CN111074071A - Method for recycling mixed rare earth carbonate precipitation wastewater - Google Patents
Method for recycling mixed rare earth carbonate precipitation wastewater Download PDFInfo
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- CN111074071A CN111074071A CN201911314904.0A CN201911314904A CN111074071A CN 111074071 A CN111074071 A CN 111074071A CN 201911314904 A CN201911314904 A CN 201911314904A CN 111074071 A CN111074071 A CN 111074071A
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- rare earth
- water
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- precipitation
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- 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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- 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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for recycling mixed rare earth carbonate precipitation wastewater, which comprises the following steps: leaching roasted ore with water to remove impurities to obtain rare earth sulfate water leaching solution, and reacting the rare earth sulfate water leaching solution with a precipitator to generate rare earth carbonate and supernatant; filtering slurry obtained after the reaction of the rare earth sulfate water leaching solution and the precipitator, wherein supernatant is precipitation wastewater, and solid is mixed rare earth carbonate; the precipitated wastewater is divided into first precipitated wastewater and second precipitated wastewater, the first precipitated wastewater is sent to a wastewater treatment workshop for wastewater treatment, salts (ammonium sulfate or sodium sulfate salts) recovered through evaporation are recovered, and the recycled water is sent to a water leaching process and a washing process; the second precipitation wastewater is sent to a water leaching process for leaching roasted ore; and (4) washing the mixed rare earth carbonate by using reuse water, and returning the generated low-concentration leaching water to the preparation process of the precipitator. The invention can realize the recycling of the mixed rare earth carbonate precipitation wastewater, reduce the discharge amount of the precipitation wastewater and improve the concentration of the precipitation wastewater.
Description
Technical Field
The invention belongs to the field of rare earth hydrometallurgy, and particularly relates to a method for recycling mixed rare earth carbonate precipitation wastewater.
Background
In the process of rare earth hydrometallurgy, the northern rare earth concentrate is decomposed by adopting a concentrated sulfuric acid high-temperature roasting method to prepare roasted ore, the roasted ore is subjected to a water leaching and impurity removing process to prepare rare earth sulfate water leaching solution, the water leaching solution is converted by ammonium salt or sodium salt to prepare mixed rare earth carbonate slurry, the mixed rare earth carbonate slurry is subjected to solid-liquid separation and washing to obtain mixed rare earth carbonate, and precipitation wastewater is removed. However, a large amount of low-concentration precipitation wastewater is discharged in the production process, and the cyclic utilization of wastewater resources is not realized.
Disclosure of Invention
The invention aims to provide a method for recycling mixed rare earth carbonate precipitation wastewater, which realizes recycling of mixed rare earth carbonate precipitation wastewater, reduces the discharge amount of precipitation wastewater, improves the concentration of precipitation wastewater and reduces the wastewater treatment cost.
The technical scheme is as follows:
the method for recycling the mixed rare earth carbonate precipitation wastewater comprises the following steps:
leaching roasted ore with water to remove impurities to obtain rare earth sulfate water leaching solution, and reacting the rare earth sulfate water leaching solution with a precipitator to generate rare earth carbonate and supernatant;
filtering slurry obtained after the reaction of the rare earth sulfate water leaching solution and the precipitator, wherein supernatant is precipitation wastewater, and solid is mixed rare earth carbonate;
the precipitated wastewater is divided into first precipitated wastewater and second precipitated wastewater, the first precipitated wastewater is sent to a wastewater treatment workshop for wastewater treatment, salts (ammonium sulfate or sodium sulfate salts) recovered through evaporation are recovered, and the recycled water is sent to a water leaching process and a washing process; the second precipitation wastewater is sent to a water leaching process for leaching roasted ore;
and (4) washing the mixed rare earth carbonate by using reuse water, and returning the generated low-concentration leaching water to the preparation process of the precipitator.
And further reacting the rare earth sulfate aqueous leaching solution with the rare earth content of 20-40 g/L and the pH value of 3.8-5.4 with a precipitator.
Furthermore, the amount of the second precipitation wastewater returned to the solid sulfuric acid rare earth water leaching process accounts for 0-20% of the total amount of the precipitation wastewater.
Furthermore, the amount of the precipitator prepared by the leaching water accounts for 0-100% of the total water amount.
Further, the precipitant is solid or liquid ammonium salt or sodium salt.
The invention has the technical effects that:
the invention realizes the recycling of the mixed rare earth carbonate precipitation wastewater, reduces the discharge amount of the precipitation wastewater, improves the concentration of the precipitation wastewater and reduces the wastewater treatment cost. And part of the precipitated wastewater is recycled for the water leaching process, so that the emission reduction of the precipitated wastewater is realized, the equipment change is small, the investment is low, and the economic benefit is obvious.
