CN106841020B - Full-automatic oxygen-deficient corrosion test device and method - Google Patents
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Abstract
A full-automatic oxygen-deficient corrosion test device and a method thereof, the device mainly comprises an automatic control system, an inert gas bottle, a reactor, a preparation device, a sealed respirator, a doser, a sample hanger, a pipeline, an electric valve, a liquid level sensor, a thermocouple, an oxygen electrode and the like; the invention also discloses a test method of the device; the preparation of the oxygen-poor water and the preparation of the solution are carried out step by step, so that solute is prevented from being blown off due to the fact that nitrogen is directly introduced into the solution to remove oxygen; all the test processes are carried out in one system, and the sealed respirator not only ensures that the system is isolated from the atmosphere, maintains the dissolved oxygen and the concentration in the reactor to be stable, but also ensures that the system breathes freely without pressure build-up; the invention can realize the accurate configuration of any oxygen-poor concentration (0 ppb-8000 ppb) test solution, and can accurately control, and the test process is carried out fully automatically.
Description
Technical Field
The invention relates to the technical field of oxygen-deficient corrosion tests, in particular to a full-automatic oxygen-deficient corrosion test device and method.
Background
In the research work of corrosion and corrosion prevention, oxygen is taken as a key influencing factor, and the corrosion phenomenon under different dissolved oxygen concentrations (oxygen-free, oxygen-poor and oxygen-rich) needs to be tested and researched. If the dissolved oxygen content in the solution is changed by directly introducing gas into the test solution, and the gas-liquid distribution coefficient of the solute in the test solution is large, the solute can be blown off greatly in the ventilation process, so that the concentration of the solution is reduced, and the test conditions are changed. If the test water with qualified dissolved oxygen is prepared in advance and then used for preparing the test solution, the dissolved oxygen content of the solution is changed due to the leakage of air in the operation process, and the reaction conditions are also changed. The current technology is difficult to realize the synchronous and accurate control of the concentration of the medicament and the concentration of dissolved oxygen in the test solution.
Disclosure of Invention
In order to solve the defects, the invention aims to provide a full-automatic oxygen-deficient corrosion test device and a method, wherein oxygen-deficient water preparation, solution preparation and a corrosion test are carried out step by step, so that solute blowing-off caused by directly ventilating the solution is avoided, and solution change caused by preparing the solution with water with qualified dissolved oxygen in an open environment is also avoided; all processes are finished in one system, and the system is always in a sealed and free breathing state, so that the system is ensured not to leak air, and the stability and controllability of the dissolved oxygen of the system are maintained; the dissolved oxygen is monitored in real time, so that the dissolved oxygen of the test solution and the concentration of the medicament are accurately controlled; all test processes are automatically controlled by a PLC and are carried out fully automatically.
In order to achieve the purpose, the invention adopts the following technical scheme:
a full-automatic oxygen-deficient corrosion test device comprises an inert gas bottle 1, a preparation device 5, a reactor 6 and a sealed breather 7, wherein a specified amount of demineralized water is filled in the preparation device 5, a certain water level is kept in the sealed breather 7, and scales are marked on the reactor 6; the inert gas bottle 1 is connected with a first pipeline L1, the first pipeline L1 is divided into two paths, one path is connected to the upper part of the demineralized water liquid level of the preparation device 5 through a second pipeline L2, the outlet of the other path is provided with a second electric valve K2, the outlet of the second electric valve K2 is divided into two paths, one path is connected to the