Carbon dioxide corrosion test apparatus

Abstract

The present application relates to a kind of experimental equipment, in particular to a kind of carbon dioxide corrosion experiment device, including reactor, reactor heating assembly, reactor heating assembly is used to segment heating for the reactor, so that the reactor is divided into first temperature section, second temperature section, third temperature section, first temperature section, second temperature section, third temperature section are respectively provided with first window, second window, third window on the side wall, first window, second window, third window are respectively provided with optical observation equipment and corrosion detection probe, the bottom of the reactor is connected with liquid inlet pipe, gas inlet pipe, the top of the reactor is provided with fourth window, gas outlet, the sample holder is set in the reactor, the sample holder is used to place sample, the sample holder is through first temperature section, second temperature section, third temperature section of the reactor.The present application can carry out carbon dioxide corrosion behavior experiment under multiple phase states.

Description

TECHNICAL FIELD

[0001] The present application relates to an experimental device, in particular to a carbon dioxide corrosion experiment device. BACKGROUND

[0002] Carbon capture, utilization and storage technology (CCUS) refers to separating CO2 in industrial production or other emission sources, directly storing or processing and injecting into new production processes to reduce CO2 emissions. CCUS is a key way to realize low-carbon utilization of fossil energy and carbon neutralization, and has important significance for mitigating global climate change and promoting low-carbon development. CO2 in CCUS will be transported by pipeline, which will be the inevitable choice in the future large-scale CCUS scenario, but the pipeline material will face complex corrosion problems in the CCUS system, which is a key challenge to the safety of the system. Due to the relatively high temperature and pressure, the phase state of CO2 in the pipeline is complex, and there are supercritical phase, liquid phase and gas phase. In addition to CO2, the pipeline also contains carbon sources and impurity gases that may be brought by different capture technologies, and contains a small amount of water. Under the medium conditions higher than the critical pressure and temperature, the solubility of CO2 in H2O is several tens of times higher than that under normal pressure, and its corrosiveness will increase sharply. At the same time, when the water content is too high, the problem of electrochemical corrosion caused by the coupling of multiple impurities will be faced. At present, the corrosion behavior and mechanism under the coupling of multiple impurities and complex phase states are not well understood, and relevant research needs to be carried out to provide data support for the large-scale construction and application of CCUS system. SUMMARY

[0003] The technical problem solved by the present application is to provide a carbon dioxide corrosion experiment device for conducting carbon dioxide corrosion behavior experiments under multiple phase states.

[0004] In order to solve the above technical problems, the present application provides the following technical solutions:

[0005] The application discloses a carbon dioxide corrosion experiment device, which comprises a reaction kettle and a reaction kettle heating assembly, the reaction kettle heating assembly is used for segmented heating of the reaction kettle, so that the reaction kettle is divided into a first temperature section, a second temperature section and a third temperature section, a temperature sensor is arranged on the side wall of each of the first temperature section, the second temperature section and the third temperature section, a first window, a second window and a third window are arranged on the side wall of each of the first temperature section, the second temperature section and the third temperature section, an optical observation device and a corrosion detection probe are arranged on each of the first window, the second window and the third window, a liquid inlet pipe and a gas inlet pipe are connected to the bottom of the reaction kettle, the liquid inlet pipe is used for introducing experimental liquid into the reaction kettle, the gas inlet pipe is used for introducing experimental gas into the reaction kettle, a fourth window and a gas outlet are arranged on the top of the reaction kettle, a sample holder is arranged in the reaction kettle, the sample holder penetrates through the first temperature section, the second temperature section and the third temperature section of the reaction kettle, and the sample holder can be placed on the positions corresponding to different temperature sections of the reaction kettle.

[0006] Further, a pressure gauge is arranged on the side wall of the reaction kettle, and the pressure gauge is used for measuring the pressure in the reaction kettle.

[0007] Further, a liquid deoxygenization assembly is further arranged, the liquid deoxygenization assembly is connected to the liquid inlet pipe, and the experimental liquid enters the reaction kettle after passing through the deoxygenization assembly.

