CN113720763A - Experimental device for simulating spent fuel aftertreatment boiling nitric acid corrosive wear - Google Patents

Experimental device for simulating spent fuel aftertreatment boiling nitric acid corrosive wear Download PDF

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Publication number
CN113720763A
CN113720763A CN202110930819.8A CN202110930819A CN113720763A CN 113720763 A CN113720763 A CN 113720763A CN 202110930819 A CN202110930819 A CN 202110930819A CN 113720763 A CN113720763 A CN 113720763A
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China
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kettle body
nitric acid
corrosive wear
sample
pressure head
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CN202110930819.8A
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Chinese (zh)
Inventor
张连民
刘政
郑玉贵
任德春
马爱利
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Priority to CN202110930819.8A priority Critical patent/CN113720763A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/02Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement

Abstract

The invention relates to the field of nitric acid corrosive wear devices, in particular to an experimental device for simulating boiling nitric acid corrosive wear in spent fuel aftertreatment. The device is provided with a corrosive wear test system, a supporting system, a transmission system, an electrochemical test system, a liquid level control system, a condensation and tail gas treatment system and an electric control system. During the experiment, the sample is connected with an external electrochemical workstation through a lead, nitric acid is injected into the polytetrafluoroethylene kettle body, and a mechanical arm of a transmission system drives a glass pressure head fixed on the polytetrafluoroethylene fixture to rub in a reciprocating manner on the surface of the sample, so that the corrosive wear simulation test is realized. The invention can simulate the real working condition of spent fuel post-treatment, research the corrosive wear behavior of the material in the post-treatment boiling nitric acid, accurately control the parameters of the nitric acid solution such as temperature, friction speed, friction stroke and the like, and realize the switching of different corrosive wear forms and the online electrochemical test and the weightlessness test of corrosive wear samples.

Description

Experimental device for simulating spent fuel aftertreatment boiling nitric acid corrosive wear
Technical Field
The invention relates to the field of nitric acid corrosive wear devices, in particular to an experimental device for simulating boiling nitric acid corrosive wear in spent fuel aftertreatment.
Background
In the spent fuel post-treatment process, part of post-treatment key equipment operates under the combined action of nitric acid corrosion and mechanical abrasion, so that the condition of nitric acid corrosion abrasion exists. Although scholars at home and abroad carry out a great deal of research on the corrosion behavior of some active materials in boiling or sub-boiling nitric acid media, few scholars carry out related research on the nitric acid corrosion wear behavior of the materials. Meanwhile, the nitric acid corrosion research reported in the literature at present usually depends on ex-situ methods such as a traditional weight loss method and a morphology observation method, which results in a plurality of important process transformation information losses, so that the nitric acid corrosion mechanism of the material cannot be deeply understood, and the design principle of the material under the condition is more difficult to be clarified. A set of corrosive wear evaluation device is set up, and the change of the corrosive wear behavior of the material is monitored in real time by means of an electrochemical in-situ test method, so that basic data of a mechanical action component, a chemical (corrosive) action component and a mechanical and chemical (corrosive) coupling action component of various materials subjected to corrosive wear in nitric acid can be obtained more conveniently. By combining electrochemical tests with weight loss, morphology and corrosion product membrane components, the corrosive wear behavior of the material in a nitric acid medium can be more systematically revealed, and the mechanical and chemical (corrosion) interaction mechanism of the material is clarified.
Disclosure of Invention
The invention aims to provide an experimental device for simulating the corrosive wear of boiling nitric acid in post-treatment of spent fuel, which solves the problem that the nitric acid corrosive wear of materials under the post-treatment working condition cannot be simulated at present, solves the problem that in-situ electrochemical test cannot be carried out in the traditional nitric acid corrosion experiment, and realizes the systematic evaluation of the nitric acid corrosive wear performance of related materials.
The technical scheme of the invention is as follows:
an experimental device for simulating corrosive wear of spent fuel postprocessing boiling nitric acid is provided with a corrosive wear testing system, a supporting system, a transmission system, an electrochemical testing system, a liquid level control system, a condensation and tail gas treatment system and an electric control system, and has the following specific structure:
the kettle body and the transmission system of the corrosive wear testing system are supported by a support system made of stainless steel materials, the support system is provided with a bottom support, a kettle body bottom frame and a base, the bottom support is installed on the base through a bolt IV, the kettle body bottom frame is installed on the bottom support through a movable bolt with adjustable height, a clamp rod with one end extending into the kettle body and a friction force bearing mechanical arm of the transmission system are kept at the same horizontal height by adjusting the height of the kettle body bottom frame, a motor of the transmission system is installed on the bottom support through a bolt III, the kettle body is arranged on the kettle body bottom frame, and the lower part of the side surface of the kettle body is fixedly connected with a bolt II on the kettle body bottom frame through a connecting piece;
a sample on a workbench in the kettle body is used as a working electrode and is connected with an external electrochemical workstation, an electrochemical testing system adopts a three-electrode system to carry out electrochemical measurement, a clamp rod in the kettle body is connected with a friction force-bearing mechanical arm of a transmission system through a bolt I, when the friction force-bearing mechanical arm moves, an induction counter fixed on a supporting part records the movement times and transmits the movement times to an electric control system, a thermocouple is arranged at the bottom in the kettle body, a temperature sensor is arranged in nitric acid in the kettle body, the thermocouple passes through the kettle body through a lead and is connected with the electric control system, and a temperature sensor passes through a glass cover plate through a lead and is connected with the electric control system; one end of a condensing pipe in the condensing and tail gas treatment system extends into the kettle body through a glass cover plate, and the other end of the condensing pipe is connected with a tail gas treatment device; the liquid level control system penetrates through the side wall of the kettle body through a hose and extends into the kettle body, and the height of the nitric acid liquid level in the kettle body is adjusted through a lifting mechanism; the transmission system drives a glass pressure head above a sample to rub on the surface of the sample through a motor, so that the corrosive wear test is realized, the electrochemical test system realizes the measurement of electrochemical data of the nitric acid corrosive wear test, the liquid level control system realizes the corrosive wear test under different dry and wet environments by controlling the nitric acid liquid level, and the condensation and tail gas treatment system realizes the circulation of nitric acid steam and the recovery of waste gas.
