CN115979939A - In-situ hydrogen permeation and corrosion coupling autoclave - Google Patents
In-situ hydrogen permeation and corrosion coupling autoclave Download PDFInfo
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- CN115979939A CN115979939A CN202310112675.4A CN202310112675A CN115979939A CN 115979939 A CN115979939 A CN 115979939A CN 202310112675 A CN202310112675 A CN 202310112675A CN 115979939 A CN115979939 A CN 115979939A
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Abstract
The invention discloses an in-situ hydrogen permeation and corrosion coupling autoclave, which comprises: the hydrogen permeation kettle is used for containing high-pressure hydrogen, and a first single window penetrates through the side wall of the hydrogen permeation kettle; the corrosion kettle is provided with a three-electrode system, the three-electrode system extends into the corrosion kettle, the side wall of the corrosion kettle is provided with a second single window in a penetrating way, the first single window and the second single window are connected in a sealing way, the first single window and the second single window are both of hollow structures, and the hydrogen permeation kettle and the corrosion kettle are mutually communicated through the first single window and the second single window; the sample clamp is arranged between the first single window and the second single window and is sealed through bolts, and the sample clamp is used for clamping and fixing a sample to be tested so that two sides of the sample to be tested are respectively exposed in the environments of the hydrogen permeation kettle and the corrosion kettle; the sample to be tested is connected with a working electrode connecting joint in the three-electrode system through a lead to form a working electrode.
Description
Technical Field
The invention relates to the technical field of hydrogen permeation test devices and corrosion test devices, in particular to an in-situ hydrogen permeation and corrosion coupling autoclave.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Hydrogen energy is an important link for promoting clean and efficient utilization of traditional fossil energy and supporting large-scale development of renewable energy. With the increase of energy demand and the improvement of environmental protection requirements, the installed capacity proportion of renewable energy sources will continuously increase in the future, but because the peak regulation capability of the current power system is limited, the phenomenon of wind abandoning and light abandoning is serious, and the development of renewable energy sources is hindered to a certain extent. The hydrogen is produced by electrolyzing water, so that large-scale energy storage and peak shaving coupling power grids are realized, the flexibility of a power system is improved, the utilization rate of renewable energy sources is favorably provided, a flexible and efficient multi-energy complementary system is formed, and the development of clean energy sources is promoted. The pipeline hydrogen transportation is an important way for realizing large-scale hydrogen transportation, and the transportation ways of pure hydrogen pipelines and hydrogen-doped natural gas pipelines are widely concerned and are vigorously developed at home and abroad at present.
On one hand, hydrogen molecules can be adsorbed on the surface of pipeline steel, dissociate to form hydrogen atoms and permeate into the metal of the pipeline, so that the plasticity and toughness of a matrix are reduced, the mechanical property of the pipeline is deteriorated, and meanwhile, the corrosion of the pipeline is aggravated by the hydrogen atoms entering the pipeline; on the other hand, for the hydrogen-doped natural gas pipeline, the conveying components contain carbon dioxide and water, so that the pipeline is subjected to internal corrosion, and meanwhile, under the actual conditions of burying, submarine pipelines and the like, corrosive substances also cause loss damage to the outer wall of the pipeline, and the permeation process of hydrogen atoms is further influenced by the internal corrosion and the external corrosion of the pipeline. Therefore, the research on the permeation corrosion of the hydrogen to the pipe and the influence on the corrosive factors of the material are particularly important for the natural gas pipeline and the pure hydrogen pipeline for hydrogen-doped transportation. The existing hydrogen permeation autoclave can only test the hydrogen permeation degree of hydrogen under an ideal non-corrosion process, and can not realize the in-situ measurement of the corrosion degree of hydrogen under the conditions of simultaneous occurrence and mutual synergistic promotion of hydrogen permeation and corrosion under the actual pipeline conveying working conditions (such as buried pipelines, submarine pipelines and the like).
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an in-situ hydrogen permeation and corrosion coupling autoclave.
