CN104591254A - Method for directly preparing rare earth chloride powder from rare earth chloride solution - Google Patents
Method for directly preparing rare earth chloride powder from rare earth chloride solution Download PDFInfo
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- CN104591254A CN104591254A CN201510083003.0A CN201510083003A CN104591254A CN 104591254 A CN104591254 A CN 104591254A CN 201510083003 A CN201510083003 A CN 201510083003A CN 104591254 A CN104591254 A CN 104591254A
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- China
- Prior art keywords
- rare earth
- earth chloride
- chloride
- powder
- spray
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/271—Chlorides
Abstract
The invention relates to a method for directly preparing rare earth chloride powder from a rare earth chloride solution, and belongs to the technical field of hydrometallurgy. The method comprises the following steps: the rare earth chloride solution is subjected to spray-drying through a spray-drying tower to form rare earth chloride powder, the rare earth chloride powder and drying hot air are separated through a cyclone separator with at least two stages, the finished product rare earth chloride powder flows out of a lower outlet of the cyclone separator, and dry gas exits from an upper outlet of the cyclone separator, enters a washing tower to be washed and cooled and is discharged by standard. According to the method, the rare earth chloride solution subjected to high-pressure atomization and the drying hot air enter the spray-drying tower, the moisture in the rare earth chloride solution is subjected to flash evaporation to form high-temperature water vapor and the rare earth chloride powder, the rare earth chloride powder and the drying hot air are subjected to air-solid separation through the cyclone separator with at least two stages under the action of a negative-pressure fan, the finished product rare earth chloride powder flows out of the lower outlet of the cyclone separator, and the gas is discharged by standard after being cooled and washed.
Description
Technical field
The present invention relates to a kind of method that re chloride directly prepares powder rare earth chloride, belong to hydrometallurgy (hydrometallurgy) technical field.
Background technology
current rare-earth trade does not also have re chloride directly to prepare the method for powder rare earth chloride, so industry blank has been filled up in this invention.
Current rare-earth trade is prepared solid chlorine rare earth and is substantially all adopted concentrating under reduced pressure technique, and this technique has following shortcoming: 1. energy consumption is higher.No matter be adopt thermal oil or steam as thermal source, all need to consume a large amount of energy in producing process, and thermosteresis in thermal source course of conveying is also very high, thermal utilization is very low, and this technique is intermittent type operation, so energy consumption is very high; 2. quality product has limitation.Adopt the solid chlorine rare earth that concentrating under reduced pressure mode is produced, REO content is generally about 45%, and water content is very high, and is block,
by after physical method fragmentation, solid particulate need be formed, do not reach the requirement of powder rare earth chloride,inconvenience is brought to the use of lower procedure.3. floor space is large.Due to the solid chlorine rare earth that concentrating under reduced pressure mode is produced, its cooling, cooling, crystallisation process is very long, so throughput and production site receive significant limitation; 4. production cost is high.The solid chlorine rare earth that concentrating under reduced pressure method is produced, cooling needs a large amount of hand breakings later, just can pack, so cost of labor and packaging, transportation cost are higher.5. security risk is high.Re chloride after concentrated is very high due to temperature, so in the process of crystallisation by cooling, employee's scald accident very easily occurs.
Summary of the invention
A kind of re chloride is the object of the present invention is to provide directly to prepare the method for powder rare earth chloride, the method energy-saving and environmental protection.
Technical solution:
Powder rare earth chloride is formed after the spray-dried tower spraying dry of re chloride of the present invention, powder rare earth chloride is together with dry-heat air, be separated through at least two stage cyclone separator, flow out finished powder body rare earth chloride by outlet under cyclonic separator, dry gas out enters qualified discharge after washing tower washing, cooling through cyclonic separator upper outlet.
The flow control that described re chloride enters spray-drying tower is 0.2 ~ 10m
3/ h.
Described spray-drying tower drying temperature is 200 ~ 600 DEG C.
Described re chloride is single re chloride or two kinds and two or more mixed chlorinated rare earth solution.
The powder rare earth chloride of institute of the present invention output can quick and complete dissolving in water.
