CN105954179A - Test method for measuring metallic material elemental sulfur stress corrosion cracking sensitivity - Google Patents
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Abstract
The invention discloses a test method for measuring metallic material elemental sulfur stress corrosion cracking sensitivity. The method includes the following steps: (1) preparing the sample: putting the sample on a processing plate, cleaning the sample, and coating porous sulfur layer on the surface of the cleaned sample; (2) preparing the oil and gas well stratum water simulated solution; (3) performing a corrosion test: putting the sample coating sulfur into the prepared oil and gas well stratum water simulated solution to perform the corrosion test; and (4) performing stress corrosion cracking sensitivity inspection after finishing the corrosion test. The problem that the sulfur layer can not contact with the sample closely is overcome effectively, moreover, the stress corrosion cracking sensitivity of the high acid oil and gas field pipeline and device material in the presence of elemental sulfur is evaluated accurately, and the test result is reliable.
Description
Technical field
The invention belongs to corrosion and protection technical field, particularly to a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity
Test method.
Background technology
Peracidity oil gas field is in recovery process, and the elementary sulfur in gas-bearing reservoir is carried by the high velocity gas stream out stratum, along with adopting communication system temperature
Degree and the change of pressure, element sulfur particle separates out from natural gas and precipitates, and causes and adopts defeated pipeline or device generation blocking and be corroded through
The production accidents such as hole, have a strong impact on the safety in production of oil gas field.
Research shows: in the case of elementary sulfur exists, elementary sulfur and H2Sx、H2S、HS-、H2O and Cl-Add Deng common effect
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 the stress of inducing materials is rotten
Erosion cracking (Liane Smith et al, 2005NACE CORROSION, Paper No.05646).
At present, the research of elementary sulfur corrosion testing is based on homogeneous corrosion and spot corrosion, and elementary sulfur is to suspend and two kinds of forms existence of deposition.
Patent publication No. " CN 104422648 A ", invention entitled " a kind of oil well pipe material deposition sulfur corrosion test method and test use thereof
Fixture " Chinese patent application describe a kind of high alloy oil well pipe deposition sulfur corrosion test method, the method is by elemental sulfur powder and mould
It is filled in fixture after intending formation water mixing preparation and sample is surrounded, carry out high temperature and pressure test after being closed by fixture, then calculate
Uniform corrosion rate and local corrosion rate.This patent application is with high alloy oil well pipe material as subjects, it is intended to overcome sulfur powder not
Can be sufficiently mixed with etchant solution, sulfur powder runs off and the problem of sulfur powder liquefaction precipitation, and research material is in high temperature deposition sulfur environment
Homogeneous corrosion and spot corrosion.
Stress corrosion cracking is a kind of main damage form that peracidity oil gas field adopts defeated pipeline and device faces, its disguised strong, danger
Evil property is big.But, the most still there is no the test method of effectively measuring elementary sulfur stress corrosion cracking.For material in elementary sulfur environment
, there is a following difficult problem in material test for stress corrosion cracking:
1) suspend or the sulfur powder of sedimentation state is water insoluble, and easily swim in solution surface or be deposited on bottom solution, be difficult to ensure card sulfur
Powder, solution and the close contact of sample；
2) prefabricated stage of stress is difficult to ensure that sulfur layer and sample keep being in close contact.
3) directly coating sulfur layer is the finest and close, affects contacting of solution and sample, thus affects Corrosion results.
Summary of the invention
It is an object of the invention to provide the test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, it is possible to have
Effect ground is evaluated peracidity oil gas field and is adopted defeated pipeline and the device materials stress corrosion opening cracking maleate sensitivity under elementary sulfur existence condition.
To achieve these goals, the present invention adopts the following technical scheme that
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, comprises the following steps:
(1) prepared by sample: processing plate dress sample, and cleans clean；At specimen surface one layer of porous sulfur layer of coating that cleaning is clean；
(2) preparation Oil/gas Well formation water simulated solution；
(3) corrosion testing: the sample of coating sulfur is put in the Oil/gas Well formation water simulated solution of preparation and carry out corrosion testing；
(4), after corrosion testing terminates, stress corrosion opening cracking maleate sensitivity inspection is carried out.
Further, step (1) specifically includes:
1.1) machining plate-like sample, axially polishes along sample with 240#-1000# sand paper, more ultrasonic with acetone and dehydrated alcohol
Auxiliary cleans up；
1.2) measure specimen size, calculate amount of deflection；
1.3) stress is applied by bend specimen；
1.4) in specimen surface coating containing leachy porous sulfur layer.
Further, in specimen surface coating containing leachy sulfur layer particularly as follows:
Being coated on sample surface to be checked by after the elemental sulfur powder ethanol wet of analytical pure rank, heating sample to 115～125 DEG C makes
The sulfur of specimen surface is in micro-melt, uses nitrogen to purge to prevent specimen surface from aoxidizing simultaneously；Elemental sulfur powder and the mass ratio of ethanol
It is 1.5～4.5:1；
Or, the elemental sulfur powder organic dispersing agent (such as n-butyl alcohol, isobutanol, propanol) of analytical pure rank is allocated as thickness slurry
Shape, spreads upon sample surface to be checked, sample is heated to 115～125 DEG C of sulfur making specimen surface and starches in micro-melt, use simultaneously
Nitrogen purges to prevent specimen surface from aoxidizing；Elemental sulfur powder is 0.2～1.2:1 with the mass ratio of dispersant.
Further, in step (2), the preparation of Oil/gas Well formation water simulated solution specifically includes:
2.1) preparation Oil/gas Well stratum simulation water, Cl-Concentration range is 0～200g/L；
2.2) the simulation water prepared is placed in hermetic container, and it is molten to remove to be passed through nitrogen continuously with the speed of 100ml/min
Dissolved oxygen in liquid, 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 formation water simulated solution injection testing container that will handle well, and seal；
3.3) in Oil/gas Well formation water simulated solution, it is passed through nitrogen with the speed of 100ml/min and again removes the dissolving in testing liquid
Oxygen, the time is every liter of solution at least 0.5h；
3.4) temperature of Oil/gas Well formation water simulated solution is risen to test objective temperature；
3.5) in test chamber, test gas it is passed through；
3.6) test period is 720h.
Further, step 3.5) in the test gas that is passed through be hydrogen sulfide gas and carbon dioxide.
Further, the pressure being passed through hydrogen sulfide gas in test chamber is 0.1～0.5MPa, is passed through the pressure of carbon dioxide
Be 0.1～0.5MPa, be passed through nitrogen supplement make test chamber in stagnation pressure reach 2MPa.
Further, Cl in Oil/gas Well formation water simulated solution in step (2)-Concentration is 107g/L, HCO3 -Concentration is 0.34g/L,
SO4 2-Concentration is 0.30g/L, Ca2+Concentration is 15.02g/L, Na++K+Concentration is 50.93g/L, Mg2+Concentration is 0.94g/L.
Further, step 3.4) in target temperature be 60 DEG C.
Further, step 1.3) in apply stress by four-point bending.
Relative to prior art, the method have the advantages that the present invention effectively overcomes sulfur layer and sample not to be in close contact
Problem, and then evaluation peracidity oil gas field adopts defeated pipeline and the device materials stress corrosion cracking under elementary sulfur existence condition exactly
Sensitivity, result of the test is reliable；Elemental sulfur and ethanol or dispersant, be heated to 115～125 DEG C, ethanol or dispersion by sample
Agent is volatilized, and forms loose structure in the sulfur layer of coating, forms porous sulfur layer after cooling；Make solution can by pore with
The contact of sample, thus ensure Corrosion results；Effectively overcome directly coating sulfur layer the finest and close, affect connecing of solution and sample
Touch, thus the problem affecting Corrosion results.
