CN108285809B - Start-up method of double series Fischer-Tropsch reaction device - Google Patents
Start-up method of double series Fischer-Tropsch reaction device Download PDFInfo
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- 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
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Abstract
A method for starting a double series Fischer-Tropsch reaction device comprises the following steps: adding heavy diesel oil into a single synthesis reactor, adding the iron-based catalyst prepared by a reduction system into the synthesis reactor after reaching a certain amount, gradually starting the double-series Fischer-Tropsch reaction device, pressing half of the mixed materials in the synthesis reactor into the other synthesis reactor when the reactors are operated at full load, so that the loads of the two synthesis reactors reach 50% or more, and respectively supplementing the catalysts into the two synthesis reactors through the reduction reactors until the two catalysts are operated at full load. According to the invention, by changing the original start scheme of the two series of Fischer-Tropsch synthesis devices, the original start raw materials are saved, the low-load operation time of the Fischer-Tropsch reactor is shortened, the overall start time is shortened, the two Fischer-Tropsch reaction systems reach more than 50% of load in a short time and stably operate, the start cost is saved, and the economic benefit is rapidly created.
Description
Technical Field
The invention belongs to the field of chemical equipment, and particularly relates to a starting method of a double-series Fischer-Tropsch reaction device.
Background
The domestic Fischer-Tropsch synthesis industrialization device is built and put into production in 2009 successively, and enterprises such as inner Mongolia Guita coal oil production Limited liability company and Shanxi Lu coal-based synthetic oil Limited company are provided, the scale is 16-18 ten thousand tons per year, and the enterprises are single/set reaction systems. The megaton Fischer-Tropsch synthesis device is built for starting from 2016 to 2017, and is respectively a 400-ten-thousand-ton/year coal-to-oil and 120-ten-ton/year fine chemical demonstration project of inner Mongolia Guyitai chemical company, and the megaton project of the Luan group is about to start. The megaton grade Fischer-Tropsch synthesis devices are two series or multiple series Fischer-Tropsch synthesis reaction systems, and are different from single series Fischer-Tropsch synthesis devices in start-up. The device can be driven quickly to reach full load, and the driving cost is saved, which is a subject to be researched and solved by each enterprise.
The design capacity of a million-ton grade Fischer-Tropsch reaction system slurry bed reactor is 50 ten thousand tons per year, and the 120 ten thousand tons per year fine chemical demonstration project of the inner Mongolia Guyitai chemical industry finite responsibility company is two sets of Fischer-Tropsch reaction systems. The conventional two-series Fischer-Tropsch synthesis reactor start scheme is that a certain amount of start oil is added into a Fischer-Tropsch synthesis reactor, a reduced iron-based catalyst is waited to be added into a synthesis reaction system under certain temperature and pressure, the two reactors are started in sequence, because the two synthesis reactors are provided with one reduction reactor, and the calculation is carried out according to the design scale of the reduction reactor, the maximum load of the reduction reactor runs, the reduction is required for 3-4 times at least, and the load of a single synthesis reactor can reach the catalyst dosage required by full load. And the two reactors are started in sequence, the two reactors respectively run with the load of less than 50 percent once, the low-load operation of the Fischer-Tropsch slurry bed reactor is very unfavorable for the system, and a series of defects of product non-continuous delivery, system blockage and the like are easily caused.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a method for starting up a two-train fischer-tropsch reactor, so as to solve at least one of the above problems.
The invention is realized by the following technical scheme:
the invention provides a method for starting a double-series Fischer-Tropsch reaction device, which comprises the following steps:
two synthesis reactors connected in series;
the gasification furnace is connected with the two synthesis reactors and provides feed gas for reaction; and
and the reduction reactor is connected with the two synthesis reactors and provides a catalyst for the reaction.
