CN118256750A - Treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ore - Google Patents
Treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ore Download PDFInfo
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- CN118256750A CN118256750A CN202410327800.8A CN202410327800A CN118256750A CN 118256750 A CN118256750 A CN 118256750A CN 202410327800 A CN202410327800 A CN 202410327800A CN 118256750 A CN118256750 A CN 118256750A
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- rare earth
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- fluoride ions
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 58
- -1 fluoride ions Chemical class 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 25
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 38
- 239000003513 alkali Substances 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- 229910004261 CaF 2 Inorganic materials 0.000 claims abstract description 17
- 238000002386 leaching Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000002351 wastewater Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 30
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 21
- 229910052731 fluorine Inorganic materials 0.000 claims description 21
- 239000011737 fluorine Substances 0.000 claims description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 239000013049 sediment Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 239000007800 oxidant agent Substances 0.000 claims description 7
- KBTJYNAFUYTSNN-UHFFFAOYSA-N [Na].OO Chemical compound [Na].OO KBTJYNAFUYTSNN-UHFFFAOYSA-N 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 150000001450 anions Chemical class 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 claims description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 7
- 238000006479 redox reaction Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000003113 alkalizing effect Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006115 defluorination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction 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
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
-
- 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ores, which comprises the following steps: the freshly mined rare earth carbonate ore is concentrated and piled up, and the rare earth carbonate ore is crushed and milled to obtain particles with consistent particle size; the obtained particles are cleaned, and the filtering wastewater generated by the cleaning is subjected to leaching treatment by adding acid and alkali independently; the clean rare earth ore particles are intensively led into an acid adding area, after acid mixing, the mixed solution is led into an alkali adding area for full reaction, and the produced precipitate CaF 2 is collected and filtered by a filter screen to finish solid-liquid separation; treating the separated precipitate to obtain a precipitate CaF 2; the collected and stored precipitate CaF 2 has the advantages that rare earth carbonate ore can be rapidly filtered and separated, and is comprehensively treated in an acid adding area and an alkali adding area to form white precipitate CaF 2, so that products obtained by recycling fluoride ions are effectively treated, and environmental pollution caused by improper treatment is avoided.
Description
Technical Field
The invention belongs to the technical field of rare earth ore treatment, and particularly relates to a treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ore.
Background
Rare earth ore is an important strategic resource and is widely used in the fields of electronics, aerospace, military and the like. However, rare earth ores contain a large amount of fluoride ions, which not only affect the separation and extraction of rare earth but also cause environmental pollution. Therefore, how to effectively reduce the fluoride ion content in the rare earth ore becomes an important problem for the development of the rare earth industry.
Patent document with application number of CN115927884A discloses a method for removing fluorine from leaching liquid of rare earth ore, which comprises the following steps: adding the solution A into the fluorine-containing rare earth ore leaching solution, stirring and adjusting the pH value of the fluorine-containing ionic rare earth ore leaching solution, clarifying and carrying out solid-liquid separation to obtain a solution B, adding the solution C into the solution B, clarifying and carrying out solid-liquid separation to obtain a precipitate, adding the solution D into the precipitate, carrying out filter pressing and carrying out solid-liquid separation after stirring leaching to obtain the rare earth ore with low fluorine content. The method is suitable for carrying out defluorination operation on the leaching liquid of fluorine-containing rare earth carbonate ore, rare earth oxalate ore, carbon grass mixed rare earth ore or oxidized rare earth ore. According to the method, the fluorine and the rare earth are separated after the compound of the rare earth fluorine is dissolved in the ammonium salt solution and then solid-liquid separation is carried out. After the treatment by the method provided by the invention, the fluorine element content in the rare earth ore leaching liquid can be greatly reduced, and the subsequent processing and production of rare earth can be ensured to be smoothly carried out.
Although the above patent can effectively remove the fluoride ions, the operation process is complex, the cost is high, the efficiency is low, and a certain environmental risk exists, but only through mixed acid leaching, a great amount of pungent and toxic gas can be generated, the surrounding air quality is seriously affected, and meanwhile, the separated precipitate cannot be effectively treated, so that a more efficient, simple and economic method is needed to reduce the fluoride ion content in the rare earth ore.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ore, which can effectively reduce the concentration of the fluoride ions and improve the purity and quality of the rare earth ore under the condition of not damaging rare earth elements in the rare earth ore, thereby meeting the requirements of industrial production and solving the problems in the prior art.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ores comprises the following steps:
S1, preparing raw materials: the freshly mined rare earth carbonate ores are concentrated and piled up and are integrated;
s2, pretreatment: crushing and grinding the rare earth carbonate ore to obtain particles with consistent particle sizes;
s3, cleaning and leaching and filtrate treatment: cleaning the obtained particles to obtain clean rare earth ore particles, and leaching the filtered wastewater generated by cleaning by adding acid and alkali independently;
s4, adjusting the PH value: the clean rare earth ore particles are intensively led into an acid adding area, after acid mixing, the mixed solution is led into an alkali adding area for full reaction, so that Ca 2+ and F - are combined into CaF 2 which is difficult to dissolve in water, and the fluorine reduction treatment is completed;
S5, adding a mixed reagent: the mixed reagent adopts Na salt reagent, and is introduced into an alkali adding region to neutralize anions in the alkali adding region, so that the content of Ca 2+ is improved, and the fluorine removal rate reaches 93.4%;
S6, precipitation treatment: the sediment CaF2 generated after the fluorine reduction treatment is collected and filtered through a filter screen, so that solid-liquid separation is completed;
s7, sediment treatment: treating the separated precipitate, such as washing, drying, etc., to obtain precipitate CaF 2;
s8, collecting sediment: the treated precipitate CaF 2 is collected and stored for further use or disposal.