The invention can realize continuous precipitation, filtration, washing and wastewater treatment by a control mode, and the cyclic utilization of the precipitated wastewater can reduce energy consumption and production cost.
Drawings
FIG. 1 is a process flow diagram of the method for recycling waste water from mixed rare earth carbonate precipitation in the invention.
Detailed Description
The following description sufficiently illustrates specific embodiments of the invention to enable those skilled in the art to practice and reproduce it.
As shown in FIG. 1, it is a process flow diagram of the method for recycling waste water from mixed rare earth carbonate precipitation in the present invention.
The method for recycling the mixed rare earth carbonate precipitation wastewater specifically comprises the following steps:
step 1: leaching roasted ore with water to remove impurities to obtain rare earth sulfate water leaching solution, and reacting the rare earth sulfate water leaching solution with a precipitator to generate rare earth carbonate and supernatant;
step 2: filtering slurry obtained after reaction of the rare earth sulfate water leaching solution and the precipitator by solid-liquid separation equipment, wherein supernatant is precipitation wastewater (containing ammonium sulfate or sodium sulfate), and solid is mixed rare earth carbonate;
reacting rare earth sulfate aqueous solution with the rare earth content of 20-40 g/L and the pH value of 3.8-5.4 with a precipitator (solid or liquid ammonium salt or sodium salt). And transforming the rare earth sulfate water leaching solution by ammonium salt or sodium salt to prepare the mixed rare earth carbonate slurry.
And step 3: shunting high-concentration precipitation wastewater to form first precipitation wastewater and second precipitation wastewater, treating the first precipitation wastewater in a wastewater treatment workshop, recovering salts (ammonium sulfate or sodium sulfate) through evaporation, and sending the reuse water to a water leaching process and a washing process; the second precipitation wastewater is sent to a water leaching process for leaching roasted ore;
the amount of the high-concentration second precipitation wastewater returned to the solid sulfuric acid rare earth water leaching process accounts for 0-20% of the total amount of the precipitation wastewater.
And 4, step 4: and (4) washing the mixed rare earth carbonate by using reuse water, and returning the generated low-concentration leaching water to the preparation process of the precipitator.
The whole process realizes the full cyclic utilization of wastewater resources, can improve the concentration of precipitated wastewater, and reduces the wastewater treatment cost. And (3) adopting continuous or intermittent filtering equipment for the mixed rare earth carbonate to respectively recover high-concentration precipitation wastewater and low-concentration leaching water. The amount of the precipitator prepared from the low-concentration leaching water accounts for 0-100% of the total water amount.
Example 1
Rare earth sulfate solution REO 30g/L, pH 5.4, rare earth sulfate water leaching solution given flow 25m3H, precipitant concentration 2N, 7m3H, high-concentration supernatant liquid 32m is produced after the precipitation is finished3H, returning the high-concentration precipitation wastewater to the water leaching process for 6.4m3And h, no rare earth double salt is generated in the water leaching process, the concentration of the rare earth sulfate solution is not changed, the content of the rare earth in the discharged slag still meets less than 5 percent, the washing water is reused for preparing the precipitator, and the quality of the rare earth carbonate product meets the requirement.
Example 2
The rare earth sulfate solution REO is 30g/L, the pH is 5.4, the rare earth solution has given flow rate of 25m3H, precipitant concentration 2N, 7m3H, high-concentration supernatant liquid 32m is produced after the precipitation is finished3H, returning the high-concentration precipitation wastewater to the water leaching process for 3.2m3And h, no rare earth double salt is generated in the water leaching process, the concentration of the rare earth sulfate solution is not changed, the content of the rare earth in the discharged slag still meets less than 5 percent, the washing water is reused for preparing the precipitator, and the quality of the rare earth carbonate product meets the requirement.
Example 3
The rare earth sulfate solution REO is 25g/L, the pH is 5.4, the rare earth solution has given flow rate of 25m3H, precipitant concentration 2N, 6m3H, high-concentration supernatant 31m is produced after the precipitation is finished3H, returning the high-concentration precipitation wastewater to the water leaching process for 6.2m3And h, no rare earth double salt is generated in the water leaching process, the concentration of the rare earth sulfate solution is not changed, the content of the rare earth in the discharged slag still meets less than 5 percent, 100 percent of washing water is reused for preparing the precipitator, and the quality of the rare earth carbonate product meets the requirement.
