CN1078498A - The new preparation method of mixed chlorinated rare earth - Google Patents
The new preparation method of mixed chlorinated rare earth Download PDFInfo
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- CN1078498A CN1078498A CN93104719A CN93104719A CN1078498A CN 1078498 A CN1078498 A CN 1078498A CN 93104719 A CN93104719 A CN 93104719A CN 93104719 A CN93104719 A CN 93104719A CN 1078498 A CN1078498 A CN 1078498A
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- rare earth
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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
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- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of is the method that main raw material prepares mixed chlorinated rare earth with the f_c_ce_la concentrate, be that concentrate is carried out pickling with impurity such as flush away calcium with dilute hydrochloric acid earlier, use 7-8N hydrochloric acid to dissolve the part rare earth compound then, filter, filtrate is stand-by, filter cake uses 50-70% sodium hydroxide solution to decompose again, make not by the whole ceriums of the molten residue of acid, rare earth compounds such as lanthanum are converted into rare-earth hydroxide, adding above-mentioned stand-by filtrate at last carries out molten entirely, add a small amount of sulfuric acid again to remove impurity such as barium salt, during repeated hydrogenation oxidation ammonia carries out and impurity such as deironing thorium, filter, filtrate concentrating forms.
Description
The present invention relates to the method for making of mixed chlorinated rare earth, particularly prepare the method for making of rare earth chloride from Sichuan Mianning rare earth ore concentrate.
In the prior art, be to decompose rare-earth mineral, make rare earth wherein all change into rare-earth hydroxide, use the above-mentioned oxyhydroxide of dissolving with hydrochloric acid again, make mixed chlorinated rare earth with excessive alkali lye for the ordinary method of preparation mixed chlorinated rare earth from bastnasite.The shortcoming of this method is that the consumption of acid and alkali is big, thereby the production cost height.
The object of the present invention is to provide a kind of method that from bastnasite, prepares mixed chlorinated rare earth.Its advantage is acid, and the alkali consumption is few, the yield height, and flow process is simple.
Embodiment of the present invention are as follows:
Be divided into four step operations: the first step is pickling; With the impurity such as calcium in the 0.5N hydrochloric acid flush away concentrate, generally be the raw material concentrate and the ratio of 0.5N hydrochloric acid content is 1: (2.5-3.5), temperature is controlled between 80-90 ℃, and churning time is about 0.5 hour.Filter then, abandon filtrate, get filter cake.
Second step was acidleach: the ore deposit filter cake that leaches pickling with 7-8N hydrochloric acid, the raw material concentrate is 1 with the ratio of 7-8N hydrochloric acid content: (1.5-1.8), temperature is controlled between 85-95 ℃, churning time 0.5-1 hour, filter then, the filtrate reservation that contains superfluous acid is stand-by, and filter cake descends operation to handle again, and filtrate at this moment generally is that part rare earth carbonate in the ore is converted into mixed chloride.
The 3rd step was that alkali transforms: be to be that the sodium hydroxide solution of 50-70% and second one the residue acidleach ore filter cake that goes out without acidleach react the generation rare-earth hydroxide with concentration, this step can be converted into rare-earth hydroxide with rare-earth minerals such as the residue cerium that goes out without acidleach in the ore, lanthanums.Wherein wt is 1 than the ore weight that is the first step with the solid sodium hydroxide ratio: 0.5-0.7.Temperature is controlled at 150-250 ℃, pressure be 0.1-0.5MPa(generally be contain in the concentrate cerium amount greatly then pressure and temp want high).The reactant washing is filtered, its filter cake is carried out next step operation handle.
The 4th step was molten entirely: the filter cake (rare-earth hydroxide) in second step is mixed with the solution of the first step acidleach and is heated to 85-95 ℃, make rare-earth hydroxide all be converted into mixed chlorinated rare earth, add a small amount of 50% sulfuric acid again, thoroughly to remove impurity such as barium, add aqua ammonia at last again and transfer PH4 to filter to abandon filter residue, then filtrate is concentrated and become mixed chlorinated rare earth of the present invention.
Following preference elaborates to the present invention, but does not limit the scope of the invention.
Example 1: with 1 kilogram of pulverizing is 200 purpose Sichuan Mianning rare earth ore concentrates (contain mix rare earth oxide are 55%), carries out pickling half an hour with 3 liters of 0.5N salt acid soak, and temperature is controlled at 85 ℃ ± 2 ℃, filter then, abandon the first step filtrate, get filter cake, add 1800 milliliters of 8N hydrochloric acid, be heated to 90 ℃, be incubated 45 minutes, filter, the second step filtrate keeps, filter cake adds 1000 milliliter of 60% sodium hydroxide solution, and control pressure is 0.15MPa, and temperature is 200 ℃, totally 0.5 hour, wash with water to neutrality, filter, abandon filtrate, filter cake adds the filtrate in second step, temperature is 90 ℃, and the content by lead in the concentrate and barium adds 50% sulfuric acid 0.1kg simultaneously, is incubated 0.5 hour, add ammoniacal liquor again and transfer PH4, filter, abandon filter residue, then filtrate is carried out the negative pressure condensing crystal and be mixed chlorinated rare earth yield 85% mass analysis of the present invention and see Table 1.
