CN102153143B - Technology method and device for preparing ammonium diuranate - Google Patents
Technology method and device for preparing ammonium diuranate Download PDFInfo
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- CN102153143B CN102153143B CN 201110089807 CN201110089807A CN102153143B CN 102153143 B CN102153143 B CN 102153143B CN 201110089807 CN201110089807 CN 201110089807 CN 201110089807 A CN201110089807 A CN 201110089807A CN 102153143 B CN102153143 B CN 102153143B
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Abstract
The invention provides a technology method and a device for preparing ammonium diuranate. The technology is used for preparing ADU (ammonium diuranate) with high conversion activity from UO2F2 solution which is prepared by hydrolyzing UF6 and serves as a raw material by performing an ADU precipitation reaction of the UO2F2 solution and ammonia in a reactor. In the technological process, ADU slurry which is formed after prior batch of precipitation is completed is used as detained ADU slurry; and the detained ADU slurry is added into the UO2F2 solution to start to carry out next precipitation batch. The ADU prepared by adopting the technical scheme of the invention has high conversion activity and can be used for preparing UO2 powder with high sintering activity. The invention also designs a device for the ADU precipitation technology. By the device, the ADU preparation technology can be ensured to be carried out safely. Meanwhile, the technology method has the advantages that the technology method has short process and little equipment and automatic control operation is convenient to realize, etc.
Description
Technical field
The invention belongs to the Nuclear Fuel Element for PWR preparing technical field, relate in particular to process of preparing and the device of a kind of ammonium diuranate (ADU).
Background technology
The ADU method is to develop into the earliest industrial-scale production ceramic grade UO
2The method of powder, dominate aspect the production of power reactor oxide fuel element is still one of main production method at present in the world always.
The chemical molecular formula of ammonium diuranate is written as (NH usually
4)
2U
2O
7, but in fact it is non-stoichiometric compound, and deposition condition is different, and sedimentary chemical constitution is not identical yet, can use general formula (NH
4)
2U
nO
3n+1Expression, n is between 2～4 generally speaking.The reaction formula of ADU precipitation is as follows:
2UO
2F
2+6NH
3·H
2O→(NH
4)
2U
2O
7+4NH
4F+3H
2O
ADU method depositing technology is divided into continuous precipitation and batch precipitation dual mode.The home and abroad is utilizing ADU method industrial-scale production ceramic grade UO at present
2In the powder technology field, what all adopt is continuous precipitation technique, ADU batch of precipitation UO
2Powder technology does not also form industrial scale production, because batch precipitation is compared with continuous precipitation, the ADU powder of preparing has higher activity of conversion, more is conducive to prepare the UO with high sintering activity
2Therefore powder needs a kind of ADU batch of depositing technology new, that can realize industrial scale production of research and development.
Summary of the invention
The object of the present invention is to provide a kind of ADU batch of depositing technology method that can realize that industrial scale produces and device thereof.
Realize the technical scheme of the object of the invention: a kind of process of preparing of ammonium diuranate, it comprises the steps:
(1) with UF
6Be prepared into the UO that uranium concentration is 70～130g/L by the gasification hydrolysis process
2F
2Solution;
(2) be the UO of 70～130g/L to above-mentioned steps (1) gained uranium concentration
2F
2The adding mass percent concentration is 20%～28% ammoniacal liquor in the solution, control NH
3With the mol ratio of U ion be 1: (24～34), add the ammoniacal liquor time at 3min～10min, temperature of reaction is at 20 ℃～50 ℃, sedimentation time obtains the ADU slurry at 3min～10min;
(3) aging to the capable stirring of above-mentioned steps (2) gained ADU slurry, digestion time is 4～12min, and aging temperature is 20 ℃～50 ℃, and ADU precipitation crystalline size is grown up, and the ADU slurry after wearing out is as being detained the ADU slurry;
(4) repeat above-mentioned steps (1), obtain the UO of 70～130g/L
2F
2Solution;
(5) to the UO of 70～130g/L of step (4) gained
2F
2The delay ADU slurry that adds above-mentioned steps (3) gained in the solution, volume and the UO of delay ADU slurry
2F
2The volume ratio of solution is controlled at 1: (0.3～5.0); And then to add mass percent concentration be 20%～28% ammoniacal liquor, control NH
3With the mol ratio of U ion be 1: (24～34), the ammonification time, temperature of reaction was at 20 ℃～50 ℃ at 3min～10min, sedimentation time obtains the ADU slurry at 3min～10min; Aging to the capable stirring of this ADU slurry, digestion time is 4～12min, and aging temperature is 20 ℃～50 ℃, the ADU slurry after obtaining wearing out;
(6) the ADU slurry after aging to step (5) gained carries out solid-liquid separation, and then dry, control ADU powder water ratio finally obtains qualified ADU powder less than 3%.
