CN114570289B - Fixed bed catalytic reactor and application thereof in removal of hydrazine nitrate and hydroxylamine nitrate - Google Patents
Fixed bed catalytic reactor and application thereof in removal of hydrazine nitrate and hydroxylamine nitrate Download PDFInfo
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- CN114570289B CN114570289B CN202011392431.9A CN202011392431A CN114570289B CN 114570289 B CN114570289 B CN 114570289B CN 202011392431 A CN202011392431 A CN 202011392431A CN 114570289 B CN114570289 B CN 114570289B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
- C01B21/46—Purification; Separation ; Stabilisation
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
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- 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
Abstract
The application discloses a fixed bed catalytic reactor and application of the fixed bed catalytic reactor in removing a small amount of hydrazine nitrate and hydroxylamine nitrate in nitric acid. The fixed bed catalytic reactor comprises a shell, a feed liquid distribution plate and a feed liquid conveying core pipe, wherein the shell is enclosed to form a cavity; the top of the shell is provided with a feed liquid inlet and a product outlet; the feed liquid distribution plate is positioned at the inner lower part of the cavity; the feed liquid conveying core pipe is positioned in the cavity; the upper end of the feed liquid conveying core pipe is communicated with the feed liquid inlet; the lower end of the feed liquid conveying core pipe penetrates through the feed liquid distribution plate and is located above the bottom of the shell. By utilizing the reactor, the preheated feed liquid is decomposed into nitrogen, hydrogen and water by hydrazine nitrate and hydroxylamine nitrate under the action of the supported ruthenium catalyst, so that the treatment of the nuclear power waste liquid can be safely and efficiently carried out.
Description
Technical Field
The application relates to a fixed bed catalytic reactor and application thereof in removal of hydrazine nitrate and hydroxylamine nitrate, belonging to the field of nuclear power waste treatment and environmental protection.
Background
Nuclear power is a green low-carbon clean energy with high technical maturity, and is an important preferred technical route for solving energy problems for human beings in the future. However, the safety problem of the strongly radioactive waste, namely the spent fuel, is one of the main factors restricting the large-scale popularization and application of nuclear power. The nuclear reactor nuclear fuel has low overall utilization rate, spent fuel containing unconverted uranium is an important nuclear element resource, and at present, a nuclear fuel closed circulation route is adopted to separate, purify and further utilize nuclear elements such as uranium, plutonium and neptunium in the spent fuel. For example, PUREX procedure: dissolving spent fuel rods by nitric acid, extracting tributyl phosphate and n-dodecane organic diluent, and reducing and back-extracting by reducing agents such as hydrazine nitrate and/or hydroxylamine nitrate to realize separation, purification and enrichment of nuclear elements. In the process, a large amount of nitric acid waste liquid containing hydrazine nitrate and hydroxylamine nitrate is generated, according to the principle of minimizing radioactive waste after spent fuel post-treatment, the waste liquid needs to recycle nitric acid in the subsequent process, and the distilled residue is subjected to vitrification solidification and deep burying treatment. Hydrazine nitrate and hydroxylamine nitrate have strong reducibility, are easily oxidized and explosive substances with high energy content, and need to be removed in order to eliminate the explosion risk in the concentration treatment process of the waste liquid. The method for removing hydrazine nitrate and hydroxylamine nitrate mainly comprises the steps of adding an oxidant such as sodium nitrite or introducing dinitrogen tetroxide gas and the like to oxidize the hydrazine nitrate, the hydroxylamine nitrate and the like into nitrogen, water, nitrogen oxides and other products for removal, and has the defects that: the consumption of the oxidant is high, the cost is high, the reaction is severe, and certain safety risk exists; when sodium nitrite is used as an oxidant, new solid waste sodium nitrate is easily generated; the nitrogen dioxide utilization is low and there is a risk of leakage. The ruthenium-based catalyst can decompose hydrazine nitrate and hydroxylamine nitrate into nitrogen, ammonia, hydrogen and water, a large amount of gas is released in the reaction, the gas flows disorderly in the reaction liquid, the contact of solid and liquid (the catalyst and the feed liquid) is damaged, and the reaction is very insufficient.
Disclosure of Invention
Aiming at the problems in the waste liquid treatment process, the application discloses a ruthenium-based catalyst-based catalytic reactor for removing hydrazine nitrate and hydroxylamine nitrate in nitric acid, which can efficiently, safely, economically and environmentally realize the recovery treatment of spent fuel.