The driving method comprises the following steps:
(1) adding heavy diesel oil into the first synthesis reactor;
(2) after feeding is completed, the pressure of the first synthesis reactor is increased to 1.5-2.0MPa, heavy diesel oil is supplemented by a heavy diesel oil feeding pump, and the liquid level of the first synthesis reactor is maintained at 55-65%;
(3) when the gas production of the gasification furnace reaches 20 multiplied by 104Nm3After the reaction time is more than h, heating the first synthesis reactor to 230-250 ℃, and pressing a catalyst into the first synthesis reactor by the reduction reactor;
(4) when the load of the first synthesis reactor reaches 100%, dividing the mixed material in the first synthesis reactor into half parts to the second synthesis reactor, and then dividing the produced gas of the gasification furnace into half parts respectively to the first synthesis reactor and the second synthesis reactor;
(5) both synthesis reactors were gradually increased from 50% load to 100% load.
Preferably, the two-series Fischer-Tropsch reaction is subjected to a gas tightness check prior to step (1).
Preferably, in the step (2), the pressure increasing rate of the first synthesis reactor is less than or equal to 0.5 MPa/h.
Preferably, in the step (3), the temperature rising rate of the first synthesis reactor is less than or equal to 5 ℃/h.
Preferably, the catalyst is an iron-based catalyst.
According to the technical scheme, the starting method of the double-series Fischer-Tropsch reaction device has the following beneficial effects:
(1) the invention saves the consumption of the heavy diesel oil for driving and the driving cost.
(2) The invention reduces the low-load running time of the Fischer-Tropsch synthesis reactor to the minimum, reduces the difficulty of the low-load operation of the Fischer-Tropsch synthesis reactor, reduces the difficulty of the operation of operators and lightens the influence of the low-load operation on the system.
(3) The invention ensures the consistency of the content and the activity of the catalyst in the two reactors, provides convenience for the on-line replacement of the catalyst in the later period, reduces the difficulty, ensures the consistency of products of the two reactors and ensures the product quality.
Drawings
FIG. 1 is a schematic diagram of a two series Fischer-Tropsch reactor in an embodiment of the invention;
[ description of reference ]
1-a reduction reactor; 2-a first synthesis reactor;
3-a second synthesis reactor; 4-dewaxing filtration unit.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
A method for starting a double series Fischer-Tropsch reaction device comprises the following steps: adding heavy diesel oil into a single synthesis reactor, adding the iron-based catalyst prepared by a reduction system into the synthesis reactor after reaching a certain amount, gradually starting the double-series Fischer-Tropsch reaction device, pressing half of the mixed materials in the synthesis reactor into the other synthesis reactor when the reactors are operated at full load, so that the loads of the two synthesis reactors reach 50% or more, and respectively supplementing the catalysts into the two synthesis reactors through the reduction reactors until the two catalysts are operated at full load. According to the invention, by changing the original start scheme of the two series of Fischer-Tropsch synthesis devices, the original start raw materials are saved, the low-load operation time of the Fischer-Tropsch reactor is shortened, the overall start time is shortened, the two Fischer-Tropsch reaction systems reach more than 50% of load in a short time and stably operate, the start cost is saved, and the economic benefit is rapidly created.
Specifically, the invention provides a method for starting a double series Fischer-Tropsch reaction device, which comprises the following steps: two synthesis reactors connected in series; the gasification furnace is connected with the two synthesis reactors and provides feed gas for reaction; and a reduction reactor connected with the two synthesis reactors for providing catalyst for reaction.
The driving method comprises the following steps:
(1) adding heavy diesel oil into the first synthesis reactor;
(2) after the feeding is finished, boosting the pressure of the first synthesis reactor to 1.5-2.0MPa, supplementing heavy diesel oil by using a heavy diesel oil feeding pump, and maintaining the liquid level of the first synthesis reactor at 55-65%;
(3) when the gas production of the gasification furnace reaches 20 multiplied by 104Nm3After the reaction time is more than h, heating the first synthesis reactor to 230-250 ℃, and pressing a catalyst into the first synthesis reactor by the reduction reactor;
(4) when the load of the first synthesis reactor reaches 100%, dividing the mixed material in the first synthesis reactor into half parts to the second synthesis reactor, and then dividing the produced gas of the gasification furnace into half parts respectively to the first synthesis reactor and the second synthesis reactor;
(5) both synthesis reactors were gradually increased from 50% load to 100% load.
A check of gas tightness was carried out on the two-series Fischer-Tropsch reaction batch before step (1).
In the step (2), the pressure increasing rate of the first synthesis reactor is less than or equal to 0.5 MPa/h.