Example 4
The rare earth sulfate solution REO is 25g/L, the pH is 5.4, the given flow rate of the rare earth solution is 100m3H, precipitant concentration 2N, 23m3H, high-concentration supernatant liquor 123m is produced after the precipitation is finished3H, returning the high-concentration precipitation wastewater to the water leaching process for 25m3And h, no rare earth double salt is generated in the water leaching process, the concentration of the rare earth sulfate solution is not changed, the content of the rare earth in the discharged slag still meets less than 5 percent, 100 percent of washing water is reused for preparing the precipitator, and the quality of the rare earth carbonate product meets the requirement.
The terminology used herein is for the purpose of description and illustration, rather than of limitation. As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, it should also be understood that the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the meets and bounds of the claims, or equivalences of such meets and bounds are therefore intended to be embraced by the appended claims.
Claims (5)
1. The method for recycling the mixed rare earth carbonate precipitation wastewater comprises the following steps:
leaching roasted ore with water to remove impurities to obtain rare earth sulfate water leaching solution, and reacting the rare earth sulfate water leaching solution with a precipitator to generate rare earth carbonate and supernatant;
filtering slurry obtained after the reaction of the rare earth sulfate water leaching solution and the precipitator, wherein supernatant is precipitation wastewater, and solid is mixed rare earth carbonate;
the precipitated wastewater is divided into first precipitated wastewater and second precipitated wastewater, the first precipitated wastewater is sent to a wastewater treatment workshop for wastewater treatment, salts (ammonium sulfate or sodium sulfate salts) recovered through evaporation are recovered, and the recycled water is sent to a water leaching process and a washing process; the second precipitation wastewater is sent to a water leaching process for leaching roasted ore;
and (4) washing the mixed rare earth carbonate by using reuse water, and returning the generated low-concentration leaching water to the preparation process of the precipitator.
2. The method for recycling the waste water generated by precipitating the rare earth mixed carbonate according to claim 1, wherein the precipitant reacts with the rare earth sulfate aqueous leaching solution which contains 20-40 g/L of rare earth and has a pH value of 3.8-5.4.
3. The method for recycling waste water from rare earth precipitation by mixed carbonate according to claim 1, wherein the amount of the second precipitation waste water returned to the solid rare earth sulfate water leaching process accounts for 0-20% of the total amount of the precipitation waste water.
4. The method for recycling waste water generated by precipitating rare earth mixed carbonate according to claim 1, wherein the amount of the precipitant prepared from the leaching water is 0-100% of the total water amount.
5. The method for recycling waste water generated by precipitating rare earth mixed carbonate according to claim 1, wherein the precipitating agent is solid or liquid ammonium salt or sodium salt.
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| CN201911314904.0A CN111074071A (en) | 2019-12-19 | 2019-12-19 | Method for recycling mixed rare earth carbonate precipitation wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114737049A (en) * | 2021-12-27 | 2022-07-12 | 包头华美稀土高科有限公司 | Method for removing phosphorus in rare earth leaching solution |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967559A (en) * | 2010-07-20 | 2011-02-09 | 包头市京瑞新材料有限公司 | Self recycling method of waste water in rare earth carbonate precipitation |
| US20160068929A1 (en) * | 2014-09-08 | 2016-03-10 | Patrick R. Taylor | EXTRACTION OF RARE EARTH METALS FROM NdFeB USING SELECTIVE SULFATION ROASTING |
| CN108728642A (en) * | 2018-06-28 | 2018-11-02 | 武汉工程大学 | A kind of method of weathered superficial leaching rare-earth ore leachate ammonium bicarbonate precipitation rare earth Mother liquor multiplexing recovering rare earth |
| CN109207717A (en) * | 2018-09-04 | 2019-01-15 | 包头稀土研究院 | In sulfuric acid rare earth infusion and cleans and recycle the method for preparing high-purity mixed chlorinated rare earth |
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- 2019-12-19 CN CN201911314904.0A patent/CN111074071A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967559A (en) * | 2010-07-20 | 2011-02-09 | 包头市京瑞新材料有限公司 | Self recycling method of waste water in rare earth carbonate precipitation |
| US20160068929A1 (en) * | 2014-09-08 | 2016-03-10 | Patrick R. Taylor | EXTRACTION OF RARE EARTH METALS FROM NdFeB USING SELECTIVE SULFATION ROASTING |
| CN108728642A (en) * | 2018-06-28 | 2018-11-02 | 武汉工程大学 | A kind of method of weathered superficial leaching rare-earth ore leachate ammonium bicarbonate precipitation rare earth Mother liquor multiplexing recovering rare earth |
| CN109207717A (en) * | 2018-09-04 | 2019-01-15 | 包头稀土研究院 | In sulfuric acid rare earth infusion and cleans and recycle the method for preparing high-purity mixed chlorinated rare earth |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114737049A (en) * | 2021-12-27 | 2022-07-12 | 包头华美稀土高科有限公司 | Method for removing phosphorus in rare earth leaching solution |
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