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CN113702564B - Method for detecting separation degree of actinium-227 in rare earth wastewater - Google Patents

Method for detecting separation degree of actinium-227 in rare earth wastewater Download PDF

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CN113702564B
CN113702564B CN202110956166.0A CN202110956166A CN113702564B CN 113702564 B CN113702564 B CN 113702564B CN 202110956166 A CN202110956166 A CN 202110956166A CN 113702564 B CN113702564 B CN 113702564B
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rare earth
actinium
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earth wastewater
concentration
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CN113702564A (en
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张魁芳
刘志强
朱薇
曹洪杨
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Institute of Resource Utilization and Rare Earth Development of Guangdong Academy of Sciences
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/02—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/62—Heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F2001/007—Processes including a sedimentation step
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

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  • Hydrology & Water Resources (AREA)
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Abstract

The invention discloses a method for detecting separation degree of actinium-227 in rare earth wastewater. The method comprises the following steps: adding calcium oxide or calcium hydroxide into the rare earth wastewater to adjust the pH value of the rare earth wastewater solution to 6.0, and measuring the concentration of calcium ions in the supernatant fluid and marking the concentration as W 1; filtering and separating filter residues, adding soluble carbonate into the rare earth wastewater solution with the pH value adjusted, precipitating and separating calcium ions and actinium-227 ions in the rare earth wastewater solution, adjusting the pH value of the rare earth wastewater solution to 7.0-10.0, measuring the concentration of calcium ions in supernatant fluid and marking the concentration as W 2, and calculating the separation rate of calcium ions in the rare earth wastewater solution as follows: w 1-W2/W1 is multiplied by 100 percent, and the separation rate of actinium-227 in the rare earth wastewater solution is evaluated by the separation rate of calcium ions. According to the invention, the separation rate of the actinium-227 ions is evaluated by utilizing the characteristic that the performance of the precipitation separation process of the calcium ions and the actinium-227 ions is similar, and the separation rate of the calcium ions.

