CN111392756A - Process for extracting high-purity rare earth oxide from fluorescent powder waste - Google Patents
Process for extracting high-purity rare earth oxide from fluorescent powder waste Download PDFInfo
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- CN111392756A CN111392756A CN202010373150.2A CN202010373150A CN111392756A CN 111392756 A CN111392756 A CN 111392756A CN 202010373150 A CN202010373150 A CN 202010373150A CN 111392756 A CN111392756 A CN 111392756A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- C22B59/00—Obtaining rare earth metals
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- C—CHEMISTRY; METALLURGY
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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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
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Abstract
The invention provides a process for extracting high-purity rare earth oxide from fluorescent powder waste, and relates to the technical field of fluorescent powder waste recovery. The process for extracting the high-purity rare earth oxide from the fluorescent powder waste comprises the following steps: s1, preparing fluorescent powder waste, and crushing the fluorescent powder waste to obtain fine powdery fluorescent powder waste; s2, adding the crushed fluorescent powder waste into the reaction kettle, then adding a proper amount of clear water into the reaction kettle, heating and stirring for a period of time. According to the invention, the rare earth elements which are difficult to leach are conveniently extracted by means of hydrochloric acid leaching and sodium carbonate adding roasting, the effect is obvious, meanwhile, the recovery rate of the rare earth elements is further improved by means of dissolving the hydrochloric acid solution and thiourea, the impurities of iron, silicon and aluminum in the solution can be rapidly and effectively removed by means of matching of the alkaline solution and the flocculating agent, and the purity of the recovered and produced rare earth oxide is further improved.
Description
Technical Field
The invention relates to the technical field of fluorescent powder waste recovery, in particular to a process for extracting high-purity rare earth oxide from fluorescent powder waste.
Background
At present, China is in the stage of rapid development of science and technology, the production technology is rapidly improved, the product is rapidly updated, due to factors of production and use, domestic fluorescent powder waste reaches dozens of thousands of tons every year, the quantity of the waste is very large, the fluorescent powder waste contains a certain amount of rare earth elements, and the rare earth elements have great recycling value.
In the prior art, the process for extracting and recovering rare earth elements such as europium, yttrium and the like from the fluorescent powder waste materials generally comprises the steps of directly roasting the fluorescent powder waste materials, then leaching by adopting an acid solution, then precipitating and removing impurities, and roasting at a high temperature to produce rare earth oxides.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a process for extracting high-purity rare earth oxide from fluorescent powder waste, and solves the defects in the prior art.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a process for extracting high purity rare earth oxides from phosphor waste, said process comprising the steps of:
s1, preparing fluorescent powder waste, and crushing the fluorescent powder waste to obtain fine powdery fluorescent powder waste;
s2, adding the crushed fluorescent powder waste into a reaction kettle, then adding a proper amount of clear water into the reaction kettle, heating and stirring for a period of time;
s3, slowly adding a hydrochloric acid solution into the reaction kettle for dissolving, and removing supernatant in the reaction kettle after clarification; continuously adding clear water into the reaction kettle to clean the substances in the reaction kettle;
s4, after cleaning, taking out filter residues in the reaction kettle, adding sodium carbonate, uniformly mixing, and then sending the mixture into a roasting furnace for roasting treatment;
s5, adding an oxidant into the roasted solid, adding clear water into the oxidized solid to prepare slurry, adding a hydrochloric acid solution and thiourea into the slurry to dissolve, filtering the solution to obtain rare earth chloride feed liquid, and then removing impurities;
s6, adding an alkaline solution and a flocculating agent into the rare earth chloride feed liquid, fully stirring, standing for a period of time, and then filtering and removing impurities to obtain a rare earth chloride solution;
s7, slowly adding an oxalic acid solution into the rare earth chloride solution, heating and stirring to obtain a rare earth oxalic acid substance;
s8, burning the obtained rare earth oxalic acid at high temperature, and then dehydrating, carbonizing and oxidizing to obtain the high-purity rare earth oxide.
Preferably, the time for the pulverization treatment of the phosphor waste in the step 1 is 5-10min, and the particle size of the powdered phosphor waste is 3000-5000 meshes.
