CN108982187B - Gas protection sulfur coating device and coating method thereof - Google Patents
Gas protection sulfur coating device and coating method thereof Download PDFInfo
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- CN108982187B CN108982187B CN201811045968.0A CN201811045968A CN108982187B CN 108982187 B CN108982187 B CN 108982187B CN 201811045968 A CN201811045968 A CN 201811045968A CN 108982187 B CN108982187 B CN 108982187B
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 64
- 239000011593 sulfur Substances 0.000 title claims abstract description 64
- 238000000576 coating method Methods 0.000 title claims abstract description 49
- 239000011248 coating agent Substances 0.000 title claims abstract description 35
- 238000005485 electric heating Methods 0.000 claims abstract description 17
- 238000002347 injection Methods 0.000 claims abstract description 15
- 239000007924 injection Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 71
- 239000002184 metal Substances 0.000 claims description 43
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000004880 explosion Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 230000005587 bubbling Effects 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 description 22
- 230000007797 corrosion Effects 0.000 description 22
- 238000011160 research Methods 0.000 description 15
- 239000007788 liquid Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 3
- 230000008021 deposition Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000004677 hydrates Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 108010085603 SFLLRNPND Proteins 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
Abstract
The invention discloses a coating method of a gas protection sulfur coating device, which comprises two sets of gas protection devices, wherein the first set of gas protection devices comprises a first high-temperature-resistant wide-mouth bottle, a first gas catcher and an electric heating sleeve, the first high-temperature-resistant wide-mouth bottle is sealed by a first rubber plug, a first gas inlet and outlet pipeline communicated with the first high-temperature-resistant wide-mouth bottle is arranged on the first rubber plug, the first gas catcher is communicated with an outlet of the first gas outlet pipeline, and a tip mouth with a glass cock is arranged on the side wall of the first high-temperature-resistant wide-mouth bottle; the second gas protection device comprises a second high-temperature-resistant wide-mouth bottle and a second gas catcher, the second high-temperature-resistant wide-mouth bottle passes through a second rubber plug, a second gas inlet and outlet pipeline and an injection pipe which are communicated with the second high-temperature-resistant wide-mouth bottle are arranged on the second rubber plug, and the second gas catcher is communicated with the outlet of the second gas outlet pipeline; the coating method adopting the device can effectively avoid the oxidization of sulfur powder in the preparation link of the coated sulfur test sample.
Description
Technical Field
The invention relates to a gas protection sulfur coating device and a coating method thereof, which are suitable for preparing laboratory coating sulfur test research samples, can effectively avoid the oxidization problem in the heating and melting process of sulfur powder, and ensure the reliability of sample preparation during the coating sulfur corrosion resistance test research.
Background
In the production and development process of the high-sulfur gas reservoir, when the solubility of the elemental sulfur in the gas reaches critical saturation, the temperature and the pressure are continuously reduced, and the elemental sulfur is separated out and deposited under certain conditions. During the transport of sulfur-containing oil and gas, liquid hydrates can partially dissolve gaseous elemental sulfur, and when these liquid hydrates evaporate, particulate sulfur deposits can form at the bottom of the pipeline. Elemental sulfur corrosion is one of the most serious corrosion in oil and gas field development, and because the sulfur element is in the third period, the outermost layer is 6 electrons, electrons are easy to lose, the sulfur compound has multiple valence, and the sulfur compound is rich and colorful. The variety of the existence forms of the sulfur elements makes the sulfur corrosion mechanism rich and complex, and although the corrosion mechanism of sulfur has been studied to a certain extent, the corrosion rule and mechanism of sulfur in the high-temperature and high-pressure environment are still the current research hot spot. The currently commonly used sulfur element corrosion research methods include the following three methods: (1) Directly adding sulfur powder into the corrosion solution, forming a suspension sulfur-containing solution through a stirrer, and carrying out corrosion research on the suspension sulfur solution; (2) Placing the sample at the bottom of the container, and burying the sample in sulfur deposited at the bottom of the container to perform corrosion resistance study; (3) And (3) coating sulfur powder on the surface of the metal test piece, and placing the metal test piece in a corrosive medium to perform corrosion resistance test. The methods are applicable to corrosion researches in different forms, and the corrosion research of the 1 st suspended sulfur solution can realize the corrosion research of the sulfur-containing suspension solution on a sample, and does not study the corrosion caused by sulfur deposition; the 2 nd method is characterized in that the corrosion of deposited sulfur is studied, but the combination mode is that the surface of a sample is covered with the whole surface of the sample in a loose way, which is not in accordance with the actual condition of most pipeline sulfur corrosion, the on-site corrosion failure mode is realized, particularly, the sulfur deposition is attached to the inner wall of a pipeline in a single-sided, discontinuous point-shaped or irregular mode at the inclined position of a downhole tubular column, the low-lying position of a pipeline or the position of rapid pressure drop of downstream equipment, the corrosion test in the sulfur coating mode is more similar to the actual condition, and the 3 rd research method is the research method which is in most accordance with the on-site working condition. However, in the research process, it is found that, because the bottom of the well or some of the conveying medium does not contain oxygen, the preparation method of melting sulfur powder (the melting point of elemental sulfur is 115.217 ℃) by heating, which is commonly used in the preparation process, and coating the sulfur powder on the surface of the sample has problems, which can lead to oxidation of the sulfur powder and bring errors to experimental research.
