CN105954179B - A kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity - Google Patents
A kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity Download PDFInfo
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Abstract
The present invention discloses a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, includes the following steps：(1) prepared by sample：It processes plate and fills sample, and is clean；One layer of porous sulphur layer is coated in clean specimen surface；(2) oil/gas well water flooding simulated solution is prepared；(3) corrosion test：The sample for coating sulphur is put into the oil/gas well water flooding simulated solution of preparation and carries out corrosion test；(4) after corrosion test, stress corrosion opening cracking maleate sensitivity inspection is carried out.The present invention can effectively overcome the problems, such as that sulphur layer cannot be in close contact with sample, and then accurately evaluate peracidity oil gas field and adopt the stress corrosion opening cracking maleate sensitivity of defeated pipeline and device materials under elementary sulfur existence condition, and test result is reliable.
Description
Technical field
The invention belongs to corrosion and protection technical field, more particularly to a kind of measuring metallic materials elementary sulfur stress corrosion is opened
Split the test method of sensibility.
Background technology
For peracidity oil gas field in recovery process, the elementary sulfur in gas-bearing reservoir is carried by the high velocity gas stream out stratum, with adopting
The variation of defeated system temperature and pressure, element sulfur particle are precipitated and precipitate from natural gas, cause to adopt defeated pipeline or device occurs
The production accidents such as blocking and corrosion failure, seriously affect the safety in production of oil gas field.
Research shows that：Exist in elementary sulfur, elementary sulfur and H2Sx、H2S、HS-、H2O and Cl-Etc. collective effects add
The acute corrosion of carbon steel and corrosion resistant alloy, failure mode is based on the local corrosion of pitting initiation, it is also possible to which inducing materials are answered
Power corrosion cracking (Liane Smith et al, 2005NACE CORROSION, Paper No.05646).
Currently, the research of elementary sulfur corrosion test, based on homogeneous corrosion and spot corrosion, elementary sulfur is to suspend and deposit two kinds
Form exists.Patent publication No. " 104422648 A of CN ", a kind of entitled " oil well pipe material deposition sulfur corrosion experiment side
The Chinese patent application of method and its test fixture " describes a kind of high alloy oil well pipe deposition sulfur corrosion test method, the party
Method will be filled in fixture after simple substance sulphur powder and simulated formation aqueous solution mixing preparation and surround sample, be carried out after fixture is closed
High temperature and pressure test, then calculate uniform corrosion rate and local corrosion rate.The patent application is with high alloy oil well pipe material
Subjects, it is intended to overcome the problems, such as that sulphur powder cannot be sufficiently mixed with etchant solution, sulphur powder is lost in and sulphur powder liquefaction precipitation, and
Homogeneous corrosion and spot corrosion of the research material in high temperature deposition sulphur environment.
Stress corrosion cracking is a kind of main damage form that peracidity oil gas field adopts that defeated pipeline and device face, hidden
Property is strong, harmfulness is big.However, the current test method still without effectively measuring elementary sulfur stress corrosion cracking.For element
Material stress corrosion split test in sulphur environment, there are following problems：
1) it suspends or the sulphur powder of sedimentation state is not soluble in water, and easily swim in solution surface or be deposited on solution bottom, it is difficult
Ensure the close contact of sulphur powder, solution and sample；
2) prefabricated stage of stress is difficult to ensure that sulphur layer keeps being in close contact with sample.
3) directly coating sulphur layer is excessively fine and close, contact of the solution with sample is influenced, to influence Corrosion results.
Invention content
The purpose of the present invention is to provide a kind of experiment sides of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity
Method can effectively evaluate peracidity oil gas field and adopt the stress corrosion of defeated pipeline and device materials under elementary sulfur existence condition and open
Split sensibility.
To achieve the goals above, the present invention adopts the following technical scheme that：
A kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, includes the following steps：
(1) prepared by sample：It processes plate and fills sample, and is clean；It is porous in one layer clean of specimen surface coating
Sulphur layer；
(2) oil/gas well water flooding simulated solution is prepared；
(3) corrosion test：The sample for coating sulphur is put into the oil/gas well water flooding simulated solution of preparation and carries out corrosion test；
(4) after corrosion test, stress corrosion opening cracking maleate sensitivity inspection is carried out.