The method utilizes ruthenium-based catalyst to catalytically decompose hydrazine nitrate and hydroxylamine nitrate in feed liquid into nitrogen, ammonia, hydrogen and water in a fixed bed mode, thereby achieving the purpose of removal, and the reaction equation is as follows:
according to one aspect of the present application, a fixed bed catalytic reactor is provided.
A fixed bed catalytic reactor comprises a shell, a feed liquid distribution plate and a feed liquid conveying core pipe, wherein the shell is enclosed to form a cavity;
the top of the shell is provided with a feed liquid inlet and a product outlet;
the feed liquid distribution plate is positioned at the inner lower part of the cavity;
the feed liquid conveying core pipe is positioned in the cavity;
the upper end of the feed liquid conveying core pipe is communicated with the feed liquid inlet;
the lower end of the feed liquid conveying core pipe penetrates through the feed liquid distribution plate and is located above the bottom of the shell.
The feed liquid enters the bottom of the shell through the feed liquid inlet and the feed liquid conveying core pipe and then passes through the feed liquid distribution plate and can be fully contacted with the catalyst bed layer, the feed liquid passes through the catalyst bed layer from bottom to top, so that gas generated after reaction quickly flows out of the catalyst bed layer, the gas and the feed liquid are not interfered with each other, the feed liquid can be fully contacted with the catalyst, and the reaction is complete.
The feed liquid inlet and the product outlet are positioned at the same side, and an upper feeding and discharging mode is adopted, so that the device is safer and more economical.
Optionally, a sieve plate is arranged above the inside of the shell;
and a spring is arranged on the sieve plate.
Specifically, one end of the spring contacts the screen plate and the other end contacts the top of the housing.
The spring and the sieve plate can compact the catalyst bed layer together to prevent the catalyst bed from loosening, and the whole catalyst bed can be stabilized due to the elasticity of the spring.
Optionally, the housing comprises a reactor end cap and a catalyst packing cartridge;
the reactor end cover is hermetically connected with the catalyst filling cylinder.
Optionally, the end cover of the reactor and the catalyst filling cylinder are hermetically connected by adopting a flange structure, and the sealing element is made of fluororubber.
Optionally, the reactor end cap has an inner diameter of 140 to 160mm and a height of 25 to 35mm.
Specifically, the reactor end cap is 304 stainless steel.
Optionally, the feed liquid inlet and the product outlet are both disposed in the end cap of the reactor.
Optionally, the inner diameter of the catalyst filling cylinder is consistent with the inner diameter of the end cover of the reactor, and the height of the cylinder is 160-200 mm.
Specifically, the catalyst filling cylinder is made of 304 stainless steel. The inner diameter of the cylinder is 140-160 mm, which is consistent with the inner diameter of the end cover.
Optionally, the drift diameter of the feed liquid inlet is 6-10 mm.
Specifically, the material of the feed liquid inlet is 304 stainless steel material.
Optionally, the feed liquid conveying core pipe is a hollow pipe, the inner diameter of the hollow pipe is 4-6 mm, the outer diameter of the hollow pipe is 10-12 mm, and the length of the hollow pipe is 200-300 mm.
Optionally, the feed liquid conveying core pipe is positioned at the axial center of the reactor.
Specifically, the material of the feed liquid conveying core pipe is 304 stainless steel.
One end of the feed liquid conveying core pipe is connected with the feed liquid inlet, and the other end of the feed liquid conveying core pipe is arranged at the bottom of the reactor and used for conveying feed liquid.
Optionally, the feed liquid distribution plate is a multilayer sintered net, the thickness of the feed liquid distribution plate is 1-2 mm, and the filtering precision of the feed liquid distribution plate is 40-80 meshes.
Optionally, the wire diameter of the compression spring is 2-4 mm, and the maximum working stroke is not less than 10mm.
Specifically, the material of the compression spring is 304 stainless steel material. The compression spring is matched with the sieve plate and used for compressing the catalyst bed layer.
Optionally, the drift diameter of the product outlet is 10-12 mm.
Specifically, the material of the product outlet is 304 stainless steel material.
Optionally, the fixed bed catalytic reactor is wholly wrapped with heat insulation cotton; the thickness of the heat-insulating layer is 50-80 mm.
Optionally, the thickness of the insulating layer is not less than 50mm.
Specifically, the heat preservation cotton is made of aluminum silicate.