Disclosure of Invention
The invention provides a gas protection sulfur coating device and a coating method thereof, which are designed for avoiding oxidization of sulfur powder caused by heating and melting of the sulfur powder in air in a sample preparation link of a sulfur coating test research, and can effectively avoid oxidization of the sulfur powder in the sample preparation link of the sulfur coating test.
The invention is realized by adopting the following technical scheme:
a gas-shielded sulfur coating device, which comprises a first set of gas-shielded device for carrying out the melting treatment of sulfur powder under a protective atmosphere, and a second gas-shielded device for the gas shielding of the coating process; wherein,
the first set of gas protection device comprises a first high-temperature-resistant wide-mouth bottle, a first gas catcher and an electric heating sleeve, wherein the electric heating sleeve is used for heating the first high-temperature-resistant wide-mouth bottle;
the second gas protection device comprises a second high-temperature-resistant wide-mouth bottle and a second gas catcher, the second high-temperature-resistant wide-mouth bottle is sealed through a second rubber plug, a second air inlet pipeline, a second air outlet pipeline and an injection pipe which are communicated with the second high-temperature-resistant wide-mouth bottle are arranged on the second rubber plug, and the second gas catcher is communicated with the outlet of the second air outlet pipeline;
when in use, the sulfur powder to be heated is arranged in the first high-temperature-resistant wide-mouth bottle, and the metal sample to be sulfur-coated is arranged in the second high-temperature-resistant wide-mouth bottle and is positioned right below the outlet of the injection pipe.
The invention is further improved in that the first set of gas protection devices further comprises a thermometer which is communicated from the first rubber stopper to the inside of the first high temperature resistant jar.
A further development of the invention is that the first inlet line is provided with a first flowmeter.
The invention is further improved in that the second inlet line is provided with a second flowmeter.
A further improvement of the invention is that the filling pipe is provided with a glass tap.
The invention is further improved in that valves are arranged on the first air inlet pipeline and the first air outlet pipeline.
The invention is further improved in that valves are arranged on the second air inlet pipeline and the second air outlet pipeline.
The gas protection sulfur coating method adopts the gas protection sulfur coating device, and comprises the following steps:
1) Preparation of a metal sample: preparing a metal sample according with the required size according to the requirement;
2) Preparation of a metal sample: polishing a metal sample to the finish of 800# abrasive paper or higher, and finally cleaning, drying, measuring the size and weighing; preparing paper sheets with the same size, drawing the shape of the required coated sulfur on the paper sheets, cutting off, pasting the paper sheets on test pieces, recording the pasting area and the shape, and placing the metal test sample in a second high-temperature-resistant wide-mouth bottle;
3) Oxygen removal by the gas protection device: respectively placing sulfur powder with set quality and prepared metal samples into two high-temperature-resistant wide-mouth bottles, opening an inert gas inlet valve, and carrying out deoxidization treatment on a second high-temperature-resistant wide-mouth bottle at least for 20min according to the volume of the container per liter at a minimum speed of 100mL/min, wherein the smoothness of a gas inlet and outlet pipeline is ensured during deoxidization, and the explosion of accumulated gas in the second high-temperature-resistant wide-mouth bottle under higher pressure is avoided;
4) Melting sulfur powder: starting an electric heating sleeve to 115 ℃ to melt sulfur powder, and introducing nitrogen at a small uninterrupted flow rate all the time, wherein the size of the nitrogen is controlled according to bubbles in the first gas catcher solution, and the gas inflow is indicated by the bubbling of the bubbles;
5) And opening a piston on a tip at one side of the first high-temperature-resistant wide-mouth bottle, discarding a few drops of molten sulfur which flows out first, coating the molten sulfur on the exposed part of the surface of the metal sample through an injection pipe, taking out the metal sample after cooling and fixing, and removing paper sheets to obtain the metal sample coated into a fixed shape and size.
The invention has the following beneficial technical effects:
the gas protection sulfur coating device and the coating method thereof provided by the invention have the advantages that the structure is simple, the operation is convenient, the oxidation caused by the heating process of sulfur powder in the research of a sulfur coating corrosion test can be avoided, the coating effect of the sulfur powder is ensured, the cost is low, and the gas protection sulfur coating device and the coating method thereof are easy to popularize in other fields needing solid or solid-liquid substance heating coating.
Drawings
FIG. 1 is a schematic view of a first set of gas protection devices;
in the figure: 1-electric heating sleeve, 2-first high temperature resistant wide-mouth bottle, 3-sulfur powder, 4-first air inlet pipeline, 5-thermometer, 6-first rubber plug, 7-first flowmeter, 8-first air outlet pipeline, 9-first gas catcher, 10-tip mouth with glass cock.
FIG. 2 is a schematic diagram of a second set of gas-shield apparatus;
in the figure: 11-second high temperature resistant wide-mouth bottle, 12-metal sample, 13-second inlet line, 14-second rubber stopper, 15-second flowmeter, 16-second outlet line, 17-second gas trap, 18-injection tube (with glass cock).
Detailed Description
The invention is further described below with reference to the drawings and examples.
The invention is designed for avoiding the oxidization of sulfur powder caused by the heating and melting of the sulfur powder in the air in the sample preparation link of the test research of the coating sulfur.
The invention provides a gas protection sulfur coating device which comprises two sets of gas protection devices, namely a first set of gas protection device and a second set of gas protection device.
As shown in fig. 1, the first set of gas protection device is used for carrying out the melting treatment of sulfur powder in a protective atmosphere and comprises an electric heating sleeve 1, a first high-temperature-resistant wide-necked bottle 2 (one side of which is provided with a tip 10 with a glass cock), a first air inlet pipeline 4, a first flowmeter 7, a thermometer 5, a first rubber plug 6, a first air outlet pipeline 8 and a first gas catcher 9; the second gas protection device is used for gas protection of the coating process and comprises a second high temperature resistant jar 11, a second gas inlet line 13, a second flowmeter 15, a second rubber stopper 14, a second gas outlet line 16, a second gas trap 17 and an injection tube 18 (with a glass plug).
In the first set of gas protection device, a first high-temperature-resistant wide-mouth bottle 2 is arranged in an electric heating sleeve 1, heating temperature is controlled through the electric heating sleeve 1, sulfur powder 3 is melted, and meanwhile, heating temperature is determined and calibrated through a measured thermometer 5. The first high temperature resistant wide-mouth bottle 2 is sealed through a first rubber plug 6, three holes are formed in the first rubber plug 6, one is used for installing a thermometer 5, the other two are respectively used for installing a first air inlet pipeline 4 and a first air outlet pipeline 8, the first air inlet pipeline 4 and the first air outlet pipeline 8 are both flexible pipes and ensure the length enough to operate, the first air inlet pipeline 4 stretches into the bottom of the first high temperature resistant wide-mouth bottle 2, and the first air outlet pipeline 8 is located at the lower end of the first rubber plug 6. High purity inert gas is introduced through the first air inlet line 4 to displace air from the first high temperature resistant jar 2 for a period of time related to flow rate and volume of the first high temperature resistant jar 2, the flow rate being controlled by the first flow meter 7. The gas is discharged through the first gas outlet pipeline 8, so that the first high-temperature-resistant wide-mouth bottle 2 is ensured not to have excessively high pressure accumulation, and the safety is ensured. The end of the first gas outlet pipeline 8 is connected with a first gas catcher 9, and the flow of the discharged gas can be observed through the first gas catcher 9. The tip 10 with a glass cock is arranged on one side of the first high-temperature-resistant wide-mouth bottle 2, a piston is arranged on the tip 10 with the glass cock, a round hole is arranged on the piston, and the outflow of molten sulfur can be controlled by adjusting the round hole of the piston, so that the molten sulfur can be coated on the surface of the metal sample 12.
When in use, the utility model is characterized in that: 1) The required amount of sulfur powder 3 is filled into a first high temperature resistant wide-mouth bottle 2, a thermometer 5 and a first air inlet pipeline 4 are connected on a first rubber plug 6, and the first high temperature resistant wide-mouth bottle 2 is sealed; 2) Placing the first high-temperature-resistant wide-mouth bottle 2 in the electric heating sleeve 1, introducing inert gas to displace air in the first high-temperature-resistant wide-mouth bottle 2, calculating and determining displacement time according to the first high-temperature-resistant wide-mouth bottle 2 and the adopted gas flow, observing the gas flow condition through the first gas catcher 9, and avoiding oversized or bubble-free production; 3) After the displacement is finished, an air inlet valve is regulated, so that the first gas catcher 9 keeps slow occurrence of bubbles (micro positive pressure); 4) Setting the temperature of the heating sleeve to a required temperature, starting a switch, and displaying the temperature through a thermometer 5 to adjust the temperature setting of the electric heating sleeve 1 so as to enable the electric heating sleeve to be at the sulfur powder melting temperature; 5) After the sulfur powder is melted, the switch of the electric heating sleeve 1 is closed; 6) The application of the molten sulfur is accomplished through a sharp nozzle on one side of the first gas trap 9.
In the second set of gas protection device, a second air inlet pipeline 13 is used for introducing inert gas, a second air outlet pipeline 17 is used for exhausting gas, the function of the second air inlet pipeline is consistent with that of the first gas protection device, an injection pipe 18 is arranged in the middle of a second rubber plug 14, and a valve is arranged at the upper part of the injection pipe 18 to inject molten sulfur through the injection pipe, so that the molten sulfur is coated on the surface of a metal sample 12 in a second high-temperature-resistant wide-mouth bottle 11.
The invention provides a gas protection sulfur coating method, which comprises the following steps:
1) Preparation of a metal sample: the metal sample 12 is machined to the desired dimensions as required, preferably to a rectangular metal sample of 40 x 10 x 3mm, which may be perforated at one end of the sample, for subsequent corrosion studies, which may be suspended.
2) Preparation of a metal sample: polishing the metal sample 12 to the finish of 800# abrasive paper or higher, and finally cleaning, drying, measuring the size and weighing; a sheet of paper of the same size was prepared, the shape of the desired sulfur-coated (usually circular or linear with a certain width) was drawn on the sheet, cut off, stuck to the test piece (either one or both sides), and the stuck area and shape were recorded, and the metal sample 12 was placed in the second high temperature-resistant jar 11.
3) Oxygen removal by the gas protection device: respectively placing sulfur powder 3 with set quality and a prepared metal sample 12 into two high-temperature-resistant wide-mouth bottles, opening an inert gas inlet valve, and carrying out deoxidization treatment on a second high-temperature-resistant wide-mouth bottle 11 by introducing at least 20min per liter according to the volume of a container at a minimum rate of 100mL/min, wherein a gas inlet and outlet pipeline is ensured to be smooth during deoxidization, so that explosion of accumulated gas in the second high-temperature-resistant wide-mouth bottle 11 under higher pressure is avoided.
4) Melting sulfur powder: the electric heating sleeve 1 is started to 115 ℃ to melt the sulfur powder 3, and nitrogen is always introduced at a small flow rate during the period, the size of the nitrogen can be controlled according to bubbles in the solution of the first gas catcher 9, and the occurrence of bubbles indicates that the gas flows in.
5) And opening a piston on a tip at one side of the first high-temperature-resistant wide-mouth bottle 2, discarding 2 drops of molten sulfur which flow out firstly, coating molten sulfur on the exposed part of the surface of the metal sample 12 through an injection pipe 18, taking out the metal sample 12 after cooling and fixing, and removing paper sheets to obtain the metal sample 12 coated into a fixed shape and size.
Examples
The preparation of a 316L stainless steel material coated sulfur corrosion test sample is exemplified.
1) Preparing a metal sample. Preparing a strip-shaped metal sample, and punching holes at the end of the metal sample for hanging or fixing; the metal sample is sanded and polished by sand paper, deoiled by solvent, dehydrated by alcohol, dried, then weighed and measured for size.
2) The surface of the metal sample is provided with a bare part with the diameter of 5mm, the rest is covered by paper, and the metal sample is placed in a second high-temperature-resistant wide-mouth bottle 11 for deoxidization treatment, and then micro-positive pressure treatment is carried out for standby.
3) Melting of sulfur powder. Placing 100g of sulfur powder 3 into a first high-temperature-resistant wide-mouth bottle 2, connecting a first air inlet pipeline 4, a first air outlet pipeline 8 and a thermometer 5, and sealing a bottle mouth; deoxidizing the first high-temperature-resistant wide-mouth bottle 2 by using nitrogen; after the deoxidation is completed, reducing the flow of inert gas to ensure that the first high-temperature-resistant wide-mouth bottle 2 is kept at micro positive pressure, so as to avoid air from entering; and opening the electric heating sleeve 1, heating to 119 ℃ of sulfur powder melting point, melting the sulfur powder, and closing the electric heating sleeve 1 when the temperature is stable.
4) And (5) sulfur powder coating. Taking out the first high-temperature-resistant wide-mouth bottle 2 with the heat-insulating glove, opening a sharp-mouth piston with a glass cock on the first high-temperature-resistant wide-mouth bottle 2, discarding 2 drops of molten sulfur at the front end, closing the piston, then rapidly connecting the piston with an injection port of the second high-temperature-resistant wide-mouth bottle 11, opening two pistons, and coating liquid sulfur on the surface of the metal sample 12; after cooling, the metal coupon 12 was tapped to confirm the coating was firm and the coating was complete.
Claims (6)
1. A gas-shielded sulfur coating device, which is characterized by comprising a first set of gas-shielded devices for carrying out the melting treatment of sulfur powder under a protective atmosphere, and a second set of gas-shielded devices for the gas shielding of the coating process; wherein,
the first set of gas protection device comprises a first high-temperature-resistant wide-mouth bottle (2), a first gas catcher (9) and an electric heating sleeve (1) for heating the first high-temperature-resistant wide-mouth bottle (2), wherein the first high-temperature-resistant wide-mouth bottle (2) is sealed through a first rubber plug (6), a first air inlet pipeline (4) and a first air outlet pipeline (8) which are communicated with the first high-temperature-resistant wide-mouth bottle (2) are arranged on the first rubber plug (6), the first gas catcher (9) is communicated at the outlet of the first air outlet pipeline (8), and a sharp nozzle (10) with a glass cock is arranged on the side wall of the first high-temperature-resistant wide-mouth bottle (2);
the second set of gas protection device comprises a second high-temperature-resistant wide-mouth bottle (11) and a second gas catcher (17), the second high-temperature-resistant wide-mouth bottle (11) is sealed by a second rubber plug (14), a second air inlet pipeline (13), a second air outlet pipeline (16) and an injection pipe (18) which are communicated with the second high-temperature-resistant wide-mouth bottle (11) are arranged on the second rubber plug (14), and the second gas catcher (17) is communicated at the outlet of the second air outlet pipeline (16);
when in use, the sulfur powder (3) to be heated is arranged in the first high-temperature-resistant wide-mouth bottle (2), and the metal sample (12) to be sulfur-coated is arranged in the second high-temperature-resistant wide-mouth bottle (11) and is positioned right below the outlet of the injection pipe (18);
the first set of gas protection device also comprises a thermometer which is communicated with the inside of the first high-temperature-resistant wide-mouth bottle (2) from the first rubber stopper (6);
a glass cock is provided on the injection tube (18).
2. A gas-shielded sulfur coating device according to claim 1, characterized in that the first inlet line (4) is provided with a first flow meter (7).
3. A gas-shielded sulfur coating device according to claim 2, characterized in that the second inlet line (13) is provided with a second flowmeter (15).
4. A gas-shielded sulfur coating apparatus according to claim 1, wherein valves are provided on both the first inlet line (4) and the first outlet line (8).
5. A gas-shielded sulfur coating apparatus according to claim 1, wherein the second inlet line (13) and the second outlet line (16) are each provided with a valve.
