CN113526558B - Method for preparing uranium nitrate by reducing uranyl nitrate through catalytic hydrogenation - Google Patents
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Abstract
The invention discloses a method for preparing uranium nitrate (tetravalent uranium) by reducing uranyl nitrate (hexavalent uranium) through catalytic hydrogenation. The gas-liquid mixture is subjected to online dropwise addition of a hydrazine nitrate or hydrazine solution to enable the solution to be converted from an oxidation state to a reduction state and then enter a high-pressure gas-liquid separator for separation, nitrogen oxides in a gas phase are absorbed and separated by alkali liquor, hydrogen enters a high-pressure hydrogen storage tank after being pressurized by a compressor, a liquid-phase product is discharged from the bottom of the separator and enters a normal-pressure liquid-phase product hydrogen replacement tower, dissolved hydrogen in the liquid phase is removed in the tower by using a nitrogen bubbling device, so that the safety of a subsequent process is ensured, and the obtained gas enters a high-pressure tail gas treatment system.
Description
Technical Field
The invention relates to a technological process for preparing tetravalent uranium, in particular to a technological process for preparing uranium nitrate (tetravalent uranium) by catalytic hydrogenation reduction of uranyl nitrate (hexavalent uranium).
Background
With large-scale development and application of nuclear power, clean treatment and efficient recycling of nuclear spent fuel become key points for further development of nuclear power. At present, the technology mainly adopted by domestic and foreign post-treatment plants is Purex process flow. In the process, valuable uranium plutonium elements are extracted into an organic phase through an extraction unit, so that the valuable uranium plutonium elements are separated from most of splinter elements, and the purpose of decontamination is achieved; and subsequently, adding tetravalent uranium as a reducing agent, reducing the tetravalent plutonium into trivalent plutonium, and allowing the trivalent plutonium to enter a water phase, wherein the hexavalent uranium still remains in an oil phase, so that the efficient separation and purification of the uranium plutonium are realized. The biggest advantage of this process is, will newly add tetravalent uranium oxidation to hexavalent while reducing lipophilic tetravalent plutonium to the trivalent of hydrophilicity, has realized like this that uranium/plutonium clean separation and high-efficient utilization are realized under the prerequisite of not introducing any impurity ion. Therefore, in order to realize the above process, in addition to the due extraction process, it is very important to develop a process for reducing hexavalent uranium to form tetravalent uranium and related reaction equipment for the whole process development and utilization.
In the current technology of China, the preparation of the uranium is mainly dependent on electrolysis, and the content of the uranium in the prepared feed liquid is only 75% (the total uranium concentration is 200g/l, and the uranium concentration is 150 g/l). The low-concentration tetravalent uranium causes that the content of plutonium in the current subsequent process of China is only 3g/l (French UP3, UP2-800 is 6g/l), which brings great pressure to the subsequent plutonium purification and recycling, and increases the system load and the processing cost. In addition, the Chinese atomic energy science research institute also provides a technological process for preparing uranium nitrate by catalytic reduction of uranyl nitrate with hydrazine nitrate, wherein in the reaction process, hydrazine nitrate can react with uranyl nitrate in a way of (1), and hydrazine nitrate can also carry out thermal decomposition reaction in the presence of a catalyst in a way of (2). In a related reactor, the reaction (1) and the reaction (2) are a parallel reaction process, if the residence time of the reaction liquid is insufficient, the reaction (1) cannot be completely carried out, the uranyl nitrate conversion rate is relatively high, but when the residence time of the reaction liquid is too long, the hydrazine nitrate catalytic decomposition reaction (2) is transitionally carried out, so that the product liquid is converted from a reduction state to an oxidation state, the uranium tetravalence nitrate generated by the reaction is further oxidized into the uranyl nitrate, and the hexavalent uranium conversion rate is reduced. Therefore, in order to obtain a high uranyl nitrate conversion rate in the process, the residence time of the reaction liquid needs to be accurately controlled so that the hydrazine nitrate conversion rate is 30-40%, and the special requirement on the residence time of the reactor brings great difficulty to the industrialization of the process.
N 2 H 5 NO 3 +HNO 3 +2UO 2 (NO 3 ) 2 ＝2U(OH)(NO 3 ) 3 +2H 2 O+N 2 (1)
3N 2 H 5 NO 3 +HNO 3 ＝4NH 4 NO 3 +N 2 (2)
In the hydrogenation catalytic reduction process disclosed in the patent, hydrogen gas as a reducing agent reacts as shown in equation (3) under the action of a catalyst, so that uranyl nitrate is catalytically reduced to uranium nitrate.
