CN-122016625-A - Variable ammonia alcohol hydrogen environment multi-type corrosion testing device and testing method

CN122016625ACN 122016625 ACN122016625 ACN 122016625ACN-122016625-A

Abstract

The invention relates to the field of development of material mechanical property testing devices, in particular to a variable ammonia alcohol hydrogen environment multi-type corrosion testing device and a testing method, wherein the device comprises a first reaction kettle, a second reaction kettle and a third reaction kettle, the first reaction kettle is a constant-load tensile stress corrosion device, the second reaction kettle is a constant-displacement stress corrosion device, the third reaction kettle is an electrochemical corrosion testing device, the first reaction kettle, the second reaction kettle and the third reaction kettle are respectively connected with a gas distribution device for supplying gas and a tail gas recovery device for recovering tail gas through pipelines, the first reaction kettle, the second reaction kettle and the third reaction kettle are respectively connected with a stepless pressure regulating device through pipelines, and the first reaction kettle, the second reaction kettle and the third reaction kettle are respectively connected with a water bath circulation temperature control device through water jackets. The device and the method can accurately simulate the actual working condition and synchronously or asynchronously realize the constant load tensile stress corrosion test, the constant displacement stress corrosion test and the electrochemical corrosion test under different ammonia, alcohol and hydrogen corrosion environments.

Inventors

LI JIAQING
He Shuaizhen
LIN ZETAO
YAN BOYU
HU JIAZHUANG
WEI HONGDA
FANG BOHAN

Assignees

福州大学

Dates

Publication Date: 20260512
Application Date: 20260317

Claims (10)

