CN111575485A - Recovery processing method for reducing radioactivity of rare earth slag - Google Patents
Recovery processing method for reducing radioactivity of rare earth slag Download PDFInfo
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- CN111575485A CN111575485A CN202010386545.6A CN202010386545A CN111575485A CN 111575485 A CN111575485 A CN 111575485A CN 202010386545 A CN202010386545 A CN 202010386545A CN 111575485 A CN111575485 A CN 111575485A
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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
- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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
- 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
- C22B60/0234—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors sulfurated 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
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/0278—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries by chemical methods
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- 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 discloses a recovery processing method for reducing the radioactivity of rare earth slag, which belongs to the technical field of chemical production and comprises the following steps: primary leaching reaction: adding rare earth slag into a clean reaction tank, introducing recovery liquid of secondary leaching reaction, carrying out solid-liquid separation on reaction liquid under certain conditions, collecting filtrate A and filter residue A, adding the filtrate A into a blending tank, adding raw lime slurry, adjusting the pH value of the filtrate A, stabilizing for a period of time, continuously carrying out solid-liquid separation on the filtrate A, collecting filtrate B and filter residue B, introducing the filtrate B into an oxalic acid precipitation tank, adding oxalic acid for precipitation, introducing into a plate-and-frame filter after the precipitation is finished, and collecting the obtained filter residue, namely a rare earth oxalate product.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a recovery processing method for reducing radioactivity of rare earth slag.
Background
Monazite is a phosphate mineral of rare earth and thorium, and is an important raw material with industrial value for preparing cerium and light rare earth. Due to good sorting property, the grade of rare earth is about 60%, and the content of thorium is generally 5-7%. In addition, monazite concentrates often have small amounts of other minerals such as ilmenite (FeTiO 3), zirconite (ZrSiO 3), rutile (TiO 2), and quartzite (SiO 2). The monazite is a mineral mainly containing light rare earth, but has higher content of medium and heavy rare earth than mixed light rare earth concentrate, whether the monazite has a mineral with comprehensive utilization value or not, and elements such as thorium, uranium, phosphorus and the like except the rare earth should be comprehensively recovered
The mixed rare earth chloride concentrate is prepared by taking monazite concentrate as a raw material, firstly obtaining a mixture of hydroxides of rare earth and thorium and trisodium phosphate by adopting an alkaline process, then dissolving the mixture of hydroxides of rare earth and thorium by hydrochloric acid, adjusting the pH value to 3.5-4.5 to ensure that most of rare earth is preferentially dissolved out and thorium, uranium, iron and the like are rarely dissolved, so that most of rare earth is separated from radioactive elements of thorium, uranium and other impurities, a small amount of rare earth, uranium and thorium exist in an insoluble form and are called as radioactive acid dissolving slag, and finally removing impurities from rare earth leachate, filtering, concentrating and crystallizing to obtain the mixed rare earth chloride concentrate. The radioactive acid dissolving slag left after rare earth is extracted from monazite concentrate through alkaline decomposition also contains valuable resources such as REO, ThO2, U3O8 and undecomposed zirconite, monazite and the like, and ThO2 in a sample is determined through sampling and analyzing the radioactive acid dissolving slag (dry slag); 15.72% U3O 8; 2.72% REO; 7.64 percent
Calculated by 1750 tons of radioactive acid dissolving slag (dry slag) produced every year, the slag contains 133.7 tons of REO, 275.10 tons of ThO2 and 47.6 tons of U3O8, and it can be seen that the slag contains a large amount of useful elements such as rare earth, thorium, uranium and the like, and the uranium and the thorium are radioactive elements and pollute the surrounding environment, so that a process method needs to be developed as soon as possible to realize optimization and green treatment of resources.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a recycling method for reducing the radioactivity of rare earth slag, which can reduce the radioactivity of the rare earth slag, enrich uranium and thorium elements, and recycle rare earth elements in the rare earth slag, thereby realizing the optimization of resources and green and environment-friendly treatment.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A recovery processing method for reducing the radioactivity of rare earth slag comprises the following steps:
s1, primary leaching reaction: adding the rare earth slag into a clean reaction tank, introducing the recovery liquid of the secondary leaching reaction, and reacting under certain conditions to obtain reaction liquid A;
s2, introducing the reaction solution A into a plate and frame filter for solid-liquid separation, and collecting filtrate A and filter residue A;
s3, adding the filtrate A into a blending tank, adding the raw lime slurry, adjusting the pH value of the filtrate A, stabilizing for a period of time, introducing the filtrate A into a plate-and-frame filter to continuously perform solid-liquid separation, and collecting filtrate B and filter residue B;
and S4, introducing the filtrate B into an oxalic acid precipitation tank, adding oxalic acid for precipitation, introducing into a plate and frame filter after precipitation is finished, and collecting the obtained filter residue, namely the rare earth oxalate product.
