CN104458396B - The preparation facilities and method of a kind of metallurgical composite pipe internal coated layer intercrystalline corrosion samples - Google Patents
The preparation facilities and method of a kind of metallurgical composite pipe internal coated layer intercrystalline corrosion samples Download PDFInfo
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- CN104458396B CN104458396B CN201410771221.9A CN201410771221A CN104458396B CN 104458396 B CN104458396 B CN 104458396B CN 201410771221 A CN201410771221 A CN 201410771221A CN 104458396 B CN104458396 B CN 104458396B
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Abstract
The invention discloses a kind of preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples and method, including container, cover plate, source of the gas, Regulation Control device, heater and the power supply for providing electric energy；The opening of the cover plate and upper vessel portion is tightly connected, source of the gas is connected by pipeline with the entrance of Regulation Control device, the outlet of Regulation Control device is connected with the inside of container, heater includes controller and heater strip, controller is fixed on the outside of container, heater strip is located in container, and power supply is connected by controller with heater strip.Internal coated layer fusion area metal need not be thinned in the present invention, prepare speed soon, and the metallurgical composite pipe internal coated layer intercrystalline corrosion samples prepared are applied to the result obtained in Huey test accurately, reliably.
Description
Technical field
The invention belongs to composite bimetal pipe internal coated layer decay resistance detection field, it is related in a kind of metallurgical composite pipe and covers
The preparation facilities and method of layer intercrystalline corrosion samples.
Background technology
When conveying highly corrosive medium, composite bimetal pipe has taken into account the corrosion resistance and low-alloy of corrosion resistant alloy
The obdurability of pipe line steel, and price is less expensive, thus promoted the use of in oil-gas pipeline field.Composite bimetal pipe
Decay resistance is determined by the corrosion resistant alloy of internal coated layer, and the Evaluation of corrosion resistance of corrosion resistant alloy is mainly intercrystalline corrosion examination
Test., it is necessary to prepare the intercrystalline corrosion samples of certain size according to government test standard GB/T 4334 requirement before experiment.For
Mechanical bimetal composite multiple tube, corrosion-resistant alloy layer can directly be peeled off and removed, and be processed into the sample of given size tried
Test；For metallurgical composite pipe, due to there are the fused layers of certain ingredients transition between internal coated layer and base tube, if only simply
Corrosion-resistant alloy layer is peeled off and removes and carries out corrosion test, there can be gradient difference on composition on same sample, in acidity
In medium, sample forms galvanic cell in itself, causes result of the test deviation.
At present, coating metal is usually thinned and peeled off by laboratory using the method for wire cutting, to remove the molten of composition transition
Close layer.But the metallurgical composite pipe of different process, fused layers variable thickness is caused, especially as internal coated layer thickness≤2mm, wire cutting
Stripping removal is very difficult, and the sample of preparation is extremely difficult to require.
The A of Chinese patent CN 102564827 use non-test face epoxy resin sealing method, i.e., spray epoxy powder
In the non-test face of sample, epoxy resin is thermally formed the preparation that diaphragm completes sample.But this method can not be complete
Ensure the compactness that epoxy resin layer is combined with parent metal, moreover, epoxy resin layer often has stomata, carry out intercrystalline corrosion examination
When testing, epoxy resin layer can be soaked due to long-term acid etching, may make acid accumulator penetration parent metal, so that accelerated corrosion, makes
It is invalid into result of the test.
Chinese patent 13SG1F1075 chooses sample, and the method inlayed using heat according to the regulation of the preparation of metallographic specimen
In one layer of resin of combination that the outer surface of parent metal is fine and close, sample is set only to expose coating-corrosion-resistant alloy layer.Both processing had been reduced
Difficulty, in turn ensure that only coating etch in corrosive liquid.But this method is to use metallography microscope Microscopic observation corrosion cracking,
Therefore complex polishing, polishing process are needed；In addition, provided according to product standard API SPEC 5LD or SY/T 6623,
It is preferential that crackle is evaluated using bending method after internal coated layer Huey test, and sample prepared by this method can only use metallographic method
Evaluate corrosion cracking.
The content of the invention
It is an object of the invention to the shortcoming for overcoming above-mentioned prior art, there is provided a kind of metallurgical composite pipe internal coated layer intergranular
Internal coated layer fusion area metal need not be thinned in the preparation facilities and method of corrosion sample, the device and method, prepare speed soon, and
And the metallurgical composite pipe internal coated layer intercrystalline corrosion samples prepared be applied to the result that is obtained in Huey test it is accurate, can
Lean on.
To reach above-mentioned purpose, the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention includes
Container, cover plate, source of the gas, Regulation Control device, heater and the power supply for providing electric energy；
The opening of the cover plate and upper vessel portion is tightly connected, and source of the gas is connected by pipeline with the entrance of Regulation Control device
Connect, the outlet of Regulation Control device is connected with the inside of container, heater includes controller and heater strip, controller is fixed
In the outside of container, heater strip is located in container, and power supply is connected by controller with heater strip.
The heater strip is resistance wire.
Sealing gasket is provided between the opening and cover plate of the upper vessel portion.
The opening of the cover plate and upper vessel portion is sealedly and fixedly connected by some fasteners；
The cover plate is cylindrical structural, and two neighboring fastener is 30 ° with the central angle that cover plate central is constituted.
The thickness of the cover plate is 15mm.
A diameter of 200-300mm of the container, the height of container is 150-200mm, and wall of a container thickness is 15mm.
The range of regulation of the Regulation Control device is 1 standard atmospheric pressure -30MPa.
The container is prepared by high strength steel and formed.
The preparation method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention comprises the following steps：
1) internal coated layer is peeled off from metallurgical composite pipe according to size as defined in Huey test standard, wherein, internal coated layer
Fused layers without wire cutting be thinned, obtain pending sample；
2) a certain amount of thermoplastic acrylic resin powder, absolute ethyl alcohol and Ludox are taken, is stirred, slurry is obtained, so
The slurry of preparation is uniformly brushed to step 1 afterwards) on the obtained non-test face of pending sample, coating layer thickness is 1-2mm, then
Dried, wherein, the ratio of thermoplastic acrylic resin powder, absolute ethyl alcohol and Ludox is 10-30g：100mL：2-
3mL；
3) by through step 2) the obtained pending sample of drying is positioned in container, faces the non-test of pending sample
On, then by cover plate sealed container, controller and Regulation Control device are then adjusted, the temperature in container is adjusted to 150-
200 DEG C, pressure is adjusted to 20-30MPa, and keeps 3-5mim, until forming one layer of densification on the non-test face of pending sample
Resin protective layer, Regulation Control device and controller are then adjusted again, make the pressure in container adjust to normal atmosphere pressure,
Temperature is down to room temperature, obtains metallurgical composite pipe internal coated layer intercrystalline corrosion samples.
The invention has the advantages that：
The preparation facilities and method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention are preparing metallurgy again
When closing pipe internal coated layer intercrystalline corrosion samples, only need first peel off internal coated layer from metallurgical composite pipe, the fused layers of internal coated layer without
Wire cutting is thinned, and obtains pending sample；Then slurry is coated on the non-test face of pending sample again, be placed into after drying
In container, by adjusting pressure and temperature in container, you can form one layer of densification on the non-test face of pending sample
Resin protective layer, it is ensured that only sample coating corrode in corrosive liquid, so as to improve Huey test result
Accuracy, metallurgical composite pipe internal coated layer intercrystalline corrosion samples prepared by the present invention meet bending method and metallographic method evaluation intercrystalline corrosion
The requirement of crackle, and preparation method is simply, conveniently.
Brief description of the drawings
Fig. 1 is structural representation of the invention；
Fig. 2 is the schematic diagram of the heater 6 of the present invention；
Fig. 3 is workflow diagram of the present invention.
Wherein, 1 be container, 2 be sealing gasket, 3 be cover plate, 4 be fastener, 5 be Regulation Control device, 6 be heater,
6-1 is that controller, 6-2 are that resistance wire, 6-3 are thermocouple, 7 are pipeline, 8 are source of the gas.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings：
With reference to Fig. 1, Fig. 2 and Fig. 3, the preparation facilities bag of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention
Include container 1, cover plate 3, source of the gas 8, Regulation Control device 5, heater 6 and the power supply for providing electric energy；The cover plate 3 with
The opening on the top of container 1 is tightly connected, and source of the gas 8 is connected by pipeline 7 with the entrance of Regulation Control device 5, Regulation Control dress
The outlet for putting 5 is connected with the inside of container 1, and heater 6 includes controller 6-1 and heater strip, and controller 6-1 is fixed on appearance
The outside of device 1, heater strip is located in container 1, and power supply is connected by controller 6-1 with heater strip.
It should be noted that the heater strip is resistance wire 6-2, present invention additionally comprises for measuring container inner wall temperature
Thermocouple 6-3；Sealing gasket 2 is provided between the opening and cover plate 3 on the top of container 1；If the opening on cover plate 3 and the top of container 1 by
Dry fastener 4 is sealedly and fixedly connected；The cover plate 3 is cylindrical structural, and two neighboring fastener 4 is constituted with the center of cover plate 3
Central angle is 30 °；The thickness of cover plate 3 is 15mm；A diameter of 200-300mm of container 1, the height of container 1 is 150-200mm,
The wall thickness of container 1 is 15mm；The range of regulation of Regulation Control device 5 is 1 standard atmospheric pressure -30MPa；Container 1 is by high-strength
Degree steel is prepared from.
