CN101643847B - Preparation method of tributyl phosphate extraction resin for zirconium-hafnium separation - Google Patents
Preparation method of tributyl phosphate extraction resin for zirconium-hafnium separation Download PDFInfo
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Abstract
The invention relates to tributyl phosphate extraction resin for zirconium-hafnium separation and a preparation method thereof. The preparation method is characterized by comprising the following steps: adding a solvent into a reaction kettle, wherein the solvent is a mixture of water and alcohols and the mixed weight ratio of the water and the alcohols is 100:2-100; after the solvent is stirred evenly, adding resin into the solvent, wherein the weight ratio of the solvent to the resin is 100:5-100; after the mixture is stirred evenly, adding tributyl phosphate into the mixture, wherein the weight ratio of the tributyl phosphate to the resin is 15-400:100; and stirring the mixture for 0.5 to 20 hours at the temperature of between 10 and 100 DEG C, and filtering the mixture to obtain the TBP extraction resin. The TBP-resin prepared by the method serving as the extraction resin for filling an extraction chromatographic column can effectively separate zirconium and hafnium, fully exerts the advantages of a liquid-liquid extraction process such as large TBP extracted zirconium capacity and large zirconium-hafnium separation coefficient, and eliminates the problem of emulsification produced by liquid-liquid extraction so as to successfully implement a zirconium-hafnium TBP extraction separation process.
Description
Technical field
The present invention relates to a kind of tributyl phosphate extraction resin and preparation method thereof, particularly a kind of zirconium hafnium separates with tributyl phosphate extraction resin and preparation method thereof.
Background technology
The occurring in nature zirconium with hafnium symbiosis always be in the same place, expect atomic level zirconium and hafnium, can only adopt extracting process to separate zirconium and hafnium.Once used TBP-hydrochloric acid in the past, the liquid-liquid extraction technical process extracting and separating zirconium and the hafnium of nitric acid mixing acid system are produced zirconium oxide at atomic energy level and hafnia.The characteristics of this flow process are that the extracted organic phase capacity is big, and separation factor is high, and the extraction equipment production capacity is big, just can obtain qualified zirconium oxide at atomic energy level and hafnia simultaneously through flash liberation.But fatal shortcoming is that emulsification problem can't solve in extraction process, and well-known, emulsification is the formidable enemy who realizes smoothly in the liquid-liquid extraction process.Because emulsion produces two phases that extract can not effectively be separated, finally cause the liquid-liquid extraction flow process to carry out.
Therefore provide a kind of extraction zirconium capacity big, the zirconium hafnium that zirconium hafnium separation factor is big separates with tributyl phosphate extraction resin and preparation method thereof just becomes the technical barrier that this technical field urgent need is wanted.
Summary of the invention
It is big that one of the object of the invention provides a kind of extraction zirconium capacity, and the zirconium hafnium that zirconium hafnium separation factor is big separates with tributyl phosphate (hereinafter to be referred as TBP) extration resin.
Above-mentioned purpose of the present invention reaches through following technical scheme:
A kind of zirconium hafnium separates uses tributyl phosphate extraction resin, and it is characterized in that: the weight ratio of said tributyl phosphate and resin is 15～400: 100; Said resin is vinylbenzene-divinylbenzene resin, vinylbenzene-TEB 3K, styrene-propene acid methyl esters, vinylbenzene-trimethylammonium vinylformic acid glyceryl ester; Vinylbenzene-dimethacrylate ethanol ester, voltalef, tetrafluoroethylene; Vilaterm, polyacrylonitrile, or urethane.
A kind of optimal technical scheme is characterized in that: the size-grade distribution of said resin, median size be at 80～150 orders, and size distribution should be 90% in 20% scope of median size.
A kind of optimal technical scheme; It is characterized in that: the mean pore size of said resin 20～150
, average specific surface area is in 300～1000 meters squared per gram.
A kind of optimal technical scheme is characterized in that: said solvent is 100: 5～100 with the weight resin ratio.
It is big that another object of the present invention provides a kind of extraction zirconium capacity, and the zirconium hafnium that zirconium hafnium separation factor is big separates the preparation method with tributyl phosphate extraction resin.
