Preparation method of uranium-adsorbing strongly-basic resin with narrow distribution particle size

文档序号：101906 发布日期：2021-10-15 浏览：34次中文

阅读说明：本技术 吸附铀的窄分布粒径强碱性树脂的制备方法 (Preparation method of uranium-adsorbing strongly-basic resin with narrow distribution particle size ) 是由李默陈树森宿延涛王库王凤菊宋艳勾阳飞王海珍常华李子明于 2021-07-23 设计创作，主要内容包括：本发明公开了一种吸附铀的窄分布粒径强碱性树脂的制备方法。该制备方法包括如下步骤：(1)在多层斜叶桨式搅拌器的搅拌作用下,向包括有机分散剂、无机分散剂和水的分散相中加入包括苯乙烯、二乙烯苯、引发剂和致孔剂的有机相,然后进行聚合反应,得到苯乙烯-二乙烯苯共聚物；其中,所述多层斜叶桨式搅拌器的桨叶向下倾斜设置；所述有机分散剂选自聚乙烯醇或明胶中的一种；所述无机分散剂选自高岭土、聚磷酸钠或六偏磷酸铵和碳酸钙的组合物中的一种；(2)将苯乙烯-二乙烯苯共聚物依次进行氯甲基化和三甲胺胺化,得到强碱性树脂。本发明方法制备得到的强碱性树脂对铀的吸附容量高。(The invention discloses a preparation method of uranium adsorption resin with strong basicity and narrow particle size distribution. The preparation method comprises the following steps: (1) under the stirring action of a multilayer inclined blade paddle type stirrer, adding an organic phase comprising styrene, divinylbenzene, an initiator and a pore-foaming agent into a dispersed phase comprising an organic dispersant, an inorganic dispersant and water, and then carrying out polymerization reaction to obtain a styrene-divinylbenzene copolymer; wherein blades of the multilayer inclined blade paddle type stirrer are arranged in a downward inclined mode; the organic dispersant is selected from one of polyvinyl alcohol or gelatin; the inorganic dispersant is selected from one of kaolin, sodium polyphosphate or a composition of ammonium hexametaphosphate and calcium carbonate; (2) and (3) carrying out chloromethylation and trimethylamine amination on the styrene-divinylbenzene copolymer in sequence to obtain the strong-alkaline resin. The strong-basicity resin prepared by the method has high uranium adsorption capacity.)

1. A preparation method of uranium adsorption strongly-basic resin with narrow distribution particle size is characterized by comprising the following steps:

(1) adding an organic phase comprising 10-40 parts by weight of styrene, 0.5-7 parts by weight of divinylbenzene, 0.1-3 parts by weight of an initiator and 7-30 parts by weight of a pore-forming agent into a dispersed phase comprising 0.5-10 parts by weight of an organic dispersant, 0.5-10 parts by weight of an inorganic dispersant and 20-80 parts by weight of water under the stirring action of a multilayer inclined blade paddle stirrer, and then carrying out polymerization reaction to obtain a styrene-divinylbenzene copolymer;

blades of the multilayer inclined blade paddle type stirrer are arranged in a downward inclined mode, and an included angle between each blade and the stirring shaft is 30-55 degrees; the organic dispersant is selected from one of polyvinyl alcohol or gelatin; the inorganic dispersant is selected from one of kaolin, sodium polyphosphate or a composition of ammonium hexametaphosphate and calcium carbonate;

(2) and (3) carrying out chloromethylation and trimethylamine amination on the styrene-divinylbenzene copolymer in sequence to obtain the uranium-adsorbed strong-base resin with narrow distribution particle size.

2. The method according to claim 1, wherein the organic dispersant and the inorganic dispersant are selected from one of the following combinations:

(A) the organic dispersant is polyvinyl alcohol, and the inorganic dispersant is kaolin;

(B) the organic dispersant is gelatin, and the inorganic dispersant is sodium polyphosphate;

(C) the organic dispersant is polyvinyl alcohol, and the inorganic dispersant is a composition of ammonium hexametaphosphate and calcium carbonate.