Optionally, the screen plate may be a screen plate or a mesh, and is made of 304 stainless steel.
Optionally, the fixed bed catalytic reactor comprises a reactor end cap and a catalyst packing cartridge;
the reactor end cover is hermetically connected with the catalyst filling cylinder;
the upper part of the catalyst filling cylinder is provided with a sieve plate, and the lower part of the catalyst filling cylinder is provided with a feed liquid distribution plate;
the reactor end cover is provided with a feed liquid inlet, the feed liquid inlet is connected with a feed liquid conveying core pipe, and the feed liquid conveying core pipe penetrates through the sieve plate and the feed liquid distribution plate until the bottom of the catalyst filling cylinder is approached.
As a specific embodiment, the fixed bed catalytic reactor comprises:
the device comprises a feed liquid inlet (1), a reactor end cover (2), a compression spring (3), a feed liquid conveying core pipe (4), a catalyst filling cylinder (5), a feed liquid distribution plate (6), heat-insulating cotton (7), a stainless steel sieve plate (8) and a product outlet (9);
the top of the reactor end cover (2) is provided with a feed liquid inlet (1) and a product outlet (9), and the catalyst filling cylinder (5) is used for filling the catalyst and is hermetically connected with the reactor end cover (2) through a flange. The catalyst bed layer is pressed by a stainless steel sieve plate (8) through a pressing spring (3). The feed liquid inlet (1) is used for inputting feed liquid, the feed liquid is conveyed to the bottom of the catalyst filling cylinder (5) through the feed liquid conveying core pipe (4) on the axis of the reaction area, the feed liquid is uniformly distributed by the feed liquid distribution plate (6) and is applied to the bottom of the catalyst bed layer from bottom to top, the feed liquid is contacted with the catalyst to carry out catalytic reaction, and a product is discharged from the product outlet (9) after passing through the stainless steel sieve plate (8). The outside of the reactor is wholly wrapped with heat insulation cotton (7).
According to a second aspect of the present application, a method for removing hydrazine nitrate and hydroxylamine nitrate from nitric acid is provided.
A method for removing hydrazine nitrate and hydroxylamine nitrate in nitric acid adopts the fixed bed catalytic reactor.
Optionally, a feed liquid containing hydrazine nitrate, hydroxylamine nitrate and nitric acid is conveyed to the bottom of the shell through a feed liquid inlet and a feed liquid conveying core pipe, the feed liquid is uniformly distributed by a feed liquid distribution plate and then applied to a catalyst bed layer from bottom to top, the feed liquid is contacted with a catalyst to perform catalytic reaction, and a product is discharged through a product outlet.
Optionally, in the feed liquid, the concentration of the nitric acid is 0.5-2.0 mol/L; the concentration of the hydrazine nitrate is 0.1-0.5 mol/L; the concentration of the hydroxylamine nitrate is 0.1-0.5 mol/L.
Optionally, the concentration of nitric acid in the feed liquid is 1.0mol/L; the concentration of the hydrazine nitrate is 0.1mol/L; the concentration of hydroxylamine nitrate was 0.3mol/L.
The feed liquid treated by the method is a solution for treating nuclear power waste, and inevitably contains a very small amount of nuclear elements. The feed solution, as used herein, contains 0.06g/L of hexavalent uranium.
Optionally, the catalyst is loaded into a catalyst loading cartridge; the catalyst is a load type ruthenium-based catalyst, the granularity is 4-8 meshes, porous active carbon is used as a carrier, and the load capacity of ruthenium is 1-5 wt%.
In the present application, the supported ruthenium-based catalyst can be selected from the prior art.
Alternatively, the operating conditions of the fixed-bed catalytic reactor are: the preheating temperature of the feed liquid is 60-95 ℃; the flow rate of the feed liquid is 0.02-4.0L/min.
Optionally, the pre-heating temperature is independently selected from any value of 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ or a range value between any two.
Optionally, the flow rate of the feed liquid is independently selected from any of 0.02L/min, 0.03L/min, 0.04L/min, 0.05L/min, 0.06L/min, 0.07L/min, 0.08L/min, 0.1L/min, 0.15L/min, 0.2L/min, 0.5L/min, 1L/min, 1.5L/min, 2L/min, 2.5L/min, 3L/min, 3.5L/min, 4L/min, or a range between any two thereof.