Preferably, the stirring time of the fluorescent powder waste in the step 2 is 30-50min, and the temperature in the reaction kettle is set to be 40-60 ℃.
Preferably, the time for adding the hydrochloric acid solution to dissolve in the step 3 is 5-7h, the frequency for cleaning the filter residue is 3-5 times, and the concentration of the hydrochloric acid solution is 2-4 mol/L.
Preferably, the mixing time of the filter residue and the sodium carbonate in the step 4 is 10-20min, the roasting time of the mixture in the roasting furnace is 2-4h, and the roasting temperature is 400-.
Preferably, in the step 5, the solid oxidation time is 2-4h, the concentration of the hydrochloric acid solution is 3-5 mol/L, the mass ratio of the addition amount of the thiourea to the slurry is 1:35-45, the solution time of the slurry is 80-100min, and the solution temperature is 70-90 ℃.
Preferably, in the step 6, the alkaline solution is a sodium hydroxide solution, a potassium hydroxide solution or a mixed solution of the sodium hydroxide solution and the potassium hydroxide solution in any proportion, the concentration of the alkaline solution is 2-4 mol/L, and the flocculating agent is prepared from an inorganic flocculating agent and polyacrylamide.
Preferably, the heating temperature in the step 7 is controlled to be 60-70 ℃, and the stirring treatment time is 40-60 min.
Preferably, the temperature for the high-temperature roasting of the rare earth oxalate in the step 8 is 900-.
(III) advantageous effects
The invention provides a process for extracting high-purity rare earth oxide from fluorescent powder waste. The method has the following beneficial effects:
according to the invention, the rare earth elements which are difficult to leach are conveniently extracted by means of hydrochloric acid leaching and sodium carbonate adding roasting, the effect is obvious, meanwhile, the recovery rate of the rare earth elements is further improved by means of dissolving the hydrochloric acid solution and thiourea, the impurities of iron, silicon and aluminum in the solution can be rapidly and effectively removed by means of matching of the alkaline solution and the flocculating agent, and the purity of the recovered and produced rare earth oxide is further improved.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides a process for extracting high-purity rare earth oxide from fluorescent powder waste, which comprises the following steps:
s1, preparing fluorescent powder waste, and crushing the fluorescent powder waste to obtain fine powdery fluorescent powder waste, wherein the crushing time of the fluorescent powder waste is 10min, the granularity of the powdery fluorescent powder waste is 3000 meshes, the contact area of the crushed powdery fluorescent powder waste and a solution is larger, and the extraction time can be shortened to a certain extent;
s2, adding the crushed fluorescent powder waste into a reaction kettle, then adding a proper amount of clear water into the reaction kettle, heating and stirring for a period of time, wherein the stirring time of the fluorescent powder waste is 50min, and the temperature in the reaction kettle is set to be 40 ℃;
s3, slowly adding a hydrochloric acid solution into the reaction kettle to dissolve, removing supernatant in the reaction kettle after clarification, continuously adding clear water into the reaction kettle to clean substances in the reaction kettle, wherein the hydrochloric acid solution is added for dissolving for 7 hours, the cleaning frequency of filter residues is 3 times, and the concentration of the hydrochloric acid solution is 2 mol/L;
s4, after cleaning, taking out filter residues in the reaction kettle, adding sodium carbonate, uniformly mixing, and then sending the mixture into a roasting furnace for roasting treatment, wherein the mixing time of the filter residues and the sodium carbonate is 20min, the roasting time of the mixture in the roasting furnace is 4h, and the roasting temperature is 400 ℃;
s5, adding an oxidant into the roasted solid, adding clear water into the oxidized solid to prepare slurry, adding a hydrochloric acid solution and thiourea into the slurry to dissolve, filtering the solution to obtain rare earth chloride feed liquid, and then removing impurities, wherein the solid is oxidized for 4 hours, the concentration of the hydrochloric acid solution is 3 mol/L, the mass ratio of the addition amount of the thiourea to the slurry is 1:35, the solution time of the slurry is 100min, and the solution temperature is 70 ℃;
s6, adding an alkaline solution and a flocculating agent into the rare earth chloride feed liquid, fully stirring, standing for a period of time, and then filtering and removing impurities to obtain a rare earth chloride solution, wherein the alkaline solution is a sodium hydroxide solution, a potassium hydroxide solution or a mixed solution of the sodium hydroxide solution and the potassium hydroxide solution in any proportion, the concentration of the alkaline solution is 2 mol/L, the flocculating agent is prepared from an inorganic flocculating agent and polyacrylamide, the alkaline solution can react with iron, silicon and aluminum impurities to generate precipitates, and then the flocculating agent can adsorb and aggregate the precipitates, so that the precipitates in the solution can be treated more cleanly;
s7, slowly adding an oxalic acid solution into the rare earth chloride solution, heating and stirring to obtain a rare earth oxalic acid substance, wherein the heating temperature is controlled to be 60 ℃, and the stirring treatment time is 60 min;
s8, burning the obtained rare earth oxalate at high temperature, dehydrating, carbonizing and oxidizing to obtain the high-purity rare earth oxide, wherein the high-temperature roasting temperature of the rare earth oxalate is 900 ℃.
