CN1546609A - Suppressing and slowing method of coking in ethylene cracking furnace tube - Google Patents
Suppressing and slowing method of coking in ethylene cracking furnace tube Download PDFInfo
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- CN1546609A CN1546609A CNA200310110224XA CN200310110224A CN1546609A CN 1546609 A CN1546609 A CN 1546609A CN A200310110224X A CNA200310110224X A CN A200310110224XA CN 200310110224 A CN200310110224 A CN 200310110224A CN 1546609 A CN1546609 A CN 1546609A
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Abstract
The invention discloses a method for suppressing and slowing coking in ethylene cracking furnace tube comprising the steps of, (1) atmosphere processing, using the gaseous mixture produced from liquid ammonia decomposition as reducing gas to process the boiler tube atmosphere, (2) alloying treatment, preparing the alloy powder and adhesive into pulp, coating onto the surface of the processed furnace tube, drying and solidifying at 50-120 deg. C, placing into heating-furnace for diffusion treatment, cooling the furnace tube after the completion of the treatment, and removing the alloy powder coating on the furnace tube surface.
Description
Technical field
The present invention relates to a kind of surface and carry out the method that anti-coking is handled, suppress and slow down generation and the deposition of coke on the boiler tube inwall in the hydrocarbon cracking process Ethylene Cracking Furnace Tubes.More particularly, the present invention relates to a kind of atmosphere and alloying combination treatment form alloy layer on the boiler tube surface method, reduce catalytic coking, thereby reduce generation and the deposition of coke at the boiler tube inwall, reduce the carburizing trend of boiler tube, prolong the coke cleaning period and the work-ing life of boiler tube.
Background technology
Ethene is the basic material of synthesising fibre, plastics, rubber, and 95% ethene is from the cracking of hydro carbons in the world.The raw material of hydrocarbon cracking system ethene is divided into hydrocarbon gas (ethane, propane, associated gas, refinery gas etc.) and liquid hydrocarbon (petroleum naphtha, gasoline, kerosene, diesel oil, heavy oil etc.).In the cracking process of hydro carbons, when generating alkene, also generate coke, it is favourable for raising yield of ethene, inhibition coking to reduce hydrocarbon partial pressure, and the industrial water vapour that uses reduces hydrocarbon partial pressure as thinner.Different cracking stocks, the consumption of water vapour are also different.In pyrolyzer, cracking stock enters into radiation section through the convection zone preheating, and multiple reactions such as, polymerization crosslinked in radiation section generation chain rupture, dehydrogenation, aromizing, condensation, dehydrogenation, isomerization generate alkene, aromatic hydrocarbons, bituminous matter, carbene and coke.Sedimentation of coke brings a lot of harms on the boiler tube surface, because the thermal conductivity ratio steel alloy of burnt layer is much lower, there is the local local thermal resistance of burnt layer big, make the radial symmetry gradient of boiler tube become big, cause the furnace tube outer wall temperature to raise, influence the life-span of boiler tube, and do not reach the cracking temperature of requirement in the boiler tube; Because coking increases fluid flow resistance, increase falls in boiler tube pressure, and material pressure increases, and is unfavorable to cracking; Because coking causes boiler tube carburizing trend to increase, and reduced the intensity of boiler tube, so the boiler tube of pyrolyzer need regularly carry out coke cleaning.Coke cleaning method commonly used is that water vapour-air burns method, makes coke burn into carbonic acid gas and removes, and whole process need two to three days will consume a large amount of heat energy, and shorten the production time.
In the hydrocarbon cracking process, the coking of cracking furnace pipe inwall has three processes: the one, and the free radical reaction of hydrocarbon cracking generates aromatic hydrocarbons, and the aromatic hydrocarbons condensation forms coke, is deposited on the boiler tube surface; The 2nd, hydrocarbon cracking generates alkynes, and the carbon granules that the alkynes dehydrogenation generates is deposited on the boiler tube surface; The 3rd, the catalytic coking of the metallic iron on boiler tube surface, nickel and oxide compound thereof.Preceding two kinds of cokings can be by improving processing condition and the agent of adding technology anti-coking reduces, and a kind of coking in back has only the surface composition by changing boiler tube to reduce coking.Existing Ethylene Cracking Furnace Tubes, the technology of inhibition and slow down coking mainly contains four classes:
The first kind is an online treatment, behind the boiler tube coke cleaning, adopts organic sulfide, basic metal, alkaline-earth metal, trialkylphosphine oxide and stain control agent etc. that boiler tube is handled, online film forming or formation inorganic coating, suppress coking and carbon distribution, all will handle again behind each coke cleaning, operation sequence is many.Patent CN1345261A, CN1236827A, CN1155572A, CN1140197A, CN85101540A and US6228253 belong to this type of.
Second class is that atmosphere is handled, and mainly is that new boiler tube is carried out surface treatment, and the iron, the nickel content that reduce the boiler tube surface suppress catalytic coking, and coke generates and deposition thereby reduce.Patent US5630887, US6436202 belong to this type of, and its atmosphere of using is reducing atmosphere, main hydrogen, carbon monoxide and rare gas element, and gas passes through frozen water during processing.This method is thinner at the alloy layer that the boiler tube surface forms, and generally has only several microns, and maximum tens microns, the boiler tube life-span is shorter.
The 3rd class is to form inorganic coating on the boiler tube surface, with K
2O, SiO
2, Al
2O
3, ZnO, MgO, Co
3O
4, Na
2O, ZrO
2Be coated onto on the boiler tube Deng inorganics, carry out sintering, form glass coating or ceramic coating, isolated hydro carbons and metallic contact reduce iron, nickel catalytic coking, and coke generates and deposition thereby reduce, and patent US6423415 belongs to this type of.The shortcoming of this technology is that the coefficient of expansion of inorganic coating and boiler tube matrix differs bigger, and after the temperature of process production, coke cleaning changed repeatedly, the life-span of coating can be affected.
The 4th class is to form metal alloy layer on the boiler tube surface, adopt methods such as chemical Vapor deposition process, physical vaporous deposition, hot sputter, plasma spraying, hot melt plating, plating, at boiler tube surface deposition one deck alloy, carry out heat diffusion treatment, form alloy layer, the alloy layer kind mainly contains Cr-Al-Re, Cr-Al-Ti-Si, Cr-Al-Si-Mn etc., reduces iron, nickel catalytic coking, thereby the minimizing sedimentation of coke, patent US6537388 belongs to this type of.Patent US6537388 mainly is by methods such as chemical Vapor deposition process, physical vaporous deposition, hot sputters, earlier at alloy substrate surface deposition one deck Chromium coating, the coating that contains aluminium, silicon again at coatingsurface deposition one deck, carry out DIFFUSION TREATMENT then, after this alloy layer industry is on probation, coke cleaning period is 45～60 days, and the continuous production time lengthening is few.
Summary of the invention
The present invention is directed to the defective that prior art exists, invented a kind of method that suppresses and slow down the ethylene cracking tube coking, using the present invention handles the boiler tube surface, change the surface composition of boiler tube, can suppress and slow down catalytic coking, reduce the carburizing trend of boiler tube simultaneously, prolong the work-ing life of boiler tube.
The present invention decomposes liquefied ammonia, make reducing gas, with reducing atmosphere boiler tube is handled, reduced iron, the nickel content on boiler tube surface, the alloy powder slip that will contain elements such as aluminium, silicon, chromium, rare earth again is coated onto the boiler tube surface, cryodrying is solidified, carry out High temperature diffusion then and handle, form a kind of new alloy layer on the boiler tube surface, this alloy layer can reduce the coking rate of boiler tube, reduce carburizing trend, improve the work-ing life of boiler tube.
Particularly, the present invention is a kind of method that suppresses and slow down the ethylene cracking tube coking, comprises the steps:
1) atmosphere is handled: the H that contains that decomposes the back generation with liquefied ammonia
2, N
2And micro-NH
3, H
2O, O
2Gas mixture be reducing gas, boiler tube is carried out atmosphere to be handled, treating processes is: begin per minute from room temperature and heat up 5 ℃～10 ℃, insulation is 20 minutes～3 hours during to 800 ℃, per minute heats up 3 ℃～5 ℃ to t ℃ subsequently, t ℃ of following constant temperature 15 hours～80 hours, 850 ℃≤t≤1250 ℃, processing finished back furnace cooling boiler tube.
