CN103342769B - A kind of preparation method of molybdenum separation resin - Google Patents
A kind of preparation method of molybdenum separation resin Download PDFInfo
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- CN103342769B CN103342769B CN201310253398.5A CN201310253398A CN103342769B CN 103342769 B CN103342769 B CN 103342769B CN 201310253398 A CN201310253398 A CN 201310253398A CN 103342769 B CN103342769 B CN 103342769B
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- benzoinoxime
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Abstract
The present invention relates to a kind of preparation method of molybdenum separation resin, comprise the following steps: (1) preparation dispersant solution; (2) preparation is containing the organic phase of α-benzoinoxime; (3) styrene-divinylbenzene prepolymer is prepared; (4) synthetic resins: join in dispersant solution by styrene-divinylbenzene prepolymer, stirs and makes it be dispersed into pearl body, after being slowly warming up to 65-70 DEG C; Add the organic phase containing α-benzoinoxime, continue to be warming up to 80-85 DEG C, reaction 10-15 hour, stops heating, Temperature fall; When temperature is down to 40-50 DEG C, filtered by reaction mixture, washing precipitate, dries naturally.Adopt the molybdenum separation resin that the inventive method is obtained, its Stability Analysis of Structures, when extracting for molybdenum, the stability of extraction chromatography is fine, substantially increase the selectivity of α-benzoinoxime to molybdenum, experimental test shows, the saturated adsorption capacity of molybdenum separation resin provided by the invention is every gram of dried resin 36-43mg molybdenum.
Description
Technical field
The invention belongs to molybdenum abstraction technique field, be specifically related to a kind of preparation method of molybdenum separation resin.
Background technology
α-benzoinoxime has special chemical optionally reagent to molybdenum, and traditional using method has two kinds: one is by ethanol in α-benzoinoxime dissolving, mixes with the dissolving containing molybdenum, makes molybdenum form precipitation; Another method is dissolved in by α-benzoinoxime in chloroform or ethyl acetate, fully vibrates, realize the extraction to Microamounts of Mo with the solution containing Microamounts of Mo.In trace analysis, it is desirable to rapidly molybdenum optionally to be separated, often with diatomite or kel-F(chemical name: voltalef) powder is for supporter, and after silanization, by α-benzoinoxime physical adsorption on it, after dry, dress post uses.Extraction chromatography stability prepared by this method is poor, has the phenomenon that molybdenum runs off.Therefore, that develops a kind of stability has special optionally resin syntheses processes to be necessary to molybdenum.
Summary of the invention
For the defect existed in prior art, the object of this invention is to provide a kind of preparation method of molybdenum separation resin, the resin structure adopting the method obtained is stablized, and it is good for extraction chromatography stability during molybdenum extracting and separating.
For reaching above object, the technical solution used in the present invention is: a kind of preparation method of molybdenum separation resin, comprises the following steps:
(1) prepare dispersant solution: under agitation join in deionized water by low-molecular-weight wax class dispersion agent, be warmed up to 45-50 DEG C, make both dissolve completely;
(2) preparation is containing the organic phase of α-benzoinoxime: joined by α-benzoinoxime in organic solvent, stirs and α-benzoinoxime is dissolved, then add tackifier, ultrasonic disperse 30-40 minute;
(3) styrene-divinylbenzene prepolymer is prepared: vinylbenzene, Vinylstyrene and initiator are mixed, stir, be warming up to 65-70 DEG C, make reactant generation prepolymerization reaction 30-40 minute, obtain styrene-divinylbenzene prepolymer;
(4) synthetic resins: the styrene-divinylbenzene prepolymer that step (3) obtains is joined in the dispersant solution that step (1) obtains, stir and make it be dispersed into pearl body, after being slowly warming up to 65-70 DEG C; In gained mixture, add the organic phase containing α-benzoinoxime that step (2) obtains, continue to be warming up to 80-85 DEG C, react 10-15 hour at this temperature, stop heating, Temperature fall; When temperature is down to 40-50 DEG C, reaction mixture is filtered, washes throw out with water, naturally dry, obtain the synthetic resins containing α-benzoinoxime.
In the inventive method, (1), (2), (3) step in no particular order order.
Further, in step (1), described low-molecular-weight wax class dispersion agent is selected from the one in polyvinyl alcohol, oxidic polyethylene alcohol or polymaleic acid; The concentration of dispersant solution is 1.5-2wt%.
Further again, described dispersion agent is polyvinyl alcohol.
Further, in step (2), described organic solvent be selected from acetone, chloroform, ethyl acetate or ethanol one or more; The proportioning of α-benzoinoxime and organic solvent is 1g:10-20mL.