In order to achieve the purpose, the invention is realized by the following technical scheme:
an in situ hydrogen infiltration and corrosion coupled autoclave comprising:
the hydrogen permeation kettle is used for containing high-pressure hydrogen, and a first single window penetrates through the side wall of the hydrogen permeation kettle;
the corrosion kettle is provided with a three-electrode system, the three-electrode system extends into the corrosion kettle, the side wall of the corrosion kettle is provided with a second single window in a penetrating way, the first single window and the second single window are connected in a sealing way, the first single window and the second single window are both of hollow structures, and the hydrogen permeation kettle and the corrosion kettle are communicated with each other through the first single window and the second single window;
the sample clamp is arranged between the first single window and the second single window and is sealed through bolts, and the sample clamp is used for clamping and fixing a sample to be tested so that two sides of the sample to be tested are respectively exposed in the environments of the hydrogen permeation kettle and the corrosion kettle;
the sample to be tested is connected with a working electrode connecting joint in the three-electrode system through a lead to form a working electrode.
Working electrode of three-electrode system 、 Reference electrode 、 The counter electrode is composed of a sample as a working electrode, and is connected with a working electrode connecting joint through a lead, and the reference electrode is a high-temperature high-pressure reference electrode.
In some embodiments, the first single viewing window and the second single viewing window are both of a three-step structure, the first step and the third step are hollow cylindrical, the second step is of a trumpet-shaped structure, the large diameter end of the trumpet-shaped structure is connected with the end part of the third step, and the small diameter end of the trumpet-shaped structure is connected with the end part of the first step.
Preferably, the sample clamp comprises a large gland, a clamping part is arranged in the large gland, and the first single view window and the second single view window are compressed through bolts and used for fixing the large gland.
Further preferably, the large gland is of a cylindrical structure, the inside of the large gland is of a hollow second-order structure, and the inner diameters of the first order and the second order which are sequentially connected are sequentially increased.
Preferably, the large gland is tightly matched with the three-step structure of the first single window and the second single window, and a sealing element is arranged between the large gland and the first single window.
Further preferably, the inner wall of the second stage in the large gland is provided with a first clamping part and a second clamping part for clamping the sample. The clamping force between the first clamping portion and the second clamping portion is maintained by the bolt.
In some embodiments, the corrosion kettle comprises a corrosion kettle body and a corrosion kettle cover, the corrosion kettle body and the corrosion kettle cover are connected through a bolt, and a sealing element is arranged between the corrosion kettle body and the corrosion kettle cover.
Preferably, the kettle cover of the corrosion kettle is provided with a gas channel, and the outer end of the gas channel is used for being connected with a valve.
In some embodiments, the hydrogen permeation kettle comprises a hydrogen permeation kettle body and a hydrogen permeation kettle cover, the hydrogen permeation kettle body and the hydrogen permeation kettle cover are connected through a bolt, and a sealing element is arranged between the hydrogen permeation kettle body and the hydrogen permeation kettle cover.
The hydrogen permeation kettle cover is provided with a gas channel, and the outer side end of the gas channel is used for being connected with a valve.
The beneficial effects achieved by one or more of the embodiments of the invention described above are as follows:
(1) According to the invention, two kettles are coupled, so that the hydrogen permeation test and the corrosion test can be respectively carried out on two surfaces of a sample at the same time under a high-pressure state. The three-electrode system can test the quantitative change of the corrosion degree under the coupling action of hydrogen permeation and corrosion in situ by an electrochemical method, and solves the problem that the existing hydrogen permeation autoclave can only test the hydrogen permeation degree of hydrogen in an ideal non-corrosion process, but cannot realize the in-situ measurement of the corrosion degree under the action of the simultaneous occurrence and mutual synergistic promotion of hydrogen permeation and corrosion under the actual pipeline conveying working conditions (such as buried pipelines, submarine pipelines and the like). Compared with the existing autoclave which can only simulate the non-corrosion process, the simulation test effect of the invention is more accurate and is closer to the actual situation.
(2) According to the invention, a sealing structure is arranged between the clamping part and the sample through the space between the single window of the permeation kettle and the gland and the space between the single window of the corrosion kettle and the gland; through using bolted construction to be connected between infiltration cauldron single window and the corrosion kettle single window, prevent that the inside hydrogen of autoclave from leaking, ensure that two cauldron coupling stage cauldron internal pressure maintain certain numerical value, guarantee test environment's security.
