CN112961995A - Method for improving monazite concentrate alkali decomposition rate - Google Patents
Method for improving monazite concentrate alkali decomposition rate Download PDFInfo
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- CN112961995A CN112961995A CN202011400684.6A CN202011400684A CN112961995A CN 112961995 A CN112961995 A CN 112961995A CN 202011400684 A CN202011400684 A CN 202011400684A CN 112961995 A CN112961995 A CN 112961995A
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- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 96
- 239000003513 alkali Substances 0.000 title claims abstract description 95
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 title claims abstract description 52
- 229910052590 monazite Inorganic materials 0.000 title claims abstract description 52
- 239000012141 concentrate Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000002002 slurry Substances 0.000 claims abstract description 66
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 17
- 238000000926 separation method Methods 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 238000010790 dilution Methods 0.000 claims description 10
- 239000012895 dilution Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000001488 sodium phosphate Substances 0.000 claims description 8
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 8
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 8
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- -1 rare earth chloride Chemical class 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 39
- 239000000443 aerosol Substances 0.000 abstract description 8
- 230000002285 radioactive effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 abstract description 5
- 238000009835 boiling Methods 0.000 abstract description 4
- 230000036541 health Effects 0.000 abstract description 4
- 238000003723 Smelting Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 12
- 238000005265 energy consumption Methods 0.000 description 7
- 230000009467 reduction Effects 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 208000009043 Chemical Burns Diseases 0.000 description 1
- 208000018380 Chemical injury Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052585 phosphate mineral Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000012857 radioactive material Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of rare earth smelting production, and particularly relates to a method for improving the alkali decomposition rate of monazite concentrate. The ore pulp and concentrated alkali liquor obtained by grinding the monazite concentrate are put into a totally-enclosed alkali decomposition tank, the temperature of the alkali decomposition reaction is controlled to be 80-160 ℃, the pressure is controlled to be 0.01-0.5 MPa, the reaction time is 4-12 h, and the total alkalinity of the pulp is 15-25% when the alkali decomposition is complete. The ground qualified monazite concentrate ore pulp and a high-concentration sodium hydroxide solution are added into a fully-closed decomposition tank together for mixing, and the slight-pressure alkali decomposition reaction is carried out by utilizing the self reaction heat or external heating, so that the pollution to the environment and the harm to the human health caused by the reaction heat loss, aerosol and radioactive slurry are avoided, and the hot slurry splashed out during boiling is effectively prevented from scalding and chemically burning field operators.
Description
Technical Field
The invention belongs to the technical field of rare earth smelting production, and particularly relates to a method for improving the alkali decomposition rate of monazite concentrate. The method realizes the full-closed micropressure control of the decomposition process in the alkali decomposition reactor, and has the advantages of simple process, convenient operation, reliable operation, safety, environmental protection and high alkali decomposition rate.
Background
Monazite is an industrial rare earth phosphate mineral, and the content of rare earth oxides in monazite concentrate is generally REO: 50% -60%, and the monazite concentrate is generally treated by a caustic soda decomposition method in industry.
Industrially, the traditional monazite concentrate alkaline decomposition reactor is an open type decomposition tank, qualified monazite concentrate ore pulp after grinding is mixed with a high-concentration sodium hydroxide solution in the alkaline decomposition reactor, the reaction is carried out at a higher temperature, and rare earth phosphate is converted into rare earth hydroxide through the alkaline decomposition reaction, so that the purpose of separating rare earth from phosphorus is achieved. And obtaining clear liquid containing trisodium phosphate and an alkali cake through solid-liquid separation, and respectively using the clear liquid and the alkali cake for the production of the subsequent procedures.
The traditional open type alkali decomposition reaction tank has the following defects: the equipment is open, so that the harm to the health of operators and the environment caused by aerosol on an operation site and the risk factor that the splashed slurry can scald operators on the site exist; the heat preservation effect of the equipment is poor, the heat utilization rate is reduced, and the energy consumption is high.
The traditional alkali decomposition reactor has low heat utilization rate, generally realizes the decomposition efficiency as high as possible by a mode of improving the reaction temperature and prolonging the decomposition reaction time through external heating, and has the problems of high energy consumption of equipment, low heat utilization rate and low alkali decomposition rate (generally 96 percent).
The traditional alkali decomposition reactor is open equipment, a production device is not sealed, so that the leakage of materials and the burning (burning) of hot slurry splashed out during boiling hurt field operators, and simultaneously, the problems of the influence of aerosol and radioactive slurry on the field environment and the harm to human health exist.