According to the invention, the rare earth elements which are difficult to leach are conveniently extracted by means of hydrochloric acid leaching and sodium carbonate adding roasting, the effect is obvious, meanwhile, the recovery rate of the rare earth elements is further improved by means of dissolving the hydrochloric acid solution and thiourea, the impurities of iron, silicon and aluminum in the solution can be rapidly and effectively removed by means of matching of the alkaline solution and the flocculating agent, and the purity of the recovered and produced rare earth oxide is further improved.
Example two:
the embodiment of the invention provides a process for extracting high-purity rare earth oxide from fluorescent powder waste, which comprises the following steps:
s1, preparing fluorescent powder waste, and crushing the fluorescent powder waste to obtain fine powdery fluorescent powder waste, wherein the crushing time of the fluorescent powder waste is 7min, and the granularity of the powdery fluorescent powder waste is 4000 meshes;
s2, adding the crushed fluorescent powder waste into a reaction kettle, then adding a proper amount of clear water into the reaction kettle, heating and stirring for a period of time, wherein the stirring time of the fluorescent powder waste is 40min, and the temperature in the reaction kettle is set to be 50 ℃;
s3, slowly adding a hydrochloric acid solution into the reaction kettle to dissolve, removing supernatant in the reaction kettle after clarification, continuously adding clear water into the reaction kettle to clean substances in the reaction kettle, wherein the hydrochloric acid solution is added for dissolving for 6 hours, the cleaning frequency of filter residues is 4 times, and the concentration of the hydrochloric acid solution is 3 mol/L;
s4, after cleaning, taking out filter residues in the reaction kettle, adding sodium carbonate, uniformly mixing, and then sending the mixture into a roasting furnace for roasting treatment, wherein the mixing time of the filter residues and the sodium carbonate is 15min, the roasting time of the mixture in the roasting furnace is 3h, and the roasting temperature is 500 ℃;
s5, adding an oxidant into the roasted solid, adding clear water into the oxidized solid to prepare slurry, adding a hydrochloric acid solution and thiourea into the slurry to dissolve, filtering the solution to obtain rare earth chloride feed liquid, and then removing impurities, wherein the solid is oxidized for 3 hours, the concentration of the hydrochloric acid solution is 4 mol/L, the mass ratio of the addition amount of the thiourea to the slurry is 1:40, the solution time of the slurry is 90min, and the solution temperature is 80 ℃;
s6, adding an alkaline solution and a flocculating agent into the rare earth chloride feed liquid, fully stirring, standing for a period of time, and then filtering and removing impurities to obtain a rare earth chloride solution, wherein the alkaline solution is a sodium hydroxide solution, a potassium hydroxide solution or a mixed solution of the sodium hydroxide solution and the potassium hydroxide solution in any proportion, the concentration of the alkaline solution is 3 mol/L, and the flocculating agent is prepared from an inorganic flocculating agent and polyacrylamide;
s7, slowly adding an oxalic acid solution into the rare earth chloride solution, heating and stirring to obtain a rare earth oxalic acid substance, wherein the heating temperature is controlled to be 65 ℃, and the stirring treatment time is 50 min;
s8, burning the obtained rare earth oxalate at high temperature, dehydrating, carbonizing and oxidizing to obtain the high-purity rare earth oxide, wherein the high-temperature roasting temperature of the rare earth oxalate is 1000 ℃.