UO 2 (NO 3 ) 2 +HNO 3 +H 2 ＝U(OH)(NO 3 ) 3 +H 2 O (3)
Compared with hydrazine nitrate catalytic reduction, the hydrogen catalytic reduction has no side reaction, and the reducing agent H2 is excessive in the reaction process, so that the retention time of the reaction liquid in the reactor can be increased, the conversion rate of hexavalent uranium is ensured to be more than 98%, and the difficulty of process industrialization is reduced. In the process of preparing the tetravalent uranium by catalytic reduction of hexavalent uranium by hydrazine nitrate, if the thermal decomposition reaction (2) of the hydrazine nitrate is included, the conversion of the same molar quantity of uranyl nitrate almost consumes the same molar quantity of hydrazine and hydrogen, but the cost of each molar of hydrazine nitrate is nearly two orders of magnitude higher than that of the hydrogen, so the process is more economical.
Disclosure of Invention
The invention aims to provide a technological process for preparing tetravalent uranium.
In order to achieve the purpose, the invention provides a process for preparing uranium nitrate (tetravalent uranium) by catalytic hydrogenation reduction of uranyl nitrate (hexavalent uranium), which comprises the following steps that a mixed solution of uranyl nitrate and nitric acid in a raw material liquid storage tank and a high-pressure hydrogen storage tank are metered by a metering pump and a flowmeter and then enter a catalytic hydrogenation reactor, hexavalent uranium is catalytically reduced into tetravalent uranium under the action of a catalyst and high-pressure hydrogen, a gas-liquid mixture of product liquid and excessive hydrogen leaves the reactor, hydrazine nitrate or hydrazine is dripped on line and then enters a high-pressure gas-liquid separator 4 for gas-liquid separation, wherein the gas-phase mixture flows out from the top end of the separator, enters a tail gas absorption tower, NOx generated in the reaction process is absorbed and removed by alkali liquor, then is pressurized and circulated, then enters a high-pressure hydrogen storage tank for standby, and a liquid-phase product flows out from the bottom of the separator 4 and enters a product liquid-hydrogen replacement tower, after the liquid phase dissolved hydrogen in the tower is removed by nitrogen displacement, the gas phase enters a high-level discharge waste gas treatment system, and the liquid phase is used as a product to enter the next process.
The main reaction generated in the process is that uranyl nitrate reacts with hydrogen and nitric acid under the action of a catalyst to generate uranium nitrate, and the reaction is shown as a formula (3). In addition, during the reaction process, the reaction temperature and the reactor pressure need to be optimized to avoid the catalytic reduction of nitric acid to nitrous acid under the action of a catalyst, as shown in the reaction formula (4):
HNO 3 +H 2 ＝HNO 2 +H 2 O (4)
further decomposition of nitrous acid:
2HNO 2 ＝NO+NO 2 +H 2 O (5)
the nitrogen oxides formed in reaction (5) can poison the catalyst during the reaction.
Wherein the raw material liquid in the storage tank comprises the following components in percentage by mass: uranyl nitrate: 5% -40%; nitric acid: 1% -20%; water: balance of
The final mass concentration of hydrazine nitrate and/or hydrazine in the gas-liquid mixture after the online dropwise addition is 0-10% (preferably 1-5%, more preferably 1-3%).
Wherein the catalytic hydrogenation reactor can be one or more of fluidized bed, fixed bed or slurry bed with heat exchange jacket, and has an operation temperature of-20-100 deg.C and an operation pressure of 0.1-20MPa (gauge pressure), preferably 2-20MPa
Wherein the catalyst in the catalytic hydrogenation reactor can be prepared by loading one or more noble metals of Pt, Ru, Ir or Au on SiO 2 C or TiO 2 Of (a) one or more oxides (preferably SiO) 2 Or TiO 2 One or both) of noble metal supported on a carrier, wherein the noble metal loading is 0.01% to 10% (preferably 1% to 5%). Mixing uranyl nitrate in the raw material liquid storage tank with nitric acid, then enabling the mixed mixture and circulating hydrogen to enter a high-pressure hydrogenation reactor filled with a catalyst through one end of the reactor, catalytically reducing the uranyl nitrate into uranium nitrate by the hydrogen, and enabling excessive hydrogen and a product uranium nitrate to pass through the reactorThe other end of the reactor flows out of the reactor. The gas-liquid mixture is subjected to online dropwise addition of a hydrazine nitrate or hydrazine solution and then enters a high-pressure gas-liquid separator for separation, a gas phase is decompressed from the top of the separator and then enters a gas-phase tail gas washing tower, nitric oxide in the gas phase is absorbed and separated by alkali liquor, hydrogen is pressurized by a compressor and then enters a high-pressure hydrogen storage tank, a liquid-phase product is discharged from the bottom of the separator and enters a normal-pressure liquid-phase product hydrogen displacement tower, dissolved hydrogen in the liquid phase is removed in the tower by using a nitrogen bubbling device, so that the safety of a subsequent process is ensured, and the obtained gas enters a high-pressure tail gas treatment system.