Disclosure of Invention
The invention aims to provide a method for improving the alkali decomposition rate of monazite concentrate. The ground qualified monazite concentrate ore pulp and a high-concentration sodium hydroxide solution are added into a fully-closed decomposition tank together for mixing, and the slight-pressure alkali decomposition reaction is carried out by utilizing the self reaction heat or external heating, so that the pollution to the environment and the harm to the human health caused by the reaction heat loss, aerosol and radioactive slurry are avoided, and the hot slurry splashed out during boiling is effectively prevented from scalding and chemically burning field operators.
The invention can realize the micro-pressure alkali decomposition in a fully closed system, has simple process, convenient operation, stable and reliable operation, safety, environmental protection, high heat utilization efficiency, effective reduction of energy consumption and high alkali decomposition rate, and has greater advantages in the aspects of energy consumption reduction and alkali decomposition rate improvement compared with the traditional mode.
The invention can carry out the technical processes of dilution, aging and one-time washing of the slurry in a totally closed system, shortens the technical process, reduces the material transfer frequency, optimizes the operation mode and effectively avoids the pollution problem of radioactive materials and aerosol.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for improving the alkali decomposition rate of monazite concentrate comprises the steps of putting ore pulp and concentrated alkali liquor obtained by grinding the monazite concentrate into a fully-closed alkali decomposition tank, controlling the temperature of an alkali decomposition reaction to be 80-160 ℃, controlling the pressure to be 0.01-0.5 MPa, and controlling the reaction time to be 4-12 h, wherein the total alkalinity of the slurry is 15-25% when the alkali decomposition is completed.
REO in the monazite concentrate: 50 to 60 percent.
And (3) putting the ore pulp of minus 325 meshes and concentrated alkali liquor obtained by grinding the monazite concentrate into a fully-closed alkali decomposition tank.
Ore pulp obtained by grinding monazite concentrate and concentrated alkali liquor with the mass fraction of 50-60% are put into a totally-enclosed alkali decomposition tank.
The liquid-solid mass ratio of the concentrated alkali liquor to the monazite concentrate is 2: 1-8: 1.
The alkali decomposition rate reaches over 99.5 percent.
The alkali decomposition reaction process is a fully-closed micropressure control reaction, the heating mode is steam heating, and the parameter control of the material reaction temperature and pressure in the tank body is ensured by establishing a linkage relation between the measured temperature and a heating and pressure control system.
Adding hot water with the volume being one time of that of monazite concentrate into slurry with complete decomposition reaction for dilution, stirring for 0.5h, then closing the stirring, aging for 8-12 h, maintaining the temperature of the material to be higher than 80 ℃, siphoning supernatant, adding hot water with the volume being one time of that of the slurry with the volume being one time of that of the bottom slurry, carrying out multiple countercurrent washing on the bottom slurry, carrying out solid-liquid separation on the washed slurry, wherein a filter cake obtained by the solid-liquid separation is an alkali cake used for preparing a rare earth chloride product by preferential dissolution of hydrochloric acid, and combining primary washing water of the slurry with the aging solution for preparing a trisodium phosphate product.
And adding hot water with the quantity of the bottom slurry being one volume of the weight of the bottom slurry to carry out multiple times of countercurrent washing on the bottom slurry, wherein the washing water temperature is higher than 70 ℃, and carrying out solid-liquid separation on the washed slurry.
And carrying out solid-liquid separation on the washed slurry, and washing until the pH value is 7-8.
The beneficial effects obtained by the invention are as follows:
the alkali decomposition reaction process is carried out in a totally-enclosed decomposition tank, and the micro-pressure alkali decomposition reaction is carried out by utilizing self reaction heat or external heating, so that the environmental pollution and the human body harm caused by reaction heat loss, aerosol and radioactive slurry are avoided, and the hot slurry splashed out in the stirring process is effectively prevented from scalding and harming field operators who are chemically burned.
The technological process is carried out in a fully-closed reactor, and the processes of alkali decomposition, slurry dilution, aging, primary washing and the like are completed in a fully-closed system, so that the technological process is shortened, the material transfer frequency is reduced, the operation mode is optimized, and the pollution problem of radioactive slurry and aerosol is effectively avoided.
