CN113834765A - Device and method for testing corrosion resistance of material - Google Patents

Device and method for testing corrosion resistance of material Download PDF

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Publication number
CN113834765A
CN113834765A CN202010513971.1A CN202010513971A CN113834765A CN 113834765 A CN113834765 A CN 113834765A CN 202010513971 A CN202010513971 A CN 202010513971A CN 113834765 A CN113834765 A CN 113834765A
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China
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reaction kettle
pressure
temperature
corrosion resistance
kettle
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CN202010513971.1A
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黄传艳
王世洁
翟科军
崔龙兵
苏鹏
李林涛
万小勇
李渭亮
徐燕东
黄亮
张佳
彭明旺
马国锐
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China Petroleum and Chemical Corp
Sinopec Northwest Oil Field Co
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China Petroleum and Chemical Corp
Sinopec Northwest Oil Field Co
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    • 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

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Abstract

The invention provides a device and a method for testing the corrosion resistance of a material, which comprises a reaction kettle, wherein a temperature regulating device and a stirring device are arranged on the reaction kettle, and corrosive liquid is contained in the reaction kettle; the control box is connected with the reaction kettle and controls the temperature adjusting device and the stirring device; and the gas supply system is connected with the reaction kettle and used for supplying gas which does not influence the experiment to the reaction kettle and adjusting the gas pressure in the reaction kettle. The device is suitable for the research of high-temperature and high-pressure corrosion behaviors and mechanisms, solves the problem that the traditional corrosion evaluation experiment can not be carried out on various strong corrosion media under the conditions of high temperature and high pressure, does not need a special kettle for special purpose, and can meet the test requirements of various high-temperature and high-pressure conditions only by using one test device.

Description

Device and method for testing corrosion resistance of material
Technical Field
The invention relates to a device and a method for testing corrosion resistance of a material, in particular to a device and a method for testing corrosion resistance of a material under high temperature and high pressure.
Background
The metal corrosion is spread in various fields of industry, agriculture and national defense construction, the service life of the material is shortened, and huge economic loss is caused and even serious harm is caused. Among them, the high-temperature high-pressure multiphase flow environment in oil and gas wells and a plurality of corrosive components such as H2S, CO2, Cl-cause various pipelines or structures to fail in the form of acid or alkali corrosion under high temperature and high pressure. The simulation experiment of the high-temperature and high-pressure corrosion process is an important means for screening and evaluating oil/gas pipelines, screening and evaluating corrosion inhibitors and researching the corrosion resistance and corrosion mechanism of the materials. However, under the conditions of high temperature and high pressure, the experimental device has high requirements on high temperature resistance, high pressure resistance, acid resistance, alkali resistance and salt resistance, the experimental device is easy to corrode and lose efficacy, and meanwhile, the price of related products in the market is high at present, so that the extensive research on the high-temperature and high-pressure corrosion behavior and mechanism is greatly influenced.
At present, the commonly used autoclave is a stainless steel kettle with the pressure below 10MPa, and can not meet special test requirements, such as high temperature and high pressure, various corrosion conditions and the like. For some harsh corrosive environments, standard parts often cannot be adopted and need to be customized again, taking a hydrochloric acid corrosion resistance experiment as an example, a hastelloy reaction kettle is customized, the manufacturing cost is about 20 ten thousand, and the development of tests is limited to a certain extent. The problem of high cost is solved by a manufacturer by embedding the Hastelloy liner, but the bottom of the liner is easy to corrode when acid-base corrosion environments are found to be alternated.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a device and a method for testing the corrosion resistance of a material, which are suitable for researching high-temperature and high-pressure corrosion behaviors and mechanisms, solve the problem that the traditional corrosion evaluation experiment can not be carried out on various strong corrosion media under the conditions of high temperature and high pressure, do not need special kettles for special use any more, and can meet the testing requirements of various conditions of high temperature and high pressure by only using one testing device.