Optionally, a feed liquid containing hydrazine nitrate, hydroxylamine nitrate and nitric acid is conveyed to the bottom of the catalyst filling cylinder through a feed liquid inlet and a feed liquid conveying core pipe, is uniformly distributed by a feed liquid distribution plate from bottom to top and is applied to the bottom of a catalyst bed layer in the catalyst filling cylinder, the feed liquid is contacted with the catalyst to perform catalytic reaction, and a product is discharged through a product outlet.
As a specific implementation mode, the method comprises the following steps:
introducing feed liquid preheated to above 60-95 ℃, wherein the feed liquid comprises 0.5-2.0 mol/L nitric acid, 0.1-0.5 mol/L hydrazine nitrate and 0.1-0.5 mol/L hydroxylamine nitrate. The flow rate of the feed liquid is 0.02-4.0L/min, the catalytic reaction is started to continuously treat the feed liquid, and effluent liquid of a product outlet is taken to detect the contents of hydrazine nitrate and hydroxylamine nitrate.
A catalyst filling cylinder 5 is taken, a feed liquid distribution plate 6 and a feed liquid conveying core pipe 4 are sequentially installed, ruthenium-based catalysts with 4-8 mesh particle sizes are filled, and a stainless steel sieve plate 8, a compression spring 3 and a reactor end cover 2 are installed. The feed liquid input pipe and the product transmission pipe are respectively connected with the feed liquid inlet 1 and the product outlet 9 in a sealing way by clamping sleeves.
The beneficial effects that this application can produce include:
1) The fixed bed catalytic reactor provided by the application is cleaner and more environment-friendly in a mode of treating hydrazine nitrate and hydroxylamine nitrate based on the catalytic decomposition of a ruthenium-based catalyst compared with a traditional mode of adding an oxidant, and has no potential safety hazard.
2) According to the fixed bed catalytic reactor provided by the application, the working mode of the reactor is that a certain amount of catalyst is put in once to carry out removal, and the economic efficiency of the fixed bed catalytic reactor is superior to that of a mode of continuously adding an oxidant.
3) The fixed bed catalytic reactor provided by the application adopts a fixed bed continuous working mode, is simple to operate, is flexible and convenient, and can be efficiently connected with a subsequent treatment process.
Drawings
FIG. 1 is a sectional view of a fixed bed catalytic reactor.
Wherein, 1-feed liquid inlet 2-reactor end cover 3-compression spring
4-feed liquid conveying core pipe 5-catalyst filling cylinder 6-feed liquid distribution plate
7-heat preservation cotton 8-stainless steel sieve plate 9-product outlet
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Unless otherwise specified, the raw materials in the examples of the present application were purchased commercially, and if not specified, the test methods were performed by the conventional methods, and the equipment settings were the settings recommended by the manufacturers.
Wherein the catalyst is a supported ruthenium-based catalyst, the granularity is 4-8 meshes, porous activated carbon is used as a carrier, the ruthenium loading is 5wt%, and the preparation method is an impregnation method.
The analysis method in the examples of the present application is as follows:
and (3) testing and analyzing the contents of the solution hydrazine nitrate and hydroxylamine nitrate after the reaction by using a potentiometric titration method.
As shown in fig. 1. The reactor is designed in a fixed bed mode and comprises a material liquid inlet, a reactor end cover, a compression spring, a material liquid conveying core pipe, a catalyst filling cylinder, a material liquid distribution plate, heat preservation cotton, a stainless steel sieve plate and a product outlet.
As shown in figure 1, a feed liquid inlet 1 and a product outlet 9 are arranged at the top of a reactor end cover 2, a catalyst filling cylinder 5 is used for filling a catalyst and is connected with the reactor end cover 2 in a sealing way through a flange, and the sealing piece is made of fluororubber. The catalyst bed layer is pressed by a stainless steel sieve plate 8 through a pressing spring 3. The feed liquid inlet 1 is used for feeding feed liquid, the feed liquid is conveyed to the bottom of the catalyst filling cylinder 5 through the feed liquid conveying core pipe 4 on the axis of the reaction zone, the feed liquid is uniformly distributed to the bottom of the catalyst bed layer from bottom to top through the feed liquid distribution plate 6, the feed liquid is contacted with the catalyst to perform catalytic reaction, and a product is discharged from the product outlet 9 after passing through the stainless steel sieve plate 8. The outside of the reactor is wholly wrapped with heat insulation cotton 7.