The process of preparing of aforesaid a kind of ammonium diuranate, its step (1) is described with UF
6Be prepared into UO by the gasification hydrolysis process
2F
2Solution is with UF
6Be heated to more than 70 ℃, make UF
6Gasification is then with deionized water and UF
6The reverse contact of gas, the reaction that is hydrolyzed is prepared into the UO that uranium concentration is 70～130g/L
2F
2Solution.
Ammonium diuranate preparation facilities of the present invention, it comprises a column precipitator, the column precipitator outside is provided with watercooling jacket; The column precipitator top connects UO
2F
2The solution input duct; The column precipitator outlet at bottom is connected with circulation magnetic pump, and the circulation magnetic force pump discharge is divided into the two-way pipeline, and one the tunnel is the circulation stirring pipeline, and another road is the fluid pipeline; The circulation stirring pipeline is connected with interchanger, is connected with the column precipitator top through behind the interchanger; The fluid pipeline is connected to precipitation storage fluid column top; Precipitation storage liquid column bottom connects precipitation storage fluid column Pump for giving-out entrance, and the outlet of precipitation storage fluid column Pump for giving-out connects the horizontal centrifuge entrance; Below the horizontal centrifuge outlet, connect drying machine; The ammoniacal liquor header tank is connected to by the ammoniacal liquor pipeline on the feed liquor pipeline of circulation magnetic pump of column precipitator bottom.
The preparation facilities of aforesaid a kind of ammonium diuranate, the aspect ratio of its described column precipitator are 10～45, and column precipitator is provided with liquidometer and is used for level monitoring.
The preparation facilities of aforesaid a kind of ammonium diuranate, its described circulation stirring pipeline is provided with pneumavalve three; Described fluid pipeline is provided with pneumavalve four; Described UO
2F
2The solution input duct is provided with pneumavalve one; Described ammoniacal liquor pipeline is provided with pneumavalve two and under meter.
The preparation facilities of aforesaid a kind of ammonium diuranate, its described interchanger adopts cooling circulating water as heat-eliminating medium.
Effect of the present invention is: technique of the present invention is with UF
6The UO of hydrolysis preparation gained
2F
2Solution is raw material, carries out the ADU precipitin reaction with ammoniacal liquor in reactor, and preparation has the ADU of high activity of conversion.In the technological process, the ADU slurry of formation will be detained ADU slurry adding UO as being detained the ADU slurry after previous batch of precipitation finished
2F
2Solution begins to carry out next one precipitation batch.Adopt the ADU of technical solution of the present invention preparation to have good activity of conversion, can be for the preparation of the UO with high sintering activity
2Powder.The present invention has also designed a kind of device for the ADU depositing technology, and it can guarantee the carrying out of ADU safe preparation process.Have simultaneously flow process short, equipment is few, is convenient to realize the advantages such as automatic operation.
Description of drawings
Fig. 1 is the preparation facilities figure of a kind of ammonium diuranate of the present invention (ADU).
Among the figure: 1. ammoniacal liquor header tank; 2. column precipitator; 3. circulation magnetic pump; 4. interchanger; 5. precipitation is store fluid column; 6. precipitation is store the fluid column Pump for giving-out; 7. whizzer; 8. drying machine; 9. watercooling jacket; 10.UO
2F
2The solution input duct; 11. pneumavalve one; 12. circulation stirring pipeline; 13. fluid pipeline; 14. ammoniacal liquor pipeline; 15. pneumavalve two; 16. under meter; 17. pneumavalve three; 18. pneumavalve four; 19. liquidometer;
Among the figure: A.UO
2F
2Solution; B1. cool off upper water; B2. cool off lower water; C. ammoniacal liquor; The D.ADU slurry; The E.ADU filter cake; F. centrifuge mother liquor; The G.ADU powder;
Liquidometer;
Under meter.