In one aspect of the present invention, a device for testing corrosion resistance of a material is provided, which includes:
the reaction kettle is provided with a temperature adjusting device and a stirring device, and corrosive liquid is contained in the reaction kettle;
the control box is connected with the reaction kettle and controls the temperature adjusting device and the stirring device; and
connect reation kettle's gas supply system, gas supply system to reation kettle provides the gas that does not influence the experiment, and adjusts atmospheric pressure in the reation kettle.
The invention has the further improvement that the reaction kettle comprises a high-pressure kettle body, the upper end of the high-pressure kettle body is provided with a high-pressure kettle cover, the high-pressure kettle cover is provided with an air inlet pipe and an air outlet pipe, and the air inlet pipe is connected with the air supply system; and the stirring device is fixed on the autoclave cover.
The invention is further improved in that the temperature adjusting device comprises a heating device arranged on the side wall of the autoclave body, a heat preservation and insulation layer is arranged on the outer layer of the heating device, and a polytetrafluoroethylene inner container is arranged on the inner layer of the heating device.
The stirring device is further improved in that the stirring device comprises a control motor connected with the control box, a rotating shaft of the control motor is rotatably connected to the middle part of the reaction kettle cover, and the rotating shaft extends into the reaction kettle; the end part of the rotating shaft is provided with a stirring paddle;
wherein the height of the stirring paddle in the reaction kettle is not more than two thirds of the height of the high-pressure kettle body.
The invention has the further improvement that a temperature sensor hole is arranged on the autoclave cover, a temperature sensor is arranged in the temperature sensor hole, and the temperature sensor is connected with the control box; the control box controls the heating device to start and stop according to the temperature information detected by the temperature sensor.
The invention is further improved in that a pressure sensor hole is arranged on the autoclave cover, a pressure gauge is arranged on the pressure sensor hole, and a pressure sensor is arranged on the pressure gauge.
The invention has the further improvement that the upper end of the high-pressure kettle body is provided with an annular connecting body connected with the high-pressure kettle cover, and the positions on the connecting body corresponding to the edge of the high-pressure kettle cover are both provided with connecting holes; and the high-pressure kettle body is connected with the high-pressure kettle cover by installing bolts in the connecting holes.
The invention is further improved in that hastelloy C-276 is overlaid on the inner wall of the autoclave body.
In another aspect of the invention, the invention also provides a method for testing the corrosion resistance of the material at high temperature and high pressure, and the device is used for testing the corrosion resistance of the material; the method comprises the following steps:
injecting the corrosive liquid into the reaction kettle, closing the high-pressure kettle cover, controlling the temperature regulating device by the control box to heat the corrosive liquid to the experimental temperature and keep the temperature, and starting the stirring device to a preset rotating speed;
putting a sample to be tested into a reaction kettle, supplying gas which does not influence the experiment into the reaction kettle through a gas supply system, and stopping gas supply when the pressure in the reaction kettle reaches a set value;
and starting a corrosion experiment, observing the corrosion process of the corrosion liquid on the sample to be tested, and recording the time.
The invention is further improved in that the corrosive liquid is 20% HCl or saturated salt water.
Compared with the prior art, the invention has the advantages that:
the device and the method for testing the corrosion resistance of the material are suitable for researching high-temperature and high-pressure corrosion behaviors and mechanisms, solve the problem that a plurality of strong corrosion media cannot be subjected to corrosion evaluation experiments under high-temperature and high-pressure conditions in the past, do not need special kettles, and can meet the testing requirements of the plurality of high-temperature and high-pressure conditions by using one testing device.
Drawings
Preferred embodiments of the present invention will be described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic structural diagram of a material corrosion resistance testing device according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the construction of an autoclave lid according to an embodiment of the invention;
FIG. 3 is a graph of the average corrosion rate of coupons at 80 deg.C, 120 deg.C, 10MPa, 20MPa, 30MPa for 1 day in one example;
FIG. 4 is a graph of the average corrosion rate of coupons at 80 deg.C, 120 deg.C, 10MPa, 20MPa, 30MPa for 2 days in one example;
FIG. 5 is a graph showing the average corrosion rate of coupons at 80 deg.C, 120 deg.C, 10MPa, 20MPa, and 30MPa for 3 days in one example.
