CN100391847C - RE salt preparing process and apparatus - Google Patents
RE salt preparing process and apparatus Download PDFInfo
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- CN100391847C CN100391847C CNB2005100630331A CN200510063033A CN100391847C CN 100391847 C CN100391847 C CN 100391847C CN B2005100630331 A CNB2005100630331 A CN B2005100630331A CN 200510063033 A CN200510063033 A CN 200510063033A CN 100391847 C CN100391847 C CN 100391847C
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 150000003839 salts Chemical class 0.000 title claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 40
- 238000001556 precipitation Methods 0.000 claims abstract description 32
- -1 rare earth salt Chemical class 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 14
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 9
- 239000003595 mist Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 238000004062 sedimentation Methods 0.000 claims description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000000443 aerosol Substances 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 230000009189 diving Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 18
- 238000005516 engineering process Methods 0.000 abstract description 9
- 239000000047 product Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract 2
- 239000002244 precipitate Substances 0.000 abstract 2
- 238000003825 pressing Methods 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 description 4
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000001099 ammonium carbonate Substances 0.000 description 3
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- JJEJDZONIFQNHG-UHFFFAOYSA-N [C+4].N Chemical compound [C+4].N JJEJDZONIFQNHG-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 description 1
- OXHNIMPTBAKYRS-UHFFFAOYSA-H lanthanum(3+);oxalate Chemical compound [La+3].[La+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O OXHNIMPTBAKYRS-UHFFFAOYSA-H 0.000 description 1
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000009856 non-ferrous metallurgy Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a rare earth salt preparing method and a device which belong to the nonferrous metallurgical technology. The present invention has the technology that the concentration of prepared rare earth salt solution is from 0.04 to 1.2 mol/l, precipitant concentration is from 0.1 to 3.5 mol/l, and the prepared solutions are mixed for 3 to 30 minutes according to a mass flow rate of REO to precipitant of 1: 1.1 to 1.7; when temperature is from 15 DEG C to 60 DEG C and rotation speed is from 150 turns per minute to 890 turns per minute, the solution enters a clarifier for precipitation through a discharging opening of a mixer after being mixed for 3 to 30 minutes, the precipitate is pumped into a plate and frame press by a mud pump, and rare earth precipitation salts are obtained. The present invention has the devices that a material feeding hole and a precipitant feeding hole are arranged at the bottom part of a cylinder, the lower bottom end of a stirring paddle is provided with vortex flow stirring blades, the upper layer stirring blades are oblique blades, the central conic bottom of the cylinder is provided with a mixing sub-chamber, and the upper part of the cylinder is provided with a porous mist discharging plate. The present invention adopts fast precipitation and solid-liquid separation, realizes the serialization production of precipitates, improves the production capacity and production efficiency of the device, and improves the product quality. The filter pressing treatment for waste water avoids yield loss caused by control errors and simultaneously ensures the simplification of waste water treatment process.
Description
One, technical field
The invention belongs to nonferrous metallurgy technology, relate to the preparation method and the device for carrying out said of rare-earth salts.
Two, background technology
The production method that rare earth salts (single-element or complex element) adopts at present mainly contains following two kinds of methods: (1) earth solution directly adds solid precipitation (conversion) agent after allotment, forms rare earth salts; (2) earth solution directly adds precipitation (conversion) agent solution after allotment, forms rare earth salts.
In the existing precipitation process, adding along with precipitation agent, the deposition condition of different steps is changing, cause the variation that rare earth salts forms, and along with the earth solution density loss, precipitation agent adding speed improves or totally add-on is excessive, finally causes the rare earth salts crystallisation process to produce fluctuation, and quality product is inconsistent.With regard to multiple batches of, owing to can't reach the unanimity of operation, also produce difference between causing batch, strengthened the fluctuation of quality product.
The employing prior art is made directly mixing, periodical operation of the conventional employing of rare earth salts, and the forming process time is longer, and rare earth salts easily forms peritectoid, and attached procedures such as absorption cause quality product restive, and the quality fluctuation amplitude is big, and consistence is poor.In addition, take the batch operation process, must cause before and after the technology store, the transhipment amount increases, and stores, conversion unit is huge, the overall investment amount is big.It is big to form corresponding non-rare earths salt amount in precipitation (conversion) process, and concentration is low not easy to be recycled.