2) Alloying Treatment: alloy powder for preparing and binding agent furnishing slurries, be coated onto the boiler tube surface after atmosphere is handled,, be put into then and carry out DIFFUSION TREATMENT in the process furnace 50 ℃～120 ℃ following baking and curing.Treating processes is: begin per minute from room temperature and heat up 5 ℃～10 ℃, insulation is 0.5 hour～3 hours during to 400 ℃, per minute heats up 5 ℃～8 ℃ to 850 ℃ subsequently, 850 ℃ are incubated 1～3 hour, and per minute heats up 3 ℃～6 ℃ to T ℃ subsequently, 900 ℃≤T≤1200 ℃, T ℃ of following constant temperature 3～7 hours, processing finishes the postcooling boiler tube, removes the unnecessary alloy powder coating in boiler tube surface, can suppress alloy layer with slow down coking in boiler tube surface formation.Described alloy powder is made up of for dispersion agent the aluminium of content 5%～30%, 1%～10% silicon, 5%～20% chromium, 0.5%～5% rare earth, 0.5%～3% catalyzer and all the other.Catalyzer is ammonium chloride, Sodium Fluoride, sodium aluminum fluoride etc., and dispersion agent is aluminium sesquioxide, clay powder, silicon-dioxide etc.Binding agent is formed as edible Gelatinum oxhide, polyvinyl alcohol etc. and water allotment by natural adhesive and synthetic adhesive, and the content of dried binding agent is 3%～15%, and all the other are water.Above-mentioned percentage composition is weight percentage, and used dispersion agent of the present invention and binding agent are this area product commonly used, and the present invention selects not add restriction to it.
Its chromium content of the manageable boiler tube of the present invention can be from 18 weight % to 40 weight %, and nickel content can be from 9 weight % to 50 weight %.
The present invention compares with conventional online coating treatment technology, and the present invention is the primary treatment life-time service, does not increase operation sequence.Compare with existing atmosphere treatment technology, with the boiler tube that the present invention handles, its alloy layer thickness reaches more than 100 microns, and the life-span is longer.Compare with existing glass ceramic coating treatment technology, with the boiler tube that the present invention handles, the coefficient of expansion of alloy layer and boiler tube matrix is about the same, and the life-span of alloy layer is not acted upon by temperature changes.Be laminated with a layer treatment technology with the metal of patent US6537388 and compare, the present invention suppresses and to slow down the effect of tube coking better, and coking test in laboratory shows that it is 50～90% that the boiler tube that present technique is handled suppresses coking rate.
Embodiment
Embodiment 1
The processing of HK alloy furnace tubes by adopting: the first step, one section HK alloy furnace tubes by adopting is made test specimen, before the test that its surface-conditioning is clean, with its surperficial composition of scanning electron microscope analysis, test specimen is put in the atmosphere processing vessel, feed liquefied ammonia in the container and decompose the gas mixture that the back produces, boiler tube is carried out atmosphere to be handled, treating processes is: begin per minute from room temperature and heat up 5 ℃, insulation is 0.5 hour during to 800 ℃, per minute heats up 3 ℃ to 1150 ℃ subsequently, about 30 hours of 1150 ℃ of following constant temperature, uses its surface composition of scanning electron microscope analysis after the off-test again.
Second step, to consist of: aluminium 20%, chromium 15%, silicon 7%, rare earth ferrosilicon alloy 3%, ammonium chloride 1.5% and all the other are the alloy powder of aluminium sesquioxide and the edible Gelatinum oxhide aqueous solution for preparing in advance, be deployed into the slurry of proper viscosity, slurry is coated onto the test specimen surface of handling through the first step, in drying baker with its oven dry, be put into then and carry out DIFFUSION TREATMENT in the process furnace, treating processes is: begin per minute from room temperature and heat up 10 ℃, insulation is 1 hour during to 400 ℃, per minute heats up 8 ℃ to 850 ℃ subsequently, 850 ℃ are incubated 2 hours, per minute heats up 6 ℃ to 1100 ℃ subsequently, and 1100 ℃ of following constant temperature 3 hours, processing finished the postcooling boiler tube, remove the unnecessary alloy powder coating in boiler tube surface, use its surface composition of scanning electron microscope analysis again, the alloy layer iron nickel content that analysis revealed forms is lower, and alloy layer thickness is about 150 microns, energy suppresses and slows down catalytic coking, and concrete outcome sees Table 1.
Table 1 HK boiler tube is handled back element variation data (wt%)
| Element | Be untreated | Atmosphere is handled | Alloying Treatment |
| ?Cr | ?24.47 | ?61.63 | ?36.2 |
| ?Ni | ?19.35 | ?8.68 | ?5.67 |
| ?Fe | ?54.68 | ?26.69 | ?17.1 |
| ?Al | ?- | ?- | ?38.62 |
Embodiment 2
The processing of HP alloy: the first step, one section on-the-spot HP alloy furnace tubes by adopting that uses is made test specimen, before the test that its surface-conditioning is clean, with its surperficial composition of scanning electron microscope analysis, test specimen is put in the atmosphere processing vessel, feed liquefied ammonia in the container and decompose the gas mixture that the back produces, boiler tube is carried out atmosphere to be handled, treating processes is: begin per minute from room temperature and heat up 7 ℃, insulation is 2 hours during to 800 ℃, per minute heats up 4 ℃ to 1000 ℃ subsequently, about 50 hours of 1000 ℃ of following constant temperature, uses its surface composition of scanning electron microscope analysis after the off-test again.
Second step, to consist of: aluminium 7%, chromium 10%, silicon 5%, rare earth ferrosilicon alloy 3%, ammonium chloride 1%, Sodium Fluoride 0.5% and all the other are the alloy powder of clay powder and the polyvinyl alcohol water solution for preparing in advance, be deployed into the slurry of proper viscosity, slurry is coated onto the test specimen surface of handling through the first step, in drying baker with its oven dry, be put into then and carry out DIFFUSION TREATMENT in the process furnace, treating processes is: begin per minute from room temperature and heat up 8 ℃, insulation is 0.5 hour during to 400 ℃, per minute heats up 6 ℃ to 850 ℃ subsequently, 850 ℃ are incubated 1 hour, per minute heats up 4 ℃ to 1000 ℃ subsequently, and 1000 ℃ of following constant temperature 2 hours, processing finished the postcooling boiler tube, remove the unnecessary alloy powder coating in boiler tube surface, use its surface composition of scanning electron microscope analysis again, this alloy layer iron of analysis revealed nickel content is lower, and alloy layer thickness is about 100 microns, energy suppresses and slows down catalytic coking, and concrete outcome sees Table 2.
Table 2 HP boiler tube processing element delta data (wt%)
| Element | Be untreated | Atmosphere is handled | Alloying Treatment |
| ?Cr | ?19.91 | ?89.90 | ?23.33 |
| ?Ni | ?42.43 | ?2.39 | ?2.07 |
| ?Fe | ?32.65 | ?4.37 | ?2.61 |
| ?Si | ?0.18 | ?0.23 | ?0.20 |
| ?Mn | ?0.91 | ?0.61 | ?6.27 |
| ?O | ?1.33 | ?- | ?28.00 |
| ?Al | ?- | ?- | ?36.54 |
Embodiment 3
Carry out the coking test in the laboratory, alloy layer suppresses and the performance of slow down coking to estimate.The HK boiler tube test specimen that embodiment 1 is handled well is installed to experiment with in the pyrolyzer, tests.Be deposited on the quantity of boiler tube inwall coke with the weighting method measurement, how much come to determine that according to coking amount alloy layer suppresses and the performance of slow down coking.
Make raw material with petroleum naphtha, the coking test-results sees Table 3, and the result shows that the tube coking after the processing reduces about 90%, and inhibition and slow down coking effect are very obvious.Test conditions is as follows:
Boiler tube is of a size of: 12 * 2 * 400.
Cracking stock: petroleum naphtha
Carburettor temperature: 650 ℃
Pyrolyzer temperature: 900 ℃
Oil/water: 1: 0.5
Table 3 naphtha cracking coking test-results
| Test specimen | Time (hr) | With oil mass (g) | Coking amount (mg) | Coking rate (mg/cm 2·hr) | Press down burnt rate (%) |
| Sample is untreated | ????23.9 | ??2500.6 | ????6596 | ????2.75 | |
| Treatment samples 1 | ????24.1 | ??2711.1 | ????741 | ????0.306 | ????88.87 |
| Treatment samples 2 | ????24 | ??2563.4 | ????568 | ????0.236 | ????91.42 |
Embodiment 4
With embodiment 3, cracking stock changes diesel oil into, tests, and test-results sees Table 4, and the result shows that for the cracking stock that weighs some, the boiler tube after the processing reduces coking about 70%, and it is obvious to suppress the coking effect.Test conditions is as follows:
Boiler tube is of a size of: 12 * 2 * 400.
Cracking stock: diesel oil
Carburettor temperature: 700 ℃
Pyrolyzer temperature: 940 ℃
Oil/water: 1: 0.9
Table 4, gas oil pyrolysis coking test-results
| Test specimen | Time (hr) | With oil mass (g) | Coking amount (mg) | Coking rate (mg/cm 2.hr) | Press down burnt rate (%) |
| Sample is untreated | ????5.72 | ????399.5 | ????1777 | ????3.09 | |
| Treatment samples | ????5.07 | ????567.0 | ????505 | ????0.991 | ??67.93 |
Embodiment 5
With embodiment 3, make cracking stock with petroleum naphtha, raising vaporization, cracking temperature are tested, and test-results sees Table 5, and the boiler tube after the processing can reduce coking about 55%.Test conditions is as follows:
Boiler tube is of a size of: 12 * 2 * 400.
