CN101929945B - Low-temperature dew point corrosion experiment method for phosphorus in yellow phosphorus tail gas on boiler material and device thereof - Google Patents
Low-temperature dew point corrosion experiment method for phosphorus in yellow phosphorus tail gas on boiler material and device thereof Download PDFInfo
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Abstract
The invention relates to a low-temperature dew point corrosion experiment method for phosphorus in yellow phosphorus tail gas on a boiler material, and a device thereof, in particular to a yellow phosphorus tail gas phosphorus component low-temperature dew point corrosion experiment method and a device for implementing the method. A yellow phosphorus tail gas phosphorus component low-temperature dew point corrosion experiment system is contained, and consists of a heating temperature control system, a condensation reflux system and a tail gas treatment system. The experiment heating temperature control device adopts an air heating jacket, and has good temperature control capacity and quick, even and stable heating; and a tail gas absorbing device is arranged, so pollution is free in the experiment. The method and the device can perform dew point corrosion study on acids, can better simulate the low-temperature dew point corrosion of impurities such as the phosphorus on the boiler material in the yellow phosphorus tail gas comprehensive utilization, and also can be used for comprehensive utilization study on other industrial waste gases (tail gases).
Description
Technical field
The present invention relates to a kind of low-temperature dew point corrosion experiment method, especially a kind of low-temperature dew point corrosion simulation experiment method of yellow phosphoric tail gas phosphorus component.
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, (CO 85%～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 of Yunnan Province's promulgation in 2010: yellow phosphorus enterprise must build comprehensive utilization of resources facilities such as yellow phosphoric tail gas, slag, and the fire extinguishing torch, and phosphorus production enterprise is faced with the challenge of existence.
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 almost scrapped, 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 superheating surface appearance corrosion and fouling in 3-4 month boiler, and heat exchange efficiency is not high and need frequently change parts or the like.
Find that through the corrosion experiment in early stage gas-side corrosion is bigger for the boiler influence.Its reason is to use untreated yellow phosphoric tail gas, and yellow phosphoric tail gas also contains many harmful and high materials that corrode except that being rich in CO, mainly contain impurity such as phosphorus, sulphur, arsenic, fluorine, and wherein arsenic and fluorine can be easier to remove by washing and alkali cleaning.Phosphorus is mainly with PH
3And P
4Form exists, and content is respectively PH
3400～900mg/Nm
3, P
4300～700mg/Nm
3Sulphur is mainly with H
2S, COS, CS
2Exist etc. form, content is respectively 800～3000mg/Nm
3, 20～2000mg/Nm
3, 1～50mg/Nm
3Because phosphorus, sulphur in the yellow phosphoric tail gas are difficult to efficient purification, PH
3, P
4And H
2S burning back generates P
2O
5And SO
2, in the system of opening wide, meet H
2Formed extremely strong phosphoric acid and the sulfuric acid of corrosivity behind the O, serious low-temperature dew point corrosion takes place when the lower temperature of boiler operatiopn easily, especially the corrosion to superheater tube and drum is bigger, flue gas abrasive action in addition, cause the tube wall attenuate serious, even perforation, boiler life reduces.
Therefore, China's yellow phosphoric tail gas is failed well as the boiler fuel recycling because it corrodes 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
The purpose of this invention is to provide yellow phosphoric tail gas phosphorus component low-temperature dew point corrosion simulation experiment method: i.e. the dewpoint temperature calculation of thermodynamics of chamber simulation yellow phosphoric tail gas by experiment, the dewpoint temperature when the phosphorus component dewfall that obtains different content becomes phosphoric acid and the concentration of dewfall acid.The dewfall acid (phosphoric acid) of preparing this kind concentration is an amount of, gets some kind boiler materials and makes in the environment that standard specimen is soaked in different corrosive mediums (phosphoric acid) concentration gradient 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.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 SEM, EDS, analyses such as XRD, XPS done, in conjunction with above analysis result and corrosive medium composition, the sample before and after the test is done measuring mechanical property simultaneously.Launch the cold end corrosion thermodynamic study, draw the dew point corrosion thermodynamics and kinetics rule of objectionable impurities phosphorus at last boiler material.
Another object of the present invention provides yellow phosphoric tail gas phosphorus component low-temperature dew point corrosion simulation experiment system: it is made up of heating temperature-controlling system, condensing reflux system, exhaust treatment system three parts, sees shown in Figure 1.Heating temperature-controlling system (I) selects 500ml digital display temperature control electrical heating cover (6) to be contained on the iron stand (1) of band iron clamp (2), five mouthfuls of flasks of self-control 500ml (4) that will fill corrosive liquid (7) are put into the electrical heating cover, the temperature-sensing probe (8) of electrical heating cover inserts the corrosive liquid from a bite of five mouthfuls of flasks (4), and temperature-sensing probe (8) is connected with flask by plug.Condensing reflux system (II) uses iron clamp (2 fixing snakelike condensing reflux pipes of 500mm (3), condenser pipe is connected with five mouthfuls of flasks by plug, chilled water feeds from the lower end water inlet of condenser pipe (3), discharge from the water delivering orifice of upper end, its excess-three mouth of five mouthfuls of flasks is respectively applied for and holds three parallel samples (5), sample (5) hangs and is immersed in fully in the corrosive liquid (7) with teflon line-transect (13), and polytetrafluoroethylene wire is connected with flask by plug.Exhaust treatment system (III) links to each other by conduit (10) coil condenser (3) outlet side with continuous 3 alkali lye absorption bottles (11), conduit and absorption bottle are tightly connected by plug.Test method and flow process: see that Fig. 2 is described.
Beneficial effect of the present invention: phosphorus is to solve in the yellow phosphoric tail gas comprehensive utilization to the low-temperature dew point corrosion experiment method of boiler material and device thereof in the yellow phosphoric tail gas, to a kind of operable approach and the device of the difficult problem of boiler material cold end corrosion harm.This method and device have been avoided factors such as on-the-spot tail gas amount instability, temperature and tail gas composition be restive, and it is controlled to have tail gas amount in the simulation test, dewpoint temperature, concentration, advantage such as the test period is flexible.
The present invention simulates the low-temperature dew point corrosion of yellow phosphoric tail gas phosphorus component more accurately, and can set different test temperatures and corrosive medium concentration of component as required and study yellow phosphoric tail gas the dew point corrosion of boiler material is furtherd investigate, help the research that yellow phosphoric tail gas is done the fuel comprehensive utilization.The dew point corrosion test device 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 also is applicable to the secondary utilization research such as the various industrial gaseous wastees that contain sour corrosion gas.
Description of drawings
Fig. 1 is the synoptic diagram of apparatus of the present invention.
Fig. 2 is a method flow diagram of the present invention.
Among the figure: the 1-iron stand; The 2-iron clamp; The 3-serpentine condenser; Five mouthfuls of flasks of 4-500ml; The 5-sample; 6-500ml electrical heating cover; 7-reagent (phosphoric acid solution); 8-temperature-sensing probe (coating the anticorrosive PTFE cover); 9-digital display temperature control instrument; The 10-wireway; The 11-250ml conical flask; 12-.NaOH solution; 13-teflon line-transect.
Embodiment
Further specify flesh and blood of the present invention with example below, but content of the present invention is not limited to this.
Yellow phosphoric tail gas phosphorus component low-temperature dew point corrosion simulation test method of operating of the present invention:
(1) will treat that pilot boiler is processed into standard sample with steel raw material with reference to national standard 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 handle, put into oven drying.Sample is weighed, numbered.With above boiler plate raw material according to national standard processing equipment performance sample, 6 groups of every kind of materials, every group of 3 parallel samples.Prepare the phosphoric acid of the variable concentrations of corresponding various dewpoint temperatures, choose in the five mouthfuls of flasks of experiment to be heated of packing in right amount at every turn.
(2) call through test device power supply is set required holding temperature (dewpoint temperature of calculating), simultaneously begins to import chilled water in the condenser pipe, avoids reagent concentration to change, and reaches sample to be put into flask after setting test temperature.Test period is 8h, and the routine weighing time is 0h, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h.Arrival is weighed the time, takes out sample rapidly from flask, and hair-dryer is dry also to be cooled to room temperature, in precision is to weigh on 1/10000 the electronic balance.
(3) weigh finish after, continue test, until the next time point of weighing, repeat above step.Behind the 8h, the stopping device power supply takes out the last batch of sample.
(4) 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.
Yellow phosphoric tail gas phosphorus sulfur multi-component high temperature corrosion simulation test device comprises: heating temperature-controlling system, condensing reflux system, exhaust treatment system three part groups.See shown in Figure 1, heating temperature-controlling system (I): select 500ml digital display temperature control electrical heating cover (6) for use, the temperature control scope: room temperature～400 ℃, its temperature-sensing probe (8) is outer to coat homemade anticorrosive PTFE cover, the high-temperature acid corrosion can either be avoided, experimental temperature can be accurately controlled again.Condensing reflux system (II): the snakelike condensing reflux pipe (3) of selecting general mouthful of 500mm, make 5 mouthfuls of 500ml flasks (4) by oneself, condenser pipe is connected with flask by plug, chilled water feeds from the lower end water inlet of condenser pipe (3), discharge from the water delivering orifice of upper end, guarantee the heating of flask internal cause and the abundant condensing reflux of vaporized reagents steam, make the concentration maintenance substantially constant of reagent.Temperature-sensing probe (8) inserts the reagent from another mouthful of five mouthfuls of flasks (4), and temperature-sensing probe (8) is connected with flask by plug.Its excess-three mouth of five mouthfuls of flasks is respectively applied for and holds three parallel samples (5), and sample (5) hangs and is immersed in fully in the reagent (7) with the teflon line-transect, and polytetrafluoroethylene wire is connected with flask by plug.Exhaust treatment system: the test tail gas of discharging from coil condenser (3) outlet side enters continuous 3 alkali lye absorption bottles (11), and the tail gas of feeding all is absorbed.Contain the NaOH alkali lye of concentration 5% in preceding two alkali lye absorption bottles, contain the NaOH alkali lye of concentration 10% in last alkali lye absorption bottle, promptly require tail gas in the alkali lye absorption bottle, to be in unsaturated state, be beneficial to abundant absorption tail gas.
Embodiment 1 selects conventional utility boiler material 20g for use, 304, adopt said method, experiment phosphoric acid concentration 30%, 60%, 85%, 40 ℃ of experimental temperatures, 80 ℃, the anti-dew point corrosion performance of two kinds of materials of 120 ℃ of checks, show that by the corrosion kinetics CURVE STUDY material 304 compares with 20g and have suitable corrosion stability, the corrosion of material aggravates with the increase of temperature and concentration, but temperature is more more obvious than the influence of phosphoric acid concentration to the influence of material corrosion, the chemical composition of surface corrosion morphology analysis illustrative material self is very big to the extent of corrosion influence, 304 corrosion stabilitys than 20g are well owing to contain Cr and two kinds of corrosion-resistant materials of Ni in 304 materials, they the time exist and to have improved 304 stainless tolerate P-levels acid dew piont corrosion performances greatly, provide foundation to the construction material selection of high temperature phosphoric acid industry.
Embodiment 2 these experimental techniques also are applicable to the research of material corrosion resistance to sulfuric acid dew point, corrosion resistance to sulfuric acid dew point for check S TEN3 steel and CRIA steel, adopt this method, experiment sulfuric acid concentration 30%, 60%, 85%, 60 ℃, 80 ℃, 110 ℃ of experimental temperatures show S-TEN by the corrosion kinetics CURVE STUDY
3Steel and CRIA steel have better corrosion resistance to sulfuric acid dew point. and higher 4～12 times than plain carbon steel, S-TEN wherein
3More superior, its corrosion mechanism be the analysis showed that on the basis of chromium-copper steel add an amount of alloying element Sb or Ti is useful to the corrosion resistance to sulfuric acid dew point that improves S-TEN3 and CRIA respectively.