Above-mentioned purpose of the present invention reaches through following technical scheme:
A kind of zirconium hafnium separates the preparation method with tributyl phosphate extraction resin, and its step is following:
At first, in reaction kettle, add solvent, said solvent is water-alcohols mixture, and its mixed weight ratio is 100: 2～100;
Secondly, after stirring, add resin, the weight ratio of said solvent and said resin is 100: 5～100;
At last, stir the back and add tributyl phosphate, said tributyl phosphate with described in the weight ratio of resin be 15～400: 100, in 10～100 ℃ of TRs, stirred 0.5～20 hour, filter and obtain the TBP-extration resin.
A kind of optimal technical scheme is characterized in that: the mixed weight ratio of said solvent is 100: 10～30.
A kind of optimal technical scheme is characterized in that: said solvent is water-USP Kosher class, the water-ethylene glycol class, and water-USP Kosher or water-ethylene glycol mix class.
A kind of optimal technical scheme is characterized in that: the weight ratio of solvent and said resin is 100: 20～50 described in the said step (2).
A kind of optimal technical scheme is characterized in that: the weight ratio of resin is 45～400: 100 described in tributyl phosphate described in the said step (3) and the step (2).
A kind of optimal technical scheme is characterized in that: the TR described in the said step (3) is 20 ℃～45 ℃, and churning time is 2～15 hours.
A kind of optimal technical scheme is characterized in that: said resin is vinylbenzene-divinylbenzene resin, vinylbenzene-TEB 3K; Styrene-propene acid methyl esters, vinylbenzene-trimethylammonium vinylformic acid glyceryl ester, vinylbenzene-dimethacrylate ethanol ester; Voltalef, tetrafluoroethylene, Vilaterm; Polyacrylonitrile, or urethane; The size-grade distribution of said resin, median size be at 80～150 orders, and size distribution should be 90% in 20% scope of median size; The mean pore size of said resin be 20～150
, average specific surface area is in 300～1000 meters squared per gram.
A kind of optimal technical scheme; It is characterized in that: the mean pore size of said resin be 90～100
, average specific surface area is in 600～800 meters squared per gram.
Beneficial effect:
Adopt the TBP-resin of the present invention's preparation, fill out extracting chromatographic column, effectively separate zirconium and hafnium as extration resin; Both given full play to the advantage of liquid-liquid extraction technology, TBP extraction zirconium capacity is big, and zirconium hafnium separation factor is big; Single extraction can get two kinds of specification product; Zirconium oxide at atomic energy level and atomic level hafnia, quality product is high, and is stable.Eliminated the emulsification problem that liquid-liquid extraction produces again, made TBP extracting and separating zirconium and hafnium technology smooth implementation.
The size-grade distribution of said resin, median size be preferably at 80～150 orders, and size distribution should be 90% in 20% scope of median size.Particle diameter is too big, can reduce the theoretical plate number of resin column, and separating power is reduced.The too small resistance of pillar that then can make of particle diameter increases, and needs higher pressure.Wide " hangover " phenomenon that then can make of size distribution is serious.
The aperture of said resin and specific surface area select the resin mean pore size 20～150
, specific surface area is in 300～1000 meters squared per gram.If the aperture is too little, though specific surface area is big, to the shielding effect that is adsorbed with of TBP, adsorption effect is bad.If the too big corresponding specific surface area in aperture is just little, and is also little to the adsorptive capacity of TBP.Therefore resin is preferably selected mean pore size 90～100
, and specific surface area is at the resin of 600～800 meters squared per gram.
Said TBP is 15～400: 100 with the weight resin ratio.If TBP is lower than 15 parts, loading capacity is little, and extraction efficiency is low.If the amount of TBP is higher than 400 parts, loading capacity is excessive, the resin supersaturation, and the extraction swapace reduces, and extraction efficiency also descends.Therefore preferably selecting TBP and weight resin ratio is 45～400: 100.
Solvent is 100: 5～100 with the weight resin ratio, if amount of resin is lower than 5 parts, causes resin absorption TBP difficulty, if amount of resin is higher than 100 parts, makes resin absorption TBP operational difficulty.Therefore preferably selective solvent compares 100: 20～50 with weight resin.
The temperature of said resin absorption TBP is at 10 ℃～100 ℃.If temperature is lower than 10 ℃, the viscosity of TBP is increased, cause resin absorption TBP difficulty, if temperature is higher than 100 ℃, the solubleness of TBP is increased, the amount of resin absorption TBP reduces.Therefore preferably select TR at 20 ℃～45 ℃.
The said resin absorption TBP time is controlled at 0.5～20 hour, if be lower than 0.5 hour, the amount of resin absorption TBP is little, and loading capacity is just little, and extraction efficiency is just low.If be higher than 20 hours, resin absorption TBP has reached balance, and the time, long again TBP adsorptive capacity can not increase yet, and only can increase power consumption.Therefore the resin absorption TBP time preferably was controlled at 2～15 hours.
Said solvent comprises: water-USP Kosher class, and the water-ethylene glycol class, water-USP Kosher and terepthaloyl moietie mix class, mixed solvent weight ratio, water: terepthaloyl moietie (USP Kosher) 100: 2～100.If the glycols add-on is lower than 2 parts, TBP solubleness in solvent increases, and reduces the adsorptive capacity of resin to TBP, if the glycols add-on is higher than 100 parts, solution viscosity increases, and influences resin to the TBP adsorptive capacity.Therefore in the resin absorption TBP mixed solvent weight ratio of water-alcohol be preferably 100: 10～30.
Embodiment
Embodiment-1
25 kilograms of the deionized waters that adding measures in reaction kettle; Add 2.5 kilograms of USP Kosher while stirring, add 14 kilograms of polystyrene-divinylbenzene resins (commercially available, median size 80～100 orders) after stirring again; 7.5 kilograms of the TBP that adding measures after stirring; Whipping temp remains on 35 ℃, stirs 5 hours, filters and obtains the 34%TBP extration resin.
Embodiment-2
20 kilograms of the deionized waters that adding measures in reaction kettle, 7.5 kilograms of the terepthaloyl moietie that adding while stirring measures are after stirring; Add PS-14 kilograms of (self-controls of methyl acrylate resin again; Median size 100～150 orders), 9 kilograms of the TBP that adding measures after stirring, whipping temp remains on 25 ℃; Stirred 8 hours, and filtered and obtain the 39%TBP extration resin.
Embodiment-3
20 kilograms of the deionized waters that adding measures in reaction kettle, 3 kilograms of the terepthaloyl moietie that adding while stirring measures, 4 kilograms of USP Kosher; After stirring, add PS-16 kilograms of trimethylammonium methyl acrylates (self-control, median size 80～150 orders) again; 13 kilograms of the TBP that adding measures after stirring; Whipping temp remains on 45 ℃, stirs 15 hours, filters and obtains the 45%TBP extration resin.
Embodiment-4
In reaction kettle, add 25 kilograms of the deionized waters measure, add 4 kilograms of the glycol ethers that measure while stirring, it is (commercially available to add 14 kilograms of polystyrene-divinylbenzene resins after stirring again; Median size 80～100 orders); After stirring, 3.5 kilograms of the TBP that adding measures, whipping temp remains on 100 ℃; Stirred 5 hours, and filtered and obtain the 16%TBP extration resin.
Embodiment-5
20 kilograms of the deionized waters that adding measures in reaction kettle, 6 kilograms of the terepthaloyl moietie that adding while stirring measures are after stirring; Add PS-14 kilograms of (self-controls of dimethacrylate ethanol ester again; Median size 80～150 orders), 28 kilograms of the TBP that adding measures after stirring, whipping temp remains on 85 ℃; Stirred 12 hours, and filtered and obtain the 28%TBP extration resin.
Embodiment-6
20 kilograms of the deionized waters that adding measures in reaction kettle, 5 kilograms of the terepthaloyl moietie that adding while stirring measures are after stirring; Add (the self-control of 14 kilograms of PS-TEB 3Ks again; Median size 80～150 orders), 56 kilograms of the TBP that adding measures after stirring, whipping temp remains on 30 ℃; Stirred 15 hours, and filtered and obtain the 81%TBP extration resin.
Embodiment-7
15 kilograms of the deionized waters that adding measures in reaction kettle add 10 kilograms of USP Kosher, 5 kilograms of the terepthaloyl moietie that measures, after stirring while stirring; It is (commercially available to add 30 kilograms of polyacrylonitrile again; Median size 80～100 orders), 4.5 kilograms of the TBP that adding measures after stirring, whipping temp remains on 20 ℃; Stirred 18 hours, and filtered and obtain the 13%TBP extration resin.
Embodiment-8
25 kilograms of the deionized waters that adding measures in reaction kettle, 0.5 kilogram of the terepthaloyl moietie that adding while stirring measures is after stirring; Add PS-10 kilograms of (self-controls of trimethylammonium vinylformic acid glyceryl ester again; Median size 100～150 orders), 30 kilograms of the TBP that adding measures after stirring, whipping temp remains on 10 ℃; Stirred 20 hours, and filtered and obtain the 75%TBP extration resin.
Embodiment-9
29 kilograms of the deionized waters that adding measures in reaction kettle, 1 kilogram of the USP Kosher that adding while stirring measures is after stirring; It is (commercially available to add 6 kilograms of Vinylpyrrolidone polymers again; Median size 100～150 orders), 2.7 kilograms of the TBP that adding measures after stirring, whipping temp remains on 50 ℃; Stirred 2 hours, and filtered and obtain the 21%TBP extration resin.
Embodiment-10
38 kilograms of the deionized waters that adding measures in reaction kettle add 1 kilogram of terepthaloyl moietie, 1 kilogram of the USP Kosher that measures, after stirring while stirring; It is (commercially available to add 2 kilograms of polyvinyl esters again; Median size 80～150 orders), 5 kilograms of the TBP that adding measures after stirring, whipping temp remains on 90 ℃; Stirred 0.5 hour, and filtered and obtain the 65%TBP extration resin.
Above-mentioned enforcement prepares the TBP extration resin, adopts patent announcement 101209858A separating zirconium hafnium by tributyl phosphate extraction chromatography method, and getting 10 kilograms of diameters of packing into respectively is 80mm, long in the post of 850mm, preparating acid strength of solution 4.5 mol; Zirconium feed liquid zirconium and hafnium total concn 0.314 mol, hafnium oxide content 2.07%, free acid concentration 5 mol; Pickle solution concentration 4.05 mol; Anti-zirconium liquid concentration 1.07 mol.
Various TBP extration resin extracting and separating zirconiums and hafnium
| Embodiment (extracting resin) | Acid solution (liter) | Zirconium feed liquid (liter) | Pickle solution (liter) | Anti-zirconium liquid (liter) | ZrO 2Concentration (mol) | HfO 2Content (%) | ZrO 2Yield (%) |
| 1 | 5.5 | 1.5 | 8.8 | 1.4 | 0.313 | ＜0.01 | 92 |
| 2 | 5.5 | 1.5 | 8.8 | 1.35 | 0.33 | ＜0.01 | 93 |
| 3 | 5.5 | 1.5 | 8.8 | 1.1 | 0.41 | ＜0.01 | 95 |
| 4 | 5.5 | 1.5 | 8.8 | 1.5 | 0.17 | ＜0.01 | 55 |
| 5 | 5.5 | 1.5 | 8.8 | 1.2 | 0.27 | ＜0.01 | 70 |
| 6 | 5.5 | 1.5 | 8.8 | 1.3 | 0.19 | ＜0.01 | 53 |
| 7 | 5.5 | 1.5 | 8.8 | 1.2 | 0.16 | ＜0.01 | 52 |
| 8 | 5.5 | 1.5 | 8.8 | 1.1 | 0.25 | ＜0.01 | 60 |
| 9 | 5.5 | 1.5 | 8.8 | 1.5 | 0.20 | ＜0.01 | 65 |
| 10 | 5.5 | 1.5 | 8.8 | 1.4 | 0.28 | ＜0.01 | 85 |
Can draw from above result, with the TBP extration resin of the inventive method preparation, extraction zirconium capacity is big, and zirconium hafnium separation factor is big, and single extraction can obtain two kinds of specification product, zirconium oxide at atomic energy level and hafnia, and quality product is high, stable.The TBP extration resin is after using repeatedly, and the extracting and separating ability remains unchanged.
Claims (8)
1. a zirconium hafnium separates the preparation method with tributyl phosphate extraction resin, and its step is following:
(1) in reaction kettle, add solvent, said solvent is water-alcohols mixture, and its mixed weight ratio is 100: 2～100;
(2) stir after, add resin, the weight ratio of said solvent of step (1) and said resin is 100:5～100; Said resin is vinylbenzene-divinylbenzene resin, vinylbenzene-TEB 3K, styrene-propene acid methyl esters, vinylbenzene-trimethylammonium vinylformic acid glyceryl ester; Vinylbenzene-dimethacrylate ethanol ester, voltalef, tetrafluoroethylene; Vilaterm, polyacrylonitrile, or urethane;
(3) stir the back and add tributyl phosphate, the weight ratio of resin is 15～400: 100 described in said tributyl phosphate and the step (2), in 10～100 ℃ of TRs, stirs 0.5～20 hour, filters and obtains the TBP-extration resin.
2. the preparation method of tributyl phosphate extraction resin according to claim 1 is characterized in that: the median size of said resin is at 80～150 orders, and size distribution should be 90% in 20% scope of median size; The mean pore size of said resin in
average specific surface area in 300～1000 meters squared per gram.
3. the preparation method of tributyl phosphate extraction resin according to claim 1, it is characterized in that: the mixed weight ratio of solvent described in the said step (1) is 100: 10～30.
4. the preparation method of tributyl phosphate extraction resin according to claim 3, it is characterized in that: said solvent is water-USP Kosher, water-ethylene glycol, the mixture of water-USP Kosher and water-ethylene glycol.
5. according to the preparation method of each described tributyl phosphate extraction resin among the claim 1-4, it is characterized in that: the weight ratio of solvent and said resin is 100: 20～50 described in the said step (2).
6. the preparation method of tributyl phosphate extraction resin according to claim 5, it is characterized in that: the weight ratio of resin is 45～400: 100 described in tributyl phosphate described in the said step (3) and the step (2).
7. the preparation method of tributyl phosphate extraction resin according to claim 6, it is characterized in that: the TR described in the said step (3) is 20 ℃～45 ℃, and churning time is 2～15 hours.
8. the preparation method of tributyl phosphate extraction resin according to claim 7 is characterized in that: the mean pore size of said resin for
average specific surface area in 600～800 meters squared per gram.
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| CN2008101177200A CN101643847B (en) | 2008-08-04 | 2008-08-04 | Preparation method of tributyl phosphate extraction resin for zirconium-hafnium separation |
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| CN2008101177200A CN101643847B (en) | 2008-08-04 | 2008-08-04 | Preparation method of tributyl phosphate extraction resin for zirconium-hafnium separation |
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| CN101643847B true CN101643847B (en) | 2012-04-25 |
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| CN104046777B (en) * | 2013-03-12 | 2016-04-27 | 北京有色金属研究总院 | By the method for tributyl phosphate resin fractionating, extracting and separating zirconium and hafnium |
| CN103789547B (en) * | 2014-01-15 | 2015-10-21 | 中国科学院长春应用化学研究所 | A kind of ionic liquid extration resin and methods for making and using same thereof |
| CN109874342A (en) * | 2015-10-30 | 2019-06-11 | Ii－Vi 有限公司 | The purposes of fluoropolymer resin, preparation method and its extraction (one or more) precious metal that composite extractant enhances |
| CN106929695B (en) * | 2015-12-29 | 2019-06-18 | 核工业北京化工冶金研究院 | A kind of Solvent Extraction Separation zirconium hafnium technique |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101209858A (en) * | 2006-12-28 | 2008-07-02 | 北京有色金属研究总院 | Method for separating zirconium hafnium by tributyl phosphate extraction chromatography method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101209858A (en) * | 2006-12-28 | 2008-07-02 | 北京有色金属研究总院 | Method for separating zirconium hafnium by tributyl phosphate extraction chromatography method |
Non-Patent Citations (1)
| Title |
|---|
| 黄礼煌.稀土提取技术.《稀土提取技术》.冶金工业出版社,2006,342-344. * |
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