CN112143917A - Method for destroying oxalic acid in evaporation and concentration of plutonium oxalate precipitation mother liquor in Purex process - Google Patents

Method for destroying oxalic acid in evaporation and concentration of plutonium oxalate precipitation mother liquor in Purex process Download PDF

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Publication number
CN112143917A
CN112143917A CN202010830586.XA CN202010830586A CN112143917A CN 112143917 A CN112143917 A CN 112143917A CN 202010830586 A CN202010830586 A CN 202010830586A CN 112143917 A CN112143917 A CN 112143917A
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mother liquor
oxalate precipitation
evaporation
concentration
plutonium oxalate
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刘金平
何辉
唐洪彬
李斌
刘占元
李峰峰
申震
李高亮
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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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
    • 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
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C19/00—Arrangements for treating, for handling, or for facilitating the handling of, fuel or other materials which are used within the reactor, e.g. within its pressure vessel
    • G21C19/42—Reprocessing of irradiated fuel
    • G21C19/44—Reprocessing of irradiated fuel of irradiated solid fuel
    • G21C19/48—Non-aqueous processes
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors
    • 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
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
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  • Environmental & Geological Engineering (AREA)
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  • High Energy & Nuclear Physics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention belongs to the technical field of spent fuel post-treatment, and relates to a method for destroying oxalic acid in evaporation and concentration of plutonium oxalate precipitation mother liquor in a Purex process. The destruction method sequentially comprises the following steps: (1) adding part of plutonium oxalate precipitation mother liquor to be evaporated and concentrated and Mn in an evaporation and concentration container2+The solution of (1) is heated to boiling after being uniformly mixed, and evaporation concentration is started; (2) adding the rest plutonium oxalate precipitation mother liquor to be evaporated and concentrated into the evaporation and concentration container under continuous heating, and controlling the addition rate and the heating power to ensure that the evaporation rate of the plutonium oxalate precipitation mother liquor is 0.8-1.2 times of the addition rate of the plutonium oxalate precipitation mother liquor; (3) after the addition of the rest mother liquor of plutonium oxalate precipitation to be evaporated and concentrated is finished, the mother liquor is continuously heated for a certain time to continuously destroy the residual oxalic acid in the concentrated liquor. Benefit toThe method can better destroy oxalic acid in the mother liquor of plutonium oxalate precipitation in the process of evaporation and concentration.