The present invention be by re chloride after high-pressure atomization, jointly enter in spray-drying tower with dry-heat air, after moisture flash distillation contained by re chloride, form superheated vapor and powder rare earth chloride, under the effect of negative-pressure air fan, jointly carry out gas solid separation through at least two stage cyclone separator, flow out finished powder body rare earth chloride by outlet under cyclonic separator, gas is qualified discharge after overcooling washing.
Feature of the present invention is:
1, in production process, namely material has product output after dropping into, and can carry out technique adjustment in time, constant product quality, homogeneity is high, and achieves continuous seepage.
2, because heat exchange area in production process is large, achieve flash distillation, so heat utilization efficiency is very high, reduce energy consumption.
3, product is suitable for various forms of packaging, also can adopt fully-automatic packaging, reduce staff labor intensity, improve production on-site environment, eliminate potential safety hazard.
4, transportation cost and packing cost is reduced.
5, only need 2 ~ 3 operative employees completely, significantly reduce cost of labor.
6, product is powder rare earth chloride, improves product hierarchy, has filled up industry blank, for lower procedure is provided convenience.
Embodiment
Embodiment 1,
Get 5000L lanthanum chloride solution (REO percentage composition is 260g/l) ready stand-by.Start charging when spray-drying tower being warmed up to 300 DEG C, feed rate is 10L/min, and through dried powder rare earth chloride together with dry-heat air, after 1 grade of cyclonic separator, powder rare earth chloride flows out via outlet under cyclonic separator; Gas enters 2 grades of cyclonic separators, and powder rare earth chloride flows out via outlet under cyclonic separator; The finished product exporting outflow under 1 grade, 2 grades cyclonic separators is packed, 2 grades of cyclonic separator expellant gas qualified discharge after washing tower washing.Finished product Lanthanum trichloride REO content is 59.03% after testing, and dissolution rate is very fast, and solution is limpid and dissolving is complete.
Embodiment 2
Get 5000L lanthanum chloride solution (REO percentage composition is 260g/l) ready stand-by.By spray-drying tower intensification, temperature adjusts to 350 DEG C, and feed rate is 17L/min, is separated through 2 grades of cyclonic separators, and detecting finished product REO content is 52.56%, and dissolution rate is very fast, and solution is limpid and dissolving is complete.Mode of operation is with embodiment 1
Embodiment 3
Temperature adjusts to 400 DEG C, and feed rate is 17L/min, and detecting finished product REO content is 55.79%, and dissolution rate is very fast, and solution is limpid and dissolving is complete.Mode of operation is with embodiment 1
Embodiment 4
Temperature adjusts to 450 DEG C, and feed rate is 17L/min, and detecting finished product REO content is 59.34%, and dissolution rate is very fast, and solution is limpid and dissolving is complete.Mode of operation is with embodiment 1
Embodiment 5
Temperature adjusts to 620 DEG C, and feed rate is 17L/min, and detecting finished product REO content is 61.04%, and occur a small amount of insolubles, technical Analysis is Lanthanum monochloride monoxide.Mode of operation is with embodiment 1
Embodiment 6
Get 5000L lanthanum-cerium chloride solution (REO percentage composition is 302g/l) ready stand-by, start charging when spray-drying tower being warmed up to 300 DEG C, feed rate is 17L/min, and detecting finished product REO content is 51.07%, and dissolution rate is very fast, and solution is limpid and dissolving is complete.Mode of operation is with embodiment 1
6, temperature adjusts to 350 DEG C, and feed rate is 17L/min, and detecting finished product REO content is 53.89%, and dissolution rate is very fast, and solution is limpid and dissolving is complete.Mode of operation is with embodiment 1
7, temperature adjusts to 400 DEG C, and feed rate is 17L/min, and detecting finished product REO content is 57.07%, and dissolution rate is very fast, and solution is limpid and dissolving is complete.Mode of operation is with embodiment 1
8, temperature adjusts to 450 DEG C, and feed rate is 17L/min, and detecting finished product REO content is 59.87%, and dissolution rate is very fast, and solution is limpid and dissolving is complete.Mode of operation is with embodiment 1
9, temperature adjusts to 615 DEG C, and feed rate is 17L/min, and detecting finished product REO content is 62.58%, and dissolution rate is very fast, and occur a small amount of insolubles, technical Analysis is Lanthanum monochloride monoxide cerium.Mode of operation is with embodiment 1
Rare earth chloride in the present invention is the enriched substance of any one or two or more rare earth element in 15 kinds of rare earth elements.