The method has the advantages of simple process, convenient operation, stable and reliable operation, safety, environmental protection, high heat utilization efficiency, effective reduction of energy consumption, high alkali decomposition rate and larger advantages in the aspects of energy consumption and alkali decomposition rate compared with the traditional mode.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The technical scheme of the invention is carried out according to the following steps:
firstly, ore pulp of-325 meshes and concentrated alkali liquor (NaOH: 50-60 mass percent) obtained by grinding monazite concentrate (REO: 50-60%) are put into a totally-closed alkali decomposition tank, and a stirring device, steam heating equipment and an automatic control system are started simultaneously. The liquid-solid mass ratio of the concentrated alkali liquor to the monazite concentrate is 2: 1-8: 1, the temperature of alkali decomposition reaction is controlled to be 80-160 ℃, the pressure is controlled to be 0.01-0.5 MPa, and the reaction time is 4-12 h. When the alkali decomposition is complete, the total alkalinity of the slurry is 15-25%, and the alkali decomposition rate is more than 99.5%.
The alkali decomposition reaction process is a fully-closed micropressure control reaction, the heating mode is steam heating, and the parameter control of the material reaction temperature and pressure in the tank body is ensured by establishing a linkage relation between the measured temperature and a heating and pressure control system.
Adding hot water with the volume being one time of that of monazite concentrate into slurry with complete decomposition reaction for dilution, stirring for 0.5h, then closing the stirring, aging for 8-12 h, maintaining the temperature of the material to be higher than 80 ℃, siphoning supernatant, adding hot water with the volume being one time of that of the slurry with the volume being one time of that of the bottom slurry into the slurry, carrying out multiple countercurrent washing on the bottom slurry, wherein the washing water temperature is higher than 70 ℃, feeding the washed slurry into a solid-liquid separation system at the rear section, washing until the pH value is 7-8, and obtaining a filter cake by solid-liquid separation, namely an alkali cake which is used for preparing rare earth chloride products by preferential dissolution of hydrochloric. The first wash of the slurry is combined with the aging solution for the preparation of the trisodium phosphate product.
[ example 1 ]
1t of monazite concentrate (REO: 56.24%) is ground to obtain-325-mesh slurry, the slurry is added into a fully-closed alkali decomposition tank, 2.8t of concentrated alkali liquor (NaOH: 54.2%) is added, and a stirring device, steam heating equipment and an automatic control system are started. The reaction temperature is gradually increased from 83 ℃ to 148 ℃, the pressure is controlled to be not more than 0.05MPa, and the reaction time is 10.0 h. The decomposition reaction was complete and the heating system was turned off. Adding hot water with the weight of 4t of monazite concentrate into the slurry for dilution, continuously stirring for 0.5h, closing stirring, keeping the temperature of the material at more than 80 ℃, aging for 12h, siphoning supernatant, adding a certain amount of hot water with the volume being twice as large as that of the bottom slurry according to the amount of the bottom slurry to carry out multiple countercurrent washing on the bottom slurry, wherein the washing water temperature is more than 70 ℃, feeding the washed slurry into a solid-liquid separation system at the rear section, washing until the pH value is 7-8, and obtaining a filter cake through solid-liquid separation, namely an alkali cake.
Sampling, sending to analyze and detect the total alkalinity and the alkali decomposition rate in the slurry with complete alkali decomposition reaction, wherein the total alkalinity is as follows: 17.9 percent and the alkali decomposition rate is 99.67 percent.
[ example 2 ]
1t of monazite concentrate (REO: 51.86%) is ground to obtain-325-mesh slurry, the slurry is added into a totally-closed alkali decomposition tank, 3.1t of concentrated alkali liquor (NaOH: 52.9%) is added, and a stirring device, steam heating equipment and an automatic control system are started. The reaction temperature is gradually increased from 81 ℃ to 145 ℃, the pressure is controlled to be not more than 0.05MPa, and the reaction time is 9.5 h. The decomposition reaction was complete and the heating system was turned off. The specific operation modes of adding water to the slurry for dilution, aging, siphoning supernatant, multiple countercurrent washing, filtering and the like are the same as in example 1.
Sampling, sending to analyze and detect the total alkalinity and the alkali decomposition rate in the slurry with complete alkali decomposition reaction, wherein the total alkalinity is as follows: 19.5% and an alkali decomposition rate of 99.79%.
[ example 3 ]
1t of monazite concentrate (REO: 54.12%) is ground to obtain-325-mesh slurry, the slurry is added into a fully-closed alkali decomposition tank, 2.9t of concentrated alkali liquor (NaOH: 51.7%) is added, and a stirring device, steam heating equipment and an automatic control system are started. The reaction temperature is gradually increased from 82 ℃ to 155 ℃, the pressure is controlled to be not more than 0.05MPa, and the reaction time is 11.5 h. The decomposition reaction was complete and the heating system was turned off. The specific operation modes of adding water to the slurry for dilution, aging, siphoning supernatant, multiple countercurrent washing, filtering and the like are the same as in example 1.
