CN101100707A - Saponification method of acidic extract for separating rare earth - Google Patents
Saponification method of acidic extract for separating rare earth Download PDFInfo
- Publication number
- CN101100707A CN101100707A CNA2007100254722A CN200710025472A CN101100707A CN 101100707 A CN101100707 A CN 101100707A CN A2007100254722 A CNA2007100254722 A CN A2007100254722A CN 200710025472 A CN200710025472 A CN 200710025472A CN 101100707 A CN101100707 A CN 101100707A
- Authority
- CN
- China
- Prior art keywords
- saponification
- extract liquid
- acid extract
- acid
- rare earth
- Prior art date
- 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.)
- Pending
Links
Images
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
Saponification of extracting liquid, especially for acid one of trcacting earth-rare to be separated, is carried out by: (1) mixing acid extracting material with diluting agent as acid extracting liquid, (2) adding water into magnesium oxide as saponifying liquid, and (3) mixing the both liquid said above and stirring uniformly, taking upper saponified organic-phase solution as acid extracting liquid. The advantages include (1) cheaper than ammonia and sodium hydroxide and by-product with simple components to be treated and recovered easily, and (2) widely available, e.g., hydrochloric acid, sulfuric acid or nitric acid system.
Description
Technical field
The present invention relates to a kind of method for saponification of extraction liquid, particularly a kind of Rare Earth Separation method for saponification of acid extract liquid.
Background technology
The Rare Earth Separation extraction process carries out under low acidic conditions, its extracting power and water balance acidity are inversely proportional to, rare earth ion of general extraction will be replaced three hydrogen ions and be entered water, increase along with acidity, extraction liquid extracting rare-earth ability descends rapidly, therefore will carry out saponification reaction to extraction liquid.The acid extract liquid that common Rare Earth Separation is used is made up of three parts, acidic extractant, thinner, saponifying agent, Rare Earth Separation generally comprises following step with the method for saponification of acid extract liquid at present: (1) mix: acidic extractant and thinner are fully mixed, prepare acid extract liquid; (2) mix: the saponification liquor of preparation acid extract liquid; (3) saponification reaction: will go up the two acid extract liquid prepared of step and the saponification liquor of acid extract liquid and mix, and carry out the saponification reaction of acid extract liquid, the saponification organic phase solution on upper strata is through saponified Rare Earth Separation acid extract liquid.In the method for saponification of present Rare Earth Separation with acid extract liquid, the saponifying agent that uses in the saponification liquor step of preparation acid extract liquid mainly contains ammoniacal liquor, sodium hydroxide, and they exist following defective: (1) cost height.Need when the shortcoming that first kind of ammoniacal liquor is made saponifying agent is saponification that waste water with all generations all evaporates, crystallization, the ammonium salt crystallization in the waste water is come out, could handle qualified discharge.The energy that consumes is too big, the processing cost height, and also very harsh to the requirement of equipment.The environmental protection treatment cost had reduced when the shortcoming that second kind of sodium hydroxide is made saponifying agent was saponification, but production cost increases huge, its production cost is compared with the ammoniacal liquor saponification, increased about 50% than ammoniacal liquor saponified production cost, the cost for wastewater treatment of comprehensive ammoniacal liquor, it is suitable substantially with the ammoniacal liquor saponification that the sodium hydroxide saponified is produced comprehensive cost, the cost height; (2) applicable scope is limited.The hydrochloric acid system rare earth extraction of making that is suitable for that has through the saponified extraction liquid separates usefulness, and what have is suitable for sulfuric acid system, and what have is suitable for nitric acid system, restricted application.Be not suitable for sulfuric acid system as sodium hydroxide.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the method for saponification of a kind of cost Rare Earth Separation low, applied widely with acid extract liquid is provided.
Realize that the above-mentioned purpose technical scheme is: a kind of Rare Earth Separation method for saponification of acid extract liquid, described method steps is as follows:
(1) mix: acidic extractant and thinner are fully mixed, prepare acid extract liquid;
(2) mix: make saponifying agent with magnesium oxide, in magnesium oxide, add the entry stirring and obtain magnesium hydroxide slurry, prepare the saponification liquor of acid extract liquid;
(3) saponification reaction: will go up the two acid extract liquid prepared of step and the saponification liquor of acid extract liquid and mix, and carry out the saponification reaction of acid extract liquid, upper strata saponified organic phase solution is the Rare Earth Separation extraction liquid.
Further, the acidic extractant described in the first step is a kind of among phosphorus oxygen type acidic extractant P204, the P507, or a kind of in the carboxylic-acid acidic extractant naphthenic acid, stearic acid, and described thinner is a kerosene, or the mixture of kerosene and isooctyl alcohol.
Further, the weight percent concentration of magnesium hydroxide slurry is 1%～10% in the second step mix.
Further, the temperature of the saponification reaction of acid extract liquid is 10 ℃～70 ℃ described in the 3rd step.
Further, the saponification reaction time in the saponification reaction of acid extract liquid is 10min～15min described in the 3rd step.
Further, the saponification value after the saponification reaction of acid extract liquid is 0.3N～0.6N described in the 3rd step.
Realize that the main technique equipment that the present invention needs is: make-up tank, soap tank etc.
After adopting technique scheme, have a lot of benefits: (1) cost is low.Magnesium oxide is made saponifying agent, and making saponifying agent with ammoniacal liquor, sodium hydroxide, to compare cost low, and the by product composition is single; Subsequent products is handled convenient, is convenient to recycle, and processing cost is lower equally; (2) applied widely.What the inventive method was prepared is applicable to the Rare Earth Separation of hydrochloric acid, sulfuric acid, nitric acid three big acid systems through saponified acid extract liquid, applied widely.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Major equipment: make-up tank, soap tank.
Embodiment one
As shown in Figure 1, a kind of Rare Earth Separation method for saponification of acid extract liquid, described method steps is as follows:
(1) mix: getting acid phosphorus oxygen type acidic extractant P204 by weight percentage is 30L, fully mixes 10min with diluent kerosene 60L, prepares acid extract liquid;
(2) mix: make saponifying agent with magnesium oxide, get magnesium oxide 0.72kg, add entry 71.28kg and stir in magnesium oxide, the weight percent concentration of preparing magnesium hydroxide slurry is the saponification liquor of 1% acid extract liquid;
(3) saponification reaction: will go up the two 90L acid extract liquid prepared of step and the saponification liquor of 72kg acid extract liquid and mix, carry out the saponification reaction of acid extract liquid, temperature in the saponification reaction is 10 ℃, fully stir, the saponification reaction time is 15min, clarify layering then, the saponification organic phase solution on upper strata is through saponified Rare Earth Separation acid extract liquid, extracted organic phase consist of P204 magnesium salts-P204-kerosene.The saponification value that records after the saponification reaction is 0.36N.
Embodiment two
As shown in Figure 1, a kind of Rare Earth Separation method for saponification of acid extract liquid, described method steps is as follows:
(1) mix: getting acid phosphorus oxygen type acidic extractant P507 by weight percentage is 30L, fully mixes 10min with diluent kerosene 30L, prepares acid extract liquid;
(2) mix: make saponifying agent with magnesium oxide, get magnesium oxide 0.8kg, add entry 7.2kg and stir in magnesium oxide, the weight percent concentration of preparing magnesium hydroxide slurry is the saponification liquor of 10% acid extract liquid;
(3) saponification reaction: will go up the two 60L acid extract liquid prepared of step and the saponification liquor of 8kg acid extract liquid and mix, carry out the saponification reaction of acid extract liquid, temperature in the saponification reaction is 70 ℃, fully stir, the saponification reaction time is 10min, clarify layering then, the saponification organic phase solution on upper strata is through saponified Rare Earth Separation acid extract liquid, extracted organic phase consist of P507 magnesium salts-P507-kerosene.The saponification value that records after the saponification reaction is 0.59N.
Embodiment three
As shown in Figure 1, a kind of Rare Earth Separation method for saponification of acid extract liquid, described method steps is as follows:
(1) mix: getting carboxylic-acid acidic extractant naphthenic acid by weight percentage is 50L, and with thinner isooctyl alcohol 50L, kerosene 150L fully mixes 10min, prepares acid extract liquid;
(2) mix: make saponifying agent with magnesium oxide, get magnesium oxide 1.7kg, add entry 19.55kg and stir in magnesium oxide, the weight percent concentration of preparing magnesium hydroxide slurry is the saponification liquor of 6% acid extract liquid;
(3) saponification reaction: will go up the two 250L acid extract liquid prepared of step and the saponification liquor of 21.25kg acid extract liquid and mix, carry out the saponification reaction of acidic extractant, temperature in the saponification reaction is 35 ℃, fully stir, the saponification reaction time is 12min, clarify layering then, the saponification organic phase solution on upper strata is through saponified Rare Earth Separation acid extract liquid, extracted organic phase consist of naphthenic acid magnesium salts-naphthenic acid-isooctyl alcohol-kerosene.The saponification value that records after the saponification reaction is 0.32N.