(3) When the corrosion kettle is coupled with the hydrogen permeation kettle, the corrosion kettle and the hydrogen permeation kettle are connected into a whole through the bolt, and after the bolt is removed, the corrosion kettle is provided with the conical plug, so that a high-temperature high-pressure corrosion test can be independently carried out; an electrolytic cell is configured for the hydrogen permeation kettle, and then the hydrogen permeation test can be independently carried out. Thereby realizing the multi-purpose of one kettle, realizing the function diversification of the device and maximizing the value.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 shows an isometric view of an in situ hydrogen permeation and corrosion coupled autoclave in an embodiment of the invention;
FIG. 2 shows a front view of an in situ hydrogen infiltration and corrosion coupled autoclave in an embodiment of the invention;
FIG. 3 shows a top view of an in situ hydrogen permeation and corrosion coupled autoclave in an embodiment of the present invention;
FIG. 4 shows a cross-sectional view of an in-situ hydrogen infiltration and corrosion coupled autoclave in an embodiment of the invention.
In the figure, 1, hydrogen permeates the kettle cover of the kettle; 2. a hydrogen permeation kettle body; 3. corroding the kettle cover of the kettle; 4. corroding the kettle body of the kettle; 5. the working electrode is connected with a joint; 6. a reference electrode; 7. a counter electrode; 8. a large gland; 9. a first clamping portion; 10. a second clamping portion; 11. a first single window; 12. a sample (working electrode); 13. a large bolt; 14. a small bolt; 15. a second single window; 16. an air intake passage; 17. an exhaust passage; 18. the blast valve is connected with the channel; 19. an instrument and meter interface.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The present invention will be further described with reference to the following examples.
As shown in fig. 1-4, the present embodiment provides an in-situ hydrogen permeation and corrosion coupled autoclave, which includes a hydrogen permeation kettle, a corrosion kettle, and a sample clamp, wherein the hydrogen permeation kettle 2 and the corrosion kettle body 4 are both autoclaves, the hydrogen permeation kettle can be filled with high-pressure hydrogen gas, and the corrosion kettle can be filled with a portion of corrosive solution and high-pressure gas. The sample anchor clamps can be used for centre gripping sample (working electrode) 12, and sample (working electrode) 12 one side contacts with the inside hydrogen of hydrogen infiltration cauldron body 2, and sample (working electrode) 12 opposite side passes through the wire and links to each other with working electrode attach fitting 5 to contact with corrosive solution, constitute three electrode system in the corrosion cauldron, real-time supervision sample (working electrode) 12 corrodes electrochemical signal under hydrogen infiltration and the influence of corrosion coupling, and then calculates the degree of corrosion.
As shown in fig. 1-4, the hydrogen permeation kettle body 2 has a first single window 11, the corrosion kettle body 4 has a second single window 15, and the hydrogen permeation kettle cover 1 and the corrosion kettle cover 3 are respectively provided with an air inlet channel 16, an air outlet channel 17, a burst valve connecting channel 18 and an instrument interface 19. The kettle cover 3 of the corrosion kettle is also provided with a three-electrode system, and the three-electrode system of the corrosion kettle consists of a sample (working electrode) 12 、 Reference electrode 6 、 A counter electrode 7, a lead wire led out from a sample (working electrode) 12 is connected with the working electrode connecting joint 5, and a reference electrode 6 is a high-temperature high-pressure reference electrode.
The hydrogen permeation kettle cover 1 is connected with the hydrogen permeation kettle body 2, the corrosion kettle cover 3 is connected with the corrosion kettle body 4 through the large bolts 13, the first single window and the second single window are connected through the small bolts 14, and then the two large pressing covers 8 are pressed tightly, so that the clamping part is clamped tightly, and the fixing of the sample (working electrode) 12 is realized.
This embodiment is through hydrogen infiltration cauldron and corrosion kettle coupling, and the simulation pipeline takes place hydrogen infiltration and corruption simultaneously to realize the normal position measurement of degree of corrosion. Compared with the existing high-pressure kettle which can only simulate hydrogen permeation under an ideal non-corrosive process, the simulation effect is more accurate and is closer to the actual situation.
