CN116162494A - Method and system for treating heavy raw oil - Google Patents
Method and system for treating heavy raw oil Download PDFInfo
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- CN116162494A CN116162494A CN202111416086.2A CN202111416086A CN116162494A CN 116162494 A CN116162494 A CN 116162494A CN 202111416086 A CN202111416086 A CN 202111416086A CN 116162494 A CN116162494 A CN 116162494A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000003921 oil Substances 0.000 claims abstract description 213
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 126
- 239000001257 hydrogen Substances 0.000 claims abstract description 126
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 122
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 106
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 76
- 238000006243 chemical reaction Methods 0.000 claims abstract description 73
- 238000004821 distillation Methods 0.000 claims abstract description 67
- 239000000852 hydrogen donor Substances 0.000 claims abstract description 65
- 239000003054 catalyst Substances 0.000 claims abstract description 52
- 239000002002 slurry Substances 0.000 claims abstract description 51
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 37
- 239000000047 product Substances 0.000 claims abstract description 35
- 238000011069 regeneration method Methods 0.000 claims abstract description 29
- 230000008929 regeneration Effects 0.000 claims abstract description 28
- 239000000295 fuel oil Substances 0.000 claims abstract description 17
- 238000004064 recycling Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 50
- 238000000926 separation method Methods 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 9
- 238000005292 vacuum distillation Methods 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- MGNZXYYWBUKAII-UHFFFAOYSA-N cyclohexa-1,3-diene Chemical compound C1CC=CC=C1 MGNZXYYWBUKAII-UHFFFAOYSA-N 0.000 claims description 6
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 claims description 6
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 4
- 239000011280 coal tar Substances 0.000 claims description 3
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 3
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 claims description 3
- 208000012839 conversion disease Diseases 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 40
- 230000000694 effects Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present disclosure relates to a method and system for treating heavy feedstock oil, the method comprising: the raw oil, the catalyst and the hydrogen donor are subjected to hydrogenation reaction, and hydrogenation reaction products are obtained and separated to obtain high-fraction oil; carrying out steam stripping treatment on the high-fraction oil, and carrying out atmospheric distillation on the obtained steam stripping tower bottom oil to obtain a hydrogen supply agent and an atmospheric tower bottom oil after hydrogen supply; subjecting the atmospheric bottom oil to reduced pressure distillation to obtain a heavy oil product and unconverted oil containing a catalyst; returning a portion of said unconverted oil to said slurry bed reactor for continued reaction; carrying out hydrogenation regeneration treatment on the hydrogen donor and the hydrogen after hydrogen supply to obtain a regenerated hydrogen donor; and returning part of the regenerated hydrogen donor to the slurry bed reactor for recycling. By adopting the method disclosed by the disclosure, the recycling of the hydrogen donor, the catalyst and unconverted oil can be realized, the reaction conversion rate is improved, and the hydrogenation reaction can be performed under safer conditions.
Description
Technical Field
The present disclosure relates to the field of petrochemical industry, and in particular, to a method and system for processing heavy feedstock oil.
Background
At present, oil refining enterprises face the continuous rising of crude oil price, poor crude oil properties, rising of light oil demand and more strict competitive pressure of fuel oil and environmental standards, at present, the types of residual oil hydrogenation processes in the world are of 4 kinds, namely fixed bed, boiling bed, moving bed and slurry bed residual oil hydrogenation, and the slurry bed hydrogenation technology has the advantages of being capable of processing the worst residual oil, even coal, but the reaction system pressure is high, the chemical hydrogen consumption is increased compared with that of the fixed bed, the boiling bed and the moving bed, and the equipment investment is high. Therefore, the reduction of the pressure of the reaction system is of great importance for the energy saving and consumption reduction of the whole device.
In slurry bed residual oil hydrogenation, a reaction system is in a high-pressure and hydrogen-critical state, raw oil is poor in property and serious in coking, and in addition, because the molecular weight of hydrogen is low, leakage is easy to escape, so that a large safety risk is caused; meanwhile, the device has high equipment investment and high safety risk under the high-pressure condition, which brings great trouble to the stable, safe and long-period operation of the slurry bed residual oil hydrogenation device adopting the prior art.
Disclosure of Invention
It is an object of the present disclosure to provide a method and system for treating heavy feedstock oils that allows slurry bed reactions to be performed at low pressure, non-hydrogen conditions.
To achieve the above object, a first aspect of the present disclosure provides a method of treating heavy raw oil, the method comprising: the raw oil, the catalyst and the hydrogen supply agent are contacted in a slurry bed reactor to carry out hydrogenation reaction, so as to obtain a hydrogenation reaction product; the hydrogenation reaction product is subjected to hot high-pressure separation and cold high-pressure separation to obtain a first gas phase and high-fraction oil; subjecting the high-fraction oil to steam stripping treatment to obtain a second gas phase and a bottom oil of a steam stripping tower; performing atmospheric distillation on the stripping tower bottom oil to obtain a third gas phase, a hydrogen donor after hydrogen supply, a light oil product and atmospheric tower bottom oil; subjecting the atmospheric bottoms to reduced pressure distillation to obtain a fourth vapor phase, a heavy oil product, and unconverted oil containing catalyst; returning a portion of said unconverted oil to said slurry bed reactor for continued reaction; sending the hydrogen donor and hydrogen after hydrogen supply into a hydrogen donor regeneration unit for hydrogenation regeneration treatment to obtain a regenerated hydrogen donor; and returning part of the regenerated hydrogen supply agent to the slurry bed reactor for recycling, and sending the other part of the regenerated hydrogen supply agent out of the system as a light fraction.
Optionally, the raw oil is one or more selected from atmospheric residuum, vacuum wax oil, coking wax oil, deasphalted oil and coal tar; the hydrogen donor is one or more selected from cyclohexane, methylcyclohexane, decalin and cyclohexadiene; the catalyst is an oil-soluble organic homogeneous molybdenum catalyst and/or a supported nickel-molybdenum ultrafine powder catalyst.
Optionally, the reaction conditions of the hydrogenation reaction include: the reaction temperature is 150-450 ℃, the reaction pressure is 5-70 bar, the reaction time is 0.5-10 h, and the mass ratio of the hydrogen donor to the raw oil is below 2; preferably 1 or less.
Optionally, the method further comprises, before entering the slurry bed reactor, pressurizing the mixed raw material obtained by mixing the raw material oil, the catalyst and the hydrogen donor to 0.5-7 MPa, exchanging heat with the hydrogenation reaction product, and then heating to 150-450 ℃;
optionally, the stripping medium of the stripping treatment is steam.
Optionally, the temperature cutting point of the third gas phase and the hydrogen donor after hydrogen supply is 40-80 ℃, the temperature cutting point of the hydrogen donor after hydrogen supply and the light oil product is 130-160 ℃, and the temperature cutting point of the light oil product and the atmospheric tower bottom oil is 300-360 ℃; the temperature cut point of the fourth gas phase and the heavy oil product is 300-360 ℃, and the temperature cut point of the heavy oil product and the unconverted oil is 480-540 ℃.
Optionally, the ratio of the fraction of unconverted oil returned to the slurry bed reactor to the total weight of unconverted oil is 1 or less, preferably 0.8 or less; the ratio of the part of the regenerated hydrogen-donor returned to the slurry bed reactor to the total weight of the regenerated hydrogen-donor is 0.2 to 1, preferably 0.8 to 1.
Optionally, the conditions of the hydro-regeneration treatment include: the reaction temperature is 150-250 ℃, the reaction pressure is 0.5-5MPa, the reaction time is 0.1-1 h, and the volume ratio of the hydrogen to the hydrogen donor after hydrogen supply is 10-300: 1.
a second aspect of the present disclosure provides a system for treating heavy feedstock oil, the system comprising a hydrogenation reaction unit, a high pressure separation unit, a stripping unit, an atmospheric distillation unit, a reduced pressure distillation unit, and a hydrogen donor regeneration unit; the hydrogenation reaction unit comprises a slurry bed reactor, a raw oil inlet, a catalyst inlet, a hydrogen supply agent inlet and a hydrogenation reaction product outlet; the high-pressure separation unit comprises a hydrogenation reaction product inlet, a first gas phase outlet and a high-pressure oil separation outlet; the stripping unit comprises a high-pressure oil inlet, a stripping medium inlet, a second gas phase outlet and a stripping tower bottom oil outlet; the atmospheric distillation unit comprises an atmospheric distillation tower; the atmospheric distillation tower comprises a stripping tower bottom oil inlet, a third gas phase outlet, a hydrogen supply agent outlet after hydrogen supply, a light oil product outlet and an atmospheric tower bottom oil outlet; the reduced pressure distillation unit comprises a reduced pressure distillation tower; the pressure reduction distillation tower comprises an atmospheric tower bottom oil inlet, a fourth gas phase outlet, a heavy oil product outlet and an unconverted oil outlet; the hydrogen supply agent regeneration unit comprises a hydrogenation reactor; the hydrogenation reactor comprises a hydrogen supply agent inlet, a hydrogen inlet and a regenerated hydrogen supply agent outlet after hydrogen supply; wherein, the hydrogenation reaction product outlet of the hydrogenation reaction unit is communicated with the hydrogenation reaction product inlet of the high-pressure separation unit through a hydrogenation reaction product pipeline; the high-pressure separation unit is communicated with the stripping unit through a high-pressure oil inlet; the stripping bottom oil outlet of the stripping unit is communicated with the stripping bottom oil inlet of the atmospheric distillation tower; the atmospheric bottom oil outlet of the atmospheric distillation tower is communicated with the atmospheric bottom oil inlet of the vacuum distillation tower; the unconverted oil outlet of the reduced pressure distillation tower is communicated with the raw oil inlet of the hydrogenation reaction unit; the hydrogen supply agent outlet after hydrogen supply of the atmospheric distillation tower is communicated with the hydrogen supply agent inlet after hydrogen supply of the hydrogen supply agent regeneration unit; the regenerated hydrogen supply agent outlet of the hydrogen supply agent regeneration unit is communicated with the hydrogen supply agent inlet of the hydrogenation reaction unit.
Optionally, according to the flow direction of the raw materials, the hydrogenation reaction unit further comprises a feeding pipeline, a feeding pump, a feeding heat exchanger and a reaction feeding heating furnace which are communicated in sequence; the feed pipeline is provided with the raw oil inlet, a catalyst inlet and a hydrogen supply agent inlet, the outlet of the feed pump is communicated with the cold medium side inlet of the feed heat exchanger, the cold medium side outlet of the feed heat exchanger is communicated with the inlet of the reaction feed heating furnace, and the outlet of the reaction feed heating furnace is communicated with the raw material inlet of the slurry bed reactor;
optionally, the heat medium side of the feed heat exchanger is in communication with the hydrogenation reaction product line.
Optionally, the unconverted oil outlet line of the vacuum distillation tower is divided into two streams, one stream is communicated with the raw oil inlet of the slurry bed reactor, and the other stream is sent out of the system; the regenerated hydrogen supply agent outlet pipeline of the hydrogen supply agent regeneration unit is divided into two parts, one part is communicated with the hydrogen supply agent inlet of the slurry bed reactor, and the other part is sent out of the system.
Through the technical scheme, by adopting the method disclosed by the disclosure, the hydrogen supply agent after hydrogen supply is subjected to hydrogenation regeneration treatment, and part of regenerated hydrogen supply agent is returned to the slurry bed reactor for continuous reaction, so that the recycling of the hydrogen supply agent can be realized; the unconverted oil containing the catalyst, which is obtained by further separating the bottom oil of the normal pressure tower, is returned to the slurry bed reactor, so that the catalyst and the unconverted oil can be recycled, the use amount of the catalyst is reduced, and the reaction conversion rate is improved; the method can reduce the consumption of the hydrogen donor, the product is easy to separate, the hydrogenation operation pressure of the hydrogen donor is low, and the hydrogenation reaction can be carried out under safer conditions.
Additional features and advantages of the present disclosure will be set forth in the detailed description which follows.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosure, and are incorporated in and constitute a part of this specification, illustrate the disclosure and together with the description serve to explain, but do not limit the disclosure. In the drawings:
fig. 1 is a process flow diagram of an embodiment of a method of treating heavy feedstock oil of the present disclosure.
Description of the reference numerals
P1, a feed pump; E. a feed heat exchanger; f1, a reaction feeding heating furnace; r1, a slurry bed reactor; d1, a cold/hot high-pressure separator; t1, a stripping tower; t2, an atmospheric distillation tower; t3, a reduced pressure distillation tower; f2, a reaction feeding heating furnace; r2, a hydrogenation reactor; 1. raw oil; 2. a hydrogen donor; 3. a catalyst; 4. mixing materials; 5. exchanging heat to mix materials; 6. preheating and mixing materials; 7. hydrogenation reaction products; 8. hydrogenation reaction products after heat exchange; 9. a first gas phase; 10. high-pressure oil separation; 11. a second gas phase; 12. stripping the bottoms; 13. a third gas phase; 14. hydrogen gas; 15. a hydrogen donor after hydrogen supply; 16. a light oil product; 17. a pipeline; 18. an external throwing hydrogen donor; 19. regenerating the hydrogen donor; 20. an atmospheric bottom oil; 21. A fourth gas phase; 22. a heavy oil product; 23. unconverted oil containing catalyst; 24. the unconverted oil containing the catalyst is thrown outwards.
Detailed Description
Specific embodiments of the present disclosure are described in detail below with reference to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the disclosure, are not intended to limit the disclosure.
A first aspect of the present disclosure provides a method of treating heavy feedstock oil, the method comprising: the raw oil, the catalyst and the hydrogen supply agent are contacted in a slurry bed reactor to carry out hydrogenation reaction, so as to obtain a hydrogenation reaction product; the hydrogenation reaction product is subjected to hot high-pressure separation and cold high-pressure separation to obtain a first gas phase and high-fraction oil; subjecting the high-fraction oil to steam stripping treatment to obtain a second gas phase and steam stripping bottom oil; performing atmospheric distillation on the stripping tower bottom oil to obtain a third gas phase, a hydrogen donor after hydrogen supply, a light oil product and atmospheric tower bottom oil; subjecting the atmospheric bottoms to reduced pressure distillation to obtain a fourth gas phase, a heavy oil product, and unconverted oil containing catalyst; returning a portion of said unconverted oil to said slurry bed reactor for continued reaction; sending the hydrogen donor and hydrogen after hydrogen supply into a hydrogen donor regeneration unit for hydrogenation regeneration treatment to obtain a regenerated hydrogen donor; and returning part of the regenerated hydrogen supply agent to the slurry bed reactor for recycling, and sending the other part of the regenerated hydrogen supply agent out of the system as a light fraction.
Through the technical scheme, by adopting the method disclosed by the disclosure, the hydrogen supply agent after hydrogen supply is subjected to hydrogenation regeneration treatment, and part of regenerated hydrogen supply agent is returned to the slurry bed reactor for continuous reaction, so that the recycling of the hydrogen supply agent can be realized; the unconverted oil containing the catalyst, which is obtained by further separating the bottom oil of the normal pressure tower, is returned to the slurry bed reactor, so that the catalyst and the unconverted oil can be recycled, the use amount of the catalyst is reduced, and the reaction conversion rate is improved; the method can reduce the consumption of the hydrogen donor, the product is easy to separate, the hydrogenation operation pressure of the hydrogen donor is low, and the hydrogenation reaction can be carried out under safer conditions.
In one embodiment, the methods described herein are capable of processing a number of heavy feedstock oils of high viscosity and high impurity content, which may be selected from one or more of atmospheric residuum, vacuum wax oil, coker wax oil, deasphalted oil, and coal tar, for example.
In one embodiment, the flow ratio of regenerated hydrogen donor to fresh hydrogen donor returned to the slurry bed reactor is from 0.1 to 99:1.
in one embodiment, the hydrogen donor is one or more selected from cyclohexane, methylcyclohexane, decalin and cyclohexadiene. In the above embodiment, the hydrogen donor is used to replace the hydrogen in the prior art, so that the pressure in the hydrogen transfer reaction process can be reduced, the safety of the reaction is further enhanced, and meanwhile, the hydrogenation reaction effect is not much different from the reaction effect of using hydrogen.
In one embodiment, the mass ratio of the hydrogen donor to the raw oil is 2 or less, preferably 1 or less, and more preferably 0.3 to 1. In this embodiment, the mass ratio of the hydrogen donor to the raw oil is controlled to be a certain ratio, so that the addition amount of the hydrogen donor can be reduced while ensuring a good hydrogenation effect, and the cost can be further reduced.
In one embodiment, the catalyst is an oil-soluble organic homogeneous molybdenum-based catalyst and/or a supported nickel-molybdenum-based ultrafine powder-based catalyst. Wherein, the oil-soluble organic homogeneous molybdenum catalyst can also be used as a reaction raw material to carry out continuous reaction in a slurry bed reactor. In this embodiment, the catalyst can perform a catalytic function and further can make the reaction more complete, and therefore, the efficiency and the completion of the hydrogenation reaction can be further improved.
In one embodiment, the reaction conditions of the hydrogenation reaction include: the reaction temperature is 150-450 ℃, the reaction pressure is 5-70 bar, and the reaction time is 0.5-10 h.
In this embodiment, in order to enhance the reaction effect of the hydrogenation reaction, the conditions of the hydrogenation reaction and the amount of the reactants are selected; by further preferably selecting the relevant reaction conditions, the effect of the hydrogenation reaction can be further enhanced.
In one embodiment, the method further comprises, before entering the slurry bed reactor, pressurizing the mixed raw material obtained by mixing the raw material oil, the catalyst and the hydrogen donor to 0.5-7 MPa, introducing the mixed raw material into a tube side of a feed heat exchanger, exchanging heat with the hydrogenation reaction product flowing through a shell side of the feed heat exchanger, and then heating to 150-450 ℃ through a reaction feed heating furnace. In this embodiment, the mixed raw materials can quickly reach the reaction temperature when entering the slurry bed reactor, and then the reaction is carried out.
Optionally, subjecting the separated high-fraction oil from the hydrogenation reaction product to a stripping treatment; the stripping treatment is carried out in a stripping tower, and the stripping medium is water vapor.
In one embodiment, the hot high pressure separation and cold high pressure separation are performed in a cold/hot high pressure separator, and the first gas phase and the high-pressure oil are separated by flash evaporation.
In one embodiment, the atmospheric distillation is performed in an atmospheric distillation tower, the temperature cut point of the third gas phase and the hydrogen donor after hydrogen supply is 40-80 ℃, the temperature cut point of the hydrogen donor after hydrogen supply and the light oil product is 130-160 ℃, and the temperature cut point of the light oil product and the atmospheric bottom oil is 300-360 ℃. Wherein the fraction interval of the hydrogen donor after hydrogen supply obtained by atmospheric distillation is 40-195 ℃, preferably 45-75 ℃;
in one embodiment, the reduced pressure distillation is performed in a reduced pressure distillation column, the fourth gas phase and the heavy oil product have a temperature cut point of 300 to 360 ℃, and the heavy oil product and the unconverted oil have a temperature cut point of 480 to 540 ℃. Wherein the distillation range of unconverted oil containing catalyst is 400-1000 deg.C, preferably 520-1000 deg.C.
In the above embodiment, the first gas phase, the second gas phase, the third gas phase and the fourth gas phase are light hydrocarbons, and the first gas phase, the second gas phase, the third gas phase and the fourth gas phase are led out of the system.
In one embodiment, the ratio of the portion of unconverted oil returned to the slurry bed reactor to the total weight of unconverted oil is 1 or less, preferably 0.8 or less.
In one embodiment, the ratio of the portion of the regenerated hydrogen-donor returned to the slurry bed reactor to the total weight of the regenerated hydrogen-donor is from 0.2 to 1, preferably from 0.8 to 1.
In one embodiment, after the hydrogen donor to be generated is mixed with hydrogen, the mixture is heated by a reaction feeding heating furnace and then enters a hydrogenation reactor for hydrogenation regeneration reaction; the conditions of the hydrogenation regeneration reaction include: the reaction temperature is 150-250 ℃, preferably 180-220 ℃; the reaction pressure is 0.5-5MPa, preferably 2.5-3.5 MPa; the reaction time is 0.1-1 h, and the volume ratio of the hydrogen to the hydrogen donor to be generated is 10-300: 1.
a second aspect of the present disclosure provides a system for treating heavy feedstock oil, the system comprising a hydrogenation reaction unit, a high pressure separation unit, a stripping unit, an atmospheric distillation unit, a reduced pressure distillation unit, and a hydrogen donor regeneration unit; the hydrogenation reaction unit comprises a slurry bed reactor, a raw oil inlet, a catalyst inlet, a hydrogen supply agent inlet and a hydrogenation reaction product outlet; the high-pressure separation unit comprises a hydrogenation reaction product inlet, a first gas phase outlet and a high-pressure oil separation outlet; the stripping unit comprises a high-pressure oil inlet, a stripping medium inlet, a second gas phase outlet and a stripping tower bottom oil outlet; the atmospheric distillation unit comprises an atmospheric distillation tower; the atmospheric distillation tower comprises a stripping tower bottom oil inlet, a third gas phase outlet, a hydrogen supply agent outlet after hydrogen supply, a light oil product outlet and an atmospheric tower bottom oil outlet; the reduced pressure distillation unit comprises a reduced pressure distillation tower; the pressure reduction distillation tower comprises an atmospheric tower bottom oil inlet, a fourth gas phase outlet, a heavy oil product outlet and an unconverted oil outlet; the hydrogen supply agent regeneration unit comprises a hydrogenation reactor; the hydrogenation reactor comprises a hydrogen supply agent inlet, a hydrogen inlet and a regenerated hydrogen supply agent outlet after hydrogen supply; the hydrogenation reaction product outlet of the hydrogenation reaction unit is communicated with the hydrogenation reaction product inlet of the high-pressure separation unit through a hydrogenation reaction product pipeline, so that a hydrogenation reaction product generated by hydrogenation reaction enters the high-pressure separation unit for separation; the high-pressure separation unit is provided with a high-pressure oil inlet, a high-pressure oil outlet and a high-pressure oil outlet, wherein the high-pressure oil inlet is communicated with the high-pressure oil outlet of the high-pressure separation unit; the stripping bottom oil outlet of the stripping unit is communicated with the stripping bottom oil inlet of the atmospheric distillation tower, so that the stripping bottom oil enters the atmospheric distillation tower to be subjected to atmospheric distillation; the atmospheric bottom oil outlet of the atmospheric distillation tower is communicated with the atmospheric bottom oil inlet of the vacuum distillation tower, so that the atmospheric bottom oil obtained by atmospheric distillation enters the vacuum distillation tower for vacuum distillation; the unconverted oil outlet of the reduced pressure distillation tower is communicated with the raw oil inlet of the hydrogenation reaction unit, so that unconverted oil in the reduced pressure distillation tower returns to the hydrogenation reaction unit to continue the reaction; the hydrogen supply agent outlet after hydrogen supply of the atmospheric distillation tower is communicated with the hydrogen supply agent inlet after hydrogen supply of the hydrogen supply agent regeneration unit, and is used for feeding the hydrogen supply agent after hydrogen supply into the hydrogen supply agent regeneration unit for hydrogenation regeneration treatment; the regenerated hydrogen supply agent outlet of the hydrogen supply agent regeneration unit is communicated with the hydrogen supply agent inlet of the hydrogenation reaction unit and is used for returning regenerated hydrogen supply agent to the hydrogenation reaction unit to participate in the reaction.
In one embodiment, the hydrogenation reaction unit further comprises a feeding pipeline, a feeding pump, a feeding heat exchanger and a reaction feeding heating furnace which are communicated in sequence according to the flow direction of the raw materials; the feed pipeline is provided with the raw oil inlet, the catalyst inlet and the hydrogen supply agent inlet, and the outlet of the feed pump is communicated with the cold medium side inlet of the feed heat exchanger and is used for enabling the mixed material to enter the heat exchanger for heat exchange; the cold medium side outlet of the feeding heat exchanger is communicated with the inlet of the reaction feeding heating furnace and is used for preheating the mixed material after heat exchange in the reaction feeding heating furnace; the outlet of the reaction feeding heating furnace is communicated with the raw material inlet of the slurry bed reactor and is used for feeding the preheated mixture into the slurry bed reactor for hydrogenation reaction.
Optionally, the heat medium side of the feeding heat exchanger is communicated with the hydrogenation reaction product pipeline and is used for enabling the hydrogenation reaction product after the reaction to enter the feeding heat exchanger to exchange heat with the mixed material.
In one embodiment, the unconverted oil outlet line of the vacuum distillation column is split into two streams, one stream being in communication with the feed oil inlet of the slurry bed reactor for returning a portion of the unconverted oil to the slurry bed reactor for further reaction; another strand is sent out of the system;
in one embodiment, the regenerated hydrogen-supplying agent outlet pipeline of the hydrogen-supplying agent regeneration unit is divided into two parts, and one part is communicated with the hydrogen-supplying agent inlet of the slurry bed reactor and is used for returning regenerated hydrogen-supplying agent to the slurry bed reactor to participate in the reaction; the other strand is sent out of the system.
In one embodiment, as shown in fig. 1, a method of treating heavy feedstock oil includes:
after the raw oil 1, the hydrogen supply agent 2 and the catalyst 3 are mixed and then boosted by a feed pump P1, the mixture is heated by a feed heat exchanger E and a reaction feed heating furnace F1, the mixture enters a slurry bed reactor R1 for hydrogenation reaction, an obtained hydrogenation reaction product 7 is subjected to heat exchange by the feed heat exchanger E and then enters a cold/hot high-pressure separator D1, a first gas phase 9 and high-pressure oil 10 are obtained through separation, the high-pressure oil 10 enters a stripping tower T1, a second gas phase 11 and a stripping tower bottom oil 12 are stripped, the stripping tower bottom oil 12 is sent to an atmospheric distillation tower T2, a third gas phase 13, the hydrogen supply agent 15 after hydrogen supply, a light oil product 16 and an atmospheric tower bottom oil 20 are obtained, the atmospheric tower bottom oil 20 enters a vacuum distillation tower T3, a fourth gas phase 21, a heavy oil product 22 and unconverted oil 23 containing the catalyst oil are obtained after further distillation, a part of the unconverted oil 23 containing the catalyst is returned to an inlet of the feed pump P1, and a part of unconverted oil 24 containing the catalyst is thrown outside and sent to a device for further treatment;
the hydrogen-supplying agent 15 after hydrogen supply is mixed with the hydrogen 14, heated by a reaction feeding heating furnace F2, then enters a hydrogenation reactor R2 for hydrogenation reaction, a part of the reaction product is thrown out of the hydrogen-supplying agent 18 as light fraction oil to be sent out of the boundary zone, and a part of the regenerated hydrogen-supplying agent 19 is returned to the inlet of a feeding pump P1.
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The raw oil used in the following examples and comparative examples is vacuum residuum, and specific parameters are shown in Table 1; the catalyst is an oil-soluble organic homogeneous molybdenum catalyst.
TABLE 1 index of raw oil
| Index (I) | Numerical value |
| Density (20 ℃ C.)/(g/cm) 3 ) | 1073 |
| Viscosity (20 ℃ C.)/(mPa.s) | 900 |
| Wt% of sulfur | 3.6 |
| Ni(ppm) | 41 |
| V(ppm) | 108 |
| Asphaltenes wt% | 11 |
Example 1
Mixing 100t/h of raw oil 1, a hydrogen supplier 2 (cyclohexane, the once-loading amount is 100t, the flow after stabilization is 10 t/h) and an oil-soluble organic homogeneous molybdenum catalyst 3 (the once-loading amount is 20t, the flow after stabilization is 1.5 t/h), then heating F1 to 70bar and 425 ℃ through a feed pump P1, a feed heat exchanger E and a reaction feed heating furnace, feeding into a slurry bed reactor R1, and carrying out hydrogenation reaction under the conditions of 425 ℃ and 7MPa for 1h; wherein the mass ratio of the hydrogen donor to the raw oil is 0.5:1; the hydrogenation reaction product 7 is subjected to heat exchange by a feeding heat exchanger E and then enters a cold/hot high-pressure separator D1, the first gas phase 9 and high-pressure oil 10 are obtained through separation, the high-pressure oil 10 enters a stripping tower T1, a second gas phase 11 and stripping tower bottom oil 12 are stripped, the stripping tower bottom oil 12 is sent to an atmospheric distillation tower T2 to obtain a third gas phase 13 (the distillation range is 40-80 ℃), a hydrogen-supplying agent 15 (the distillation range is 80-140 ℃), a light oil product 16 (the distillation range is 140-350 ℃) and an atmospheric tower bottom oil 20 (the distillation range is more than 350 ℃), the atmospheric tower bottom oil 20 enters a reduced pressure distillation tower T3, the fourth gas phase 21 (the distillation range is 40-120 ℃), a heavy oil product 22 (the distillation range is 350-520 ℃) and unconverted oil 23 containing catalyst oil are obtained through further distillation under the condition of 7mmHg, 95% of the unconverted oil 23 containing catalyst is returned to the inlet of a feeding pump P1, and the unconverted oil 24 containing catalyst is sent to be further processed.
The hydrogen supply agent 15 after hydrogen supply is mixed with the hydrogen 14, heated by a reaction feed heating furnace F2 and then enters a hydrogenation reactor R2, hydrogenation reaction is carried out for 0.5h under the conditions of 200 ℃ and 2MPa, the regenerated hydrogen supply agent 19 with the concentration of 40t/h in the reaction product returns to the inlet of a feed pump P1, the rest of the hydrogen supply agent 18 is taken as external light fraction oil to be sent out of a boundary zone, and the weight ratio of the regenerated hydrogen supply agent 19 to the external light fraction oil is 9:1.
Example 2
The method for treating heavy feedstock oil is the same as in example 1, except that the reaction conditions for the hydrogenation reaction include: the reaction temperature is 425 ℃, the reaction pressure is 70bar, the reaction time is 1h, and the mass ratio of the hydrogen donor to the raw oil is 0.3:1.
Example 3
The method for treating heavy feedstock oil is the same as in example 1, except that the reaction conditions for the hydrogenation reaction include: the reaction temperature is 425 ℃, the reaction pressure is 70bar, the reaction time is 1h, and the mass ratio of the hydrogen donor to the raw oil is 0.2:1.
Example 4
The method for treating heavy feedstock oil is the same as in example 1, except that the reaction conditions for the hydrogenation reaction include: the reaction temperature is 425 ℃, the reaction pressure is 70bar, the reaction time is 1h, and the mass ratio of the hydrogen donor to the raw oil is 0.1:1.
Comparative example 1
The raw oil and the catalyst are respectively boosted and heated and then mixed, hydrogen is compressed by a new hydrogen compressor and heated by a hydrogen heating furnace, and then mixed with the raw oil and the catalyst and enters a slurry bed reactor, the reaction pressure is 18MPag, and the reaction temperature is 430 ℃. The hydrogen partial pressure was 11MPag, and the catalyst to oil ratio was 200ppm.
Table 2 product properties of examples and comparative examples
From a comparison of the data in examples 1-4 and comparative example 1, as shown in Table 2, it can be seen that the conversion of the reaction can be improved using the methods and systems described in the present disclosure. As is clear from the comparison of the data in examples 1 to 4, the reaction effect is good when the mass ratio of the hydrogen donor to the raw oil is preferably 0.3 to 1.
The preferred embodiments of the present disclosure have been described in detail above with reference to the accompanying drawings, but the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solutions of the present disclosure within the scope of the technical concept of the present disclosure, and all the simple modifications belong to the protection scope of the present disclosure.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations are not described further in this disclosure in order to avoid unnecessary repetition.
Moreover, any combination between the various embodiments of the present disclosure is possible as long as it does not depart from the spirit of the present disclosure, which should also be construed as the disclosure of the present disclosure.
Claims (10)
1. A method of treating heavy feedstock oil, the method comprising:
the raw oil, the catalyst and the hydrogen supply agent are contacted in a slurry bed reactor to carry out hydrogenation reaction, so as to obtain a hydrogenation reaction product;
the hydrogenation reaction product is subjected to hot high-pressure separation and cold high-pressure separation to obtain a first gas phase and high-fraction oil;
subjecting the high-fraction oil to steam stripping treatment to obtain a second gas phase and steam stripping bottom oil;
performing atmospheric distillation on the stripping tower bottom oil to obtain a third gas phase, a hydrogen donor after hydrogen supply, a light oil product and atmospheric tower bottom oil;
subjecting the atmospheric bottoms to reduced pressure distillation to obtain a fourth gas phase, a heavy oil product, and unconverted oil containing catalyst; returning a portion of said unconverted oil to said slurry bed reactor for continued reaction;
sending the hydrogen donor and hydrogen after hydrogen supply into a hydrogen donor regeneration unit for hydrogenation regeneration treatment to obtain a regenerated hydrogen donor; and returning part of the regenerated hydrogen supply agent to the slurry bed reactor for recycling, and sending the other part of the regenerated hydrogen supply agent out of the system as a light fraction.
2. The method according to claim 1, wherein the raw oil is one or more selected from the group consisting of atmospheric residuum, vacuum wax oil, coker wax oil, deasphalted oil and coal tar;
the hydrogen donor is one or more selected from cyclohexane, methylcyclohexane, decalin and cyclohexadiene;
the catalyst is an oil-soluble organic homogeneous molybdenum catalyst and/or a supported nickel-molybdenum ultrafine powder catalyst.
3. The method according to claim 1, wherein the reaction conditions of the hydrogenation reaction comprise: the reaction temperature is 150-450 ℃, the reaction pressure is 5-70 bar, the reaction time is 0.5-10 h, and the mass ratio of the hydrogen donor to the raw oil is below 2; preferably 1 or less.
4. The method according to claim 1, further comprising, before entering the slurry bed reactor, pressurizing a mixed raw material obtained by mixing raw material oil, a catalyst and a hydrogen donor to 0.5 to 7MPa, exchanging heat with the hydrogenation reaction product, and then heating to 150 to 450 ℃;
optionally, the stripping medium of the stripping treatment is steam.
5. The method of claim 1, wherein the third gas phase has a temperature cut point of the hydrogen donor after hydrogen donor of 40 to 80 ℃, a temperature cut point of the hydrogen donor after hydrogen donor and the light oil product of 130 to 160 ℃, and a temperature cut point of the light oil product and the atmospheric bottom oil of 300 to 360 ℃;
the temperature cut point of the fourth gas phase and the heavy oil product is 300-360 ℃, and the temperature cut point of the heavy oil product and the unconverted oil is 480-540 ℃.
