CN117168978A - Corrosion pit volume-based evaluation method for hydrogen sulfide stress corrosion resistance of oil well pipe - Google Patents
Corrosion pit volume-based evaluation method for hydrogen sulfide stress corrosion resistance of oil well pipe Download PDFInfo
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- 238000005260 corrosion Methods 0.000 title claims abstract description 99
- 230000007797 corrosion Effects 0.000 title claims abstract description 99
- 239000003129 oil well Substances 0.000 title claims abstract description 32
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 26
- 238000011156 evaluation Methods 0.000 title claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 55
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000005452 bending Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000004364 calculation method Methods 0.000 claims abstract description 14
- 238000005259 measurement Methods 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 12
- 238000004381 surface treatment Methods 0.000 claims abstract description 12
- 238000013001 point bending Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 2
- 239000012085 test solution Substances 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
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- 229910000831 Steel Inorganic materials 0.000 description 5
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- RBORURQQJIQWBS-QVRNUERCSA-N (4ar,6r,7r,7as)-6-(6-amino-8-bromopurin-9-yl)-2-hydroxy-2-sulfanylidene-4a,6,7,7a-tetrahydro-4h-furo[3,2-d][1,3,2]dioxaphosphinin-7-ol Chemical compound C([C@H]1O2)OP(O)(=S)O[C@H]1[C@@H](O)[C@@H]2N1C(N=CN=C2N)=C2N=C1Br RBORURQQJIQWBS-QVRNUERCSA-N 0.000 description 1
- 206010041541 Spinal compression fracture Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses an evaluation method for hydrogen sulfide stress corrosion resistance of an oil well pipe based on a corrosion pit volume, which comprises the following steps: (1) sample processing and surface treatment; (2) bending load test; (3) etch pit parameter measurement and volume calculation. The method comprises the steps of testing the stress corrosion resistance of the oil well pipe material in a service environment or a simulated actual environment, evaluating the hydrogen sulfide stress corrosion resistance of the oil well pipe material by calculating the volume of a corrosion pit, quantitatively grading a sample which is not invalid under bending loading, evaluating the practicability of the oil well pipe material in a specific working condition environment, and guiding material selection and equipment maintenance.
Description
Technical Field
The invention provides a method for accurately evaluating the hydrogen sulfide stress corrosion resistance of an oil well pipe, in particular to a method for further evaluating the stress corrosion resistance of the oil well pipe by analyzing the corrosion pit volume on the surface of a sample which is not failed in bending loading, and belongs to the field of corrosion performance detection.
Background
The steel for oil well pipe accounts for 40% or more of the total amount of steel for petroleum industry. In recent years, with the exploration and development of ultra-deep, ultra-high temperature and ultra-high corrosion harsh environment oil and gas wells, the working condition environment of the oil and gas wells is generally provided with high temperature, high pressure and high CO 2 High H 2 S, high Cl - The characteristics of high mineralization degree, and the complex and harsh working conditions and the special operation process lead to the stress corrosion failure of the oil well pipe, thereby seriously affecting the normal production operation of the oil and gas field.
Stress corrosion cracking (Stress Corrosion Cracking-SCC) refers to the phenomenon of delayed cracking, or delayed fracture, of a tensile stressed metallic material in some specific media due to the synergistic effect of the corrosive media and stress. Compared with other forms of corrosion damage, the stress corrosion cracking crack has the advantages of high crack growth speed, burst fracture and highest risk coefficient.
According to the situation, the oil well pipe is required to be subjected to hydrogen sulfide stress corrosion performance detection and evaluation before practical application, and the standard TM 0177-2016H 2 Sulfide stress corrosion cracking and stress corrosion cracking resistance of metals in S environment, and GB/T4157-20The 17 methods of the laboratory test of the metal cracking resistance in the hydrogen sulfide environment in the special form comprise a standard tensile test, a bending beam test, a C-shaped ring test, a double cantilever beam test (DCB) and the like. The tensile, bending and C-shaped ring tests can directly evaluate the hydrogen sulfide corrosion resistance of the oil well pipe, but have the defects of severe test conditions, high sample processing precision requirements, failure and non-failure information only given by test results, and cannot quantitatively evaluate the hydrogen sulfide corrosion resistance grade. The standard double cantilever beam test provides the capability of measuring the EC expansion resistance, K of the metal material ISSC For SSC, K IEC The method is used for EC under more common conditions, and according to the crack initiation type of a fracture mechanism test, the method is expressed as a critical stress intensity factor, and the method can quantify the direct grade of crack propagation resistance, but has the advantages of complex model design and theoretical calculation, high requirements on quality of operators, difficult field test and incapability of realizing the method.