Embodiment four
As shown in Figure 1, a kind of Rare Earth Separation method for saponification of acid extract liquid, described method steps is as follows:
(1) mix: getting carboxylic-acid acidic extractant stearic acid by weight percentage is 30L, and with thinner isooctyl alcohol 30L, kerosene 90L fully mixes 10min, prepares acid extract liquid;
(2) mix: make saponifying agent with magnesium oxide, get magnesium oxide 1.5kg, add entry 28.5kg and stir in magnesium oxide, the weight percent concentration of preparing magnesium hydroxide slurry is the saponification liquor of 5% acid extract liquid;
(3) saponification reaction: will go up the two 150L acid extract liquid prepared of step and the saponification liquor of 30kg acid extract liquid and mix, carry out the saponification reaction of acid extract liquid, temperature in the saponification reaction is 40 ℃, fully stir, the saponification reaction time is 15min, clarify layering then, the saponification organic phase solution on upper strata is through saponified Rare Earth Separation acid extract liquid, extracted organic phase consist of stearic acid magnesium salts-stearic acid-isooctyl alcohol-kerosene.The saponification value that records after the saponification reaction is 0.45N.
Remove the various embodiments described above, other be equal to or adopting by equivalent the inventive method all within protection domain of the present invention.
Claims (6)
1, a kind of Rare Earth Separation method for saponification of acid extract liquid is characterized in that described method steps is as follows:
(1) mix: acidic extractant and thinner are fully mixed, prepare acid extract liquid;
(2) mix: make saponifying agent with magnesium oxide, in magnesium oxide, add the entry stirring and obtain magnesium hydroxide slurry, prepare the saponification liquor of acid extract liquid;
(3) saponification reaction: will go up the two acid extract liquid prepared of step and the saponification liquor of acid extract liquid and mix, and carry out the saponification reaction of acid extract liquid, upper strata saponified organic phase solution is the Rare Earth Separation extraction liquid.
2, according to the method for saponification of the described Rare Earth Separation of claim 1 with acid extract liquid, it is characterized in that: the acidic extractant described in the first step is a kind of among phosphorus oxygen type acidic extractant P204, the P507, or a kind of in the carboxylic-acid acidic extractant naphthenic acid, stearic acid, described thinner is a kerosene, or the mixture of kerosene and isooctyl alcohol.
3, according to the method for saponification of the described Rare Earth Separation of claim 1 with acid extract liquid, it is characterized in that: the weight percent concentration of magnesium hydroxide slurry is 1%～10% in the second step mix.
4, according to the method for saponification of the described Rare Earth Separation of claim 1 with acid extract liquid, it is characterized in that: the temperature of the saponification reaction of acid extract liquid is 10 ℃～70 ℃ described in the 3rd step.
5, according to the method for saponification of the described Rare Earth Separation of claim 1 with acid extract liquid, it is characterized in that: the saponification reaction time described in the 3rd step in the saponification reaction of acid extract liquid is 10min～15min.