Description

Method for detecting separation degree of actinium-227 in rare earth wastewater
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for detecting the separation degree of actinium-227 in rare earth wastewater.
Background
The south ionic rare earth contains a certain amount of actinium-227, and actinium-227 is a daughter of uranium-235, belongs to a very toxic natural radionuclide, and the relative danger of inhaled alpha-radiation is far more than that of radium-226. Along with the separation and extraction of rare earth products by southern ionic rare earth enterprises, a considerable part of actinium-227 enters rare earth wastewater, so that the pollution is serious and the separation is necessary.
The direct measuring method of actinium-227 includes amplification analysis method, alpha energy spectrum and HPGe-gamma spectrum method, etc. these methods are expensive and special, and rare earth enterprises have no such equipment and operation condition. At present, rare earth enterprises mainly indirectly judge the concentration of actinium-227 by simply adopting low-background alpha and beta measuring instruments to measure the total alpha and total beta. However, studies have found that as parent uranium-235 is separated and removed during the extraction process, the actinide-227 radioactivity just entering the wastewater may be very low, but will increase significantly after a period of time, reaching a 99.2% equilibrium only about 140 days (actinide 7 half-lives) and the radioactivity may increase hundreds of times. For this reason, only the total α and total β data detected after equilibration (around 140 days) will reflect the true level of this actinide-227 concentration.
Based on the characteristics, in the actual production of rare earth enterprises, the real separation degree of actinium-227 in the precipitation separation process in the wastewater cannot be reflected rapidly and accurately, so that the radioactivity of the wastewater is difficult to control and exceeds the standard seriously, and huge pressure is brought to the environment. Therefore, a method for rapidly detecting the separation degree of actinium-227 in rare earth wastewater is urgently needed.
Disclosure of Invention
The invention solves the problems in the prior art, and aims to provide a method for detecting the separation degree of actinium-227 in rare earth wastewater, which improves the problem of overlong detection period of the separation degree of actinium-227 in the existing rare earth wastewater.
In order to achieve the above purpose, the invention adopts the following technical scheme: a method for detecting separation degree of actinium-227 in rare earth wastewater, comprising the following steps: adding calcium oxide or calcium hydroxide into the rare earth wastewater to adjust the pH value of the rare earth wastewater solution to 6.0, and measuring the concentration of calcium ions in the supernatant fluid and marking the concentration as W 1; filtering and separating filter residues, adding soluble carbonate into the rare earth wastewater solution with the pH value adjusted, precipitating and separating calcium ions and actinium-227 ions in the rare earth wastewater solution, adjusting the pH value of the rare earth wastewater solution to 7.0-10.0, measuring the concentration of calcium ions in supernatant fluid and marking the concentration as W 2, and calculating the separation rate of calcium ions in the rare earth wastewater solution as follows: w 1-W2/W1 is multiplied by 100 percent, and the separation rate of actinium-227 in the rare earth wastewater solution is evaluated by the separation rate of calcium ions.
Preferably, the rare earth wastewater is rare earth wastewater containing actinium-227, the total alpha concentration is 100-31000 Bq/L, and the total beta concentration is 100-6100 Bq/L.
Preferably, the soluble carbonate is sodium carbonate.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the invention, by utilizing the characteristic that the performances of the precipitation separation process of calcium ions and actinium-227 ions are similar, the separation rate of actinium-227 ions is evaluated by using the calcium ions as a reference element and the separation rate of calcium.
2. The method can calculate the actinium-227 separation degree immediately after the separation operation is finished, and compared with the prior method that the solution is placed for 140 days and then measured, the method greatly shortens the detection time, and can rapidly judge the actinium-227 removal effect of the rare earth wastewater after precipitation treatment.
3. The method provided by the invention does not need expensive equipment, and has simple and convenient experimental and analysis processes and strong practicability.
Detailed Description
The following examples are further illustrative of the invention and are not intended to be limiting thereof. The equipment and reagents used in the present invention are conventional commercially available products in the art, unless specifically indicated.
A method for detecting separation degree of actinium-227 in rare earth wastewater, comprising the following steps: adding calcium oxide or calcium hydroxide into the rare earth wastewater to adjust the pH value of the rare earth wastewater solution to 6.0, and measuring the concentration of calcium ions in the supernatant fluid and marking the concentration as W 1; after filtering and separating filter residues, adding sodium carbonate into the rare earth wastewater solution with the pH value adjusted, precipitating and separating calcium ions and actinium-227 ions in the rare earth wastewater solution, adjusting the pH value of the rare earth wastewater solution to 7.0-10.0, measuring the concentration of calcium ions in supernatant fluid, marking the concentration as W 2, and calculating the separation rate of calcium ions in the rare earth wastewater solution as follows: w 1-W2/W1 is multiplied by 100 percent, and the separation rate of actinium-227 in the rare earth wastewater solution is evaluated by the separation rate of calcium ions.
After the actinium-227 rare earth-containing wastewater used in examples 1 to 4 and comparative examples 1 to 3 below was left for 140 days, the total alpha concentration was 258Bq/L and the total beta concentration was 172Bq/L.
Example 1
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to be 3201mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH to 7.0, stirring for 30min, standing, measuring the concentration of Ca ions in the supernatant to 316mg/L, calculating the separation rate of Ca ions to 90.13%, and according to the separation rate of calcium ions, knowing that the separation rate of actinium-227 in the wastewater is about 90%, and most of actinium-227 is separated.
Example 2
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to be 3201mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH to 8.0, stirring for 30min, standing, measuring the concentration of Ca ions in the supernatant to 14.5mg/L, calculating the separation rate of Ca ions to be 99.55%, and knowing that the separation rate of actinium-227 in the wastewater is close to 100% according to the separation rate of calcium ions, wherein the actinium-227 is almost completely separated.
Example 3
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to be 3201mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH value to 9.0, stirring for 30min, standing, measuring the concentration of Ca ions in the supernatant to 3.6mg/L, calculating the separation rate of Ca ions to 99.89%, and knowing that the separation rate of actinium-227 in the wastewater is close to 100% according to the separation rate of calcium ions, wherein the actinium-227 is almost completely separated.
Example 4
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to be 3201mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH to 10.0, stirring for 30min, standing, measuring the concentration of Ca ions in the supernatant to be 2.2mg/L, calculating the separation rate of Ca ions to be 99.93%, and knowing that the separation rate of actinium-227 in the wastewater is close to 100% according to the separation rate of calcium ions, wherein the actinium-227 is almost completely separated.