1. A multi-type corrosion testing device for a variable ammonia alcohol hydrogen environment comprises a first reaction kettle (4), a second reaction kettle (5) and a third reaction kettle (6), and is characterized in that hollowed-out bottom plates (31) are fixed in the first reaction kettle (4) and the second reaction kettle (5), the bottom plates (31) in the first reaction kettle (4) are used for being fixed below a sample (27) to be tested, a plurality of levers (12) hanging weights, which are arranged outside the first reaction kettle (4), of the sample (27) to be tested are connected with one another through different force arms, the bottom plates (31) in the second reaction kettle (5) are used for supporting a C-ring sample (29) and a T-WOL sample (30), a resistance probe corrosion detector (32) is externally connected to the second reaction kettle (5), electrode groups (33) are arranged in the third reaction kettle (6), the electrode groups (33) are connected with an external electrochemical workstation (8), the first reaction kettle (4), the second reaction kettle (5) and the third reaction kettle (6) are connected with a first reaction kettle (4) through a gas supply pipeline (6), a second reaction kettle (5) through a gas supply pipeline (4), a gas supply pipeline (4) and a gas supply pipeline (4) respectively and a continuous reaction kettle (4) and a continuous reaction kettle (5) respectively and a continuous reaction kettle (5) and a continuous reaction kettle (6) and a continuous reaction kettle respectively The third reaction kettle (6) is also respectively connected with a water bath circulation temperature control device.
2. The multi-type corrosion testing device for the variable ammonia alcohol hydrogen environment according to claim 1, wherein the gas distribution device comprises a plurality of rows of gas pipelines, one end of each row of gas pipelines is connected with a steel bottle through a first fully-closed safety valve (9A), a flowmeter (1) electrically connected with a control panel (2) is arranged on each row of gas pipelines, the other end of each row of gas pipelines is integrated with a connecting valve (11), the upper ends of the first reaction kettle (4), the second reaction kettle (5) and the third reaction kettle (6) are respectively provided with a first gas path interface (26A), and each first gas path interface (26A) is respectively connected with the connecting valve (11) through a pipeline.
3. The multi-type corrosion testing device for the variable ammonia alcohol hydrogen environment according to claim 2 is characterized in that a second totally-closed safety valve (9B) controlled by a direct-current motor (3) is arranged at the output end side of the connecting valve (11), the direct-current motor (3) is controlled by a control panel (2), and a third totally-closed safety valve (9C) is arranged on the first air path interface (26A).
4. The multi-type corrosion testing device for the variable ammonia alcohol hydrogen environment according to claim 1, 2 or 3, wherein the tail gas recovery device comprises a rectification separation tower (13), the upper ends of the first reaction kettle (4), the second reaction kettle (5) and the third reaction kettle (6) are respectively provided with a gas path interface II (26B), the gas path interfaces II (26B) are respectively connected with the rectification separation tower (13) through pipelines, the liquid phase output end of the rectification separation tower (13) is conveyed to the main body area of a waste liquid storage box (14) through a liquid discharge pipeline to finish storage, the gas phase output end of the rectification separation tower (13) is led into the upper space of the waste liquid storage box (14) through an exhaust pipeline, and the waste liquid storage box (14) is connected with a waste gas absorption tower (15).
5. The variable ammonia alcohol hydrogen environment multi-type corrosion testing device according to claim 1, wherein the stepless pressure regulating device comprises reaction kettle pressure regulating cylinders (35) which are respectively arranged in a first reaction kettle (4), a second reaction kettle (5) and a third reaction kettle (6), the reaction kettle pressure regulating cylinders (35) are provided with pressure regulating pistons (36), the reaction kettle pressure regulating cylinders (35) are respectively connected with a pressurizing constant-flow pump (23) through pipelines, and the pressurizing constant-flow pump (23) is connected with a hydraulic oil storage tank (22).
6. The variable ammonia alcohol hydrogen environment multi-type corrosion testing device according to claim 1,2, 3, 4 or 5 is characterized in that the upper ends of the first reaction kettle (4), the second reaction kettle (5) and the third reaction kettle (6) are respectively connected with a safety valve (24) and a pressure sensor (25), and the electrochemical workstation (8) and the resistance probe corrosion detector (32) are respectively connected with a computer (7).
7. The multi-type corrosion testing device for the variable ammonia alcohol hydrogen environment according to claim 1, wherein the water bath circulation temperature control device comprises a water bath circulation temperature control box (20) with a temperature control panel (21), water jackets (34) are respectively arranged on the side surfaces of the first reaction kettle (4), the second reaction kettle (5) and the third reaction kettle (6), a water outlet (18) of the water bath circulation temperature control box (20) is connected with a water inlet end of the water jacket (34) through a circulating pump (16) and an electromagnetic valve (17), and a water inlet (19) of the water bath circulation temperature control box (20) is connected with a water outlet end of the water jacket (34).
8. A method for testing multi-type corrosion in a variable ammonia hydrogen environment, comprising the device for testing multi-type corrosion in a variable ammonia hydrogen environment according to any one of claims 1 to 7, comprising the steps of: Firstly, preparing and installing, namely hanging a plurality of samples (27) to be tested into a first reaction kettle (4), fixing the lower part of the samples (27) with a bottom plate (31), and jointly externally connecting the plurality of samples (27) with a lever (12) hung with weights through different force arms to ensure that the samples (27) carry out constant load tensile tests under different loads in an environment of ammonia alcohol hydrogen stress corrosion; Secondly, loading operation, namely adding weights on the other side of a lever (12) connected with a sample (27) to be tested to apply load, measuring the deformation of the sample (27), and determining the actual load applied to the sample (27) according to a pre-calibrated deformation-load relation; Placing the sample (27) to be detected in a target environment, keeping the environment condition stable in the process, and monitoring the state of the sample (27); And fourthly, recording results, namely observing the conditions of cracks, crack propagation or fracture of the sample (27), recording corresponding time, stress change and other data, completing the test, and finally summarizing the corrosion resistance of the sample (27) in an ammonia/alcohol/hydrogen environment.
9. A method for testing multi-type corrosion in a variable ammonia hydrogen environment, comprising the device for testing multi-type corrosion in a variable ammonia hydrogen environment according to any one of claims 1 to 7, comprising the steps of: firstly, preparing and applying stress, namely measuring the size of a C-shaped ring sample (29), and calculating the change amount of the outer diameter of the C-shaped ring sample (29); Secondly, sample treatment and loading, namely cleaning a C-shaped ring sample (29), then placing the C-shaped ring sample (29) on a bottom plate (31) of a second reaction kettle (5), introducing nitrogen into the second reaction kettle (5) at a certain speed, and repeating the operation for three times; Thirdly, filling liquid ammonia and regulating the environment, namely cooling the second reaction kettle (5) to be below a designated temperature by using a water bath circulation temperature control device, slowly introducing ammonia gas at a certain flow rate to liquefy the second reaction kettle, and metering the gas injection amount; Under the set temperature and pressure conditions, carrying out liquid ammonia corrosion tests on the C-shaped ring samples (29) at specified intervals, so as to ensure that only corrosive media contact key stress areas and surfaces of the C-shaped ring samples (29) and avoid contact stress arc sections such as hollowed-out bottom plates (31); Fifthly, after the test is finished and the sample is taken out, slowly releasing liquid ammonia containing impurities to normal pressure, neutralizing the gas by a tail gas recovery device, and then discharging the gas; And (sixth) calculating the corrosion rate, namely weighing the weight of the C-shaped ring sample (29) before and after corrosion, and calculating the corrosion rate mm/a by adopting a weight increasing method and combining a formula CR= (W1-W0) ×87600/(A.T.D), wherein W0 is the weight before corrosion, W1 is the weight after corrosion, A is the surface area of the sample, T is the test duration, and D is the material density.
10. A method for testing multi-type corrosion in a variable ammonia hydrogen environment, comprising the device for testing multi-type corrosion in a variable ammonia hydrogen environment according to any one of claims 1 to 7, comprising the steps of: firstly, preparing a sample, namely taking a steel pipe made of a required material, linearly cutting the steel pipe into a required size specification, carrying out rough grinding by metallographic abrasive paper and fine grinding by water abrasive paper to a specified thickness, and cleaning and drying the steel pipe for later use; Secondly, preparing a device and the environment, namely building an electrode group (33), preparing ammonia solution with certain concentration as electrolyte, introducing nitrogen for a period of time, evacuating the oxygen of the solution, introducing oxygen to a specified pressure by using a mass flow controller, and controlling a third reaction kettle (6) to a specified temperature by using a water bath circulation temperature control device; thirdly, measuring open-circuit potential, namely placing the electrode group (33) into electrolyte with adjusted parameters, connecting an electrochemical workstation (8), monitoring the open-circuit potential until the open-circuit potential is stable, and recording a stable value; fourthly, potentiodynamic polarization test, namely scanning from the cathode to the anode according to a specified range and a specified speed by taking a stable open-circuit potential as a reference, recording a polarization curve, and using Tafil to fit corrosion current density and corrosion potential; And fifthly, post-treatment and characterization, namely cleaning and drying the sample by using an acid slow-release solution containing hexamethylenetetramine and absolute ethyl alcohol, observing the surface morphology by using a scanning electron microscope, and analyzing corrosion products by using an energy dispersion X-ray spectrometer and X-ray diffraction.