Compared with the prior art, the invention has the substantial characteristics that:
1. compared with the method for preparing uranium nitrate by electrocatalytic reduction of uranyl nitrate, the conversion rate of hexavalent uranium can reach more than 98 percent;
2. compared with the method for preparing the uranium by catalytic reduction of hydrazine nitrate, the method avoids the occurrence of related side reactions and ensures that the conversion rate of the hexavalent uranium is more than 98%;
3. compared with the existing preparation process of tetravalent uranium, the method has the advantages of high conversion rate of the original gas, low cost of hydrogen and good economy.
Drawings
FIG. 1 is a process flow diagram of the present invention; wherein: 1. a raw material liquid storage tank; 2. a hydrogen gas storage tank; 3. a catalytic hydrogenation reactor; 4. a high pressure gas-liquid separation tank; 5. a reaction tail gas absorption tower; 6. a product liquid hydrogen gas replacement tower; 7. an alkali liquor storage tank.
Detailed Description
The adopted device comprises a raw material liquid storage tank, a hydrogen gas storage tank, a catalytic hydrogenation reactor, a high-pressure gas-liquid separation tank, a reaction tail gas absorption tower, a product liquid hydrogen displacement tower and an absorption alkali liquor storage tank;
metering a mixed solution of uranyl nitrate and nitric acid in a raw material liquid storage tank by a flowmeter, metering hydrogen in a high-pressure hydrogen storage tank by a metering pump, then feeding the mixed solution into a catalytic hydrogenation reactor, carrying out catalytic reduction on hexavalent uranium in uranyl nitrate into tetravalent uranium under the action of a supported noble metal catalyst and the hydrogen in the catalytic hydrogenation reactor, after a gas-liquid mixture of product liquid and excessive (corresponding to uranyl nitrate) hydrogen leaves the catalytic hydrogenation reactor, dropwise adding hydrazine nitrate and/or hydrazine on line, feeding the mixture into a high-pressure gas-liquid separator (with the operating pressure of 4MPa (gauge pressure)) for gas-liquid separation, wherein the gas-phase mixture flows out from the top end of the separator, enters a reaction tail gas absorption tower, absorbs and removes NOx (X is 1-2) generated in the reaction process by alkali liquor (sodium hydroxide with the alkali liquor of 3M), then carries out pressure circulation, and then rubs the mixture and returns to a hydrogen storage tank for circulation, and the liquid-phase product flows out from the bottom of the gas-liquid separator and enters a product liquid-hydrogen gas displacement tower, the gas phase enters a high-level discharge waste gas treatment system after the liquid-phase dissolved hydrogen in the tower is removed by nitrogen displacement, and the liquid-phase product is the product.
The top in the reaction tail gas absorption tower is equipped with alkali lye shower nozzle, and the shower nozzle passes through the pump and links to each other with the alkali lye storage tank through the pipeline, and reaction tail gas absorption tower bottom is equipped with the alkali lye return line who links to each other with the alkali lye storage tank.
And a tail gas discharge port is arranged at the top of the liquid hydrogen displacement tower. And a tail gas discharge port with a valve is arranged at the top of the reaction tail gas absorption tower.
Example 1
The treatment capacity of the reaction solution was 62.5kg/h, and UO in the stock solution tank 2 (NO 3 ) 2 Is 0.31 (31%) by mass, HNO 3 The content was 0.1 (10%) and H 2 The O content is 0.59 (59%), and the concentration of hexavalent uranium is 208 g/L; after hydrazine nitrate is dripped on line, the final mass content of the hydrazine nitrate in the high-pressure gas-liquid separation tank is ensured to be 2%; the catalyst is Pt/SiO with the average grain diameter of 100 microns 2 (noble metal loading 1%). The reactor is a fluidized bed reactor. The flow rate of hydrogen was 180Nm 3 The temperature of the reactor is 30 ℃, the pressure is 4.0Mpa (gauge pressure), the conversion rate of the export uranyl nitrate is 98%, and the content of tetravalent uranium in the product liquid is 204 g/L.
Example 2
The difference from example 1 (the rest and the process are the same as those) is that UO in the stock solution tank 2 (NO 3 ) 2 0.20 (20%) HNO 3 The content was 0.1 (10%) and H 2 The O content is 0.7 (70%), the concentration of hexavalent uranium is 134.2g/L, and the conversion rate of export uranyl nitrate is 98Percent, the content of the tetravalent uranium in the product liquid is 131.5 g/L.
Example 3
The difference from example 2 is that (the rest and the process are the same as) UO in stock solution storage tank 2 (NO 3 ) 2 Is HNO 3 The content was 0.2 (20%) and H 2 The O content is 0.6 (60%), the concentration of hexavalent uranium is 134.2g/L, the conversion rate of export uranyl nitrate is 98.1%, and the content of tetravalent uranium in a product liquid is 132 g/L.
Example 4
The difference from the embodiment 2 is that the final mass content of the hydrazine nitrate in the high-pressure gas-liquid separation tank is ensured to be 1 percent; the conversion rate of the exported uranyl nitrate is 98 percent, and the content of tetravalent uranium in the product liquid is 131.5 g/L.
Example 5
The difference from the embodiment 2 is that (the rest and the process are the same as the above process) hydrazine nitrate and hydrazine are dripped on line, so that the final mass content of the hydrazine nitrate and the hydrazine in the high-pressure gas-liquid separation tank is ensured to be 5%; the conversion rate of the export uranyl nitrate is 98.1 percent, and the content of tetravalent uranium in the product liquid is 132 g/L.
Example 6
The difference from the example 2 is that (the rest and the process are the same as) the temperature of the reactor is-20 ℃, the pressure is 2.0Mpa (gauge pressure), the conversion rate of the export uranyl nitrate is 98.1%, and the content of the tetravalent uranium in the product liquid is 132 g/L.
Example 7
The difference from the example 2 is that (the rest and the process are the same as) the temperature of the reactor is-20 ℃, the pressure is 8.0MPa (gauge pressure), the conversion rate of the export uranyl nitrate is 98.1 percent, and the content of the tetravalent uranium in the product liquid is 132 g/L.
Example 8
The difference from the example 2 is that (the rest and the process are the same as) the temperature of the reactor is 40 ℃, the pressure is 20.0Mpa (gauge pressure), the conversion rate of the export uranyl nitrate is 98%, and the content of the tetravalent uranium in the product liquid is 131.5 g/L.
Comparative example 1
The difference from example 1 is that (the rest and the process are the same as) the reaction temperature is 60 ℃, the conversion rate of the export uranyl nitrate is 90%, the content of the tetravalent uranium in the product liquid is 188g/L, but reaction (5) is carried out due to the higher temperature in the reaction process, and the activity of the catalyst is obviously reduced in a shorter time due to the generation of a large amount of nitrogen oxides.
Comparative example 2
Compared with the embodiment 1, the difference lies in that after the online dropwise addition of the rest components (the same as the process), the final mass content of hydrazine nitrate in the high-pressure gas-liquid separation tank is ensured to be 0.1%, the conversion rate of the export uranyl nitrate is 98%, the content of tetravalent uranium in the product liquid is 120g/L, and the tetravalent uranium generated after leaving the reactor is further oxidized into hexavalent uranium by nitric acid;
comparative example 3
The difference compared to example 1 is that (the rest and the process are the same) UO is present in the stock solution reservoir 2 (NO 3 )2 mass content of 0.31 (31%), HNO 3 The content was 0.02 (2%) and H 2 The O content is 0.67 percent (67 percent), the conversion rate of the output uranyl nitrate is 75 percent due to insufficient concentration of nitric acid in the conversion process, and the content of tetravalent uranium in the product liquid is 156 g/L;
comparative example 4
Compared with example 1, it differs in that (the rest and the process are the same as) the catalyst is Pt/Al with an average particle size of 100 microns 2 O 3 (noble metal loading is 1%), the conversion rate of the exported uranyl nitrate is 98%, the content of tetravalent uranium in the product liquid is 204g/L, but the conversion rate of the uranyl nitrate is obviously reduced along with the progress of the reaction due to the dissolution of alumina in the reaction process.