Example three:
the embodiment of the invention provides a process for extracting high-purity rare earth oxide from fluorescent powder waste, which comprises the following steps:
s1, preparing fluorescent powder waste, and crushing the fluorescent powder waste to obtain fine powdery fluorescent powder waste, wherein the crushing time of the fluorescent powder waste is 5min, and the granularity of the powdery fluorescent powder waste is 5000 meshes;
s2, adding the crushed fluorescent powder waste into a reaction kettle, then adding a proper amount of clear water into the reaction kettle, heating and stirring for a period of time, wherein the stirring time of the fluorescent powder waste is 30min, and the temperature in the reaction kettle is set to be 60 ℃;
s3, slowly adding a hydrochloric acid solution into the reaction kettle to dissolve, removing supernatant in the reaction kettle after clarification, continuously adding clear water into the reaction kettle to clean substances in the reaction kettle, wherein the hydrochloric acid solution is added for dissolving for 5 hours, the filter residue is cleaned for 5 times, and the concentration of the hydrochloric acid solution is 4 mol/L;
s4, after cleaning, taking out filter residues in the reaction kettle, adding sodium carbonate, uniformly mixing, and then sending the mixture into a roasting furnace for roasting treatment, wherein the mixing time of the filter residues and the sodium carbonate is 10min, the roasting time of the mixture in the roasting furnace is 2h, and the roasting temperature is 600 ℃;
s5, adding an oxidant into the roasted solid, adding clear water into the oxidized solid to prepare slurry, adding a hydrochloric acid solution and thiourea into the slurry to dissolve, filtering the solution to obtain rare earth chloride feed liquid, and then removing impurities, wherein the solid is oxidized for 4 hours, the concentration of the hydrochloric acid solution is 5 mol/L, the mass ratio of the addition amount of the thiourea to the slurry is 1:45, the solution time of the slurry is 80min, and the solution temperature is 90 ℃;
s6, adding an alkaline solution and a flocculating agent into the rare earth chloride feed liquid, fully stirring, standing for a period of time, and then filtering and removing impurities to obtain a rare earth chloride solution, wherein the alkaline solution is a sodium hydroxide solution, a potassium hydroxide solution or a mixed solution of the sodium hydroxide solution and the potassium hydroxide solution in any proportion, the concentration of the alkaline solution is 4 mol/L, and the flocculating agent is prepared from an inorganic flocculating agent and polyacrylamide;
s7, slowly adding an oxalic acid solution into the rare earth chloride solution, heating and stirring to obtain a rare earth oxalic acid substance, wherein the heating temperature is controlled to be 70 ℃, and the stirring treatment time is 40 min;
s8, burning the obtained rare earth oxalate at high temperature, dehydrating, carbonizing and oxidizing to obtain the high-purity rare earth oxide, wherein the high-temperature roasting temperature of the rare earth oxalate is 1100 ℃.