Sampling, sending to analyze and detect the total alkalinity and the alkali decomposition rate in the slurry with complete alkali decomposition reaction, wherein the total alkalinity is as follows: 17.5 percent and the alkali decomposition rate is 99.61 percent.
The invention relates to a novel method for improving the alkali decomposition rate of monazite concentrate, and belongs to the technical field of rare earth hydrometallurgy. The alkali decomposition process is to add the grinded monazite ore concentrate pulp and high-concentration sodium hydroxide solution into a fully closed reactor to carry out micro-pressure alkali decomposition reaction. Compared with the traditional mode, the process comprises the steps of placing reaction materials in a fully-closed system, and carrying out alkali decomposition reaction by utilizing self reaction heat or external heating under the condition of micro pressure, so that the heat loss of reaction, environmental pollution or human body harm caused by aerosol and radioactive slurry are avoided, and hot slurry splashed out in the boiling process is effectively prevented from scalding field operators and chemical burn operators; compared with the traditional mode, the method has the advantages of convenient operation and stable and reliable operation; safe and environment-friendly, high heat utilization efficiency, effective reduction of energy consumption and high alkali decomposition rate.
A new technology for improving the alkali decomposition rate of monazite concentrate comprises the following steps: firstly, adding a certain amount of grinded qualified monazite concentrate pulp and a certain amount of high-concentration sodium hydroxide solution into a fully-closed alkali decomposition reaction tank, starting a steam heating device, a stirring device and an automatic control system, and starting reaction under the conditions of set liquid-solid ratio, temperature and pressure. After the reaction is finished, the slurry is subjected to the processes of hot water dilution, aging, clear liquid siphoning, multi-stage countercurrent washing, filtering and the like to obtain clear liquid of trisodium phosphate and alkali cake, and the clear liquid and the alkali cake are applied to the production process of the post-procedure.
The qualified monazite concentrate ore pulp after grinding has the content of rare earth oxide as REO: 50 to 60 percent and the granularity is that the particle passes through-325 meshes. The high-concentration sodium hydroxide solution is NaOH: 50-60 percent of the composition can be prepared and used immediately. And adding the grinded qualified monazite concentrate ore pulp and a high-concentration sodium hydroxide solution into a fully-closed alkali decomposition tank, wherein the liquid-solid ratio of the concentrated alkali liquor to the monazite concentrate is 2: 1-8: 1. Meanwhile, the heating equipment, the stirring device and the automatic control system are started, the heating mode adopts steam jacket heating, the temperature is controlled to be 80-160 ℃, the pressure is controlled to be 0.01-0.5 MPa, and the reaction time is 4-12 h. And after the monazite concentrate alkali decomposition reaction is completed, closing the heating temperature control system. Adding hot water with the volume which is one time of the weight of the monazite concentrate into the slurry with complete alkali decomposition reaction for dilution, stirring for 0.5h, then closing the stirring, aging for about 8-12 h, keeping the temperature of the material to be higher than 80 ℃, and siphoning the supernatant. And adding hot water with the volume being one time of the total weight of the bottom slurry into the tank to carry out multiple times of countercurrent washing on the bottom slurry, wherein the washing water temperature is higher than 70 ℃, washing until the pH value is 7-8, and feeding the washed slurry into a solid-liquid separation system at the rear section to respectively obtain trisodium phosphate clear liquid and alkali cake. The alkali decomposition reaction process is micro-pressure control in a fully-closed reactor, and the controllable parameters of the material reaction temperature, pressure and the like in the tank body are ensured by establishing a linkage relation between the measured temperature and a heating and pressure control system. When the alkali decomposition is complete, the total alkalinity is 15% -25%, and the alkali decomposition rate is more than 99.5%. The obtained trisodium phosphate clear solution is used for preparing trisodium phosphate by-products, and the obtained alkali cake is dissolved by hydrochloric acid to prepare mixed rare earth chloride products.
Claims (10)
1. A method for improving the alkali decomposition rate of monazite concentrate is characterized by comprising the following steps: the ore pulp and concentrated alkali liquor obtained by grinding the monazite concentrate are put into a totally-enclosed alkali decomposition tank, the temperature of the alkali decomposition reaction is controlled to be 80-160 ℃, the pressure is controlled to be 0.01-0.5 MPa, the reaction time is 4-12 h, and the total alkalinity of the pulp is 15-25% when the alkali decomposition is complete.