demineralized water of the preparation device 5 through a third pipeline L3, the other path is connected with a sixth pipeline L6 led into the reactor 6 through a fourth pipeline L4, a fifth pipeline L5 inserted to the upper part of the demineralized water level of the preparation device 5 is also connected with the sixth pipeline L6 led into the reactor 6, the seventh pipeline L7 is communicated with the water in the reactor 6 and the sealed respirator 7, an eighth pipeline L8 positioned on the water level of the sealed respirator 8 is connected to the outside, the gas discharged in the test process is discharged to the outside, and the test device is in a sealed and non-pressure-holding state; the second pipeline L2, the fourth pipeline L4 and the fifth pipeline L5 are respectively provided with a first electric valve K1, a third electric valve K3 and a fourth electric valve K4, the fourth pipeline L4 is provided with a doser 2, an oxygen electrode 3 and a first thermocouple R1 are inserted into desalted water of the preparation device 5, a second thermocouple R2 and a liquid level sensor Y are inserted into the reactor 6, and the top of the reactor is hung with a sample hanger 4; the system is characterized by also comprising a control system consisting of a PLC8, a man-machine operation interface 9 and a display interface 10, wherein the control system is connected with a first electric valve K1, a second electric valve K2, a third electric valve K3, a fourth electric valve K4, a first thermocouple R1, a second thermocouple R2, an oxygen electrode 3 and a liquid level sensor Y; the PLC8 receives signals transmitted by the first thermocouple R1, the second thermocouple R2, the liquid level sensor Y and the oxygen electrode 3, and opens or closes the first electric valve K1, the second electric valve K2, the third electric valve K3 and the fourth electric valve K4 according to the set upper and lower limit values and the set delay time so as to achieve the purpose of controlling the preparation of the oxygen-enriched water, the preparation of the solution, the progress and the end of the test.
The first thermocouple R1 and the second thermocouple R2 are used for monitoring the temperature in the preparation vessel 5 and the reactor 6, and the values and signals are transmitted to the display interface 10 and the PLC8, respectively.
The level sensor Y is located in the reactor 6 for monitoring the solution level, the values and signals being transmitted to the display interface 10 and the PLC8, respectively.
The oxygen electrode 3 is positioned in the preparation device 5 and is used for detecting the dissolved oxygen content in the preparation device 5, and the numerical value and the signal are respectively transmitted to the display interface 10 and the PLC8; the preparation device 5 is used for preparing oxygen-depleted water with specified dissolved oxygen concentration.
The valve bodies of the first electric valve K1, the second electric valve K2, the third electric valve K3 and the fourth electric valve K4 are made of stainless steel or plastic corrosion-resistant materials, and the opening and closing of the valves are automatically controlled by a PLC8.
The human-computer operation interface 9 is used for setting test parameters, wherein the test parameters comprise dissolved oxygen content, solution liquid level, test time and test temperature; the display interface 10 receives and displays values from the oxygen electrode 3, the first thermocouple R1, the second thermocouple R2, and the level sensor Y.
And the nitrogen cylinder 1 is connected into the test device through a first pipeline L1 and is used for oxygen removal and conveying of oxygen-poor water and test agents in the solution preparation process.
The doser 2 is made of a corrosion-resistant material; the sample hanging device 4 is made of corrosion-resistant material and is used for hanging a corrosion test piece.
The preparation device 5, the reactor 6 and the sealed breather 7 are columnar, spherical, triangular or square, and are made of stainless steel, organic glass, glass or plastic corrosion-resistant materials; the first pipeline L1, the second pipeline L2, the third pipeline L3, the fourth pipeline L4, the fifth pipeline L5, the sixth pipeline L6, the seventh pipeline L7 and the eighth pipeline L8 are made of stainless steel, glass or plastic corrosion-resistant materials.