Three, summary of the invention
The technical problem that the present invention solves is: accurately control inlet amount, make separating of rare earth salts and non-rare earths salt, reach production process continuously, guarantee the consistence of quality product; Reduce processing step and solid-liquid separation number of times simultaneously, improved the rare earth yield, and improved the regeneration of non-rare earths salt.
The present invention produces rare-earth salts continuous precipitation method processing step:
Adopt following processing step:
(1) rare earths salt being formulated as concentration is 0.04-1.2mol/l, simultaneously precipitation agent is formulated as concentration 0.1-3.5mol/l;
(2) with the above-mentioned rare earths salt for preparing by material inlet, precipitation agent by the reagent opening for feed in mass rate ratio: REO: precipitation agent=1: 1.1-1.7 enters the mixing tank chamber of diving, temperature is 15-75 ℃, rotating speed is 150-890 rev/min, utilize the eddy current stirring rake with finishing mixing process by inclination stirring rake and traverse baffle in above-mentioned raw materials and the reagent suction cylindrical shell, mixed 3-30 minute;
(3) discharge port of mixture by mixing tank entered carry out sedimentation in the settler, the aerosol that reaction process produced is evenly got rid of by going out the mist plate;
(4) sedimentation is good material obtains precipitating rare earth salt by slush pump injection plate-and-frame filter press.
REO is rare earth oxide and its esters.
Rare earths salt is sulfuric acid rare earth, salt acid rare earth or rare earth nitrate.
Precipitation agent is bicarbonate of ammonia, oxalic acid, ammoniacal liquor, sodium hydroxide, sodium bicarbonate or yellow soda ash.
Produce the device of rare-earth salts, form by cylindrical shell, traverse baffle, material inlet, precipitation agent opening for feed, discharge port, material inlet and precipitation agent opening for feed are located at the cylindrical shell bottom, be positioned at that the bottom is the eddy current stirring rake under the stirring rake at cylindrical shell center, the upper strata blade is the inclination stirring rake, be provided with the latent chamber of mixing tank at the bottom of the cylindrical shell center cone, cylindrical shell top is provided with porous and goes out the mist plate.
Basic point choice of the present invention the solution precipitation mode that is easy to control, by allotment to material concentration and temperature, the allotment of precipitation agent concentration and temperature, make the starting condition that forms the precipitation salt reach consistent, utilize the flow of two kinds of materials of volume pump stepless control, finish the forming process of salt at short notice by high-speed mixing, the absorption and the peritectoid of harmful element have been overcome, and utilize centrifugal settling, centrifuging to finish the roughly the same separation of mother liquor of salt synchronously, guarantee the consistence of its physical properties and chemical property, thereby guarantee quality product.
The improvement of present device combines the advantage of conventional sedimentation, mixing equipment, and technological process is efficiently finished.Its technology has reduced the process and the solid-liquid separation number of times of former technology, has improved the rare earth yield.In addition, utilize ammonium bicarbonate solution to precipitate, eliminated the solubilizing reaction time of carbon ammonium in the former technology, quicken the heavy process of carbon, reduced in the precipitation process, improved quality product the containing and the absorption of non-rare earth impurity.Thereby cancelled next step washing procedure, controlled the generation of washes, improved waste water ammonium salt concentration relatively, reduced the total amount of waste water, for condition has been created in wastewater treatment.
The output product: 46.3 tons of REO 〉=45% of carbonated rare earth do not divide into groups
23.6 tons of REO 〉=45% of Phosbloc
14 tons of REO 〉=45% of cerous carbonate
9.3 tons of REO 〉=35% of Sedemesis
7.5 tons of REO 〉=35% of lanthanum oxalate
6 tons of REO 〉=75% of lanthanum hydroxide
The present invention takes the rapid subsidence solid-liquid separation, has fundamentally realized the continuity of technology, and the change batch operation is continuous operation, has improved the throughput of equipment, and production efficiency significantly improves.And the press filtration of waste water is handled, be the yield losses that brings for fear of the control error, also be in order to guarantee the simplification of wastewater treatment process simultaneously.
Four, description of drawings
Accompanying drawing 1 is process flow sheet of the present invention;
Accompanying drawing 2 is the structural representation of device of the present invention.
Five, embodiment
Embodiment 1: produce mixed rare earth carbonate continuous precipitation method processing step with the rare earth sulfuric acid salts solution:
(1) the sulfuric acid rare earth mixing solutions being formulated as concentration is 0.04-0.3mol/l, simultaneously precipitation agent bicarbonate of ammonia is formulated as concentration 1-1.5mol/l;
(2) the above-mentioned sulfuric acid rare earth mixing solutions for preparing is passed through reagent opening for feed 8 in mass rate ratio: REO: NH by material inlet 9, ammonium bicarbonate soln
4HCO
3=1: 1.3-1.7 enters the latent chamber 7 of mixing tank, and temperature is 15-45 ℃, and rotating speed is 350-750 rev/min, utilizes eddy current stirring rake 6 with finishing mixing process by inclination stirring rake 3 and traverse baffle 5 in above-mentioned raw materials and the reagent suction cylindrical shell 4, mixes 3-12 minute;
(3) will react the mixed rare earth carbonate that the generates discharge port 1 by mixing tank and enter and carry out sedimentation in the settler, the aerosol that reaction process produced is evenly got rid of by going out mist plate 2;
(4) sedimentation is good mixed rare earth carbonate obtains the mixed rare earth carbonate deposited salt by slush pump injection plate-and-frame filter press.
Embodiment 2: produce cerous carbonate continuous precipitation method processing step with cerous nitrate solution:
(1) cerous nitrate solution being formulated as concentration is 0.1-1mol/l, simultaneously precipitation agent bicarbonate of ammonia is formulated as concentration 1-3.5mol/l;
(2) the above-mentioned cerous nitrate solution for preparing is passed through reagent opening for feed 8 in mass rate ratio: REO: NH by material inlet 9, ammonium bicarbonate soln
4HCO
3=1: 1.3-1.7 enters the latent chamber 7 of mixing tank, and temperature is 25-50 ℃, and rotating speed is 255-600 rev/min, utilizes eddy current stirring rake 6 with finishing mixing process by inclination stirring rake 3 and traverse baffle 5 in above-mentioned raw materials and the reagent suction cylindrical shell 4, mixes 5-12 minute;
(3) will react the mixed rare earth carbonate that the generates discharge port 1 by mixing tank and enter and carry out sedimentation in the settler, the aerosol that reaction process produced is evenly got rid of by going out mist plate 2;
(4) sedimentation is good cerous carbonate obtains the cerous carbonate deposited salt by slush pump injection plate-and-frame filter press.
Embodiment 3: produce rare-earth oxalate continuous precipitation method processing step with solution of cerium chloride by oxidation:
(1) rare-earth chlorination cerium solution being formulated as concentration is 0.04-0.6mol/l, simultaneously precipitation agent oxalic acid is formulated as concentration 0.7-1.1mol/l;
(2) the above-mentioned solution of cerium chloride by oxidation for preparing is passed through reagent opening for feed 8 in mass rate ratio: REO: H by material inlet 9, oxalic acid solution
2C
2O
4=1: 1.1-1.6 enters the latent chamber 7 of mixing tank, and temperature is 15-75 ℃, and rotating speed is 180-325 rev/min, utilizes eddy current stirring rake 6 with finishing mixing process by inclination stirring rake 3 and traverse baffle 5 in above-mentioned raw materials and the reagent suction cylindrical shell 4, mixes 10-15 minute;
(3) will react the Sedemesis that the generates discharge port 1 by mixing tank and enter and carry out sedimentation in the settler, the aerosol that reaction process produced is evenly got rid of by going out mist plate 2;
(4) sedimentation is good Sedemesis obtains the Sedemesis deposited salt by slush pump injection plate-and-frame filter press.
Claims (4)
1. the preparation method of rare-earth salts is characterized in that: adopt following processing step:
(1) rare earths salt being formulated as concentration is 0.04-1.2mol/l, simultaneously precipitation agent is formulated as concentration 0.1-3.5mol/l;
(2) with the above-mentioned rare earths salt for preparing by material inlet (9), precipitation agent by reagent opening for feed (8) in mass rate ratio: REO: precipitation agent=1: 1.1-1.7 enters the mixing tank chamber (7) of diving, temperature is 15-75 ℃, rotating speed is 150-890 rev/min, utilize eddy current stirring rake (6) with finishing mixing process by inclination stirring rake (3) and traverse baffle (5) in above-mentioned raw materials and the reagent suction cylindrical shell (4), mixed 3-30 minute;
(3) discharge port (1) of mixture by mixing tank entered carry out sedimentation in the settler, the aerosol that reaction process produced is evenly got rid of by going out mist plate (2);
(4) sedimentation is good material obtains precipitating rare earth salt by slush pump injection plate-and-frame filter press.