The preparation method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention comprises the following steps：
1) internal coated layer is peeled off from metallurgical composite pipe according to size as defined in Huey test standard, wherein, internal coated layer
Fused layers without wire cutting be thinned, obtain pending sample；
2) a certain amount of thermoplastic acrylic resin powder, absolute ethyl alcohol and Ludox are taken, is stirred, slurry is obtained, so
The slurry of preparation is uniformly brushed to step 1 afterwards) on the obtained non-test face of pending sample, coating layer thickness is 1-2mm, then
Dried, wherein, the ratio of thermoplastic acrylic resin powder, absolute ethyl alcohol and Ludox is 10-30g：100mL：2-
3mL；
3) by through step 2) the obtained pending sample of drying is positioned in container 1, makes the non-test face of pending sample
Upward, then by cover plate 3 container 1 is sealed, then adjusts controller 6-1 and Regulation Control device 5, make the temperature in container 1
Adjust to 150-200 DEG C, pressure is adjusted to 20-30MPa, and keep 3-5mim, until shape on the non-test face of pending sample
Into one layer of fine and close resin protective layer, Regulation Control device 5 and controller 6-1 are then adjusted again, adjust the pressure in container 1
To normal atmosphere pressure, temperature is down to room temperature, obtains metallurgical composite pipe internal coated layer intercrystalline corrosion samples.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (7)
1. a kind of preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples, it is characterised in that including container (1), cover plate
(3), source of the gas (8), Regulation Control device (5), heater (6) and the power supply for providing electric energy；
The cover plate (3) and the opening on container (1) top are tightly connected, and source of the gas (8) passes through pipeline (7) and Regulation Control device
(5) entrance is connected, and the outlet of Regulation Control device (5) is connected with the inside of container (1), and heater (6) includes control
Device (6-1) processed and heater strip, controller (6-1) are fixed on the outside of container (1), and heater strip is located in container (1), and power supply passes through
Controller (6-1) is connected with heater strip；
Sealing gasket (2) is provided between the opening and cover plate (3) on container (1) top；
The range of regulation of the Regulation Control device (5) is 1 standard atmospheric pressure -30MPa.
2. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, it is characterised in that institute
Heater strip is stated for resistance wire (6-2).
3. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, it is characterised in that institute
State cover plate (3) and the opening on container (1) top is sealedly and fixedly connected by 12 fasteners (4)；
The cover plate (3) is cylindrical structural, and two neighboring fastener (4) is 30 ° with the central angle that cover plate (3) center is constituted.
4. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, it is characterised in that institute
The thickness for stating cover plate (3) is 15mm.
5. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, it is characterised in that institute
A diameter of 200-300mm of container (1) is stated, the height of container (1) is 150-200mm, and the wall thickness of container (1) is 15mm.
6. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, it is characterised in that institute
Container (1) is stated to form by high strength steel preparation.
7. a kind of preparation method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples, it is characterised in that based on described in claim 1
Metallurgical composite pipe internal coated layer intercrystalline corrosion samples preparation facilities, comprise the following steps：
1) internal coated layer is peeled off from metallurgical composite pipe according to size as defined in Huey test standard, wherein, internal coated layer it is molten
Close layer to be thinned without wire cutting, obtain pending sample；
2) a certain amount of thermoplastic acrylic resin powder, absolute ethyl alcohol and Ludox are taken, is stirred, slurry is obtained, then will
The slurry of preparation is uniformly brushed to step 1) on the obtained non-test face of pending sample, coating layer thickness is 1-2mm, then is carried out
Drying, wherein, the ratio of thermoplastic acrylic resin powder, absolute ethyl alcohol and Ludox is 10-30g：100mL：2-3mL；
3) by through step 2) the obtained pending sample of drying is positioned in container (1), faces the non-test of pending sample
On, then by cover plate (3) by container (1) sealing, then regulation controller (6-1) and Regulation Control device (5), make container (1)
Interior temperature is adjusted to 150-200 DEG C, and pressure is adjusted to 20-30MPa, and keeps 3-5mim, until the non-examination of pending sample
One layer of resin protective layer of formation on face is tested, Regulation Control device (5) and controller (6-1) are then adjusted again, is made in container (1)
Pressure is adjusted to normal atmosphere pressure, and temperature is down to room temperature, obtains metallurgical composite pipe internal coated layer intercrystalline corrosion samples.
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