CN1210895A - Solvent extraction process for improving purity of strontium and barium salts - Google Patents
Solvent extraction process for improving purity of strontium and barium salts Download PDFInfo
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- CN1210895A CN1210895A CN97116891A CN97116891A CN1210895A CN 1210895 A CN1210895 A CN 1210895A CN 97116891 A CN97116891 A CN 97116891A CN 97116891 A CN97116891 A CN 97116891A CN 1210895 A CN1210895 A CN 1210895A
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- Prior art keywords
- strontium
- solution
- extraction
- organic phase
- acid
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 25
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 17
- 159000000009 barium salts Chemical class 0.000 title claims description 7
- 238000000638 solvent extraction Methods 0.000 title claims description 5
- 238000000605 extraction Methods 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- 239000011575 calcium Substances 0.000 abstract description 16
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 abstract description 16
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052791 calcium Inorganic materials 0.000 abstract description 15
- 239000012535 impurity Substances 0.000 abstract description 13
- 229910001631 strontium chloride Inorganic materials 0.000 abstract description 4
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 7
- 229910000018 strontium carbonate Inorganic materials 0.000 description 6
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 5
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 4
- 229910052667 lazurite Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052788 barium Inorganic materials 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- -1 common vitriol Chemical compound 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Chemical compound [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The process is used to separate Ca and other impurities from strontium chloride or strontium nitrate solution. Through multi-stage counter-current extraction with auxiliary washing, the content of calcium and other impurities in strontium chloride or strontium nitrate solution is reduced to the designed level and strontium product is made to reach required purity. The washing step can recover strontium extracted together with impurities and this can reduce loss of strontium while ensuring the high purity of strontium product.In addition, the process has less pollution and is favourable to large-scale production.
Description
The invention belongs to isolation technique, particularly improve strontium and barium salt purity separation technology with solvent extration.
Metal inorganic salt is the important chemical product, because there are abundant mineral wealth in China, the salt of strontium, barium and oxide compound are one of important export Chemicals, and annual export volume reaches ten tens thousand of tons.The removal of impurities process of present strontium or barium salt and oxide compound production method adopts oxyhydroxide more, carbonate or sulfate precipitation.The operation of precipitate and separate is irreversible often, and simple process commonly used is finished, and promptly adds precipitation agent in a reactor impurity formation solid is separated, and this throw out solubleness in main composition and impurity generation is effective when differing greatly.As can from the solution of strontium or barium, removing heavy metal effectively.But element that chemical property is similar such as calcium, strontium, common vitriol, carbonate, the oxalate solubleness of barium are more or less the same.Thereby when an element be major ingredient, dense, and in addition the two is an impurity component, concentration is very low, when removing with the precipitator method, main composition is coprecipitation, and causes damage.Because the separation factor between these elements is very low, often in order to guarantee that the rate of recovery can not deep impurity-removing, so most of product purity is not high.With the process of producing Strontium carbonate powder from the lazurite in Sichuan is example, contains Strontium Sulphate and about 5% lime carbonate and 10% Strontium carbonate powder about 70% in the ore.For removing calcium, at present, at first embathe in process of production with hydrochloric acid, the molten lime carbonate that goes, also make the Strontium carbonate powder dissolving so simultaneously, this part solution is whole ventings in Production Flow Chart now, do not give recovery, loss accounts for more than 10% of whole strontium amount, and, in order to reduce the loss of strontium, soaking when molten, fully deliming better, so that in final Strontium carbonate powder, still contain 0.5% to 1.2% lime carbonate.
Solvent extraction has been applied to nuclear fuel gradually since the fifties, the production of rare earth, rare, rare expensive and non-ferrous metal is a kind of efficient height, more easy-operating good separation method.Extraction process is a reversible reaction, finishes by the multi-stage countercurrent mode usually.Thereby impurity and main composition to the constantly exchange mutually of another level, both can reach very high separation factor by one-level when separating, can guarantee the very high rate of recovery again, were particularly suitable for the separation and the recovery of the close composition of character.
Extracting process of the present invention has following benefit to improving strontium or barium salt production: (1) improves comprehensive recovery; (2) promote quality product; (3) help scale operation; (4) reduce pollution.