The experimental device for simulating the corrosive wear of the spent fuel post-treatment boiling nitric acid is characterized in that a corrosive wear test system is provided with a kettle body, a workbench, a clamp rod, a pressure head, a counter weight part and a thermocouple, wherein the workbench is positioned in the center of the bottom in the kettle body, a sample for the corrosive wear test is placed on the workbench, the glass pressure head is fixed at the bottom of the pressure head and the counter weight part, the pressure head and the counter weight part are fixed above the workbench through the clamp rod, and the thermocouple is arranged at the bottom in the kettle body.
Simulation spent fuel aftertreatment boiling nitric acid erosive wear's experimental apparatus, erosive wear test system's cauldron body top is equipped with glass cover plate, and thermocouple and workstation are installed to its interior bottom, and cauldron body side lower part trompil passes through the hose with liquid level control system and links to each other, sets up four apertures and a macropore on the cauldron body top glass cover plate, wherein: an auxiliary electrode, a sample and a temperature sensor for controlling temperature for electrochemical test are arranged in nitric acid in a kettle body, leading-out leads of the auxiliary electrode and the sample extend out of the kettle body through small holes to be connected with an electrochemical workstation, leading-out leads of the temperature sensor extend out of the kettle body through the small holes to be connected with an electric control system, a salt bridge extends into the kettle body through the small holes, and sealing gaskets are respectively arranged at the four small holes; the condenser pipe passes through the macropore and extends to the inner cavity of the kettle body, the lower end of the condenser pipe is positioned above the nitric acid liquid level in the kettle body, and the glass cover plate is fixed on the kettle body through angle iron arranged outside the kettle body.
In the experimental device for simulating the corrosive wear of the spent fuel post-treatment boiling nitric acid, in a corrosive wear test system, a workbench is positioned in the center of the bottom in a kettle body, the workbench is formed by fixing a thin gasket, a gasket I and a gasket II which are arranged from top to bottom through rivets and screws, the top of the workbench is provided with the thin gasket, and a corrosive wear sample is placed at a central window of the thin gasket; the thermocouples are distributed at the bottom of the kettle body and protected by polytetrafluoroethylene sleeves, the thermocouples are distributed around a workbench at the bottom of the kettle body in an annular mode, the sample is arranged on the workbench, and the thermocouples and the temperature sensor are connected with an electric control system through wires.
Simulation spent fuel aftertreatment boiling nitric acid corrosive wear's experimental apparatus, pressure head and counter weight part include the glass pressure head, the counter weight cavity, the balancing weight, the glass pressure head passes through the fixed cover of glass pressure head and installs in counter weight cavity bottom center blind hole department, the glass pressure head is installed in the fixed cover center hole department of glass pressure head, the lower extreme and the sample of glass pressure head are corresponding, the balancing weight of different masses is placed to counter weight cavity inside, the counter weight cavity top is sealed through the nut, the counter weight cavity is fixed on counter weight cavity anchor clamps during the experiment, the screw hole is seted up along the horizontal direction to the side of counter weight cavity anchor clamps, the one end of anchor clamps pole pass through the connecting rod with the screw hole is connected.
The experimental device for simulating the corrosion and abrasion of the spent fuel post-treatment boiling nitric acid comprises a transmission system, a friction force-bearing mechanical arm, a motor, an eccentric crankshaft connecting rod and a friction stroke induction counter, wherein the friction force-bearing mechanical arm is made of stainless steel materials and is of a screw structure and horizontally arranged, one end of the eccentric crankshaft connecting rod is connected with the clamp rod through a bolt I, the other end of the eccentric crankshaft connecting rod is connected with one end of the eccentric crankshaft connecting rod through a screw through a sliding block, the other end of the eccentric crankshaft connecting rod is connected with a rotary turntable arranged at the output end of the motor through a screw, the sliding block is arranged on the sliding rail and is in sliding fit with the sliding rail, the reciprocating motion of the friction force-bearing mechanical arm is controlled by driving an eccentric crankshaft connecting rod through a motor, the motor is connected with an electric control system through a lead, and an induction counter is arranged below the joint of the friction force-bearing mechanical arm and the clamp rod and is connected with the electric control system through a lead.
