CN103342769A - Preparation method of molybdenum separation resin - Google Patents
Preparation method of molybdenum separation resin Download PDFInfo
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- CN103342769A CN103342769A CN2013102533985A CN201310253398A CN103342769A CN 103342769 A CN103342769 A CN 103342769A CN 2013102533985 A CN2013102533985 A CN 2013102533985A CN 201310253398 A CN201310253398 A CN 201310253398A CN 103342769 A CN103342769 A CN 103342769A
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- xixiangwo
- separation resin
- molybdenum separation
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Abstract
The invention relates to a preparation method of molybdenum separation resin. The preparation method comprises the following steps of: (1) preparing a dispersing agent solution; (2) preparing an alpha-benzoinoxime contained organic phase; (3) preparing a styrene-divinylbenzene prepolymer; and (4) synthesizing the resin: adding the styrene-divinylbenzene prepolymer into the dispersing agent solution, stirring the mixture so that the styrene-divinylbenzene prepolymer is dispersed into bead bodiese, and slowly heating to 65-70 DEG C; adding the alpha-benzoinoxime contained organic phase, continuing to heat to 80-85 DEG C, reacting for 10-15h, stopping heating and naturally cooling the alpha-benzoinoxime contained organic phase; and when the temperature is reduced to 40-50 DEG C, filtering a reaction mixture, cleaning a sediment and naturally airing the sediment. The molybdenum separation resin obtained by using the method provided by the invention is stable in structure, firmness of an extraction color layer is good when the molybdenum separation resin is used for molybdenum extraction, and the selectivity of the alpha-benzoinoxime to molybdenum is greatly improved; and experiments and tests prove that the molybdenum separation resin provided by the invention has the saturation adsorption capacity as follows: 36-43mg of molybdenum is contained in each gram of dry resin.
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-An Xixiangwo is that molybdenum is had optionally reagent of special chemistry, and traditional using method has two kinds: a kind of is with in the ethanol in the α-An Xixiangwo dissolving, mixes with the dissolving that contains molybdenum, makes molybdenum form precipitation; Another method is that α-An Xixiangwo is dissolved in chloroform or the ethyl acetate, fully vibrates with the solution that contains micro-molybdenum, realizes the extraction to micro-molybdenum.In trace analysis, hope can optionally be separated molybdenum rapidly, and often with diatomite or kel-F(chemical name: voltalef) powder is supporter, and behind silanization, on it, dry back dress post uses with the α-An Xixiangwo physical adsorption.The extraction chromatography stability of this method preparation is poor, the phenomenon that has molybdenum to run off.Therefore, develop a kind of stability molybdenum is had special optionally resin synthetic method is necessary.
Summary of the invention
At the defective that exists in the prior art, the purpose of this invention is to provide a kind of preparation method of molybdenum separation resin, the resin structure that adopts this method to make is stable, and the extraction chromatography stability was good when it was used for the molybdenum extracting and separating.
For reaching above purpose, the technical solution used in the present invention is: a kind of preparation method of molybdenum separation resin may further comprise the steps:
(1) preparation dispersant solution: under agitation low-molecular-weight wax class dispersion agent is joined in the deionized water, be warmed up to 45-50 ℃, both are dissolved fully;
(2) preparation contains the organic phase of α-An Xixiangwo: α-An Xixiangwo is joined in the organic solvent, stir and make the α-An Xixiangwo dissolving, add tackifier then, ultra-sonic dispersion 30-40 minute;
(3) preparation vinylbenzene-Vinylstyrene prepolymer: vinylbenzene, Vinylstyrene and initiator are mixed, stir, be warming up to 65-70 ℃, make reactant generation prepolymerization reaction 30-40 minute, obtain vinylbenzene-Vinylstyrene prepolymer;
(4) synthetic resins: vinylbenzene-Vinylstyrene prepolymer that step (3) is obtained joins in the dispersant solution that step (1) obtains, and stirs to make it be dispersed into the pearl body, slowly be warming up to 65-70 ℃ after; Add the organic phase that contains α-An Xixiangwo that step (2) obtains in the gained mixture, continue to be warming up to 80-85 ℃, reaction is 10-15 hour under this temperature, stops heating, naturally cooling; When temperature is down to 40-50 ℃, reaction mixture is filtered, wash throw out with water, dry naturally, namely get the synthetic resins that contains α-An Xixiangwo.
In the inventive method, (1), (2), (3) step order in no particular order.
Further, in the step (1), described low-molecular-weight wax class dispersion agent is selected from a kind of in polyvinyl alcohol, oxidic polyethylene alcohol or the polymaleic acid; The concentration of dispersant solution is 1.5-2 wt%.
Further again, described dispersion agent is polyvinyl alcohol.
Further, in the step (2), described organic solvent is selected from one or more in acetone, chloroform, ethyl acetate or the ethanol; The proportioning of α-An Xixiangwo 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 the 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 the 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 the step (4), vinylbenzene-Vinylstyrene prepolymer, dispersant solution and the volume ratio that contains the α-An Xixiangwo organic phase are (2-1): (2-1): 1.