The four-point bending test in the ASTM G39-2021 standard is a conventional method for evaluating the stress corrosion resistance of the oil well pipe, adopts an A-method standard solution, has simple equipment, has low requirements on operators, only uses 10 times of amplification to observe whether cracks exist on the surface of a sample, only gives out failure and non-failure information on test results, and can not evaluate the stress corrosion resistance performance grade of the sample for the sample without failure, needs to be comprehensively evaluated by combining other experimental means, prolongs the test period or needs to purchase new equipment, and has high cost requirements.
Disclosure of Invention
The invention aims to provide an evaluation method for the hydrogen sulfide stress corrosion resistance of an oil well pipe based on the corrosion pit volume, which is characterized in that a bending loading non-failure sample is subjected to surface rust removal treatment, the stress corrosion resistance of the oil well pipe is evaluated through surface morphology analysis, corrosion pit parameter measurement and corrosion pit volume calculation, and the hydrogen sulfide stress corrosion resistance of the sulfur-resistant oil well pipe is further quantitatively rated.
The evaluation method for the hydrogen sulfide stress corrosion resistance of the oil well pipe based on the corrosion pit volume comprises the following steps:
(1) Sample processing and surface treatment: processing the sample into a proper size and performing surface treatment;
(2) Bending load test: according to the nominal yield strength of the oil well pipe, bending loading test is carried out on the sample according to a certain loading proportion, then the clamp and the sample are integrally put into a closed storage tank for hydrogen sulfide stress corrosion test, after a certain test period is completed, the sample which is not failed is subjected to surface rust removal treatment and is cleaned;
(3) Corrosion pit parameter measurement and volume calculation: and carrying out morphological analysis and parameter measurement on the corrosion pit on the surface of the sample by adopting a microscope, and calculating the volume of the corrosion pit as a final result. Since the corrosion loss amount of the sample surface was correlated with the volume of the corrosion pit, the hydrogen sulfide stress corrosion resistance of the oil well pipe material was evaluated by calculating the volume of the corrosion pit.
Further, the surface treatment is used for removing residues and grease on the surface of the sample, an ultrasonic cleaner is adopted for cleaning the sample twice in acetone, and then absolute ethyl alcohol is used for cleaning the sample once; the time for one time of cleaning is 1-2min.
Further, the certain loading proportion is 50% -90% of the nominal yield strength, the test solution is NaCE standard A solution, and the test period is 360-720h.
Further, the bending loading test adopts a four-point bending loading mode, so that uniform longitudinal tensile stress is generated on the convex surface part of the sample between two inner fulcra, the stress is linearly reduced to zero from the inner fulcra to the outer fulcra, and the stress on the surface of the sample is uniform.
Further, the non-failed test sample is: the test specimen after completing the hydrogen sulfide stress corrosion test period was not broken, and the surface of the test specimen was observed with a 10-fold magnifying glass, and macroscopic cracks were not seen.
Further, the specimen surface is a surface area generating uniform longitudinal tensile stress, i.e., a surface of a convex specimen.
Further, the microscope is a laser confocal microscope, and proper magnification is selected; for the convenience of observation and calculation, the sample is placed on the stage as required, the longitudinal direction or length direction of the sample is parallel to the X-axis, the transverse direction or width direction of the sample is parallel to the Y-axis, the length direction of the etch pit is the Y-axis, and the width direction is the X-axis.
Further, the corrosion pit is uniformly deformed under the action of longitudinal tensile stress, and the original punctiform corrosion pit is expanded along the direction perpendicular to the tensile stress, so that the corrosion pit is lengthened and deepened, and a ship-shaped corrosion pit with a certain width is formed.
Further, the non-failure sample is subjected to surface rust removal treatment, and then is cleaned and dried.
Further, the parameter measurements are measuring the length, width and depth of the etch pit.
Further, the boat-shaped corrosion pit has a length of l (in μm), a width of d (in μm), a depth of h (in μm), a cross section perpendicular to the length direction of approximately a semi-elliptical shape, and an area of S (in μm 2 ) The volume V (in μm) of the etch pit was calculated by the integral method 3 )；
The calculation formula of the ship-shaped corrosion pit volume is simplified as follows:
further, the smaller the volume of the corrosion pit, the better the hydrogen sulfide stress corrosion resistance of the oil well pipe material.
The invention has the beneficial effects that:
the method comprises the steps of testing the stress corrosion resistance of the oil well pipe material in a service environment or a simulated actual environment, evaluating the hydrogen sulfide stress corrosion resistance of the oil well pipe material by calculating the volume of a corrosion pit, quantitatively grading a sample which is not invalid in bending loading, evaluating the practicability of the oil well pipe material in a specific working condition environment, guiding material selection and equipment maintenance, and ensuring that the evaluation method is accurate.