Further again, described organic solvent is the mixture of acetone and chloroform, and the volume ratio of acetone and chloroform is (2-1): 1.
Further, in step (2), tackifier are polystyrene or Triglycol distearate; The concentration of tackifier is 0.4-2wt%, and namely the weight of tackifier accounts for the 0.4-2% of organic phase gross weight.
Further, in step (3), described initiator is dibenzoyl peroxide, Diisopropyl azodicarboxylate or Potassium Persulphate.
Further again, the weight ratio of vinylbenzene, Vinylstyrene and initiator is 4:1:(0.2-0.5).
Further, in step (4), styrene-divinylbenzene prepolymer, dispersant solution and the volume ratio containing α-benzoinoxime organic phase are (2-1): (2-1): 1.
The present invention makes the prepolymer polymerization of α-benzoinoxime and styrene-divinylbenzene generate resin within specified temperatures, the Stability Analysis of Structures of gained resin, when extracting for molybdenum, the stability of extraction chromatography is fine, substantially increase the selectivity of α-benzoinoxime to molybdenum, experimental test shows, the saturated adsorption capacity of the resin that the present invention obtains is every gram of dried resin 36-43mg molybdenum.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Reagent in embodiment all can be buied from market.
embodiment 1
(1) dispersant solution is prepared: under agitation joined in 50mL deionized water by 0.8g dispersion agent (polyvinyl alcohol), be warmed up to 50 DEG C, dispersion agent is dissolved completely, obtains dispersant solution;
(2) preparation is containing the organic phase of α-benzoinoxime: joined by 1g α-benzoinoxime in the mixture (volume ratio is 2:1) of 25mL organic solvent-acetone and chloroform, stirring makes α-benzoinoxime dissolve, then 0.1g tackifier polystyrene is added, ultrasonic disperse 30-40 minute, obtains the organic phase containing α-benzoinoxime;
(3) styrene-divinylbenzene prepolymer is prepared: 40g vinylbenzene, 10g Vinylstyrene and 2g initiator (dibenzoyl peroxide) are mixed, stir, be warming up to 65-70 DEG C, make reactant generation prepolymerization reaction 30-40 minute, obtain styrene-divinylbenzene prepolymer;
(4) synthetic resins: the styrene-divinylbenzene prepolymer that 50mL step (3) obtains is joined in the dispersant solution that 50mL step (1) obtains, stir and make it be dispersed into pearl body, after being slowly warming up to 70 DEG C; In gained mixture, add the organic phase containing α-benzoinoxime that 25mL step (2) obtains, continue to be warming up to 85 DEG C, react 10 hours at this temperature, stop heating, Temperature fall; When temperature is down to 50 DEG C, reaction mixture is filtered, washes throw out with water, naturally dry, obtain the synthetic resins containing α-benzoinoxime.
embodiment 2
Preparation method with embodiment 1, unlike:
In the dispersant solution of step (1) with oxidic polyethylene alcohol for dispersion agent; In step (2) with 25mL ethyl acetate and acetone (volume ratio is for 2:1) for organic solvent dissolution 1g α-benzoinoxime, tackifier adopt polystyrene; Be initiator with dibenzoyl peroxide in step (3), in step (4), styrene-divinylbenzene prepolymer, dispersant solution and the volume containing the organic phase of α-benzoinoxime are respectively 50mL, 50mL, 30mL, and styrene-divinylbenzene prepolymer and the temperature of reaction containing the organic phase of α-benzoinoxime are 85 DEG C, the time is 15 hours.
embodiment 3
Preparation method with embodiment 1, unlike:
Be dispersion agent with polymaleic acid in the dispersant solution of step (1); The organic phase of step (2) is with ethanol and acetone for organic solvent dissolution α-benzoinoxime, and tackifier adopt Triglycol distearate; Be initiator with Potassium Persulphate in step (3), in step (4), styrene-divinylbenzene prepolymer, dispersant solution and the volume containing the organic phase of α-benzoinoxime are respectively 50mL, 50mL, 30mL, and styrene-divinylbenzene prepolymer and the temperature of reaction containing the extraction phase of α-benzoinoxime are 85 DEG C, the time is 15 hours.
embodiment 4
Preparation method with embodiment 1, unlike:
Be dispersion agent with polyvinyl alcohol in the dispersant solution of step (1); The organic phase of step (2) take ethyl acetate as organic solvent dissolution α-benzoinoxime, and tackifier adopt polystyrene; Be initiator with Diisopropyl azodicarboxylate in step (3), in step (4), styrene-divinylbenzene prepolymer, dispersant solution and the volume containing the organic phase of α-benzoinoxime are respectively 50mL, 50mL, 30mL, and styrene-divinylbenzene prepolymer and the temperature of reaction containing the organic phase of α-benzoinoxime are 85 DEG C, the time is 15 hours.
application examples
Prepare molybdenum carrier soln, adopted metric measurement, performance test has been carried out to the resin containing α-benzoinoxime prepared by embodiment of the present invention 1-4, lists in table 1.
Table 1
In addition, sample for embodiment 1 carries out subject range test, under concentration of hydrochloric acid is 0.0001 ~ 3mol/L, concentration of nitric acid 0.001 ~ 6mol/L, hydrofluoric acid concentration 0.000001 ~ 0.05mol/L situation, synthetic resins containing α-benzoinoxime prepared by the present invention can Absorption quantity molybdenum, and time of equilibrium adsorption is less than 5s.
Above-described embodiment just illustrates of the present invention, and the present invention also can implement with other ad hoc fashion or other particular form, and does not depart from main idea of the present invention or essential characteristic.Therefore, description embodiment from the viewpoint of any all should be considered as illustrative but not determinate.Scope of the present invention should be illustrated by the claim of adding, any also should be within the scope of the present invention with the intention of claim and the change of scope equivalence.
Claims (8)
1. a preparation method for molybdenum separation resin, comprises the following steps:
(1) prepare dispersant solution: under agitation join in deionized water by low-molecular-weight wax class dispersion agent, be warmed up to 45-50 DEG C, make both dissolve completely;
(2) preparation is containing the organic phase of α-benzoinoxime: joined by α-benzoinoxime in organic solvent, stirs and α-benzoinoxime is dissolved, then add tackifier, ultrasonic disperse 30-40 minute; Wherein, tackifier are polystyrene or Triglycol distearate; The concentration of tackifier is 0.4-2wt%;
(3) styrene-divinylbenzene prepolymer is prepared: vinylbenzene, Vinylstyrene and initiator are mixed, stir, be warming up to 65-70 DEG C, make reactant generation prepolymerization reaction 30-40 minute, obtain styrene-divinylbenzene prepolymer;
(4) synthetic resins: the styrene-divinylbenzene prepolymer that step (3) obtains is joined in the dispersant solution that step (1) obtains, stir and make it be dispersed into pearl body, after being slowly warming up to 65-70 DEG C; In gained mixture, add the organic phase containing α-benzoinoxime that step (2) obtains, continue to be warming up to 80-85 DEG C, react 10-15 hour at this temperature, stop heating, Temperature fall; When temperature is down to 40-50 DEG C, reaction mixture is filtered, washes throw out with water, naturally dry, obtain the synthetic resins containing α-benzoinoxime.
2. the preparation method of a kind of molybdenum separation resin according to claim 1, is characterized in that, in step (1), described low-molecular-weight wax class dispersion agent is selected from the one in polyvinyl alcohol, oxidic polyethylene alcohol or polymaleic acid; The concentration of dispersant solution is 1.5-2wt%.
3. the preparation method of a kind of molybdenum separation resin according to claim 2, is characterized in that, described dispersion agent is polyvinyl alcohol.
4. the preparation method of a kind of molybdenum separation resin according to claim 1, is characterized in that, in step (2), described organic solvent be selected from acetone, chloroform, ethyl acetate or ethanol one or more; The proportioning of α-benzoinoxime and organic solvent is 1g:10-20mL.
5. the preparation method of a kind of molybdenum separation resin according to claim 4, is characterized in that, described organic solvent is the mixture of acetone and chloroform, and the volume ratio of acetone and chloroform is (2-1): 1.
6. the preparation method of a kind of molybdenum separation resin according to claim 1, is characterized in that, in step (3), described initiator is dibenzoyl peroxide, Diisopropyl azodicarboxylate or Potassium Persulphate.
7. the preparation method of a kind of molybdenum separation resin according to claim 6, is characterized in that, the weight ratio of vinylbenzene, Vinylstyrene and initiator is 4:1:(0.2-0.5).
8. according to the preparation method of the arbitrary described a kind of molybdenum separation resin of claim 1-7, it is characterized in that, in step (4), styrene-divinylbenzene prepolymer, dispersant solution and the volume ratio containing α-benzoinoxime organic phase are (2-1): (2-1): 1.
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| CN109285616B (en) * | 2018-11-16 | 2020-08-21 | 中国原子能科学研究院 | From235Extraction from U fission products99Device for extracting Mo and extracting Mo by using device99Method for Mo |
| CN114717430B (en) * | 2022-04-19 | 2023-03-07 | 中国原子能科学研究院 | Method for extracting molybdenum from uranium fission products and ionic liquid system |
| CN116217785B (en) * | 2023-03-09 | 2024-06-11 | 核工业北京化工冶金研究院 | Molybdenum separation resin and preparation method and application thereof |
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