Description

Variable ammonia alcohol hydrogen environment multi-type corrosion testing device and testing method Technical Field The invention relates to the field of development of material mechanical property testing devices, in particular to a variable ammonia alcohol hydrogen environment multi-type corrosion testing device and a testing method. Background The hydrogen is produced by water electrolysis, and then the hydrogen, nitrogen, carbon dioxide and other synthetic ammonia and methanol are used for replacing fossil raw materials and fuels, so that deep decarburization in multiple industries is promoted. The integrated mode of 'hydrogen, ammonia, alcohol and terminal application' becomes a key scheme for energy and industrial transformation under a double-carbon target. Hydrogen is used as 'final energy source' in 21 st century, and has the advantages of high energy density (39.72 kW.h/kg), zero carbon emission, various sources, wide application range and the like. The hydrogen can realize large-scale and long-period energy storage, and can be used for absorbing intermittent renewable energy sources such as wind power, photovoltaic and the like, replacing the traditional fossil energy sources and greatly reducing carbon emission. Hydrogen provides a new choice for energy systems to clean low carbon conversions. The ammonia serving as a hydrogen storage medium has the advantages of high hydrogen content (17.7% by mass), low storage and transportation cost, no carbon emission at the terminal, high safety and the like. The zero-carbon cyclic economic route of 'high-efficiency synthesis, safe storage and transportation and no carbon-ammonia-hydrogen utilization' taking ammonia as a hydrogen storage carrier provides a new method for realizing rapid adjustment of an energy structure and accelerating the carbon neutralization process. Methanol has the advantages of high energy density, convenient storage and transportation, green and safety, and the like. The synthesis process can fix carbon dioxide, and the carbon dioxide released in the use process can participate in biological circulation again, so that closed-loop circulation of carbon is realized. The methanol provides a new path for pushing the deep decarburization of energy and recycling the carbon dioxide. At present, chinese hydrogen, ammonia and alcohol are mainly transported by means of tank trucks and trailers, and along with the rapid growth of the market demand of hydrogen-ammonia-alcohol, large-caliber high-pressure pipelines become a main form of safety transportation in the future of China. It is worth noting that hydrogen embrittlement can lead to fatigue cracking of a hydrogen transmission pipeline, particularly the temperature difference change of a long-distance pipeline is large, the brittle failure risk is further increased, ammonia is easy to interact with media such as air, water and the like, so that the pipeline is invalid due to corrosion in a long-term service process, methanol is easy to react with the media such as oxygen and the like, and water in the methanol can form electrolyte, so that the pipeline is electrochemically corroded. Therefore, the corrosion resistance of the pipeline material under the conditions of variable hydrogen, ammonia and alcohol environments and various corrosion types is systematically evaluated, and the corrosion resistance characteristics of the pipeline material under different complex working conditions are clear, so that the method has important engineering significance. The research of the testing device and the method still has obvious defects, and the deep research is needed. Therefore, the invention aims to develop a device and a method capable of synchronously or asynchronously realizing testing of various corrosion samples in various environments so as to accurately simulate and reproduce the corrosion behavior of materials under the actual working conditions. Disclosure of Invention The invention aims to provide a variable ammonia alcohol hydrogen environment multi-type corrosion test device and a test method, which can accurately simulate actual working conditions and synchronously or asynchronously realize constant load tensile stress corrosion test, constant displacement stress corrosion test and electrochemical corrosion test under different ammonia alcohol hydrogen corrosion environments by changing temperature and pressure and ammonia alcohol hydrogen gas components. The technical scheme includes that the variable ammonia alcohol hydrogen environment multi-type corrosion testing device comprises a first reaction kettle, a second reaction kettle and a third reaction kettle, hollow bottom plates are fixed in the first reaction kettle and the second reaction kettle, the bottom plates in the first reaction kettle are used for being fixed below a sample to be tested, a plurality of the sample to be tested are connected with a same lever hung with weights outside the first reaction kettle through di