The experimental device for simulating the corrosion and abrasion of the spent fuel postprocessing boiling nitric acid comprises an electrochemical testing system, wherein the electrochemical testing system is composed of a three-electrode system, a working electrode, an auxiliary electrode and a reference electrode are respectively and externally connected with an electrochemical workstation, the working electrode is formed by connecting a lead with a sample, the auxiliary electrode is an electrode sealed by polytetrafluoroethylene, the reference electrode is placed in a beaker filled with saturated potassium chloride aqueous solution, and nitric acid in a kettle body is connected with the saturated potassium chloride aqueous solution in the beaker through a salt bridge;
the salt bridge is composed of a glass salt bridge main body, a plug and porous nano ceramics, the glass salt bridge main body is of an inverted U-shaped tubular structure, the porous nano ceramics are installed at the positions, contacted with a solution, of two ends of the glass salt bridge main body, an upward opening position is arranged in the middle of the glass salt bridge main body, and the opening position is sealed through the plug.
The experimental device for simulating the spent fuel aftertreatment boiling nitric acid corrosive wear comprises a liquid level control system, a hose, a lifting mechanism and a tank body, wherein the tank body is communicated with a kettle body of a corrosive wear testing system through the hose, the hose moves up and down, the tank body is arranged on the lifting mechanism, the height of the nitric acid liquid level in the kettle body in the experimental process is adjusted through the lifting mechanism, wet grinding occurs when the liquid level of the kettle body is higher than a sample, and dry grinding occurs when the liquid level of the kettle body is lower than the sample.
Simulation spent fuel aftertreatment boiling nitric acid erosive wear's experimental apparatus, condensation and tail gas processing system are equipped with condenser pipe, circulation tank, tail gas processing apparatus, vertical condenser pipe one end is continuous with cauldron internal chamber through the aperture on the glass apron of the cauldron body downwards, during the condenser pipe other end is buckled and is connected the rubber tube downwards and let in tail gas processing apparatus, circulation tank passes through the middle part of circulation pipeline cladding condenser pipe.
The experimental device for simulating the corrosion and the abrasion of the spent fuel postprocessing boiling nitric acid is characterized in that an electric control system is provided with a temperature control part, a moving speed control part and a friction frequency recording part, wherein: the temperature control part is connected with the thermocouple and the temperature sensor, and the temperature of the solution is accurately controlled by monitoring the temperature of the nitric acid solution in real time; the speed control part is connected with the motor, and the speed of the friction force bearing mechanical arm is adjusted by controlling different rotating speeds of the motor; the friction frequency recording part is connected with the induction counter and directly reads the friction frequency.
The design idea of the invention is as follows:
the invention is based on the practical engineering problems: in the spent fuel post-treatment process, part of key equipment is used under the combined action of nitric acid corrosion and mechanical abrasion, and the condition of nitric acid corrosion abrasion exists, but effective research cannot be carried out on the equipment due to the lack of a corresponding corrosion abrasion device for simulation. Therefore, a set of experimental device for simulating corrosive wear of spent fuel reprocessing boiling nitric acid is developed, the corrosion and wear interaction mechanism of related materials can be explored, the corrosion-resistant and wear-resistant selection principle of the materials under different service working conditions is determined, and related corrosion-resistant and wear-resistant basic data are accumulated.
The material which can be used for a long time in the boiling nitric acid is limited, and from the aspects of long-term use and safety, polytetrafluoroethylene is selected as the kettle body of the corrosive wear device, and stainless steel material is selected as the friction force-bearing mechanical arm. The parts such as the lead wire and the thermocouple used in the nitric acid need to be protected by a polytetrafluoroethylene sleeve. Simultaneously, in order to meet the requirements of energy conservation and environmental protection, equipment is designed and built to be miniaturized as much as possible, the volume of the kettle body is not more than 10L, and a condensation and tail gas treatment device is designed to circulate and treat waste gas of the generated nitric acid steam.
In order to realize in-situ electrochemical measurement, the three electrodes are arranged during electrochemical test, and the reference electrode cannot be used at high temperature, so that a salt bridge is connected with the nitric acid solution.
In order to realize the corrosive wear test under the alternation of dry grinding, wet grinding and dry-wet grinding of the sample, a liquid level control system is adopted to adjust the height of the nitric acid liquid level in the polytetrafluoroethylene kettle body.
The invention has the following advantages and beneficial effects:
1. the invention realizes the simulation of nitric acid corrosion abrasion on different types and sizes of materials under the working condition of spent fuel aftertreatment.
2. The invention adopts a modular design, and each part of the device can be conveniently disassembled, combined and reconstructed.
3. The kettle body of the corrosive wear test system is connected with the liquid level control system through the polytetrafluoroethylene hose, so that the corrosive wear test under the alternation of dry grinding, wet grinding and dry and wet of a sample can be realized.
4. The invention can control the abrasion speed of the glass pressure head on the surface of the sample by controlling the moving speed of the friction force-bearing mechanical arm, thereby realizing the corrosive abrasion test at different abrasion speeds.
5. The invention can heat the nitric acid solution by controlling the thermocouple and feed back the nitric acid solution by the temperature sensor, thereby realizing the corrosion wear test at different temperatures
6. The main body of the invention adopts polytetrafluoroethylene and stainless steel materials, so that the cost is controlled on the premise of ensuring safety, and the invention has economic benefit.
7. The invention adopts a condensation and tail gas treatment device, realizes condensation circulation of nitric acid steam and harmless treatment of nitric acid waste gas, and is energy-saving and environment-friendly.
Drawings
FIG. 1 is a schematic view of the main structure of the present invention.
FIG. 2 is a schematic view of a work table according to the present invention.
