CN101393110A - Phosphorus sulfur multi-component high temperature corrosion test system and test methods of yellow phosphorus end gas - Google Patents
Phosphorus sulfur multi-component high temperature corrosion test system and test methods of yellow phosphorus end gas Download PDFInfo
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- CN101393110A CN101393110A CNA2008100587104A CN200810058710A CN101393110A CN 101393110 A CN101393110 A CN 101393110A CN A2008100587104 A CNA2008100587104 A CN A2008100587104A CN 200810058710 A CN200810058710 A CN 200810058710A CN 101393110 A CN101393110 A CN 101393110A
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- 238000012360 testing method Methods 0.000 title claims abstract description 69
- 230000007797 corrosion Effects 0.000 title claims abstract description 62
- 238000005260 corrosion Methods 0.000 title claims abstract description 62
- 238000010998 test method Methods 0.000 title claims abstract description 14
- OTYNBGDFCPCPOU-UHFFFAOYSA-N phosphane sulfane Chemical compound S.P[H] OTYNBGDFCPCPOU-UHFFFAOYSA-N 0.000 title claims description 10
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 title description 7
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- 239000000523 sample Substances 0.000 claims description 26
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 23
- 229910052863 mullite Inorganic materials 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 18
- 239000000919 ceramic Substances 0.000 claims description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 229910052573 porcelain Inorganic materials 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
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- 229910000831 Steel Inorganic materials 0.000 claims description 4
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 17
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Abstract
The invention relates to a high temperature corrosion test system and a high temperature corrosion test method, in particular to a high temperature corrosion test system and a high temperature corrosion test method for phosphor-sulfur polycomponent of yellow phosphoric tail gas. The high temperature corrosion test system for the phosphor-sulfur polycomponent of the yellow phosphoric tail gas comprises a high temperature corrosion simulation test system for the phosphor-sulfur polycomponent of the yellow phosphoric tail gas, which consists of four parts, namely a medium distribution system, a heating temperature control system, a tail gas treatment system and a concentration determination system. A hearth of a test device of the high temperature corrosion test system adopts a nonmetallic heating element, namely a siliconit, so that the high temperature corrosion test system has good corrosion resistance, is quick in heating, and is safe and stable; the high temperature corrosion test system is provided with a tail gas absorption apparatus, so that no pollutant is generated in the test; polycomponent etchant gas can be injected, so that the high temperature corrosion test system and method can well simulate the high temperature corrosion research on boiler materials during the process of comprehensive utilization of the yellow phosphoric tail gas; and simultaneously the high temperature corrosion test system and method can also be used for comprehensive utilization of other industrial waste gas (tail gas).
Description
Technical field
The present invention relates to a kind of high-temperature corrosion testing system and method, especially a kind of yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion test system and test method.
Background technology
Produce a large amount of yellow phosphoric tail gas in the yellow phosphorus industry production process, produce 1 ton of yellow phosphorus and produce yellow phosphoric tail gas 2500-3000Nm approximately
3Reaching 83.07 ten thousand tons with national output phosphor in 2006 is example, and the yellow phosphoric tail gas generation is up to 2,300,000,000 Nm
3According to one's analysis, the yellow phosphoric tail gas complicated component, (CO85%～95%V) and objectionable constituent (phosphorus, sulphur, arsenic etc.), directly a day lamp is put or put to sky, is not only the wasting of resources, and causes serious atmospheric pollution to contain a large amount of greenhouse gases." yellow phosphorus industry access condition " issued in various places in recent years, and the investment construction of yellow phosphorus enterprise is controlled in strictness, and to existing small scale, heavy-polluted small-sized yellow phosphorus enterprise carries out time limit and eliminates, closes, removes." Yunnan Province's yellow phosphorus industry access condition " regulation as in June, 2005 Yunnan Province's promulgation: newly throwing phosphorus production device separate unit designed capacity must be more than 10000 ton/year, existing separate unit must eliminate, close, remove before the end of the year 2007 below 10000 tons/year.Comprehensive utilization of resources facilities such as the necessary synchronized construction yellow phosphoric tail gas of new project, slag.