Drawings
FIG. 1 shows the three-dimensional morphology (loading ratio: 50% and 720 h) of the sample after washing in example 1.
FIG. 2 shows the three-dimensional morphology (loading ratio 80% and 360 h) of the sample after washing in example 2.
FIG. 3 shows the three-dimensional morphology (loading ratio 90%, 720 h) of the sample after washing in example 3.
Fig. 4 is a simplified diagram of a boat-type corrosion pit.
Fig. 5 is a schematic illustration of parameter measurements of a boat-type corrosion pit, where a is a top view, b is a front view, and c is a side view.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
Example 1
The specimens used in the test were A, B two kinds of 110S oil country tubular goods, which were two different kinds of oil country tubular goods (for example, oil country tubular goods having different materials or different processes such as rolling and heat treatment, and the explanation of the following examples is the same here). Three parallel samples of each material, test methods consisted of a sample processing and surface treatment, b bending loading test, c etch pit parameter measurement, d etch pit volume calculation.
Processing the sample in the step a to obtain a sample with the size of 115mm, 15mm, 5mm and the surface finish of 0.3 mu m; the surface treatment adopts acetone to wash twice, absolute ethyl alcohol to wash once, and residues and grease on the surface are removed;
b, loading the bending loading test in a four-point bending loading mode according to 50% of the nominal yield strength of the oil well pipe, after loading, integrally placing the sample and the clamp into a closed storage tank for performing a stress corrosion resistance test, wherein the sample solution is saturated hydrogen sulfide A solution (nace standard), the test period is 720h, after the test is finished, removing the surface corrosion products of the samples which are not failed according to the standard GB/T-19292.4, cleaning, and placing the samples into a dryer for 24h;
c, in the step of measuring the corrosion pit parameters, a laser confocal microscope is adopted, the amplification factor is 400, a sample is placed on an objective table according to the requirement, the longitudinal direction, namely the length direction, of the sample is parallel to an X-axis, the transverse direction, namely the width direction, of the sample is parallel to a Y-axis, namely the length direction, namely the corrosion pit is the Y-axis, the width direction is the X-axis, the surface morphology is shown in fig. 1, 3 corrosion pits are selected from the surface of each steel sample, and the length l, the width d and the depth h of the corrosion pits are calculated through matched software;
and d, carrying out corrosion pit volume calculation in the step c into a formula (1), obtaining the volume of the corrosion pit, taking the average value of the three volumes, and calculating the result as shown in the table 1, wherein the result can be seen from the result: the hydrogen sulfide stress corrosion resistance of the material A is better than that of the material B.
Table 1 results of calculation of etch pit volume on sample surface
Example 2
The test samples used in the test are A, B two 110S oil well pipes, three parallel samples of each material, and the test method comprises the steps of sample processing and surface treatment, bending loading test b, corrosion pit parameter measurement c and corrosion pit volume calculation d.
Processing the sample in the step a to obtain a sample with the size of 115mm, 15mm, 5mm and the surface finish of 0.3 mu m; the surface treatment adopts acetone to wash twice, absolute ethyl alcohol to wash once, and residues and grease on the surface are removed;
b, loading the bending loading test in a four-point bending loading mode according to 80% of the nominal yield strength of the oil well pipe, after loading, integrally placing the sample and the clamp into a closed storage tank for performing a stress corrosion resistance test, wherein the sample solution is saturated hydrogen sulfide A solution (nace standard), the test period is 360h, after the test is finished, removing the surface corrosion products of the samples which are not failed according to the standard GB/T-19292.4, cleaning, and placing the samples into a dryer for 24h;
c, in the step of measuring the parameters of the corrosion pits, a laser confocal microscope is adopted, the amplification factor is 400, a sample is placed on a stage according to the requirement, the longitudinal direction, namely the length direction, of the sample is parallel to an X-axis, the transverse direction, namely the width direction, of the sample is parallel to a Y-axis, namely the length direction, namely the Y-axis, the width direction, of the corrosion pits is the X-axis, the surface morphology is shown in fig. 2, 3 corrosion pits are selected from the surface of the sample of each steel grade, and the length l, the width d and the depth h of the corrosion pits are calculated through matched software;
and d, calculating the volume of the corrosion pit in the step c, namely, bringing the parameters measured in the step c into a formula (1), obtaining the volume of the corrosion pit, taking the average value of the three volumes, and calculating the result as shown in the table 2, wherein the result can be seen. The hydrogen sulfide stress corrosion resistance of the material A is better than that of the material B.