As shown in FIG. 2 and FIG. 3, the single window 11 is located on the side wall of the kettle body, and is welded with the kettle body to form a whole, and is a hollow shell structure, the single window is a three-step structure, the first step and the third step are cylindrical, the first step is connected with the side wall of the kettle body, the diameter of the first step is smaller than that of the other steps, the diameter of the third step is larger, the second step is horn-shaped, and the first step and the third step are connected.
As shown in fig. 4, the sample clamp is composed of a large gland 8, a first clamping part 9 and a second clamping part 10, and is installed between a single window 11 of the hydrogen permeation kettle body 2 and a single window 15 of the corrosion kettle body 4 after the sample clamp is assembled. And then the single window 11 of the hydrogen permeation kettle body 2 and the single window 15 of the corrosion kettle body 4 are connected through a small bolt 14, so that the coupling of the hydrogen permeation kettle and the corrosion kettle is realized.
Big gland 8 is the cylinder structure, and big gland is inside to be cavity second order structure, and the internal diameter of consecutive first order, second order increases in proper order.
The second stage inside the large gland 8 is provided with a first clamping portion 9 and a second clamping portion 10 for clamping a sample (working electrode) 12. The first clamping part 9 is a second-order hollow cylinder, a cylinder with a set depth and a larger diameter is cut in the bottom, a rectangular groove is dug, an O-shaped sealing ring is arranged, and a cylinder with a set depth and a smaller diameter is cut in the top, so that a through hole is formed together. The second clamping part 10 is a three-step hollow cylinder, the outer diameter of the first step is sequentially increased, a through hole is formed in the first step, a rectangular groove is dug at the top, and an O-shaped sealing ring is arranged.
The sample (working electrode) 12 is a circular thin sheet, and is fixed by the first clamping portion 9 and the second clamping portion 10, and the sealing of high-pressure hydrogen is realized by the O-ring, and the fixing of the sample is realized by the small bolt 14, and the clamping force between the first clamping portion 9 and the second clamping portion 10 is maintained by the small bolt 14.
In order to prevent high-pressure gas in the autoclave body from leaking out of the single view window 11, the joint of the three-electrode structure and the valve cover, the sample clamp is connected with the single view window 11 in a sealing mode, and meanwhile the sample and the joint of the three-electrode structure and the valve cover are subjected to the same sealing treatment. Four O-shaped sealing rings are adopted. The four O-ring seals are respectively located between the first clamping portion 9 and the sample (working electrode) 12, between the second clamping portion 10 and the sample (working electrode) 12, between the large gland 8 and the third stage of the first single window 11 of the autoclave body 2, and between the large gland 8 and the third stage of the second single window 15 of the autoclave body 4.
The sample clamp is of a hollow structure and is used for clamping a sample (working electrode) 12, so that one side of the sample (working electrode) 12 is in contact with hydrogen in the hydrogen permeation kettle, and the other side of the sample (working electrode) 12 is connected with the working electrode connecting joint 5 through a lead and is in contact with a medium in the corrosion kettle.
The whole kettle body is made of Hastelloy, is a nickel-based corrosion-resistant alloy, has good corrosion resistance, hydrogen embrittlement resistance and thermal stability, and ensures the stability of the kettle body in the test process and the safety of the test.
When the coupling autoclave is assembled, the hydrogen permeation kettle cover 1 is connected with the hydrogen permeation kettle single-view window kettle body 2 through a large bolt 13; the O-shaped sealing rings are arranged in two rectangular grooves of a first clamping part 9 and a second clamping part 10, and a sample (working electrode) 12 is fixed through the first clamping part 9 and the second clamping part 10; the first clamping part 9 and the second clamping part 10 are arranged between two large gland second-stage hollow cylinders, and a sample (working electrode) 12 is clamped;
connecting the working electrode to the joint 5 、 Reference electrode 6 、 The counter electrode 7 and the kettle cover 3 of the corrosion kettle form a whole through screw threads, and the kettle cover 3 of the corrosion kettle is connected with the kettle body 4 of the single-view window of the corrosion kettle through a large bolt 13; leading out a lead and a sample from a working electrode connecting joint 5 in a three-electrode systemAs an electrode) 12 is connected at the rear end; the single window 11 of the hydrogen permeation kettle body 2 and the single window 15 of the corrosion kettle body 4 are connected through the small bolt 14, so that the sample (working electrode) 12 is fixed, the coupling of the hydrogen permeation kettle and the corrosion kettle is realized, and the installation is finished.