In the invention, the obtained high-purity rare earth oxide is subjected to rare earth element detection, the content of europium, yttrium and terbium is determined according to a GB-T14635-2008 rare earth metal and compound chemical analysis method thereof, and the recovery rate of the europium, yttrium and terbium is analyzed;
wherein W represents the recovery (%) of europium, yttrium or terbium;
M1the content (g) of europium, yttrium or terbium in the rare earth elements is measured;
M2the theoretical content (g) of europium, yttrium or terbium detection;
at the same time, compared to the prior art (where the comparative examples were in the conventional manner), the results are obtained as shown in table 1 below:
TABLE 1
As can be seen from Table 1, in the invention, the recovery rates of europium, yttrium and terbium in the extracted high-purity rare earth oxide are obviously improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A process for extracting high-purity rare earth oxide from fluorescent powder waste is characterized by comprising the following steps: the process comprises the following steps:
s1, preparing fluorescent powder waste, and crushing the fluorescent powder waste to obtain fine powdery fluorescent powder waste;
s2, adding the crushed fluorescent powder waste into a reaction kettle, then adding a proper amount of clear water into the reaction kettle, heating and stirring for a period of time;
s3, slowly adding a hydrochloric acid solution into the reaction kettle for dissolving, and removing supernatant in the reaction kettle after clarification; continuously adding clear water into the reaction kettle to clean the substances in the reaction kettle;
s4, after cleaning, taking out filter residues in the reaction kettle, adding sodium carbonate, uniformly mixing, and then sending the mixture into a roasting furnace for roasting treatment;
s5, adding an oxidant into the roasted solid, adding clear water into the oxidized solid to prepare slurry, adding a hydrochloric acid solution and thiourea into the slurry to dissolve, filtering the solution to obtain rare earth chloride feed liquid, and then removing impurities;
s6, adding an alkaline solution and a flocculating agent into the rare earth chloride feed liquid, fully stirring, standing for a period of time, and then filtering and removing impurities to obtain a rare earth chloride solution;
s7, slowly adding an oxalic acid solution into the rare earth chloride solution, heating and stirring to obtain a rare earth oxalic acid substance;
s8, burning the obtained rare earth oxalic acid at high temperature, and then dehydrating, carbonizing and oxidizing to obtain the high-purity rare earth oxide.
2. The process of claim 1 for extracting high purity rare earth oxides from phosphor waste, wherein: the time for crushing the fluorescent powder waste in the step 1 is 5-10min, and the granularity of the powdery fluorescent powder waste is 3000-5000 meshes.
3. The process of claim 1 for extracting high purity rare earth oxides from phosphor waste, wherein: the stirring time of the fluorescent powder waste in the step 2 is 30-50min, and the temperature in the reaction kettle is set to be 40-60 ℃.
4. The process for extracting high-purity rare earth oxide from fluorescent powder waste according to claim 1, wherein the time for adding hydrochloric acid solution to dissolve in the step 3 is 5-7h, the number of times for cleaning filter residue is 3-5, and the concentration of hydrochloric acid solution is 2-4 mol/L.
5. The process of claim 1 for extracting high purity rare earth oxides from phosphor waste, wherein: in the step 4, the mixing time of the filter residue and the sodium carbonate is 10-20min, the roasting time of the mixture in the roasting furnace is 2-4h, and the roasting temperature is 400-600 ℃.
6. The process of claim 1, wherein in the step 5, the solid oxidation time is 2-4h, the concentration of the hydrochloric acid solution is 3-5 mol/L, the mass ratio of the thiourea to the slurry is 1:35-45, the solution time of the slurry is 80-100min, and the solution temperature is 70-90 ℃.
7. The process of claim 1, wherein in the step 6, the alkaline solution is sodium hydroxide solution, potassium hydroxide solution or a mixture of sodium hydroxide solution and potassium hydroxide solution in any proportion, the concentration of the alkaline solution is 2-4 mol/L, and the flocculating agent is prepared from an inorganic flocculating agent and polyacrylamide.
8. The process of claim 1 for extracting high purity rare earth oxides from phosphor waste, wherein: in the step 7, the heating temperature is controlled to be 60-70 ℃, and the stirring treatment time is 40-60 min.
9. The process of claim 1 for extracting high purity rare earth oxides from phosphor waste, wherein: the high-temperature roasting temperature of the rare earth oxalate in the step 8 is 900-1100 ℃.
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| CN114959319A (en) * | 2022-06-30 | 2022-08-30 | 包头稀土研究院 | Method for treating solid obtained by alkaline decomposition process of mixed rare earth concentrate |
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| CN114959319B (en) * | 2022-06-30 | 2023-09-08 | 包头稀土研究院 | Method for treating solid matters obtained by mixed rare earth concentrate alkaline decomposition process |
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Application publication date: 20200710 |