Further, step (1) specifically includes：
1.1) machining plate-like sample is axially polished with 240#-1000# sand paper along sample, then with acetone and anhydrous second
Alcohol ultrasonic wave added cleans up；
1.2) specimen size is measured, amount of deflection is calculated；
1.3) stress is applied by bend specimen；
1.4) contain leachy porous sulphur layer in specimen surface coating.
Further, it is coated containing leachy sulphur layer in specimen surface and is specially：
Will after the elemental sulfur powder ethanol wet that pure rank be analyzed be coated on sample surface to be checked, heating sample to 115~
125 DEG C so that the sulphur of specimen surface is in micro- melt, while using nitrogen purging to prevent specimen surface from aoxidizing；Simple substance sulphur powder with
The mass ratio of ethyl alcohol is 1.5~4.5：1；
Alternatively, the elemental sulfur powder for analyzing pure rank is allocated as gluing with organic dispersing agent (such as n-butanol, isobutanol, propyl alcohol)
Thick slurry shape is applied to sample surface to be checked, and sample is heated to 115~125 DEG C so that the sulphur slurry of specimen surface is in micro- melt, together
Shi Caiyong nitrogen is purged to prevent specimen surface from aoxidizing；The mass ratio of simple substance sulphur powder and dispersant is 0.2~1.2：1.
Further, the preparation of oil/gas well water flooding simulated solution specifically includes in step (2)：
2.1) oil/gas well stratum simulation water, Cl are prepared-Concentration range is 0~200g/L；
2.2) prepared simulation water is placed in closed container, and with the rate of 100ml/min be continuously passed through nitrogen with
The dissolved oxygen in solution is removed, the continuously deoxidizing time is every liter of solution at least 1h.
Further, step (3) specifically includes：
3.1) sample handled well is placed in test chamber；
3.2) the oil/gas well water flooding simulated solution injection testing container that will be handled well, and seal；
3.3) nitrogen is passed through into oil/gas well water flooding simulated solution with the rate of 100ml/min to remove in testing liquid again
Dissolved oxygen, the time is every liter of solution at least 0.5h；
3.4) temperature of oil/gas well water flooding simulated solution is risen into test objective temperature；
3.5) test gas is passed through into test chamber；
3.6) test period is 720h.
Further, the test gas being passed through in step 3.5) is hydrogen sulfide gas and carbon dioxide gas.
Further, the pressure that hydrogen sulfide gas is passed through in test chamber is 0.1~0.5MPa, is passed through carbon dioxide gas
Pressure be 0.1~0.5MPa, be passed through nitrogen supplement so that stagnation pressure reaches 2MPa in test chamber.
Further, Cl in oil/gas well water flooding simulated solution in step (2)-A concentration of 107g/L, HCO3 -It is a concentration of
0.34g/L, SO4 2-A concentration of 0.30g/L, Ca2+A concentration of 15.02g/L, Na++K+A concentration of 50.93g/L, Mg2+It is a concentration of
0.94g/L。
Further, target temperature is 60 DEG C in step 3.4).
Further, stress is applied by four-point bending in step 1.3).
Compared with the existing technology, the invention has the advantages that：The present invention effectively overcomes sulphur layer cannot be tight with sample
The tactile problem of contiguity, and then accurately evaluate peracidity oil gas field and adopt defeated pipeline and device materials under elementary sulfur existence condition
Stress corrosion opening cracking maleate sensitivity, test result are reliable；Elemental sulfur and ethyl alcohol or dispersant, 115~125 are heated to by sample
DEG C, ethyl alcohol or dispersant volatilize, and form porous structure in the sulphur layer of coating, porous sulphur layer is formed after cooling；So that molten
Contact of the liquid energy enough by stomata with sample, to ensure Corrosion results；The effective directly coating sulphur layer that overcomes is excessively fine and close,
Contact of the solution with sample is influenced, the problem of to influence Corrosion results.
Specific implementation mode
The application further illustrated the present invention below by embodiment and effect.
A kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, stress loading mode are 4 points
Bending, specifically includes following steps：
(1) prepared by sample：
1) machining plate-like sample is axially polished with 240#-1000# sand paper along sample, then with acetone and absolute ethyl alcohol
Ultrasonic wave added cleans.
2) specimen size is measured, amount of deflection is calculated.
3) stress is applied by bend specimen.
4) specimen surface coats sulphur, forms porous sulphur layer：
Method one：Sample surface to be checked, heating sample will be coated on after the elemental sulfur powder ethanol wet for analyzing pure rank
To 115~125 DEG C so that the sulphur of specimen surface is in micro- melt, while using nitrogen purging to prevent specimen surface from aoxidizing；It is single
The mass ratio of matter sulphur powder and ethyl alcohol is 1.5~4.5：1.
Method two：The elemental sulfur powder for analyzing pure rank is allocated as with organic dispersing agent (such as n-butanol, isobutanol, propyl alcohol)
Sticky pulpous state is applied to sample surface to be checked, and sample is placed in crucible ware and is heated to 115~125 DEG C so that specimen surface
Sulphur slurry be in micro- melt, while use nitrogen purge to prevent specimen surface from aoxidizing；The mass ratio of simple substance sulphur powder and dispersant is
0.2~1.2：1.
(2) oil/gas well water flooding simulated solution is prepared：
1) oil/gas well stratum simulation water, Cl are prepared-Concentration range is 0~200g/L.
2) prepared simulation water is placed in closed container, and is continuously passed through high pure nitrogen (100ml/min) to remove
Dissolved oxygen in solution, the continuously deoxidizing time is different because of liquor capacity, every liter of solution at least 1h.
(3) corrosion test：
1) sample handled well is placed in test chamber；
2) the testing liquid injection testing container that will be handled well, and seal；
3) it is passed through high pure nitrogen (100ml/min) into testing liquid and removes dissolved oxygen in testing liquid, time again
It is every liter of solution at least 0.5h.
4) testing liquid temperature is risen into test objective temperature.
5) test gas (such as high-pure hydrogen sulfide gas, high-purity carbon dioxide gas) is passed through into test chamber to corresponding
Partial pressure and stagnation pressure.
6) test period is 720h.
(4) stress corrosion opening cracking maleate sensitivity inspection：
1) check whether sample is broken.
2) specimen surface deposition sulphur and corrosion product are removed, it is whether cracked using micro- sem observation specimen surface.
Embodiment 1
(1) prepared by sample：It selects peracidity oil gas field to integrate defeated with L245M as test material, is processed into 115 × 15 × 4mm
Plate tensile sample, after being polished step by step with 240#-1000# sand paper, cleaned with acetone, absolute ethyl alcohol ultrasonic wave added successively, and measured
Specimen size.According to test material intensity and size, amount of deflection is calculated, and stress is applied by bend specimen.Pure rank will be analyzed
Simple substance sulphur powder ethyl alcohol (mass ratio 4.5：1) sample surface to be checked is coated on after soaking, heating sample is to 120 DEG C so that examination
The sulphur on sample surface is in micro- melt, while using nitrogen purging to prevent specimen surface from aoxidizing, until the micro- molten sulfur of specimen surface
Layer solidification.
(2) oil/gas well water flooding simulated solution is prepared：Simulated solution is prepared according to certain oil gas field stratum water constituent, in solution
Cl-A concentration of 107g/L, HCO3 -A concentration of 0.34g/L, SO4 2-A concentration of 0.30g/L, Ca2+A concentration of 15.02g/L, Na++K+
A concentration of 50.93g/L, Mg2+A concentration of 0.94g/L.Deoxygenation 4h is sealed, it is spare.
(3) corrosion test：The sample handled well and the testing liquid handled well are placed in high temperature and high pressure kettle, sealed immediately
Lid, and it is passed through high pure nitrogen deoxygenation 2h.Testing liquid temperature is risen to 60 DEG C.0.5MPa partial pressures are successively squeezed into kettle again
CO2With the H of 0.1MPa partial pressures2S is supplemented with high pure nitrogen and so that stagnation pressure reaches 2MPa in kettle, carries out simulation oil gas field operating mode and member
Corrosion test under plain sulphur existence condition, test period 720h.