In the step (3), the heating rate of the first synthesis reactor is less than or equal to 5 ℃/h.
The catalyst is an iron-based catalyst.
The method for operating a two-series Fischer-Tropsch reactor according to the present invention will be described in further detail with reference to the following specific examples and the accompanying drawings.
Examples
A method for starting a double series Fischer-Tropsch reaction device. FIG. 1 is a schematic diagram of a two-series Fischer-Tropsch reaction apparatus according to an embodiment of the present invention. As shown in fig. 1, includes a reduction reactor 1, a first synthesis reactor 2, a second synthesis reactor 3, and a dewaxing filtering unit 4. Wherein, the two synthesis reactors are connected in series; the gasification furnace is connected with the two synthesis reactors and provides feed gas for reaction; and the reduction reactor is connected with the two synthesis reactors and provides a catalyst for the reaction.
The starting method of the double series Fischer-Tropsch reaction device comprises the following steps:
(1) and introducing nitrogen into the two series of Fischer-Tropsch reaction devices, and carrying out air tightness test.
(2) Reducing the pressure to 0.5MPa, and starting a circulating gas compressor.
(3) And starting a steam drum heating system.
(4) And heating the synthesis reaction device to 245-255 ℃, and boosting the pressure to 2.0 MPa. The heating rate is less than or equal to 5 ℃/h, and the pressure rise rate is less than or equal to 0.5 MPa/h. And when the pressure of the system is stabilized at 1.8-2.2 MPa, debugging a back flushing system and a wax outlet system, pumping out the wax outlet system of the reactor to a stripping tower process, and establishing liquid phase circulation of a tail gas decarburization unit.
(5) And (3) keeping the temperature of the synthesis reaction device at 245-255 ℃ for 24 hours, checking the thermal expansion condition of the reactor, the pipeline and the support and hanger condition, checking the system leakage, and ensuring that the hot nitrogen circulation continuous operation of the synthesis circulation gas compressor meets 72 hours.
(6) And (3) depressurizing the synthesis reaction device to 0.35-0.5 MPa, and performing system hot-pressing.
(7) And cooling the synthesis reaction device to 115-125 ℃, wherein the cooling rate is less than or equal to 5 ℃/h, and preparing to start the heavy diesel.
(8) Before the heavy firewood is introduced, the oil-water separator and the stripping tower have the operating conditions. Leading about 250-270 tons of heavy diesel oil to a synthesis reactor through a middle tank area to a heavy diesel oil reducing pipeline, and continuously adding about 590-610 tons of start-up heavy diesel oil when the temperature is raised to 150 ℃.
(9) And after the material pressing of the start-up reactor is finished, the system starts to boost pressure. And boosting the pressure to 1.8-2.2 MPa, and starting to heat the system at a heating rate of less than or equal to 5 ℃/h. And (4) heating to the circulating heat exchange separator and the light oil separator to establish liquid levels, and carrying out system oil combined transportation and instrument debugging. The hot nitrogen combined transportation of the wax outlet system of the reactor is already debugged, and the debugging is not needed at the moment. And (3) supplementing the heavy firewood by using a heavy firewood supplementing pump, and maintaining the liquid level of the reactor at about 60%. And when the pressure of the system is stabilized at 1.8-2.2 MPa, the tail gas decarbonization unit establishes liquid phase circulation.
(10) And carrying out synthesis gas isobaric replacement, wherein the total sulfur content of the synthesis gas is controlled to be less than or equal to 0.05ppm in the synthesis gas replacement process. In the displacement process, the synthesis gas H is adjusted2The ratio of/CO is 1.62-1.68; after the synthesis gas is qualified by replacement, the pressure of the synthesis reaction device is increased to 2.72-2.78 MPa, and the pressure increasing rate is 0.5 MPa/h; and (3) supplementing the heavy firewood by using a heavy firewood supplementing pump, and maintaining the liquid level of the reactor at about 60%.
(11) After the gasification feeding and gas production, the synthesis gas simultaneously satisfies 20 multiplied by 104Nm3And (4) raising the temperature of the synthesis reaction device to 230-250 ℃ according to the requirement of the temperature of the synthesis reaction device, pressing the catalyst to the synthesis system by the reduction system, and starting the Fischer-Tropsch synthesis reaction device.
(12) When the start-up series reaches 100% (or 120%) load, the catalyst slurry of the start-up series is divided into half by a No. 3 discharge line to the standby start-up series, and the two series respectively half feed the purified gas generated by gasification.
(13) The two series were stepped up from 50% (or 60%) load to over 100% load.
In conclusion, the original start scheme of the double-series Fischer-Tropsch synthesis device is changed, so that the original start raw materials are saved, the low-load operation time of the Fischer-Tropsch reactor is shortened, the overall start time is shortened, the two Fischer-Tropsch reaction systems reach more than 50% of load in a short time and stably operate, the start cost is saved, and the economic benefit is quickly created. .
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method of starting up a two series fischer-tropsch reaction plant, the two series fischer-tropsch reaction plant comprising:
two synthesis reactors connected in series;
the gasification furnace is connected with the two synthesis reactors and provides feed gas for reaction; and
a reduction reactor connected with the two synthesis reactors for providing catalyst for reaction;
the driving method comprises the following steps:
(1) adding heavy diesel oil into the first synthesis reactor;
(2) after feeding is completed, the pressure of the first synthesis reactor is increased to 1.5-2.0MPa, heavy diesel oil is supplemented by a heavy diesel oil feeding pump, and the liquid level of the first synthesis reactor is maintained at 55-65%;
(3) when the gas production of the gasification furnace reaches 20 multiplied by 104Nm3After the reaction time is more than h, heating the first synthesis reactor to 230-250 ℃, and pressing a catalyst into the first synthesis reactor by the reduction reactor;
(4) when the load of the first synthesis reactor reaches 100%, dividing the mixed material in the first synthesis reactor into half parts to the second synthesis reactor, and then dividing the produced gas of the gasification furnace into half parts respectively to the first synthesis reactor and the second synthesis reactor;
(5) both synthesis reactors were gradually increased from 50% load to 100% load.
2. Method for the start-up of a dual series fischer-tropsch reaction plant according to claim 1, characterized in that the dual series fischer-tropsch reaction is subjected to a gas tightness check prior to step (1).
3. The method for starting up a two-series Fischer-Tropsch reactor according to claim 1, wherein in the step (2), the pressure increase rate of the first synthesis reactor is less than or equal to 0.5 MPa/h.
4. The start-up method for a dual-series Fischer-Tropsch reaction device according to claim 1, wherein, in the step (3), the temperature rise rate of the first synthesis reactor is less than or equal to 5 ℃/h.
5. Method for the start-up of a dual series fischer-tropsch reactor according to claim 1, wherein the catalyst is an iron based catalyst.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002096834A2 (en) * | 2001-05-25 | 2002-12-05 | Bp Exploration Operating Company Limited | Fischer-tropsch process |
| CN101687832A (en) * | 2007-05-08 | 2010-03-31 | 巴斯夫欧洲公司 | Be used to prepare the method for alkene oxide |
| CN102863982A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Work starting method for slurry bed Fisher-Tropsch synthesis |
| CN103007835A (en) * | 2011-09-22 | 2013-04-03 | 中国石油化工股份有限公司 | Fischer-Tropsch synthesis device starting method |
| CN106350095A (en) * | 2016-08-24 | 2017-01-25 | 内蒙古伊泰煤制油有限责任公司 | Method for shortening Fischer-Tropsch synthesis reaction system start-up time |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002096834A2 (en) * | 2001-05-25 | 2002-12-05 | Bp Exploration Operating Company Limited | Fischer-tropsch process |
| CN101687832A (en) * | 2007-05-08 | 2010-03-31 | 巴斯夫欧洲公司 | Be used to prepare the method for alkene oxide |
| CN102863982A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Work starting method for slurry bed Fisher-Tropsch synthesis |
| CN103007835A (en) * | 2011-09-22 | 2013-04-03 | 中国石油化工股份有限公司 | Fischer-Tropsch synthesis device starting method |
| CN106350095A (en) * | 2016-08-24 | 2017-01-25 | 内蒙古伊泰煤制油有限责任公司 | Method for shortening Fischer-Tropsch synthesis reaction system start-up time |
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