acrylonitrile, divinyl benzene, styrene, acrylic acid, acrylamide, butadiene, pentadiene and triallyl isocyanurate; b) mixing the gel with acrylonitrile, and performing electron beam irradiation to obtain a graft cross-linked body; c) and mixing the grafted cross-linked body with hydroxylamine for reaction to obtain the uranyl adsorbing material. The synthetic method provided by the invention is low in cost, and the synthesized uranyl adsorbing material is large in adsorption capacity, good in uranyl adsorption selectivity and good in use stability.
Description
Technical Field
The invention belongs to the field of adsorption materials, and particularly relates to a synthetic method and application of a uranyl adsorption material.
Background
Uranium is an important nuclear power raw material, and therefore, the development of uranium resources is an important requirement for the development of nuclear power in China. The land uranium resources in China are extremely deficient, and the total amount of the uranium resources in seawater is about 45 hundred million tons, which is equivalent to 1000 times of the uranium content in the land ore. Therefore, uranium extraction from seawater is a promising nuclear fuel supply source and is a necessary trend for the development of the future nuclear industry.
Uranium is typically present in the ocean as the formation of uranyl ions. Since the last 60 s, countries such as japan, the united states, and france have been engaged in research on projects for extracting uranium from seawater, and various adsorbing materials for adsorbing uranyl ions from seawater have been developed. However, these adsorbents generally have problems such as high production cost, low adsorption capacity, poor adsorption selectivity, and poor stability in use.
Disclosure of Invention
In view of the above, the present invention aims to provide a synthetic method of a uranyl adsorption material and an application thereof, and the synthetic method provided by the present invention has the advantages of low cost, large adsorption capacity of the synthesized uranyl adsorption material, good uranyl adsorption selectivity, and good use stability.
The invention provides a synthetic method of a uranyl adsorbing material, which comprises the following steps:
a) mixing the fiber, the polymer, the double bond monomer and water, and performing electron beam irradiation to obtain gel;
the polymer comprises one or more of polyvinyl alcohol, polyvinylpyrrolidone, polystyrene and polyacrylonitrile;
the double-bond monomer comprises one or more of acrylonitrile, divinyl benzene, styrene, acrylic acid, acrylamide, butadiene, pentadiene and triallyl isocyanurate;
b) mixing the gel with acrylonitrile, and performing electron beam irradiation to obtain a graft cross-linked body;
c) and mixing the grafted cross-linked body with hydroxylamine for reaction to obtain the uranyl adsorbing material.
Preferably, in step a), the fibers comprise one or more of straw fibers, cotton fibers, bamboo fibers, bagasse fibers, and wood pulp fibers.
Preferably, in the step a), the mass ratio of the fiber, the polymer, the double bond monomer and the water is (10-20): (100-150): (3-30): (400-600).
Preferably, in the step a), the irradiation dose of the electron beam is 100-200 kGy.
Preferably, in the step b), the mass ratio of the gel, the acrylonitrile and the hydroxylamine is (7-15): (1-2).
Preferably, in the step b), the irradiation dose of the electron beam is 40-80 kGy.
Preferably, the mass ratio of the gel in the step b) to the hydroxylamine in the step c) is (7-15): (3-6).
Preferably, in the step c), the reaction temperature is 60-90 ℃.
Preferably, in the step c), the reaction time is 5-8 h.
The invention provides application of the adsorption material synthesized by the method in the technical scheme in uranium extraction from seawater.
Compared with the prior art, the invention provides a synthetic method and application of a uranyl adsorbing material. The synthesis method provided by the invention comprises the following steps: a) mixing the fiber, the polymer, the double bond monomer and water, and performing electron beam irradiation to obtain gel; the polymer comprises one or more of polyvinyl alcohol, polyvinylpyrrolidone, polystyrene and polyacrylonitrile; the double bond monomer comprises acrylonitrile and bisOne or more of vinylbenzene, styrene, acrylic acid, acrylamide, butadiene, pentadiene, and triallyl isocyanurate; b) mixing the gel with acrylonitrile, and performing electron beam irradiation to obtain a graft cross-linked body; c) and mixing the grafted cross-linked body with hydroxylamine for reaction to obtain the uranyl adsorbing material. According to the invention, the low-cost plant fiber is used as a skeleton raw material of the adsorption material, the plant fiber is firstly mixed with the polymer and the double-bond monomer for electron beam irradiation, and the activity of hydroxyl in the fiber is improved through electron beam irradiation, so that the plant fiber, the double-bond monomer and the high-molecular polymer can form a spongy gel full of a large number of holes; then mixing the gel with acrylonitrile for reaction to obtain a cross-linked body grafted with an acrylonitrile group so as to improve the performance of the gel; and finally, mixing the cross-linked body and hydroxylamine for reaction to make the cross-linked body have amidoxime group. The adsorbing material provided by the invention has a very large specific surface area, and can provide extremely high physical adsorption holes and a large amount of chemical ion exchange space; meanwhile, amidoxime groups in the adsorbing material can selectively adsorb uranyl ions, so that the adsorbing material has high adsorption rate and good adsorption selectivity on the uranyl ions. The adsorbing material provided by the invention can play double roles of physical adsorption and chemical ion exchange, so that uranyl ions can be efficiently fixed on the inner surface and the outer surface of the material body. In addition, the adsorbing material provided by the invention has high strength, is beneficial to elution and repeated use of uranyl ions, and shows good use stability. The experimental results show that: the apparent density of the adsorbing material with the particle size of 30-80 meshes provided by the embodiment of the invention is 0.4-0.6 g/cm3The inside of the adsorbing material particles is filled with holes, so that the specific surface area is large; preparing a solution containing 0.9mg/L uranium ions, adsorbing for 2 weeks under a static condition by using the adsorbing material provided by the embodiment, and determining that the adsorption capacity is more than 4.1mg/g after elution; a solution containing 10mg/L uranium ions is prepared, the adsorbing material provided by the embodiment is used for adsorbing for one day under a static condition, the adsorption amount is determined to be more than 23mg/g after elution, the adsorption amount of the adsorbing material after elution for the third time is more than 85%, and the repeated utilization rate of the adsorbing material is high.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a digital photograph of the uranyl adsorbing material provided in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a uranyl adsorbing material which is prepared by the following method:
a) mixing the fiber, the polymer, the double bond monomer and water, and performing electron beam irradiation to obtain gel;
the polymer comprises one or more of polyvinyl alcohol, polyvinylpyrrolidone, polystyrene and polyacrylonitrile;
the double-bond monomer comprises one or more of acrylonitrile, divinyl benzene, styrene, acrylic acid, acrylamide, butadiene, pentadiene and triallyl isocyanurate;
b) mixing the gel with acrylonitrile, and performing electron beam irradiation to obtain a graft cross-linked body;
c) and mixing the grafted cross-linked body with hydroxylamine for reaction to obtain the uranyl adsorbing material.
In the present invention, the fiber, polymer, double bond monomer and water are first mixed. Wherein the fibers include, but are not limited to, one or more of straw fibers, cotton fibers, bamboo fibers, bagasse fibers, and wood pulp fibers; the fineness of the fiber is preferably more than or equal to 30 meshes, and more preferably more than or equal to 40 meshes; the ash content of the fibers is preferably less than or equal to 2 wt%; the polymer comprises one or more of polyvinyl alcohol, polyvinylpyrrolidone, polystyrene and polyacrylonitrile; the polyvinyl alcohol preferably comprises one or more of polyvinyl alcohol 1799, polyvinyl alcohol 2099, polyvinyl alcohol 1788 and polyvinyl alcohol 1792; the polyvinylpyrrolidone preferably comprises polyvinylpyrrolidone k 90; the number average molecular weight of the polystyrene is preferably 10000-50000; the number average molecular weight of the polyacrylonitrile is preferably equal to or more than 10000. In one embodiment provided by the present invention, the polystyrene is a polystyrene emulsion, and the solid content of the polystyrene emulsion is preferably 20 to 40 wt%, and specifically may be 30 wt%. In one embodiment provided by the invention, the polymer comprises polyvinyl alcohol and polystyrene emulsion, and the mass ratio of the polyvinyl alcohol to the polystyrene emulsion is preferably (80-120): (8-12), more preferably 100: 10. In the present invention, the double bond monomer includes one or more of acrylonitrile, divinylbenzene, styrene, acrylic acid, acrylamide, butadiene, pentadiene, and triallyl isocyanurate. In one embodiment provided by the invention, the double-bond monomer comprises styrene and acrylonitrile, and the mass ratio of the styrene to the acrylonitrile is preferably (10-30): (0.5 to 1.5), more preferably 20: 0.9; in another embodiment provided by the invention, the double-bond monomer comprises acrylonitrile, divinylbenzene and styrene, and the mass ratio of the acrylonitrile to the divinylbenzene to the styrene is preferably (1-1.5): (0.1-0.3): (2-6), more preferably 1.2:0.2: 4. In the invention, the mass ratio of the fiber, the polymer, the double-bond monomer and the water is preferably (10-20): (100-150): (3-30): (400-600), more preferably (11-18): (110-140): (5-21): (500-600), most preferably (11-17): (110-130): (5.4-20.9): (500-600), specifically 17:130:20.9:500, 13:110:5.4:50 or 11:130:20.9: 60. In the invention, the mixed system preferably further comprises fatty alcohol-polyoxyethylene ether; the grade of the fatty alcohol-polyoxyethylene ether preferably comprises AEO-3 and/or AEO-9; the mass ratio of the fatty alcohol-polyoxyethylene ether to the water is preferably (0.1-1): (400-600), more preferably 0.5: (500-600). In the present invention, isopropyl alcohol is preferably further included in the mixed system; the mass ratio of the isopropanol to the water is preferably (5-15): (400-600), more preferably (10-12): (500-600). And (3) after the materials are uniformly mixed, carrying out electron beam irradiation. The dose of the electron beam irradiation is preferably 100-200 kGy, and specifically can be 100kGy, 110kGy, 120kGy, 130kGy, 140kGy, 150kGy, 160kGy, 170kGy, 180kGy, 190kGy or 200 kGy. After irradiation, a gel is formed.
After obtaining the gel, the gel is mixed with acrylonitrile. The mass ratio of the gel to the acrylonitrile is preferably (7-15): (1-2), more preferably 10: (1.2-1.8), specifically 10:1.2, 10:1.5 or 10: 1.8. In the present invention, in order to sufficiently mix the gel with the acrylonitrile, it is preferable to cut the gel into colloidal particles and then mix the colloidal particles with the acrylonitrile. And (4) uniformly mixing the gel with acrylonitrile, and then performing electron beam irradiation. The electron beam irradiation dose is preferably 40-80 kGy, and the electron beam irradiation dose can be 40kGy, 45kGy, 50kGy, 55kGy, 60kGy, 65kGy, 70kGy, 75kGy or 80 kGy. After the irradiation is finished, a graft cross-linked body is formed. In the invention, the acrylonitrile is grafted to the fiber gel, so that the grafting amount and the grafting efficiency of the acrylonitrile of the fiber gel are increased, and the adsorbing material can have both good adsorbability and strong selectivity. .
After the graft cross-linked body is obtained, the graft cross-linked body is mixed with hydroxylamine. Wherein, the hydroxylamine is preferably hydroxylamine hydrochloride; the mass ratio of the hydroxylamine to the raw materials for preparing the graft cross-linked body, namely the gel, is preferably (3-6): (7-15), more preferably (4-4.8): 10, and more specifically 4:10, 4.5:10 or 4.8: 10. The graft cross-linked material is mixed with hydroxylamine and reacted. Wherein the reaction temperature is preferably 60-90 ℃, and specifically can be 60, 70, 80 or 90 ℃; the reaction time is preferably 5-8 h, and specifically can be 5, 6, 7 or 8 h. And obtaining the uranyl adsorbing material after the reaction is finished.
According to the invention, the low-cost plant fiber is used as a skeleton raw material of the adsorption material, the plant fiber is firstly mixed with the polymer and the double-bond monomer for electron beam irradiation, and the activity of hydroxyl in the fiber is improved through electron beam irradiation, so that the plant fiber, the double-bond monomer and the high-molecular polymer can form a spongy gel full of a large number of holes; then mixing the gel with acrylonitrile for reaction to obtain a cross-linked body grafted with an acrylonitrile group so as to improve the performance of the gel; and finally, mixing the cross-linked body and hydroxylamine for reaction to make the cross-linked body have amidoxime group. The adsorbing material provided by the invention has a very large specific surface area, and can provide extremely high physical adsorption holes and a large amount of chemical ion exchange space; meanwhile, amidoxime groups in the adsorbing material can selectively adsorb uranyl ions, so that the adsorbing material has high adsorption rate and good adsorption selectivity on the uranyl ions. The adsorbing material provided by the invention can play double roles of physical adsorption and chemical ion exchange, so that uranyl ions can be efficiently fixed on the inner surface and the outer surface of the material body. In addition, the adsorbing material provided by the invention has high strength, is beneficial to elution and repeated use of uranyl ions, and shows good use stability.
In addition, the synthesis method provided by the invention has the advantages of simple process, quick production, low cost, short irradiation reaction time, accurate and controllable absorbed dose, and is very suitable for large-scale production.
The experimental results show that: the apparent density of the adsorbing material with the particle size of 30-80 meshes provided by the embodiment of the invention is 0.4-0.6 g/cm3The inside of the adsorbing material particles is filled with holes, so that the specific surface area is large; preparing a solution containing 0.9mg/L uranium ions, adsorbing for 2 weeks under a static condition by using the adsorbing material provided by the embodiment, and determining that the adsorption capacity is more than 4.1mg/g after elution; a solution containing 10mg/L uranium ions is prepared, the adsorbing material provided by the embodiment is used for adsorbing for one day under a static condition, the adsorption amount is determined to be more than 23mg/g after elution, the adsorption amount of the adsorbing material after elution for the third time is more than 85%, and the repeated utilization rate of the adsorbing material is high.
The invention also provides application of the adsorption material synthesized by the method in the technical scheme in uranium extraction from seawater. In the application provided by the invention, the adsorption material is used for adsorbing uranyl in seawater, so that uranium extraction in seawater is realized.
For the sake of clarity, the following examples are given in detail.
Example 1
(1) Putting 17 parts by weight of straw fiber (the fineness is more than or equal to 30 meshes and the ash content is less than or equal to 2 wt%) into a mixing tank, adding 500 parts by weight of clear water, 130 parts by weight of polyvinyl alcohol (brand 1799), 20 parts by weight of styrene, 0.9 part by weight of acrylonitrile, 0.5 part by weight of fatty alcohol-polyoxyethylene ether (brand AEO-3) and 10 parts by weight of isopropanol, and uniformly stirring;
(2) feeding the feed liquid prepared in the step (1) to an electron beam for irradiation, so that the absorption dose of the feed liquid reaches 110kGy, and obtaining the gel sheet;
(3) shearing the gel plate obtained in the step (2) into colloidal particles by a cutting machine;
(4) adding 10 parts by weight of the particles obtained in the step (3) into 1.5 parts by weight of acrylonitrile, uniformly mixing, and irradiating under electron beams until the irradiation dose reaches 50kGy to obtain a graft cross-linked body;
(5) and (3) adding 4 parts by weight of hydroxylamine hydrochloride into the grafted crosslinking body in the step (4), and controlling the temperature to react for 6 hours at 80 ℃ to obtain the uranyl adsorbing material.
In the embodiment, the particle size of the uranyl adsorbing material finally prepared is controlled to be 30-80 meshes by controlling the size of the colloidal particles in the step (3).
The digital photograph of the uranyl adsorbent obtained as described above is taken, and as a result, fig. 1 is a digital photograph of the uranyl adsorbent provided in example 1 of the present invention.
Example 2
(1) Putting 13 parts by weight of wood pulp fiber (the fineness is more than or equal to 40 meshes and the ash content is less than or equal to 2 wt%) into a mixing tank, adding 500 parts by weight of clear water, 100 parts by weight of polyvinyl alcohol (grade 1788), 10 parts by weight of polystyrene emulsion (solid content is 30 wt%, and the number average molecular weight is about 1 ten thousand), 1.2 parts by weight of acrylonitrile, 0.5 part by weight of fatty alcohol-polyoxyethylene ether (grade AEO-9), 10 parts by weight of isopropanol, 0.2 part by weight of divinylbenzene and 4 parts by weight of styrene, and uniformly stirring;
(2) feeding the feed liquid prepared in the step (1) to an electron beam for irradiation, so that the absorption dose of the feed liquid reaches 140kGy, and obtaining a gel plate;
(3) shearing the gel plate obtained in the step (2) into colloidal particles by a cutting machine;
(4) adding 10 parts by weight of the particles obtained in the step (3) into 1.2 parts by weight of acrylonitrile, uniformly mixing, and irradiating under electron beams until the irradiation dose reaches 65kGy to obtain a graft cross-linked body;
(5) and (3) adding 4.5 parts by weight of hydroxylamine hydrochloride into the grafted crosslinking body in the step (4), and reacting for 7 hours at the temperature of 70 ℃ to obtain the uranyl adsorbing material.
In the embodiment, the particle size of the uranyl adsorbing material finally prepared is controlled to be 30-80 meshes by controlling the size of the colloidal particles in the step (3).