The used extraction agent of the present invention comprises carboxylic acid, naphthenic acid, organic phosphoric acid and organic phospho acid, as: lipid acid, two-2-ethylhexyl phosphoric acid (Chinese commodity title P204), two-2-ethylhexyl phosphonic acid, two-2-ethylhexyl fat (Chinese commodity title P507) etc.Above-mentioned extraction agent adds a small amount of properties-correcting agent and is dissolved in together in kerosene or the solvent oil and is made into organic phase.Extraction process comprises steps such as extraction, washing and back extraction.
The object of the present invention is achieved like this.Because the alkaline-earth metal similar performance, separation factor is little, and the present invention adopts the method for multi-stage counter current extraction, impurity such as separating calcium from strontium chloride or strontium nitrate solution.By multi-stage counter current extraction, be aided with washing procedure and can make the calcium impurities in strontium chloride or the strontium nitrate solution be reduced to design level, make the strontium product reach desired purity.Washing procedure can make the strontium that is extracted together with impurity obtain reclaiming, with the loss reduction arrival 1% of strontium.Thereby both guaranteed the high purity of strontium product, guaranteed the high-recovery of strontium again.The concrete practice is:
1.5% to 50% acidic extractant and an amount of properties-correcting agent add the kerosene wiring solution-forming, promptly are organic phases.
2. work out the extraction process condition according to the foreign matter content of material solution.2 to 5 grades of general extractions, the ratio of organic phase and feed liquid water flow is 0.3 to 1,2 to 8 minutes residence time, stirring velocity: 300～600rpm.
3. select suitable inorganic acid solution to carry out countercurrent washing.
4. with inorganic salt, example hydrochloric acid, salpeter solution carry out countercurrent reextraction, 2 to 3 grades of back extraction progression.The ratio of organic phase and water flow is 1 to 10,2 to 8 minutes residence time, stirring velocity 300～600rpm.
Positively effect of the present invention is:
(1) can be with solvent extraction with the calcium in salt acid elution lime carbonate, the strontium solution, strontium Separation and Recovery respectively, thus the strontium rate of recovery is improved more than 10%, and eliminate the pollution that discharging hydrochloric acid washings causes.
(2) also can be without the step of the salt acid elution lime carbonate described in (1), and directly lazurite is converted into strontium nitrate solution, remove calcium and other impurity in the solution with extraction process again, shortened process, improve the output and the quality of product, make the calcium carbonate content in the top grade Strontium carbonate powder drop to below 0.2% other impurity from present 0.5%, as heavy metals such as iron, also can correspondingly reduce.
(3) because extraction process does not produce slag, thereby avoid heavy work such as scavenger precipitation slag, help automatization and implement scale operation.
In producing, barium salt also can carry out similar process modification.
Embodiment:
(1) lazurite decomposes the strontium nitrate solution that generates, and contains strontium 164.2g/L, calcium 6.2g/L, with 10% (V/V) to the kerosin of the P204 of 30% (V/V) and a small amount of properties-correcting agent through five grades extraction, the secondary washing, calcium can be reduced to 0.1g/L, the rate of recovery 97% to 99.5% of strontium nitrate.Calcium can hydrochloric acid or the nitric acid back extraction prepare calcium product.Extraction agent returns use.
(2) the hydrochloric acid leaching liquid of the hydrochloric acid leacheate of lazurite or strontianite contains strontium 62.4g/L, calcium 25.1g/L, with 20% (V/V) to the kerosin of 45% (V/V) P507 and a small amount of properties-correcting agent through five grades extraction, three grades of washings, calcium can be reduced to 0.1g/L.The rate of recovery 95% to 99.5% of strontium nitrate.Calcium can hydrochloric acid or the nitric acid back extraction prepare calcium product.Extraction agent returns use.