Furthermore, in the S1, the mass ratio of the rare earth slag to the recovery liquid of the secondary leaching reaction is 1: 4-6.
Further, in the S1, the reaction condition is 70-90 ℃, and the reaction time is 3-5 h.
Further, in S1, the secondary leaching reaction process includes the following steps:
s11, collecting the filter residue A obtained in the S2 as secondary residue, and drying and crushing the secondary residue to obtain secondary dry residue;
s12, transferring the secondary dry slag into a clean reaction tank, adding concentrated sulfuric acid, and reacting under certain conditions to obtain reaction liquid B;
s13, introducing the reaction solution B into a plate-and-frame filter for solid-liquid separation, collecting filtrate C and filter residue C, wherein the collected filtrate C is the recovery solution of the secondary leaching reaction in S1;
s14, placing the filter residue C into a residue washing tank, adding clear water for washing, adding the filter residue C into a plate-and-frame filter for solid-liquid separation after washing, and collecting the obtained filter residue, namely the radioactivity-removed residue.
Further, in the step S12, the mass ratio of the secondary dry slag to the concentrated sulfuric acid is 1.25-1.5: 1.
further, in the S12, the reaction condition is 100-110 ℃, and the reaction time is 1.5-2.5 h.
Further, in the step S3, the stabilization time is 0.4-0.6 h.
In step S3, the obtained residue B is uranium thorium residue, and is used to extract uranium, thorium, and rare earth elements.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) after the rare earth slag is treated by the treatment method, the radioactivity of the rare earth slag is greatly reduced, and the 232Th radioactivity =90.3Bq/g in the rare earth slag meets the requirement range of the I-type rare earth associated radioactive solid waste: 1Bq/g < activity concentration of uranium (thorium) single nuclide is less than or equal to 400Bq/g, and the standard of landfill is achieved.
(2) The treatment method can recover rare earth from rare earth slag, the total recovery rate of the rare earth reaches 3 percent, and uranium and thorium are enriched by hydroxide, wherein the total recovery rate of the rare earth is 70 percent, the uranium and thorium contain ThO232.85 percent and U3O85.50 percent, and the method can be used for separating and extracting thorium and uranium raw materials in the next step.
(3) The method can reduce the radioactivity of the rare earth slag, enrich uranium and thorium elements, and recycle the rare earth elements in the rare earth slag, thereby realizing the optimization of resources and the green and environment-friendly treatment.
Drawings
FIG. 1 is a process flow diagram of the treatment process of the present invention;
FIG. 2 is a flow chart of a method of the present invention;
FIG. 3 is a flow chart of a process for the secondary leaching reaction of the present invention.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; but not all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
Example 1:
a recovery processing method for reducing the radioactivity of rare earth slag comprises the following steps:
s1, primary leaching reaction: adding the rare earth slag into a clean reaction tank, introducing a recovery liquid of secondary leaching reaction, wherein the mass ratio of the rare earth slag to the recovery liquid of the secondary leaching reaction is 1:4, and reacting for 3 hours at 70 ℃ to obtain a reaction liquid A;
s2, introducing the reaction solution A into a plate and frame filter for solid-liquid separation, and collecting filtrate A and filter residue A;
s3, adding the filtrate A into a blending tank, adding the raw lime slurry, adjusting the pH value of the filtrate A, stabilizing for 0.4h, introducing the filtrate A into a plate-and-frame filter for continuous solid-liquid separation, collecting filtrate B and residue B, wherein the residue B is uranium thorium residue and can be used for extracting elements such as uranium, thorium, rare earth and the like;
and S4, introducing the filtrate B into an oxalic acid precipitation tank, adding oxalic acid for precipitation, introducing into a plate and frame filter after precipitation is finished, and collecting the obtained filter residue, namely the rare earth oxalate product.