FIG. 3 is a schematic view of the thermocouple arrangement according to the present invention.
FIG. 4 is a schematic view of the indenter, the weight portion and the clamp of the present invention.
FIG. 5 is a schematic representation of a salt bridge according to the present invention.
In the figure: 1. a circulating water tank; 2. an electrochemical workstation; 3. a condenser tube; 4. a tail gas treatment device; 5. a salt bridge; 6. a gasket; 7. a cover plate; 8. a reference electrode; 9. an auxiliary electrode; 10. a ram and a counterweight portion; 11. a clamp rod; 12. a temperature sensor; 13. a work table; 14. a sample; 15. a thermocouple; 16. a hose; 17. a lifting mechanism; 18. a tank body; 19. angle iron; 20. a kettle body; 21. a gasket; 22. a bolt I; 23. a bolt II; 24. an induction counter; 25. a friction force-bearing mechanical arm; 26. a slider; 27. an eccentric crankshaft connecting rod; 28. a screw; 29. rotating the turntable; 30. an electronic control system; 31. a slide rail; 32. a motor; 33. a bottom bracket; 34. a bottom frame of the kettle body; 35. the height of the movable bolt can be adjusted; 36. a bolt III; 37. a bolt IV; 38. a balancing weight; 39. a connecting rod; 40. a pressure head fixing sleeve; 41. a pressure head; 42. a counterweight cavity; 43. a counterweight cavity clamp; 44. a nut; 45. a salt bridge body; 46. a plug; 47. porous nanoceramic; 48. a shim; 49. a gasket I; 50. a gasket II; 51. a base.
Detailed Description
As shown in fig. 1, the experimental apparatus for simulating corrosive wear of boiling nitric acid after spent fuel reprocessing of the present invention comprises a corrosive wear testing system, a supporting system, a transmission system, an electrochemical testing system, a liquid level control system, a condensation and tail gas treatment system and an electric control system 30, and the experimental apparatus mainly comprises: the device comprises a circulating water tank 1, an electrochemical workstation 2, a condenser pipe 3, a tail gas treatment device 4, a salt bridge 5, a sealing gasket 6, a glass cover plate 7, a reference electrode 8, an auxiliary electrode 9, a pressure head and balance weight part 10, a polytetrafluoroethylene clamp rod 11, a temperature sensor 12, a workbench 13, a sample 14, a thermocouple 15, a polytetrafluoroethylene hose 16, a lifting mechanism 17, a polytetrafluoroethylene tank 18, angle iron 19, a polytetrafluoroethylene kettle body 20, a polytetrafluoroethylene sealing gasket 21, a bolt I22, a bolt II23, an induction counter 24, a friction force-bearing mechanical arm 25, a sliding block 26, an eccentric crankshaft connecting rod 27, a bolt 28, a rotary turntable 29, an electric control system 30, a sliding rail 31, a motor 32, a bottom support 33, a kettle body bottom frame 34, a height-adjustable movable bolt 35, a bolt III36, a bolt IV37, a balancing weight 38, a connecting rod 39, a glass pressure head fixing sleeve 40, a glass pressure head 41, Counter weight cavity 42, counter weight cavity anchor clamps 43, polytetrafluoroethylene nut 44, glass salt bridge main part 45, polytetrafluoroethylene stopper 46, porous nanometer pottery 47, polytetrafluoroethylene shim 48, polytetrafluoroethylene shim I49, polytetrafluoroethylene shim II50, base 51, the concrete structure is as follows:
the polytetrafluoroethylene kettle body 20 and the transmission system of the corrosive wear test system are supported by a supporting system made of stainless steel materials, the supporting system is provided with a bottom support 33, a kettle bottom frame 34 and a base 51, the bottom support 33 is installed on the base 51 through a bolt IV37, the kettle bottom frame 34 is installed on the bottom support 33 through a movable bolt 35 with adjustable height, and by adjusting the height of the kettle bottom frame 34, a polytetrafluoroethylene clamp rod 11 with one end extending into the polytetrafluoroethylene kettle body 20 and a friction force bearing mechanical arm 25 of the transmission system are kept at the same horizontal height, so that the clamp rod 11 and the friction force bearing mechanical arm 25 are conveniently connected by a matched bolt I22 and a sealing gasket 21. The motor 32 of the transmission system is arranged on the bottom bracket 33 through a bolt III36, the polytetrafluoroethylene kettle body 20 is arranged on the kettle body bottom frame 34, and the lower part of the side surface of the polytetrafluoroethylene kettle body 20 is fixedly connected with a bolt II23 on the kettle body bottom frame 34 through a connecting piece.
