CN1730681A - Production method of acid extractant saponifying organic phase used in rare earth extraction separation - Google Patents
Production method of acid extractant saponifying organic phase used in rare earth extraction separation Download PDFInfo
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- CN1730681A CN1730681A CNA2004100509484A CN200410050948A CN1730681A CN 1730681 A CN1730681 A CN 1730681A CN A2004100509484 A CNA2004100509484 A CN A2004100509484A CN 200410050948 A CN200410050948 A CN 200410050948A CN 1730681 A CN1730681 A CN 1730681A
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- acidic extractant
- saponification
- organic phase
- rare earth
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a process for acidic extracting agent saponified organic phase in rare earth extraction separation, which comprises, (1) acidic extracting agent solution preparation, consisting of mixing acidic extracting agent, kerosene, alcoholic solution, (2) preparation of saponification liquor of the acidic extracting agent, consisting of charging chlorides, calcium carbonate or calcium hydroxide, calcium oxide or magnesium carbonate, magnesium hydroxide, magnesium oxide into a mixing tank, charging right amount of water, fully stirring, (3) saponification of acidic extracting agent, consisting of loading the acidic extracting agent solution and the saponification liquor of the acidic extracting agent into an extraction tank, controlling the reaction temperature and fully stirring, stewing and separating the upper layer acidic extracting agent.
Description
Technical field
The present invention relates to be used for the isolating acidic extractant of rare earth extraction, particularly a kind of rare earth extraction separates the making method of acidic extractant saponification organic phase.
Background technology
The method of extracting and separating carbonated rare earth and rare earth oxide is to adopt technical hydrochloric acid and carbonated rare earth or rare earth oxide to carry out chemical reaction at present, makes it to become the water re chloride.Carry out chemical reaction with sodium hydroxide or aqua ammonia and acidic extractant, making it to become has the saponification organic phase solution.Above-mentioned water re chloride and above-mentioned saponification organic phase solution and hydrochloric acid,, reach the isolating purpose of the rare earth extraction in carbonated rare earth or the rare earth oxide by the method for fractionation extraction.The shortcoming of aforesaid method is a complex process, and the consumption of hydrochloric acid, sodium hydroxide is big, separates 1 ton of rare earth oxide and need consume 10 tons of hydrochloric acid and 10 tons of sodium hydroxide or aqua ammonia, and cost is higher, also adverse environment protection.
Summary of the invention
The objective of the invention is at above-mentioned traditional method complex process, consume the shortcoming that chemical solvents is many, cost is high, work out the making method that a kind of rare earth extraction separates acidic extractant saponification organic phase, technology is simple, avoid sodium hydroxide or aqua ammonia, particularly ammonia nitrogen reduces cost to the pollution of environment.
The object of the present invention is achieved like this:
1, preparation acid extract agent solution
By acidic extractant solution weight per-cent:
Take by weighing the acidic extractant of 30-60, acidic extractant comprises: extraction agent P507, extraction agent P204, extraction agent P272, extraction agent naphthenic acid; Take by weighing kerosene or the kerosene of 10-60 and the alcohols of 10-30 of 40-70, comprise isooctyl alcohol, secondary octanol.
Above-mentioned acidic extractant and kerosene or kerosene, alcoholic solution are mixed, fully stirred 10 to 50 minutes, organic phase promptly is that concentration is the acid extract agent solution of 0.1M to 2M.
2, the saponification liquid of preparation acidic extractant
By adding weight percent meter before the water:
Take by weighing the muriate of 1-20, comprise sodium-chlor, calcium chloride or ammonium chloride or other muriates;
Take by weighing the lime carbonate of 1-20 or calcium hydroxide, calcium oxide or magnesiumcarbonate, magnesium hydroxide, magnesium oxide;
Pack in the mixing tank, add an amount of water, fully mix and stir the saponified liquid of making acidic extractant.
3, the saponification of acidic extractant
By acidic extractant and saponification liquid total weight percent:
The saponification liquid of above-mentioned acid extract agent solution and acidic extractant is packed in the extractor, 10 to 50 ℃ of control reaction temperature, fully mix stir 10 to 60 minutes after, acidic extractant static, that separate the upper strata is the saponification organic phase, be used for the rare earth extraction of carbonated rare earth or rare earth oxide is separated, isolating muriate water is reusable.