The test method of the full-automatic oxygen-deficient corrosion test device comprises the following steps:
the first step is oxygen-deficient water preparation: adding a specified amount of desalted water into the preparation device 5, and setting test time, test temperature, liquid medicine volume and dissolved oxygen content by a human-computer operation interface 9; the PLC8 automatically controls to open the second electric valve K2 and the fourth electric valve K4, inert gas is introduced into desalted water in the preparation device 5 through the first pipeline L1 and the third pipeline L3 to be deoxidized, the gas enters the reactor 6 through the fifth pipeline L5 and the sixth pipeline L6 to be deoxidized, the gas enters the sealed respirator 7 through the seventh pipeline L7, and finally the gas is exhausted to the outside through the eighth pipeline L8;
the second step is test solution preparation: after the oxygen electrode 3 detects that the oxygen-poor water-soluble oxygen in the preparation device 5 meets the test requirements, the PLC8 automatically controls to close the second electric valve K2 and the fourth electric valve K4, automatically opens the first electric valve K1 and the third electric valve K3 after the content and the temperature of the dissolved oxygen in the preparation device reach the set values for 3min, inert gas enters the preparation device 5 through the first pipeline L1 and the second pipeline L2, the oxygen-poor water in the preparation device 5 and the test medicament in the medicament adding device 2 are added into the reactor 6 through the third pipeline L3, the fourth pipeline L4, the sixth pipeline L6 and the medicament adding device 2, the first electric valve K1 and the third electric valve K3 are automatically closed after the liquid level in the reactor 6 reaches the set values, the test solution preparation is completed, and the test is started;
the third step is corrosion test: when the test time reaches a set value, the heating system is automatically closed, and a test ending prompt tone is sent.
Compared with the prior art, the invention has the following advantages:
the invention can realize the configuration of the oxygen-poor test solution with any dissolved oxygen concentration (0 ppb-8000 ppb), and the preparation of the oxygen-poor water and the solution preparation are carried out step by step, thereby avoiding solute blowing-off caused by directly introducing gas into the solution and avoiding the change of the dissolved oxygen caused by using water with qualified dissolved oxygen to configure the solution in an open environment. All processes are completed in one system, and the system is always in a sealed and free breathing state, so that the system is ensured not to leak air, and the dissolved oxygen and the medicament concentration of the system are maintained stable. The dissolved oxygen is monitored in real time, and the dissolved oxygen of the test solution and the concentration of the medicament are accurately controlled. All test processes are automatically controlled by a PLC and are carried out fully automatically.
Drawings
FIG. 1 is a schematic structural diagram of a full-automatic oxygen-deficient corrosion test apparatus according to the present invention.
Detailed Description
The structural and operational principles of the present invention are explained in further detail below with reference to the accompanying drawings and the detailed description.
Example 1:
as shown in fig. 1, the full-automatic oxygen-deficient corrosion test device of this embodiment mainly includes an inert gas bottle 1, a doser 2, an oxygen electrode 3, a sample hanger 4, a preparation device 5, a reactor 6, a sealed respirator 7, pipelines (L1-L8), electric valves (K1-K4), thermocouples (R1, R2), a liquid level sensor Y, and a PLC8 control system.
All the containers are square, and the containers, the pipelines and the electric valves are all made of PVC materials.
In the test method of the corrosion test device of the embodiment, the dissolved oxygen concentration is 0ppb, the test temperature is 40 ℃, the test time is 4h, and the solution volume is 600mL, the test device is placed in a constant temperature water bath at 40 ℃, the sample hanger is used for hanging a carbon steel corrosion test piece 4, and 1000mL of demineralized water is added into the preparation device 5. The first step is oxygen-deficient water preparation: PLC8 automatic control opens second motorised valve K2 and fourth motorised valve K4, and nitrogen gas carries out the deoxidization through the demineralized water that first pipeline L1 and third pipeline L3 let in the preparation ware 5, and gas gets into reactor 6 through fifth pipeline L5 and sixth pipeline L6 again, gets into sealed respirator 7 through seventh pipeline L7 again, and is discharged gas to outdoor by eighth pipeline L8 at last, has accomplished the deoxidization to reactor 6 and system's pipeline. After 20min, the dissolved oxygen content is stabilized between 0ppb and 2ppb, and the second electric valve K2 and the fourth electric valve K4 are automatically closed. The second step is test solution preparation: after dissolved oxygen and temperature reach set values and are kept stable for 3min, the first electric valve K1 and the third electric valve K3 are automatically opened, nitrogen enters the preparation device 5 through the first pipeline L1 and the second pipeline L2, oxygen-poor water in the preparation device 5 and test agents in the chemical adding device 2 are added into the reactor 6 through the third pipeline L3, the fourth pipeline L4, the sixth pipeline L6 and the chemical adding device 2, when the liquid level in the reactor 6 rises to 600mL, the first electric valve K1 and the third electric valve K3 are automatically closed, test solution preparation is completed, and a test is started. When the test time reaches 4h, the heating system is automatically closed, and a test ending prompt tone is sent.