Since the nineties in 20th century, domestic some enterprise or research unit carried out some trials to utilizing yellow phosphoric tail gas as boiler fuel.Mainly be the fuel that yellow phosphoric tail gas is used as middle low-pressure boiler, as be used for dried feed, produce hot water and steam etc., but the corrosion mechanism research to tail gas under yellow phosphoric tail gas combustion characteristics and the high temperature is few, it is worked as conventional combustion gas utilization, cause the boiler component material corrosion to lose efficacy, shorten equipment life greatly.For example: Yunnan chemical industrial company, finish " yellow phosphoric tail gas replaces the energy-conservation technological transformation project of boiler combustion coal " end of the year 1998, yet utilize in the process when finding the yellow phosphoric tail gas burning corrosion of boiler very serious as fuel at yellow phosphoric tail gas, after 3 months operation, boiler is scrapped because of corrosion punctures, and mounted three complete equipments are forced to stop; Sichuan chemical company once developed 2 40 tons of/hour steam boilers that use yellow phosphoric tail gas, just scrapped because of seriously corroded in 40 days as a result; Nanjing chemical research institute, a 100Kg/cm
2Heat interchanger is scrapped because of corrosion less than a month Tube Sheet of Heat Exchanger; Yunnan phosphorus goods company invests to build three hot-water boilers, moves that corrosion and fouling appear in superheating surface in 3～4 months boilers, and heat exchange efficiency is not high and need the frequent parts or the like of changing.
Therefore, China's yellow phosphoric tail gas is failed well as the boiler fuel recycling owing to its high temperature corrosion especially severe always at present.The anticorrosion that yellow phosphoric tail gas is made boiler fuel be phosphorus production enterprise increasingly competitive, seek the important technology on the road of energy-saving and emission-reduction, consumption reduction under the situation of entry criteria increasingly stringent.
Summary of the invention
Solve yellow phosphoric tail gas difficult problem to boiler material high temperature corrosion harm in comprehensive utilization, certainly will will start with to the research of the high temperature corrosion mechanism of boiler material from yellow phosphoric tail gas.And the site test complicated condition, influence factor is many, and the control difficulty is big; It is controlled that simulation test has factor, the accuracy height, and advantage such as the test period is flexible is the important means of research yellow phosphoric tail gas high temperature corrosion mechanism.
Purpose of the present invention just provides a kind of objectionable constituent such as phosphorus, sulphur of studying in the yellow phosphoric tail gas to the simulation experiment system and the test method of boiler material high temperature corrosion.The anticorrosion technique research of making boiler fuel for yellow phosphoric tail gas provides reliable accurate simulation experiment system and test method.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
High-temperature corrosion testing system comprises corrosive medium gas distributing system, heating temperature-controlling system, exhaust treatment system, concentration determination system.
Described corrosive medium gas distributing system (I) comprises 3 gas cylinders, N at least
2Gas cylinder (19), PH
3Gas cylinder (20), H
2S gas cylinder (21), insert suspended body flowmeter (22) by pipeline respectively, flowmeter (22) other end all inserts gas mixing device (23), the gas mixing device endpiece is connected with the high-temperature corrosion device burner hearth (3) of heating in the temperature-controlling system, etchant gas mixes through gas mixing device (23), and the burner hearth outlet side is furnished with vacuum pump (25).
Described heating temperature-controlling system (II) comprises heating part and automatic temperature-adjusting control section; the critical piece of heating part has high temperature silicon carbon-point (7); run through one-shot forming mullite burner hearth (3) up and down; be fixed on alumina silicate fibre insulation material outside; sample evenly is placed on burner hearth central authorities, and the device skin is anti-rust metal shell (1), has safeguard protection cover (15); Elema is in series, and the two ends lead-in wire links to each other with controllable silicon automatic temperature-adjusting controller electric furnace binding post.