Wherein, the secondary leaching reaction process comprises the following steps:
s11, collecting the filter residue A obtained in the S2 as secondary residue, and drying and crushing the secondary residue to obtain secondary dry residue;
s12, transferring the secondary dry slag into a clean reaction tank, and adding concentrated sulfuric acid, wherein the mass ratio of the secondary dry slag to the concentrated sulfuric acid is 1.25: reacting for 1.5h at the temperature of 1,100 ℃ to obtain reaction liquid B;
s13, introducing the reaction solution B into a plate-and-frame filter for solid-liquid separation, collecting filtrate C and filter residue C, wherein the collected filtrate C is the recovery solution of the secondary leaching reaction in S1;
s14, placing the filter residue C into a residue washing tank, adding clear water for washing, adding the filter residue C into a plate-and-frame filter for solid-liquid separation after washing, and collecting the obtained filter residue, namely the radioactivity-removed residue.
Example 2:
a recovery processing method for reducing the radioactivity of rare earth slag comprises the following steps:
s1, primary leaching reaction: adding the rare earth slag into a clean reaction tank, introducing a recovery liquid of secondary leaching reaction, wherein the mass ratio of the rare earth slag to the recovery liquid of the secondary leaching reaction is 1:5, and reacting for 4 hours at 80 ℃ to obtain a reaction liquid A;
s2, introducing the reaction solution A into a plate and frame filter for solid-liquid separation, and collecting filtrate A and filter residue A;
s3, adding the filtrate A into a blending tank, adding the raw lime slurry, adjusting the pH value of the filtrate A, stabilizing for 0.5h, introducing the filtrate A into a plate-and-frame filter for continuous solid-liquid separation, collecting filtrate B and residue B, wherein the residue B is uranium thorium residue and can be used for extracting elements such as uranium, thorium, rare earth and the like;
and S4, introducing the filtrate B into an oxalic acid precipitation tank, adding oxalic acid for precipitation, introducing into a plate and frame filter after precipitation is finished, and collecting the obtained filter residue, namely the rare earth oxalate product.
Wherein, the secondary leaching reaction process comprises the following steps:
s11, collecting the filter residue A obtained in the S2 as secondary residue, and drying and crushing the secondary residue to obtain secondary dry residue;
s12, transferring the secondary dry slag into a clean reaction tank, and adding concentrated sulfuric acid, wherein the mass ratio of the secondary dry slag to the concentrated sulfuric acid is 1.4: reacting for 2 hours at the temperature of 1,105 ℃ to obtain reaction liquid B;
s13, introducing the reaction solution B into a plate-and-frame filter for solid-liquid separation, collecting filtrate C and filter residue C, wherein the collected filtrate C is the recovery solution of the secondary leaching reaction in S1;
s14, placing the filter residue C into a residue washing tank, adding clear water for washing, adding the filter residue C into a plate-and-frame filter for solid-liquid separation after washing, and collecting the obtained filter residue, namely the radioactivity-removed residue.
Example 3:
a recovery processing method for reducing the radioactivity of rare earth slag comprises the following steps:
s1, primary leaching reaction: adding the rare earth slag into a clean reaction tank, introducing a recovery liquid of secondary leaching reaction, wherein the mass ratio of the rare earth slag to the recovery liquid of the secondary leaching reaction is 1:6, and reacting for 5 hours at 90 ℃ to obtain a reaction liquid A;
s2, introducing the reaction solution A into a plate and frame filter for solid-liquid separation, and collecting filtrate A and filter residue A;
s3, adding the filtrate A into a blending tank, adding the raw lime slurry, adjusting the pH value of the filtrate A, stabilizing for 0.6h, introducing the filtrate A into a plate-and-frame filter for continuous solid-liquid separation, collecting filtrate B and residue B, wherein the residue B is uranium thorium residue and can be used for extracting elements such as uranium, thorium, rare earth and the like;
and S4, introducing the filtrate B into an oxalic acid precipitation tank, adding oxalic acid for precipitation, introducing into a plate and frame filter after precipitation is finished, and collecting the obtained filter residue, namely the rare earth oxalate product.
Wherein, the secondary leaching reaction process comprises the following steps:
s11, collecting the filter residue A obtained in the S2 as secondary residue, and drying and crushing the secondary residue to obtain secondary dry residue;
s12, transferring the secondary dry slag into a clean reaction tank, and adding concentrated sulfuric acid, wherein the mass ratio of the secondary dry slag to the concentrated sulfuric acid is 1.5: reacting for 2.5h at the temperature of 1,110 ℃ to obtain reaction liquid B;
s13, introducing the reaction solution B into a plate-and-frame filter for solid-liquid separation, collecting filtrate C and filter residue C, wherein the collected filtrate C is the recovery solution of the secondary leaching reaction in S1;
s14, placing the filter residue C into a residue washing tank, adding clear water for washing, adding the filter residue C into a plate-and-frame filter for solid-liquid separation after washing, and collecting the obtained filter residue, namely the radioactivity-removed residue.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto; any person skilled in the art is within the technical scope of the present disclosure; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.