Adopt rare earth extraction of the present invention to separate the making method of acidic extractant saponification organic phase, not only technology is simple but also the muriate water is reusable, reduces the pollution of chemical substance to environment, reduces production costs.
Specific embodiments
Embodiment 1:
Item Weight is by kilogram (down with),
1, preparation acid extract agent solution
Take by weighing extraction agent P507:200 kilogram, kerosene: 200 kilograms, mix, fully stirred 30 minutes, organic phase promptly is that concentration is the acid extract agent solution of 1.5M.
2, the saponification liquid of preparation acidic extractant
Take by weighing 10 kilograms in sodium-chlor, 6 kilograms in calcium oxide, in the mixing tank of packing into, add 84 kilograms of entry, fully mix and stir the saponification liquid of making acidic extractant.
3. the saponification of acidic extractant
400 kilograms of above-mentioned acidic extractants and 100 kilograms of saponification liquid are packed in the extractor, 40 ℃ of control reaction temperature, fully mix stir 30 minutes after, static, as to separate upper strata saponification organic phase, be used for the rare earth extraction of carbonated rare earth or rare earth oxide is separated, isolating muriate water is reusable.
Embodiment 2:
Item Weight is by kilogram (down with),
2, preparation acid extract agent solution
Take by weighing extraction agent P272:100 kilogram, P507:100 kilogram kerosene: 200 kilograms, mix, fully stirred 30 minutes, organic phase promptly is that concentration is the acid extract agent solution of 1.5M.
2, the saponification liquid of preparation acidic extractant
Take by weighing 10 kilograms of ammonia chlorides, 10 kilograms in calcium hydroxide, in the mixing tank of packing into, add 80 kilograms of entry, fully mix and stir the saponification liquid of making acidic extractant.
3. the saponification of acidic extractant
400 kilograms of above-mentioned acidic extractants and 100 kilograms of saponification liquid are packed in the extractor, 40 ℃ of control reaction temperature, fully mix stir 30 minutes after, static, as to separate upper strata saponification organic phase, be used for the rare earth extraction of carbonated rare earth or rare earth oxide is separated, isolating muriate water is reusable.
Embodiment 3:
Item Weight is by kilogram (down with),
3, preparation acid extract agent solution
Take by weighing extraction agent P204:200 kilogram, kerosene: 200 kilograms, mix, fully stir 30
Minute, organic phase promptly is that concentration is the acid extract agent solution of 1.5M.
2, the saponification liquid of preparation acidic extractant
Take by weighing 10 kilograms in magnesium chloride, 4 kilograms in magnesium oxide, in the mixing tank of packing into, add 86 kilograms of entry, fully mix and stir the saponification liquid of making acidic extractant.
3. the saponification of acidic extractant
400 kilograms of above-mentioned acidic extractants and 100 kilograms of saponification liquid are packed in the extractor, 40 ℃ of control reaction temperature, fully mix stir 30 minutes after, static, as to separate upper strata saponification organic phase, be used for the rare earth extraction of carbonated rare earth or rare earth oxide is separated, isolating muriate water is reusable.
Embodiment 4:
Item Weight is by kilogram (down with),
4, preparation acid extract agent solution
Take by weighing the extraction agent naphthenic acid: 100 kilograms, secondary octanol: 100 kilograms, kerosene: 200 kilograms, mix, fully stirred 30 minutes, organic phase promptly is that concentration is the acid extract agent solution of 0.75M.
2, the saponification liquid of preparation acidic extractant
Take by weighing 10 kilograms in calcium chloride, 10 kilograms in lime carbonate, in the mixing tank of packing into, add 80 kilograms of entry, fully mix and stir the saponification liquid of making acidic extractant.
3. the saponification of acidic extractant
400 kilograms of above-mentioned acidic extractants and 100 kilograms of saponification liquid are packed in the extractor, 40 ℃ of control reaction temperature, fully mix stir 30 minutes after, static, as to separate upper strata saponification organic phase, be used for the rare earth extraction of carbonated rare earth or rare earth oxide is separated, isolating muriate water is reusable.
Embodiment 5:
Item Weight is by kilogram (down with),
5, preparation acid extract agent solution
Take by weighing extraction agent P507:200 kilogram, isooctyl alcohol: 80 kilograms, kerosene: 120 kg, mix, fully stirred 30 minutes, organic phase promptly is that concentration is the acid extract agent solution of 1.5M.