Claims (5)
1. a re chloride directly prepares the method for powder rare earth chloride, it is characterized in that, powder rare earth chloride is formed after the spray-dried tower spraying dry of re chloride, powder rare earth chloride is together with dry-heat air, be separated through at least two stage cyclone separator, flow out finished powder body rare earth chloride by outlet under cyclonic separator, dry gas out enters qualified discharge after washing tower washing, cooling through cyclonic separator upper outlet.
2. a kind of re chloride directly prepares the method for powder rare earth chloride according to claim 1, it is characterized in that, the flow control that re chloride enters spray-drying tower is 0.2 ~ 10m
3/ h.
3. according to claims 1 or 2, a kind of re chloride directly prepares the method for powder rare earth chloride, it is characterized in that, spray-drying tower drying temperature is 200 ~ 600 DEG C.
4. a kind of re chloride directly prepares the method for powder rare earth chloride according to claim 1, it is characterized in that, described re chloride is single re chloride or two kinds and two or more mixed chlorinated rare earth solution.
5. a kind of re chloride directly prepares the method for powder rare earth chloride according to claim 1, it is characterized in that, the powder rare earth chloride of institute's output can quick and complete dissolving in water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510083003.0A CN104591254A (en) | 2015-02-16 | 2015-02-16 | Method for directly preparing rare earth chloride powder from rare earth chloride solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510083003.0A CN104591254A (en) | 2015-02-16 | 2015-02-16 | Method for directly preparing rare earth chloride powder from rare earth chloride solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104591254A true CN104591254A (en) | 2015-05-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510083003.0A Pending CN104591254A (en) | 2015-02-16 | 2015-02-16 | Method for directly preparing rare earth chloride powder from rare earth chloride solution |
Country Status (1)
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| CN (1) | CN104591254A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271354A (en) * | 2015-09-23 | 2016-01-27 | 北方稀土生一伦高科技有限公司 | Method for producing rare earth chloride powder |
| CN112499661A (en) * | 2020-12-21 | 2021-03-16 | 湖南中核金原新材料有限责任公司 | Preparation method of flaky chlorinated rare earth |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327950A (en) * | 2001-07-27 | 2001-12-26 | 中国科学院上海硅酸盐研究所 | Process for preparing spherical rare-earth compound with uniformly distributed components by spray reaction |
| WO2004016553A2 (en) * | 2002-08-14 | 2004-02-26 | Altair Nanomaterials Inc. | Rare earth metal compounds, methods of making, and methods of using the same |
| WO2006076964A2 (en) * | 2005-01-19 | 2006-07-27 | Merck Patent Gmbh | Method for producing mixed oxides by way of spray pyrolysis |
| CN103833064A (en) * | 2014-01-03 | 2014-06-04 | 东北大学 | Preparation method for rare earth oxide through jet pyrolysis of rare earth chloride solution |
-
2015
- 2015-02-16 CN CN201510083003.0A patent/CN104591254A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327950A (en) * | 2001-07-27 | 2001-12-26 | 中国科学院上海硅酸盐研究所 | Process for preparing spherical rare-earth compound with uniformly distributed components by spray reaction |
| WO2004016553A2 (en) * | 2002-08-14 | 2004-02-26 | Altair Nanomaterials Inc. | Rare earth metal compounds, methods of making, and methods of using the same |
| WO2006076964A2 (en) * | 2005-01-19 | 2006-07-27 | Merck Patent Gmbh | Method for producing mixed oxides by way of spray pyrolysis |
| CN103833064A (en) * | 2014-01-03 | 2014-06-04 | 东北大学 | Preparation method for rare earth oxide through jet pyrolysis of rare earth chloride solution |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271354A (en) * | 2015-09-23 | 2016-01-27 | 北方稀土生一伦高科技有限公司 | Method for producing rare earth chloride powder |
| CN112499661A (en) * | 2020-12-21 | 2021-03-16 | 湖南中核金原新材料有限责任公司 | Preparation method of flaky chlorinated rare earth |
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Application publication date: 20150506 |