Example 2:
as shown in figure 1, the full-automatic oxygen-deficient corrosion test device and method mainly comprise a nitrogen cylinder 1, a doser 2, an oxygen electrode 3, a sample hanging device 4, a preparation device 5, a reactor 6, a sealed breather 7, pipelines (L1-L8), electric valves (K1-K4), thermocouples (R1 and R2), a liquid level sensor Y, a PLC8 control system and the like.
All containers are columnar, the material is organic glass, and the pipeline and the electric valve are made of PVC materials.
According to the test method of the corrosion test device, the dissolved oxygen concentration is 700ppb, the test temperature is 45 ℃, the test time is 4h, and the solution volume is 700mL, the test device is placed in a constant-temperature water bath at 45 ℃, a carbon steel corrosion test piece is hung on a sample hanging device (4), and 1000mL of demineralized water is added into a preparation device (5). The first step is oxygen-deficient water preparation: PLC8 automatic control opens second motorised valve K2 and fourth motorised valve K4, and nitrogen gas carries out the deoxidization through the demineralized water that first pipeline L1 and third pipeline L3 let in the preparation ware 5, and gas gets into reactor 6 through fifth pipeline L5 and sixth pipeline L6 again, gets into sealed respirator 7 through seventh pipeline L7 again, and is discharged gas to outdoor by eighth pipeline L8 at last, has accomplished the deoxidization to reactor 6 and system's pipeline. After 16min, the dissolved oxygen content is stabilized between 700ppb and 720ppb, and the second electric valve K2 and the fourth electric valve K4 are automatically closed. The second step is test solution preparation: after dissolved oxygen and temperature reach set values and are kept stable for 3min, the first electric valve K1 and the third electric valve K3 are automatically opened, nitrogen enters the preparation device 5 through the first pipeline L1 and the second pipeline L2, oxygen-poor water in the preparation device 5 and test agents in the chemical adding device 2 are added into the reactor 6 through the third pipeline L3, the fourth pipeline L4, the sixth pipeline L6 and the chemical adding device 2, when the liquid level in the reactor 6 rises to 700mL, the first electric valve K1 and the third electric valve K3 are automatically closed, test solution preparation is completed, and a test is started. When the test time reaches 4h, the heating system is automatically closed, and a test ending prompt tone is sent.
Example 3:
as shown in figure 1, the full-automatic oxygen-deficient corrosion test device and method mainly comprise a nitrogen cylinder 1, a doser 2, an oxygen electrode 3, a sample hanger 4, a preparation device 5, a reactor 6, a sealed breather 7, pipelines (L1-L8), electric valves (K1-K4), thermocouples (R1 and R2), a liquid level sensor Y, a PLC8 control system and the like.
All containers are spherical, made of glass, pipelines are made of polytetrafluoroethylene, and the electric valve is made of 304 stainless steel.
In the test method of the corrosion test device of the embodiment, the dissolved oxygen concentration of 6000ppb, the test temperature of 50 ℃, the test time of 5h and the solution volume of 500mL are set by a human-computer interface, the test device is placed in a constant-temperature water bath at 50 ℃, the sample hanging device 4 is hung on a carbon steel corrosion test piece, and 1000mL of demineralized water is added into the preparation device 5. The first step is oxygen-deficient water preparation: PLC8 automatic control opens second motorised valve K2 and fourth motorised valve K4, and nitrogen gas carries out the deoxidization through the demineralized water that first pipeline L1 and third pipeline L3 let in the preparation ware 5, and gas gets into reactor 6 through fifth pipeline L5 and sixth pipeline L6 again, gets into sealed respirator 7 through seventh pipeline L7 again, and is discharged gas to outdoor by eighth pipeline L8 at last, has accomplished the deoxidization to reactor 6 and system's pipeline. After 16min, the dissolved oxygen content is stabilized between 6000ppb and 6050ppb, and the second electric valve K2 and the fourth electric valve K4 are automatically closed. The second step is test solution preparation: after dissolved oxygen and temperature reach set values and are kept stable for 3min, the first electric valve K1 and the third electric valve K3 are automatically opened, nitrogen enters the preparation device 5 through the first pipeline L1 and the second pipeline L2, oxygen-poor water in the preparation device 5 and test agents in the chemical adding device 2 are added into the reactor 6 through the third pipeline L3, the fourth pipeline L4, the sixth pipeline L6 and the chemical adding device 2, when the liquid level in the reactor 6 rises to 500mL, the first electric valve K1 and the third electric valve K3 are automatically closed, test solution preparation is completed, and a test is started. When the test time reaches 5h, the heating system is automatically closed, and a test ending prompt tone is sent.