Described exhaust treatment system (III) comprises that at least 3 taper absorption bottles (28) connect successively, and the alkali lye that is used for absorption test tail gas is housed in the absorption bottle, is furnished with vacuum pump (24) and coil condenser (25) before absorption bottle.
Described concentration determination system (IV) comprises at least 3 taper absorption bottles (30), a small size vacuum aspiration pump (27), acid-resisting rubber plug and thickening rubber tube are tightly connected, and before entering the small size vacuum aspiration pump, join coil condenser (25), the distilled water that is used to absorb from the gas attack medium of burner hearth is housed respectively in the absorption bottle.
The present invention provides a kind of yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion test method simultaneously, to treat pilot boiler steel raw material 20g before the test, 20G, 16MnR is processed into standard sample, 6 groups of every kind of materials, every group of 3 parallel samples, polishing rust-removal is carried out on the surface to be handled, put into oven drying, rectangle porcelain side ship is cleaned, and puts into more than the baking oven 30min, weighs more than three times, until empty porcelain side ship mass conservation, sample is put into porcelain side's ship, weigh, numbering is processed into the mechanical property sample with above boiler plate raw material, 6 groups of every kind of materials, every group of 3 parallel samples; Call through test device power supply, uni-directional push-button switch 14 is transferred to " ON " shelves, button on digital display temperature indication adjusting apparatus 10 operation interfaces is transferred to " setting " retaining, operation knob, set 1200 ℃ of required holding temperatures, 1000 ℃, 900 ℃, 800 ℃, 750 ℃, 700 ℃, 650 ℃, 600 ℃, 550 ℃, 500 ℃, after temperature is set and finished button is transferred to " measurement " and keep off; Adjusting pressuring knob 13 on automatic temperature-controlled instrument 9 operation interfaces of KSY type controllable silicon, regulation voltage is to 220V; Digital display temperature indication adjusting apparatus 10 real-time digitals show the temperature in the mullite flame-proof burner hearth 3 in the temperature-rise period; After reaching the setting holding temperature, digital display temperature indication adjusting apparatus 10 auxiliary reclays discharge; Under the effect of auxiliary reclay, the connected sum of control contactor disconnects, reach power supply and outage, make test unit can remain on 1200 ℃, 1000 ℃, 900 ℃, 800 ℃, 750 ℃, 700 ℃, 650 ℃, 600 ℃, 550 ℃ of the temperature of setting, 500 ℃ of constant temperature work device; Reach and set porcelain side's ship that sample will be housed after the test temperature and put into burner hearth, close ceramic pipe tail gas hole 4, open N
2Gas cylinder 19 valves are regulated flow to 15L/min, and inflated with nitrogen in mullite flame-proof burner hearth 3 is guaranteed to be full of nitrogen in the mullite flame-proof burner hearth 3, closes N
2Gas cylinder 19 valves start vacuum pump 24, burner hearth are vacuumized three times repeatedly; Feed hybrid corrosion dielectric gas (H
2S+PH
3): volume 1:1, concentration content is respectively 4000mg/Nm
3, 3000mg/Nm
3, 2000mg/Nm
3, 1000mg/Nm
3, 500mg/Nm
3, 100mg/Nm
3Test period is 48h, and the routine weighing time is 0h, 8h, 16h, 24h, 32h, 40h, 48h; Arrival is weighed the time, closes PH earlier
3Gas cylinder 20, H
2S gas cylinder 21 valves and gas mixing device 23 are opened N
2Gas cylinder 19, inflated with nitrogen in burner hearth is removed residue etchant gas in the burner hearth; Close N
2Gas cylinder 19, the side's of taking-up ship is put into drying basin immediately and is cooled to room temperature, in precision is to weigh on 1/10000 the electronic balance; Weigh finish after, open N successively
2 Gas cylinder 19, vacuum pump 24, inflated with nitrogen vacuumizes; Continue test,, repeat above step until the next time point of weighing.Behind the 48h, close PH
3Gas cylinder 20, H
2S gas cylinder 21 valves and gas mixing device 23 are opened N
2Gas cylinder 19, inflated with nitrogen is removed in the burner hearth and is remained etchant gas in burner hearth; The stopping device power supply takes out the last batch of sample; Get blank sample and 3 samples that uniform corrosion is separated by wherein, make metallographic examination, XRD, SEM and EDS and analyze; The mechanical property sample is done bending test, impulse test, tension test.
The principle (technical scheme) of the yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion simulation experiment method that the present invention relates to is as follows:
Yellow phosphoric tail gas combustion high temperature corrosion test is simulated in the chamber by experiment, with phosphorous, the distribution of sulfur corrosion medium, mix and to be transported to the high temperature corrosion test unit, get some kind boiler materials and make in the environment that standard specimen is exposed to different corrosive concentration gradients and thermograde.The mass change of periodic logging corrosion sample is observed surface topography in the process of the test, and sampling is regularly preserved.By metallographic examination, XRD, analysis means such as SEM and EDS, the structure of analytical sample, corrosion product surface topography and corrosion product composition are done measuring mechanical property to the sample before and after the test.Study phosphorous, the sulfur corrosion medium high temperature corrosion thermodynamics and kinetics rule to boiler material with this, the research of making gas fired-boiler fuel for yellow phosphoric tail gas provides accurate and reliable laboratory data and theory.
Described high-temperature corrosion testing system comprises corrosive medium gas distributing system, heating temperature-controlling system, exhaust treatment system, concentration determination system.Wherein the corrosive medium gas distributing system comprises at least 3 gas cylinders, is connected to gas mixing device by pipeline, and wherein each pipeline is respectively fitted with flowmeter.The gas mixing device endpiece is connected with the high-temperature corrosion device burner hearth of heating in the temperature-controlling system.The burner hearth outlet side is furnished with vacuum pump, is used for removing the impurity composition of air before the test.The heating temperature-controlling system comprises heating part and automatic temperature-adjusting control section composition.The critical piece of heating part has the high temperature silicon carbon-point, runs through one-shot forming mullite burner hearth up and down, is fixed on alumina silicate fibre insulation material outside.Sample evenly is placed on burner hearth central authorities.The device skin is the anti-rust metal shell, has the safeguard protection cover.Elema is in series, and the two ends lead-in wire links to each other with controllable silicon automatic temperature-adjusting controller electric furnace binding post.Exhaust treatment system comprises that at least 3 taper absorption bottles connect successively, and acid-resisting rubber plug and thickening rubber tube are tightly connected, and are furnished with coil condenser before entering absorption bottle.Alkali lye is housed in the absorption bottle, is used for absorption test tail gas, prevent tail gas harm and atmospheric pollution in the process.The concentration determination system comprises at least 3 taper absorption bottles, a small size vacuum aspiration pump, and acid-resisting rubber plug and thickening rubber tube are tightly connected, and join coil condenser before entering the small size vacuum aspiration pump.Distilled water is housed respectively in the absorption bottle, is used to absorb gas attack medium from burner hearth.
Process flow diagram of the present invention such as Fig. 1: launch from the dynamics and thermodynamics two aspects of the high temperature corrosion of phosphorus sulphur, control different corrosive concentration and temperature, the specimen surface product be will corrode then and metallographic and OM, XRD, analyses such as SEM, EDS done, simultaneously in conjunction with above analysis result and corrosive medium composition, launch the high temperature corrosion thermodynamic study, draw phosphorus, sulfur corrosion medium high temperature corrosion thermodynamics and kinetics rule at last boiler material.
Beneficial effect of the present invention: simulate the yellow phosphoric tail gas high temperature corrosion more accurately, and can set different test temperatures and corrosive medium concentration of component as required and study yellow phosphoric tail gas the high temperature corrosion of boiler material is furtherd investigate, help the research that yellow phosphoric tail gas is done the fuel comprehensive utilization.The high temperature corrosion test unit that the present invention relates to is an atmospheric pressure state, and stability in use is good, security performance is high.Test method technology is simpler and clearer, and equipment is easy to get and low cost of manufacture.This test method still is used for the secondary utilization research such as industrial gaseous wastees such as blast furnace gases.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples, but do not limit the present invention with this.
Fig. 1 is a yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion simulation experiment method process flow diagram;
Fig. 2 is that yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion simulation experiment method device is always schemed;
Fig. 3 is that high temperature corrosion test unit profile construction synoptic diagram and A are to view.
.19.N among Fig. 2
2Gas cylinder 20.PH
3Gas cylinder 21.H
2 S gas cylinder 22. suspended body flowmeters 23. gas mixing devices 24. vacuum pumps 25. coil condensers 26. valves 27. small-sized aspiration pump 28. alkali lye absorption bottle 29.NaOH solution 30. concentration detect bottle 31. distilled water.
.1. 5. ceramic pipe pyrometer couple holes, anti-rust metal shell 2. alumina silicate fibre heat-insulation layer 3. mullite flame-proof burner hearths, 4. ceramic pipe tail gas holes, the 6. ceramic pipe corrosive mediums that spray paint advance the automatic temperature-controlled instrument 10. digital display temperature of hole 7. isometrical Elema 8. sample 9.KSY type controllable silicons indication adjusting apparatus 11. A.C. voltmeters 12. alternating current ammeters 13. adjusting pressuring knobs 14. uni-directional push-button switches 15. safeguard protection covers 16. handgrips 17. fire doors 18. bases among Fig. 3.
Embodiment
Embodiment: hot test Unit Installation of the present invention is arranged: corrosive medium gas distributing system I, heating temperature-controlling system II, exhaust treatment system III, four parts of the IV of concentration determination system according to pilot system are installed successively.
Corrosive medium gas distributing system I: be with manometric N
2Gas cylinder 19, PH
3Gas cylinder 20, H
2S gas cylinder 21 connects suspended body flowmeter 22 by pipeline respectively, and flowmeter 22 other ends all insert gas mixing device 23, and etchant gas mixes through gas mixing device 23.
Etchant gas leads to heating temperature-controlling system II after gas mixing device 23 mixes, be that the ceramic pipe corrosive medium enters hole 6 specifically, it is high-temperature ceramic that the ceramic pipe corrosive medium advances hole 6 materials, insert mullite flame-proof burner hearth 3, ceramic pipe and mullite flame-proof burner hearth 3 intersections are added with sealing shroud, guarantee that burner hearth possesses good sealing effectiveness.Hot test device burner hearth body critical piece is that 8 isometrical Elemas 7 of nonmetal heating element evenly vertically are arranged in mullite flame-proof burner hearth 3 central authorities, and runs through mullite flame-proof burner hearth 3 up and down.Series connection (parallel connection also can, look actual use power) mullite flame-proof burner hearth 3 once waters moulding by fire resistive material, can stand the certain high temperature thermal load, can guarantee the good whole sealing again.Device is outer to be the anti-rust metal shell 1 that sprays paint, and has safeguard protection cover 15.Spraying paint, filling thickness is a 150mm alumina silicate fibre heat-insulation layer 2 between anti-rust metal shell 1 and the mullite flame-proof burner hearth 3.Sample 8 is put into rectangle porcelain side ship, evenly is placed on mullite flame-proof burner hearth 3 bottom surface central authorities.Pyrometer couple thermometric end adds ceramic sheath and is entered in the mullite flame-proof burner hearth 3 directly over the sample by ceramic pipe pyrometer couple hole 5.The pyrometer couple cold junction connects compensating wire, with compensating wire by the positive and negative automatic temperature-controlled instrument 9 temperature input ends of KSY type controllable silicon of correctly receiving.Automatic temperature-controlled instrument 9 user interfaces of KSY type controllable silicon comprise digital display temperature indication adjusting apparatus 10, A.C. voltmeter 11, alternating current ammeter 12, adjusting pressuring knob 13, uni-directional push-button switch 14.Pyrometer couple cold junction compensation lead is connected with digital display temperature indication adjusting apparatus 10 on the automatic temperature-controlled instrument 9 of KSY type controllable silicon, reaches temperature and shows and the effect of controlling.Automatic temperature-controlled instrument 9 power inputs of KSY type controllable silicon