CN111004933A - Six-stage continuous complete dissolution method for monazite optimal dissolution slag - Google Patents
Six-stage continuous complete dissolution method for monazite optimal dissolution slag Download PDFInfo
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- CN111004933A CN111004933A CN201911362863.2A CN201911362863A CN111004933A CN 111004933 A CN111004933 A CN 111004933A CN 201911362863 A CN201911362863 A CN 201911362863A CN 111004933 A CN111004933 A CN 111004933A
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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
- 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
- C22B3/10—Hydrochloric acid, other halogenated 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0221—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching
- C22B60/0226—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors
- C22B60/023—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors halogenated ion as active agent
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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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0291—Obtaining thorium, uranium, or other actinides obtaining thorium
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Abstract
The invention belongs to the technical field of smelting and separating of monazite of rare earth ore, and particularly relates to a six-stage continuous complete dissolution method of monazite optimal dissolution slag. Continuously dissolving radioactivity optimum dissolving slag left after rare earth is extracted from monazite concentrate through alkaline decomposition by adopting six grades of hydrochloric acid; leaching reaction, wherein the concentration of residual acid after the reaction is controlled to be 2.5mol/L, and hydrochloric acid needs to be added when the hydrochloric acid is insufficient; adjusting and optimizing the addition of hydrogen peroxide, and keeping the valence state of cerium element at + 4; boiling, performing solid-liquid separation after aging, and introducing filtrate containing uranium and thorium into the subsequent uranium and thorium extraction and recovery process. The invention can recover uranium and thorium radionuclide to the maximum extent, and improve the resource utilization rate of valuable rare earth elements.
Description
Technical Field
The invention belongs to the technical field of smelting and separating of monazite of rare earth ore, and particularly relates to a six-stage continuous complete dissolution method of monazite optimal dissolution slag.
Background
With the development of science and technology, rare earth elements gradually show their special physical and chemical properties in modern functional materials such as metallurgy, petrochemical industry, glass ceramics, permanent magnetic materials, luminescent materials, hydrogen storage materials, etc., and have become support materials in high and new technical fields such as information, biology, new materials and new energy. The continuous expansion of the application of the rare earth and the continuous improvement of the quality requirement of the rare earth product promote the development of rare earth production enterprises and the improvement of the separation technology level.
Monazite is one of the most widely distributed and important rare earth minerals, is rich in rare earth, uranium, thorium and other precious resources, and has a chemical expression of (Ce, La and Th) PO4. China develops various process flows by researching the smelting separation process of monazite from the 70 th of the 20 th century,the more mature industrial production process mainly comprises a sulfuric acid roasting method and a caustic soda leaching method. However, for a long time, monazite concentrate is mainly used for extracting rare earth chloride and phosphorus, and the problems of waste gas, waste water and waste residues generated in the production process are not reasonably treated, so that huge environmental pollution and pressure are caused. At present, most enterprises for smelting and producing monazite in China adopt a caustic soda digestion process, the emission of waste gas and waste water is reduced to a certain extent, but most enterprises do not carry out radioactive element recovery treatment on the generated waste residues, and only carry out concentrated stacking overstock on the generated radioactive waste residues, so that a large amount of waste of strategic resources such as thorium, uranium and the like is caused, and the method is a potential threat to the environment, and therefore, the development of green, pollution-free and effective recycling of the monazite waste residues has important significance.
The invention aims to perform optimized full-solution leaching treatment on the radioactive optimum-dissolution slag generated by the monazite concentrate classical alkali decomposition process, improve the resource utilization rate of valuable rare earth elements, recover uranium and thorium radionuclides to the maximum extent, reduce environmental pollution and form a green cycle process for comprehensively recovering monazite resources. The filtrate after solid-liquid separation has better filtering effect, and creates good conditions for the subsequent extraction and recovery of uranium and thorium.
Disclosure of Invention
The invention aims to provide a six-stage continuous complete dissolution method of monazite optimal slag, which aims to comprehensively recycle uranium and thorium radionuclides in radioactive optimal slag left after rare earth is extracted from monazite concentrate through alkaline decomposition.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a six-stage continuous complete dissolution method of monazite slag,
(1) continuously dissolving radioactivity optimum dissolving slag left after rare earth is extracted from monazite concentrate through alkaline decomposition by adopting six grades of hydrochloric acid;
(2) leaching reaction, wherein the concentration of residual acid after the reaction is controlled to be 2.5mol/L, and hydrochloric acid needs to be added when the hydrochloric acid is insufficient;
(3) adjusting and optimizing the addition of hydrogen peroxide, and keeping the valence state of cerium element at + 4; boiling, performing solid-liquid separation after aging, and introducing filtrate containing uranium and thorium into the subsequent uranium and thorium extraction and recovery process.