2, the saponification liquid of preparation acidic extractant
Take by weighing 10 kilograms in sodium-chlor, 8 kilograms of magnesium hydroxides, in the mixing tank of packing into, add 82 kilograms of entry, fully mix and stir the saponification liquid of making acidic extractant.
3. the saponification of acidic extractant
400 kilograms of above-mentioned acidic extractants and 100 kilograms of saponification liquid are packed in the extractor, 40 ℃ of control reaction temperature, fully mix stir 30 minutes after, static, as to separate upper strata saponification organic phase, be used for the rare earth extraction of carbonated rare earth or rare earth oxide is separated, isolating muriate water is reusable.
Claims (4)
1, rare earth extraction separates the making method of acidic extractant saponification organic phase, it is characterized in that:
(1), preparation acid extract agent solution
By acidic extractant solution weight per-cent:
Take by weighing the acidic extractant of 30-60, take by weighing kerosene or the kerosene of 10-60 and the alcohols of 10-30 of 40-70, above-mentioned acidic extractant and kerosene or kerosene, alcoholic solution are mixed, fully stirred 10 to 50 minutes, organic phase promptly is that concentration is the acid extract agent solution of 0.1M to 2M;
(2), the saponification liquid of preparation acidic extractant
By adding weight percent meter before the water:
Take by weighing the muriate of 1-20, take by weighing the lime carbonate of 1-20 or calcium hydroxide, calcium oxide or magnesiumcarbonate, magnesium hydroxide, magnesium oxide, in the mixing tank of packing into, add an amount of water, fully mix and stir the saponified liquid of making acidic extractant;
(3), the saponification of acidic extractant
By acidic extractant and saponification liquid total weight percent:
The saponification liquid of above-mentioned acid extract agent solution and acidic extractant is packed in the extractor, 10 to 50 ℃ of control reaction temperature, fully mix stir 10 to 60 minutes after, acidic extractant static, that separate the upper strata is the saponification organic phase.
2, rare earth extraction according to claim 1 separates the making method of acidic extractant saponification organic phase, and it is characterized in that: above-mentioned muriate comprises sodium-chlor, calcium chloride or ammonium chloride.
3, rare earth extraction according to claim 1 separates the making method of acidic extractant saponification organic phase, and it is characterized in that: above-mentioned acidic extractant comprises: extraction agent P507, extraction agent P204, extraction agent P272, extraction agent naphthenic acid.
4, rare earth extraction according to claim 1 separates the making method of acidic extractant saponification organic phase, and it is characterized in that: above-mentioned alcohols comprises isooctyl alcohol, secondary octanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100509484A CN1323175C (en) | 2004-08-04 | 2004-08-04 | Production method of acid extractant saponifying organic phase used in rare earth extraction separation |
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| CNB2004100509484A CN1323175C (en) | 2004-08-04 | 2004-08-04 | Production method of acid extractant saponifying organic phase used in rare earth extraction separation |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008101396A1 (en) * | 2007-02-08 | 2008-08-28 | General Research Institute For Nonferrous Metals | Preprocessing method of an organic extractant and the preprocessed product and the use thereof |
| CN101260466B (en) * | 2007-02-08 | 2010-07-14 | 有研稀土新材料股份有限公司 | Pretreatment method for organic extracting agent and application thereof |
| CN101948483A (en) * | 2010-08-20 | 2011-01-19 | 王德兴 | Method for preparing calcium soap by utilizing quick lime and method for processing produced emulsified compound |
| CN102071314A (en) * | 2011-01-31 | 2011-05-25 | 赣州力赛科新技术有限公司 | Alkaline earth metal saponification and extraction method of acidic extractant |