Claims (8)
1. A method for preparing uranium nitrate by reducing uranyl nitrate through catalytic hydrogenation,
the adopted device comprises a raw material liquid storage tank, a hydrogen gas storage tank, a catalytic hydrogenation reactor, a high-pressure gas-liquid separation tank, a reaction tail gas absorption tower, a product liquid hydrogen displacement tower and an absorption alkali liquor storage tank;
metering a mixed solution of uranyl nitrate and nitric acid in a raw material liquid storage tank (1) by a flowmeter, metering hydrogen in a high-pressure hydrogen storage tank (2) by a metering pump, then feeding the hydrogen into a catalytic hydrogenation reactor (3), catalytically reducing hexavalent uranium in uranyl nitrate into tetravalent uranium under the action of a supported noble metal catalyst and hydrogen in the catalytic hydrogenation reactor (3), after a product liquid and a gas-liquid mixture of hydrogen which is excessive relative to uranyl nitrate leave the catalytic hydrogenation reactor, dropwise adding hydrazine nitrate and/or hydrazine on line, feeding the mixture into a high-pressure gas-liquid separator (4) for gas-liquid separation, wherein the gas-phase mixture flows out from the top end of the separator, enters a reaction tail gas absorption tower, NOx generated in the reaction process is absorbed and removed by alkali liquor, is subjected to pressure circulation, and then returns to enter a hydrogen gas storage tank for circulation and standby, wherein X in the NOx is 1-2, and a liquid-phase product flows out from the bottom of the gas-liquid separator (4) and enters a product liquid-hydrogen gas displacement tower (6), after liquid-phase dissolved hydrogen in the tower is removed by nitrogen displacement, the gas phase enters a high-level discharge waste gas treatment system and is directly discharged, and a liquid-phase product is a product;
wherein the raw material liquid in the raw material liquid storage tank (1) comprises the following components in percentage by mass: uranyl nitrate: 5% -40%; nitric acid: 5% -20%; the balance of water;
and (2) dropwise adding hydrazine nitrate and/or hydrazine on line, wherein the final mass concentration of the hydrazine nitrate and/or hydrazine in the dropwise added mixture is 1-10%.
2. The process according to claim 1, wherein the catalytic hydrogenation reactor (3) is one or more of a fluidized bed with a heat exchange jacket, a fixed bed or a slurry bed, and the operating temperature is-20 to 50 ℃ and the operating pressure is 0.1 to 20 Mpa;
the treatment capacity of the reaction solution is 62.5kg/h, and the flow rate of the hydrogen is 160-240Nm 3 /h。
3. The process of claim 1 wherein the catalyst in the catalytic hydrogenation reactor is supported on SiO by one or more noble metals of Pt, Ru, Ir, or Au 2 C or TiO 2 Wherein the noble metal loading is 0.01% to 10%.
4. The method of claim 1, wherein the alkaline solution is 1-5M sodium hydroxide.
5. The process according to claim 1, wherein the high pressure gas-liquid separator (4) is operated at a pressure of 0.1 to 20Mpa gauge.
6. The method of claim 1, wherein an alkali liquor spray head is arranged at the top in the reaction tail gas absorption tower, the alkali liquor spray head is connected with an alkali liquor storage tank (7) through a pipeline via a pump, and an alkali liquor return pipeline connected with the alkali liquor storage tank (7) is arranged at the bottom of the reaction tail gas absorption tower.
7. The method of claim 1, wherein the top of the liquid hydrogen displacement column (6) is provided with a tail gas discharge port.
8. The method according to claim 1, characterized in that the feed liquid in the feed liquid storage tank (1) comprises the following components in percentage by mass: uranyl nitrate: 20% -35%; nitric acid: 8% -20%; the balance of water; dropping hydrazine nitrate and/or hydrazine on line, wherein the final mass concentration of the hydrazine nitrate and/or hydrazine in the mixture after dropping is 1-5%;
the loading amount of the noble metal in the catalyst is 1-5%;
the operation temperature of the catalytic hydrogenation reactor (3) is 20-40 ℃, the operation pressure is 2-8Mpa, and the flow rate of hydrogen is 180-200Nm 3 /h；
The operating pressure of the high-pressure gas-liquid separator (4) is 2-8 Mpa.
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| CN115522081B (en) * | 2022-09-26 | 2023-10-20 | 核工业北京化工冶金研究院 | Method for preparing uranium oxide product from alkaline uranium qualified liquid |
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