Cracking stock: diesel oil
Carburettor temperature: 700 ℃
Pyrolyzer temperature: 940 ℃
Oil/water: 1: 0.8
Table 5,8 hours coking test-results of naphtha cracking
| Test specimen | Time (hr) | With oil mass (g) | Coking amount (mg) | Coking rate (mg/cm 2.hr) | Press down burnt rate (%) |
| Sample is untreated | ????8.25 | ????756.6 | ????802 | ????1.62 | |
| Treatment samples 1 | ????8.16 | ????777.0 | ????340 | ????0.694 | ????57.16 |
| Treatment samples 2 | ????7.5 | ????786.3 | ????369 | ????0.820 | ????49.38 |
| Treatment samples 3 | ????8.25 | ????779.5 | ????361 | ????0.729 | ????55.00 |
From embodiment 3～5 as can be seen, boiler tube is after the technology of the present invention is handled, and coking rate can reduce by 50%～90%, and inhibition and slow down coking effect are apparent in view.
Claims (1)
1, a kind of method that suppresses and slow down the ethylene cracking tube coking is characterized in that comprising the steps:
1) atmosphere is handled: the H that contains that decomposes the back generation with liquefied ammonia
2, N
2And micro-NH
3, H
2O, O
2Gas mixture be reducing gas, boiler tube is carried out atmosphere to be handled, treating processes is: begin per minute from room temperature and heat up 5 ℃～10 ℃, insulation is 20 minutes～3 hours during to 800 ℃, per minute heats up 3 ℃～5 ℃ to t ℃ subsequently, t ℃ of following constant temperature 15 hours～80 hours, 850 ℃≤t≤1250 ℃, processing finished the postcooling boiler tube;
2) Alloying Treatment: alloy powder for preparing and binding agent furnishing slurries, be coated onto the boiler tube surface after atmosphere is handled,, be put into then and carry out DIFFUSION TREATMENT in the process furnace 50 ℃～120 ℃ following baking and curing; Treating processes is: begin per minute from room temperature and heat up 5 ℃～10 ℃, insulation is 0.5 hour～3 hours during to 400 ℃, per minute heats up 5 ℃～8 ℃ to 850 ℃ subsequently, 850 ℃ are incubated 1～3 hour, and per minute heats up 3 ℃～6 ℃ to T ℃ subsequently, 900 ℃≤T≤1200 ℃, T ℃ of following constant temperature 3～7 hours, processing finishes the postcooling boiler tube, removes the unnecessary alloy powder coating in boiler tube surface, can suppress alloy layer with slow down coking in boiler tube surface formation; Described alloy powder is that 5%～30% aluminium, 1%～10% silicon, 5%～20% chromium, 0.5%～5% rare earth, 0.5%～3% catalyzer and all the other are formed for dispersion agent by content; Described catalyzer is ammonium chloride, Sodium Fluoride or sodium aluminum fluoride, and described percentage composition is weight percentage.
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|---|---|---|---|
| CN 200310110224 CN1219023C (en) | 2003-12-12 | 2003-12-12 | Suppressing and slowing method of coking in ethylene cracking furnace tube |
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|---|---|---|---|
| CN 200310110224 CN1219023C (en) | 2003-12-12 | 2003-12-12 | Suppressing and slowing method of coking in ethylene cracking furnace tube |
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| CN1219023C CN1219023C (en) | 2005-09-14 |
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|---|---|---|---|---|
| CN101565808B (en) * | 2008-04-23 | 2011-01-19 | 中国石油大学(北京) | Method for processing high-temperature alloy furnace tube |
| CN101724827B (en) * | 2008-10-24 | 2011-06-15 | 中国石油化工股份有限公司 | Method for reducing ethylene cracking furnace tube coking and improving ethylene selectivity |
| CN102226260A (en) * | 2011-05-05 | 2011-10-26 | 华东理工大学 | Method for improving thermophysical property of coking inhibition silicon/sulfur composite coating of ethene cracking apparatus |
| CN102399573A (en) * | 2010-09-16 | 2012-04-04 | 中国石油化工股份有限公司 | Catalytic cracking furnace tube with catalytic cracking activity and manufacturing method thereof |
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2003
- 2003-12-12 CN CN 200310110224 patent/CN1219023C/en not_active Expired - Fee Related
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| CN101724827B (en) * | 2008-10-24 | 2011-06-15 | 中国石油化工股份有限公司 | Method for reducing ethylene cracking furnace tube coking and improving ethylene selectivity |
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| CN112724717A (en) * | 2020-12-28 | 2021-04-30 | 葛卫江 | Catalytic coating for ethylene cracking furnace |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1219023C (en) | 2005-09-14 |
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