3. The method according to claim 1, wherein the organic phase is added to the dispersed phase in a single addition or dropwise by a peristaltic pump.

4. The method of claim 1, further comprising the step of preparing a dispersed phase:

dissolving a dispersion phase raw material comprising 0.5-10 parts by weight of an organic dispersant, 0.5-10 parts by weight of an inorganic dispersant and 20-80 parts by weight of water under the stirring action of a multi-layer inclined blade paddle stirrer to obtain a dispersion phase;

5. The method according to claim 1, wherein the polymerization is carried out at 60 to 85 ℃ for 1 to 4 hours; and then preserving heat for 2-6 h at 87-100 ℃, and naturally cooling to 30-60 ℃.

6. The preparation method according to claim 1, wherein the porogen is selected from one or more of toluene, isooctane, xylene and benzene, and the initiator is selected from one of benzoyl peroxide or azobisisobutyronitrile.

7. The production method according to claim 1, wherein in the step (1), the reaction product obtained by the polymerization reaction is subjected to filtration and water washing to obtain a solid reactant; and (3) boiling the solid reactant in water, filtering and drying to obtain the styrene-divinylbenzene copolymer.

8. The method of claim 1, wherein the chloromethylation comprises the steps of:

swelling the styrene-divinylbenzene copolymer in chloromethyl ether for 0.5-5 h, and then adding a catalyst for reacting for 17-30 h to obtain a chloromethylated styrene-divinylbenzene copolymer;

wherein the catalyst is selected from one of ferric chloride, zinc chloride and aluminum chloride.

9. The method of claim 1, wherein the trimethylamine amination comprises the steps of:

swelling the chloromethylated styrene-divinylbenzene copolymer in an alcohol solution for 0.5-5 h, then dropwise adding a trimethylamine aqueous solution, and reacting for 5-10 h at 20-38 ℃ after dropwise adding.

10. The method according to any one of claims 1 to 9, further comprising the following steps after trimethylamine amination:

transforming the styrene-divinylbenzene copolymer subjected to trimethylamine amination by adopting a hydrochloric acid aqueous solution to obtain a transformed polymer; and screening the transformed polymer to obtain the uranium-adsorbing resin with strong basicity and narrow distribution particle size.

Technical Field

The invention relates to a preparation method of uranium adsorption resin with strong basicity and narrow particle size distribution.

Background

Uranium is the most common radionuclide contaminant in nature, and mining, chemical refining, concentration and other nuclear-related activities may involve radionuclide contaminants. The removal and enrichment of uranium is of great concern. The common methods for removing and enriching uranium at present comprise a precipitation method, an adsorption method, a liquid-liquid extraction method, a half-wave rectification alternating current electrochemical method and the like. Among them, the adsorption method has the advantages of simple operation, low cost, large-scale application and the like, and is widely applied.

CN101139418A discloses a levextrel resinThe preparation method comprises the steps of uniformly mixing styrene and a cross-linking agent divinylbenzene, then adding an initiator, an amide compound extracting agent, a diluent and a pore-forming agent, and uniformly stirring at room temperature to prepare an oil phase; adding a dispersing agent, a dispersion aid agent and a surfactant into water to prepare a dispersed phase; and adding the oil phase into the dispersed phase, stirring for dispersion, heating for polymerization, cooling after the reaction is finished, and sequentially washing, filtering and drying to obtain the extraction resin particles. The initiator is benzoyl peroxide or azodiisobutyronitrile; the diluent is any one or two of kerosene, n-octanol, n-octane, chloroform, toluene, benzyl alcohol and n-dodecane; the pore-forming agent is any one or two of toluene, n-heptane and liquid paraffin; the dispersing agent is selected from any one of gelatin, polyacrylic acid, polymethyl methacrylate salt, maleic anhydride-styrene copolymer, methylcellulose, hydroxypropyl cellulose, sodium alginate or polyvinyl alcohol; the auxiliary dispersing agent is any one of magnesium carbonate, calcium phosphate, talcum powder, basic magnesium carbonate particles or calcium hydroxy phosphate; the surfactant is selected from sodium dodecyl sulfonate, sodium dodecyl sulfate or sodium dodecyl benzene sulfonate. The method prepares the levextrel resin, namely the para-Sr²⁺Has good adsorption capacity, but has weak adsorption performance on uranium.

CN111040065A discloses a method for preparing a solvent-free gel type styrene cation exchange resin, which comprises: uniformly stirring styrene, divinylbenzene, a third monomer and an initiator to obtain an oil phase; uniformly mixing polyvinyl alcohol, sodium chloride and water, adding an oil phase, and reacting to obtain white balls; and (3) carrying out sulfonation reaction on the white balls and sulfuric acid, and obtaining the solvent-free gel type styrene cation exchange resin after the reaction is finished. The method requires introducing a third monomer; the dispersing agent is selected from polyvinyl alcohol and sodium chloride, and the dispersing effect of the dispersing agent on styrene and divinyl benzene monomers is not good; the cation exchange resin has strong ability to process calcium, magnesium and other ions in water, but is not ideal enough for processing uranium.

CN105399888A discloses a preparation method of uranium absorption resin. The method comprises the following steps: (1) adding styrene, divinylbenzene and an initiator into a styrene-divinylbenzene polymer with low crosslinking degree to obtain an oil phase; then adding a dispersion phase containing water, polyvinyl alcohol and gelatin into the oil phase to obtain gel type polystyrene-divinylbenzene white spheres; (2) preparing chloromethyl ether by adopting an in-situ synthesis method, and chloromethylating gel type polystyrene-divinylbenzene white spheres; (3) and (3) aminating the gel type polystyrene-divinylbenzene white spheres subjected to chloromethylation to obtain the uranium absorption resin. In the method, polyvinyl alcohol and gelatin are used as dispersing agents, so that the dispersing effect is poor; the disperse phase is added into the oil phase, so that the dispersion of the monomers is not facilitated, ion agglomeration is easily caused, the particle size of the obtained resin is influenced, and the adsorption effect of the resin on uranium is influenced.

Disclosure of Invention

In view of the above, the present invention aims to provide a method for preparing a uranium-adsorbing resin with a strong basicity and a narrow particle size distribution. The strong-base resin obtained by the method has high adsorption capacity to uranium.

The technical purpose is achieved through the following technical scheme.

The invention provides a preparation method of uranium adsorption resin with strong basicity and narrow particle size distribution, which comprises the following steps:

According to the preparation method of the present invention, preferably, the organic dispersant and the inorganic dispersant are selected from one of the following combinations:

(A) the organic dispersant is polyvinyl alcohol, and the inorganic dispersant is kaolin;

(B) the organic dispersant is gelatin, and the inorganic dispersant is sodium polyphosphate;

(C) the organic dispersant is polyvinyl alcohol, and the inorganic dispersant is a composition of ammonium hexametaphosphate and calcium carbonate.

According to the preparation method of the present invention, preferably, the organic phase is added to the dispersed phase in a one-time addition manner or in a dropwise manner by using a peristaltic pump.

The preparation method according to the present invention preferably further comprises the step of preparing a dispersed phase:

According to the preparation method of the invention, preferably, the polymerization reaction is firstly carried out for 1-4 hours at 60-85 ℃; and then preserving heat for 2-6 h at 87-100 ℃, and naturally cooling to 30-60 ℃.

According to the preparation method of the present invention, preferably, the porogen is selected from one or more of toluene, isooctane, xylene and benzene, and the initiator is selected from one of benzoyl peroxide or azobisisobutyronitrile.

According to the preparation method of the present invention, preferably, the reaction product obtained from the polymerization reaction is filtered and washed with water to obtain a solid reactant; and (3) boiling the solid reactant in water, filtering and drying to obtain the styrene-divinylbenzene copolymer.