Claims (10)
1. The utility model provides a full-automatic poor oxygen corrosion test device which characterized in that: the device comprises an inert gas bottle (1), a preparation device (5), a reactor (6) and a sealed breather (7), wherein a specified amount of demineralized water is filled in the preparation device (5), a certain water level is kept in the sealed breather (7), and the reactor (6) is marked with scales; the inert gas bottle (1) is connected with a first pipeline (L1), the first pipeline (L1) is divided into two paths, one path is connected to the position above the demineralized water liquid level of the preparation device (5) through a second pipeline (L2), the other path is provided with a second electric valve (K2), the outlet of the second electric valve (K2) is divided into two paths, one path is connected to the demineralized water of the preparation device (5) through a third pipeline (L3), the other path is connected with a sixth pipeline (L6) introduced into the reactor (6) through a fourth pipeline (L4), a fifth pipeline (L5) inserted to the position above the demineralized water level of the preparation device (5) is also connected with the sixth pipeline (L6) introduced into the reactor (6), a seventh pipeline (L7) is communicated with the water in the reactor (6) and the sealed respirator (7), an eighth pipeline (L8) positioned on the water level of the sealed respirator (8) is connected to the outside, discharged gas in the test process is discharged to the outside, and the test device is in a sealed and non-pressure-holding state; the second pipeline (L2), the fourth pipeline (L4) and the fifth pipeline (L5) are respectively provided with a first electric valve (K1), a third electric valve (K3) and a fourth electric valve (K4), the fourth pipeline (L4) is provided with a doser (2), an oxygen electrode (3) and a first thermocouple (R1) are inserted into desalted water of the preparation device (5), a second thermocouple (R2) and a liquid level sensor (Y) are inserted into the reactor (6), and the top of the reactor is hung with a sample hanger (4); the device is characterized by also comprising a control system consisting of a PLC (8), a man-machine operation interface (9) and a display interface (10), wherein the control system is connected with a first electric valve (K1), a second electric valve (K2), a third electric valve (K3), a fourth electric valve (K4), a first thermocouple (R1), a second thermocouple (R2), an oxygen electrode (3) and a liquid level sensor (Y); the PLC (8) receives signals transmitted by the first thermocouple (R1), the second thermocouple (R2), the liquid level sensor (Y) and the oxygen electrode (3), and opens or closes the first electric valve (K1), the second electric valve (K2), the third electric valve (K3) and the fourth electric valve (K4) according to set upper and lower limit values and delay time so as to achieve the purpose of controlling oxygen-enriched water preparation, solution preparation, test proceeding and ending.
2. The full-automatic oxygen-deficient corrosion test device according to claim 1, characterized in that: the first thermocouple (R1) and the second thermocouple (R2) are used for monitoring the temperature in the preparation device (5) and the reactor (6), and the numerical value and the signal are respectively transmitted to the display interface (10) and the PLC (8).
3. The full-automatic oxygen-deficient corrosion test device according to claim 1, characterized in that: the liquid level sensor (Y) is positioned in the reactor (6) and is used for monitoring the liquid level of the solution, and the numerical value and the signal are respectively transmitted to the display interface (10) and the PLC (8).