A sample 14 on a workbench 13 in a polytetrafluoroethylene kettle body 20 is used as a working electrode to be connected with an external electrochemical workstation 2, and a three-electrode system is adopted for electrochemical measurement, a polytetrafluoroethylene clamp rod 11 in the polytetrafluoroethylene kettle body 20 is connected with a friction force-bearing mechanical arm 25 of a transmission system through a bolt I22, when the friction force-bearing mechanical arm 25 moves, an induction counter 24 fixed on a supporting part records the movement times and transmits the movement times to an electric control system 30, a thermocouple 15 protected by polytetrafluoroethylene is arranged at the bottom in the kettle body 20, a temperature sensor 12 is arranged in nitric acid in the kettle body 20, a lead protected by polytetrafluoroethylene of the thermocouple 15 penetrates through the kettle body 20 to be connected with the electric control system 30, and a lead protected by polytetrafluoroethylene of the temperature sensor 12 penetrates through a glass cover plate 7 to be connected with the electric control system 30, so that temperature control can be carried out; one end of a condensing pipe 3 in the condensing and tail gas treatment system extends into the kettle body 20 through a small hole at one position of a glass cover plate 7, and the other end of the condensing pipe is connected with a tail gas treatment device 4; the liquid level control system penetrates through the side wall of the polytetrafluoroethylene kettle body 20 through the polytetrafluoroethylene hose 16 and extends into the kettle body 20, and the nitric acid liquid level in the kettle body 20 is adjusted by the aid of the lifting mechanism 17. The corrosive wear test system simulates a boiling nitric acid environment under the condition of aftertreatment working conditions, the transmission system drives the glass pressure head 41 above the sample 14 to rub on the surface of the sample 14 through the motor 32, the corrosive wear test is realized, the electrochemical test system realizes the measurement of electrochemical data of the nitric acid corrosive wear test, the liquid level control system realizes the corrosive wear test under different dry and wet environments by controlling the nitric acid liquid level, and the condensation and tail gas treatment system realizes the circulation of nitric acid vapor and the recovery of waste gas.
Corrosive wear test system is equipped with the polytetrafluoroethylene cauldron body 20, polytetrafluoroethylene workstation 13, polytetrafluoroethylene anchor clamps pole 11, pressure head and counter weight part 10, thermocouple 15 with polytetrafluoroethylene protection, polytetrafluoroethylene workstation 13 is located the central authorities of the bottom in the polytetrafluoroethylene cauldron body 20, place the sample 14 that is used for corrosive wear to test on the workstation 13, glass pressure head 41 is fixed in the pressure head and the counter weight part 10 bottom with polytetrafluoroethylene protection, pressure head and counter weight part 10 are fixed in workstation 13 top through polytetrafluoroethylene anchor clamps pole 11, protected thermocouple 15 arranges the bottom in cauldron body 20.
The polytetrafluoroethylene cauldron body 20 top of corrosive wear test system is equipped with glass apron 7, and thermocouple 15 and workstation 13 are installed to its inner bottom, and polytetrafluoroethylene cauldron body 20 side lower part trompil passes through polytetrafluoroethylene hose 16 with liquid level control system and links to each other, and polytetrafluoroethylene cauldron body 20 can hold 1 ~ 5L's nitric acid, has opened four apertures and a macropore on the glass apron 7 of top, wherein: an auxiliary electrode 9, a sample 14 and a temperature sensor 12 for controlling temperature for electrochemical test are arranged in nitric acid in a kettle body 20, leading-out wires of the auxiliary electrode 9 and the sample 14 extend out of the kettle body through small holes to be connected with an electrochemical workstation 2, leading-out wires of the temperature sensor 12 extend out of the kettle body through the small holes to be connected with an electric control system 30, a salt bridge 5 extends into the kettle body through the small holes, and sealing gaskets 6 are respectively arranged at the four small holes; the condenser tube 3 extends to the inner cavity of the kettle body 20 through the big hole, the lower end of the condenser tube 3 is positioned above the nitric acid liquid level in the kettle body 20, and the whole glass cover plate 7 is fixed on the kettle body 20 by angle iron 19 arranged outside the polytetrafluoroethylene kettle body 20.
As shown in FIG. 2, in the corrosive wear test system, a polytetrafluoroethylene worktable 13 is positioned at the center of the bottom in a polytetrafluoroethylene kettle body 20, the worktable 13 is formed by fixing a polytetrafluoroethylene thin gasket 48, a polytetrafluoroethylene gasket I49 and a polytetrafluoroethylene gasket II50 which are arranged from top to bottom by polytetrafluoroethylene rivets and screws, the polytetrafluoroethylene thin gasket 48 is arranged at the top of the worktable 13, and a corrosive wear sample 14 can be placed at the central window of the polytetrafluoroethylene thin gasket 48, so that the corrosive wear test of samples with different shapes and sizes can be realized.
As shown in fig. 3, in the corrosive wear test system, the thermocouples 15 are arranged at the bottom of the teflon kettle body 20 and protected by teflon sleeves, the thermocouples 15 are arranged around the workbench 13 at the bottom of the kettle body 20 in an annular shape, the sample 14 is arranged on the workbench 13, the thermocouples 15 and the temperature sensor 12 protected by teflon are connected with the electric control system 30 through leads protected by teflon sleeves, and the accurate temperature control of the nitric acid solution within 20-200 ℃ can be realized.
As shown in fig. 4, the pressure head and weight portion 10 includes a glass pressure head 41, a sealable weight cavity 42 made of teflon, and a weight block 38, the glass pressure head 41 is installed at a blind hole at the bottom of the weight cavity 42 through a glass pressure head fixing sleeve 40, the glass pressure head 41 is installed at a central hole of the glass pressure head fixing sleeve 40, the lower end of the glass pressure head 41 corresponds to the sample 14, in the experiment, the surface of the sample is abraded, the counterweight blocks 38 with different masses can be placed in the counterweight cavity 42, the balance weight of 10 g-5000 g can be realized, the top of the whole balance weight cavity 42 is sealed by a polytetrafluoroethylene nut 44, the balance weight cavity 42 is fixed on a balance weight cavity clamp 43 made of polytetrafluoroethylene during an experiment, a threaded hole is formed in the side surface of the balance weight cavity clamp 43 along the horizontal direction, and one end of a polytetrafluoroethylene clamp rod 11 is connected with the threaded hole through a connecting rod 39.