Detailed description of the invention
Application and the effect of the present invention is further illustrated below by embodiment.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, stress loading mode is four-point bending, tool
Body comprises the following steps:
(1) prepared by sample:
1) machining plate-like sample, axially polishes along sample with 240#-1000# sand paper, then surpasses with acetone and dehydrated alcohol
Sound auxiliary is cleaned.
2) measure specimen size, calculate amount of deflection.
3) stress is applied by bend specimen.
4) specimen surface coating sulfur, formation porous sulfur layer:
Method one: being coated on sample surface to be checked by after the elemental sulfur powder ethanol wet of analytical pure rank, heating sample is extremely
115～125 DEG C of sulfur making specimen surface are in micro-melt, use nitrogen to purge to prevent specimen surface from aoxidizing simultaneously；Elemental sulfur powder
It is 1.5～4.5:1 with the mass ratio of ethanol.
Method two: the elemental sulfur powder organic dispersing agent (such as n-butyl alcohol, isobutanol, propanol) of analytical pure rank is allocated as thickness
Pulpous state, spreads upon sample surface to be checked, sample is placed in crucible ware be heated to 115～125 DEG C of sulfur slurries making specimen surface in
Micro-melt, uses nitrogen to purge to prevent specimen surface from aoxidizing simultaneously；Elemental sulfur powder is 0.2～1.2:1 with the mass ratio of dispersant.
(2) Oil/gas Well formation water simulated solution preparation:
1) preparation Oil/gas Well stratum simulation water, Cl-Concentration range is 0～200g/L.
2) the simulation water prepared is placed in hermetic container, and is passed through high pure nitrogen (100ml/min) continuously 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 testing:
1) sample handled well is placed in test chamber；
2) the testing liquid's injection testing container that will handle well, and seal；
3) in testing liquid, it is passed through high pure nitrogen (100ml/min) again remove the dissolved oxygen in testing liquid, time
It is every liter of solution at least 0.5h.
4) testing liquid's temperature is risen to test objective temperature.
5) in test chamber, test gas (such as high-pure hydrogen sulfide gas, high-purity carbon dioxide gas etc.) it is passed through to accordingly
Dividing potential drop and stagnation pressure.
6) test period is 720h.
(4) stress corrosion opening cracking maleate sensitivity inspection:
1) check whether sample ruptures.
2) remove specimen surface deposition sulfur and corrosion product, utilize microscope to observe whether specimen surface crackle occurs.
Embodiment 1
(1) prepared by sample: selects peracidity oil gas field to integrate defeated L245M as test material, is processed into 115 × 15 × 4mm's
Plate tensile sample, after polishing step by step with 240#-1000# sand paper, cleans with acetone, dehydrated alcohol ultrasonic wave added, and measures sample successively
Size.According to test material intensity and size, calculate amount of deflection, and apply stress by bend specimen.Simple substance by analytical pure rank
Being coated on sample surface to be checked after sulfur powder ethanol (mass ratio is 4.5:1) moistening, heating sample to 120 DEG C makes specimen surface
Sulfur be in micro-melt, use nitrogen to purge to prevent specimen surface from aoxidize, until specimen surface micro-molten sulfur layer solidifies simultaneously.
(2) Oil/gas Well formation water simulated solution preparation: become assignment system simulated solution according to certain oil gas field formation water, the Cl in solution-
Concentration is 107g/L, HCO3 -Concentration is 0.34g/L, SO4 2-Concentration is 0.30g/L, Ca2+Concentration is 15.02g/L, Na++K+
Concentration is 50.93g/L, Mg2+Concentration is 0.94g/L.Seal deoxygenation 4h, standby.
(3) corrosion testing: the sample handled well and the testing liquid handled well are placed in high temperature and high pressure kettle, cover immediately,
And it is passed through high pure nitrogen deoxygenation 2h.Testing liquid's temperature is risen to 60 DEG C.The CO of 0.5MPa dividing potential drop is successively squeezed into again in still2
H with 0.1MPa dividing potential drop2S, supplements stagnation pressure in making still and reaches 2MPa, be simulated oil gas field operating mode and unit with high pure nitrogen
Corrosion testing under element sulfur existence condition, test period is 720h.
