CN106591796B - A method of manganese picotite coating is prepared in cracking furnace pipe inner surface online - Google Patents
A method of manganese picotite coating is prepared in cracking furnace pipe inner surface online Download PDFInfo
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- CN106591796B CN106591796B CN201510666272.XA CN201510666272A CN106591796B CN 106591796 B CN106591796 B CN 106591796B CN 201510666272 A CN201510666272 A CN 201510666272A CN 106591796 B CN106591796 B CN 106591796B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G9/00—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G9/14—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils in pipes or coils with or without auxiliary means, e.g. digesters, soaking drums, expansion means
- C10G9/16—Preventing or removing incrustation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1088—Olefins
- C10G2300/1092—C2-C4 olefins
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to prepare manganese picotite coatings art in cracking furnace pipe inner surface online, disclose a kind of new online method for preparing manganese picotite coating in cracking furnace pipe inner surface, this approach includes the following steps, 1) cracking furnace tube is after coke cleaning operation, preprocessing solution containing chromium compound and manganese compound and carrier gas are injected into the cracking furnace pipe that cracking heater outlet temperature is 400-1000 DEG C, and carry out vapor deposition 2-24h in boiler tube inner wall；2) after vapor deposition, at 700-1100 DEG C, under the atmosphere containing inert gas and the mixed gas of oxidizing gas, it is passivated processing 1-10 hours.
Description
Technical field
The present invention relates to the methods that one kind prepares manganese picotite coating in cracking furnace pipe inner surface online.
Background technique
Ethylene is one of most important basic material of petrochemical industry.The method of production ethylene is at present with pyrolysis in tubular furnace
Based on technology, worldwide it is widely applied.A but unavoidable problem in the production process of ethylene
It is coking and carburizing of the cracker during military service.Coking in cracking process can make boiler tube internal diameter become smaller, pipe internal pressure
Drop increases, and shortens the cycle of operation of pyrolysis furnace；It, must blowing out when tube wall temperature reaches tolerance limit or pressure drop reaches a certain level
Carry out coke cleaning operation.Boiler tube inner wall coking hinders being normally carried out for cracking reaction, influences yield of ethene, reduces production efficiency, and
And be easy to promote boiler tube inner wall carburizing under high temperature, cause furnace tube material performance to weaken.
Existing inhibition method for coke mainly include the following types: (1) control raw material and production process, using hydrotreating,
The techniques such as Aromatics Extractive Project reduce arene content, improve hydrogen content；(2) change under the premise of guaranteeing heat-resisting alloy steel high-temperature behavior
Into the ingredient of alloy, the content that can cause the elements such as Fe, Ni of catalytic coking is reduced as far as possible；(3) change boiler tube construction,
Augmentation of heat transfer；(4) coking inhibitor is added in cracking stock, but dirt can be brought to downstream product by adding coking inhibitor
Dye, and have a degree of corrosion to ethylene boiler tube.
It in CN101565808A, CN101565807A, is handled by special atmosphere, generates manganese in cracking furnace pipe inner surface
Picotite coating can effectively reduce the coking of pyrolysis furnace, extend the pyrolysis furnace cycle of operation.But the technology is needed to newly splitting
Boiler tube processed offline is solved, cannot be on cracker to cracking furnace pipe, directly processing prepares manganese to especially old cracking furnace pipe online
Picotite coating.
Summary of the invention
The purpose of the present invention is to provide a kind of new online manganese picotite coating is prepared in cracking furnace pipe inner surface
Method.
To achieve the goals above, the painting of manganese picotite is prepared in cracking furnace pipe inner surface online the present invention provides a kind of
The method of layer, wherein this approach includes the following steps,
1) cracking furnace tube infuses the preprocessing solution containing chromium compound and manganese compound and carrier gas after coke cleaning operation
Enter in the cracking furnace pipe for being 400-1000 DEG C to cracking heater outlet temperature, and carries out vapor deposition 2-24h in boiler tube inner wall；
2) after vapor deposition, at 700-1100 DEG C, in the mixed gas containing inert gas and oxidizing gas
Under atmosphere, it is passivated processing 1-10 hours.
Through the above technical solutions, the present invention has the following advantages that.
1) can be with the cracking furnace pipe on online processing cracking furnace installation, generating in cracking furnace pipe inner surface has excellent resistive connection
The manganese picotite coating of burnt performance.
It 2), can be instant when being fallen off with the manganese picotite coating of the increase cracking furnace pipe inner surface of cracking number
The online manganese picotite coating for repairing cracking furnace pipe inner surface.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
It is provided by the invention to include the following steps online in the method that cracking furnace pipe inner surface prepares manganese picotite coating,
1) cracking furnace tube infuses the preprocessing solution containing chromium compound and manganese compound and carrier gas after coke cleaning operation
Enter in the cracking furnace pipe for being 400-1000 DEG C to cracking heater outlet temperature, and carries out vapor deposition 2-24h in boiler tube inner wall；
2) after vapor deposition, at 700-1100 DEG C, in the mixed gas containing inert gas and oxidizing gas
Under atmosphere, it is passivated processing 1-10 hours.
The present invention is to provide the methods for preparing manganese picotite coating in the boiler tube inner surface of pyrolysis furnace online.For institute
It states pyrolysis furnace to be not particularly limited, can be this field conventionally used for cracking such as naphtha, heavy diesel fuel and hydrogenation tail oils
Pyrolysis furnace.It for example can be IV type pyrolysis furnace of CRT- as such pyrolysis furnace.
According to the present invention, in cracking furnace tube after coke cleaning operation, by the way that the pre- of chromium compound and manganese compound will be contained
Processing solution and carrier gas are injected into the cracking furnace pipe that cracking heater outlet temperature is 400-1000 DEG C, can be made containing chromium compound
It is pre- thermal evaporation with the preprocessing solution of manganese compound, and sink after decomposing chromium compound and manganese compound in boiler tube inner wall gas phase
Product, obtains manganese picotite coating.In order to preferably form firm coating, it is preferable that in step 1), will be closed containing chromaking
The preprocessing solution and carrier gas of object and manganese compound are injected into the cracking furnace pipe that cracking heater outlet temperature is 700-850 DEG C,
Boiler tube inner wall carries out vapor deposition 5-20h.
According to the present invention, the preprocessing solution contains chromium compound and manganese compound.The chromium compound can be this
Field is commonly used for preparing the compound to form manganese picotite coating.Preferably, the chromium compound is chromium acetylacetonate, different
It is one or more in propyl alcohol chromium and chromic nitrate.
In addition, the manganese compound can be for commonly used in the art for the compounds that preparation forms manganese picotite coating.
Preferably, the manganese compound is one or more in manganese acetylacetonate, isopropanol manganese and manganese nitrate.
According to the present invention, in order to form stronger manganese picotite coating, preferably in the preprocessing solution,
The molar ratio of Cr and Mn element is 0.5-5:1, more preferable 0.5-2:1.
In the present invention, as the solvent of the preprocessing solution, there is no particular limitation, as long as institute can sufficiently be dissolved
State chromium compound and manganese compound.Preferably, the solvent of the preprocessing solution be water, methanol, ethyl alcohol, ethylene glycol, benzene,
One of toluene, ethylbenzene and tetrahydrofuran are a variety of.More preferably one of ethyl alcohol, benzene and tetrahydrofuran or a variety of.
According to the present invention, for the concentration of the preprocessing solution, there is no particular limitation, as long as being capable of forming the manganese
Picotite coating.Preferably, in the preprocessing solution, total concentration of the chromium compound and manganese compound is 1-
15 weight %, more preferably 2-7.5 weight %.
According to the present invention, in step 1), the preprocessing solution can be injected from convection section or across section, preferably from cross
Span injection.
According to the present invention, the carrier gas enters inside cracking furnace pipe and evenly dispersed for carrying deposition liquid, to split
Solution boiler tube inner surface obtains uniform depositing coating.It can be one in inert gas, air and vapor as the carrier gas
Kind is a variety of.In addition, the inert gas is one of nitrogen, argon gas and helium or a variety of.
According to the present invention, chemically consider in terms of the deposition uniformity of vapour deposition coating and firmness, it is preferably described
Preprocessing solution and the weight flow rate of carrier gas ratio are 1:1-50, more preferably 1:5-30.
In the present invention, it can be selected according to the size of cracking furnace tube as the injection rate of the carrier gas, as long as
Ensure that carrier gas can be evenly distributed in each group cracking furnace pipe by Venturi tube, for example, the CRT- IV that production capacity is 60,000 tons
The cracking furnace tube of type, the injection rate of the carrier gas can be 11t (ton)/h or more, preferably 12-18t/h.
According to the present invention, after vapor deposition, at 700-1100 DEG C, mixed containing inert gas and oxidizing gas
Under the atmosphere for closing gas, it is passivated processing 1-10 hours.
In the present invention, it by the Passivation Treatment of step 2), can remove the carbon deposit in depositing coating, make to be deposited on boiler tube
The metal oxide and boiler tube of inner wall interpenetrate at high temperature, form firm coating.Firm apply is formed from further
The aspect of layer considers that preferably the temperature of Passivation Treatment is 700-850 DEG C, and the Passivation Treatment time is 2-5 hours.
According to the present invention, in step 2), the preferably described mixed gas includes inert gas, the 5-20 body of 75-95 volume %
The O of product %2And/or CO2With the vapor of 0-5 volume %.As such mixed gas, consider from cost, it is preferably empty
Gas.
It according to the present invention, can be 0.5-50 μm, preferably 2-30 μm by the thickness of coating obtained by the above method.
The present invention will be described in detail by way of examples below, but the present invention is not limited in following embodiments.
Embodiment 1
The present embodiment is for illustrating for method of the invention to be used for prepare manganese picotite in cracking furnace pipe inner surface online
Coating.
In the present embodiment, industrial pyrolysis furnace is IV type pyrolysis furnace of CRT-, and cracking stock is naphtha, produces 60000 tons of second per year
Alkene, 100 days pyrolysis furnace longest cycles of operation of original when cracking naphtha.After burning, switching cracking heater outlet temperature (COT) is
750 DEG C, injecting chromium acetylacetonate and manganese acetylacetonate across section, (total concentration of chromium acetylacetonate and manganese acetylacetonate is 5
The molar ratio of weight %, chromium and manganese carries out vapor deposition 8 hours for the benzole soln and water vapour of 2:1), wherein chromium acetylacetonate
Injection rate with the benzole soln of manganese acetylacetonate is 2 tons/h, and the injection rate of vapor is 15 tons/h.
After deposition, at 750 DEG C under air atmosphere constant temperature 3 hours.Then charging is switched to water vapour and COT
830 DEG C are warming up to, investment naphtha produces ethylene after stablizing, and the pyrolysis furnace cycle of operation is 200 days.
Embodiment 2
The present embodiment is for illustrating for method of the invention to be used for prepare manganese picotite in cracking furnace pipe inner surface online
Coating.
In the present embodiment, industrial pyrolysis furnace is IV type pyrolysis furnace of CRT-, and cracking stock is naphtha, produces 60000 tons of second per year
Alkene, 100 days pyrolysis furnace longest cycles of operation of original when cracking naphtha.After burning, switching cracking heater outlet temperature temperature is
700 DEG C, across section inject isopropanol chromium and isopropanol manganese (total concentration of isopropanol chromium and isopropanol manganese is 7.5 weight %,
The molar ratio of chromium and manganese be 1:1) tetrahydrofuran solution and water vapour carry out vapor deposition 20 hours, wherein isopropanol chromium and
The injection rate of the tetrahydrofuran solution of isopropanol manganese is 0.36 ton/h, and the injection rate of vapor is 18 tons/h.
After deposition, at 700 DEG C under air atmosphere constant temperature 5 hours.Then charging is switched to water vapour and COT
830 DEG C are warming up to, investment naphtha produces ethylene after stablizing, and the pyrolysis furnace cycle of operation is 160 days.
Embodiment 3
The present embodiment is for illustrating for method of the invention to be used for prepare manganese picotite in cracking furnace pipe inner surface online
Coating.
In the present embodiment, industrial pyrolysis furnace is IV type pyrolysis furnace of CRT-, and cracking stock is naphtha, produces 60000 tons of second per year
Alkene, 100 days pyrolysis furnace longest cycles of operation of original when cracking naphtha.After burning, switching cracking heater outlet temperature COT temperature
It is 850 DEG C, injecting chromic nitrate and manganese nitrate across section, (total concentration of chromic nitrate and manganese nitrate is 2 weight %, chromium and manganese
Molar ratio is 1:2) ethanol solution and water vapour carry out vapor deposition 5 hours, wherein the ethanol solution of chromic nitrate and manganese nitrate
Injection rate be 2.4 tons/h, the injection rate of vapor is 12 tons/h.
After deposition, at 850 DEG C under air atmosphere constant temperature 2 hours.Then charging is switched to water vapour and COT
830 DEG C are dropped to, investment naphtha produces ethylene after stablizing, and the pyrolysis furnace cycle of operation is 180 days.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (12)
1. the method that one kind prepares manganese picotite coating in cracking furnace pipe inner surface online, which is characterized in that this method includes
Following steps,
1) preprocessing solution containing chromium compound and manganese compound is injected by cracking furnace tube after coke cleaning operation with carrier gas
It cracks in the cracking furnace pipe that heater outlet temperature is 400-1000 DEG C, and carries out vapor deposition 2-24h in boiler tube inner wall；
2) after vapor deposition, at 700-1100 DEG C, in the atmosphere containing inert gas and the mixed gas of oxidizing gas
Under, it is passivated processing 1-10 hours；
Wherein, in the preprocessing solution, total concentration of the chromium compound and manganese compound is 1-15 weight %, Cr and Mn
The molar ratio of element is 0.5-5:1；
The manganese compound is one or more in manganese acetylacetonate, isopropanol manganese and manganese nitrate.
2. according to the method described in claim 1, wherein, in step 1), by the pre- place containing chromium compound and manganese compound
Reason solution and carrier gas are injected into the cracking furnace pipe that cracking heater outlet temperature is 700-850 DEG C, and carry out gas phase in boiler tube inner wall
Deposit 5-20h.
3. according to the method described in claim 1, wherein, the chromium compound is chromium acetylacetonate, isopropanol chromium and chromic nitrate
One of or it is a variety of.
4. method described in any one of -3 according to claim 1, wherein in the preprocessing solution, Cr and Mn element
Molar ratio is 0.5-2:1.
5. method described in any one of -3 according to claim 1, wherein the solvent of the preprocessing solution be water, methanol,
One of ethyl alcohol, ethylene glycol, benzene, toluene, ethylbenzene and tetrahydrofuran are a variety of.
6. according to the method described in claim 5, wherein, in the preprocessing solution, the chromium compound and manganese compound
Total concentration is 2-7.5 weight %.
7. method described in any one of -3 according to claim 1, wherein the carrier gas is that inert gas, air and water steam
One of gas is a variety of.
8. method described in any one of -3 according to claim 1, wherein the weight flow rate of the preprocessing solution and carrier gas
Than for 1:1-50.
9. according to the method described in claim 8, wherein, the weight flow rate ratio of the preprocessing solution and carrier gas is 1:5-30.
10. method described in any one of -3 according to claim 1, wherein in step 2), the mixed gas includes 75-
The O of the inert gas of 95 volume %, 5-20 volume %2And/or CO2And the vapor of 0-5 volume %.
11. method described in any one of -3 according to claim 1, wherein in step 1), the preprocessing solution is from right
It flows section or is injected across section.
12. according to the method for claim 11, wherein in step 1), the preprocessing solution is injected from across section.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565807A (en) * | 2008-04-23 | 2009-10-28 | 中国石油大学(北京) | Method for processing high-temperature alloy furnace tube |
| CN102251225A (en) * | 2010-05-21 | 2011-11-23 | 中国石油化工股份有限公司 | Treatment method and coating pretreatment liquid for reducing coking of furnace tube of hydrocarbon cracking furnace |
| CN103788983A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Coking-resistant hydrocarbon cracking furnace pipe and preparation method thereof |
-
2015
- 2015-10-15 CN CN201510666272.XA patent/CN106591796B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565807A (en) * | 2008-04-23 | 2009-10-28 | 中国石油大学(北京) | Method for processing high-temperature alloy furnace tube |
| CN102251225A (en) * | 2010-05-21 | 2011-11-23 | 中国石油化工股份有限公司 | Treatment method and coating pretreatment liquid for reducing coking of furnace tube of hydrocarbon cracking furnace |
| CN103788983A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Coking-resistant hydrocarbon cracking furnace pipe and preparation method thereof |
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