CN115305366A - Production method of rare earth silicate ore - Google Patents
Production method of rare earth silicate ore Download PDFInfo
- Publication number
- CN115305366A CN115305366A CN202210992425.XA CN202210992425A CN115305366A CN 115305366 A CN115305366 A CN 115305366A CN 202210992425 A CN202210992425 A CN 202210992425A CN 115305366 A CN115305366 A CN 115305366A
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- CN
- China
- Prior art keywords
- rare earth
- ore
- phosphorus
- production method
- production
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Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 42
- -1 rare earth silicate Chemical class 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000006004 Quartz sand Substances 0.000 claims abstract description 9
- 239000010436 fluorite Substances 0.000 claims abstract description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011574 phosphorus Substances 0.000 claims abstract description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000003723 Smelting Methods 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229910052590 monazite Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- UXBZSSBXGPYSIL-UHFFFAOYSA-N phosphoric acid;yttrium(3+) Chemical compound [Y+3].OP(O)(O)=O UXBZSSBXGPYSIL-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of rare earth ore production, and discloses a production method of rare earth silicate ore. The method comprises mixing phosphorus-containing rare earth ore, quartz sand, carbon and fluorite, and melting at high frequency. The invention reacts the phosphorus-containing rare earth ore into the silicic acid rare earth ore, improves the dissolution recovery rate of the rare earth hydrochloride in the ore to more than 94 percent, and shortens the production flow; the rare earth silicate ore is obtained, and the production cost is reduced.
Description
Technical Field
The invention relates to the technical field of rare earth ore production, in particular to a production method of rare earth silicate ore.
Background
The rare earth chloride is produced by converting rare earth in ore into rare earth hydroxide by using sodium hydroxide, obtaining rare earth hydroxide ore, washing phosphate by using water, and dissolving the rare earth hydroxide ore by using hydrochloric acid. However, the rare earth recovery rate of the method is only about 90%, the process consumes a large amount of sodium hydroxide, the washing time is long, and the cost is too high.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a production method of rare earth silicate ore.
The rare earth silicate ore in the application refers to rare earth silicate obtained by reacting rare earth in rare earth phosphate ore with silicon dioxide, and is a raw material for producing rare earth chloride.
In order to achieve the purpose, the invention adopts the technical scheme that:
a process for preparing rare-earth silicate ore includes such steps as mixing phosphorus-contained rare-earth ore, quartz sand, carbon and fluorite, and high-frequency smelting reaction.
Preferably, the content of the rare earth oxide in the phosphorus-containing rare earth ore is 40-60%.
Preferably, the phosphorus-containing rare earth ore, the quartz sand, the carbon and the fluorite are mixed according to the weight ratio of 10 (1-2) to (0.5-1.5).
Preferably, the melting reaction is carried out at 1700-1800 ℃ for 30-40min.
The main chemical reactions of the production method adopted by the invention are as follows: (phosphorus of the reaction formula exceeds the boiling point)
Compared with the prior art, the invention has the following beneficial effects:
the production method of the invention enables the phosphorus-containing rare earth ore to react into the silicic acid rare earth ore, improves the dissolution recovery rate of the rare earth hydrochloric acid in the ore to be more than 94 percent, and shortens the production flow; the rare earth silicate ore is obtained, and the production cost is reduced.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments. It is to be understood that these descriptions are only illustrative and are not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
The recovery rate detection method used in the embodiment of the invention refers to GB/T14635.2-93.
The raw materials used in the embodiment of the invention comprise more than 95 percent of silicon dioxide in quartz sand, more than 80 percent of fixed carbon in carbon powder and more than 60 percent of calcium fluoride in fluorite;
example 1
Mixing 200g of monazite ore ground to 300 meshes, 30g of quartz sand, 30g of carbon powder (reducing agent) and 20g of fluorite (catalyst), wherein the total amount of rare earth in the monazite ore is 50%;
putting the mixed ore into a high-frequency furnace graphite crucible, electrifying, heating to melt the mixed ore, heating to 1720 ℃, keeping the temperature, reacting for 30 minutes, and discharging;
grinding the ore after the melting reaction to 300 meshes, fully sieving, and detecting that the REO content is 52%.
100g of ground ore powder is taken and added into a 1000mL beaker filled with 300mL of water, hydrochloric acid is added for stirring reaction, the acidity is kept at 0.7 mol for 3 hours, the reaction is complete, the slurry with complete reaction is filtered by a suction filter, a filter cake is washed for three times, 2100mL of filtrate is obtained, the content of REO detected is 23.77g per liter, 49.917g of rare earth is recovered, and the recovery rate is 95.99%.
Example 2
Mixing 200g of xenotime ground to 300 meshes, 30g of quartz sand, 30g of carbon powder and 20g of fluorite, wherein the content of rare earth in the xenotime is 46 percent;
putting the mixed ore into a high-frequency furnace graphite crucible, electrifying to heat up to melt the mixed ore, heating to 1720 ℃, and carrying out heat preservation reaction for 40 minutes to discharge;
grinding the ore after the melting reaction to 300 meshes, and detecting that the REO content is 47.3%.
100g of ground ore powder is put into a 1000mL beaker with 300mL of water, hydrochloric acid is added to stir and react, and the acidity is kept at 0.7 mol for three 3 hours without becoming complete reaction. And (3) carrying out suction filtration on the slurry with complete reaction by using a suction filter, washing a filter cake for 3 times to obtain 2005mL of filtrate, detecting that the content of REO is 22.41 g per liter, recovering 44.93 g of rare earth, and recovering 94.99 percent.