6. A gas-shielded sulfur coating method, characterized in that the method employs a gas-shielded sulfur coating apparatus according to any one of claims 1 to 5, comprising the steps of:
1) Preparation of a metal sample: preparing a metal sample (12) according to the required size according to the requirement;
2) Preparation of a metal sample: polishing a metal sample (12) to a finish of 800# sandpaper or a higher finish, and finally cleaning, drying, measuring the size and weighing; preparing paper sheets with the same size, drawing the shape of the required sulfur coating on the paper sheets, cutting off, pasting the paper sheets on test pieces, recording the pasting area and the shape, and placing a metal sample (12) in a second high-temperature-resistant wide-mouth bottle (11);
3) Oxygen removal by the gas protection device: respectively placing sulfur powder (3) with set quality and a prepared metal sample (12) into two high-temperature-resistant wide-mouth bottles, opening an inert gas inlet valve, and carrying out deoxidization treatment on a second high-temperature-resistant wide-mouth bottle (11) according to the volume of the container at least by introducing 20min per liter at a minimum rate of 100mL/min, wherein a gas inlet and outlet pipeline is ensured to be unblocked during deoxidization, so that the explosion of accumulated gas in the second high-temperature-resistant wide-mouth bottle (11) under higher pressure is avoided;
4) Melting sulfur powder: the electric heating sleeve (1) is started to 115 ℃ to melt the sulfur powder (3), and nitrogen is always introduced at a small uninterrupted flow rate during the melting, the size of the nitrogen is controlled according to bubbles in the solution of the first gas catcher (9), and the gas inflow is indicated by the bubbling;
5) And opening a piston on a tip at one side of the first high-temperature-resistant wide-mouth bottle (2), discarding a few drops of molten sulfur which flows out first, coating molten sulfur on the exposed part of the surface of the metal sample (12) through an injection pipe (18), taking out the metal sample (12) after cooling and fixing, and removing paper sheets to obtain the metal sample (12) coated into a fixed shape and size.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19836215A1 (en) * | 1997-08-12 | 1999-02-18 | Elementar Analysensysteme Gmbh | Reactor for an elemental analysis system |
| CN201855700U (en) * | 2010-10-09 | 2011-06-08 | 中国石油化工股份有限公司 | Low-oxygen processing device for laboratory polymer solution |
| CN203758889U (en) * | 2014-01-21 | 2014-08-06 | 中国科学院金属研究所 | Device applied to environment corrosion split test in wet hydrogen sulfide environment |
| CN104828782A (en) * | 2014-02-07 | 2015-08-12 | 苏尔瓦瑞斯公司 | Micronized sulphur powder and method of production of same |
| CN106110913A (en) * | 2016-06-17 | 2016-11-16 | 中国工程物理研究院化工材料研究所 | Standard Gases stream generation apparatus |
| CN205943263U (en) * | 2016-06-03 | 2017-02-08 | 蒋玥培 | Environment -friendly experimental apparatus that sulphur and oxygen fully react |
| CN206990287U (en) * | 2017-03-17 | 2018-02-09 | 中国石油化工股份有限公司 | For determining the purging absorption plant of hydrogen sulfide content |
| CN108489886A (en) * | 2018-03-07 | 2018-09-04 | 中国石油天然气集团有限公司 | A kind of gas storage tube corrosion simulator and the analogy method based on the device |
| CN208953347U (en) * | 2018-09-07 | 2019-06-07 | 中国石油天然气集团有限公司 | A kind of gas shield sulphur coating unit |
-
2018
- 2018-09-07 CN CN201811045968.0A patent/CN108982187B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19836215A1 (en) * | 1997-08-12 | 1999-02-18 | Elementar Analysensysteme Gmbh | Reactor for an elemental analysis system |
| CN201855700U (en) * | 2010-10-09 | 2011-06-08 | 中国石油化工股份有限公司 | Low-oxygen processing device for laboratory polymer solution |
| CN203758889U (en) * | 2014-01-21 | 2014-08-06 | 中国科学院金属研究所 | Device applied to environment corrosion split test in wet hydrogen sulfide environment |
| CN104828782A (en) * | 2014-02-07 | 2015-08-12 | 苏尔瓦瑞斯公司 | Micronized sulphur powder and method of production of same |
| CN205943263U (en) * | 2016-06-03 | 2017-02-08 | 蒋玥培 | Environment -friendly experimental apparatus that sulphur and oxygen fully react |
| CN106110913A (en) * | 2016-06-17 | 2016-11-16 | 中国工程物理研究院化工材料研究所 | Standard Gases stream generation apparatus |
| CN206990287U (en) * | 2017-03-17 | 2018-02-09 | 中国石油化工股份有限公司 | For determining the purging absorption plant of hydrogen sulfide content |
| CN108489886A (en) * | 2018-03-07 | 2018-09-04 | 中国石油天然气集团有限公司 | A kind of gas storage tube corrosion simulator and the analogy method based on the device |
| CN208953347U (en) * | 2018-09-07 | 2019-06-07 | 中国石油天然气集团有限公司 | A kind of gas shield sulphur coating unit |
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