In the examples, the parameters of the components comprised by the fixed-bed catalytic reactor are specified below:
the drift diameter of the feed liquid inlet is 6mm;
the inner diameter of the end cover of the reactor is 150mm, and the height of the end cover of the reactor is 30mm;
the wire diameter of the compression spring is 3mm, and the maximum working stroke is not less than 10mm;
the feed liquid conveying core pipe is a hollow pipe, the inner diameter of the hollow pipe is 6mm, the outer diameter of the hollow pipe is 10mm, and the length of the hollow pipe is 260mm;
the inner diameter of the catalyst filling cylinder is consistent with the inner diameter of the end cover of the reactor, and the cylinder height is 180mm;
the feed liquid distribution plate is a multilayer sintered net, the thickness is 2mm, and the filtering precision is 80 meshes;
the drift diameter of the product outlet is 10mm.
The materials of the parts are all 304 stainless steel.
The heat preservation cotton is made of aluminum silicate and has the thickness of 60mm.
Example 1
Weighing 700g of catalyst, placing the catalyst in a catalyst filling cylinder (5), covering a stainless steel sieve plate (8) above the feed liquid distribution plate (6), compacting the catalyst by using a compression spring, covering an end cover of the reactor, and screwing. Preheating feed liquid containing 0.3mol/L hydroxylamine nitrate, 0.1mol/L hydrazine nitrate, 1.0mol/L nitric acid and 0.06g/L hexavalent uranium to 60 ℃, pumping the feed liquid into a reactor for reaction through a feed liquid port (1) at the flow rate of 50mL/min, enabling the solution after reaction to flow out of a product outlet (9), and measuring the content of the hydrazine nitrate and the hydroxylamine nitrate in the solution after reaction to be 0.0002mol/L and 0.000005mol/L respectively.
Example 2
Weighing 700g of catalyst, placing the catalyst in a catalyst filling cylinder (5), covering a stainless steel sieve plate (8) above a feed liquid distribution plate (6), compacting the catalyst by using a compression spring, covering an end cover of a reactor, and screwing. Preheating feed liquid containing 0.3mol/L hydroxylamine nitrate, 0.1mol/L hydrazine nitrate, 1.0mol/L nitric acid and 0.06g/L hexavalent uranium to 80 ℃, pumping the feed liquid into a reactor for reaction through a feed liquid port (1) at the flow rate of 50mL/min, enabling the solution after the reaction to flow out of a product outlet (9), and measuring the content of the hydrazine nitrate in the solution after the reaction to be 0.00001mol/L and the content of hydroxylamine nitrate to be 0.000008mol/L.
Example 3
Weighing 700g of catalyst, placing the catalyst in a catalyst filling cylinder (5), covering a stainless steel sieve plate (8) above a feed liquid distribution plate (6), compacting the catalyst by using a compression spring, covering an end cover of a reactor, and screwing. Preheating feed liquid containing 0.3mol/L hydroxylamine nitrate, 0.1mol/L hydrazine nitrate, 1.0mol/L nitric acid and 0.06g/L hexavalent uranium to 60 ℃, pumping the feed liquid into a reactor for reaction through a feed liquid port (1) at the flow rate of 70mL/min, allowing the reacted solution to flow out of a product outlet (9), and measuring the content of the hydrazine nitrate in the reacted solution to be 0.0004mol/L and the content of the hydroxylamine nitrate to be 0.000009mol/L.