As an alternative scheme of the invention, in the step S4, the pH value of the acid adding area is set to be 2.0-2.5 by adopting concentrated hydrochloric acid solution, and the pH value of the alkali adding area is set to be 4.0-4.5 by adopting lime water solution.
As an alternative scheme of the invention, the fluorine ion content in the solution before treatment in the step S4 is 4600mg/L, and the fluorine ion content in the solution after treatment is 200mg/L-300mg/L, so that the fluorine removal rate reaches 93.4%.
As an alternative to the present invention, the solution concentration during the steps S4 and S5 is maintained at 1.6mol/L.
As an alternative to the present invention, the step S4 alkalizing zone may also employ an oxidizing agent comprising hydrogen peroxide, sodium hydrogen peroxide.
The invention provides a treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ores, which has the following beneficial effects:
The method has the advantages that the rare earth carbonate ore can be rapidly filtered and separated through the whole set of treatment process, fluoride ions are fully reacted by utilizing the acid adding area and the alkali adding area, the white precipitated CaF 2 is formed, the pungent smell of the gas generated by the alkali adding area can not occur, the toxic gas is greatly reduced, the surrounding environment is further protected, the CaF 2 is subjected to subsequent washing and drying, the precipitate is collected and stored, the content of the fluoride ions is greatly reduced, and the product obtained by recycling the fluoride ions is effectively treated, so that the pollution of the surrounding environment caused by improper treatment is avoided.
Drawings
FIG.1 is a schematic flow chart of the present invention.
Detailed Description
Embodiments of the present invention are described in further detail below with reference to the accompanying drawings and examples. The following examples are illustrative of the invention but are not intended to limit the scope of the invention.
Referring to fig. 1, the present invention provides a technical solution: a treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ores comprises the following steps:
S1, preparing raw materials: the freshly mined rare earth carbonate ores are concentrated and piled up and are integrated;
S2, pretreatment: taking 50kg of fluorocarbonate rare earth ore, crushing and grinding the fluorocarbonate rare earth ore, and crushing the fluorocarbonate rare earth ore into particles with 100 meshes, thereby obtaining particles with consistent particle sizes;
S3, cleaning and leaching and filtrate treatment: cleaning and stirring the obtained particles to obtain clean rare earth ore particles, so that the fluorine content of the rare earth ore is reduced, and leaching the filtered wastewater generated by cleaning by adding acid and alkali independently;
S4, adjusting the PH value: the clean rare earth ore particles are intensively led into an acid adding area, a concentrated hydrochloric acid solution is adopted in the acid adding area in the step S4, the stirring time is set to be 2 hours in the process of mixing and stirring, the stirring temperature is set to be 15-85 ℃, the mixed solution is led into an alkali adding area, the alkali adding area adopts a lime water solution, and continuous stirring is carried out for full reaction, so that Ca 2+ and F - are combined into CaF 2 which is indissolvable in water, the chemical equation is Ca 2++2F-＝CaF2, white precipitation is generated, the fluorine reduction treatment is completed, the fluorine ion content in the solution before the treatment in the step S4 is 4600mg/L, and the fluorine ion content in the treated solution is 200-300 mg/L;
In the step S4, an oxidant comprising hydrogen peroxide, sodium peroxide and sodium hydrogen peroxide can be used in the alkali adding area to enable fluoride ions in the rare earth ore to undergo oxidation-reduction reaction with the oxidant to generate fluoride, the reaction condition can be oxidation-reduction reaction at normal temperature and normal pressure, and the oxidation-reduction reaction speed can be accelerated when the reaction temperature reaches above 60 ℃;
S5, adding a mixed reagent: the mixed reagent adopts Na salt reagent, and is introduced into an alkali adding region to neutralize anions in the alkali adding region, so that the content of Ca 2+ is improved, and the fluorine removal rate reaches 93.4%; the concentration of the solution in the treatment process of the step S4 and the step S5 is kept at 1.6mol/L;
S6, precipitation treatment: the sediment CaF 2 generated after the fluorine reduction treatment is collected and filtered through a filter screen, so that the solid-liquid separation is completed;
s7, sediment treatment: treating the separated precipitate, such as washing, drying, etc., to obtain precipitate CaF 2;
s8, collecting sediment: the treated precipitate CaF 2 is collected and stored for further use or disposal.
In example 2, in step S4, the pH value of the acid adding area is set to be 2.0-2.5 by using concentrated hydrochloric acid solution, the pH value of the acid adding area is detected periodically, the pH value of the alkali adding area is set to be 4.0-4.5 by using lime water solution, and the pH value of the alkali adding area is detected periodically.
Example 3, the fluorine ion content in the solution before treatment in step S4 was 4600mg/L, and the fluorine ion content in the solution after treatment was 200mg/L to 300mg/L, so that the fluorine removal rate reached 93.4%.
In example 4, the concentration of the solution in the treatment process of steps S4 and S5 is kept at 1.6mol/L, the staff does not need to add additional water for concentration adjustment, and the whole flow is not affected.
In example 5, in the step S4, the alkaline adding region may further use an oxidizing agent including hydrogen peroxide, sodium peroxide and sodium hydrogen peroxide, and the rare earth ore is mixed with the oxidizing agent, so that the fluoride ions in the rare earth ore and the oxidizing agent undergo oxidation-reduction reaction to generate fluoride, and less pollution gas is generated, thereby protecting the surrounding environment.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. A treatment method for efficiently reducing fluoride ions in fluorocarbonate rare earth ores is characterized by comprising the following steps: the method comprises the following steps:
S1, preparing raw materials: the freshly mined rare earth carbonate ores are concentrated and piled up and are integrated;
s2, pretreatment: crushing and grinding the rare earth carbonate ore to obtain particles with consistent particle sizes;
s3, cleaning and leaching and filtrate treatment: cleaning the obtained particles to obtain clean rare earth ore particles, and leaching the filtered wastewater generated by cleaning by adding acid and alkali independently;
s4, adjusting the PH value: the clean rare earth ore particles are intensively led into an acid adding area, after acid mixing, the mixed solution is led into an alkali adding area for full reaction, so that Ca 2+ and F - are combined into CaF 2 which is difficult to dissolve in water, and the fluorine reduction treatment is completed;
S5, adding a mixed reagent: the mixed reagent adopts Na salt reagent, and is introduced into an alkali adding region to neutralize anions in the alkali adding region, so that the content of Ca 2+ is improved, and the fluorine removal rate reaches 93.4%;
S6, precipitation treatment: the sediment CaF 2 generated after the fluorine reduction treatment is collected and filtered through a filter screen, so that the solid-liquid separation is completed;
s7, sediment treatment: treating the separated precipitate, such as washing, drying, etc., to obtain precipitate CaF 2;
s8, collecting sediment: the treated precipitate CaF 2 is collected and stored for further use or disposal.
2. The method for efficiently reducing fluoride ions in a rare earth fluorocarbonate ore according to claim 1, characterized by comprising the steps of: in the step S4, the acid adding area adopts concentrated hydrochloric acid solution, the PH value of the acid adding area is set to be 2.0-2.5, the alkali adding area adopts lime water solution, and the PH value of the alkali adding area is set to be 4.0-4.5.
3. The method for efficiently reducing fluoride ions in a rare earth fluorocarbonate ore according to claim 1, characterized by comprising the steps of: the fluorine ion content in the solution before treatment in the step S4 is 4600mg/L, and the fluorine ion content in the solution after treatment is 200mg/L-300mg/L, so that the fluorine removal rate reaches 93.4%.
4. The method for efficiently reducing fluoride ions in a rare earth fluorocarbonate ore according to claim 1, characterized by comprising the steps of: the concentration of the solution during the treatment in steps S4 and S5 was maintained at 1.6mol/L.
5. The method for efficiently reducing fluoride ions in a rare earth fluorocarbonate ore according to claim 1, characterized by comprising the steps of: the alkaline adding zone of step S4 can also use an oxidant comprising hydrogen peroxide, sodium hydrogen peroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410327800.8A CN118256750A (en) | 2024-03-20 | 2024-03-20 | Treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410327800.8A CN118256750A (en) | 2024-03-20 | 2024-03-20 | Treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ore |
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| Publication Number | Publication Date |
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| CN118256750A true CN118256750A (en) | 2024-06-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202410327800.8A Pending CN118256750A (en) | 2024-03-20 | 2024-03-20 | Treatment method for efficiently reducing fluoride ions in fluorocarbonic acid rare earth ore |
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| Country | Link |
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| CN (1) | CN118256750A (en) |
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- 2024-03-20 CN CN202410327800.8A patent/CN118256750A/en active Pending
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