Claims (4)
1. phosphorus is characterized in that comprising to the low-temperature dew point corrosion experiment method of boiler material in the yellow phosphoric tail gas:
(1) the dewpoint temperature calculation of thermodynamics of chamber simulation yellow phosphoric tail gas by experiment, the dewpoint temperature when the phosphorus component dewfall that obtains different content becomes phosphoric acid and the concentration of dewfall acid; The dewfall acid of preparing this kind concentration is phosphoric acid, gets some kind boiler materials and makes in the environment that standard specimen is soaked in different corrosive medium concentration of phosphoric acid gradients and thermograde;
(2) mass change of periodic logging corrosion sample in the process of the test is observed surface topography, and sampling is regularly preserved;
(3) by metallographic examination, XRD, SEM and EDS analysis means, 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;
(4) research of making gas fired-boiler fuel for yellow phosphoric tail gas provides accurate and reliable laboratory data and theory;
The concrete steps of described test method are as follows:
(1) will treat that pilot boiler is processed into standard sample with steel raw material with reference to national standard 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, sample is weighed, numbered, with above boiler plate raw material according to national standard processing equipment performance sample, 6 groups of every kind of materials, every group of 3 parallel samples are prepared the phosphoric acid of the variable concentrations of corresponding various dewpoint temperatures, choose in the five mouthfuls of flasks of experiment to be heated of packing in right amount at every turn;
(2) connect in the yellow phosphoric tail gas phosphorus to the low-temperature dew point corrosion test unit power supply of boiler material, set the dewpoint temperature of required calculating, begin to import chilled water in the condenser pipe simultaneously, avoid reagent concentration to change, after reaching the setting test temperature sample is put into flask, test period is 8h, the routine weighing time is 0h, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, arrival is weighed the time, from flask, take out sample rapidly, hair-dryer is dry also to be cooled to room temperature, in precision is to weigh on 1/10000 the electronic balance;
(3) weigh finish after, continue test, until the next time point of weighing, repeat above step, behind the 8h, the stopping device power supply takes out the last batch of sample;
(4) get emptyly, do metallographic examination, XRD, SEM and EDS analysis from sample and 3 samples that uniform corrosion is separated by wherein; The mechanical property sample is done bending test, impulse test, tension test;
Phosphorus comprises the low-temperature dew point corrosion test unit of boiler material in the described yellow phosphoric tail gas: heating temperature-controlling system, condensing reflux system, exhaust treatment system three parts, described heating temperature-controlling system (I) comprising: digital display temperature control electrical heating cover (6), the outer anticorrosive PTFE cover that coats of its temperature-sensing probe (8); Described condensing reflux system (II) comprising: condenser pipe (3), five mouthfuls of flasks (4), condenser pipe is connected with five mouthfuls of flasks by plug, chilled water feeds from the lower end water inlet of condenser pipe (3), discharge from the water delivering orifice of upper end, temperature-sensing probe (8) inserts the reagent from another mouthful of five mouthfuls of flasks (4), temperature-sensing probe (8) is connected with five mouthfuls of flasks by plug, its excess-three mouth of five mouthfuls of flasks is respectively applied for and holds three parallel samples (5), parallel sample (5) hangs and is immersed in fully in the reagent (7) with the teflon line-transect, and the teflon line-transect is connected with flask by plug.
2. according to phosphorus in the described yellow phosphoric tail gas of claim 1 low-temperature dew point corrosion experiment method of boiler material be is characterized in that: described digital display temperature control electrical heating cover is a 500ml digital display temperature control electrical heating cover, the temperature control scope: room temperature～400 ℃.
3. according to phosphorus in the described yellow phosphoric tail gas of claim 1 low-temperature dew point corrosion experiment method of boiler material be is characterized in that: described condenser pipe is the snakelike condensing reflux pipe of general mouthful of 500mm; Described five mouthfuls of flasks are the flask of 5 mouthfuls of 500ml of self-control.
According to phosphorus in the described yellow phosphoric tail gas of claim 1 to the low-temperature dew point corrosion experiment method of boiler material, it is characterized in that: described exhaust treatment system is: the test tail gas of discharging from condenser pipe (3) outlet side enters continuous 3 alkali lye absorption bottles (11), and the tail gas of feeding all is absorbed; Contain the NaOH alkali lye of concentration 5% in preceding two alkali lye absorption bottles, contain the NaOH alkali lye of concentration 10% in last alkali lye absorption bottle, tail gas is in unsaturated state in the alkali lye absorption bottle.
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| CN102680350B (en) * | 2012-06-01 | 2014-03-19 | 南京大学 | Scale inhibitor performance evaluation method suitable for circulating cooling water systems |
| CN102692438B (en) * | 2012-06-15 | 2014-03-26 | 哈尔滨工程大学 | Dew point corrosion experiment device capable of realizing electrochemical tests |
| CN105277482B (en) * | 2014-07-07 | 2018-07-06 | 中石化洛阳工程有限公司 | A kind of distilling apparatus overhead system dew point corrosion test method |
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| CN114486709A (en) * | 2022-03-15 | 2022-05-13 | 中国核动力研究设计院 | Three-phase corrosion test device and test method |
| CN117387363B (en) * | 2023-12-06 | 2024-02-06 | 东营广大金科机器人有限公司 | Dew point inspection assembly of roller-hearth type natural gas heating furnace and use method |
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| CN201212875Y (en) * | 2008-06-05 | 2009-03-25 | 昆明理工大学 | Yellow phosphoric tail gas high temperature corrosion simulating test device |
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