According to the preparation method of the present invention, preferably, the chloromethylation comprises the following steps:

swelling the styrene-divinylbenzene copolymer in chloromethyl ether for 0.5-5 h, and then adding a catalyst for reacting for 17-30 h to obtain a chloromethylated styrene-divinylbenzene copolymer;

wherein the catalyst is selected from one of aluminum chloride, zinc chloride and ferric chloride.

According to the preparation method of the present invention, preferably, the trimethylamine amination comprises the steps of:

According to the preparation method of the invention, the method preferably further comprises the following steps after the amination of trimethylamine:

According to the invention, the specific inorganic dispersant and organic dispersant are adopted to act synergistically, so that the particle size distribution of organic beads is more uniform, the organic beads are more stable, and the adhesion of microspheres in the polymerization process is reduced; the multi-layer inclined blade paddle type stirrer is adopted, and the arrangement of the blades is beneficial to enabling the organic phase to generate turbulence in the dispersed phase under the action of stirring shearing force, so that the stirring strength is more uniform, and the organic droplets are stable and not adhered; this helps to increase the adsorption capacity of the strongly basic resin for uranium. According to the preferable technical scheme of the invention, the peristaltic pump is adopted to dropwise add the organic phase into the dispersed phase, so that the reaction is more stable, the uniformity of the resin structure is improved, the structure of a reaction product is more stable, and the adsorption capacity of the strong basic resin to uranium is improved.

Detailed Description

The present invention is described in more detail below, but the present invention is not limited thereto.

The resin with strong basicity and narrow particle size distribution for adsorbing uranium in the invention means that the resin has strong basicity and the particle size distribution of resin particles is narrow, and uranium can be adsorbed. Strong basicity is a term commonly used in the art and is therefore clear. Narrow particle size distribution is also a term commonly used in the art and is therefore clear. For example, the particle size is 0.5 to 1.0 mm. The uranium adsorbing narrow distribution particle size strong base resin can also be called as ion exchange resin.

The preparation method comprises the following steps: (1) a step of polymerization; (2) chloromethylation; (3) and (3) aminating trimethylamine. In certain embodiments, one or more of the steps of preparing the dispersed phase, transforming, and sieving are also included. The details are as follows.

< step of polymerization reaction >

Under the stirring action of a multilayer inclined blade paddle type stirrer, an organic phase comprising styrene, divinylbenzene, an initiator and a pore-foaming agent is added into a dispersed phase comprising an organic dispersant, an inorganic dispersant and water, and then a polymerization reaction is carried out to obtain the styrene-divinylbenzene copolymer.

The blades of the multi-layer inclined blade paddle type stirrer are arranged downwards. The included angle between the paddle and the stirring shaft is 30-55 degrees; preferably 35-50 degrees; more preferably 40 to 50 degrees. So can make the organic phase produce the torrent in the dispersed phase, stir slightly more evenly, organic droplet is stable not adhesion, improves the adsorption capacity of resin to uranium. The number of the layers of the blades of the multilayer inclined blade type stirrer can be more than two, and preferably 2-5. Therefore, the adsorption capacity of the resin to uranium can be guaranteed to be improved, the stirrer is low in cost, and the energy consumption is low.

The stirring speed of the multilayer inclined blade paddle type stirrer is 80-300 rpm; preferably, the stirring speed is 100-250 rpm; more preferably 220 to 250 rpm. This helps to better disperse the organic phase in the dispersed phase and to increase the adsorption capacity of the resin for uranium.

In the present invention, the dispersed phase includes an organic dispersant, an inorganic dispersant and water. In certain embodiments, the dispersed phase is comprised of an organic dispersant, an inorganic dispersant, and water. The organic dispersant is selected from one of polyvinyl alcohol or gelatin. The inorganic dispersant is one selected from kaolin, sodium polyphosphate, sodium hexametaphosphate and calcium carbonate. The water may be deionized water. Preferably, the organic and inorganic dispersants are selected from one of the combinations shown below: (A) the organic dispersant is polyvinyl alcohol, and the inorganic dispersant is kaolin; (B) the organic dispersant is gelatin, and the inorganic dispersant is sodium polyphosphate; (C) the organic dispersant is polyvinyl alcohol, and the inorganic dispersant is a composition of ammonium hexametaphosphate and calcium carbonate. More preferably, the organic dispersant is polyvinyl alcohol and the inorganic dispersant is a combination of ammonium hexametaphosphate and calcium carbonate. The organic dispersing agent and the inorganic dispersing agent have synergistic effect, so that organic beads can be more stable, the adhesion of microspheres in the polymerization process is reduced, and the adsorption quantity of resin to uranium is improved.