Claims (8)
1. A recovery processing method for reducing the radioactivity of rare earth slag is characterized by comprising the following steps: the method comprises the following steps:
s1, primary leaching reaction: adding the rare earth slag into a clean reaction tank, introducing the recovery liquid of the secondary leaching reaction, and reacting under certain conditions to obtain reaction liquid A;
s2, introducing the reaction solution A into a plate and frame filter for solid-liquid separation, and collecting filtrate A and filter residue A;
s3, adding the filtrate A into a blending tank, adding the raw lime slurry, adjusting the pH value of the filtrate A, stabilizing for a period of time, introducing the filtrate A into a plate-and-frame filter to continuously perform solid-liquid separation, and collecting filtrate B and filter residue B;
and S4, introducing the filtrate B into an oxalic acid precipitation tank, adding oxalic acid for precipitation, introducing into a plate and frame filter after precipitation is finished, and collecting the obtained filter residue, namely the rare earth oxalate product.
2. A recovery processing method for reducing the radioactivity of rare earth residues according to claim 1, wherein: in the S1, the mass ratio of the rare earth slag to the recovery liquid of the secondary leaching reaction is 1: 4-6.
3. A recovery processing method for reducing the radioactivity of rare earth residues according to claim 1, wherein: in the S1, the reaction condition is 70-90 ℃ and the reaction time is 3-5 h.
4. A recovery processing method for reducing the radioactivity of rare earth residues according to claim 1, wherein: in the S1, the secondary leaching reaction process comprises the following steps:
s11, collecting the filter residue A obtained in the S2 as secondary residue, and drying and crushing the secondary residue to obtain secondary dry residue;
s12, transferring the secondary dry slag into a clean reaction tank, adding concentrated sulfuric acid, and reacting under certain conditions to obtain reaction liquid B;
s13, introducing the reaction solution B into a plate-and-frame filter for solid-liquid separation, collecting filtrate C and filter residue C, wherein the collected filtrate C is the recovery solution of the secondary leaching reaction in S1;
s14, placing the filter residue C into a residue washing tank, adding clear water for washing, adding the filter residue C into a plate-and-frame filter for solid-liquid separation after washing, and collecting the obtained filter residue, namely the radioactivity-removed residue.
5. A recycling process to reduce the radioactivity of rare earth residues according to claim 4, wherein: in the S12, the mass ratio of the secondary dry slag to the concentrated sulfuric acid is 1.25-1.5: 1.
6. a recycling process to reduce the radioactivity of rare earth residues according to claim 4, wherein: in the S12, the reaction condition is 100-110 ℃, and the reaction time is 1.5-2.5 h.
7. A recovery processing method for reducing the radioactivity of rare earth residues according to claim 1, wherein: in the S3, the stabilizing time is 0.4-0.6 h.
8. A recovery processing method for reducing the radioactivity of rare earth residues according to claim 1, wherein: and in the S3, the obtained filter residue B is uranium thorium residue and is used for extracting uranium, thorium and rare earth elements.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114107661A (en) * | 2021-11-30 | 2022-03-01 | 湖南中核金原新材料有限责任公司 | Method for improving filtering performance of monazite high-quality slag |
| CN114645137A (en) * | 2022-03-17 | 2022-06-21 | 四川省冕宁县方兴稀土有限公司 | Method for resource utilization of iron-thorium waste residues |
| CN114645137B (en) * | 2022-03-17 | 2024-05-31 | 四川省冕宁县方兴稀土有限公司 | Method for recycling iron thorium waste residues |
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| CN110357300A (en) * | 2019-07-16 | 2019-10-22 | 湛江市红日稀土有限公司 | A method of reducing Phosphorus From Wastewater content, COD content |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114107661A (en) * | 2021-11-30 | 2022-03-01 | 湖南中核金原新材料有限责任公司 | Method for improving filtering performance of monazite high-quality slag |
| CN114107661B (en) * | 2021-11-30 | 2022-08-12 | 湖南中核金原新材料有限责任公司 | Method for improving filtering performance of monazite high-quality slag |
| CN114645137A (en) * | 2022-03-17 | 2022-06-21 | 四川省冕宁县方兴稀土有限公司 | Method for resource utilization of iron-thorium waste residues |
| CN114645137B (en) * | 2022-03-17 | 2024-05-31 | 四川省冕宁县方兴稀土有限公司 | Method for recycling iron thorium waste residues |
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