(4) stress corrosion opening cracking maleate sensitivity inspection：It after experiment, checks whether sample is broken, removes specimen surface
Sulphur and corrosion product whether there is crackle with micro- sem observation specimen surface.L245M materials are judged as a result, in elementary sulfur to exist
Sensitivity of Stress Corrosion under environment.
Embodiment 2
(1) prepared by sample：It with 316L is test material to select oil gas field sour natural gas processing unit, it is processed into 115 ×
The plate tensile sample of 15 × 4mm after being polished step by step with 240#-1000# sand paper, is cleaned with acetone, absolute ethyl alcohol ultrasonic wave added successively,
And measure specimen size.According to test material intensity and size, amount of deflection is calculated, and stress is applied by bend specimen.It will analysis
The elemental sulfur powder of pure rank organic dispersing agent (such as n-butanol, mass ratio 1.2：1) it is allocated as sticky pulpous state, is applied to sample
Sample is heated to 125 DEG C so that the sulphur slurry of specimen surface is in micro- melt by surface to be checked, and high pure nitrogen is purged to prevent sample table
Face aoxidizes.Until the micro- molten sulfur layer solidification of specimen surface.
(2) oil/gas well water flooding simulated solution is prepared：Simulated solution is prepared according to certain oil gas field stratum water constituent, in solution
Cl-A concentration of 107g/L, HCO3 -A concentration of 0.34g/L, SO4 2-A concentration of 0.30g/L, Ca2+A concentration of 15.02g/L, Na++K+
A concentration of 50.93g/L, Mg2+A concentration of 0.94g/L.Deoxygenation 4h is sealed, it is spare.
(3) corrosion test：The sample handled well and the testing liquid handled well are placed in high temperature and high pressure kettle, sealed immediately
Lid, and it is passed through high pure nitrogen deoxygenation 2h.Testing liquid temperature is risen to 60 DEG C.1.0MPa partial pressures are successively squeezed into kettle again
CO2With the H of 0.5MPa partial pressures2S is supplemented with high pure nitrogen and so that stagnation pressure reaches 2MPa in kettle, carries out simulation oil gas field operating mode and member
Corrosion test under plain sulphur existence condition, test period 720h.
(4) stress corrosion opening cracking maleate sensitivity inspection：It after experiment, checks whether sample is broken, removes specimen surface
Sulphur and corrosion product whether there is crackle with micro- sem observation specimen surface.Judging 316L materials as a result, there are rings in elementary sulfur
Sensitivity of Stress Corrosion under border.
Claims (8)
1. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, which is characterized in that including following
Step：
(1) prepared by sample：Machining plate-like sample, and it is clean；One layer, which is coated, in clean specimen surface contains stomata
Sulphur layer；
(2) oil/gas well water flooding simulated solution is prepared；
(3) corrosion test：The sample for coating sulphur is put into the oil/gas well water flooding simulated solution of preparation and carries out corrosion test；
(4) after corrosion test, stress corrosion opening cracking maleate sensitivity inspection is carried out；
Step (1) specifically includes：
1.1) machining plate-like sample is axially polished with 240#-1000# sand paper along sample, then super with acetone and absolute ethyl alcohol
Sound auxiliary cleans up；
1.2) specimen size is measured, amount of deflection is calculated；
1.3) stress is applied by bend specimen；
1.4) contain leachy sulphur layer in specimen surface coating；
It is coated containing leachy sulphur layer in specimen surface and is specially：
Sample surface to be checked will be coated on after the elemental sulfur powder ethanol wet for analyzing pure rank, heating sample is to 115~125 DEG C
So that the sulphur of specimen surface is in micro- melt, while using nitrogen purging to prevent specimen surface from aoxidizing；Simple substance sulphur powder and ethyl alcohol
Mass ratio be 1.5~4.5：1；
Alternatively, the elemental sulfur powder for analyzing pure rank is allocated as sticky pulpous state with dispersant, it is applied to sample surface to be checked, will be tried
Sample is heated to 115~125 DEG C so that the sulphur slurry of specimen surface is in micro- melt, while using nitrogen purging to prevent specimen surface oxygen
Change；The dispersant is n-butanol, isobutanol or propyl alcohol；The mass ratio of simple substance sulphur powder and dispersant is 0.2~1.2：1.
2. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity according to claim 1,
It is characterized in that, the preparation of oil/gas well water flooding simulated solution specifically includes in step (2)：
2.1) oil/gas well stratum simulation water, Cl are prepared-Concentration range is 0~200g/L；
2.2) prepared simulation water is placed in closed container, and is continuously passed through nitrogen with the rate of 100ml/min to remove
Dissolved oxygen in solution, continuously deoxidizing time are every liter of solution at least 1h.
3. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity according to claim 1,
It is characterized in that, step (3) specifically includes：
3.1) sample handled well is placed in test chamber；
3.2) the oil/gas well water flooding simulated solution injection testing container that will be handled well, and seal；
3.3) into oil/gas well water flooding simulated solution with the rate of 100ml/min be passed through nitrogen remove again it is molten in testing liquid
Oxygen is solved, the time is every liter of solution at least 0.5h；
3.4) temperature of oil/gas well water flooding simulated solution is risen into test objective temperature；
3.5) test gas is passed through into test chamber；
3.6) test period is 720h.
4. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity according to claim 3,
It is characterized in that, the test gas being passed through in step 3.5) is hydrogen sulfide gas and carbon dioxide gas.
5. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity according to claim 4,
It is characterized in that, the pressure for being passed through hydrogen sulfide gas in test chamber is 0.1~0.5MPa, it is passed through the pressure of carbon dioxide gas
For 0.1~0.5MPa, nitrogen supplement is passed through so that stagnation pressure reaches 2MPa in test chamber.
6. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity according to claim 1,
It is characterized in that, Cl in oil/gas well water flooding simulated solution in step (2)-A concentration of 107g/L, HCO3 -A concentration of 0.34g/L,
SO4 2-A concentration of 0.30g/L, Ca2+A concentration of 15.02g/L, Na++K+A concentration of 50.93g/L, Mg2+A concentration of 0.94g/L.
7. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity according to claim 3,
It is characterized in that, target temperature is 60 DEG C in step 3.4).
8. a kind of test method of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity according to claim 3,
It is characterized in that, applying stress by four-point bending in step 1.3).
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| CN109211759B (en) * | 2017-07-04 | 2024-03-01 | 中国石油天然气集团公司 | Deoxidizing device for corrosion test solution and operation method thereof |
| CN108956233A (en) * | 2018-08-16 | 2018-12-07 | 武汉钢铁有限公司 | Carbon dioxide corrosion test method of the pipe line steel under bending stress |
| CN109443892B (en) * | 2018-09-26 | 2021-03-30 | 上海海隆石油管材研究所 | Method for rapidly evaluating sulfide stress corrosion cracking resistance of oil well pipe |
| CN110108630B (en) * | 2019-05-09 | 2024-05-03 | 南京工业大学 | Test method for simulating corrosion of oil product containing organic matters to petrochemical equipment |
| CN113533057A (en) * | 2020-04-22 | 2021-10-22 | 中国石油天然气股份有限公司 | Method for testing stress corrosion cracking of oil pipe |
| CN112834332A (en) * | 2020-12-29 | 2021-05-25 | 江苏容大材料腐蚀检验有限公司 | Loading detection method and monitoring system for sulfide stress corrosion uniaxial tensile test |
| CN114112837B (en) * | 2021-11-12 | 2023-12-19 | 中航光电科技股份有限公司 | Method for detecting porosity of coating |
| CN114441428A (en) * | 2022-01-14 | 2022-05-06 | 常州大学 | Metal material hydrogen sulfide corrosion experiment device |
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| CN101881709A (en) * | 2010-06-23 | 2010-11-10 | 华东理工大学 | Novel stress corrosion test specimen and experiment method |
| CN104422648B (en) * | 2013-08-30 | 2018-01-30 | 宝山钢铁股份有限公司 | A kind of oil well pipe material deposition sulfur corrosion test method and its test fixture |
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