Example 3
(1) Putting 11 parts by weight of straw fiber (the fineness is more than or equal to 30 meshes and the ash content is less than or equal to 2 wt%) into a mixing tank, adding 600 parts by weight of clear water, 130 parts by weight of polyvinyl alcohol (brand 1799), 20 parts by weight of styrene, 0.9 part by weight of acrylonitrile, 0.5 part by weight of fatty alcohol-polyoxyethylene ether (brand AEO-3) and 12 parts by weight of isopropanol, and uniformly stirring;
(2) feeding the feed liquid prepared in the step (1) to an electron beam for irradiation, so that the absorption dose of the feed liquid reaches 100kGy, and obtaining the gel sheet;
(3) shearing the gel plate obtained in the step (2) into colloidal particles by a cutting machine;
(4) adding 10 parts by weight of the particles obtained in the step (3) into 1.8 parts by weight of acrylonitrile, uniformly mixing, and irradiating under electron beams until the irradiation dose reaches 60kGy to obtain a graft cross-linked body;
(5) and (3) adding 4.8 parts by weight of hydroxylamine hydrochloride into the grafted crosslinking body in the step (4), and controlling the temperature to react for 6 hours at 80 ℃ to obtain the uranyl adsorbing material.
In the embodiment, the particle size of the uranyl adsorbing material finally prepared is controlled to be 30-80 meshes by controlling the size of the colloidal particles in the step (3).
Example 4
Performance testing
1) And sequentially carrying out apparent density test on the adsorbing materials prepared in the embodiments 1-3, wherein the results are as follows: 0.4g/cm3、0.5g/cm3、0.6g/cm3。
2) And preparing a uranium ion-containing 0.9mg/L solution, sequentially adsorbing for 2 weeks at room temperature under a static condition by using the adsorbing materials provided in the embodiments 1-3, and determining that the adsorption amounts of the solution after elution respectively reach 4.1mg/g, 4.3mg/g and 4.7 mg/g.
3) Preparing a uranium ion-containing 10mg/L solution, sequentially adsorbing for one day at room temperature under a static condition by using the adsorbing materials provided in the embodiments 1-3, and determining that the adsorption amounts reach 23mg/g, 25mg/g and 29mg/g after elution; the adsorption amounts of the adsorption materials after the third elution are respectively 85.0%, 85.2% and 85.3% of the original adsorption amount.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A synthetic method of a uranyl adsorbing material comprises the following steps:
a) mixing the fiber, the polymer, the double-bond monomer and water, and performing electron beam irradiation with the dose of 100-200 kGy to obtain gel;
the fiber comprises one or more of straw fiber, cotton fiber, bamboo fiber, bagasse fiber and wood pulp fiber, and the fineness of the fiber is more than or equal to 30 meshes;
the polymer comprises one or more of polyvinyl alcohol, polyvinylpyrrolidone, polystyrene and polyacrylonitrile;
the double-bond monomer comprises one or more of acrylonitrile, divinyl benzene, styrene, acrylic acid, acrylamide, butadiene, pentadiene and triallyl isocyanurate;
the mass ratio of the fibers, the polymer, the double-bond monomer and the water is (10-20): (100-150): (3-30): (400-600);
b) mixing the gel with acrylonitrile, and performing electron beam irradiation with the dosage of 40-80 kGy to obtain a graft cross-linked body;
c) mixing the grafted cross-linked body with hydroxylamine for reaction to obtain a uranyl adsorbing material;
the reaction temperature is 60-90 ℃, and the reaction time is 5-8 h.
2. The synthesis method according to claim 1, wherein in the step b), the mass ratio of the gel to the acrylonitrile is (7-15): (1-2).
3. The synthesis method according to claim 1, wherein the mass ratio of hydroxylamine to the raw material for preparing the graft cross-linked body, namely gel, is (3-6): (7-15).
4. Use of the adsorbing material synthesized by the method of any one of claims 1 to 3 in uranium extraction from seawater.
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| CN201710630192.8A CN107349919B (en) | 2017-07-28 | 2017-07-28 | Synthetic method and application of uranyl adsorbing material |
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| CN201710630192.8A CN107349919B (en) | 2017-07-28 | 2017-07-28 | Synthetic method and application of uranyl adsorbing material |
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| CN107349919B true CN107349919B (en) | 2020-03-27 |
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| CN109012626B (en) * | 2018-08-03 | 2021-07-02 | 中国科学院上海应用物理研究所 | Method for improving selective adsorption efficiency of uranyl ions |
| CN109482159B (en) * | 2018-12-03 | 2021-06-15 | 中广核达胜加速器技术有限公司 | Amidoxime composite fiber and preparation method thereof |
| CN113274990A (en) * | 2020-09-18 | 2021-08-20 | 董晓明 | Adsorbent for removing antimony in printing and dyeing wastewater |
| CN112121777B (en) * | 2020-09-29 | 2021-05-14 | 哈尔滨工程大学 | Preparation method of graded porous anti-pollution type uranium extraction from seawater hydrogel membrane |
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