When in use, the hydrogen permeation kettle and the corrosion kettle firstly use nitrogen to remove residual gas in the kettle body, and the nitrogen is filled and discharged for three times. And after the current is stable, filling required test substances respectively, and performing related test tests.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An in-situ hydrogen infiltration and corrosion coupled autoclave, characterized by: the method comprises the following steps:
the hydrogen permeation kettle is used for containing high-pressure hydrogen, and a first single window penetrates through the side wall of the hydrogen permeation kettle;
the corrosion kettle is provided with a three-electrode system, the three-electrode system extends into the corrosion kettle, the side wall of the corrosion kettle is provided with a second single window in a penetrating way, the first single window and the second single window are connected in a sealing way, the first single window and the second single window are both of hollow structures, and the hydrogen permeation kettle and the corrosion kettle are mutually communicated through the first single window and the second single window;
the sample clamp is arranged between the first single window and the second single window and is sealed through bolts, and the sample clamp is used for clamping and fixing a sample to be tested so that two sides of the sample to be tested are respectively exposed in the environments of the hydrogen permeation kettle and the corrosion kettle;
the sample to be tested is connected with a working electrode connecting joint in the three-electrode system through a lead to form a working electrode.
2. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 1, wherein: first single window and second single window are three-order structure, and first order and third order are hollow circular cylinder shape, and the second order is loudspeaker column structure, and its major diameter end and third order end connection, its minor diameter end and first order end connection.
3. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 2, wherein: the sample clamp comprises a large gland, a clamping part is arranged in the large gland, and the first single window and the second single window are tightly pressed through bolts and used for fixing the large gland.
4. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 3, wherein: the big gland is of a cylindrical structure, the inside of the big gland is of a hollow second-order structure, and the inner diameters of a first order and a second order which are sequentially connected are sequentially increased.
5. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 4, wherein: the big gland closely cooperates with the third order structure of first single window and the single window of second, is provided with sealing element between big gland and the first single window.
6. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 5, wherein: and a first clamping part and a second clamping part for clamping a sample are arranged on the inner wall of the second stage in the large gland.
7. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 1, wherein: the corrosion kettle comprises a corrosion kettle body and a corrosion kettle cover, the corrosion kettle body and the corrosion kettle cover are connected through bolts, and a sealing element is arranged between the corrosion kettle body and the corrosion kettle cover.
8. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 7, wherein: and a gas channel is arranged on the kettle cover of the corrosion kettle, and the outer side end of the gas channel is used for being connected with a valve.
9. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 1, wherein: the hydrogen permeation kettle comprises a hydrogen permeation kettle body and a hydrogen permeation kettle cover, the hydrogen permeation kettle body and the hydrogen permeation kettle cover are connected through bolts, and a sealing element is arranged between the hydrogen permeation kettle body and the hydrogen permeation kettle cover.
10. The in situ hydrogen infiltration and corrosion coupled autoclave of claim 9, wherein: the hydrogen permeation kettle cover is provided with a gas channel, and the outer side end of the gas channel is used for being connected with a valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310112675.4A CN115979939A (en) | 2023-02-13 | 2023-02-13 | In-situ hydrogen permeation and corrosion coupling autoclave |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310112675.4A CN115979939A (en) | 2023-02-13 | 2023-02-13 | In-situ hydrogen permeation and corrosion coupling autoclave |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116858917A (en) * | 2023-06-25 | 2023-10-10 | 中国石油大学(华东) | For supercritical CO 2 Hydrogen permeation testing device for pipeline steel in conveying environment |
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2023
- 2023-02-13 CN CN202310112675.4A patent/CN115979939A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116858917A (en) * | 2023-06-25 | 2023-10-10 | 中国石油大学(华东) | For supercritical CO 2 Hydrogen permeation testing device for pipeline steel in conveying environment |
| CN116858917B (en) * | 2023-06-25 | 2024-02-06 | 中国石油大学(华东) | For supercritical CO 2 Hydrogen permeation testing device for pipeline steel in conveying environment |
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