The transmission system is provided with a friction force-bearing mechanical arm 25, a motor 32, an eccentric crankshaft connecting rod 27 and a friction stroke induction counter 24, the friction force-bearing mechanical arm 25 is made of stainless steel materials into a screw rod structure, the friction force-bearing mechanical arm 25 is horizontally arranged, one end of the friction force-bearing mechanical arm is connected with a clamp rod 11 through a bolt I22, the other end of the friction force-bearing mechanical arm is connected with one end of the eccentric crankshaft connecting rod 27 through a slide block 26, the other end of the eccentric crankshaft connecting rod 27 is connected with a rotary turntable 29 arranged at the output end of the motor 32 through a screw 28, the slide block 26 is arranged on a slide rail 31 and is in sliding fit with the slide rail 31, the eccentric crankshaft connecting rod 27 is driven by the motor 32 to control the reciprocating motion of the friction force-bearing mechanical arm 25, the motor 32 is connected with an electric control system 30 through a lead, the induction counter 24 is arranged below the joint of the friction force-bearing mechanical arm 25 and the polytetrafluoroethylene clamp rod 11 and is connected with the electric control system 30 through a lead, the number of times the glass indenter 41 rubs back and forth across the sample surface can be accurately recorded.
The electrochemical testing system is composed of a three-electrode system, a working electrode, an auxiliary electrode 9 and a reference electrode 8 are respectively externally connected with an electrochemical workstation 2 for electrochemical testing, the working electrode is formed by connecting a lead protected by polytetrafluoroethylene with a sample 14, the auxiliary electrode 9 is an electrode sealed by polytetrafluoroethylene, the reference electrode 8 is placed in a beaker filled with saturated potassium chloride aqueous solution, nitric acid in a kettle body 20 is connected with the saturated potassium chloride aqueous solution in the beaker by a salt bridge 5, normal use of the reference electrode 8 in a use temperature range is ensured, and electrochemical real-time testing of corrosion and abrasion under boiling nitric acid is realized.
As shown in fig. 5, the salt bridge 5 is composed of a glass salt bridge main body 45, a teflon plug 46 and porous nano ceramics 47, the glass salt bridge main body 45 is an inverted U-shaped tubular structure, the porous nano ceramics 47 are installed at the parts of two ends of the glass salt bridge main body which are contacted with the solution, an upward opening part is arranged in the middle of the glass salt bridge main body 45, and the opening part is sealed by the teflon plug 46, so that the reference electrode 8 is ensured to work at a normal use temperature.
The liquid level control system comprises a polytetrafluoroethylene hose 16, a lifting mechanism 17 and a polytetrafluoroethylene tank 18, the polytetrafluoroethylene tank 18 is communicated with a polytetrafluoroethylene kettle body 20 of the corrosive wear test system through the polytetrafluoroethylene hose 16, the polytetrafluoroethylene hose 16 can move up and down, the polytetrafluoroethylene tank 18 is arranged on the lifting mechanism 17, the height of the nitric acid liquid level in the kettle body 20 in the experimental process can be adjusted through the lifting mechanism 17, wet grinding occurs when the liquid level of the kettle body 20 is higher than a sample 14, dry grinding occurs when the liquid level of the kettle body 20 is lower than the sample 14, and the liquid level control system can realize the material corrosive wear test under the alternation of dry and wet.
Condensation and tail gas processing system are equipped with condenser pipe 3, circulation tank 1, tail gas processing apparatus 4, 3 one ends of vertical condenser pipe are the aperture on the glass apron 7 of the downward polytetrafluoroethylene cauldron body 20 that passes through, link to each other with the internal cavity of cauldron 20, 3 other ends of condenser pipe buckle during the downwardly connected rubber tube lets in tail gas processing apparatus 4 (the beaker that is equipped with water), circulation tank 1 passes through the middle part of circulation pipeline cladding condenser pipe 3, flow rate and the temperature of condensate water in the condenser pipe 3 are controlled through circulation tank 1, the circulation to nitric acid steam and the recovery to waste gas have been realized.
The electronic control system 30 is provided with a temperature control part, a shift speed control part, and a friction number recording part, wherein: the temperature control part is connected with the thermocouple 15 and the temperature sensor 12, and the temperature of the nitric acid solution can be accurately controlled by monitoring the temperature of the nitric acid solution in real time; the moving speed control part is connected with the motor 32, and the moving speed of the friction force bearing mechanical arm 25 is adjusted by controlling different rotating speeds of the motor 32; the number of rubs recording section is connected to the induction counter 24 and can directly read the number of rubs.