The present invention makes the prepolymer polymerization of α-An Xixiangwo and vinylbenzene-Vinylstyrene generate resin under specific temperature, the Stability Analysis of Structures of gained resin, the stability of extraction chromatography is fine when being used for the molybdenum extraction, improved the selectivity of α-An Xixiangwo to molybdenum greatly, experimental test shows that the saturated adsorption capacity of the resin that the present invention makes is every gram dried resin 36-43mg molybdenum.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Reagent among the embodiment all can be buied from market.
Embodiment 1
(1) preparation dispersant solution: under agitation 0.8g dispersion agent (polyvinyl alcohol) is joined in the 50mL deionized water, be warmed up to 50 ℃, dispersion agent is dissolved fully, obtain dispersant solution;
(2) preparation contains the organic phase of α-An Xixiangwo: the 1g α-An Xixiangwo is joined in the mixture (volume ratio is 2:1) of 25mL organic solvent-acetone and chloroform, stirring makes the α-An Xixiangwo dissolving, add 0.1g tackifier polystyrene then, ultra-sonic dispersion 30-40 minute, obtain containing the organic phase of α-An Xixiangwo;
(3) preparation vinylbenzene-Vinylstyrene prepolymer: 40g vinylbenzene, 10g Vinylstyrene and 2g initiator (dibenzoyl peroxide) are mixed, stir, be warming up to 65-70 ℃, make reactant generation prepolymerization reaction 30-40 minute, obtain vinylbenzene-Vinylstyrene prepolymer;
(4) synthetic resins: vinylbenzene-Vinylstyrene prepolymer that 50mL step (3) is obtained joins in the dispersant solution that 50mL step (1) obtains, and stirs to make it be dispersed into the pearl body, slowly be warming up to 70 ℃ after; Add the organic phase that contains α-An Xixiangwo that 25mL step (2) obtains in the gained mixture, continue to be warming up to 85 ℃, reaction is 10 hours under this temperature, stops heating, naturally cooling; When temperature is down to 50 ℃, reaction mixture is filtered, wash throw out with water, dry naturally, namely get the synthetic resins that contains α-An Xixiangwo.
Embodiment 2
The preparation method is with embodiment 1, and different is:
Be dispersion agent with oxidic polyethylene alcohol in the dispersant solution of step (1); Be organic solvent dissolution 1g α-An Xixiangwo with 25mL ethyl acetate and acetone (volume ratio is 2:1) in the step (2), tackifier adopt polystyrene; Be initiator with the dibenzoyl peroxide in the step (3), vinylbenzene in the step (4)-Vinylstyrene prepolymer, dispersant solution and the volume that contains the organic phase of α-An Xixiangwo are respectively 50mL, 50mL, 30mL, and vinylbenzene-Vinylstyrene prepolymer is 85 ℃ with the temperature of reaction that contains the organic phase of α-An Xixiangwo, and the time is 15 hours.
Embodiment 3
The preparation method is with embodiment 1, and different is:
Be dispersion agent with the polymaleic acid in the dispersant solution of step (1); The organic phase of step (2) is the organic solvent dissolution α-An Xixiangwo with ethanol and acetone, and tackifier adopt Triglycol distearate; Be initiator with the Potassium Persulphate in the step (3), vinylbenzene in the step (4)-Vinylstyrene prepolymer, dispersant solution and the volume that contains the organic phase of α-An Xixiangwo are respectively 50mL, 50mL, 30mL, and vinylbenzene-Vinylstyrene prepolymer is 85 ℃ with the temperature of reaction that contains the extraction phase of α-An Xixiangwo, and the time is 15 hours.
Embodiment 4
The preparation method is with embodiment 1, and different is:
Be dispersion agent with the polyvinyl alcohol in the dispersant solution of step (1); The organic phase of step (2) is the organic solvent dissolution α-An Xixiangwo with the ethyl acetate, and tackifier adopt polystyrene; Be initiator with the Diisopropyl azodicarboxylate in the step (3), vinylbenzene in the step (4)-Vinylstyrene prepolymer, dispersant solution and the volume that contains the organic phase of α-An Xixiangwo are respectively 50mL, 50mL, 30mL, and vinylbenzene-Vinylstyrene prepolymer is 85 ℃ with the temperature of reaction that contains the organic phase of α-An Xixiangwo, and the time is 15 hours.
Application examples
Prepared the molybdenum carrier soln, adopted metric measurement, the resin that contains α-An Xixiangwo that embodiment of the invention 1-4 is prepared carries out performance test, lists in table 1.
Table 1
In addition, sample at embodiment 1 carries out the subject range test, be under 0.0001～3mol/L, concentration of nitric acid 0.001～6mol/L, the hydrofluoric acid concentration 0.000001～0.05mol/L situation at concentration of hydrochloric acid, the synthetic resins that contains α-An Xixiangwo of the present invention's preparation can quantitatively adsorb molybdenum, and the adsorption equilibrium time 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, the embodiment of description all should be considered as illustrative from any aspect but not be determinate.Scope of the present invention should be by additional claim explanation, and the intention of any and claim and the variation of scope equivalence also should be within the scope of the present invention.
