CN107400779A - A kind of calcium carbonate saponification P507 method - Google Patents
A kind of calcium carbonate saponification P507 method Download PDFInfo
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- CN107400779A CN107400779A CN201710521290.8A CN201710521290A CN107400779A CN 107400779 A CN107400779 A CN 107400779A CN 201710521290 A CN201710521290 A CN 201710521290A CN 107400779 A CN107400779 A CN 107400779A
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- Prior art keywords
- saponification
- calcium carbonate
- suspension
- mixed
- reaction
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- 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
Abstract
The invention discloses a kind of calcium carbonate saponification P507 method, belong to the method field of saponification organic phase.The method for aiming to provide the calcium carbonate saponification P507 that a kind of energy consumption is low, environmental pollution is small and cost is low.The technical program comprises the steps：Step 1：Calcium carbonate powder is mixed with water, sizes mixing to form suspension；Step 2：Suspension is mixed with P507, stirred, standing treats its reaction；Step 3：Levels are separated after its reaction completely, obtain the P507 after saponification.The present invention can be used for saponification P507 industrial production.
Description
Technical field
The present invention relates to the method field of saponification organic phase, especially a kind of calcium carbonate saponification P507 method.
Background technology
At present, China's rare earth extraction isolation technics level already belongs to world-class.However, nowadays the separation and Extraction uses
Most commonly used extractant is 2- ethylhexyl phosphoric acid list -2- ethylhexyls, and abbreviation P507, it belongs to acidic extractant, therefore
HA can be write a Chinese character in simplified form into as other organic acids.
It is if carrying out extracting rare-earth (RE) reaction using the P507 without saponification：3HA+RECl3=REA3+3HCl；Should
Process can release acid so as to influence extraction quantity.
Therefore, in order that organic matter P507 has certain preferable extraction quantity, before rare earth extraction separation is carried out, industry
Need its carrying out extraction saponification with alkali or salt in production.
At present, used saponification agent mainly has ammoniacal liquor (NH4OH), liquid caustic soda (NaOH), magnesium (MgO), calcium (Ca (OH)2).By
Strict regulation is carried out in being discharged to ammonia nitrogen waste water, many producers in present rare-earth trade are entered using cheap quick lime
Row is first digested to after white lime carries out saponification P507 again, and course of reaction is：
CaO+H2O=Ca (OH)2、Ca(OH)2+ 2HA=CaA2+2H2O。
It is well known that belonging to highly basic class making the pulverized limestone used in limewash, there is huge corrosiveness to human body, and
Manufactured limewash equally has very big harm to environment.
In addition, the production of pulverized limestone needs to need substantial amounts of energy consumption by lime stone high-temperature calcination, reaction principle is：
CaCO3→CaO+CO2。
The content of the invention
For above-mentioned deficiency, the present invention is intended to provide a kind of calcium carbonate saponification P507 method, this method energy consumption is low, to ring
It is low that small and cost is polluted in border.
In order to realize above-mentioned technique effect, technical scheme provided by the invention is such：A kind of calcium carbonate saponification P507
Method, it is characterised in that comprise the steps successively：
Step 1：Calcium carbonate powder is mixed with water, sizes mixing to form suspension；
Step 2：Suspension is mixed with P507, stirred, standing treats its reaction；
Step 3：Levels are separated after its reaction completely, obtain the P507 after saponification.
Preferably, the concentration of the suspension described in step 1 is 4~8mol/L.
Preferably, the concentration of the suspension described in step 1 is 6mol/L.
Preferably, the mixing speed described in step 1 is 40~50r/min, and mixing time is 20~30h.
Preferably, the mixing speed described in step 1 is 45r/min, mixing time 23h.
Preferably, Ca in the P507 and suspension described in step 22+Mixed proportion be 1L：0.225~0.25mol.
Preferably, Ca in the P507 and suspension described in step 22+Mixed proportion be 1L：0.225mol.
Preferably, the mixing speed described in step 2 be 40~50r/min, mixing time be 30~60min.
Preferably, the time of repose described in step 2 is 30min.
Preferably, the reaction temperature described in step 2 is 20~30 DEG C
Preferably, the reaction temperature described in step 2 is 25 DEG C.
Preferably, the mixing speed described in step 2 be 40r/min, mixing time 50min.
Preferably, the calcium carbonate powder described in step 1 is 200~1000 mesh.
Preferably, the calcium carbonate powder described in step 1 is 800 mesh.
The present invention carries out saponification P507 using calcium carbonate, and its reaction principle is：
CaCO3+ 2HA=CaA2+CO2+H2O。
The present invention has advantages below compared with conventional method：
1st, the technique carries out saponification using Paris white, does not use calcium lime powder, energy consumption is low, has to human and environment
Positive good action, protects environment；
2nd, the technique replaces calcium lime powder using Paris white, and its price is cheaper, is that company and relevant industries produce
Enormous benefits.
Embodiment
With reference to embodiment, claims of the present invention is described further, but not formed to this hair
Bright any restrictions, still any limited number of time modification made in the claims in the present invention protection domain, the right in the present invention
In claimed scope.
Embodiment 1：
Step 1：Calcium carbonate powder is mixed with water, sizes mixing to form suspension；
Step 2：Suspension is mixed with P507, stirred, standing treats its reaction；
Step 3：Levels are separated after its reaction completely, obtain the P507 after saponification.
Wherein, the concentration of the suspension described in step 1 is 6mol/L, and described mixing speed is 45r/min, mixing time
For 23h, described calcium carbonate powder is 800 mesh.
Wherein, Ca in the P507 and suspension described in step 22+Mixed proportion be 1L：0.225mol, described in step 2
Time of repose is 30min, and the reaction temperature described in step 2 is 25 DEG C, mixing speed described in step 2 is 40r/min, stirring when
Between be 50min.