Description

Method for destroying oxalic acid in evaporation and concentration of plutonium oxalate precipitation mother liquor in Purex process
Technical Field
The invention belongs to the technical field of spent fuel post-treatment, and relates to a method for destroying oxalic acid in evaporation and concentration of plutonium oxalate precipitation mother liquor in a Purex process.
Background
In the process of post-processing Purex of spent fuel, oxalic acid is mainly used for precipitating plutonium nitrate to obtain a plutonium product. The mother liquor of plutonium oxalate precipitation after oxalic acid precipitation contains about 2.5mol/L HNO30.1mol/L oxalic acid, 0.1g/L plutonium and 0.02g/L uranium. In the existing spent fuel post-treatment plant in China, the plutonium oxalate precipitation mother liquor is directly returned to the 2AF seasoning process section without evaporation and concentration. Because the concentration of plutonium in the mother liquor of plutonium oxalate precipitation is low, 2BP needs to be returned in large quantity in order to ensure that the concentration of 2AF plutonium reaches more than 6g/L, so that plutonium circulates in a large quantity in a plutonium purification cycle process section, the capacity is reduced, and the waste amount is increased. In order to optimize the process, the reflux ratio of 2BP is reduced, the volume of waste is reduced, the mother liquor of plutonium oxalate precipitation needs to be evaporated and concentrated, and the concentrated solution returns to the 2AF seasoning process section. To prevent the precipitation of plutonium again during the evaporative concentration of the mother liquor of plutonium oxalate precipitation and to reduce the amount of oxalic acid returned to 2AF, 99.9% of the oxalic acid was destroyed during the concentration of the mother liquor of plutonium oxalate precipitation.
At present, at home and abroad, only the technology for destroying oxalic acid in the plutonium oxalate precipitation mother liquor under the non-evaporative concentration condition exists, so that the technology for destroying oxalic acid in the process of evaporative concentration of the plutonium oxalate precipitation mother liquor needs to be developed.
Disclosure of Invention
The invention aims to provide a method for destroying oxalic acid in the evaporation and concentration of plutonium oxalate precipitation mother liquor in a Purex process, so that the oxalic acid in the plutonium oxalate precipitation mother liquor can be better destroyed in the evaporation and concentration process.
In order to achieve the purpose, in a basic embodiment, the invention provides a method for destroying oxalic acid in the evaporation and concentration of plutonium oxalate precipitation mother liquor in a Purex process, which sequentially comprises the following steps:
(1) adding part of plutonium oxalate precipitation mother liquor to be evaporated and concentrated and Mn in an evaporation and concentration container2+The solution of (1) is heated to boiling after being uniformly mixed, and evaporation concentration is started;
(2) adding the rest plutonium oxalate precipitation mother liquor to be evaporated and concentrated into the evaporation and concentration container under continuous heating, and controlling the addition rate and the heating power to ensure that the evaporation rate of the plutonium oxalate precipitation mother liquor is 0.8-1.2 times of the addition rate of the plutonium oxalate precipitation mother liquor;
(3) after the addition of the rest mother liquor of plutonium oxalate precipitation to be evaporated and concentrated is finished, the mother liquor is continuously heated for a certain time to continuously destroy the residual oxalic acid in the concentrated liquor.
In a preferred embodiment, the present invention provides a method for destroying oxalic acid in the evaporative concentration of plutonium oxalate precipitation mother liquor in the Purex process, wherein in step (1), the volume fraction of the part of plutonium oxalate precipitation mother liquor to be evaporated and concentrated, which is added, accounts for 5% to 20% of the total plutonium oxalate precipitation mother liquor to be evaporated and concentrated.
In a preferred embodiment, the present invention provides a method for destroying oxalic acid in the evaporative concentration of plutonium oxalate precipitation mother liquor in Purex process, wherein in step (1), Mn is contained2+Mn in the solution of (2)2+The concentration of (A) is 0.008-0.015 mol/L.
In a preferred embodiment, the present invention provides a method for destroying oxalic acid in the evaporative concentration of plutonium oxalate precipitation mother liquor in the Purex process, wherein in step (1), said portion of plutonium oxalate precipitation mother liquor to be evaporated and concentrated and said Mn-containing mother liquor2+The volume ratio of the solution (A) is 5-20: 100.
in a preferred embodiment, the present invention provides a method for destroying oxalic acid in the evaporative concentration of plutonium oxalate precipitation mother liquor in the Purex process, wherein in the step (2), the remaining plutonium oxalate precipitation mother liquor to be subjected to evaporative concentration is added into the evaporative concentration container by a pump.
In a preferred embodiment, the present invention provides a method for destroying oxalic acid in the evaporative concentration of plutonium oxalate precipitation mother liquor in the Purex process, wherein in step (2), the addition rate and the heating power are controlled so that the evaporation rate of plutonium oxalate precipitation mother liquor is equal to the addition rate of plutonium oxalate precipitation mother liquor.
In a preferred embodiment, the invention provides a method for destroying oxalic acid in the evaporation and concentration of plutonium oxalate precipitation mother liquor in the Purex process, wherein in the step (3), the heating is continuously carried out at the temperature of 98-103 ℃ for 15-30 min.
The method has the beneficial effects that the oxalic acid in the mother liquor of plutonium oxalate precipitation in the Purex process can be better destroyed in the evaporation and concentration process by utilizing the method for destroying the oxalic acid in the mother liquor of plutonium oxalate precipitation in the evaporation and concentration process.
The invention establishes Mn in the process of evaporation concentration of the plutonium oxalate precipitation mother liquor, aiming at the process requirements of evaporation concentration 10 times and oxalic acid destruction rate more than 99.9% in the process of Purex post-treatment of spent fuel2+A process for the catalytic oxidation of oxalic acid, determining the relevant process conditions, mainly involving the addition of Mn2+The concentration range, the oxalic acid destruction reaction time, the semi-continuous oxalic acid destruction mode, the oxalic acid destruction reaction tail end treatment method and the like fill up relevant blanks.
Drawings
FIG. 1 is a graph showing the change of oxalic acid concentration with time in the concentration by evaporation of a simulated solution of examples 1 and 2.
Detailed Description
The following further describes embodiments of the present invention by way of examples and figures.
Example 1:
(1) 3000mL of solution containing 0.1mol/L oxalic acid and 2.5mol/L nitric acid is prepared, and the solution is a simulated solution of plutonium oxalate precipitation mother liquor;
(2) in IIIA neck flask was charged with 300mL (preheated to 60 ℃) of the above simulated solution, and 50% (m/m) manganese sulfate solution was added to make Mn in the solution2+The concentration is 0.008mol/L, and the components are uniformly mixed;
(3) heating the mixed solution to boiling, continuously heating the evaporation concentration container, pumping the rest 2700mL of simulation solution into the evaporation concentration container, and controlling the pumping rate and the heating power to ensure that the evaporation rate of the simulation solution and the pumping rate of the simulation solution are both 9 mL/min;
(4) after the simulated solution is pumped in, the evaporation concentration container is continuously heated at the temperature of 98-103 ℃ for 15 min.
The change of oxalic acid concentration with time in the above simulated solution evaporative concentration is shown in FIG. 1. As can be seen from fig. 1: in the process of simulating the evaporation and concentration of the solution, the concentration of the oxalic acid is gradually reduced; after the simulated solution is added (300min), the oxalic acid in the simulated solution is continuously and rapidly destroyed to the concentration of 10-4The order of mol/L; compared with the concentration of oxalic acid in the simulated solution of 0.1mol/L, the total destruction rate of oxalic acid is more than 99.9 percent under the condition that the simulated solution is concentrated ten times.
Example 2:
(1) 3000mL of solution containing 0.1mol/L oxalic acid and 2.5mol/L nitric acid is prepared, and the solution is a simulated solution of plutonium oxalate precipitation mother liquor;
(2) a three-necked flask was charged with 300mL (preheated to 60 ℃) of the above-mentioned simulated solution, and a 50% (m/m) manganese sulfate solution was added to make Mn in the solution2+The concentration is 0.015mol/L, and the mixture is uniform;
(3) heating the mixed solution to boiling, continuously heating the evaporation concentration container, pumping the rest 2700mL of simulation solution into the evaporation concentration container, and controlling the pumping rate and the heating power to ensure that the evaporation rate of the simulation solution and the pumping rate of the simulation solution are both 9 mL/min;
(4) after the simulated solution is pumped in, the evaporation concentration container is continuously heated at the temperature of 98-103 ℃ for 30 min.
The change of oxalic acid concentration with time in the above simulated solution evaporative concentration is shown in FIG. 1. As can be seen from fig. 1: in the process of simulating the evaporation and concentration of the solution, the concentration of the oxalic acid is gradually reduced; after the simulated solution is added (300min), the simulated solution is addedOxalic acid continues to be rapidly destroyed to a concentration of 10-4The order of mol/L; compared with the concentration of oxalic acid in the simulated solution of 0.1mol/L, the total destruction rate of oxalic acid is more than 99.9 percent under the condition that the simulated solution is concentrated ten times.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.

Claims (7)

1. A method for destroying oxalic acid in evaporation and concentration of plutonium oxalate precipitation mother liquor in Purex process is characterized by sequentially comprising the following steps:
(1) adding part of plutonium oxalate precipitation mother liquor to be evaporated and concentrated and Mn in an evaporation and concentration container2+The solution of (1) is heated to boiling after being uniformly mixed, and evaporation concentration is started;
(2) adding the rest plutonium oxalate precipitation mother liquor to be evaporated and concentrated into the evaporation and concentration container under continuous heating, and controlling the addition rate and the heating power to ensure that the evaporation rate of the plutonium oxalate precipitation mother liquor is 0.8-1.2 times of the addition rate of the plutonium oxalate precipitation mother liquor;
(3) after the addition of the rest mother liquor of plutonium oxalate precipitation to be evaporated and concentrated is finished, the mother liquor is continuously heated for a certain time to continuously destroy the residual oxalic acid in the concentrated liquor.
2. The destruction method according to claim 1, wherein: in the step (1), the added part of the mother liquor of plutonium oxalate precipitation to be evaporated and concentrated accounts for 5-20% of the total mother liquor of plutonium oxalate precipitation to be evaporated and concentrated.
3. The destruction method according to claim 1, wherein: in the step (1), the Mn is contained2+Mn in the solution of (2)2+The concentration of (A) is 0.008-0.015 mol/L.
4. The destruction method according to claim 1, wherein: in step (1), said part of mother liquor of plutonium oxalate precipitation to be concentrated by evaporation and said Mn-containing solution2+The volume ratio of the solution (A) is 5-20: 100.
5. the destruction method according to claim 1, wherein: in the step (2), the remaining plutonium oxalate precipitation mother liquor to be evaporated and concentrated is added to the evaporation and concentration vessel by a pump.
6. The destruction method according to claim 1, wherein: in the step (2), the rate of addition and the heating power are controlled so that the evaporation rate of the mother liquor for plutonium oxalate precipitation is equal to the rate of addition of the mother liquor for plutonium oxalate precipitation.
7. The destruction method according to claim 1, wherein: in the step (3), the temperature for continuous heating is 98-103 ℃ and the time is 15-30 min.
CN202010830586.XA 2020-08-18 2020-08-18 Method for destroying oxalic acid in evaporation and concentration of plutonium oxalate precipitation mother liquor in Purex process Pending CN112143917A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113058296A (en) * 2021-03-24 2021-07-02 哈尔滨工程大学 Plutonium oxalate cup type continuous precipitation device
CN114420335A (en) * 2022-01-19 2022-04-29 中国原子能科学研究院 Method for continuously precipitating plutonium oxalate

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2554434A1 (en) * 1983-11-04 1985-05-10 Commissariat Energie Atomique Process for the treatment of acid nitric aqueous effluents containing oxalic acid, usable in particular for treating the mother liquors from the precipitation of plutonium oxalate
RU2111562C1 (en) * 1996-05-29 1998-05-20 Производственное объединение "МАЯК" Method for recovering oxalate mother liquors of transuranium elements
RU2248324C1 (en) * 2003-06-19 2005-03-20 ФГУП "Производственное объединение "Маяк" Method for plutonium recovery from fiberglass aerosol boron- containing filter
JP2010501735A (en) * 2006-08-31 2010-01-21 コミツサリア タ レネルジー アトミーク Solute precipitation method and equipment
CN103617818A (en) * 2013-10-29 2014-03-05 叶绍朋 Radioactive wastewater treatment technology and synthesis of treatment agent of radioactive wastewater
CN103760273A (en) * 2014-01-28 2014-04-30 中国原子能科学研究院 Analysis method for trace oxalic acid root in mother liquor of plutonium oxalate precipitation
CN106119578A (en) * 2016-06-27 2016-11-16 中国原子能科学研究院 In a kind of plutonium oxalate mother liquor of precipitation of ammonium, nitric acid oxalic acid concentrates and the integral method destroyed

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2554434A1 (en) * 1983-11-04 1985-05-10 Commissariat Energie Atomique Process for the treatment of acid nitric aqueous effluents containing oxalic acid, usable in particular for treating the mother liquors from the precipitation of plutonium oxalate
RU2111562C1 (en) * 1996-05-29 1998-05-20 Производственное объединение "МАЯК" Method for recovering oxalate mother liquors of transuranium elements
RU2248324C1 (en) * 2003-06-19 2005-03-20 ФГУП "Производственное объединение "Маяк" Method for plutonium recovery from fiberglass aerosol boron- containing filter
JP2010501735A (en) * 2006-08-31 2010-01-21 コミツサリア タ レネルジー アトミーク Solute precipitation method and equipment
CN103617818A (en) * 2013-10-29 2014-03-05 叶绍朋 Radioactive wastewater treatment technology and synthesis of treatment agent of radioactive wastewater
CN103760273A (en) * 2014-01-28 2014-04-30 中国原子能科学研究院 Analysis method for trace oxalic acid root in mother liquor of plutonium oxalate precipitation
CN106119578A (en) * 2016-06-27 2016-11-16 中国原子能科学研究院 In a kind of plutonium oxalate mother liquor of precipitation of ammonium, nitric acid oxalic acid concentrates and the integral method destroyed

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113058296A (en) * 2021-03-24 2021-07-02 哈尔滨工程大学 Plutonium oxalate cup type continuous precipitation device
CN114420335A (en) * 2022-01-19 2022-04-29 中国原子能科学研究院 Method for continuously precipitating plutonium oxalate
CN114420335B (en) * 2022-01-19 2024-02-20 中国原子能科学研究院 Method for continuously precipitating plutonium oxalate

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