During the experiment, the corrosive wear sample is installed on the workbench, the sample is connected with an external electrochemical workstation through a lead, nitric acid is injected into the polytetrafluoroethylene kettle body, and a mechanical arm of the transmission system drives a glass pressure head fixed on the polytetrafluoroethylene fixture to rub in a reciprocating manner on the surface of the sample, so that the corrosive wear simulation test is realized. According to the invention, under the condition of truly simulating the post-treatment working condition of the spent fuel, the corrosive wear behavior of the material in the boiling nitric acid is researched, the test parameters such as the temperature, the friction speed and the friction stroke of the nitric acid solution can be accurately controlled, the corrosive wear of the material under the dry-wet alternation can be simulated, and the switching of different corrosive wear forms and the online electrochemical monitoring and the weight loss test of a corrosive wear sample can be realized.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (10)

1. The utility model provides an experimental apparatus of simulation spent fuel aftertreatment boiling nitric acid erosive wear, its characterized in that, the device has erosive wear test system, braced system, transmission system, electrochemistry test system, liquid level control system, condensation and tail gas processing system and electrical system, and the concrete structure is as follows:
the kettle body and the transmission system of the corrosive wear testing system are supported by a support system made of stainless steel materials, the support system is provided with a bottom support, a kettle body bottom frame and a base, the bottom support is installed on the base through a bolt IV, the kettle body bottom frame is installed on the bottom support through a movable bolt with adjustable height, a clamp rod with one end extending into the kettle body and a friction force bearing mechanical arm of the transmission system are kept at the same horizontal height by adjusting the height of the kettle body bottom frame, a motor of the transmission system is installed on the bottom support through a bolt III, the kettle body is arranged on the kettle body bottom frame, and the lower part of the side surface of the kettle body is fixedly connected with a bolt II on the kettle body bottom frame through a connecting piece;
a sample on a workbench in the kettle body is used as a working electrode and is connected with an external electrochemical workstation, an electrochemical testing system adopts a three-electrode system to carry out electrochemical measurement, a clamp rod in the kettle body is connected with a friction force-bearing mechanical arm of a transmission system through a bolt I, when the friction force-bearing mechanical arm moves, an induction counter fixed on a supporting part records the movement times and transmits the movement times to an electric control system, a thermocouple is arranged at the bottom in the kettle body, a temperature sensor is arranged in nitric acid in the kettle body, the thermocouple passes through the kettle body through a lead and is connected with the electric control system, and a temperature sensor passes through a glass cover plate through a lead and is connected with the electric control system; one end of a condensing pipe in the condensing and tail gas treatment system extends into the kettle body through a glass cover plate, and the other end of the condensing pipe is connected with a tail gas treatment device; the liquid level control system penetrates through the side wall of the kettle body through a hose and extends into the kettle body, and the height of the nitric acid liquid level in the kettle body is adjusted through a lifting mechanism; the transmission system drives a glass pressure head above a sample to rub on the surface of the sample through a motor, so that the corrosive wear test is realized, the electrochemical test system realizes the measurement of electrochemical data of the nitric acid corrosive wear test, the liquid level control system realizes the corrosive wear test under different dry and wet environments by controlling the nitric acid liquid level, and the condensation and tail gas treatment system realizes the circulation of nitric acid steam and the recovery of waste gas.
2. The experimental device for simulating the corrosive wear of the boiling nitric acid after spent fuel treatment according to claim 1, wherein the corrosive wear testing system is provided with a kettle body, a workbench, a clamp rod, a pressure head, a counterweight part and a thermocouple, the workbench is positioned in the center of the bottom in the kettle body, a sample for the corrosive wear test is placed on the workbench, the glass pressure head is fixed at the bottom of the pressure head and the counterweight part, the pressure head and the counterweight part are fixed above the workbench through the clamp rod, and the thermocouple is arranged at the bottom in the kettle body.
3. The experimental device for simulating the corrosive wear of the boiling nitric acid after spent fuel treatment according to claim 2, wherein a glass cover plate is arranged at the top of the kettle body of the corrosive wear testing system, a thermocouple and a workbench are installed at the bottom of the kettle body, an opening at the lower part of the side surface of the kettle body is connected with the liquid level control system through a hose, and four small holes and one large hole are formed in the glass cover plate at the top of the kettle body, wherein: an auxiliary electrode, a sample and a temperature sensor for controlling temperature for electrochemical test are arranged in nitric acid in a kettle body, leading-out leads of the auxiliary electrode and the sample extend out of the kettle body through small holes to be connected with an electrochemical workstation, leading-out leads of the temperature sensor extend out of the kettle body through the small holes to be connected with an electric control system, a salt bridge extends into the kettle body through the small holes, and sealing gaskets are respectively arranged at the four small holes; the condenser pipe passes through the macropore and extends to the inner cavity of the kettle body, the lower end of the condenser pipe is positioned above the nitric acid liquid level in the kettle body, and the glass cover plate is fixed on the kettle body through angle iron arranged outside the kettle body.
4. The experimental device for simulating the corrosive wear of the boiling nitric acid after spent fuel treatment according to claim 2, wherein in the corrosive wear testing system, the workbench is positioned in the center of the bottom in the kettle body, the workbench is formed by fixing a thin gasket, a gasket I and a gasket II which are arranged from top to bottom through rivets and screws, the top of the workbench is provided with the thin gasket, and a corrosive wear sample is placed at a central window of the thin gasket; the thermocouples are distributed at the bottom of the kettle body and protected by polytetrafluoroethylene sleeves, the thermocouples are distributed around a workbench at the bottom of the kettle body in an annular mode, the sample is arranged on the workbench, and the thermocouples and the temperature sensor are connected with an electric control system through wires.