2. the preparation method of rare-earth salts according to claim 1, it is characterized in that: rare earths salt is sulfuric acid rare earth, salt acid rare earth or rare earth nitrate.
3. the preparation method of rare-earth salts according to claim 1, it is characterized in that: precipitation agent is bicarbonate of ammonia, oxalic acid, ammoniacal liquor, sodium hydroxide, sodium bicarbonate or yellow soda ash.
4. implement the device of method according to claim 1 for one kind, form by cylindrical shell (4), traverse baffle (5), material inlet (9), precipitation agent opening for feed (8), discharge port (1), it is characterized in that: material inlet (9) and precipitation agent opening for feed (8) are located at cylindrical shell (4) bottom, be positioned at that the bottom is eddy current stirring rake (6) under the stirring rake at cylindrical shell (4) center, the upper strata blade is inclination stirring rake (3), be provided with the latent chamber (7) of mixing tank at the bottom of cylindrical shell (4) center cone, cylindrical shell (4) top is provided with porous and goes out mist plate (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100630331A CN100391847C (en) | 2005-04-05 | 2005-04-05 | RE salt preparing process and apparatus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100630331A CN100391847C (en) | 2005-04-05 | 2005-04-05 | RE salt preparing process and apparatus |
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| CN1847153A CN1847153A (en) | 2006-10-18 |
| CN100391847C true CN100391847C (en) | 2008-06-04 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101277294B1 (en) * | 2010-01-28 | 2013-06-20 | 주식회사 엘지화학 | Method for preparing cerium carbonate |
| CN101831543B (en) * | 2010-05-20 | 2012-09-26 | 宜兴市长江稀土冶炼厂 | Process for precipitating rare earth continuously |
| CN104418724B (en) * | 2013-08-19 | 2016-06-08 | 中铝稀土（常州）有限公司 | A kind of oxalic rare earth precipitates water wash system |
| CN103613113A (en) * | 2013-11-26 | 2014-03-05 | 内蒙古大学 | Preparation method of rare earth oxides or carbonic acid oxidized rare earth pearl pigments |
| CN103613112A (en) * | 2013-11-26 | 2014-03-05 | 内蒙古大学 | Simple preparation method of rare earth carbonate pearlescent pigment |
| CN103708526A (en) * | 2013-11-26 | 2014-04-09 | 内蒙古大学 | Preparation method for rare earth sulfide pearlescent pigment |
| CN107188215A (en) * | 2017-05-24 | 2017-09-22 | 中国北方稀土（集团）高科技股份有限公司 | The method that reaction end is automatically adjusted in carbonated rare earth continuous precipitation production process |
| CN109319820B (en) * | 2018-10-17 | 2019-12-17 | 常州市卓群纳米新材料有限公司 | Method for removing chloride ions in nano oxides by plate-and-frame filter pressing and washing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07144915A (en) * | 1993-11-24 | 1995-06-06 | Shin Etsu Chem Co Ltd | Production of cerium carbonate and cerium oxide |
| US20030161776A1 (en) * | 1999-12-29 | 2003-08-28 | Jean-Jacques Braconnier | Method for producing rare earth borates and use of the resulting borates in luminescence |
| CN1456510A (en) * | 2002-05-10 | 2003-11-19 | 淄博华庆粉体材料技术有限公司 | Process for preparing lanthanum hydroxide |
-
2005
- 2005-04-05 CN CNB2005100630331A patent/CN100391847C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07144915A (en) * | 1993-11-24 | 1995-06-06 | Shin Etsu Chem Co Ltd | Production of cerium carbonate and cerium oxide |
| US20030161776A1 (en) * | 1999-12-29 | 2003-08-28 | Jean-Jacques Braconnier | Method for producing rare earth borates and use of the resulting borates in luminescence |
| CN1456510A (en) * | 2002-05-10 | 2003-11-19 | 淄博华庆粉体材料技术有限公司 | Process for preparing lanthanum hydroxide |
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