are connected with big current lead, and terminal dress plug links to each other with power supply.Automatic temperature-controlled instrument 9 power output ends of controllable silicon are drawn lead and are connect isometrical Elema 7 two ends.Energized at first during use transfers to " ON " shelves with uni-directional push-button switch 14, and button on digital display temperature indication adjusting apparatus 10 operation interfaces is transferred to " settings " retaining, and operation knob is set required holding temperature, after temperature is set and finished button is transferred to " measurement " and keeps off.Adjusting pressuring knob 13 on automatic temperature-controlled instrument 9 operation interfaces of KSY type controllable silicon requires to regulate suitable voltage according to the concrete heating rate of test; Digital display temperature indication adjusting apparatus 10 real-time digitals show the temperature in the mullite flame-proof burner hearth 3 in the temperature-rise period; After reaching the setting holding temperature, digital display temperature indication adjusting apparatus 10 auxiliary reclays discharge.Under the effect of auxiliary reclay, the connected sum of control contactor disconnects, and reaches power supply and outage to device, makes test unit can remain on constant temperature work under the temperature of setting.
Be development test temperature and actual corrosive concentration in the test unit burner hearth, and the relation of exhaust emissions speed, the design one cover concentration determination IV of system.From the coil condenser 25 termination road on one side of giving vent to anger, be connected to small-sized aspiration pump 27 end of bleeding, by the stereometry (volume=flow * time) of flowmeter 22 control extraction flows and the absorption of the IV of concentration determination system tail gas.Small-sized aspiration pump 27 outlet sides are received 3 concentration that are linked in sequence and are detected bottle 30, in the bottle distilled water 31 are housed.
Yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion simulation test method of operating of the present invention:
To treat before the test that pilot boiler is processed into standard sample with steel raw material 20g, 20G, 16MnR with reference to national standard " the antioxygenic property method of testing of steel " etc., 6 groups of every kind of materials, every group of 3 parallel samples.Polishing rust-removal is carried out on the surface handle, put into oven drying.Rectangle porcelain side ship is cleaned, and puts into more than the baking oven 30min, weighs more than three times, until empty porcelain side ship mass conservation.Sample is put into porcelain side's ship, weigh, number.With above boiler plate raw material according to national standard " GB/T 232-1999 metal material bend test method ", " the GB-T 229-1994 metal summer is than test with notched test piece method ", " GB/T 228-2002 metal material tensile test at room temperature method " processing equipment performance sample, 6 groups of every kind of materials, every group of 3 parallel samples.
Call through test device power supply, uni-directional push-button switch 14 is transferred to " ON " shelves, button on digital display temperature indication adjusting apparatus 10 operation interfaces is transferred to " setting " retaining, operation knob, set (1200 ℃, 1000 ℃, 900 ℃, 800 ℃, 750 ℃, 700 ℃, 650 ℃, 600 ℃, 550 ℃ of required holding temperatures, 500 ℃), after temperature is set and finished button is transferred to " measurement " and keep off.Adjusting pressuring knob 13 on automatic temperature-controlled instrument 9 operation interfaces of KSY type controllable silicon, regulation voltage is to 220V; Digital display temperature indication adjusting apparatus 10 real-time digitals show the temperature in the mullite flame-proof burner hearth 3 in the temperature-rise period; After reaching the setting holding temperature, digital display temperature indication adjusting apparatus 10 auxiliary reclays discharge.Under the effect of auxiliary reclay, the connected sum of control contactor disconnects, reach power supply and outage, make test unit can remain on temperature (1200 ℃, 1000 ℃, 900 ℃, 800 ℃, 750 ℃, 700 ℃, 650 ℃, 600 ℃, 550 ℃, 500 ℃) the constant temperature work of setting device.