Claims (9)
1. the preparation method of a molybdenum separation resin may further comprise the steps:
(1) preparation dispersant solution: under agitation low-molecular-weight wax class dispersion agent is joined in the deionized water, be warmed up to 45-50 ℃, both are dissolved fully;
(2) preparation contains the organic phase of α-An Xixiangwo: α-An Xixiangwo is joined in the organic solvent, stir and make the α-An Xixiangwo dissolving, add tackifier then, ultra-sonic dispersion 30-40 minute;
(3) preparation vinylbenzene-Vinylstyrene prepolymer: vinylbenzene, Vinylstyrene and initiator are mixed, stir, be warming up to 65-70 ℃, make reactant generation prepolymerization reaction 30-40 minute, obtain vinylbenzene-Vinylstyrene prepolymer;
(4) synthetic resins: vinylbenzene-Vinylstyrene prepolymer that step (3) is obtained joins in the dispersant solution that step (1) obtains, and stirs to make it be dispersed into the pearl body, slowly be warming up to 65-70 ℃ after; Add the organic phase that contains α-An Xixiangwo that step (2) obtains in the gained mixture, continue to be warming up to 80-85 ℃, reaction is 10-15 hour under this temperature, stops heating, naturally cooling; When temperature is down to 40-50 ℃, reaction mixture is filtered, wash throw out with water, dry naturally, namely get the synthetic resins that contains α-An Xixiangwo.
2. the preparation method of a kind of molybdenum separation resin according to claim 1 is characterized in that, in the step (1), described low-molecular-weight wax class dispersion agent is selected from a kind of in polyvinyl alcohol, oxidic polyethylene alcohol or the polymaleic acid; The concentration of dispersant solution is 1.5-2 wt%.
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 the step (2), described organic solvent is selected from one or more in acetone, chloroform, ethyl acetate or the ethanol; The proportioning of α-An Xixiangwo 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 4 is characterized in that, in the step (2), tackifier are polystyrene or Triglycol distearate; The concentration of tackifier is 0.4-2 wt%.
7. the preparation method of a kind of molybdenum separation resin according to claim 1 is characterized in that, in the step (3), described initiator is dibenzoyl peroxide, Diisopropyl azodicarboxylate or Potassium Persulphate.
8. the preparation method of a kind of molybdenum separation resin according to claim 7 is characterized in that, the weight ratio of vinylbenzene, Vinylstyrene and initiator is 4:1:(0.2-0.5).
9. according to the preparation method of the arbitrary described a kind of molybdenum separation resin of claim 1-8, it is characterized in that, in the step (4), vinylbenzene-Vinylstyrene prepolymer, dispersant solution and the volume ratio that contains the α-An Xixiangwo organic phase are (2-1): (2-1): 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691146A (en) * | 2013-12-09 | 2014-04-02 | 何小刚 | Extraction agent of impregnating resin and preparation method thereof |
| CN109285616A (en) * | 2018-11-16 | 2019-01-29 | 中国原子能科学研究院 | From235It is extracted in U fission product99The device of Mo and utilization device extraction99The method of Mo |
| CN114717430A (en) * | 2022-04-19 | 2022-07-08 | 中国原子能科学研究院 | Method for extracting molybdenum from uranium fission products and ionic liquid system |
| CN116217785A (en) * | 2023-03-09 | 2023-06-06 | 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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| WO1999040128A1 (en) * | 1998-02-06 | 1999-08-12 | Tci Incorporated | A SOLID POLYMER SORBENT FOR Mo-99 EXTRACTION AND ITS METHOD OF PRODUCTION |
| CN103337265A (en) * | 2013-06-21 | 2013-10-02 | 中国原子能科学研究院 | Chemical separation procedure for burnup analysis of spent fuel element |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999040128A1 (en) * | 1998-02-06 | 1999-08-12 | Tci Incorporated | A SOLID POLYMER SORBENT FOR Mo-99 EXTRACTION AND ITS METHOD OF PRODUCTION |
| CN103337265A (en) * | 2013-06-21 | 2013-10-02 | 中国原子能科学研究院 | Chemical separation procedure for burnup analysis of spent fuel element |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691146A (en) * | 2013-12-09 | 2014-04-02 | 何小刚 | Extraction agent of impregnating resin and preparation method thereof |
| CN103691146B (en) * | 2013-12-09 | 2016-08-10 | 何小刚 | A kind of extraction agent and preparation method thereof |
| CN109285616A (en) * | 2018-11-16 | 2019-01-29 | 中国原子能科学研究院 | From235It is extracted in U fission product99The device of Mo and utilization device extraction99The method of Mo |
| CN114717430A (en) * | 2022-04-19 | 2022-07-08 | 中国原子能科学研究院 | Method for extracting molybdenum from uranium fission products and ionic liquid system |
| 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 |
| CN116217785A (en) * | 2023-03-09 | 2023-06-06 | 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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