The final supernatants obtained in examples 1-4 were allowed to stand for 140 days, the total alpha and beta concentrations in the solutions were measured and the actual actinium-227 separation rate was reflected indirectly in the actual (total alpha + total beta) separation rate, the actinium-227 separation rate obtained was compared with the calcium ion separation rate, and the results were recorded in table 1. It can be seen that the actual actinium-227 separation rate is close to the Ca ion separation rate, and that Ca ion separation rate can be used to rapidly evaluate actinium-227 separation rate.
TABLE 1 comparison of actinium-227 separation results with calcium ion separation results in examples 1-4
Examples 1 2 3 4
Total alpha concentration (Bq/L) 20.1 4.7 0.81 0.5
Total beta concentration (Bq/L) 12.6 1.68 1.02 0.68
Actinium-227 isolation rate (%) 92.39 98.52 99.57 99.73
Ca ion separation Rate (%) 90.13 99.55 99.89 99.93
Comparative example 1
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration W 1 of the supernatant to 3201mg/L; filtering to separate filter residues, adding calcium ions and actinium-227 ions into the calcium oxide precipitation separation solution, adjusting the pH to 7.0, stirring for 30min, standing, and measuring the Ca concentration W 2 of the supernatant to 3210mg/L. In the process, the concentration W 1、W2 of the calcium reference ion basically does not change, the actual separation rate of actinium-227 is close to 80%, and the separation rate of the calcium ion cannot evaluate the separation rate of actinium-227 in the rare earth wastewater solution.
Comparative example 2
Adding sodium carbonate into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration W 1 of the supernatant; filtering to separate filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH to 7.0, stirring for 30min, standing, and measuring the concentration of Ca ions in the supernatant fluid to be W 2. The separation rate of the actual actinium-227 is more than 90%, and the separation rate of the actinium-227 in the rare earth wastewater solution cannot be evaluated.
Comparative example 3
Adding sodium carbonate into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration W 1 of the supernatant; after filtering and separating filter residues, adding calcium ions and actinium-227 ions in the calcium oxide precipitation separation solution, adjusting the pH to 10.0, stirring for 30min, standing, and measuring the concentration W 2 of Ca ions in the supernatant to 3258mg/L. In the process, the step of adding sodium carbonate does not introduce calcium reference ions W 1 very low, W 2 is far greater than W 1, the actual separation rate of actinium-227 is greater than 80%, and the separation rate of calcium ions can not evaluate the separation rate of actinium-227 in the rare earth wastewater solution.
After the actinium-227 rare earth-containing wastewater used in examples 5 to 8 and comparative examples 4 to 6 below was left for 140 days, the total alpha concentration was 30510 Bq/L and the total beta concentration was 6041Bq/L.
Example 5
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to 3282mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH to 7.0, stirring for 30min, standing, measuring the concentration of Ca ions in the supernatant to be 408mg/L, calculating the separation rate of Ca ions to be 87.57%, and according to the separation rate of calcium ions, knowing that the separation rate of actinium-227 in the wastewater is about 90%, and most of the actinium-227 is separated.
Example 6
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to 3282mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH value to 8.0, stirring for 30min, standing, measuring the Ca ion concentration of supernatant liquid to 38.1mg/L, calculating the Ca ion separation rate to be 98.84%, and knowing that the actinium-227 separation rate in the wastewater is close to 100% according to the Ca ion separation rate, wherein the actinium-227 is almost completely separated.
Example 7
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to 3282mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH value to 9.0, stirring for 30min, standing, measuring the concentration of Ca ions in the supernatant to 9.5mg/L, calculating the separation rate of Ca ions to be 99.71%, and knowing that the separation rate of actinium-227 in the wastewater is close to 100% according to the separation rate of calcium ions, wherein the actinium-227 is almost completely separated.
Example 8
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration of the supernatant to 3282mg/L; after filtering and separating filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH to 10.0, stirring for 30min, standing, measuring the concentration of Ca ions in the supernatant to 12.8mg/L, calculating the separation rate of Ca ions to be 99.61%, and knowing that the separation rate of actinium-227 in the wastewater is close to 100% according to the separation rate of calcium ions, wherein the actinium-227 is almost completely separated.
The final supernatants obtained in examples 5-8 were left for 140 days, the total alpha and beta concentrations in the solutions were measured and the actual actinium-227 separation rate was reflected indirectly as the actual (total alpha + total beta) separation rate, the actinium-227 separation rate obtained was compared with the calcium ion separation rate, and the results were recorded in table 2. It can be seen that the actual actinium-227 separation rate is close to the Ca ion separation rate, and that Ca ion separation rate can be used to rapidly evaluate actinium-227 separation rate.
TABLE 2 comparison of actinium-227 separation results with calcium ion separation results in examples 5-8
Examples 5 6 7 8
Total alpha concentration (Bq/L) 2245 651 210 159
Total beta concentration (Bq/L) 339 84.1 17.5 32.6
Actinium-227 isolation rate (%) 92.93 97.99 99.38 99.48
Ca ion separation Rate (%) 87.57 98.84 99.71 99.61
Comparative example 4
Adding calcium oxide into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration W 1 of the supernatant to 3282mg/L; filtering to separate filter residues, adding calcium ions and actinium-227 ions into the calcium oxide precipitation separation solution, adjusting the pH value to 7.0, stirring for 30min, standing, and measuring the concentration W 2 of Ca ions in the supernatant to 3285mg/L. In the process, the concentration W 1、W2 of the calcium reference ion basically does not change, the actual separation rate of actinium-227 is close to 80%, and the separation rate of the calcium ion cannot evaluate the separation rate of actinium-227 in the rare earth wastewater solution.
Comparative example 5
Adding sodium carbonate into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration W 1 of the supernatant; filtering to separate filter residues, adding sodium carbonate to precipitate and separate calcium ions and actinium-227 ions in the solution, adjusting the pH to 7.0, stirring for 30min, standing, and measuring the Ca ion concentration W 2 of the supernatant liquid. The separation rate of the actual actinium-227 is close to 90%, and the separation rate of the actinium-227 in the rare earth wastewater solution cannot be evaluated.
Comparative example 6
Adding sodium carbonate into the rare earth wastewater to adjust the pH to 6.0, stirring for 30min, standing, and measuring the Ca ion concentration W 1 of the supernatant; after filtering and separating filter residues, adding calcium ions and actinium-227 ions in the calcium oxide precipitation separation solution, adjusting the pH to 10.0, stirring for 30min, standing, and measuring the concentration W 2 of Ca ions in the supernatant to 3276mg/L. In the process, the step of adding sodium carbonate does not introduce calcium reference ions W 1 very low, W 2 is far greater than W 1, the actual separation rate of actinium-227 is greater than 80%, and the separation rate of calcium ions can not evaluate the separation rate of actinium-227 in the rare earth wastewater solution.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.