6. The process according to claim 1, characterized in that the ratio of the part of unconverted oil returned to the slurry bed reactor to the total weight of unconverted oil is 1 or less, preferably 0.8 or less;
the ratio of the part of the regenerated hydrogen-donor returned to the slurry bed reactor to the total weight of the regenerated hydrogen-donor is 0.2 to 1, preferably 0.8 to 1.
7. The method of claim 1, wherein the conditions of the hydroprocessing include: the reaction temperature is 150-250 ℃, the reaction pressure is 0.5-5MPa, the reaction time is 0.1-1 h, and the volume ratio of the hydrogen to the hydrogen donor after hydrogen supply is 10-300:1.
8. A system for treating heavy raw oil, which is characterized by comprising a hydrogenation reaction unit, a high-pressure separation unit, a stripping unit, an atmospheric distillation unit, a reduced pressure distillation unit and a hydrogen supply agent regeneration unit;
the hydrogenation reaction unit comprises a slurry bed reactor, a raw oil inlet, a catalyst inlet, a hydrogen supply agent inlet and a hydrogenation reaction product outlet;
the high-pressure separation unit comprises a hydrogenation reaction product inlet, a first gas phase outlet and a high-pressure oil separation outlet;
the stripping unit comprises a high-pressure oil inlet, a stripping medium inlet, a second gas phase outlet and a stripping tower bottom oil outlet;
the atmospheric distillation unit comprises an atmospheric distillation tower; the atmospheric distillation tower comprises a stripping tower bottom oil inlet, a third gas phase outlet, a hydrogen supply agent outlet after hydrogen supply, a light oil product outlet and an atmospheric tower bottom oil outlet;
the reduced pressure distillation unit comprises a reduced pressure distillation tower; the reduced pressure distillation column comprises an atmospheric bottom oil inlet, a fourth gas phase outlet, a heavy oil product outlet and an unconverted oil outlet;
the hydrogen supply agent regeneration unit comprises a hydrogenation reactor; the hydrogenation reactor comprises a hydrogen supply agent inlet, a hydrogen inlet and a regenerated hydrogen supply agent outlet after hydrogen supply;
wherein, the hydrogenation reaction product outlet of the hydrogenation reaction unit is communicated with the hydrogenation reaction product inlet of the high-pressure separation unit through a hydrogenation reaction product pipeline; the high-pressure separation unit is communicated with the stripping unit through a high-pressure oil inlet; the stripping bottom oil outlet of the stripping unit is communicated with the stripping bottom oil inlet of the atmospheric distillation tower; the atmospheric bottom oil outlet of the atmospheric distillation tower is communicated with the atmospheric bottom oil inlet of the vacuum distillation tower; the unconverted oil outlet of the reduced pressure distillation tower is communicated with the raw oil inlet of the hydrogenation reaction unit; the hydrogen supply agent outlet after hydrogen supply of the atmospheric distillation tower is communicated with the hydrogen supply agent inlet after hydrogen supply of the hydrogen supply agent regeneration unit; the regenerated hydrogen supply agent outlet of the hydrogen supply agent regeneration unit is communicated with the hydrogen supply agent inlet of the hydrogenation reaction unit.
9. The system of claim 8, wherein the hydrogenation reaction unit further comprises a feed line, a feed pump, a feed heat exchanger and a reaction feed heating furnace in that order in terms of feed flow direction;
the feed pipeline is provided with the raw oil inlet, the catalyst inlet and the hydrogen supply agent inlet, the outlet of the feed pump is communicated with the cold medium side inlet of the feed heat exchanger, the cold medium side outlet of the feed heat exchanger is communicated with the inlet of the reaction feed heating furnace, and the outlet of the reaction feed heating furnace is communicated with the raw material inlet of the slurry bed reactor;
optionally, the heat medium side of the feed heat exchanger is in communication with the hydrogenation reaction product line.
10. The system of claim 8, wherein the unconverted oil outlet line of the vacuum distillation column splits into two streams, one stream being in communication with the feed oil inlet of the slurry bed reactor and the other stream being sent out of the system;
the regenerated hydrogen supply agent outlet pipeline of the hydrogen supply agent regeneration unit is divided into two parts, one part is communicated with the hydrogen supply agent inlet of the slurry bed reactor, and the other part is sent out of the system.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106147846A (en) * | 2015-04-14 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of inferior heavy oil and/or the processing method of poor residuum |
| KR20200049260A (en) * | 2018-10-31 | 2020-05-08 | 단국대학교 산학협력단 | Method of upgrading extra-heavy oil using hydrogen donor solvent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106147846A (en) * | 2015-04-14 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of inferior heavy oil and/or the processing method of poor residuum |
| KR20200049260A (en) * | 2018-10-31 | 2020-05-08 | 단국대학교 산학협력단 | Method of upgrading extra-heavy oil using hydrogen donor solvent |
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