Reach and set porcelain side's ship that sample will be housed after the test temperature and put into burner hearth.Close ceramic pipe tail gas hole 4, open N
2Gas cylinder 19 valves are regulated flow to 15L/min, inflated with nitrogen in mullite flame-proof burner hearth 3.Guarantee to be full of nitrogen in the mullite flame-proof burner hearth 3, close N
2Gas cylinder 19 valves start vacuum pump 24, burner hearth are vacuumized three times repeatedly.Feed hybrid corrosion dielectric gas (H
2S+PH
3): volume 1:1, concentration content is respectively 4000mg/Nm
3, 3000mg/Nm
3, 2000mg/Nm
3, 1000mg/Nm
3, 500mg/Nm
3, 100mg/Nm
3
Test period is 48h, and the routine weighing time is 0h, 8h, 16h, 24h, 32h, 40h, 48h, 56h, 62h, 72h.Arrival is weighed the time, closes PH earlier
3Gas cylinder 20, H
2S gas cylinder 21 valves and gas mixing device 23.Open N
2Gas cylinder 19, inflated with nitrogen in burner hearth is removed residue etchant gas in the burner hearth.Close N
2Gas cylinder 19, the side's of taking-up ship is put into drying basin immediately and is cooled to room temperature, in precision is to weigh on 1/10000 the electronic balance.Weigh finish after, open N successively
2 Gas cylinder 19, vacuum pump 24, inflated with nitrogen vacuumizes.Continue test,, repeat above step until the next time point of weighing.Behind the 48h, close PH
3Gas cylinder 20, H
2S gas cylinder 21 valves and gas mixing device 23 are opened N
2Gas cylinder 19, inflated with nitrogen is removed in the burner hearth and is remained etchant gas in burner hearth.The stopping device power supply takes out the last batch of sample.Get blank sample and 3 samples that uniform corrosion is separated by wherein, make metallographic examination, XRD, SEM and EDS and analyze; The mechanical property sample is done bending test, impulse test, tension test.
Claims (6)
1, a kind of yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion test system device comprises corrosive medium gas distributing system (I), heating temperature-controlling system (II), exhaust treatment system (III), concentration determination system (IV).
2,, it is characterized in that described corrosive medium gas distributing system (I) comprises 3 gas cylinders, N at least according to the described device of claim 1
2Gas cylinder (19), PH
3Gas cylinder (20), H
2S gas cylinder (21), insert suspended body flowmeter (22) by pipeline respectively, flowmeter (22) other end all inserts gas mixing device (23), the gas mixing device endpiece is connected with the high-temperature corrosion device burner hearth (3) of heating in the temperature-controlling system, etchant gas mixes through gas mixing device (23), and the burner hearth outlet side is furnished with vacuum pump (25).
3, according to the described device of claim 1; it is characterized in that described heating temperature-controlling system (II) comprises heating part and automatic temperature-adjusting control section; the critical piece of heating part has high temperature silicon carbon-point (7); run through one-shot forming mullite burner hearth (3) up and down; be fixed on alumina silicate fibre insulation material outside; sample evenly is placed on burner hearth central authorities; the device skin is anti-rust metal shell (1); have safeguard protection cover (15); Elema is in series, and the two ends lead-in wire links to each other with controllable silicon automatic temperature-adjusting controller electric furnace binding post.
4, according to the described device of claim 1, it is characterized in that described exhaust treatment system (III) comprises that at least 3 taper absorption bottles (28) connect successively, the alkali lye that is used for absorption test tail gas is housed in the absorption bottle, before absorption bottle, is furnished with vacuum pump (24) and coil condenser (25).
5, according to the described device of claim 1, it is characterized in that described concentration determination system (IV) comprises at least 3 taper absorption bottles (30), a small size vacuum aspiration pump (27), acid-resisting rubber plug and thickening rubber tube are tightly connected, and before entering the small size vacuum aspiration pump, join coil condenser (25), the distilled water that is used to absorb from the gas attack medium of burner hearth is housed respectively in the absorption bottle.