Wherein, after the completion of the saponification described in step 3, upper strata is that organic phase lower floor is aqueous phase；Described separation method
For：Stratification and drain.
Embodiment 2：
Step 1：Calcium carbonate powder is mixed with water, sized mixing to formation suspension；
Step 2：Suspension is mixed with P507, stirred, standing treats its reaction；
Step 3：Levels are separated after its reaction completely, obtain the P507 after saponification.
Wherein, the concentration of the suspension described in step 1 is 4mol/L, and described mixing speed is 50r/min, mixing time
For 20h；Described calcium carbonate powder is 1000 mesh.
Wherein, Ca in the P507 and suspension described in step 22+Mixed proportion be 1L：0.24mol；Stirring described in step 2
Mix speed be 40r/min, mixing time 60min；Time of repose described in step 2 is 30min；Reaction temperature described in step 2
Spend for 20 DEG C.
Wherein, after the completion of the saponification described in step 4, upper strata is that organic phase lower floor is aqueous phase；Separation described in step 4
Method is：Stratification and drain.
Embodiment 3：
Step 1：Calcium carbonate powder is mixed with water, sized mixing to formation suspension；
Step 2：Suspension is mixed with P507, stirred, standing treats its reaction；
Step 3：Levels are separated after its reaction completely, obtain the P507 after saponification.
Wherein, the concentration of the suspension described in step 1 is 8mol/L, and described mixing speed is 40r/min, mixing time
For 30h；Described calcium carbonate powder is 200 mesh.
Wherein, Ca in the P507 and suspension described in step 22+Mixed proportion be 1L：0.25mol；Stirring described in step 2
Mix speed be 50r/min, mixing time 30min；Time of repose described in step 2 is 30min；Reaction temperature described in step 2
Spend for 30 DEG C.
Wherein, after the completion of the saponification described in step 4, upper strata is that organic phase lower floor is aqueous phase；Separation described in step 4
Method is：Stratification and drain.
Above-described is only presently preferred embodiments of the present invention, all timess done in the range of the spirit and principles in the present invention
What modifications, equivalent substitutions and improvements etc., should be included within the scope of the present invention.
Claims (10)
- A kind of 1. calcium carbonate saponification P507 method, it is characterised in that comprise the steps successively：Step 1：Calcium carbonate powder is mixed with water, sizes mixing to form suspension；Step 2：Suspension is mixed with P507, stirred, standing treats its reaction；Step 3：Levels are separated after its reaction completely, obtain the P507 after saponification.
- A kind of 2. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the suspension described in step 1 The concentration of liquid is 4~8mol/L.
- A kind of 3. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the suspension described in step 1 The concentration of liquid is 6mol/L.
- A kind of 4. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the stirring described in step 1 Speed is 40~50r/min, and mixing time is 20~30h.
- A kind of 5. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the stirring described in step 1 Speed is 45r/min, mixing time 23h.
- A kind of 6. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the P507 described in step 2 With Ca in suspension2+Mixed proportion be 1L：0.225~0.25mol.
- A kind of 7. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the P507 described in step 2 With Ca in suspension2+Mixed proportion be 1L：0.225mol.
- A kind of 8. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the stirring described in step 2 Speed is 40~50r/min, mixing time is 30~60min.
- A kind of 9. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the standing described in step 2 Time is 30min.
- A kind of 10. calcium carbonate saponification P507 according to claim 1 method, it is characterised in that the reaction described in step 2 Temperature is 20~30 DEG C.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730681A (en) * | 2004-08-04 | 2006-02-08 | 胡建康 | Production method of acid extractant saponifying organic phase used in rare earth extraction separation |
| US20100003176A1 (en) * | 2007-02-08 | 2010-01-07 | Xiaowei Huang | Process for pretreating organic extractants and its product and application |
| CN102041383A (en) * | 2010-12-31 | 2011-05-04 | 赣州有色冶金研究所 | Method for online saponification and Ca<2+> removal of extracting agent used for rare earth separation |
| 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 |
| CN104232949A (en) * | 2014-10-14 | 2014-12-24 | 包头稀土研究院 | Recycling method for rare earth leaching and leaching water of sulfuric acid roasted rare earth ore concentrate |
| AU2016203453A1 (en) * | 2015-05-26 | 2016-12-15 | Grirem Advanced Materials Co., Ltd | Hydrometallurgy and separation method of rare earth ores |
| CN106676266A (en) * | 2015-11-09 | 2017-05-17 | 虔东稀土集团股份有限公司 | Extraction method |
| 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 |
-
2017
- 2017-06-30 CN CN201710521290.8A patent/CN107400779A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730681A (en) * | 2004-08-04 | 2006-02-08 | 胡建康 | Production method of acid extractant saponifying organic phase used in rare earth extraction separation |
| US20100003176A1 (en) * | 2007-02-08 | 2010-01-07 | Xiaowei Huang | Process for pretreating organic extractants and its product and application |
| CN102041383A (en) * | 2010-12-31 | 2011-05-04 | 赣州有色冶金研究所 | Method for online saponification and Ca<2+> removal of extracting agent used for rare earth separation |
| 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 |
| CN104232949A (en) * | 2014-10-14 | 2014-12-24 | 包头稀土研究院 | Recycling method for rare earth leaching and leaching water of sulfuric acid roasted rare earth ore concentrate |
| AU2016203453A1 (en) * | 2015-05-26 | 2016-12-15 | Grirem Advanced Materials Co., Ltd | Hydrometallurgy and separation method of rare earth ores |
| CN106676266A (en) * | 2015-11-09 | 2017-05-17 | 虔东稀土集团股份有限公司 | Extraction method |
| 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 |
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Application publication date: 20171128 |