In the invention, the amount of water is 20-80 parts by weight; preferably 50 to 75 parts by weight; more preferably 62 to 70 parts by weight. The using amount of the organic dispersant is 0.5-10 parts by weight; preferably 1 to 5 parts by weight; more preferably 1 to 1.5 parts by weight. The using amount of the inorganic dispersant is 0.5-10 parts by weight; preferably 2 to 7 parts by weight; more preferably 3.5 to 5 parts by weight. When the inorganic dispersant is a composition of ammonium hexametaphosphate and calcium carbonate, the mass ratio of the ammonium hexametaphosphate to the calcium carbonate can be 0.5-2: 1; preferably 0.7-1.5: 1; more preferably 1:1. Such amounts enable better synergy of the inorganic dispersant and the organic dispersant, and better dispersion of the organic phase of the invention.

According to one embodiment of the invention, the dispersed phase consists of 65 parts by weight of water, 1 part by weight of polyvinyl alcohol, 2 parts by weight of calcium carbonate and 2 parts by weight of ammonium hexametaphosphate.

In the invention, the organic phase can be added into the dispersed phase in a one-time adding mode, and the organic phase can also be added into the dispersed phase in a dropping mode by a peristaltic pump. Preferably, the organic phase is added to the dispersed phase by means of a peristaltic pump in a uniform and continuous dropwise manner. The dropping time of the peristaltic pump can be 0.5-2 h; preferably 0.8 to 1.5 hours. And the peristaltic pump is adopted to dropwise add the organic phase, so that the reaction is more stable, the structure of the reaction product is more stable, and the improvement of the adsorption quantity of the resin to uranium is facilitated.

And when the temperature of the dispersed phase is 40-85 ℃, adding an organic phase into the dispersed phase. Preferably, the organic phase is added to the dispersed phase when the temperature of the dispersed phase is 60 to 80 ℃. More preferably, when the temperature of the dispersed phase is 70 to 80 ℃, the organic phase is added to the dispersed phase.

The organic phase comprises styrene, divinylbenzene, an initiator and a pore-foaming agent. In certain embodiments, the organic phase consists of styrene, divinylbenzene, an initiator, and a porogen.

In the invention, the dosage of the styrene is 10-40 parts by weight; preferably 20 to 35 parts by weight; more preferably 28 to 35 parts by weight.

In the invention, the amount of divinylbenzene can be 0.5 to 7 parts by weight; preferably 2 to 7 parts by weight; more preferably 4 to 6 parts by weight.

In the present invention, the initiator may be selected from one of benzoyl peroxide or azobisisobutyronitrile. In certain embodiments, the initiator is benzoyl peroxide. The amount of the initiator can be 0.1-3 parts by weight; preferably 0.2 to 1.5 parts by weight; more preferably 0.3 to 1 part by weight.

In the invention, the amount of the pore-foaming agent can be 7-30 parts by weight; preferably 10 to 25 parts by weight; more preferably 13 to 20 parts by weight. The porogen may be selected from one or more of toluene, isooctane, benzene or xylene. Preferably, the porogen is selected from one of the compositions shown below: (I) toluene and isooctane; (II) benzene and xylene; (III) isooctane and xylene. More preferably, the porogens are isooctane and xylene. The weight ratio of the toluene to the isooctane can be 3-5: 1. The weight ratio of benzene to xylene can be 2-3: 1. The weight ratio of isooctane to xylene can be 1: 3-5; preferably 1: 4.