[0008] Further, the liquid deoxygenization assembly is a nitrogen deoxygenization tank, the nitrogen deoxygenization tank comprises a tank body, a piston is arranged in the tank body, the upper part and the lower part of the piston are respectively connected to a nitrogen gas source, the upper part of the piston is provided with a first nitrogen gas inlet and a first nitrogen gas outlet, the lower part of the piston is used for storing experimental liquid, and the lower part of the piston is provided with a second nitrogen gas inlet, a second nitrogen gas outlet, a liquid outlet and a dissolved oxygen test probe, the liquid outlet is communicated with the liquid inlet pipe, the experimental liquid is deoxygenized by nitrogen gas introduced through the second nitrogen gas inlet, when the dissolved oxygen content of the experimental liquid meets the requirement through the test of the dissolved oxygen test probe, the first nitrogen gas inlet of the upper part of the piston is used for introducing nitrogen gas, and the experimental liquid is pressed into the reaction kettle.

[0009] Further, a gas mixing assembly, a buffer device and a pressure increasing device are further arranged, the gas mixing assembly comprises a plurality of gas cylinders, the gas outlets of the gas cylinders are communicated with the inner cavities of the buffer device, flow meters are arranged on the gas outlets of the gas cylinders, the pressure increasing device is arranged downstream of the buffer device, and the gas outlet end of the pressure increasing device is connected to the gas inlet pipe.

[0010] Further, the reaction kettle heating assembly is a flexible heating sleeve, and the flexible heating sleeve is sleeved on the outside of the reaction kettle.

[0011] Further, the sample holder is made of ceramic material.

[0012] Further, the first nitrogen inlet, the first nitrogen outlet, the second nitrogen inlet, the second nitrogen outlet and the liquid outlet are provided with switch valves.

[0013] Further, the optical observation device comprises a coaxial light source and a shooting camera.

[0014] Compared with the prior art, the carbon dioxide corrosion experiment device has at least the following beneficial effects:

[0015] The carbon dioxide corrosion experiment device has the following advantages: the reaction kettle heating assembly is used for segmented heating of the reaction kettle, so that the reaction kettle is divided into a first temperature section, a second temperature section and a third temperature section, thereby realizing segmented temperature control and corrosion simulation in different states, and realizing liquid phase corrosion, liquid phase and supercritical CO2 interface corrosion, supercritical CO2 and gas phase CO2 corrosion simulation; the sample holder penetrates through the first temperature section, the second temperature section and the third temperature section of the reaction kettle, and by placing samples and corrosion monitoring probes of different temperature sections on the sample holder, corrosion data in different phase state environments can be obtained; the reaction kettle top is provided with a viewing window, and by combining a shooting camera, the saturation moisture content data under the influence of multiple parameters such as impurity components, temperature and pressure can be tested by observing the dewing state on the viewing window; the first temperature section, the second temperature section and the third temperature section are respectively provided with observation windows, so that the corrosion state of the sample with time can be monitored by combining the shooting camera.

[0016] The carbon dioxide corrosion experiment device will be further described below in combination with the drawings. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 FIG. 1 is a structural schematic diagram of the carbon dioxide corrosion experiment device. DETAILED DESCRIPTION

[0018] As shown in FIG. 1, the carbon dioxide corrosion experiment device comprises a reaction kettle 1, a sample holder 2, a nitrogen inlet 3, a nitrogen outlet 4, a liquid inlet 5, a liquid outlet 6, a first temperature section 7, a second temperature section 8, a third temperature section 9, a viewing window 10, a shooting camera 11 and a computer 12. Figure 1As shown, the carbon dioxide corrosion experiment device of the present application comprises a reaction kettle 01, a reaction kettle heating assembly 02, and a sample holder. The reaction kettle heating assembly 02 is used for segmented heating of the reaction kettle 01, so that the reaction kettle 01 is divided into a first temperature section, a second temperature section, and a third temperature section. A temperature sensor is arranged on the side wall of each of the first temperature section, the second temperature section, and the third temperature section. A first viewing window 16, a second viewing window 17, and a third viewing window 18 are arranged on the side wall of each of the first temperature section, the second temperature section, and the third temperature section. An optical observation device and a corrosion detection probe are arranged on each of the first viewing window 16, the second viewing window 17, and the third viewing window 18. The optical observation device comprises a coaxial light source and a shooting camera. The light source projects light on the sample. The corrosion morphology characteristics of the sample and the change trend of the corrosion product over time are observed in real time through the shooting camera. The composition of the corrosion product of the sample can be tested in combination with a portable Raman device. The corrosion monitoring probe is used to monitor the change trend of the corrosion rate of the sample over time, so as to provide data support for the corrosion mechanism analysis of the sample. The bottom of the reaction kettle 01 is connected with a liquid inlet pipe 11 and a gas inlet pipe 12. The liquid inlet pipe 11 is used to introduce experimental liquid into the reaction kettle 01. The gas inlet pipe 12 is used to introduce experimental gas into the reaction kettle 01. A fourth viewing window 13 and a gas outlet 14 are arranged on the top of the reaction kettle 01. The gas outlet 14 is connected with a waste gas treatment device 15. The sample holder is arranged in the reaction kettle 01. The sample holder penetrates through the first temperature section, the second temperature section, and the third temperature section of the reaction kettle 01. The sample holder can be placed on the positions corresponding to different temperature sections of the reaction kettle 01. Specifically, the reaction kettle 01 is made of C276 material. The inner diameter of the reaction kettle 01 is 200 mm. The height of the reaction kettle 01 is not less than 1.5 meters. The fourth viewing window 13 is connected to the top of the reaction kettle 01 through a flange. The diameter of the fourth viewing window is 60 mm. The first viewing window 16, the second viewing window 17, and the third viewing window 18 are all connected to the side wall of the reaction kettle 01 through flanges. The diameters of the first viewing window 16, the second viewing window 17, and the third viewing window 18 are all 60 mm. A climbing frame is arranged on the outer wall of the reaction kettle 01, so as to facilitate personnel operation. The carbon dioxide corrosion experiment device of the present application can control the temperature in sections, realize corrosion simulation in different states, and can realize liquid phase corrosion, liquid phase and supercritical CO2 interface corrosion, and supercritical CO2 and gas phase CO2 corrosion simulation. When the carbon dioxide corrosion experiment device of the present application is used for carbon dioxide corrosion behavior experiment, a plurality of samples are placed at different heights of the sample holder. The samples at different heights are respectively a top sample, a middle sample, and a bottom sample, which correspond to the first temperature section, the second temperature section, and the third temperature section of the reaction kettle 01 respectively. Experimental liquid is injected into the reaction kettle 01. Since the reaction kettle 01 is divided into the first temperature section, the second temperature section, and the third temperature section, the samples can be placed in different states by adjusting the liquid level and the heating temperature of different temperature sections of the reaction kettle 01.When the liquid level of the experimental liquid is higher than the bottom sample, the sample immersed in the experimental solution is subjected to liquid phase corrosion; when the liquid level of the experimental liquid is controlled at the third temperature section of the reaction kettle 01, at the middle position of the height of the bottom sample, the environment of the bottom sample is between the liquid phase and the supercritical CO2 interface, and the third temperature section is adjusted to be the environmental interval of gaseous CO2, and the temperature of the second temperature section is set to be under the supercritical condition, so that the middle sample is in the supercritical CO2 environment state, and the top sample is in the corrosion simulation of gaseous CO2. Since the sample holder penetrates the first temperature section, the second temperature section and the third temperature section of the reaction kettle 01, the corrosion data in different phase environments can be obtained by placing samples and corrosion monitoring probes in different temperature sections on the sample holder. Since the reaction kettle 01 is provided with a viewing window at the top, combined with a shooting camera, the dew point data under the influence of multiple parameters such as impurity components, temperature and pressure can be tested by observing the dew point on the viewing window. The first temperature section, the second temperature section and the third temperature section are respectively provided with observation windows, which can be combined with a shooting camera to monitor the change of the sample corrosion state with time.