Embodiment
Be described further below in conjunction with process of preparing and the device of the drawings and specific embodiments to a kind of ammonium diuranate of the present invention (ADU).
Embodiment 1
Batch precipitation processing method of a kind of ammonium diuranate of the present invention (ADU) makes it can realize industrial scale production, and it comprises the steps:
(1) stock liquid preparation: UF will be housed
6Container be heated to 70 ℃, make UF
6Gasification is delivered in the hydrolysis post through pipeline, and deionized water adds and UF from the hydrolysis column top
6The reverse contact of gas, the reaction that is hydrolyzed is prepared into the UO that uranium concentration is 100g/L
2F
2Solution;
(2) ADU precipitation process: to 60 liters of uranium concentrations of above-mentioned steps (1) gained UO that is 100g/L
2F
2The adding mass percent concentration is 25% ammoniacal liquor in the solution, control NH
3With the mol ratio of U ion be 1: 30, the ammonification time, temperature of reaction was at 35 ℃ at 6min, sedimentation time obtains the ADU slurry at 7min;
(3) burin-in process: aging to the capable stirring of above-mentioned steps (2) gained ADU slurry, digestion time is 7min, and aging temperature is 35 ℃, and ADU precipitation crystalline size is grown up, and the ADU slurry after wearing out is as being detained the ADU slurry;
(4) stock liquid preparation: repeat above-mentioned steps (1), obtain the UO of 100g/L
2F
2Solution;
(5) ADU precipitation and weathering process: to the UO of the 100g/L of step (4) gained
2F
2The delay ADU slurry that adds above-mentioned steps (3) gained in the solution is used for improving the potential of hydrogen (pH value) of hydrolyzed solution, volume and the UO of delay ADU slurry
2F
2The volume ratio of solution is controlled at 1: 2.5; And then to add mass percent concentration be 25% ammoniacal liquor, control NH
3With the mol ratio of U ion be 1: 30, the ammonification time, temperature of reaction was at 35 ℃ at 6min, sedimentation time obtains the ADU slurry at 7min; Aging to the capable stirring of this ADU slurry, digestion time is 7min, and aging temperature is 35 ℃, ADU precipitation crystalline size is grown up, the ADU slurry after obtaining wearing out;
(6) the ADU slurry after aging to step (5) gained carries out the solid-liquid centrifugation, and is then dry, removes entrapped moisture, and control ADU powder water ratio finally obtains qualified ADU powder less than 3%.
The above-mentioned raw material UF that adopts
6Meet "
235The U abundance is lower than 5% concentrated uranium hexafluoride technical qualification " (GB/T13696-1997) standard.
Batch precipitation processing method of a kind of ammonium diuranate of the present invention (ADU) makes it can realize industrial scale production, and it comprises the steps:
(1) stock liquid preparation: UF will be housed
6Container be heated to more than 70 ℃, make UF
6Gasification is delivered in the hydrolysis post through pipeline, and deionized water adds and UF from the hydrolysis column top
6The reverse contact of gas, the reaction that is hydrolyzed is prepared into the UO that uranium concentration is 70g/L
2F
2Solution;
(2) ADU precipitation process: to 20 liters of uranium concentrations of above-mentioned steps (1) gained UO that is 70g/L
2F
2The adding mass percent concentration is 20% ammoniacal liquor in the solution, control NH
3With the mol ratio of U ion be 1: 24, the ammonification time, temperature of reaction was at 20 ℃ at 3min, sedimentation time obtains the ADU slurry at 3min;
(3) burin-in process: aging to the capable stirring of above-mentioned steps (2) gained ADU slurry, digestion time is 4min, and aging temperature is 20 ℃, and ADU precipitation crystalline size is grown up, and the ADU slurry after wearing out is as being detained the ADU slurry;
(4) stock liquid preparation: repeat above-mentioned steps (1), obtain the UO of 70g/L
2F
2Solution;
(5) ADU precipitation and weathering process: to the UO of the 70g/L of step (4) gained
2F
2The delay ADU slurry that adds above-mentioned steps (3) gained in the solution is used for improving the potential of hydrogen (pH value) of hydrolyzed solution, volume and the UO of delay ADU slurry
2F
2The volume ratio of solution is controlled at 1: 5; Then add mass percent concentration and be 20% ammoniacal liquor, control NH
3With the mol ratio of U ion be 1: 24, the ammonification time, temperature of reaction was at 20 ℃ at 3min, sedimentation time obtains the ADU slurry at 3min; Aging to the capable stirring of this ADU slurry, digestion time is 4min, and aging temperature is 20 ℃, ADU precipitation crystalline size is grown up, the ADU slurry after obtaining wearing out;
(6) the ADU slurry after aging to step (5) gained carries out the solid-liquid centrifugation, and is then dry, removes entrapped moisture, and control ADU powder water ratio finally obtains qualified ADU powder less than 3%.