Example 3
Mixing 200g of monazite ground to 300 meshes, 35 g of quartz sand, 28 g of carbon powder and 20g of fluorite, wherein the content of rare earth in the monazite is 50%;
putting the mixed ore into a high-frequency furnace graphite crucible, electrifying, heating to melt the mixed ore, heating to 1800 ℃, keeping the temperature, reacting for 30 minutes, and discharging;
grinding the ore after the melting reaction to 300 meshes, and detecting that the content of REO is 50.8%.
100g of the reaction mixture was put into a 1000mL beaker containing 300mL of water, and hydrochloric acid was added thereto to stir the reaction mixture for 3 hours while maintaining the acidity of 0.7 mol until the reaction was completed. And (3) filtering the slurry which is completely reacted by using a suction filter, washing the filter cake for three times to obtain 2140mL of filtrate, wherein the content of REO detected by the filtrate is 22.46 g per liter, the rare earth is recovered by 48.06g, and the recovery rate of the rare earth is 94.6%.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. A process for preparing rare-earth silicate ore includes such steps as mixing phosphorus-contained rare-earth ore, quartz sand, carbon and fluorite, and high-frequency smelting reaction.
2. The method of claim 1, wherein the phosphorus-containing rare earth ore has a rare earth oxide content of 40 to 60%.
3. The method of claim 1, wherein the phosphorus-containing rare earth ore, the quartz sand, the carbon, and the fluorite are mixed in a weight ratio of 10 (1-2) to (0.5-1.5).
4. The production method according to claim 1, wherein the melting reaction is carried out at 1700 to 1800 ℃ for 30 to 40min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210992425.XA CN115305366B (en) | 2022-08-18 | 2022-08-18 | Production method of rare earth silicate ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210992425.XA CN115305366B (en) | 2022-08-18 | 2022-08-18 | Production method of rare earth silicate ore |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115305366A true CN115305366A (en) | 2022-11-08 |
| CN115305366B CN115305366B (en) | 2024-06-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210992425.XA Active CN115305366B (en) | 2022-08-18 | 2022-08-18 | Production method of rare earth silicate ore |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039725A (en) * | 2015-06-28 | 2015-11-11 | 包头市玺骏稀土有限责任公司 | Method for recycling rare earth elements from rare earth electrolytic slag |
| CN106630636A (en) * | 2016-09-18 | 2017-05-10 | 中南大学 | Ceramic glass with lanthanum disilicate as principal crystalline phase, preparation method and application |
| CN107630143A (en) * | 2017-09-26 | 2018-01-26 | 赣南师范大学 | Method for extracting rare earth from rare earth fluorescent powder waste and fluorine-containing rare earth electrolysis waste residue |
| CN108431254A (en) * | 2016-01-12 | 2018-08-21 | 三菱综合材料株式会社 | The separation method and containing rare earth element slag of rare earth element and iron |
| CN109280781A (en) * | 2018-10-24 | 2019-01-29 | 李洪明 | A kind of method of decomposition and inversion Rare Earth Mine |
| CN109837385A (en) * | 2019-04-15 | 2019-06-04 | 李洪明 | A kind of method that Rare Earth Mine is decomposed in heating melting conversion |
| WO2020257849A1 (en) * | 2019-06-25 | 2020-12-30 | Australian Nuclear Science And Technology Organisation | Process for recovering rare earths |
| CN113025835A (en) * | 2020-07-28 | 2021-06-25 | 江西理工大学 | Method for efficiently extracting rare earth from bastnaesite |
| CN114703384A (en) * | 2022-03-31 | 2022-07-05 | 江苏南方永磁科技有限公司 | Slag remover material for rare earth recovery and preparation and use methods thereof |
-
2022
- 2022-08-18 CN CN202210992425.XA patent/CN115305366B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039725A (en) * | 2015-06-28 | 2015-11-11 | 包头市玺骏稀土有限责任公司 | Method for recycling rare earth elements from rare earth electrolytic slag |
| CN108431254A (en) * | 2016-01-12 | 2018-08-21 | 三菱综合材料株式会社 | The separation method and containing rare earth element slag of rare earth element and iron |
| CN106630636A (en) * | 2016-09-18 | 2017-05-10 | 中南大学 | Ceramic glass with lanthanum disilicate as principal crystalline phase, preparation method and application |
| CN107630143A (en) * | 2017-09-26 | 2018-01-26 | 赣南师范大学 | Method for extracting rare earth from rare earth fluorescent powder waste and fluorine-containing rare earth electrolysis waste residue |
| CN109280781A (en) * | 2018-10-24 | 2019-01-29 | 李洪明 | A kind of method of decomposition and inversion Rare Earth Mine |
| CN109837385A (en) * | 2019-04-15 | 2019-06-04 | 李洪明 | A kind of method that Rare Earth Mine is decomposed in heating melting conversion |
| WO2020257849A1 (en) * | 2019-06-25 | 2020-12-30 | Australian Nuclear Science And Technology Organisation | Process for recovering rare earths |
| CN113025835A (en) * | 2020-07-28 | 2021-06-25 | 江西理工大学 | Method for efficiently extracting rare earth from bastnaesite |
| CN114703384A (en) * | 2022-03-31 | 2022-07-05 | 江苏南方永磁科技有限公司 | Slag remover material for rare earth recovery and preparation and use methods thereof |
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| Publication number | Publication date |
|---|---|
| CN115305366B (en) | 2024-06-11 |
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