Example 2: with mixed rare earth oxide content is the concentrate that 60% f_c_ce_la concentrate replaces example 1, removes after adding sodium hydroxide solution, and pressure-controlling is at 0.3MPa, temperature is 220 ℃, all the other conditions are identical with example 1, and gained mixed chlorinated rare earth product yield is 85%, and mass analysis also sees Table 1.
Example 3: with mixed rare earth oxide content be 63% f_c_ce_la concentrate to replace the concentrate of example 1 to remove alkali reaction pressure be 0.4MPa, temperature is 240 ℃, all the other conditions are identical with example 1, the products obtained therefrom yield is 93%, mass analysis sees Table 1.
Table 1 mixed chlorinated rare earth product quality analysis of the present invention table (weight %)
Advantage of the present invention:
1. the consumption acids alkali number is little.
2. method is simple and reliable.
3. yield height.
4. product meets national standard fully.
Claims (6)
1, a kind of method for making of mixed chlorinated rare earth is characterized in that:
(1). the first step, carry out pickling earlier with the hydrochloric acid of 0.5N, temperature is 80-90 ℃.
(2). second step, carry out acidleach with the hydrochloric acid of 7-8N, temperature is 85-95 ℃.
(3). the 3rd step, transform with the 50-70% sodium hydroxide solution, pressure is 0.1-0.5MPa, temperature is 150-250 ℃.
(4). the 4th step, the pickling liquor in second step oxyhydroxide with the 3rd step to be reacted, temperature is 85-95 ℃, adding a small amount of sulfuric acid and aqua ammonia simultaneously in reaction, to transfer PH be 4 removal of impurities, filtration, filtrate concentrates.
2,, it is characterized in that the concentrate of the first step and the weight ratio of dilute hydrochloric acid are 1: (2.5-3.5) according to the method for making of claim 1.
3,, it is characterized in that the pickling concentrate in second step and the hydrochloric acid weight ratio of 7-8N are 1: (1.5-1.8) according to the method for making of claim 1.
4, according to the method for making of claim 1, it is characterized in that the acidleach filter cake in the 3rd step carries out normal pressure or the decomposition of pressurization alkali, its pressure is 0.1-0.5MPa.Temperature is 150-250 ℃.
5,, it is characterized in that the 4th step went on foot pickling liquor with second and the alkali resolvent in the 3rd step reacts according to the method for making of claim 1.
6, according to the method for making of claim 1, it is characterized in that the 4th step remove miscellaneous operation and complete molten operation steps is carried out simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93104719A CN1078498A (en) | 1993-05-08 | 1993-05-08 | The new preparation method of mixed chlorinated rare earth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93104719A CN1078498A (en) | 1993-05-08 | 1993-05-08 | The new preparation method of mixed chlorinated rare earth |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1078498A true CN1078498A (en) | 1993-11-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93104719A Pending CN1078498A (en) | 1993-05-08 | 1993-05-08 | The new preparation method of mixed chlorinated rare earth |
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| CN (1) | CN1078498A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054887C (en) * | 1995-12-30 | 2000-07-26 | 内蒙古包钢稀土高科技股份有限公司 | Process for producing low-zinc and low-magnesium mixed rare-earth metal |
| CN1077546C (en) * | 1998-06-04 | 2002-01-09 | 葛新芳 | Method for producing mixed rare-earth chloride |
| CN100587090C (en) * | 2007-11-20 | 2010-02-03 | 中国地质科学院矿产综合利用研究所 | Comprehensive utilization process of bastnaesite and celestite paragenic ore |
| CN103184332A (en) * | 2013-03-29 | 2013-07-03 | 四川省彭山宇力化工有限公司 | Method for roasting, converting and resolving fluorocarbon cerium rare earth mine by adding covering agent to calcium compound |
| CN106145176A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | The technique that a kind of alkaline process processes monazite |
-
1993
- 1993-05-08 CN CN93104719A patent/CN1078498A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054887C (en) * | 1995-12-30 | 2000-07-26 | 内蒙古包钢稀土高科技股份有限公司 | Process for producing low-zinc and low-magnesium mixed rare-earth metal |
| CN1077546C (en) * | 1998-06-04 | 2002-01-09 | 葛新芳 | Method for producing mixed rare-earth chloride |
| CN100587090C (en) * | 2007-11-20 | 2010-02-03 | 中国地质科学院矿产综合利用研究所 | Comprehensive utilization process of bastnaesite and celestite paragenic ore |
| CN103184332A (en) * | 2013-03-29 | 2013-07-03 | 四川省彭山宇力化工有限公司 | Method for roasting, converting and resolving fluorocarbon cerium rare earth mine by adding covering agent to calcium compound |
| CN103184332B (en) * | 2013-03-29 | 2015-04-22 | 四川省彭山宇力化工有限公司 | Method for roasting, converting and resolving fluorocarbon cerium rare earth mine by adding covering agent to calcium compound |
| CN106145176A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | The technique that a kind of alkaline process processes monazite |
| CN106145176B (en) * | 2015-04-21 | 2019-07-16 | 永州市湘江稀土有限责任公司 | A kind of technique of alkaline process processing monazite |
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| SE01 | Entry into force of request for substantive examination | ||
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| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |