CN102453498B - Shutdown method for heavy oil suspension bed hydrogenation process - Google Patents
Shutdown method for heavy oil suspension bed hydrogenation process Download PDFInfo
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- CN102453498B CN102453498B CN201010522189.2A CN201010522189A CN102453498B CN 102453498 B CN102453498 B CN 102453498B CN 201010522189 A CN201010522189 A CN 201010522189A CN 102453498 B CN102453498 B CN 102453498B
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Abstract
The invention discloses a shutdown method for a heavy oil suspension bed hydrogenation process. The method comprises the following steps of: after normal running of a device ends, stopping feeding raw oil; completely sweeping raw materials in the entire device and a physical flow left after a reaction with hot gas; lowering a reaction temperature to below 350 DEG C; lowering the pressure of the device to below 2MPa; feeding a distillate oil pump into the device for cleaning; cleaning at a constant temperature for a certain time interval; stopping feeding oil; increasing a gas sweeping amount; completely sweeping distillate oil for a washing device; stopping gas sweeping; lowering the temperature of the device to the normal temperature; and shutting down. Compared with the conventional suspension bed shutdown process, a shutdown operating process in the invention has the advantages of simplified operation, shortened shutdown time and contribution to saving shutdown time and saving operating cost.
Description
Technical field
The present invention relates to a kind of shut-down method of floating bed hydrogenation treatment process.Be particularly useful for the shut-down method of heavy oil floating bed hydrogenation technique under high top pressure operation condition.
Background technology
Along with the variation of petroleum products demand structure in the Devoting Major Efforts To Developing of heavy crude and world wide, market maintains sustained and rapid growth and rapid minimizing to heavy fuel oil (HFO) demand to light-weight fuel oil demand, and the deep process technology of heavy oil has become the emphasis of petroleum refining industry's exploitation.It is wide that suspension bed heavy-oil hydrogenation technology has adaptability to raw material, and the features such as flexible operation are one of important means of processing inferior heavy oil raw material.The structure of reactor of floating bed hydrogenation is simple, conventionally uses empty cylinder or has the reactor of simple inner member (as Thermal couple casing pipe etc.).Floating bed hydrogenation technology and fixed bed and boiling bed hydrogenation technology have very large difference, under normal circumstances, in suspended-bed reactor, there is no fixing beds, the catalyzer of hydrogenation reaction and raw material pass in and out reactor simultaneously, so the shut-down of floating bed hydrogenation device can have very large flexibility of operation.
The shut-down process more complicated of traditional heavy oil fixed bed or boiling bed hydrogenation, due to part or all of hydrogenation catalyst being housed in reactor, so in device shut-down process, conventionally keeping under the working pressure of 12～20MPa high pressure, temperature of reactor is down to after certain temperature, pass into residual oil in wax oil raw material displacement apparatus the catalyzer after cleaning reaction, after constant temperature cleans and finishes, temperature of reaction is further reduced, pass into again diesel oil washing catalyst, when the reaction bed temperature in reactor is down to after 200～150 ℃, stop into diesel oil, then cooling, after release, draw off the catalyzer in reactor.And the shut-down process of suspension bed residual oil hydrogenation device has no report, conventionally operate according to the shut-down process of fixed bed residual oil processing.And suspension bed residual oil hydrogenation is different with boiling bed residual oil hydrogenation process from fixed bed, owing to there is no catalyzer in reactor, catalyzer is suspended in raw material with it in-out apparatus simultaneously, so the shut-down process of suspension bed residual oil hydrogenation is washing unit, and the shut-down process of fixed bed and boiling bed residual oil hydrogenation is mainly cleaning catalyst, catalyzer is easily drawn off from reactor.So should, according to the feature of suspension bed technology, adopt shut-down scheme correspondingly, while both saving, economize wealth, can give prominence to again the advantage of this technology.
CN96102880.7 has introduced and in heavy residual oil, has pressed floating bed hydrogenation method for transformation.In this patent, just introduce under certain operational condition, adopt molybdenum, nickel active metal to carry out the conversion of suspension bed heavy-oil hydrogenation, do not emphasize the shut-down process of this technique, illustrate that it is just with reference to traditional fixed bed shut-down process, keep the operational condition of high pressure constant, temperature of reactor is reduced to after certain temperature, adopt respectively wax oil and diesel oil cleaning reaction device, then use hydrogen purge device, telegram in reply release is stopped work.This technological process more complicated, and less than the technical superiority of giving full play to suspension bed according to the feature of floating bed hydrogenation reaction unit.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of shut-down method of heavy oil floating bed hydrogenation technique, the inventive method combines with suspension bed process characteristic, has given full play to the advantage of this technique, has advantage simple to operate, cost-saving.
The shut-down method of heavy oil floating bed hydrogenation technique of the present invention comprises the steps:
After a, device reaction finish, stop into heavy oil feedstock, strengthen gas circulation amount, temperature of reactor is down to 380～350 ℃ simultaneously;
B, system pressure is down to the working pressure lower than 2MPa, then distillate is pumped into reactor and carries out constant temperature cleaning;
C, constant temperature stop oil-feed after cleaning and finishing, and keep atm number to purge, and temperature of reactor are down to room temperature simultaneously, and Pressure Drop, to normal pressure, is stopped work and finished.
Gas described in step a can be dry gas or its mixture that hydrogen, nitrogen, helium, Sweet natural gas, coal gas or reaction generate, and when total gas circulation amount is unit normal run 2～10 times of hydrogen recycle amount, purge time is 1～10 hour.The cooling rate of reactor described in step a is 5～30 ℃/h.
In step b, said distillate is any narrow fraction of boiling range between 200～450 ℃, as the cut wet goods of this boiling range scope of suspension bed residual oil hydrogenation generation.The volume space velocity that passes into distillate is 0.2～15h
-1, be preferably 1～10h
-1, constant temperature scavenging period is 5～50 hours.
The cooling rate of reactor described in step c is 5～30 ℃/h.Described gas can be dry gas or its mixture that hydrogen, nitrogen, helium, Sweet natural gas or reaction generate, and wherein when installing the gas flow of purging and be unit normal run 2～10 times of hydrogen recycle amount, purge time is 1～10 hour.
With the shut-down method comparison of the suspended-bed reactor of introducing in prior art, shut-down method of the present invention has the following advantages:
1, adopt after gas purging device, under low pressure use the shut-down scheme of heavy oil fraction oil washing unit and gas purging distillate, be different from conventional device cooling, heavy distillate and benzoline cleaning and gas purging scheme of under high pressure carrying out completely, given prominence to suspension bed technological operation feature flexibly.
2, after device normal operation finishes, stop into heavy oil feedstock, add atm number blow device, reduce temperature of reactor simultaneously, the heavy oil in device can be discharged as early as possible, shorten stoppage time.
3, adopt take high-low pressure gas purging as main in the shut-down stage, in conjunction with the device shut-down scheme of low pressure distillate washing, be conducive to suspension bed technique take washing unit as main shut-down process, can save stoppage time and running cost.
Embodiment
Further illustrate by the following examples technical scheme of the present invention and effect.
Embodiment 1
The present embodiment is heavy oil floating bed hydrogenation device shut-down method.Specific operation process is: after unit normal run finishes, stop into heavy oil feedstock, keeping, under the precursor of original hydrogen recycle amount, passing into coal gas, while making total gas circulation amount be unit normal run 3 times of hydrogen recycle amount, with the speed of 20 ℃/h, temperature of reactor is down to 350 ℃ simultaneously, after constant temperature gas purging 5 hours, system pressure is down to 1MPa, opens oil pump, the floating bed hydrogenation distillate that is pumped into 200～350 ℃ carries out constant temperature cleaning, and air speed is 4h
-1, device cleaned after 35 hours, stopped into distillate, and when total air input is increased to unit normal run, 10 of hydrogen recycle amount times are continued to purge 4 hours, then stop the supple of gas or steam, step-down, telegram in reply, the normal shut-down of finishing device.
Embodiment 2
According to the method described in embodiment 1, the present embodiment is heavy oil floating bed hydrogenation device shut-down method.Specific operation process is: after unit normal run finishes, stop into heavy oil feedstock, keeping, under the precursor of original hydrogen recycle amount 1/3, passing into Sweet natural gas, while making total gas circulation amount be unit normal run 2 of hydrogen recycle amount, with the speed of 20 ℃/h, temperature of reactor is down to 300 ℃ simultaneously, after constant temperature gas purging 6 hours, system pressure is down to 2MPa, opens oil pump, the floating bed hydrogenation distillate that is pumped into 240～350 ℃ carries out constant temperature cleaning, and air speed is 6h
-1, device cleaned after 30 hours, stopped into distillate, and when total air input is increased to unit normal run, 6 of hydrogen recycle amount times are continued to purge 5 hours, then stop the supple of gas or steam, step-down, telegram in reply, the normal shut-down of finishing device.
Embodiment 3
According to the method described in embodiment 1, the present embodiment is heavy oil floating bed hydrogenation device shut-down method.Specific operation process is: after unit normal run finishes, stop into heavy oil feedstock, switch gas-phase feed is Sweet natural gas simultaneously, while making gas circulation amount be unit normal run 5 times of hydrogen recycle amount, with the speed of 20 ℃/h, temperature of reactor is down to 320 ℃ simultaneously, gas purging is after 3 hours, system pressure is down to 0.6MPa, open oil pump, the floating bed hydrogenation distillate that is pumped into 200～350 ℃ carries out constant temperature cleaning, and air speed is 8h
-1, device cleaned after 20 hours, stopped into distillate, continued to keep gas purging 6 hours, then stop the supple of gas or steam, step-down, telegram in reply, and the normal shut-down of finishing device.
Claims (9)
1. a shut-down method for heavy oil floating bed hydrogenation technique, comprises the steps:
After a, device reaction finish, stop into heavy oil feedstock, strengthen gas circulation amount, when gas circulation amount is unit normal run 2～10 of hydrogen recycle amount times, temperature of reactor is down to 380～350 ℃ simultaneously;
B, system pressure is down to the working pressure lower than 2MPa, then distillate is pumped into reactor and carries out constant temperature cleaning;
C, constant temperature stop oil-feed after cleaning and finishing, and keep atm number to purge, and while being unit normal run for installing the gas flow of purging 2～10 times of hydrogen recycle amount, temperature of reactor is down to room temperature simultaneously, Pressure Drop, to normal pressure, is stopped work and is finished.
2. according to shut-down method claimed in claim 1, it is characterized in that, the gas described in step a is dry gas or its mixture that hydrogen, nitrogen, helium, Sweet natural gas, coal gas or reaction generate.
3. according to shut-down method claimed in claim 1, it is characterized in that, the gas purging time in step a is 1～10 hour.
4. according to shut-down method claimed in claim 1, it is characterized in that, the cooling rate of reactor described in step a is 5～30 ℃/h.
5. according to shut-down method claimed in claim 1, it is characterized in that, the distillate described in step b is any narrow fraction of boiling range between 200～450 ℃.
6. according to shut-down method claimed in claim 5, it is characterized in that, the distillate described in step b is the distillate that suspension bed residual oil hydrogenation generates.
7. according to shut-down method claimed in claim 1, it is characterized in that, the volume space velocity that passes into distillate in step b is 0.2～15h
-1, constant temperature scavenging period is 5～50 hours.
8. according to shut-down method claimed in claim 1, it is characterized in that, the cooling rate of reactor described in step c is 5～30 ℃/h.
9. according to shut-down method claimed in claim 1, it is characterized in that, in step c, the time of gas purging is 1～10 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010522189.2A CN102453498B (en) | 2010-10-15 | 2010-10-15 | Shutdown method for heavy oil suspension bed hydrogenation process |
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| CN201010522189.2A CN102453498B (en) | 2010-10-15 | 2010-10-15 | Shutdown method for heavy oil suspension bed hydrogenation process |
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| CN102453498B true CN102453498B (en) | 2014-05-21 |
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| CN104611012B (en) * | 2013-11-05 | 2016-08-17 | 中国石油化工股份有限公司 | A kind of shut-down method of fixed bed residual hydrogenation equipment |
| CN108102689B (en) * | 2016-11-25 | 2019-12-13 | 中国石油化工股份有限公司 | Shutdown method of coal tar hydrogenation process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005026292A1 (en) * | 2003-09-18 | 2005-03-24 | Eni S.P.A. | Process for the running of a reactor suitable for heterogeneous reactions combined with reactions taking place in three-phase systems |
| CN101089139A (en) * | 2006-06-16 | 2007-12-19 | 中国石油化工股份有限公司 | Shut-down method of coal tar hydrotreating process |
| CN101418231A (en) * | 2007-10-26 | 2009-04-29 | 中国石油化工股份有限公司 | A kind of shut-down method of bubbling bed hydrotreating process |
| CN101838548A (en) * | 2010-05-08 | 2010-09-22 | 何巨堂 | Emergency shutdown method for hydrocarbon hydrogenation process |
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2010
- 2010-10-15 CN CN201010522189.2A patent/CN102453498B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005026292A1 (en) * | 2003-09-18 | 2005-03-24 | Eni S.P.A. | Process for the running of a reactor suitable for heterogeneous reactions combined with reactions taking place in three-phase systems |
| CN101089139A (en) * | 2006-06-16 | 2007-12-19 | 中国石油化工股份有限公司 | Shut-down method of coal tar hydrotreating process |
| CN101418231A (en) * | 2007-10-26 | 2009-04-29 | 中国石油化工股份有限公司 | A kind of shut-down method of bubbling bed hydrotreating process |
| CN101838548A (en) * | 2010-05-08 | 2010-09-22 | 何巨堂 | Emergency shutdown method for hydrocarbon hydrogenation process |
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