6, a kind of yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion test method, it is characterized in that to treat that pilot boiler is processed into standard sample with steel raw material 20g, 20G, 16MnR before the test, 6 groups of every kind of materials, every group of 3 parallel samples, polishing rust-removal is carried out on the surface to be handled, put into oven drying, rectangle porcelain side ship is cleaned, and puts into more than the baking oven 30min, weighs more than three times, until empty porcelain side ship mass conservation, sample is put into porcelain side's ship, weigh, number, above boiler plate raw material is processed into the mechanical property sample, 6 groups of every kind of materials, every group of 3 parallel samples; Call through test device power supply, uni-directional push-button switch 14 is transferred to " ON " shelves, button on digital display temperature indication adjusting apparatus 10 operation interfaces is transferred to " setting " retaining, operation knob, set 1200 ℃ of required holding temperatures, 1000 ℃, 900 ℃, 800 ℃, 750 ℃, 700 ℃, 650 ℃, 600 ℃, 550 ℃, 500 ℃, after temperature is set and finished button is transferred to " measurement " and keep off; Adjusting pressuring knob 13 on automatic temperature-controlled instrument 9 operation interfaces of KSY type controllable silicon, regulation voltage is to 220V; Digital display temperature indication adjusting apparatus 10 real-time digitals show the temperature in the mullite flame-proof burner hearth 3 in the temperature-rise period; After reaching the setting holding temperature, digital display temperature indication adjusting apparatus 10 auxiliary reclays discharge; Under the effect of auxiliary reclay, the connected sum of control contactor disconnects, and reaches power supply and outage to device, makes test unit can remain on 800 ℃, 750 ℃, 700 ℃, 650 ℃, 600 ℃, 550 ℃ of the temperature of setting, 500 ℃ of constant temperature work; Reach and set porcelain side's ship that sample will be housed after the test temperature and put into burner hearth, close ceramic pipe tail gas hole 4, open N
2Gas cylinder 19 valves are regulated flow to 15L/min, and inflated with nitrogen in mullite flame-proof burner hearth 3 is guaranteed to be full of nitrogen in the mullite flame-proof burner hearth 3, closes N
2Gas cylinder 19 valves start vacuum pump 24, burner hearth are vacuumized three times repeatedly; Feed hybrid corrosion dielectric gas (H
2S+PH
3): volume 1:1, concentration content is respectively 4000mg/Nm
3, 3000mg/Nm
3, 2000mg/Nm
3, 1000mg/Nm
3, 500mg/Nm
3, 100mg/Nm
3Test period is 72h, and the routine weighing time is 0h, 8h, 16h, 24h, 32h, 40h, 48h, 56h, 62h, 72h; Arrival is weighed the time, closes PH earlier
3Gas cylinder 20, H
2S gas cylinder 21 valves and gas mixing device 23 are opened N
2Gas cylinder 19, inflated with nitrogen in burner hearth is removed residue etchant gas in the burner hearth; Close N
2Gas cylinder 19, the side's of taking-up ship is put into drying basin immediately and is cooled to room temperature, in precision is to weigh on 1/10000 the electronic balance; Weigh finish after, open N successively
2Gas cylinder 19, vacuum pump 24, inflated with nitrogen vacuumizes; Continue test,, repeat above step until the next time point of weighing,, behind the 72h, close PH
3Gas cylinder 20, H
2S gas cylinder 21 valves and gas mixing device 23 are opened N
2Gas cylinder 19, inflated with nitrogen is removed in the burner hearth and is remained etchant gas in burner hearth; The stopping device power supply takes out the last batch of sample; Get blank sample and 3 samples that uniform corrosion is separated by wherein, make metallographic examination, XRD, SEM and EDS and analyze; The mechanical property sample is done bending test, impulse test, tension test.
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