2. The method for increasing the rate of alkaline decomposition of monazite concentrate according to claim 1, wherein: REO in the monazite concentrate: 50 to 60 percent.
3. The method for increasing the rate of alkaline decomposition of monazite concentrate according to claim 1, wherein: and (3) putting the ore pulp of minus 325 meshes and concentrated alkali liquor obtained by grinding the monazite concentrate into a fully-closed alkali decomposition tank.
4. The method for increasing the rate of alkaline decomposition of monazite concentrate according to claim 1, wherein: ore pulp obtained by grinding monazite concentrate and concentrated alkali liquor with the mass fraction of 50-60% are put into a totally-enclosed alkali decomposition tank.
5. The method for increasing the rate of alkaline decomposition of monazite concentrate according to claim 1, wherein: the liquid-solid mass ratio of the concentrated alkali liquor to the monazite concentrate is 2: 1-8: 1.
6. The method for increasing the rate of alkaline decomposition of monazite concentrate according to claim 1, wherein: the alkali decomposition rate reaches over 99.5 percent.
7. The method for increasing the rate of alkaline decomposition of monazite concentrate according to claim 1, wherein: the alkali decomposition reaction process is a fully-closed micropressure control reaction, the heating mode is steam heating, and the parameter control of the material reaction temperature and pressure in the tank body is ensured by establishing a linkage relation between the measured temperature and a heating and pressure control system.
8. The method for increasing the rate of alkaline decomposition of monazite concentrate according to claim 1, wherein: adding hot water with the volume being one time of that of monazite concentrate into slurry with complete decomposition reaction for dilution, stirring for 0.5h, then closing the stirring, aging for 8-12 h, maintaining the temperature of the material to be higher than 80 ℃, siphoning supernatant, adding hot water with the volume being one time of that of the slurry with the volume being one time of that of the bottom slurry, carrying out multiple countercurrent washing on the bottom slurry, carrying out solid-liquid separation on the washed slurry, wherein a filter cake obtained by the solid-liquid separation is an alkali cake used for preparing a rare earth chloride product by preferential dissolution of hydrochloric acid, and combining primary washing water of the slurry with the aging solution for preparing a trisodium phosphate product.
9. The method of increasing the rate of alkaline decomposition of monazite concentrate according to claim 8, wherein: and adding hot water with the quantity of the bottom slurry being one volume of the weight of the bottom slurry to carry out multiple times of countercurrent washing on the bottom slurry, wherein the washing water temperature is higher than 70 ℃, and carrying out solid-liquid separation on the washed slurry.
10. The method of increasing the rate of alkaline decomposition of monazite concentrate according to claim 8, wherein: and carrying out solid-liquid separation on the washed slurry, and washing until the pH value is 7-8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115591676A (en) * | 2022-10-31 | 2023-01-13 | 湖南中核金原新材料有限责任公司（Cn） | Method for removing organic agents on surface of monazite flotation concentrate by thermally activating persulfate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS579890A (en) * | 1980-06-20 | 1982-01-19 | Inoue Japax Res Inc | Treatment of rare earth concentrate |
| CN106148692A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | A kind of alkaline process decomposes technique and the equipment thereof of mengite rare-earth mine |
| CN106145176A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | The technique that a kind of alkaline process processes monazite |
| CN106148687A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | The Apparatus and method for that a kind of Rare Earth Mine alkaline process decomposes |
| CN111020242A (en) * | 2019-09-09 | 2020-04-17 | 湖南中核金原新材料有限责任公司 | Process method for smelting and separating uranium, thorium and rare earth from monazite concentrate |
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2020
- 2020-12-02 CN CN202011400684.6A patent/CN112961995A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS579890A (en) * | 1980-06-20 | 1982-01-19 | Inoue Japax Res Inc | Treatment of rare earth concentrate |
| CN106148692A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | A kind of alkaline process decomposes technique and the equipment thereof of mengite rare-earth mine |
| CN106145176A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | The technique that a kind of alkaline process processes monazite |
| CN106148687A (en) * | 2015-04-21 | 2016-11-23 | 永州市湘江稀土有限责任公司 | The Apparatus and method for that a kind of Rare Earth Mine alkaline process decomposes |
| CN111020242A (en) * | 2019-09-09 | 2020-04-17 | 湖南中核金原新材料有限责任公司 | Process method for smelting and separating uranium, thorium and rare earth from monazite concentrate |
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| CN115591676A (en) * | 2022-10-31 | 2023-01-13 | 湖南中核金原新材料有限责任公司（Cn） | Method for removing organic agents on surface of monazite flotation concentrate by thermally activating persulfate |
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