In the drawings, like parts are provided with like reference numerals. The figures are not drawn to scale.
The meaning of the reference symbols in the drawings is as follows: 1. the device comprises a reaction kettle, 2, an autoclave body, 3, an autoclave cover, 11, a stirring device, 12, a control motor, 13, a rotating shaft, 14, a stirring paddle, 21, a heating device, 22, a heat preservation and insulation layer, 23, a polytetrafluoroethylene inner container, 24, a connecting body, 25, a bolt, 31, an air inlet pipe, 32, an air outlet pipe, 33, a temperature sensor hole, 34, a pressure sensor hole, 35, a connecting hole, 36, a temperature sensor, 37, a pressure sensor, 38 and a pressure gauge.
Detailed Description
In order to make the technical solutions and advantages of the present invention more apparent, exemplary embodiments of the present invention are described in further detail below with reference to the accompanying drawings. It is clear that the described embodiments are only a part of the embodiments of the invention, and not an exhaustive list of all embodiments. And the embodiments and features of the embodiments may be combined with each other without conflict.
Fig. 1 schematically shows a material corrosion resistance testing apparatus according to an embodiment of the present invention, which includes a reaction vessel 1. The reaction vessel 1 is a cylindrical reactor, and contains an etching solution for a top-view side view. Be provided with temperature regulation apparatus and agitating unit 11 on reation kettle 1, temperature regulation apparatus is used for adjusting the temperature in reation kettle 1, and agitating unit 11 is used for mixing the corrosive liquid in reation kettle 1 and the sample that awaits measuring. A control box is arranged outside the reaction kettle 1 and connected with the temperature adjusting device and the stirring device 11, and the temperature adjusting device and the stirring device 11 are controlled to operate. Reation kettle 1 still is connected with gas supply system, gas supply system provides gas for reation kettle 1 to can adjust atmospheric pressure. Wherein, the gas supply device provides gas which does not influence the experimental reaction, such as nitrogen, inert gas and the like.
In one embodiment, the reaction vessel 1 includes an autoclave body 2, and the autoclave body 2 is a cylindrical container, and an autoclave cover 3 is disposed on the upper portion of the autoclave body. As shown in fig. 2, an air inlet pipe 31 and an air outlet pipe 32 are arranged on the autoclave cover 3, the air inlet pipe is connected with the air supply system, and valves are arranged on the air inlet pipe 31 and the air outlet pipe 32. The stirring device 11 is fixed on the autoclave cover 3.
When the device for testing the corrosion resistance of the material according to the embodiment is used, the autoclave body 2 can be filled with corrosive liquid or a sample to be tested by opening and closing the autoclave cover 3. The gas inlet pipe and the gas outlet pipe on the high-pressure kettle cover 3 can adjust gas to enter and exit, and adjust the pressure in the reaction kettle 1. In this embodiment, the gas inlet pipe extends into the bottom of the reaction kettle 1, and the inlet of the gas outlet pipe is positioned at the upper part of the reaction kettle 1 and above the liquid level.
In one embodiment, as shown in fig. 1, the temperature adjusting device is arranged on the side wall of the autoclave body 2, the temperature adjusting device comprises a heating device 21, the heating device 21 is arranged in the middle of the high-pressure attachment, the outer layer of the heating device 21 is provided with a heat insulation layer 22, and the inner layer of the heating device 21 is provided with a polytetrafluoroethylene inner container 23.
In the device for testing corrosion resistance of material according to this embodiment, the temperature adjusting device can adjust the temperature in the autoclave body 1, wherein the heating device 21 is connected to the control box and controlled by the control box, and after the test experiment is started, the control box controls the heating device 21 to heat the space in the autoclave body 2. When the temperature reaches the set temperature, the control box closes the heating device 21, the temperature in the reaction kettle 1 will slowly drop under the action of the heat insulation layer 22, and after the temperature drops to a certain temperature, the heating device 21 is restarted.