The organic phase of the invention can be better dispersed in the dispersed phase of the invention by adopting the composition, thereby improving the adsorption amount of uranium by the resin.

The polymerization reaction is carried out for 1-4 hours at 60-85 ℃ (second temperature); and then preserving heat for 2-6 h at 87-100 ℃, and naturally cooling to 30-60 ℃. Preferably, the polymerization reaction is firstly carried out for 2-3 hours at 70-80 ℃ (second temperature); and then preserving heat at 90-95 ℃ for 3-5 h, and naturally cooling to 40-50 ℃.

When the temperature of the polymerization reaction system is lower than the second temperature, the temperature needs to be raised. The heating rate can be 0.5-3 ℃/min; preferably 0.5-2 ℃/min; more preferably 0.8 to 1.5 ℃/min.

The polymerization reaction can also comprise the following steps: filtering and washing a reaction product obtained by the polymerization reaction to obtain a solid reactant; and (3) boiling the solid reactant in water, filtering and drying to obtain the styrene-divinylbenzene copolymer. The filtration, water washing, water boiling, suction filtration and drying are carried out by methods commonly used in the field, and are not described herein again. The water boiling time can be 1-10 h; preferably 2-6 h.

< Chloromethylation step >

Swelling the styrene-divinylbenzene copolymer in chloromethyl ether, and then adding a catalyst for reaction to obtain the chloromethylated styrene-divinylbenzene copolymer.

In the invention, the mass ratio of the styrene-divinylbenzene copolymer to the chloromethyl ether can be 1: 1-5; preferably 1: 1-3; more preferably 1: 1.5.

The swelling time of the styrene-divinylbenzene copolymer in the chloromethyl ether can be 0.5-5 h; preferably 1-4 h; more preferably 1-2 h.

The catalyst can be selected from one of aluminum chloride, zinc chloride and ferric chloride. Preferably, the catalyst is selected from one of aluminum chloride or zinc chloride. More preferably, the catalyst is zinc chloride. The dosage of the catalyst can be 0.1-1 time of the weight of the styrene-divinylbenzene copolymer; preferably 0.3 to 0.7 times; more preferably 0.5 times.

The reaction temperature of the styrene-divinylbenzene copolymer and the chloromethyl ether can be 30-65 ℃; preferably 40-60 ℃; more preferably 45 to 55 ℃. The reaction time can be 12-36 h; preferably 18-30 h; more preferably 20 to 27 hours.

< step of trimethylamine amination >

Swelling chloromethylated styrene-divinylbenzene copolymer in alcohol solution, then dripping aqueous solution of trimethylamine, and reacting chloromethylated styrene-divinylbenzene copolymer with trimethylamine after finishing dripping.

In the present invention, the alcohol solution may be selected from one of methanol, ethanol, propanol, and isopropanol. Preferably, the alcohol solution is methanol. The swelling time of the chloromethylated styrene-divinylbenzene copolymer in the alcoholic solution can be 0.5-5 h; preferably 1-4 h; more preferably 1.5 to 3 hours.

The mass fraction of trimethylamine in the trimethylamine aqueous solution can be 10-50 wt%; preferably 20 to 40 wt%; more preferably 30 wt%. The dropping speed of the trimethylamine aqueous solution can be 10-100 ml/min; preferably 20-60 ml/min; more preferably 30 ml/min. The dropping time of the trimethylamine aqueous solution can be 15-90 min; preferably 30-60 min; more preferably 45 min.

The reaction temperature of the chloromethylated styrene-divinylbenzene copolymer and trimethylamine can be 20-38 ℃; preferably 20 to 30 ℃. The reaction time can be 5-10 h; preferably 6-8 h.

< step of preparing dispersed phase >

Dissolving water phase raw materials comprising organic dispersant, inorganic dispersant and water under the stirring action of a multilayer inclined blade paddle type stirrer to obtain a dispersed phase. The selection and amounts of the above-mentioned raw materials are as described above.

