CN104458396A - Device and method for preparing metallurgical composite pipe inner cladding layer intercrystalline corrosive sample - Google Patents
Device and method for preparing metallurgical composite pipe inner cladding layer intercrystalline corrosive sample Download PDFInfo
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- CN104458396A CN104458396A CN201410771221.9A CN201410771221A CN104458396A CN 104458396 A CN104458396 A CN 104458396A CN 201410771221 A CN201410771221 A CN 201410771221A CN 104458396 A CN104458396 A CN 104458396A
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Abstract
The invention discloses a device and a method for preparing a metallurgical composite pipe inner cladding layer intercrystalline corrosive sample. The device comprises a container, a cover plate, an air source, a pressure regulation control device, a heating device and a power supply used for providing electric energy, wherein the cover plate is connected with an opening in the upper part of the container in a sealed mode; the air source is connected with the inlet of the pressure regulation control device by virtue of a pipeline; the outlet of the pressure regulation control device is communicated with the interior of the container; the heating device comprises a controller and a heating wire; the controller is fixed on the outer side of the container; the heating wire is positioned in the container; and the power supply is connected with the heating wire by the controller. According to the device and the method disclosed by the invention, metals in a cladding fusion zone do not need to be thinned, the preparation speed is high, and the result obtained by applying the prepared metallurgical composite pipe inner cladding layer intercrystalline corrosive sample to an intercrystalline corrosive test is accurate and reliable.
Description
Technical field
The invention belongs to composite bimetal pipe internal coated layer decay resistance detection field, relate to a kind of preparation facilities and method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples.
Background technology
When conveying has high-corrosion medium, composite bimetal pipe has taken into account the corrosion resistance of corrosion resistant alloy and the obdurability of low-alloy pipe line steel, and price is cheaper, thus obtains in oil and gas pipes field and promotes the use of.The decay resistance of composite bimetal pipe is determined by the corrosion resistant alloy of internal coated layer, and the mainly Huey test of the Evaluation of corrosion resistance of corrosion resistant alloy.Before test, need the intercrystalline corrosion samples preparing certain size according to the requirement of government test standard GB/T 4334.For mechanical bimetal composite complex pipe, directly corrosion-resistant alloy layer can be peeled off and remove, and the sample being processed into given size is tested; For metallurgical composite pipe, owing to there is the fused layers of certain ingredients transition between internal coated layer and base tube, remove iff simply corrosion-resistant alloy layer being peeled off and carry out corrosion test, same sample can exist gradient difference on composition, in acid medium, sample itself forms primary element, causes test findings deviation.
At present, laboratory usually adopts the method for Linear cut by thinning for coating metal stripping, to remove the fused layers of composition transition.But the metallurgical composite pipe of different process, fused layers variable thickness causes, and special in internal coated layer thickness≤2mm, it is very difficult that Linear cut peels off removal, and the sample of preparation is difficult to reach requirement.
Chinese patent CN 102564827 A adopts non-test epoxy resin sealing method, is sprayed on non-test of sample by epoxy powder, epoxy resin is added the preparation that thermosetting diaphragm completes sample.But this method can not ensure the compactness that epoxy resin layer is combined with parent metal completely; and; epoxy resin layer often has pore; when carrying out Huey test; epoxy resin layer can soak due to long-term acid etching; acid accumulator penetration parent metal may be made, thus accelerated corrosion, cause test findings invalid.
Chinese patent 13SG1F1075 chooses sample according to the regulation of the preparation of metallographic specimen, and utilize the heat method of inlaying in the outside surface densification of parent metal in conjunction with one deck resin, make sample only expose coating-corrosion-resistant alloy layer.Both reduced difficulty of processing, in turn ensure that to only have coating etch in corrosive liquid.But the method adopts metallography microscope Microscopic observation corrosion cracking, therefore needs comparatively complicated polishing, polishing process; In addition, specify according to product standard API SPEC 5LD or SY/T 6623, after internal coated layer Huey test, the preferential bending method that adopts evaluates crackle, and sample prepared by the method can only adopt metallographic method to evaluate corrosion cracking.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned prior art, provide a kind of preparation facilities and method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples, this device and method does not need thinning internal coated layer fusion area metal, preparation speed is fast, and the metallurgical composite pipe internal coated layer intercrystalline corrosion samples prepared be applied to the result that obtains in Huey test accurately, reliable.