6, according to the method for saponification of the described Rare Earth Separation of claim 1 with acid extract liquid, it is characterized in that: the saponification value described in the 3rd step after the saponification reaction of acid extract liquid is 0.3N～0.6N.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100254722A CN101100707A (en) | 2007-08-01 | 2007-08-01 | Saponification method of acidic extract for separating rare earth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100254722A CN101100707A (en) | 2007-08-01 | 2007-08-01 | Saponification method of acidic extract for separating rare earth |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101100707A true CN101100707A (en) | 2008-01-09 |
Family
ID=39035154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100254722A Pending CN101100707A (en) | 2007-08-01 | 2007-08-01 | Saponification method of acidic extract for separating rare earth |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101100707A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102758083A (en) * | 2012-08-01 | 2012-10-31 | 中冶东方工程技术有限公司 | Method for transforming rare earth concentrated sulfuric acid roasted ores |
| CN105624439A (en) * | 2014-10-27 | 2016-06-01 | 有研稀土新材料股份有限公司 | Method for separating low-concentration rare earth ions by using magnetic fluid 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 |
| CN108862337A (en) * | 2018-08-21 | 2018-11-23 | 广西银亿新材料有限公司 | A method of pyrolysis magnesium sulfate prepares high-purity magnesium oxide |
| CN108950251A (en) * | 2018-08-01 | 2018-12-07 | 连云港高品再生资源有限公司 | The recovery method of rare earth element |
-
2007
- 2007-08-01 CN CNA2007100254722A patent/CN101100707A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102758083A (en) * | 2012-08-01 | 2012-10-31 | 中冶东方工程技术有限公司 | Method for transforming rare earth concentrated sulfuric acid roasted ores |
| CN102758083B (en) * | 2012-08-01 | 2014-09-03 | 中冶东方工程技术有限公司 | Method for transforming rare earth concentrated sulfuric acid roasted ores |
| CN105624439A (en) * | 2014-10-27 | 2016-06-01 | 有研稀土新材料股份有限公司 | Method for separating low-concentration rare earth ions by using magnetic fluid 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 |
| CN108950251A (en) * | 2018-08-01 | 2018-12-07 | 连云港高品再生资源有限公司 | The recovery method of rare earth element |
| CN108950251B (en) * | 2018-08-01 | 2021-08-24 | 连云港高品再生资源有限公司 | Method for recovering rare earth elements |
| CN108862337A (en) * | 2018-08-21 | 2018-11-23 | 广西银亿新材料有限公司 | A method of pyrolysis magnesium sulfate prepares high-purity magnesium oxide |
| CN108862337B (en) * | 2018-08-21 | 2020-11-06 | 广西银亿新材料有限公司 | Method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102766766B (en) | Non-saponification rare earth extraction separation process | |
| CN106367622B (en) | It is a kind of using aluminum sulfate as the ion adsorption type re efficient green extracting method of leaching agent | |
| CN101100707A (en) | Saponification method of acidic extract for separating rare earth | |
| WO2013177729A1 (en) | Method for separating rare-earth by coupled recycling of materials | |
| CN1872377B (en) | Method for saponifying extraction agent | |
| CN106319218A (en) | Method for recovering rare earth, aluminum and silicon from rare earth-containing aluminum and silicon wastes | |
| CN104775026A (en) | Method for extracting high-purity uranium, thorium and mixed rare earths from excellent molten slag | |
| CN109554556B (en) | Extraction separation method of rare earth elements | |
| CN104878197B (en) | Ultrasonic-assisted method for leaching potassium at low temperature under normal pressure | |
| CN105543476A (en) | Mixed extraction agents used for separating Y and method for extracting and separating Y from rare earth feed liquid | |
| CN102382979B (en) | Technique for extracting rare earth from rare earth tailing and preparing calcium sulfate whiskers | |
| CN104046806B (en) | A kind of method of recovering rare earth from waste aluminum hydrochlorate green rare-earth fluorescent powder | |
| CN107475540B (en) | A kind of technique of titanium white devil liquor recovery vanadium and titanium | |
| CN111020196B (en) | Method for separating thorium and enriching rare earth from radioactive waste residue leachate based on POAA | |
| CN103215451B (en) | Recovery method of rare earth elements in ionic rare earth smelting acid dissolution slag | |
| CN103938217A (en) | Neutral rust remover | |
| CN103740938A (en) | Method for recovering cobalt in cobalt carbonate production wastewater by saponification-free solvent extraction method | |
| JP5684885B1 (en) | Rare earth extractant and rare earth extraction method | |
| CN102925685A (en) | Compound solvent for extraction separation of tungsten and molybdenum and using method thereof | |
| CN113354024A (en) | Method for preparing nickel nitrate by using electroplating wastewater | |
| CN106222412A (en) | A kind of from containing the method for extracting vanadium vanadium solution | |
| CN1891839A (en) | Extracting agent for metal extraction, and its method and use | |
| CN107758719B (en) | A kind of environmentally friendly extracting process of high-purity ceria | |
| CN102936052B (en) | Method for recycling carboxymethylcellulose production wastewater | |
| CN108070718A (en) | A kind of method of molybdenum in double-aqueous phase system extract and separate aqueous solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |