CN210261147U - Production system of rare earth fluoride - Google Patents
Production system of rare earth fluoride Download PDFInfo
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- CN210261147U CN210261147U CN201920970551.9U CN201920970551U CN210261147U CN 210261147 U CN210261147 U CN 210261147U CN 201920970551 U CN201920970551 U CN 201920970551U CN 210261147 U CN210261147 U CN 210261147U
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Abstract
The utility model discloses a rare earth fluoride production system, which comprises a reinforced roasting unit, a transformation separation unit, a mixed acid treatment unit, a fluorination sedimentation tank and a spray drying tower; the utility model discloses when preparing rare earth fluoride, make full use of the tombarthite reinforce the waste acid gas that produces in the calcination process, obtain sulphuric acid and hydrofluoric acid after washing and separation, sulphuric acid can be recycled to reinforce the calcination unit, hydrofluoric acid is used for preparing rare earth fluoride, has both solved the environmental pollution that the waste gas was arranged outward and is caused when traditional fluorine-containing rare earth concentrate was prepared, and recycle acid resources, the synthetic rare earth fluoride of one-step process has reduced its preparation manufacturing cost; the spray drying can also well solve the problem that the rare earth fluoride is not easy to filter.
Description
The technical field is as follows:
the utility model relates to a production system especially relates to a production system of rare earth fluoride.
Background art:
rare earth fluoride is an important industrial raw material and can be used for preparing electrolytic metal, polishing powder and the like. The traditional preparation method of rare earth fluoride comprises a dry method and a wet method, wherein rare earth fluoride is produced by reacting rare earth carbonate with 45-50% hydrofluoric acid, and then the rare earth fluoride is filtered by a plate frame and roasted at low temperature to finally obtain a rare earth fluoride finished product.
In actual rare earth enterprise production, rare earth chloride can be obtained in the rare earth ore extraction process, waste acid gas can be generated in the rare earth ore roasting process, and if the production wastes are discharged, the production wastes need to be treated, so that the environmental pollution risk is increased, the resource waste is also caused, and the enterprise production cost is increased.
The utility model has the following contents:
in order to solve the above technical problem, an object of the present invention is to provide a system for producing rare earth fluoride.
The utility model discloses by following technical scheme implement: a production system of rare earth fluoride comprises a reinforced roasting unit, a transformation separation unit, a mixed acid treatment unit, a fluorination precipitation tank and a spray drying tower;
the reinforced roasting unit comprises a slurry mixing tank, a roasting kiln, a spray tower, a water leaching tank, a filter press, a P204 extraction tank, a P507 extraction tank, a hydrochloric acid storage tank and an ammonia water storage tank, wherein a slurry outlet of the slurry mixing tank is communicated with a feed inlet of the roasting kiln, a discharge outlet of the roasting kiln is communicated with a feed inlet of the water leaching tank, and a discharge outlet of the water leaching tank is communicated with a feed inlet of the filter press; the liquid outlet of the filter press is communicated with the feed inlet of the P204 extraction tank, the water phase outlet of the P204 extraction tank is communicated with the feed inlet of the P507 extraction tank, and the easily-extracted component outlet and the difficultly-extracted component outlet of the P507 extraction tank are respectively communicated with the inlets of the corresponding fluorination settling tanks;
the hydrochloric acid storage tank is respectively communicated with the back extractant inlets of the P204 extraction tank and the P507 extraction tank, and the ammonia water inlet is communicated with the ammonia water inlet of the P507 extraction tank;
a tail gas outlet of the roasting kiln is communicated with a gas inlet of the spray tower; the liquid outlet of the spray tower is communicated with a cold medium inlet of a finished product acid preheater of the mixed acid treatment unit, a finished product acid tank of the mixed acid treatment unit is communicated with a feed inlet of the slurry mixing tank, a hydrogen fluoride liquid seal tank outlet of the mixed acid treatment unit is communicated with an inlet of the fluorination precipitation tank, and a discharge outlet of the fluorination precipitation tank is communicated with the spray drying tower.
Further, the mixed acid treatment unit comprises a finished product acid preheater, a condensate water preheater, a heater, an evaporator, a finished product acid cooler, a finished product acid tank, a hydrogen fluoride liquid seal tank and a steam generator, wherein a circulation port of the evaporator is communicated with a cold medium inlet of the heater through a circulation pump; a cold medium outlet of the finished acid preheater is communicated with a cold medium inlet of the condensed water preheater, a cold medium outlet of the condensed water preheater is communicated with a cold medium inlet of the heater, and a cold medium outlet of the heater is communicated with a feed inlet of the evaporator; an acid outlet of the evaporator is communicated with a heat medium inlet of the finished product acid preheater, a heat medium outlet of the finished product acid preheater is communicated with a heat medium inlet of the finished product acid cooler, and a heat medium outlet of the finished product acid cooler is communicated with the finished product acid tank; the gas outlet of the evaporator is communicated with the inlet of the hydrogen fluoride liquid seal tank; the steam outlet of the steam generator is communicated with the heat medium inlet of the heater, the heat medium outlet of the heater is communicated with the heat medium inlet of the condensed water preheater, and the heat medium outlet of the condensed water preheater is communicated with the water inlet of the steam generator.
The utility model has the advantages that:
1. the utility model realizes the separation of two acids by setting the mixed acid processing unit and utilizing the different boiling points of sulfur trioxide and hydrogen fluoride, thereby avoiding the resource waste and saving the cost; and the design is reasonable, no waste acid or solid waste is generated, and the environmental pollution is avoided.
2. The utility model discloses when preparing rare earth fluoride, make full use of the tombarthite reinforce the waste acid gas that produces in the calcination process, the sulphuric acid that obtains can be recycled and reinforce the calcination unit, hydrofluoric acid is used for preparing rare earth fluoride, has both solved the environmental pollution that the waste gas was arranged outward and is caused when traditional fluorine-containing rare earth concentrate was prepared, has recycled sour resource again, and one-step synthesis rare earth fluoride has reduced its preparation manufacturing cost; and the problem that rare earth fluoride is not easy to filter can be well solved by adopting spray drying.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic diagram of a system according to an embodiment.
In the figure: the system comprises a pulp conditioning tank 1, a roasting kiln 2, a spray tower 3, a water leaching tank 4, a filter press 5, a P204 extraction tank 6, a P507 extraction tank 7, a hydrochloric acid storage tank 8, an ammonia water storage tank 9, a fluorination precipitation tank 10, a spray drying tower 11, a finished acid preheater 12, a condensed water preheater 13, a heater 14, an evaporator 15, a finished acid cooler 16, a finished acid tank 17, a hydrogen fluoride liquid seal tank 18, a steam generator 19 and a circulating pump 20.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
A production system of rare earth fluoride comprises a reinforced roasting unit, a transformation separation unit, a mixed acid treatment unit, a fluorination precipitation tank 10 and a spray drying tower 11;
the intensified roasting unit comprises a pulp mixing tank 1, a roasting kiln 2, a spray tower 3, a water leaching tank 4, a filter press 5, a P204 extraction tank 6, a P507 extraction tank 7, a hydrochloric acid storage tank 8 and an ammonia water storage tank 9, wherein a pulp outlet of the pulp mixing tank 1 is communicated with a feed inlet of the roasting kiln 2, a discharge outlet of the roasting kiln 2 is communicated with a feed inlet of the water leaching tank 4, and a discharge outlet of the water leaching tank 4 is communicated with a feed inlet of the filter press 5; the liquid outlet of the filter press 5 is communicated with the feed inlet of the P204 extraction tank 6, the water phase outlet of the P204 extraction tank 6 is communicated with the feed inlet of the P507 extraction tank 7, and the easy-extraction component outlet and the difficult-extraction component outlet of the P507 extraction tank 7 are respectively communicated with the inlets of the corresponding fluorination settling tanks 10;
the hydrochloric acid storage tank 8 is respectively communicated with the stripping agent inlets of the P204 extraction tank 6 and the P507 extraction tank 7, and the ammonia water inlet is communicated with the ammonia water inlet of the P507 extraction tank 7;
the mixed acid treatment unit comprises a finished product acid preheater 12, a condensed water preheater 13, a heater 14, an evaporator 15, a finished product acid cooler 16, a finished product acid tank 17, a hydrogen fluoride liquid seal tank 18 and a steam generator 19, wherein a circulating port of the evaporator 15 is communicated with a cold medium inlet of the heater 14 through a circulating pump 20; a cold medium outlet of the finished acid preheater 12 is communicated with a cold medium inlet of a condensed water preheater 13, a cold medium outlet of the condensed water preheater 13 is communicated with a cold medium inlet of a heater 14, and a cold medium outlet of the heater 14 is communicated with a feed inlet of an evaporator 15; an acid outlet of the evaporator 15 is communicated with a heat medium inlet of a finished product acid preheater 12, a heat medium outlet of the finished product acid preheater 12 is communicated with a heat medium inlet of a finished product acid cooler 16, a heat medium outlet of the finished product acid cooler 16 is communicated with a finished product acid tank 17, and the finished product acid tank 17 is communicated with a feed inlet of the pulp mixing tank 1; the air outlet of the evaporator 15 is communicated with the inlet of the hydrogen fluoride liquid seal tank 18; a steam outlet of the steam generator 19 is communicated with a heat medium inlet of the heater 14, a heat medium outlet of the heater 14 is communicated with a heat medium inlet of the condensed water preheater 13, and a heat medium outlet of the condensed water preheater 13 is communicated with a water inlet of the steam generator 19;
a tail gas outlet of the roasting kiln 2 is communicated with a gas inlet of the spray tower 3; the liquid outlet of the spray tower 3 is communicated with the cold medium inlet of the finished acid preheater 12, the outlet of the hydrogen fluoride liquid seal groove 18 is communicated with the inlet of the fluorination precipitation tank 10, and the discharge port of the fluorination precipitation tank 10 is communicated with the spray drying tower 11.
The working process is as follows:
uniformly stirring the fluorine-containing rare earth concentrate, concentrated sulfuric acid and recovered sulfuric acid according to the mass ratio of 1:1.5-1.6, adding the mixture from the tail part of the roasting kiln, and roasting the sulfuric acid at the temperature of 500-750 ℃ to obtain roasted ore and tail gas. The equation is as follows:
2REFCO3+3H2SO4＝RE2(SO4)+2HF↑+2CO2↑+2H2O
and (3) passing the waste gas containing sulfur trioxide and fluorine generated by roasting through a water spray tower to obtain mixed acid wastewater containing dilute sulfuric acid and hydrofluoric acid, evaporating and separating to generate 70% of dilute sulfuric acid which is reused in the roasting process, and simultaneously generating 10-12% of hydrofluoric acid.
Stirring and leaching 25-35g/L rare earth sulfate solution from the rare earth roasted ore and cold water, and transforming the rare earth sulfate solution with reduced concentration into 240-300g/L high-concentration mixed rare earth chloride solution by P204 extraction and hydrochloric acid back extraction.
The mixed rare earth feed liquid is distributed according to different rare earth elements between a P507 organic solution and a water phase which are not mutually soluble, and single rare earth chloride solutions of lanthanum, cerium, praseodymium, neodymium and the like are obtained through grouped multistage P507 extraction separation.
The rare earth extraction product single chlorinated rare earth solution (the concentration is 250-300g/L) and hydrofluoric acid (10-12% by weight ratio) which is obtained by recovering and separating waste gas generated in the roasting process of the rare earth mineral acid method are taken as raw materials according to the molar ratio RE3+: precipitation of HF as 1: 3.1. Precipitation conditions: firstly, adding rare earth fluoride accounting for 15 percent of the total mass of the total product as a reaction seed crystal, adopting a coprecipitation method to react under the conditions of normal temperature (30-50 ℃) and normal pressure, wherein the reaction conditions are as follows: and (3) rotating at 90 rpm, and terminating the reaction when the reaction pH is 4.0-4.5 to obtain rare earth fluoride slurry. The reaction equation is as follows:
RECl3+3HF＝REF3↓+3HCl
and (3) carrying out spray drying on the rare earth fluoride slurry, and controlling a certain feeding speed, wherein the air inlet temperature is 350-390 ℃, and the air outlet temperature is 100-110 ℃ to obtain the rare earth fluoride.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. The production system of rare earth fluoride is characterized by comprising a reinforced roasting unit, a transformation separation unit, a mixed acid treatment unit, a fluorination precipitation tank and a spray drying tower;
the reinforced roasting unit comprises a slurry mixing tank, a roasting kiln, a spray tower, a water leaching tank, a filter press, a P204 extraction tank, a P507 extraction tank, a hydrochloric acid storage tank and an ammonia water storage tank, wherein a slurry outlet of the slurry mixing tank is communicated with a feed inlet of the roasting kiln, a discharge outlet of the roasting kiln is communicated with a feed inlet of the water leaching tank, and a discharge outlet of the water leaching tank is communicated with a feed inlet of the filter press; the liquid outlet of the filter press is communicated with the feed inlet of the P204 extraction tank, the water phase outlet of the P204 extraction tank is communicated with the feed inlet of the P507 extraction tank, and the easily-extracted component outlet and the difficultly-extracted component outlet of the P507 extraction tank are respectively communicated with the inlets of the corresponding fluorination settling tanks;
the hydrochloric acid storage tank is respectively communicated with the back extractant inlets of the P204 extraction tank and the P507 extraction tank, and the ammonia water inlet is communicated with the ammonia water inlet of the P507 extraction tank;
a tail gas outlet of the roasting kiln is communicated with a gas inlet of the spray tower; the liquid outlet of the spray tower is communicated with a cold medium inlet of a finished product acid preheater of the mixed acid treatment unit, a finished product acid tank of the mixed acid treatment unit is communicated with a feed inlet of the slurry mixing tank, a hydrogen fluoride liquid seal tank outlet of the mixed acid treatment unit is communicated with an inlet of the fluorination precipitation tank, and a discharge outlet of the fluorination precipitation tank is communicated with the spray drying tower.
2. The rare earth fluoride production system of claim 1, wherein the mixed acid treatment unit comprises a finished acid preheater, a condensed water preheater, a heater, an evaporator, a finished acid cooler, a finished acid tank, a hydrogen fluoride liquid seal tank and a steam generator, and a circulation port of the evaporator is communicated with a cold medium inlet of the heater through a circulation pump; a cold medium outlet of the finished acid preheater is communicated with a cold medium inlet of the condensed water preheater, a cold medium outlet of the condensed water preheater is communicated with a cold medium inlet of the heater, and a cold medium outlet of the heater is communicated with a feed inlet of the evaporator; an acid outlet of the evaporator is communicated with a heat medium inlet of the finished product acid preheater, a heat medium outlet of the finished product acid preheater is communicated with a heat medium inlet of the finished product acid cooler, and a heat medium outlet of the finished product acid cooler is communicated with the finished product acid tank; the gas outlet of the evaporator is communicated with the inlet of the hydrogen fluoride liquid seal tank; the steam outlet of the steam generator is communicated with the heat medium inlet of the heater, the heat medium outlet of the heater is communicated with the heat medium inlet of the condensed water preheater, and the heat medium outlet of the condensed water preheater is communicated with the water inlet of the steam generator.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449651A (en) * | 2022-08-27 | 2022-12-09 | 萍乡泽昊新材料有限责任公司 | Method for dissolving rare earth raw ore |
| CN115678436A (en) * | 2022-11-04 | 2023-02-03 | 包头市科蒙新材料开发有限责任公司 | Preparation method of novel cerium-rich rare earth polishing powder |
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2019
- 2019-06-25 CN CN201920970551.9U patent/CN210261147U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449651A (en) * | 2022-08-27 | 2022-12-09 | 萍乡泽昊新材料有限责任公司 | Method for dissolving rare earth raw ore |
| CN115449651B (en) * | 2022-08-27 | 2024-05-17 | 萍乡泽昊新材料有限责任公司 | Rare earth raw ore dissolving method |
| CN115678436A (en) * | 2022-11-04 | 2023-02-03 | 包头市科蒙新材料开发有限责任公司 | Preparation method of novel cerium-rich rare earth polishing powder |
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