| CN103103351A (en) * | 2013-01-31 | 2013-05-15 | 福建省长汀金龙稀土有限公司 | Method for preparing high-purity calcium carbonate for saponifying rare earth extraction agent |
| CN101319276B (en) * | 2007-06-04 | 2013-06-19 | 北京有色金属研究总院 | Preextraction method for organic extraction agent, product and uses thereof |
| CN106756012A (en) * | 2016-11-25 | 2017-05-31 | 桂林理工大学 | A kind of method of P204/P507 calcium and magnesiums saponification |
| CN106957969A (en) * | 2017-05-17 | 2017-07-18 | 中铝稀土（江苏）有限公司 | A kind of method of separation of rare earth elements |
| CN107400779A (en) * | 2017-06-30 | 2017-11-28 | 中铝广西有色金源稀土有限公司 | A kind of calcium carbonate saponification P507 method |
| CN108977673A (en) * | 2018-07-24 | 2018-12-11 | 南昌航空大学 | The method of rare earth in collaboration leaching ion adsorption type re raw ore |
| CN115341109A (en) * | 2022-08-30 | 2022-11-15 | 四川江铜稀土有限责任公司 | Method for producing low-calcium lanthanum in rare earth industrial production |
| CN115522051A (en) * | 2022-08-27 | 2022-12-27 | 萍乡鑫森新材料有限责任公司 | Method for saponifying and extracting rare earth |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1008083B (en) * | 1987-11-22 | 1990-05-23 | 江西省稀土研究所 | Rare-earth separating method with multiple outlets by one step extraction |
| CN1015436B (en) * | 1989-03-20 | 1992-02-12 | 甘肃稀土公司 | Method for separating si, ca, la from yb by extraction |
| CN1060876A (en) * | 1991-11-05 | 1992-05-06 | 冶金工业部包头稀土研究院 | The preparation method of Samarium trioxide |
-
2004
- 2004-08-04 CN CNB2004100509484A patent/CN1323175C/en not_active Expired - Fee Related
Cited By (16)
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| US20100003176A1 (en) * | 2007-02-08 | 2010-01-07 | Xiaowei Huang | Process for pretreating organic extractants and its product and application |
| CN101260466B (en) * | 2007-02-08 | 2010-07-14 | 有研稀土新材料股份有限公司 | Pretreatment method for organic extracting agent and application thereof |
| WO2008101396A1 (en) * | 2007-02-08 | 2008-08-28 | General Research Institute For Nonferrous Metals | Preprocessing method of an organic extractant and the preprocessed product and the use thereof |
| AU2008217450B2 (en) * | 2007-02-08 | 2012-09-20 | Grirem Advanced Materials Co., Ltd | Pretreatment process for organic extractants and the pretreated products and the use thereof |
| CN101319276B (en) * | 2007-06-04 | 2013-06-19 | 北京有色金属研究总院 | Preextraction method for organic extraction agent, product and uses thereof |
| CN101948483A (en) * | 2010-08-20 | 2011-01-19 | 王德兴 | Method for preparing calcium soap by utilizing quick lime and method for processing produced emulsified compound |
| CN101948483B (en) * | 2010-08-20 | 2013-01-02 | 王德兴 | Method for preparing calcium soap by utilizing quick lime and method for processing produced emulsified compound |
| CN102071314A (en) * | 2011-01-31 | 2011-05-25 | 赣州力赛科新技术有限公司 | Alkaline earth metal saponification and extraction method of acidic extractant |
| CN103103351A (en) * | 2013-01-31 | 2013-05-15 | 福建省长汀金龙稀土有限公司 | Method for preparing high-purity calcium carbonate for saponifying rare earth extraction agent |
| CN106756012A (en) * | 2016-11-25 | 2017-05-31 | 桂林理工大学 | A kind of method of P204/P507 calcium and magnesiums saponification |
| CN106957969A (en) * | 2017-05-17 | 2017-07-18 | 中铝稀土（江苏）有限公司 | A kind of method of separation of rare earth elements |
| CN107400779A (en) * | 2017-06-30 | 2017-11-28 | 中铝广西有色金源稀土有限公司 | A kind of calcium carbonate saponification P507 method |
| CN108977673A (en) * | 2018-07-24 | 2018-12-11 | 南昌航空大学 | The method of rare earth in collaboration leaching ion adsorption type re raw ore |
| CN115522051A (en) * | 2022-08-27 | 2022-12-27 | 萍乡鑫森新材料有限责任公司 | Method for saponifying and extracting rare earth |
| CN115341109A (en) * | 2022-08-30 | 2022-11-15 | 四川江铜稀土有限责任公司 | Method for producing low-calcium lanthanum in rare earth industrial production |
| CN115341109B (en) * | 2022-08-30 | 2023-09-15 | 中稀(凉山)稀土有限公司 | Method for producing low-calcium lanthanum in rare earth industrial production |
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| CN1323175C (en) | 2007-06-27 |
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