4. The full-automatic oxygen-deficient corrosion test device according to claim 1, characterized in that: the oxygen electrode (3) is positioned in the preparation device (5) and is used for detecting the dissolved oxygen content in the preparation device (5), and the numerical value and the signal are respectively transmitted to the display interface (10) and the PLC (8); the preparation device (5) is used for preparing the oxygen-depleted water with the specified dissolved oxygen concentration.
5. The full-automatic oxygen-deficient corrosion test device and method according to claim 1, characterized in that: the valve bodies of the first electric valve (K1), the second electric valve (K2), the third electric valve (K3) and the fourth electric valve (K4) are made of stainless steel or plastic corrosion-resistant materials, and the opening and closing of the valves are automatically controlled by a PLC (8).
6. The full-automatic oxygen-deficient corrosion test device and method according to claim 1, characterized in that: the human-computer operation interface (9) is used for setting test parameters, wherein the test parameters comprise dissolved oxygen content, solution liquid level, test time and test temperature; the display interface (10) receives and displays values from the oxygen electrode (3), the first thermocouple (R1), the second thermocouple (R2) and the liquid level sensor (Y).
7. The full-automatic oxygen-deficient corrosion test device and method according to claim 1, characterized in that: the nitrogen gas bottle (1) is connected to the test device through a first pipeline (L1) and is used for oxygen removal and conveying of oxygen-poor water and test agents in the solution preparation process.
8. The full-automatic oxygen-deficient corrosion test device and method according to claim 1, characterized in that: the doser (2) is made of a corrosion-resistant material; the sample hanging device (4) is made of corrosion-resistant materials and is used for hanging a corrosion test piece.
9. The full-automatic oxygen-deficient corrosion test device and method according to claim 1, characterized in that: the preparation device (5), the reactor (6) and the sealed respirator (7) are columnar, spherical, triangular or square, and the materials are stainless steel, organic glass, glass or plastic corrosion-resistant materials; the first pipeline (L1), the second pipeline (L2), the third pipeline (L3), the fourth pipeline (L4), the fifth pipeline (L5), the sixth pipeline (L6), the seventh pipeline (L7) and the eighth pipeline (L8) are made of stainless steel, glass or plastic corrosion-resistant materials.
10. The testing method of the fully automatic oxygen-deficient corrosion testing apparatus according to any one of claims 1 to 9, characterized in that: the method comprises the following steps:
the first step is oxygen-deficient water preparation: adding a specified amount of desalted water into the preparation device (5), and setting test time, test temperature, liquid medicine volume and dissolved oxygen content by a man-machine operation interface (9); the PLC (8) automatically controls to open the second electric valve (K2) and the fourth electric valve (K4), inert gas is introduced into desalted water in the preparation device (5) through the first pipeline (L1) and the third pipeline (L3) to remove oxygen, the gas enters the reactor (6) through the fifth pipeline (L5) and the sixth pipeline (L6), the reactor (6) is removed with oxygen, the gas enters the sealed respirator (7) through the seventh pipeline (L7), and finally the gas is discharged outdoors through the eighth pipeline (L8);
the second step is test solution preparation: after the oxygen electrode (3) detects that the oxygen-poor water-soluble oxygen in the preparation device (5) meets the test requirement, the PLC (8) automatically controls to close the second electric valve (K2) and the fourth electric valve (K4), after the content and the temperature of the dissolved oxygen in the preparation device reach the set value for 3min, the first electric valve (K1) and the third electric valve (K3) are automatically opened, inert gas enters the preparation device (5) through the first pipeline (L1) and the second pipeline (L2), the oxygen-poor water in the preparation device (5) and a test medicament in the medicament adding device (2) are added into the reactor (6) through the third pipeline (L3), the fourth pipeline (L4), the sixth pipeline (L6) and the medicament adding device (2), the first electric valve (K1) and the third electric valve (K3) are automatically closed after the liquid level in the reactor (6) reaches the set value, the test solution preparation is completed, and the test is started;
the third step is corrosion test: when the test time reaches a set value, the heating system is automatically closed, and a test ending prompt tone is sent.
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