5. The experimental device for simulating boiling nitric acid corrosive wear of spent fuel reprocessing according to claim 2, wherein the pressure head and the counterweight part comprise a glass pressure head, a counterweight cavity and a counterweight block, the glass pressure head is mounted at a central blind hole at the bottom of the counterweight cavity through a glass pressure head fixing sleeve, the glass pressure head is mounted at a central hole of the glass pressure head fixing sleeve, the lower end of the glass pressure head corresponds to a sample, the counterweight block with different masses is placed inside the counterweight cavity, the top of the counterweight cavity is sealed through a nut, the counterweight cavity is fixed on a counterweight cavity fixture during an experiment, a threaded hole is formed in the side face of the counterweight cavity fixture in the horizontal direction, and one end of a fixture rod is connected with the threaded hole through a connecting rod.
6. The experimental device for simulating the corrosive wear of the boiling nitric acid in the post-treatment of the spent fuel according to claim 1, wherein the transmission system is provided with a friction force-bearing mechanical arm, a motor, an eccentric crankshaft connecting rod and a friction stroke induction counter, the friction force-bearing mechanical arm is made of stainless steel materials and is of a screw rod structure, the friction force-bearing mechanical arm is horizontally arranged, one end of the friction force-bearing mechanical arm is connected with the clamp rod through a bolt I, the other end of the friction force-bearing mechanical arm is connected with one end of the eccentric crankshaft connecting rod through a slide block and a screw, the other end of the eccentric crankshaft connecting rod is connected with a rotary turntable arranged at the output end of the motor through a screw, the slide block is arranged on the slide rail and is in sliding fit with the slide rail, the reciprocating motion of the friction force-bearing mechanical arm is controlled by driving the eccentric crankshaft connecting rod through the motor, the motor is connected with the electric control system through a lead, the induction counter is arranged below the joint of the friction force-bearing mechanical arm and the clamp rod, and is connected with an electric control system through a lead.
7. The experimental device for simulating the corrosive wear of the boiling nitric acid after spent fuel treatment according to claim 1, wherein an electrochemical test system is composed of a three-electrode system, a working electrode, an auxiliary electrode and a reference electrode are respectively and externally connected with an electrochemical workstation, the working electrode is formed by connecting a lead with a sample, the auxiliary electrode is an electrode sealed by polytetrafluoroethylene, the reference electrode is placed in a beaker filled with saturated potassium chloride aqueous solution, and the nitric acid in the kettle body is connected with the saturated potassium chloride aqueous solution in the beaker through a salt bridge;
the salt bridge is composed of a glass salt bridge main body, a plug and porous nano ceramics, the glass salt bridge main body is of an inverted U-shaped tubular structure, the porous nano ceramics are installed at the positions, contacted with a solution, of two ends of the glass salt bridge main body, an upward opening position is arranged in the middle of the glass salt bridge main body, and the opening position is sealed through the plug.
8. The experimental device for simulating the corrosive wear of the boiling nitric acid after spent fuel processing according to claim 1, wherein the liquid level control system comprises a hose, a lifting mechanism and a tank body, the tank body is communicated with the kettle body of the corrosive wear testing system through the hose, the hose moves up and down, the tank body is arranged on the lifting mechanism, the lifting mechanism is used for adjusting the height of the liquid level of the nitric acid in the kettle body in the experimental process, wet grinding occurs when the liquid level of the kettle body is higher than a sample, and dry grinding occurs when the liquid level of the kettle body is lower than the sample.
9. The experimental device for simulating the corrosive wear of the boiling nitric acid after spent fuel treatment according to claim 1, wherein the condensation and tail gas treatment system is provided with a condensation pipe, a circulating water tank and a tail gas treatment device, one end of the vertical condensation pipe downwards passes through a small hole in a glass cover plate of the kettle body and is connected with an inner cavity of the kettle body, the other end of the condensation pipe is bent and downwards connected with a rubber pipe and is led into the tail gas treatment device, and the circulating water tank covers the middle part of the condensation pipe through a circulating pipeline.
10. The experimental device for simulating the corrosive wear of the boiling nitric acid after spent fuel treatment according to claim 1, wherein the electric control system is provided with a temperature control part, a speed moving control part and a friction frequency recording part, wherein: the temperature control part is connected with the thermocouple and the temperature sensor, and the temperature of the solution is accurately controlled by monitoring the temperature of the nitric acid solution in real time; the speed control part is connected with the motor, and the speed of the friction force bearing mechanical arm is adjusted by controlling different rotating speeds of the motor; the friction frequency recording part is connected with the induction counter and directly reads the friction frequency.
CN202110930819.8A 2021-08-13 2021-08-13 Experimental device for simulating spent fuel aftertreatment boiling nitric acid corrosive wear Pending CN113720763A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114383996A (en) * 2021-12-10 2022-04-22 中国科学院金属研究所 Test device for simulating galvanic corrosion in high-temperature flowing medium environment
CN114965244A (en) * 2022-07-21 2022-08-30 太原工业学院 Method for evaluating fatigue performance of magnesium alloy welding joint in corrosive environment

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114383996A (en) * 2021-12-10 2022-04-22 中国科学院金属研究所 Test device for simulating galvanic corrosion in high-temperature flowing medium environment
CN114383996B (en) * 2021-12-10 2024-01-19 中国科学院金属研究所 Couple corrosion testing device under simulation high temperature flowing medium environment
CN114965244A (en) * 2022-07-21 2022-08-30 太原工业学院 Method for evaluating fatigue performance of magnesium alloy welding joint in corrosive environment

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