Example 4
Weighing 700g of catalyst, placing the catalyst in a catalyst filling cylinder (5), covering a stainless steel sieve plate (8) above the feed liquid distribution plate (6), compacting the catalyst by using a compression spring, covering an end cover of the reactor, and screwing. Feed liquid containing 0.3mol/L hydroxylamine nitrate, 0.1mol/L hydrazine nitrate, 1.0mol/L nitric acid and 0.06g/L hexavalent uranium is preheated to 90 ℃, the feed liquid is pumped into a reactor for reaction through a feed liquid port (1) at the flow rate of 50mL/min, the solution after the reaction flows out from a product outlet (9), and the contents of the hydrazine nitrate and the hydroxylamine nitrate in the solution after the reaction are not detected.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (8)
1. A method for removing hydrazine nitrate and hydroxylamine nitrate in nitric acid is characterized in that,
a fixed bed catalytic reactor is adopted;
the fixed bed catalytic reactor comprises a shell, a feed liquid distribution plate and a feed liquid conveying core pipe, wherein the shell is enclosed to form a cavity;
the top of the shell is provided with a feed liquid inlet and a product outlet;
the feed liquid distribution plate is positioned at the inner lower part of the cavity;
the feed liquid conveying core pipe is positioned in the cavity;
the upper end of the feed liquid conveying core pipe is communicated with the feed liquid inlet;
the lower end of the feed liquid conveying core pipe penetrates through the feed liquid distribution plate and is positioned above the bottom of the shell;
a sieve plate is arranged at the inner upper part of the shell;
a spring is arranged on the sieve plate;
the method comprises the following steps:
a feed liquid containing hydrazine nitrate, hydroxylamine nitrate and nitric acid is conveyed to the bottom of the shell through a feed liquid inlet and a feed liquid conveying core pipe, is uniformly distributed by a feed liquid distribution plate and then is applied to a catalyst bed layer from bottom to top, the feed liquid contacts with a catalyst to generate catalytic reaction, and a product is discharged through a product outlet;
in the feed liquid, the concentration of nitric acid is 0.5 to 2.0mol/L; the concentration of the hydrazine nitrate is 0.1 to 0.5mol/L; the concentration of hydroxylamine nitrate is 0.1 to 0.5mol/L;
the catalyst is a supported ruthenium-based catalyst, the granularity is 4 to 8 meshes, porous active carbon is used as a carrier, and the ruthenium loading is 1 to 5wt%;
the working conditions of the fixed bed catalytic reactor are as follows: the preheating temperature of the feed liquid is 60 to 95 ℃; the flow rate of the feed liquid is 0.02 to 4.0L/min.
2. The method of claim 1, wherein the housing comprises a reactor end cap and a catalyst loading cartridge;
the reactor end cover is hermetically connected with the catalyst filling cylinder;
the inner diameter of the end cover of the reactor is 140-160 mm, and the height of the end cover of the reactor is 25-35 mm.
3. The method as claimed in claim 1, wherein the inside diameter of the catalyst filling cylinder is consistent with the inside diameter of the reactor end cap, and the cylinder height is 160 to 200mm.
4. The method according to claim 1, wherein the drift diameter of the feed liquid inlet is 6 to 10mm;
the drift diameter of the product outlet is 10 to 12mm.
5. The method according to claim 1, wherein the feed liquid conveying core pipe is a hollow pipe, the inner diameter of the hollow pipe is 4 to 6mm, the outer diameter of the hollow pipe is 10 to 12mm, and the length of the hollow pipe is 200 to 300mm.
6. The method according to claim 1, wherein the feed liquid distribution plate is a multilayer sintered net, the thickness of the multilayer sintered net is 1-2mm, and the filtering precision is 40-80 meshes.
7. The method of claim 1, wherein the spring is a compression spring; the wire diameter of the compression spring is 2-4 mm, and the maximum working stroke is not less than 10mm.
8. The method according to claim 1, wherein the fixed bed catalytic reactor is externally and integrally wrapped with heat insulation cotton; the thickness of the heat insulation cotton is 50-80 mm.
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| JP2556221B2 (en) * | 1991-10-04 | 1996-11-20 | 動力炉・核燃料開発事業団 | Oxidation method of trivalent plutonium to tetravalent plutonium |
| CN105457564B (en) * | 2015-08-31 | 2018-02-16 | 张淮海 | Multistage indirect heat exchange radial fixed-bed reactor |
| CN106554806B (en) * | 2015-09-25 | 2018-08-10 | 中国石油天然气股份有限公司 | Bulk bed reactor and heavy oil lightening method |
| CN107519823B (en) * | 2016-06-21 | 2019-05-10 | 中国石化工程建设有限公司 | A kind of subregion radial reactor |
| CN106311092B (en) * | 2016-11-02 | 2020-05-19 | 中国原子能科学研究院 | Catalytic device for preparing U (IV) solution |
| CN111013495B (en) * | 2018-10-10 | 2022-03-11 | 中国石油化工股份有限公司 | Intersegment feeding structure of multi-section fixed bed reactor, multi-section fixed bed reactor and application of intersegment feeding structure |
| CN111249999A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Fixed bed reactor for catalytic reduction of hexavalent uranium by hydrazine nitrate and application |
| CN210332604U (en) * | 2019-08-07 | 2020-04-17 | 华东理工大学 | Radial flow heat exchange type fixed bed catalytic reactor |
| CN111871336A (en) * | 2020-08-21 | 2020-11-03 | 中国海洋石油集团有限公司 | Low-carbon alkane reforming reaction device and synthesis gas equipment |
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