In the step (1), the hydrochloric acid is 6mol/L, and the ratio of the hydrochloric acid to the optimum slag is 1.5: 1, namely one ton of excellent slag is mixed with 1.5 tons of hydrochloric acid.
In the step (2), the leaching reaction time is 4 hours, and the reaction temperature is 85-95 ℃.
In the step (3), the mass ratio of the added hydrogen peroxide to the optimal slag is 0.055: 1.
and (3) boiling at 110 ℃ for 1 h.
And (3) aging for 12 h.
The beneficial effects obtained by the invention are as follows:
the treatment method provided by the invention can be used for recovering uranium and thorium radionuclides to the maximum extent, and improving the resource utilization rate of valuable rare earth elements. Under the optimal treatment condition, the leaching rates of uranium and thorium are respectively 93.6 percent and 94.2 percent, and the total rare earth slag leaching rate reaches 94.8 percent; the solution has better filtering effect, the filtered solution is clear, and the filtering speed per unit area reaches 0.035m3/(m2H) to create good conditions for the subsequent uranium and thorium extraction process.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The six-stage continuous complete dissolution method of monazite slag comprises the following steps:
(1) after rare earth is extracted from monazite concentrate through alkaline decomposition, the remaining radioactive optimum dissolution slag is continuously dissolved by six levels of high-concentration hydrochloric acid (6mol/L), and the ratio of acid to optimum dissolution slag is 1.5: 1, namely one ton of optimum slag, and 1.5 tons of hydrochloric acid.
(2) The leaching reaction time is 4 hours, the reaction temperature is 85-95 ℃, and the concentration of the residual acid after the reaction is controlled to be 2.5mol/L (the residual acid needs to be added when the acid is insufficient).
(3) Adjusting and optimizing the adding amount of hydrogen peroxide, wherein the ratio of the adding amount of hydrogen peroxide to the optimal slag is 0.055: the purpose of adding hydrogen peroxide is to keep the cerium element in a +4 valence state. Boiling at 110 ℃ for 1h, aging for 12h, performing solid-liquid separation, and allowing uranium and thorium-containing filtrate to enter a subsequent uranium and thorium extraction and recovery process.
In the treatment method, a large number of experiments show that the increase of the use amount of the hydrochloric acid is beneficial to improving the leaching rates of uranium and thorium, when the residual acid of the solution is controlled to be 0.50mol/L, the leaching rate of uranium is 87.6%, and the leaching rates of thorium are 82.3%; when the residual acid of the solution is controlled to be 1.17mol/L, the leaching rates of uranium and thorium are both more than 92 percent; the dosage of the hydrochloric acid is continuously increased, and the leaching rate of the uranium and the thorium is slowly improved. When the leaching temperature is 90 ℃, the solution sedimentation performance is good, the filtering speed is greatly increased, the solution filtering effect is good, the filtered solution is clear, and the filtering speed per unit area is remarkably improved. The leaching time is prolonged, so that the leaching rates of uranium and thorium are improved, when the leaching time reaches 4 hours, the leaching rates of uranium and thorium tend to be gentle, the leaching time is continuously increased, and the leaching rate of uranium is not greatly improved.
The invention provides a novel six-stage continuous complete dissolution process technology for monazite optimum dissolution slag, and relates to the rare earth metallurgy industry. The method carries out full-dissolution treatment on the radioactive optimum-dissolution slag generated by the monazite concentrate classical alkali decomposition process, reasonably recycles and disposes radionuclides such as uranium, thorium and the like, and prevents radioactive elements from polluting the environment. The process technology comprises the steps of firstly, continuously dissolving high-concentration hydrochloric acid six-stage dissolved slag generated by dissolving an alkali cake generated by decomposing monazite concentrate into alkali through hydrochloric acid, controlling the concentration of residual acid after reaction, adjusting and optimizing the technological conditions of adding amount of hydrogen peroxide, boiling, aging and the like, obtaining leached ore pulp, and then, filtering and separating. And extracting and separating subsequent uranium, thorium and rare earth from the filtrate. According to the novel six-stage continuous total-dissolution process for monazite optimum-dissolution slag, under the condition of the optimal process parameters, the leaching rates of uranium and thorium are 93.6% and 94.2% respectively, and the total rare earth slag leaching rate reaches 94.8%; the solution has better filtering effect, the filtered solution is clear, and the filtering speed per unit area reaches 0.035m3/(m2H) to create good conditions for the subsequent uranium and thorium extraction process.