The blades of the multilayer inclined blade paddle type stirrer are arranged in a downward inclined mode. The included angle between the paddle and the stirring shaft is 30-55 degrees; preferably 35-50 degrees; more preferably 40 to 50 degrees. The stirring speed of the multilayer inclined blade paddle type stirrer is 80-300 rpm; preferably, the stirring speed is 100-250 rpm; more preferably 220 to 250 rpm. This enables the organic dispersant and the inorganic dispersant to be better dissolved in water to form a more uniform dispersed phase.

< transformation and/or screening step >

And (3) transforming the styrene-divinylbenzene copolymer subjected to trimethylamine amination in an HCl solution with the concentration of 0.1-20 wt% to obtain a transformed polymer. Preferably, the concentration of the HCl solution is 5-15 wt%; more preferably, the concentration of the HCl solution is 10 wt%.

The transformed polymer was sieved. Specifically, the transformed polymer is sieved, and the transformed polymer with the particle size of 0.5-1.0 mm is sieved.

Examples 1 to 3 and comparative examples 1 to 3

Uniformly mixing styrene, divinylbenzene, benzoyl peroxide and a pore-foaming agent to obtain an organic phase.

Adding deionized water into a reaction vessel, and adding an organic dispersant and an inorganic dispersant into the deionized water under the stirring action of a multilayer inclined blade paddle type stirrer to dissolve the organic dispersant and the inorganic dispersant to obtain a dispersed phase.

Heating the dispersed phase to a first temperature under the stirring action of a multi-layer inclined blade paddle stirrer, and then adding an organic phase into the dispersed phase; and polymerizing the dispersed phase and the organic phase at 75 deg.C (second temperature), maintaining at 90 deg.C for a period of time, and cooling to 45 deg.C to obtain the reaction product. The reaction product was filtered and washed with water to give a solid reactant. And boiling the solid reactant in boiling water for 4 hours, and then carrying out suction filtration and drying to obtain the styrene-divinylbenzene copolymer.

Wherein, the blades of the double-layer inclined blade paddle type stirrer are arranged in a downward inclined manner, and the included angle between the blades and the stirring shaft is shown in table 1.

Swelling styrene-divinylbenzene copolymer in chloromethyl ether for 1h (the mass ratio of the styrene-divinylbenzene copolymer to the chloromethyl ether is 1:1.5), heating to 50 ℃, adding zinc chloride (the dosage of the zinc chloride is 0.5 time of the weight of the styrene-divinylbenzene copolymer) and reacting for 24h to obtain the chloromethylated styrene-divinylbenzene copolymer.

Swelling chloromethylated styrene-divinylbenzene copolymer in methanol for 2 h; then dropwise adding a trimethylamine aqueous solution (the mass fraction of the trimethylamine is 30 wt%), wherein the dropwise adding time is 45min, and the dropwise adding speed is 30 ml/min; after the dropwise addition, the reaction is carried out for 7 hours at 25 ℃ to obtain the styrene-divinylbenzene copolymer after trimethylamine amination.

And (3) transforming the styrene-divinylbenzene copolymer subjected to trimethylamine amination in an HCl solution with the concentration of 10 wt% to obtain a transformed polymer.

And sieving the transformed polymer, and screening out the transformed polymer with the particle size of 0.5-1.0 mm to obtain the uranium-adsorbing resin with strong basicity and narrow distribution particle size.

Specific parameters are shown in table 1.

TABLE 1

Examples of the experiments

0.1g of the uranium adsorbing narrow-distribution-particle-size strongly basic resin and 201X 7 strongly basic ion exchange resin of examples 1 to 3 and comparative examples 1 to 3 were weighed, respectively, and added to 200ml of a uranium-containing leachate having a uranium concentration of 30mg/l, respectively, and adsorbed in a constant-temperature water bath oscillator, and the uranium content in the adsorbed resin was measured. The results obtained are shown in Table 2.

TABLE 2

The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.

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Preparation method of uranium-adsorbing strongly-basic resin with narrow distribution particle size

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