In one embodiment, the stirring device 11 includes a control motor 12, the control motor 12 is disposed outside the reaction kettle 1 and connected to a control box, and the control box can control the control motor 12 to start and stop. A rotating shaft 13 of the control motor 12 is connected to the autoclave cover 3, one end of the rotating shaft 13 is positioned at the upper end of the autoclave cover 3 and is connected to the control motor 12, the other end of the rotating shaft extends into the reaction kettle 1, and the end part of the rotating shaft is provided with a stirring paddle 14. In this embodiment, the height of the stirring paddle 14 in the autoclave 1 is not more than two thirds of the height of the autoclave body 2.
In a preferred embodiment, as shown in fig. 2, a temperature sensor hole 33 is formed in the autoclave cover 3, a temperature sensor 36 is arranged in the temperature sensor hole 33, and the temperature sensor 36 is connected with the control box; the control box controls the heating device 21 to start and stop according to the temperature information detected by the temperature sensor 36.
When the device for testing the corrosion resistance of the material according to the embodiment is used, the temperature control device can be automatically adjusted. After the temperature is set, the control box controls the heating device 21 to heat the reaction kettle 1, the temperature sensor 36 monitors the temperature in the reaction kettle 1 in real time in the heating process, and the heating device 21 is closed and stops heating after the temperature is heated to the set temperature. In the test experiment process, the temperature will slowly drop, and when the temperature drops to a certain value, the heating device 21 is restarted, so that the temperature in the reaction kettle 1 is kept stable.
In one embodiment, the autoclave lid 3 is provided with a pressure sensor hole 34, the pressure sensor hole 34 is provided with a pressure gauge 38, and the pressure gauge 38 is provided with a pressure sensor 37. The pressure sensor 37 can be connected to the control box, the control box is connected to the valves on the gas inlet pipe and the gas outlet pipe 32, and when the pressure in the reaction kettle 1 exceeds or is less than a preset pressure value, the control box controls the gas inlet or gas outlet to adjust. The pressure gauge 38 can display the pressure value in the reaction kettle 1, and an operator can manually adjust the pressure value according to the reading on the pressure gauge 38.
In one embodiment, the upper end of the autoclave body 2 is provided with a connecting body 24, the connecting body 24 is an annular structure, and the inner ring of the connecting body is connected with the upper end of the autoclave body 2. The connecting body 24 is opposite to the edge of the autoclave lid 3 and is connected by bolts 25.
In this embodiment, the edge of the autoclave cover 3 is provided with a plurality of connecting holes 35, the connecting body 24 of the autoclave body 2 is also provided with a plurality of connecting holes 35, and the connecting holes 35 on the autoclave cover 3 and the connecting holes 35 on the connecting body 24 are oppositely arranged. The bolts 25 pass through the two sets of opposite connecting holes 35 and are fastened through nuts, so that the autoclave cover 3 and the autoclave body 2 are fixedly connected. Through bolted connection's mode, not only connect firmly, still be convenient for the dismouting. Meanwhile, the connector 24 has a certain width and is tightly connected with the autoclave cover 3, so that the airtightness of the whole reaction kettle 1 is improved.
In this embodiment, the autoclave cover 3 is further provided with an air inlet pipe hole and an air outlet pipe hole, the air inlet pipe hole is used for installing the air inlet pipe 31, and the air storage pipe hole is used for installing the air outlet pipe 32.
In one embodiment, hastelloy C-276 is deposited on the inner wall of autoclave body 2. In this embodiment, the main body of the autoclave body 2 can be made of 316L stainless steel, embedded into the ptfe inner container 23, and part of the components are hastelloy C-276, so as to meet the requirements of high-temperature and high-pressure corrosion experiments with various corrosive media (acid, alkali and salt), and greatly reduce the manufacturing cost for producing the autoclave 1 with high-temperature and high-pressure resistance to acid, alkali and salt. The device can reach the temperature of 0-250 ℃ and the pressure of 0-50 MPa.