The above-mentioned raw material UF that adopts
6Meet "
235The U abundance is lower than 5% concentrated uranium hexafluoride technical qualification " (GB/T13696-1997) standard.
Batch precipitation processing method of a kind of ammonium diuranate of the present invention (ADU) makes it can realize industrial scale production, and it comprises the steps:
(1) stock liquid preparation: UF will be housed
6Container be heated to more than 70 ℃, make UF
6Gasification is delivered in the hydrolysis post through pipeline, and deionized water adds and UF from the hydrolysis column top
6The reverse contact of gas, the reaction that is hydrolyzed is prepared into the UO that uranium concentration is 130g/L
2F
2Solution;
(2) ADU precipitation process: to 100 liters of uranium concentrations of above-mentioned steps (1) gained UO that is 130g/L
2F
2The adding mass percent concentration is 28% ammoniacal liquor in the solution, control NH
3With the mol ratio of U ion be 1: 34, the ammonification time, temperature of reaction was at 50 ℃ at 10min, sedimentation time obtains the ADU slurry at 10min;
(3) burin-in process: aging to the capable stirring of above-mentioned steps (2) gained ADU slurry, digestion time is 12min, and aging temperature is 50C, and ADU precipitation crystalline size is grown up, and the ADU slurry after wearing out is as being detained the ADU slurry;
(4) stock liquid preparation: repeat above-mentioned steps (1), obtain the UO of 130g/L
2F
2Solution;
(5) ADU precipitation and weathering process: to the UO of the 130g/L of step (4) gained
2F
2The delay ADU slurry that adds above-mentioned steps (3) gained in the solution is used for improving the potential of hydrogen (pH value) of hydrolyzed solution, volume and the UO of delay ADU slurry
2F
2The volume ratio of solution is controlled at 1: 0.3; Then add mass percent concentration and be 28% ammoniacal liquor, control NH
3With the mol ratio of U ion be 1: 34, the ammonification time, temperature of reaction was at 50C at 10min, sedimentation time obtains the ADU slurry at 10min; Aging to the capable stirring of this ADU slurry, digestion time is 12min, and aging temperature is 50C, ADU precipitation crystalline size is grown up, the ADU after obtaining wearing out;
(6) the ADU slurry after aging to step (5) gained carries out the solid-liquid centrifugation, and is then dry, removes entrapped moisture, and control ADU powder water ratio finally obtains qualified ADU powder less than 3%.
The above-mentioned raw material UF that adopts
6Meet "
235The U abundance is lower than 5% concentrated uranium hexafluoride technical qualification " (GB/T13696-1997) standard.
Embodiment 4
As shown in Figure 1, the preparation facilities of ammonium diuranate of the present invention (ADU), comprise a column precipitator 2, column precipitator 2 adopts stainless steel or carbon steel, lining one deck heat resisting corrosion-proof corrosion material is rolled in its inside, as can selecting the F40 material, the aspect ratio of column precipitator is 10～45 (for example 10,, 20,30 or 45).Column precipitator 2 outsides are provided with watercooling jacket 9, and watercooling jacket 9 is used for the control precipitation reaction temperature.Column precipitator 2 tops connect UO
2F
2 Solution input duct 10, UO
2F
2 Solution input duct 10 is provided with pneumavalve 1.Pneumavalve 1 is chain with column precipitator 2 liquid levels, advances UO
2F
2During solution, pneumavalve 1 cuts out when column precipitator 2 interior liquid levels reach set(ting)value.Also be provided with liquidometer 19 on the column precipitator 2 and be used for level monitoring, be provided with thermometric instrument and be used for the monitoring temperature of reaction.
Ammoniacal liquor is contained in the ammoniacal liquor header tank 1, and pneumavalve 2 15 and under meter 16 are housed on the ammoniacal liquor pipeline 14, is used for add-on and the joining day of control ammoniacal liquor.The ammoniacal liquor header tank 1 that holds ammoniacal liquor is connected to by ammoniacal liquor pipeline 14 on the feed liquor pipeline of circulation magnetic pump 3 of column precipitator 2 bottoms, and ammoniacal liquor enters circulation stirring pipeline 12 by the feed liquor pipeline of circulation magnetic pump 3, and finally adds in the column precipitator 2.
Precipitation storage fluid column 5 bottoms connect precipitation storage fluid column Pump for giving-out 6 entrances, and 6 outlets of precipitation storage fluid column Pump for giving-out connect horizontal centrifuge 7 entrances; Below horizontal centrifuge 7 outlets, connect drying machine 8.Precipitation storage fluid column 5 is used for storing the ADU slurry that preparation is finished.Precipitation storage fluid column Pump for giving-out 6 is used for the ADU slurry is delivered to horizontal centrifuge 7 and drying machine 8.
Adopt device shown in Figure 1 as follows by the method steps that batch depositing technology prepares ammonium diuranate (ADU):
(1) raw material preparation: UF will be housed
6Container be heated to more than 70 ℃, make UF
6Gasification is delivered in the hydrolysis post through pipeline, and deionized water adds and UF from the hydrolysis column top
6The reverse contact of gas, the reaction that is hydrolyzed is with raw material UF
6Change into the UO that uranium concentration is 70g/L
2F
2Solution.
(2) ADU precipitation process: at first open water B1 and the lower water B2 valve of cooling in the cooling of column precipitator 2, then open UO
2F
2Solution A feed liquor pneumavalve 1 is with 20 liters of UO
2F
2Solution A flows into column precipitator 2, and when liquid level reaches when opening the pump set(ting)value, circulation magnetic pump 3 starts automatically, opens simultaneously that water B1 and cooling descend water B2 valve in the cooling of interchanger 4, when liquid level reaches the charging set(ting)value, and UO
2F
2Solution A feed liquor pneumavalve one 11 autoshutdowns, ammoniacal liquor C charging pneumavalve 2 15 is opened automatically, and 20% ammoniacal liquor flows into circulation magnetic pump 3 entrances by ammoniacal liquor header tank 1 through under meter 16, and the ammonification time is controlled in the scope of 3min, at the total NH of control
3: U=24 (mol ratio), temperature are that 20 ℃, sedimentation time are to carry out the ADU precipitation under the 3min condition, whipping process is finished in circulation by circulation magnetic pump 3, when ammoniacal liquor C add-on reaches set(ting)value, ammoniacal liquor charging pneumavalve 2 15 autoshutdowns, simultaneously ammoniacal liquor under meter automatic clear.
(3) burin-in process: after precipitation was finished, ADU slurry D carried out the approximately circulation stirring weathering process of 4min in column precipitator 2, and aging temperature is 20 ℃, made the precipitation crystalline size can reach the index of arts demand.When digestion time reached set(ting)value, ADU slurry D fluid pneumavalve 4 18 was opened automatically, and ADU slurry D is delivered to precipitation storage fluid column 5.
When (4) ADU slurry D got, at the ADU slurry D of column precipitator 2 interior reservation certain volumes, volume and the next one of being detained slurry precipitated required UO
2F
2The solution A volume ratio is controlled at about 5.
When (5) ADU slurry D got, when column precipitator 2 interior liquid levels reached set(ting)value, autoshutdown fluid pneumavalve 4 18 was opened UO simultaneously
2F
2Solution A feed liquor pneumavalve 1, the precipitation of beginning next batch.
(6) centrifugation and drying treatment: ADU slurry D is delivered to precipitation storage fluid column Pump for giving-out 6 and carries out solid-liquid separation in the whizzer 7, directly fall in the drying machine 8 by gravity from the ADU filter cake E of whizzer 7, ADU filter cake E progressively removes entrapped moisture at drying machine 8, control ADU powder G water ratio finally obtains qualified ADU powder G less than 3%.
Embodiment 5
Adopt such as 1 shown device as follows by the method steps that batch depositing technology prepares ammonium diuranate (ADU):
(1) raw material preparation: UF will be housed
6Container be heated to more than 70 ℃, make UF
6Gasification is delivered in the hydrolysis post through pipeline, and deionized water adds and UF from the hydrolysis column top
6The reverse contact of gas, the reaction that is hydrolyzed is with raw material UF
6Change into the UO that uranium concentration is 100g/L
2F
2Solution.
(2) ADU precipitation process: at first open water B1 and the lower water B2 valve of cooling in the cooling of column precipitator 2, then open UO
2F
2Solution A feed liquor pneumavalve is with 60 liters of UO
2F
2Solution A flows into column precipitator 2, and when liquid level reaches when opening the pump set(ting)value, circulation magnetic pump 3 starts automatically, opens simultaneously that water B1 and cooling descend water B2 valve in the cooling of interchanger 4, when liquid level reaches the charging set(ting)value, and UO
2F
2Solution A feed liquor pneumavalve one 11 autoshutdowns, ammoniacal liquor C charging pneumavalve 2 15 is opened automatically, and 25% ammoniacal liquor flows into circulation magnetic pump 3 entrances by ammoniacal liquor header tank 1 through under meter 16, and the ammonification time is controlled in the scope of 6min, at the total NH of control
3: U=30 (mol ratio), temperature t=35 ℃, sedimentation time are to carry out the ADU precipitation under the condition of 7min, whipping process is finished in circulation by circulation magnetic pump 3, when ammoniacal liquor C add-on reaches set(ting)value, ammoniacal liquor charging pneumavalve 2 15 autoshutdowns, simultaneously ammoniacal liquor under meter 16 automatic clears.
(3) burin-in process: after precipitation was finished, ADU slurry D carried out the approximately circulation stirring weathering process of 7min in column precipitator 2, and aging temperature is 35 ℃, made the precipitation crystalline size can reach the index of arts demand.When digestion time reached set(ting)value, ADU slurry D discharging pneumavalve 4 18 was opened automatically, and ADU slurry D is delivered to precipitation storage fluid column 5.
When (5) ADU slurry D got, at the ADU slurry D of column precipitator 2 interior reservation certain volumes, volume and the next one of being detained slurry precipitated required UO
2F
2The solution A volume ratio is controlled at about 2.5.
When (6) ADU slurry D got, when column precipitator 2 interior liquid levels reached set(ting)value, autoshutdown fluid pneumavalve 4 18 was opened UO simultaneously
2F
2Solution A feed liquor pneumavalve, the precipitation of beginning next batch.
(7) centrifugation and drying treatment: ADU slurry D is delivered to precipitation storage fluid column Pump for giving-out 6 and carries out solid-liquid separation in the whizzer 7, directly fall in the drying machine 8 by gravity from the ADU filter cake E of whizzer 7, ADU filter cake E progressively removes entrapped moisture at drying machine 8, control ADU powder G water ratio finally obtains qualified ADU powder G less than 3%.
Adopt device shown in Figure 1 as follows by the method steps that batch depositing technology prepares ammonium diuranate (ADU):
(1) raw material preparation: UF will be housed
6Container be heated to more than 70 ℃, make UF
6Gasification is delivered in the hydrolysis post through pipeline, and deionized water adds and UF from the hydrolysis column top
6The reverse contact of gas, the reaction that is hydrolyzed is with raw material UF
6Change into the UO that uranium concentration is 130g/L
2F
2Solution.