[0019] Optionally, the reaction kettle 01 is provided with a pressure gauge 19 on the side wall, which is used to measure the pressure in the reaction kettle 01.

[0020] Optionally, the carbon dioxide corrosion experiment device further comprises a liquid deoxidization assembly connected to the liquid inlet pipe 11, and the experimental liquid enters the reaction kettle 01 after deoxidization by the deoxidization assembly.

[0021] Optionally, the liquid deoxidization assembly is a nitrogen deoxidization tank 03, which comprises a tank body, a piston 31 is arranged in the tank body, the upper part and the lower part of the piston 31 are respectively connected to a nitrogen gas source, the upper part of the piston 31 is provided with a first nitrogen inlet and a first nitrogen outlet, the lower part of the piston 31 is used for storing the experimental liquid, and the lower part of the piston 31 is provided with a second nitrogen inlet, a second nitrogen outlet, a liquid outlet and a dissolved oxygen test probe. The liquid outlet is communicated with the liquid inlet pipe 11. The experimental liquid is deoxidized by nitrogen introduced through the second nitrogen inlet, and when the dissolved oxygen content of the experimental liquid meets the requirements, the first nitrogen inlet in the upper part of the piston 31 is opened to press the experimental liquid into the reaction kettle 01 by N2 pressure. The first nitrogen inlet, the first nitrogen outlet, the second nitrogen inlet, the second nitrogen outlet and the liquid outlet are all provided with a switch valve. The nitrogen deoxidization tank 03 realizes the integration of liquid filling, deoxidization and gas adjustment, can accurately control the oxygen content of the liquid, and improves the experimental precision.

[0022] Optionally, the carbon dioxide corrosion experiment device further comprises a gas mixing assembly 121, a buffer device 122 and a pressurizing device 123, the pressurizing device 123 is a booster pump, the gas mixing assembly 121 comprises a plurality of gas cylinders, the gas outlets of the gas cylinders are communicated with the inner cavities of the buffer device 122, the gas outlets of the gas cylinders are respectively provided with flow meters, the pressurizing device 123 is arranged downstream of the buffer device 122, and the gas outlet end of the pressurizing device 123 is connected with the gas inlet pipe 12. Different experimental gases are stored in the gas cylinders, the gas proportion is adjusted through the flow meters, then the gases enter the buffer device 122, the buffer device 122 is provided with a pressure sensor, the gases are pressurized through the pressurizing device 123 after being buffered by the buffer device 122, and then the gases enter the reaction kettle 01 through the gas inlet pipe 12. Through the gas cylinders and the flow meters of the gas mixing assembly 121, the content of impurity gases in the reaction kettle 01 can be slightly adjusted during the carbon dioxide corrosion behavior experiment, the components CO2, SO2 and O2 of the gases can be controlled, and the experimental precision is improved.

[0023] Optionally, the reaction kettle heating assembly 02 is a flexible heating jacket, the flexible heating jacket is sleeved outside the reaction kettle 01, and the flexible heating jacket is electric heating.

[0024] Optionally, the sample holder is made of ceramic material, the sample holder is resistant to a temperature not less than 300 DEG C, and is matched with a corrosion coupon; and the sample holder penetrates through the first temperature section, the second temperature section and the third temperature section of the reaction kettle 01.

[0025] The above-described embodiments are only used to describe the preferred embodiments of the present application, and do not limit the scope of the present application, and various modifications and improvements to the technical solutions of the present application made by those skilled in the art without departing from the design spirit of the present application shall fall within the protection scope of the present application.

Claims

1. A carbon dioxide corrosion experimental apparatus, characterized in that, The reactor includes a reactor (01) and a reactor heating assembly (02). The reactor heating assembly (02) is used to heat the reactor (01) in sections, dividing the reactor (01) into a first temperature section, a second temperature section, and a third temperature section. The height of the reactor (01) is not less than 1.5 meters. The first temperature section, the second temperature section, and the third temperature section are temperature-controlled in sections. The first temperature section, the second temperature section, and the third temperature section respectively realize liquid phase corrosion, liquid phase and supercritical CO2 interface corrosion, and supercritical CO2 and gas phase CO2 corrosion simulation. A temperature sensor is provided on the side wall of the first temperature section, the second temperature section, and the third temperature section. The sensor has a first viewing window (16), a second viewing window (17), and a third viewing window (18) respectively provided on the side walls of the first temperature segment, the second temperature segment, and the third temperature segment. Optical observation equipment and a corrosion detection probe are respectively provided on the first viewing window (16), the second viewing window (17), and the third viewing window (18). The optical observation equipment includes a coaxial light source and a camera. A liquid inlet pipe (11) and a gas inlet pipe (12) are connected to the bottom of the reaction vessel (01). The liquid inlet pipe (11) is used to introduce experimental liquid into the reaction vessel (01), and the gas inlet pipe (12) is used to introduce experimental gas into the reaction vessel (01). 1) A fourth viewing window (13) and an air outlet (14) are provided at the top. The sample rack is set inside the reactor (01). The sample rack passes through the first temperature section, the second temperature section and the third temperature section of the reactor (01). The sample rack can be placed at positions corresponding to different temperature sections of the reactor (01). It also includes a liquid deoxygenation component. The liquid deoxygenation component is connected to the liquid inlet pipe (11). The experimental liquid enters the reactor (01) after passing through the deoxygenation component. The liquid deoxygenation component is a nitrogen deoxygenation tank (03). The nitrogen deoxygenation tank (03) includes a tank body. A piston (31) is set inside the tank body. The piston (31) The upper and lower parts of the piston (31) are connected to nitrogen gas sources respectively. The upper part of the piston (31) is provided with a first nitrogen gas inlet and a first nitrogen gas outlet. The lower part of the piston (31) is used to store experimental liquid. The lower part of the piston (31) is provided with a second nitrogen gas inlet, a second nitrogen gas outlet, a liquid outlet, and a dissolved oxygen test probe. The liquid outlet is connected to the liquid inlet pipe (11). The experimental liquid is deoxygenated by nitrogen introduced through the second nitrogen gas inlet. When the dissolved oxygen test probe detects that the dissolved oxygen content of the experimental liquid meets the requirements, the first nitrogen gas inlet of the upper part of the piston (31) is used to introduce gas, and the experimental liquid is pressed into the reaction vessel (01).

2. The carbon dioxide corrosion experimental apparatus according to claim 1, characterized in that, A pressure gauge (19) is installed on the side wall of the reactor (01), and the pressure gauge (19) is used to measure the pressure inside the reactor (01).

3. The carbon dioxide corrosion experimental apparatus according to claim 2, characterized in that, It also includes a gas mixing assembly (121), a buffer device (122), and a pressurizing device (123). The gas mixing assembly (121) includes multiple gas cylinders. The outlet of each gas cylinder is connected to the inner cavity of the buffer device (122). Each gas cylinder outlet is equipped with a flow meter. The pressurizing device (123) is located downstream of the buffer device (122). The outlet of the pressurizing device (123) is connected to the inlet pipe (12).

4. The carbon dioxide corrosion experimental apparatus according to claim 3, characterized in that, The reactor heating assembly (02) is a flexible heating sleeve, which is fitted over the reactor (01).

5. The carbon dioxide corrosion experimental apparatus according to claim 4, characterized in that, The sample holder is made of ceramic material.

6. The carbon dioxide corrosion experimental apparatus according to claim 5, characterized in that, The first nitrogen inlet, the first nitrogen outlet, the second nitrogen inlet, the second nitrogen outlet, and the liquid outlet are all equipped with switching valves.

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