(4) stress corrosion opening cracking maleate sensitivity inspection: after test, check sample whether rupture, remove specimen surface sulfur and
With microscope, corrosion product, observes whether specimen surface exists crackle.Thus, pass judgment on L245M material and there is environment at elementary sulfur
Under Sensitivity of Stress Corrosion.
Embodiment 2
(1) prepared by sample: selecting oil gas field sour natural gas processing means 316L is test material, is processed into 115 × 15 × 4
The plate tensile sample of mm, after polishing step by step with 240#-1000# sand paper, cleans with acetone, dehydrated alcohol ultrasonic wave added, and surveys successively
Amount specimen size.According to test material intensity and size, calculate amount of deflection, and apply stress by bend specimen.By analytical pure rank
Elemental sulfur powder be allocated as thickness pulpous state with organic dispersing agent (such as n-butyl alcohol, mass ratio is 1.2:1), spread upon sample table to be checked
Face, is heated to sample 125 DEG C of sulfur making specimen surface and starches in micro-melt, and high pure nitrogen purges to prevent specimen surface from aoxidizing.
Until the solidification of specimen surface micro-molten sulfur layer.
(2) Oil/gas Well formation water simulated solution preparation: become assignment system simulated solution according to certain oil gas field formation water, the Cl in solution-
Concentration is 107g/L, HCO3 -Concentration is 0.34g/L, SO4 2-Concentration is 0.30g/L, Ca2+Concentration is 15.02g/L, Na++K+
Concentration is 50.93g/L, Mg2+Concentration is 0.94g/L.Seal deoxygenation 4h, standby.
(3) corrosion testing: the sample handled well and the testing liquid handled well are placed in high temperature and high pressure kettle, cover immediately,
And it is passed through high pure nitrogen deoxygenation 2h.Testing liquid's temperature is risen to 60 DEG C.The CO of 1.0MPa dividing potential drop is successively squeezed into again in still2
H with 0.5MPa dividing potential drop2S, supplements stagnation pressure in making still and reaches 2MPa, be simulated oil gas field operating mode and unit with high pure nitrogen
Corrosion testing under element sulfur existence condition, test period is 720h.
(4) stress corrosion opening cracking maleate sensitivity inspection: after test, check sample whether rupture, remove specimen surface sulfur and
With microscope, corrosion product, observes whether specimen surface exists crackle.Thus, pass judgment on 316L material to deposit at ambient at elementary sulfur
Sensitivity of Stress Corrosion.
Claims (10)
1. the test method of a measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity, it is characterised in that include following step
Rapid:
(1) prepared by sample: processing plate dress sample, and cleans clean；One layer is coated containing pore at the specimen surface that cleaning is clean
Sulfur layer；
(2) preparation Oil/gas Well formation water simulated solution；
(3) corrosion testing: the sample of coating sulfur is put in the Oil/gas Well formation water simulated solution of preparation and carry out corrosion testing；
(4), after corrosion testing terminates, stress corrosion opening cracking maleate sensitivity inspection is carried out.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 1, its
Being characterised by, step (1) specifically includes:
1.1) machining plate-like sample, axially polishes along sample with 240#-1000# sand paper, more ultrasonic with acetone and dehydrated alcohol
Auxiliary cleans up；
1.2) measure specimen size, calculate amount of deflection；
1.3) stress is applied by bend specimen；
1.4) in specimen surface coating containing leachy sulfur layer.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 1 and 2,
It is characterized in that, in specimen surface coating containing leachy sulfur layer particularly as follows:
Being coated on sample surface to be checked by after the elemental sulfur powder ethanol wet of analytical pure rank, heating sample to 115～125 DEG C makes
The sulfur of specimen surface is in micro-melt, uses nitrogen to purge to prevent specimen surface from aoxidizing simultaneously；Elemental sulfur powder and the mass ratio of ethanol
It is 1.5～4.5:1；
Or, the elemental sulfur powder dispersant of analytical pure rank is allocated as thickness pulpous state, spreads upon sample surface to be checked, by sample