A six-stage continuous complete dissolution method of monazite slag comprises the following steps: six-stage continuous dissolution of high-concentration hydrochloric acid is adopted to continuously dissolve radioactive optimum-dissolution slag left after rare earth is extracted from monazite concentrate through alkaline decomposition, the concentration of residual acid after reaction is controlled, the technological conditions of optimizing hydrogen peroxide addition, boiling, aging and the like are adjusted, and the leached ore pulp is filtered and separated. Adding the optimal slag into the molten steel according to the liquid-solid ratio of 1.5: 1, leaching for 4 hours by using concentrated hydrochloric acid with the initial concentration of 5-6 mol/L and controlling the reaction temperature to be 85-95 ℃, wherein the concentration of residual acid after leaching reaction is about 2.5 mol/L. Adding hydrogen peroxide in the proportion of 0.055t/t optimal slag (wet), boiling at 110 ℃ for 1h, aging for 12h, filtering and separating.
The first embodiment is as follows:
six-stage continuous dissolution of high-concentration hydrochloric acid is adopted to continuously dissolve radioactive optimum-dissolution slag left after rare earth is extracted from monazite concentrate through alkaline decomposition, the concentration of residual acid after reaction is controlled, the technological conditions of optimizing hydrogen peroxide addition, boiling, aging and the like are adjusted, and the leached ore pulp is filtered and separated. The filtrate after solid-liquid separation has better filtering effect, and creates good conditions for the subsequent extraction and recovery of uranium and thorium.
Example two:
based on the scheme of the first embodiment, the invention selects the optimal dissolving slag of a rare earth enterprise in province to carry out a verification experiment, and inspects and researches the influence of each process parameter on the leaching rate of the optimal dissolving slag and the filtering performance of the filtrate by regulating and controlling different reaction parameter conditions. The specific experimental data results were analyzed as follows:
a. influence of hydrochloric acid dosage on leaching effect
To improve the leaching rate of uranium, thorium and rare earth in the high-quality slag, the relationship between the dosage of hydrochloric acid and the leaching of each component needs to be considered. Taking 1000g of superior soluble slag respectively, and carrying out experiments by using different hydrochloric acid dosage, wherein the ratio of pulp liquid to solid is 1: 1.5, leaching for 4 hours at 90 ℃ by stirring. The results are shown in Table 1.
TABLE 1 influence of the amount of hydrochloric acid used
As can be seen from Table 1, the increase of the use amount of hydrochloric acid is beneficial to improving the leaching rates of uranium and thorium, when the residual acid of the solution is controlled to be 0.501mol/L, the leaching rate of uranium is 87.6%, and the leaching rates of thorium are 82.3%; when the residual acid of the solution is controlled to be 1.17mol/L, the leaching rates of uranium and thorium are both more than 92 percent; the dosage of the hydrochloric acid is continuously increased, and the leaching rate of the uranium and the thorium is slowly improved. After the dissolution is finished, the observation of the standing sedimentation effect is carried out by each batch; simultaneously, adopting an N235 extractant and a skimming liquid to perform extraction contact to investigate the extraction performance and the extraction process; the result shows that the sedimentation effect is better when the residual acid is controlled to be 2.5mol/L, the uranium extraction process is not emulsified, and the extraction efficiency is acceptable. Therefore, it was preliminarily determined that it is appropriate to control the residual acid to 2.5 mol/L.
b. Effect of Leaching temperature on filtration
The pulp viscosity can be reduced by increasing the leaching temperature, and the diffusion speed is increased. But increasing the temperature also increases the energy consumption. And taking 1000g of the optimal-solution slag respectively, and inspecting the influence of temperature on the leaching and filtering performance. When the initial hydrochloric acid amount is 6mol/L and the residual acid amount is controlled to be 2.5mol/L, the experimental results of the influence of the leaching filtration performance are shown in Table 2.
TABLE 2 influence of leaching temperature on filtration Rate
As shown in Table 2, under the same conditions of 4 hours of leaching reaction and 1 hour of solution boiling, the solution has good settling property and greatly increased filtration speed when the temperature is higher than 90 ℃, and the filtration speed per unit area reaches 0.035m3/(m2H), the solution filtering effect is good, and the filtering rate per unit area is remarkably improved.