Claims (3)

1. A method for detecting the separation degree of actinium-227 in rare earth wastewater, which is characterized by comprising the following steps: adding calcium oxide or calcium hydroxide into the rare earth wastewater to adjust the pH value of the rare earth wastewater solution to 6.0, and measuring the concentration of calcium ions in the supernatant fluid and marking the concentration as W 1; filtering and separating filter residues, adding soluble carbonate into the rare earth wastewater solution with the pH value adjusted, precipitating and separating calcium ions and actinium-227 ions in the rare earth wastewater solution, adjusting the pH value of the rare earth wastewater solution to 7.0-10.0, measuring the concentration of calcium ions in supernatant fluid and marking the concentration as W 2, and calculating the separation rate of calcium ions in the rare earth wastewater solution as follows: w 1-W2/W1 is multiplied by 100 percent, and the separation rate of actinium-227 in the rare earth wastewater solution is evaluated by the separation rate of calcium ions.
2. The method for detecting the separation degree of actinium-227 in rare earth wastewater according to claim 1, wherein the rare earth wastewater is rare earth wastewater containing actinium-227, the total alpha concentration is 100-31000 Bq/L, and the total beta concentration is 100-6100 Bq/L.
3. The method for detecting the separation degree of actinium-227 in rare earth wastewater according to claim 1, wherein the soluble carbonate is sodium carbonate.
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