For achieving the above object, the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention comprises container, cover plate, source of the gas, Regulation Control device, heating arrangement and for providing the power supply of electric energy;
The opening of described cover plate and upper vessel portion is tightly connected, source of the gas is connected by the entrance of pipeline with Regulation Control device, the outlet of Regulation Control device is connected with the inside of container, heating arrangement comprises controller and heater strip, controller is fixed on the outside of container, heater strip is positioned at container, and power supply is connected with heater strip by controller.
Described heater strip is resistance wire.
Sealing gasket is provided with between the opening of described upper vessel portion and cover plate.
The opening of described cover plate and upper vessel portion is sealedly and fixedly connected by some securing members;
Described cover plate is cylindrical structural, and the central angle that adjacent two securing members and cover plate central form is 30 °.
The thickness of described cover plate is 15mm.
The diameter of described container is 200-300mm, and the height of container is 150-200mm, and wall of a container is thick is 15mm.
The range of regulation of described Regulation Control device is 1 standard atmospheric pressure-30MPa.
Described container is formed by plow-steel preparation.
The preparation method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention comprises the following steps:
1) dimensions specified according to Huey test standard peels off internal coated layer from metallurgical composite pipe, and wherein, it is thinning that the fused layers of internal coated layer does not carry out Linear cut, obtains pending sample;
2) a certain amount of thermoplastic acrylic resin powder, absolute ethyl alcohol and silicasol is got, stir, obtain slip, then the slurry of preparation is evenly brushed to step 1) on obtain non-test of pending sample, coating thickness is 1-2mm, dry, wherein, the ratio of thermoplastic acrylic resin powder, absolute ethyl alcohol and silicasol is 10-30g:100mL:2-3mL again;
3) by through step 2) dry the pending sample obtained and be positioned in container, the non-test of pending sample is faced up, again by cover plate by seal of vessel, then adjustment control and Regulation Control device, the temperature in container is made to be adjusted to 150-200 DEG C, pressure is adjusted to 20-30MPa, and keep 3-5mim, until non-test of the pending sample upper resin protective layer forming one deck densification, and then regulate Regulation Control device and controller, the pressure in container is made to be adjusted to normal atmosphere pressure, temperature is down to room temperature, obtain metallurgical composite pipe internal coated layer intercrystalline corrosion samples.
The present invention has following beneficial effect:
The preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention and method are when preparing metallurgical composite pipe internal coated layer intercrystalline corrosion samples, only need first to peel off internal coated layer from metallurgical composite pipe, it is thinning that the fused layers of internal coated layer does not carry out Linear cut, obtains pending sample; And then slurry is coated on non-test of pending sample; prevent after oven dry in container; in the pressure passed through in adjustment container and temperature; the resin protective layer of one deck densification can be formed on non-test of pending sample; ensure that the coating only having sample is corroded in corrosive liquid; thus improve the accuracy of Huey test result; metallurgical composite pipe internal coated layer intercrystalline corrosion samples prepared by the present invention meets the requirement of bending method and metallographic method evaluation intergranular corrosion cracks, and method for making is simple, convenient.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the schematic diagram of heating arrangement 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 securing member, 5 be Regulation Control device, 6 for heating arrangement, 6-1 be controller, 6-2 is resistance wire, 6-3 be thermopair, 7 is pipeline, 8 be source of the gas.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail:
With reference to figure 1, Fig. 2 and Fig. 3, the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention comprises container 1, cover plate 3, source of the gas 8, Regulation Control device 5, heating arrangement 6 and for providing the power supply of electric energy; Described cover plate 3 is tightly connected with the opening on container 1 top, source of the gas 8 is connected by the entrance of pipeline 7 with Regulation Control device 5, the outlet of Regulation Control device 5 is connected with the inside of container 1, heating arrangement 6 comprises controller 6-1 and heater strip, controller 6-1 is fixed on the outside of container 1, heater strip is positioned at container 1, and power supply is connected with heater strip by controller 6-1.
It should be noted that, described heater strip is resistance wire 6-2, and the present invention also comprises the thermopair 6-3 for measuring vessel inner wall temperature; Sealing gasket 2 is provided with between the opening on container 1 top and cover plate 3; Cover plate 3 is sealedly and fixedly connected by some securing members 4 with the opening on container 1 top; Described cover plate 3 is cylindrical structural, and the central angle that adjacent two securing members 4 and cover plate 3 center form is 30 °; The thickness of cover plate 3 is 15mm; The diameter of container 1 is 200-300mm, and the height of container 1 is 150-200mm, and 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 formed by plow-steel preparation.
The preparation method of metallurgical composite pipe internal coated layer intercrystalline corrosion samples of the present invention comprises the following steps:
1) dimensions specified according to Huey test standard peels off internal coated layer from metallurgical composite pipe, and wherein, it is thinning that the fused layers of internal coated layer does not carry out Linear cut, obtains pending sample;
2) a certain amount of thermoplastic acrylic resin powder, absolute ethyl alcohol and silicasol is got, stir, obtain slip, then the slurry of preparation is evenly brushed to step 1) on obtain non-test of pending sample, coating thickness is 1-2mm, dry, wherein, the ratio of thermoplastic acrylic resin powder, absolute ethyl alcohol and silicasol is 10-30g:100mL:2-3mL again;
3) by through step 2) dry the pending sample obtained and be positioned in container 1, the non-test of pending sample is faced up, by cover plate 3, container 1 is sealed again, then adjustment control 6-1 and Regulation Control device 5, the temperature in container 1 is made to be adjusted to 150-200 DEG C, pressure is adjusted to 20-30MPa, and keep 3-5mim, until non-test of the pending sample upper resin protective layer forming one deck densification, and then regulate Regulation Control device 5 and controller 6-1, the pressure in container 1 is made to be adjusted to normal atmosphere pressure, temperature is down to room temperature, obtain metallurgical composite pipe internal coated layer intercrystalline corrosion samples.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the preparation facilities of a metallurgical composite pipe internal coated layer intercrystalline corrosion samples, it is characterized in that, comprising container (1), cover plate (3), source of the gas (8), Regulation Control device (5), heating arrangement (6) and for providing the power supply of electric energy;
Described cover plate (3) is tightly connected with the opening on container (1) top, source of the gas (8) is connected by the entrance of pipeline (7) with Regulation Control device (5), the outlet of Regulation Control device (5) is connected with the inside of container (1), heating arrangement (6) comprises controller (6-1) and heater strip, controller (6-1) is fixed on the outside of container (1), heater strip is positioned at container (1), and power supply is connected with heater strip by controller (6-1).
2. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, is characterized in that, described heater strip is resistance wire (6-2).
3. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, is characterized in that, is provided with sealing gasket (2) between the opening on described container (1) top and cover plate (3).
4. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, is characterized in that, described cover plate (3) is sealedly and fixedly connected by some securing members (4) with the opening on container (1) top;
Described cover plate (3) is cylindrical structural, and the central angle that adjacent two securing members (4) and cover plate (3) center form is 30 °.
5. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, is characterized in that, the thickness of described cover plate (3) is 15mm.
6. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, it is characterized in that, the diameter of described container (1) is 200-300mm, and the height of container (1) is 150-200mm, and the wall thickness of container (1) is 15mm.
7. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, is characterized in that, the range of regulation of described Regulation Control device (5) is 1 standard atmospheric pressure-30MPa.
8. the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, is characterized in that, described container (1) is formed by plow-steel preparation.
9. a preparation method for metallurgical composite pipe internal coated layer intercrystalline corrosion samples, is characterized in that, based on the preparation facilities of metallurgical composite pipe internal coated layer intercrystalline corrosion samples according to claim 1, comprises the following steps:
1) dimensions specified according to Huey test standard peels off internal coated layer from metallurgical composite pipe, and wherein, it is thinning that the fused layers of internal coated layer does not carry out Linear cut, obtains pending sample;
2) a certain amount of thermoplastic acrylic resin powder, absolute ethyl alcohol and silicasol is got, stir, obtain slip, then the slurry of preparation is evenly brushed to step 1) on obtain non-test of pending sample, coating thickness is 1-2mm, dry, wherein, the ratio of thermoplastic acrylic resin powder, absolute ethyl alcohol and silicasol is 10-30g: 100mL: 2-3mL again;
3) by through step 2) dry the pending sample obtained and be positioned in container (1), the non-test of pending sample is faced up, by cover plate (3), container (1) is sealed again, then adjustment control (6-1) and Regulation Control device (5), the temperature in container (1) is made to be adjusted to 150-200 DEG C, pressure is adjusted to 20-30MPa, and keep 3-5mim, until non-test of pending sample upper formation one deck resin protective layer, and then regulate Regulation Control device (5) and controller (6-1), the pressure in container (1) is made to be adjusted to normal atmosphere pressure, temperature is down to room temperature, obtain metallurgical composite pipe internal coated layer intercrystalline corrosion samples.
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