Claims (1)
1. one kind is improved the method for strontium and barium salt purity with solvent extraction, it is characterized in that:
(1) adding the kerosene wiring solution-forming with 5% to 50% acidic extractant and 0～15% properties-correcting agent, promptly is organic phase;
(2) work out the extraction process condition according to the foreign matter content of material solution, generally extract 2 to 5 grades, the ratio of organic phase and feed liquid water flow is 0.3 to 1,2 to 8 minutes residence time, stirring velocity: 300～600rpm;
(3) select the inorganic acid solution of hydrochloric acid or nitric acid to carry out countercurrent washing;
(4) with inorganic salt, example hydrochloric acid, salpeter solution carry out countercurrent reextraction, 2 to 4 grades of back extraction progression; The ratio of organic phase and water flow is 1 to 10,2 to 8 minutes residence time, stirring velocity 300～600rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97116891A CN1087354C (en) | 1997-09-05 | 1997-09-05 | Solvent extraction process for improving purity of strontium and barium salts |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97116891A CN1087354C (en) | 1997-09-05 | 1997-09-05 | Solvent extraction process for improving purity of strontium and barium salts |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1210895A true CN1210895A (en) | 1999-03-17 |
| CN1087354C CN1087354C (en) | 2002-07-10 |
Family
ID=5174182
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97116891A Expired - Fee Related CN1087354C (en) | 1997-09-05 | 1997-09-05 | Solvent extraction process for improving purity of strontium and barium salts |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1087354C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673028A (en) * | 2015-11-09 | 2017-05-17 | 虔东稀土集团股份有限公司 | Preparation method of alkaline earth metal compound |
| CN109319818A (en) * | 2018-11-26 | 2019-02-12 | 南昌航空大学 | A kind of method for preparing 5N grade strontium chloride |
| CN109319819A (en) * | 2018-11-26 | 2019-02-12 | 南昌航空大学 | A kind of technology for preparing 6N grade strontium nitrate |
| CN109485082A (en) * | 2018-11-23 | 2019-03-19 | 南昌航空大学 | A kind of technique directly preparing 4N grades of strontium nitrates |
| CN111850296A (en) * | 2020-07-16 | 2020-10-30 | 乐山盛和稀土股份有限公司 | Method for recovering and preparing high-purity strontium compound from rare earth ore |
| CN112680594A (en) * | 2020-12-10 | 2021-04-20 | 四川省乐山锐丰冶金有限公司 | Method for preparing strontium carbonate by recovering strontium from bastnaesite |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304295C (en) * | 2004-02-03 | 2007-03-14 | 中国科学院过程工程研究所 | Method of producing iporganic strontium salt by using high barium high calcium celestine |
| CN100336920C (en) * | 2004-02-19 | 2007-09-12 | 中国科学院过程工程研究所 | Method for directly preparing high-purifying product by barium sulphide black grey water immersion |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2595089B1 (en) * | 1986-02-28 | 1990-11-02 | Rhone Poulenc Chimie | PROCESS FOR THE PURIFICATION OF A BARIUM SALT |
| FR2614550B1 (en) * | 1987-04-29 | 1989-06-09 | Rhone Poulenc Chimie | PROCESS FOR THE PURIFICATION OF A BARIUM SALT |
| US5169609A (en) * | 1991-06-19 | 1992-12-08 | The United States Of America As Represented By The United States Department Of Energy | Combined transuranic-strontium extraction process |
| US5344623A (en) * | 1993-06-15 | 1994-09-06 | The United States Of America As Represented By The United States Department Of Energy | Process for the extraction of strontium from acidic solutions |
-
1997
- 1997-09-05 CN CN97116891A patent/CN1087354C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673028A (en) * | 2015-11-09 | 2017-05-17 | 虔东稀土集团股份有限公司 | Preparation method of alkaline earth metal compound |
| CN109485082A (en) * | 2018-11-23 | 2019-03-19 | 南昌航空大学 | A kind of technique directly preparing 4N grades of strontium nitrates |
| CN109319818A (en) * | 2018-11-26 | 2019-02-12 | 南昌航空大学 | A kind of method for preparing 5N grade strontium chloride |
| CN109319819A (en) * | 2018-11-26 | 2019-02-12 | 南昌航空大学 | A kind of technology for preparing 6N grade strontium nitrate |
| CN111850296A (en) * | 2020-07-16 | 2020-10-30 | 乐山盛和稀土股份有限公司 | Method for recovering and preparing high-purity strontium compound from rare earth ore |
| CN111850296B (en) * | 2020-07-16 | 2022-02-25 | 乐山盛和稀土股份有限公司 | Method for recovering and preparing high-purity strontium compound from rare earth ore |
| CN112680594A (en) * | 2020-12-10 | 2021-04-20 | 四川省乐山锐丰冶金有限公司 | Method for preparing strontium carbonate by recovering strontium from bastnaesite |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1087354C (en) | 2002-07-10 |
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