c. Effect of reaction time on leaching Effect
Taking 1000g of superior soluble slag respectively, controlling the initial concentration of hydrochloric acid to be 6mol/L and the residual acid to be 2.5mol/L, controlling the reaction temperature to be 90 ℃, and obtaining the experimental result of the influence of the leaching time on the leaching rate of uranium and thorium: along with the prolonging of the leaching time, the leaching rate of uranium and thorium is increased; when the leaching time reaches 4h, the leaching rate of uranium and thorium changes smoothly, the leaching time is continuously increased, and the change of the leaching rate of uranium is not greatly improved. Therefore, for economic reasons, the leaching time is preferably 4 h.
d. Effect of oxidizing agent on Leaching Rate
Taking the superior soluble slag, 1000g eachThe initial concentration of the hydrochloric acid is 6mol/L, the residual acid is controlled to be 2.5mol/L, the reaction temperature is 90 ℃, and the adding amount of the hydrogen peroxide is 0.055g (H)2O2The concentration of ferrous ions in the solution is extremely low, which indicates that the oxidation is relatively sufficient in the reaction process. Table 3 shows four leachate components.
TABLE 3 Effect of oxidizing Agents on leaching Effect
As can be seen from table 3, the oxidant added during leaching has reached a relatively suitable amount.
The optimal technological parameters are verified by developing the optimal slag hydrochloric acid dissolution technological condition experiment. Under the conditions that the initial concentration of hydrochloric acid is 6mol/L and the residual acid is controlled at 2.5mol/L, the reaction temperature is 90 ℃, the dissolution time is 4 hours, the solution is boiled for 1 hour, and the liquid-solid ratio is 1.5: 1, the leaching rates of uranium and thorium are respectively 93.6 percent and 94.2 percent, the total rare earth leaching rate reaches 94.8 percent, uranium and thorium radionuclides are recovered to the maximum extent, the resource utilization rate of valuable rare earth elements is improved, the defect of radioactive waste residue pollution of the traditional rare earth enterprises is overcome, and the green, pollution-free and effective recycling of monazite waste residues is facilitated.
Claims (6)
1. A six-stage continuous complete dissolution method of monazite slag is characterized in that:
(1) continuously dissolving radioactivity optimum dissolving slag left after rare earth is extracted from monazite concentrate through alkaline decomposition by adopting six grades of hydrochloric acid;
(2) leaching reaction, wherein the concentration of residual acid after the reaction is controlled to be 2.5mol/L, and hydrochloric acid needs to be added when the hydrochloric acid is insufficient;
(3) adjusting and optimizing the addition of hydrogen peroxide, and keeping the valence state of cerium element at + 4; boiling, performing solid-liquid separation after aging, and introducing filtrate containing uranium and thorium into the subsequent uranium and thorium extraction and recovery process.
2. The six-stage continuous complete dissolution method of monazite slag according to claim 1, which is characterized in that: in the step (1), the hydrochloric acid is 6mol/L, and the ratio of the hydrochloric acid to the optimum slag is 1.5: 1, namely one ton of excellent slag is mixed with 1.5 tons of hydrochloric acid.
3. The six-stage continuous complete dissolution method of monazite slag according to claim 1, which is characterized in that: in the step (2), the leaching reaction time is 4 hours, and the reaction temperature is 85-95 ℃.
4. The six-stage continuous complete dissolution method of monazite slag according to claim 1, which is characterized in that: in the step (3), the mass ratio of the added hydrogen peroxide to the optimal slag is 0.055: 1.
5. the six-stage continuous complete dissolution method of monazite slag according to claim 1, which is characterized in that: and (3) boiling at 110 ℃ for 1 h.
6. The six-stage continuous complete dissolution method of monazite slag according to claim 1, which is characterized in that: and (3) aging for 12 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112458291A (en) * | 2020-11-10 | 2021-03-09 | 厦门稀土材料研究所 | Method for gradually leaching ionic rare earth ore radioactive waste residues |
| CN112760485A (en) * | 2020-12-21 | 2021-05-07 | 湖南中核金原新材料有限责任公司 | Method for leaching valuable resources from optimal slag |
| CN112759112A (en) * | 2020-12-10 | 2021-05-07 | 核工业北京化工冶金研究院 | Method for precipitating uranium peroxide in uranium-containing sodium carbonate solution |
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Cited By (3)
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| CN112458291A (en) * | 2020-11-10 | 2021-03-09 | 厦门稀土材料研究所 | Method for gradually leaching ionic rare earth ore radioactive waste residues |
| CN112759112A (en) * | 2020-12-10 | 2021-05-07 | 核工业北京化工冶金研究院 | Method for precipitating uranium peroxide in uranium-containing sodium carbonate solution |
| CN112760485A (en) * | 2020-12-21 | 2021-05-07 | 湖南中核金原新材料有限责任公司 | Method for leaching valuable resources from optimal slag |
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Application publication date: 20200414 |