(2) ADU precipitation process: at first open water B1 and the lower water B2 valve of cooling in the cooling of column precipitator 2, then open UO
2F
2Solution A feed liquor pneumavalve is with 100 liters of UO
2F
2Solution A flows into column precipitator 2, and when liquid level reaches when opening the pump set(ting)value, circulation magnetic pump 3 starts automatically, opens simultaneously that water B1 and cooling descend water B2 valve in the cooling of interchanger 4, when liquid level reaches the charging set(ting)value, and UO
2F
2Solution A feed liquor pneumavalve one 11 autoshutdowns, ammoniacal liquor C charging pneumavalve 2 15 is opened automatically, and 28% ammoniacal liquor flows into circulation magnetic pump 3 entrances by ammoniacal liquor header tank 1 through under meter, and the ammonification time is controlled in the scope of 10min, at the total NH of control
3: carry out the ADU precipitation under U=34 (mol ratio), temperature t=50 ℃ the condition, whipping process is finished in circulation by circulation magnetic pump 3, when ammoniacal liquor C add-on reaches set(ting)value, ammoniacal liquor charging pneumavalve 2 15 autoshutdowns, simultaneously ammoniacal liquor under meter automatic clear.
(3) burin-in process: after precipitation was finished, ADU slurry D carried out the approximately circulation stirring weathering process of 12min in column precipitator 2, and aging temperature is 50 ℃, made the precipitation crystalline size can reach the index of arts demand.When digestion time reached set(ting)value, ADU slurry D discharging pneumavalve 4 18 was opened automatically, and ADU slurry D is delivered to precipitation storage fluid column 5.
When (4) ADU slurry D got, at the ADU slurry D of column precipitator 2 interior reservation certain volumes, volume and the next one of being detained slurry precipitated required UO
2F
2The solution A volume ratio is controlled at about 0.3.
When (5) ADU slurry D got, when column precipitator 2 interior liquid levels reached set(ting)value, autoshutdown fluid pneumavalve 4 18 was opened UO simultaneously
2F
2Solution A feed liquor pneumavalve, the precipitation of beginning next batch.
(6) centrifugation and drying treatment: ADU slurry D is delivered to precipitation storage fluid column Pump for giving-out 6 and carries out solid-liquid separation in the whizzer 7, directly fall in the drying machine 8 by gravity from the ADU filter cake E of whizzer 7, ADU filter cake E progressively removes entrapped moisture at drying machine 8, control ADU powder G water ratio finally obtains qualified ADU powder G less than 3%.
Claims (5)
1. the process of preparing of an ammonium diuranate, it is characterized in that: the method comprises the steps:
(1) with UF
6Be prepared into the UO that uranium concentration is 70～130g/L by the gasification hydrolysis process
2F
2Solution;
(2) be the UO of 70～130g/L to above-mentioned steps (1) gained uranium concentration
2F
2The adding mass percent concentration is 20%～28% ammoniacal liquor in the solution, control NH
3With the mol ratio of U ion be 1:(24～34), the ammonification time, temperature of reaction was at 20 ℃～50 ℃ at 3min～10min, sedimentation time obtains the ADU slurry at 3min～10min;
(3) above-mentioned steps (2) gained ADU slurry is stirred aging, digestion time is 4～12min, and aging temperature is 20 ℃～50 ℃, and ADU precipitation crystalline size is grown up, and the ADU slurry after aging is as being detained the ADU slurry;
(4) repeat above-mentioned steps (1), obtain the UO of 70～130g/L
2F
2Solution;
(5) to the UO of 70～130g/L of step (4) gained
2F
2The delay ADU slurry that adds above-mentioned steps (3) gained in the solution, volume and the UO of delay ADU slurry
2F
2The volume ratio of solution is controlled at 1:(0.3～5.0); And then to add mass percent concentration be 20%～28% ammoniacal liquor, control NH
3With the mol ratio of U ion be 1:(24～34), the ammonification time, temperature of reaction was at 20 ℃～50 ℃ at 3min～10min, sedimentation time obtains the ADU slurry at 3min～10min; Aging to the capable stirring of this ADU slurry, digestion time is 4～12min, and aging temperature is 20 ℃～50 ℃, the ADU slurry after obtaining wearing out;
(6) the ADU slurry after aging to step (5) gained carries out solid-liquid separation, and then dry, control ADU powder water ratio finally obtains qualified ADU powder less than 3%.
2. the process of preparing of a kind of ammonium diuranate according to claim 1, it is characterized in that: step (1) is described with UF
6Be prepared into UO by the gasification hydrolysis process
2F
2Solution is with UF
6Be heated to more than 70 ℃, make UF
6Gasification is then with deionized water and UF
6The reverse contact of gas, the reaction that is hydrolyzed is prepared into the UO that uranium concentration is 70～130g/L
2F
2Solution.