TABLE 2 calculation of etch pit volume for sample surfaces
Example 3
The test samples used in the test are A, B two 110S oil well pipes, three parallel samples of each material, and the test method comprises the steps of sample processing and surface treatment, bending loading test b, corrosion pit parameter measurement c and corrosion pit volume calculation d.
Processing the sample in the step a to obtain a sample with the size of 115mm, 15mm, 5mm and the surface finish of 0.3 mu m; the surface treatment adopts acetone to wash twice, absolute ethyl alcohol to wash once, and residues and grease on the surface are removed;
b, loading the bending loading test in a four-point bending loading mode according to 80% of the nominal yield strength of the oil well pipe, after loading, integrally placing the sample and the clamp into a closed storage tank for performing a stress corrosion resistance test, wherein the sample solution is saturated hydrogen sulfide A solution (nace standard), the test period is 720h, after the test is finished, removing the surface corrosion products of the samples which are not failed according to the standard GB/T-19292.4, cleaning, and placing the samples into a dryer for 24h;
c, in the step of measuring the corrosion pit parameters, a laser confocal microscope is adopted, the amplification factor is 400, a sample is placed on an objective table according to the requirement, the longitudinal direction, namely the length direction, of the sample is parallel to an X-axis, the transverse direction, namely the width direction, of the sample is parallel to a Y-axis, namely the length direction, namely the corrosion pit is the Y-axis, the width direction is the X-axis, the surface morphology is shown in fig. 3, 3 corrosion pits are selected from the surface of each steel sample, and the length l, the width d and the depth h of the corrosion pits are calculated through matched software;
and d, calculating the volume of the corrosion pit in the step c, namely, bringing the parameters measured in the step c into a formula (1), obtaining the volume of the corrosion pit, taking the average value of the three volumes, and calculating the result as shown in the table 3, wherein the result can be seen. The hydrogen sulfide stress corrosion resistance of the material A is better than that of the material B.
TABLE 3 calculation of etch pit volume for sample surfaces
Claims (9)
1. The evaluation method of the hydrogen sulfide stress corrosion resistance of the oil well pipe based on the corrosion pit volume is characterized by comprising the following steps of:
(1) Sample processing and surface treatment: processing the sample into a set size and performing surface treatment;
(2) Bending load test: bending and loading the sample, putting the clamp and the sample into a closed storage tank integrally for hydrogen sulfide stress corrosion test, and performing surface rust removal treatment on the sample which is not failed after the test period is completed;
(3) Corrosion pit parameter measurement and volume calculation: performing morphology analysis and parameter measurement on the corrosion pit on the surface of the sample by adopting a microscope, and calculating the volume of the corrosion pit; the hydrogen sulfide stress corrosion resistance of the oil well pipe material was evaluated by calculating the volume of the corrosion pit.
2. The evaluation method according to claim 1, wherein the loading ratio of the bending loading is 50% -90% of the yield strength of the oil well pipe, the test solution for the hydrogen sulfide stress corrosion test is NaCE standard A solution, and the test period is 360-720h.
3. The evaluation method according to claim 1, wherein the bending loading test adopts a four-point bending loading mode, so that uniform longitudinal tensile stress is generated on the surface part of the sample bulge between two inner fulcrums, the stress is linearly reduced to zero from the inner fulcrums to the outer fulcrums, and the stress on the surface of the sample is uniform.
4. The method of claim 1, wherein the non-failed test sample is: the test specimen after completing the hydrogen sulfide stress corrosion test period was not broken, and the surface of the test specimen was observed with a 10-fold magnifying glass, and macroscopic cracks were not seen.
5. The method of claim 1, wherein the microscope is a confocal laser microscope; the sample is placed on the stage, the longitudinal direction of the sample is parallel to the X-axis, the transverse direction of the sample is parallel to the Y-axis, the length direction of the etch pit is the Y-axis, and the width direction is the X-axis.
6. The method according to claim 1, wherein the etch pit is uniformly deformed by the longitudinal tensile stress, and the original punctiform etch pit is expanded in a direction perpendicular to the tensile stress, so that the etch pit becomes longer and deeper, and a boat-shaped etch pit having a certain width is formed.
7. The method of claim 1, wherein the parameter measurements are measurements of the length, width and depth of the etch pit.
8. The method of claim 7, wherein the etch pit volume is calculated as:
wherein l is the length of the etch pit in μm; d is the width of the etch pit in μm; h is the depth of the etch pit in μm and V is the etch pit volume in μm 3 。
9. The method of evaluating according to claim 1, wherein the smaller the volume of the corrosion pit is, the better the hydrogen sulfide stress corrosion resistance of the oil well pipe material is.
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