According to another aspect of the invention, a method for testing the corrosion resistance performance of the material is also provided, and the method is tested by the device for testing the corrosion resistance performance of the material in the embodiment. The method comprises the following steps:
injecting the corrosive liquid into the reaction kettle 1, closing the high-pressure kettle cover 3, controlling the temperature regulating device by the control box to heat the corrosive liquid to the experimental temperature and keep the temperature, and starting the stirring device 11 to a preset rotating speed;
putting a sample to be tested into a reaction kettle 1, supplying gas which does not influence the experiment into the reaction kettle 1 through a gas supply system, and stopping gas supply when the pressure in the reaction kettle 1 reaches a set value;
and starting a corrosion experiment, observing the corrosion process of the corrosion liquid on the sample to be tested, and recording the time.
Preferably, the corrosive solution is 20% HCl or saturated salt solution. Other corrosive liquids can be changed according to the needs of experiments.
The following is a description of specific examples.
In the case of the example 1, the following examples are given,
firstly, adding saturated salt solution into a kettle, closing a high-pressure kettle cover 3, starting a heating and heat-preserving device through an external control box, heating the corrosive liquid in the high-pressure kettle to a set temperature and preserving heat, adjusting the control box, and changing the rotating speed of a rotating shaft to enable the rotating speed to reach 20 r/min.
Then, the treated 2024 aluminum alloy test piece having a size of 50mm × 25mm × 2mm (length × width × thickness) was hung on a sample rack and placed in a kettle, the autoclave lid (3) was closed, and the bolts were tightened. Introducing nitrogen, and stopping introducing the nitrogen when the readings on the pressure gauge 38 and the pressure sensor 37 reach the preset pressure; experimental testing was started.
The corrosion of 2024 aluminum alloy in saturated saline water was tested at the same rotation speed and different temperatures and pressures by the apparatus, and the test results are shown in fig. 3, 4 and 5. FIG. 3 is a graph showing the average corrosion rate data for one day of coupons at 80 deg.C, 120 deg.C, 10MPa, 20MPa, and 30 MPa; FIG. 4 is the average corrosion rate data for two days at 80 deg.C, 120 deg.C, 10MPa, 20MPa, 30MPa coupon; FIG. 5 is the average corrosion rate data of three days after the coupon is coated at 80 deg.C, 120 deg.C and 10MPa, 20MPa and 30MPa, and by integrating the corrosion data of different coupon times, it can be known that the average corrosion rate increases with the increase of temperature, and the influence of pressure on the corrosion behavior is slight.
In the case of the example 2, the following examples are given,
firstly, adding 20% HCl into a kettle, closing a high-pressure kettle cover 3, starting a heating and heat-preserving device through an external control box, heating corrosive liquid in the high-pressure kettle to 100 ℃ and preserving heat, adjusting the control box, and changing the rotating speed of a rotating shaft to enable the rotating speed to reach 10 r/min.
After that, the treated 2024 silver-plated test tube having dimensions of 101mm × 10mm × 100mm (outer diameter × wall thickness × height) was placed in the autoclave, the autoclave lid 3 was closed, and the bolts were tightened. Introducing nitrogen, and stopping introducing the nitrogen when the readings on the pressure gauge 38 and the pressure sensor 37 are reached; experimental testing was started.
The device is used for testing the corrosion condition of the 2024 aluminum alloy silver-plated test tube in saturated saline at the rotating speed of 10r/min and under the conditions of 100 ℃ and 30MPa, and the test result shows that after 4 hours and 48 minutes of coupon corrosion, the 2024 aluminum alloy silver-plated test tube only loses 4.04g of weight, the condition of coating cracking occurs in a weak link of the coating, and the process has an optimized space.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, the appended claims are intended to be construed to include preferred embodiments and all such changes and/or modifications as fall within the scope of the invention, and all such changes and/or modifications as are made to the embodiments of the present invention are intended to be covered by the scope of the invention.

Claims (10)

1. A material corrosion resistance testing device is characterized by comprising:
the device comprises a reaction kettle (1), wherein a temperature adjusting device and a stirring device (11) are arranged on the reaction kettle (1), and corrosive liquid is contained in the reaction kettle (1);
the control box is connected with the reaction kettle (1) and controls the temperature adjusting device and the stirring device (11); and
connect the gas supply system of reation kettle (1), gas supply system to reation kettle (1) provides the gas that does not influence the experiment, and adjusts atmospheric pressure in reation kettle (1).