3. ammonium diuranate preparation facilities that is used for the process of preparing of ammonium diuranate claimed in claim 1, it is characterized in that: this device comprises a column precipitator (2), column precipitator (2) outside is provided with watercooling jacket (9); Column precipitator (2) top connects UO
2F
2Solution input duct (10);
Column precipitator (2) outlet at bottom is connected with circulation magnetic pump (3), and circulation magnetic pump (3) outlet is divided into the two-way pipeline, and one the tunnel is circulation stirring pipeline (12), and another road is fluid pipeline (13);
Circulation stirring pipeline (12) is connected with interchanger (4), through being connected with column precipitator (2) top behind the interchanger (4); Fluid pipeline (13) is connected to precipitation storage fluid column (5) top; Precipitation storage fluid column (5) bottom connects precipitation storage fluid column Pump for giving-out (6) entrance, and precipitation storage fluid column Pump for giving-out (6) outlet connects horizontal centrifuge (7) entrance; Connect drying machine (8) in horizontal centrifuge (7) outlet below;
Ammoniacal liquor header tank (1) is connected to by ammoniacal liquor pipeline (14) on the feed liquor pipeline of circulation magnetic pump (3) of column precipitator (2) bottom;
Described circulation stirring pipeline is provided with pneumavalve three (17); Described fluid pipeline (13) is provided with pneumavalve four (18); Described UO
2F
2Solution input duct (10) is provided with pneumavalve one (11); Described ammoniacal liquor pipeline (14) is provided with pneumavalve two (15) and under meter (16).
4. the preparation facilities of a kind of ammonium diuranate according to claim 3, it is characterized in that: the aspect ratio of described column precipitator (2) is 10～45, column precipitator (2) is provided with liquidometer (19) and is used for level monitoring.
5. the preparation facilities of a kind of ammonium diuranate according to claim 3 is characterized in that: described interchanger (4) adopts cooling circulating water as heat-eliminating medium.
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| US9567237B2 (en) | 2012-11-16 | 2017-02-14 | Honeywell International Inc. | Separation and recovery of molybdenum values from uranium process distillate |
| CN106636692B (en) * | 2016-12-28 | 2018-11-30 | 中核四0四有限公司 | A kind of uranium purification process of ammonium diuranate |
| CN114477295A (en) * | 2020-11-13 | 2022-05-13 | 中核北方核燃料元件有限公司 | Method for treating uranium in centrifugal mother liquor by using membrane separation technology |
| CN112390290A (en) * | 2020-11-20 | 2021-02-23 | 中核北方核燃料元件有限公司 | High-purity UF for thorium-based molten salt reactor4Preparation method |
| CN118373455A (en) * | 2024-04-18 | 2024-07-23 | 核工业北京化工冶金研究院 | Method for preparing sodium diuranate yellow cake product from uranium-rich slurry |
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|---|---|---|---|---|
| CN86103859A (en) * | 1985-06-04 | 1987-02-18 | 三菱金属株式会社 | The method of transfer UF 6 to UF 2 |
| EP0498138A1 (en) * | 1991-02-04 | 1992-08-12 | Institute Of Nuclear Energy Research, Chinese Atomic Energy Council | Process for converting uranyl compounds to UO2 via ADU |
| CN1922110A (en) * | 2003-12-24 | 2007-02-28 | 原子燃料工业株式会社 | Liquid stock for dropping, method for preparing liquid stock for dropping, method for preparing uranyl nitrate solution, and method for preparing polyvinyl alcohol solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86103859A (en) * | 1985-06-04 | 1987-02-18 | 三菱金属株式会社 | The method of transfer UF 6 to UF 2 |
| EP0498138A1 (en) * | 1991-02-04 | 1992-08-12 | Institute Of Nuclear Energy Research, Chinese Atomic Energy Council | Process for converting uranyl compounds to UO2 via ADU |
| CN1922110A (en) * | 2003-12-24 | 2007-02-28 | 原子燃料工业株式会社 | Liquid stock for dropping, method for preparing liquid stock for dropping, method for preparing uranyl nitrate solution, and method for preparing polyvinyl alcohol solution |
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