It is heated to 115～125 DEG C of sulfur making specimen surface to starch in micro-melt, uses nitrogen to purge to prevent specimen surface from aoxidizing simultaneously；Institute
Stating dispersant is n-butyl alcohol, isobutanol or propanol；Elemental sulfur powder is 0.2～1.2:1 with the mass ratio of dispersant.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 1, its
Being characterised by, in step (2), the preparation of Oil/gas Well formation water simulated solution specifically includes:
2.1) preparation Oil/gas Well stratum simulation water, Cl-Concentration range is 0～200g/L；
2.2) the simulation water prepared is placed in hermetic container, and it is molten to remove to be passed through nitrogen continuously with the speed of 100ml/min
Dissolved oxygen in liquid, the continuously deoxidizing time is every liter of solution at least 1h.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 1, its
Being characterised by, step (3) specifically includes:
3.1) sample handled well is placed in test chamber；
3.2) the Oil/gas Well formation water simulated solution injection testing container that will handle well, and seal；
3.3) in Oil/gas Well formation water simulated solution, it is passed through nitrogen with the speed of 100ml/min and again removes the dissolving in testing liquid
Oxygen, the time is every liter of solution at least 0.5h；
3.4) temperature of Oil/gas Well formation water simulated solution is risen to test objective temperature；
3.5) in test chamber, test gas it is passed through；
3.6) test period is 720h.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 5, its
Be characterised by, step 3.5) in the test gas that is passed through be hydrogen sulfide gas and carbon dioxide.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 6, its
Being characterised by, the pressure being passed through hydrogen sulfide gas in test chamber is 0.1～0.5MPa, and the pressure being passed through carbon dioxide is
0.1～0.5MPa, be passed through nitrogen supplement make test chamber in stagnation pressure reach 2MPa.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 1, its
It is characterised by, Cl in Oil/gas Well formation water simulated solution in step (2)-Concentration is 107g/L, HCO3 -Concentration is 0.34g/L, SO4 2-
Concentration is 0.30g/L, Ca2+Concentration is 15.02g/L, Na++K+Concentration is 50.93g/L, Mg2+Concentration is 0.94g/L.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 5, its
Be characterised by, step 3.4) in target temperature be 60 DEG C.
The test method of a kind of measuring metallic materials elementary sulfur stress corrosion opening cracking maleate sensitivity the most according to claim 5, its
Be characterised by, step 1.3) in apply stress by four-point bending.
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Cited By (8)
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| 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 |
| CN109211759A (en) * | 2017-07-04 | 2019-01-15 | 中国石油天然气集团公司 | A kind of deaerating plant and its operating method for corrosion test solution |
| CN109443892A (en) * | 2018-09-26 | 2019-03-08 | 上海海隆石油管材研究所 | The method of Fast Evaluation oil well pipe resisting sulfide stress corrosion cracking performance |
| CN110108630A (en) * | 2019-05-09 | 2019-08-09 | 南京工业大学 | A kind of test method that petrochemical equipment is corroded for simulating the oil product containing organic matter |
| 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 |
| 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 |
| CN114112837A (en) * | 2021-11-12 | 2022-03-01 | 中航光电科技股份有限公司 | Method for detecting porosity of plating layer |
| CN114441428A (en) * | 2022-01-14 | 2022-05-06 | 常州大学 | Metal material hydrogen sulfide corrosion experiment device |
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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 |
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| CN110108630A (en) * | 2019-05-09 | 2019-08-09 | 南京工业大学 | A kind of test method that petrochemical equipment is corroded for simulating the oil product containing organic matter |
| 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 |
| CN114112837A (en) * | 2021-11-12 | 2022-03-01 | 中航光电科技股份有限公司 | Method for detecting porosity of plating layer |
| 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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