2. The material corrosion resistance testing device according to claim 1, wherein the reaction kettle (1) comprises an autoclave body (2), an autoclave cover (3) is arranged at the upper end of the autoclave body (2), an air inlet pipe (31) and an air outlet pipe (32) are arranged on the autoclave cover (3), and the air inlet pipe is connected with the air supply system; and the stirring device (11) is fixed on the autoclave cover (3).
3. The material corrosion resistance testing device according to claim 2, wherein the temperature adjusting device comprises a heating device (21) arranged on the side wall of the autoclave body (2), the outer layer of the heating device (21) is provided with a heat insulation layer (22), and the inner layer of the heating device (21) is provided with a polytetrafluoroethylene inner container (23).
4. The material corrosion resistance testing device according to claim 3, wherein the stirring device (11) comprises a control motor (12) connected with the control box, a rotating shaft (13) of the control motor (12) is rotatably connected to the middle part of the cover of the reaction kettle (1), and the rotating shaft (13) extends into the reaction kettle (1); the end part of the rotating shaft (13) is provided with a stirring paddle (14);
wherein the height of the stirring paddle (14) in the reaction kettle (1) is not more than two thirds of the height of the high-pressure kettle body (2).
5. The material corrosion resistance testing device according to any one of claims 1 to 4, wherein a temperature sensor hole (33) is formed in the autoclave cover (3), a temperature sensor (36) is arranged in the temperature sensor hole (33), and the temperature sensor (36) is connected with the control box; the control box controls the heating device (21) to start and stop according to the temperature information detected by the temperature sensor (36).
6. The material corrosion resistance testing device according to any one of claims 1 to 5, wherein a pressure sensor hole (34) is formed in the autoclave cover (3), a pressure gauge (38) is arranged on the pressure sensor hole (34), and a pressure sensor (37) is arranged on the pressure gauge (38).
7. The material corrosion resistance testing device according to claim 6, wherein an annular connecting body (24) connected with the autoclave cover (3) is arranged at the upper end of the autoclave body (2), and connecting holes (35) are arranged on the connecting body (24) and at positions corresponding to the edge of the autoclave cover (3); the high-pressure kettle body (2) and the high-pressure kettle cover (3) are connected through mounting bolts (25) in the connecting holes (35).
8. The device for testing the corrosion resistance of the material according to claim 6, wherein hastelloy C-276 is overlaid on the inner wall of the autoclave body (2).
9. A method for testing corrosion resistance of a material at high temperature and high pressure, which is characterized by comprising the steps of testing by the device for testing corrosion resistance of a material according to any one of claims 1 to 8; it includes:
injecting the corrosive liquid into the reaction kettle (1), closing the high-pressure kettle cover (3), controlling the temperature regulating device by the control box to heat the corrosive liquid to an experimental temperature and preserve heat, and starting the stirring device (11) to a preset rotating speed;
putting a sample to be tested into a reaction kettle (1), providing gas which does not influence the experiment into the reaction kettle (1) through a gas supply system, and stopping gas supply when the pressure in the reaction kettle (1) reaches a set value;
and starting a corrosion experiment, observing the corrosion process of the corrosion liquid on the sample to be tested, and recording the time.
10. The method for testing the corrosion resistance of the material under high temperature and high pressure according to claim 9, wherein the corrosion solution is 20% HCl or saturated salt solution.
CN202010513971.1A 2020-06-08 2020-06-08 Device and method for testing corrosion resistance of material Pending CN113834765A (en)

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Publication number Priority date Publication date Assignee Title
CN115672212A (en) * 2022-08-25 2023-02-03 中国工程物理研究院激光聚变研究中心 Method for removing shell type HDC microsphere silicon mold core with micropores and corrosion device
CN115672212B (en) * 2022-08-25 2024-06-21 中国工程物理研究院激光聚变研究中心 Method for removing silicon mold cores of microporous shell type HDC microspheres

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Application publication date: 20211224