Boiling bed-fixed bed system and starting method thereof

Abstract

The invention relates to a petrochemical production process, and discloses a fluidized bed-fixed bed system and a starting method. The fluidized bed-fixed bed system comprises a reaction unit, the reaction unit comprises a fluidized bed reactor and a fixed bed reactor which are communicated with each other, and the starting method comprises the following steps: 1) filling the reaction unit with a catalyst; (2) introducing inert gas into the reaction unit in the step (1) to replace air, and after the replacement is qualified, continuously introducing the inert gas to carry out pressure boosting air tightness on the reaction unit; (3) introducing hydrogen to carry out pressure-boosting airtight and synchronous heating on the reaction unit until the pressure is boosted to the operation pressure and the airtight is qualified; 4) feeding start-up oil into the reaction unit, and flushing the catalyst bed layer; and (5) vulcanizing the catalyst in the reaction unit which is qualified after flushing in the step (4), and after the vulcanization is completed, feeding raw oil, thereby completing the start-up of the fluidized bed-fixed bed system. The method has the advantages of being safe, reliable and high in operability.

Description

Technical Field

[0001] The invention relates to a petrochemical production process, and in particular to a fluidized bed-fixed bed system and a start-up method thereof. Background Art

[0002] Both the fluidized bed process and the fixed bed process have actual industrial application devices, but the fluidized bed-fixed bed direct combination process has no industrial application yet. There are applications for processes similar to the fluidized bed-fixed bed, but a fractionation system is set up between the fluidized bed and the fixed bed, such as the coal tar fluidized bed-fixed bed combination process. There are very few introductions to the start-up methods of the fluidized bed-fixed bed process, and most of them remain at the "paper talk" stage. The start-up methods in the prior art do not fully consider the actual start-up steps of the device, equipment protection, and possible risks in the process.

[0003] CN 108070402B introduces a method for starting a combined process of an ebullated bed and a fixed bed. The catalyst is loaded into an ebullated bed reactor and a fixed bed reactor from the top, and the connecting pipeline between the ebullated bed and the fixed bed is pressurized to increase the pressure. After the pressure is increased to the pressure required for the reaction, the start-up oil enters from the pipeline between the ebullated bed and the fixed bed, and enters the ebullated bed reactor and the fixed bed reactor respectively to wet the catalyst. After the catalyst is wetted, the reactor is started and the device operates normally.

[0004] However, the above patents may have the following problems in actual operation:

[0005] (1) If the catalyst is loaded into the reactor after the nitrogen replacement and full-pressure airtightness of the device are completed, the loading of the catalyst will bring air into the reaction system, and the catalyst needs to be replaced again after loading. In addition, the addition port needs to be opened when loading the agent, and this sealing point may be a leakage point for subsequent airtightness.

[0006] (2) If the catalyst is loaded into the reactor before the nitrogen replacement of the device is completed and the full pressure is airtight, then during the emergency pressure relief test during the start-up process, the catalyst in the ebullating bed reactor will be in a "boiling" state, causing catalyst wear. On the one hand, the catalyst strength is reduced, and the powder produced will become scale for the normal operation of the device, blocking the pipeline or causing the pressure drop of the subsequent fixed bed reactor to increase, affecting the long cycle of the device. On the other hand, once the boiling catalyst runs into the fixed bed reactor, it will cause the pressure drop of the device to increase after the start-up oil injection. Summary of the invention

[0007] The purpose of the present invention is to overcome the above-mentioned defects existing in the start-up of an ebullated bed-fixed bed combination device in the prior art, and to provide an ebullated bed-fixed bed system and a start-up method thereof. The present invention has the advantages of safety, reliability and strong operability.

[0008] In order to achieve the above object, the present invention provides a start-up method of an ebullated bed-fixed bed system, wherein the ebullated bed-fixed bed system comprises a reaction unit, wherein the reaction unit comprises an ebullated bed reactor and a fixed bed reactor connected to each other, and the start-up method comprises the following steps:

[0009] 1) loading the catalyst into the reaction unit;

[0010] 2) introducing an inert gas into the reaction unit in step 1) to displace the air, and after the replacement is qualified, continuing to introduce the inert gas to pressurize the reaction unit to make it airtight;

[0011] 3) Introduce hydrogen to increase the pressure and airtightness of the reaction unit and simultaneously increase the temperature until the pressure is increased to the operating pressure and the airtightness is qualified;

[0012] 4) feeding the start-up oil into the reaction unit to flush the catalyst bed;

[0013] 5) The catalyst in the reaction unit that has passed the flushing in step 4) is sulfurized. After the sulfurization is completed, the feedstock oil is cut in, and the operation of the ebullating bed-fixed bed system is completed.

[0014] Another aspect of the present invention provides an ebullating bed-fixed bed system, the system comprising:

[0015] The reaction unit comprises a raw material subunit, a heat exchange subunit, a fluidized bed reactor subunit and a fixed bed reactor subunit which are sequentially connected in series along the material flow direction; wherein the raw material subunit is connected to an oil injection pipeline and a liquid injection pipeline, the liquid injection pipeline is used to feed a sulfiding agent to the reaction unit to sulfide the catalyst in the reaction unit, and the oil injection pipeline is used to feed a start-up oil to the reaction unit to flush the catalyst bed;

[0016] an inert gas unit, connected to the reaction unit, and used to provide an inert gas to the reaction unit;

[0017] The new hydrogen unit is connected to the heat exchange subunit and is used to provide hydrogen to the reaction unit.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] (1) The ebullated bed-fixed bed system provided by the present invention is suitable for the start-up process combining the ebullated bed process and the fixed bed process. When the system is used for start-up, air can be effectively prevented from being introduced during catalyst loading;

[0020] (2) The present invention proposes for the first time to combine the fluidized bed start-up process with the fixed bed start-up process, thus filling the gap in the existing start-up methods;

[0021] (3) The start-up method of the fluidized bed-fixed bed system provided by the present invention is safe, reliable and highly operable. The method fully considers the shutdown and start-up characteristics of the fluidized bed process and the fixed bed process, and fully identifies the connection and potential risks of each step of the start-up of the fluidized bed-fixed bed process, effectively avoiding the introduction of flammable medium start-up oil before full pressure airtightness, and preventing the safety risks and extended start-up time brought by subsequent unqualified airtightness to the reaction unit treatment. Furthermore, it can also avoid catalyst wear or catalyst leakage caused by emergency pressure relief test, and realize the effective connection of the start-up process when the two processes are combined. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 is a schematic diagram of the start-up process of the fluidized bed-fixed bed system of some embodiments of the present invention;

[0023] Figure 2 It is a schematic diagram of the start-up process of the fluidized bed-fixed bed system of other embodiments of the present invention.

[0024] Description of reference numerals: Figure 2 middle:

[0025] D100, interstage separation tank D101, pre-filter raw material tank D102, post-filter raw material tank D103, hot high-pressure separator D104, hot low-pressure separator D105, cold high-pressure separator D106, cold low-pressure separator A101: hot high-gas air cooling P101, pre-filter booster pump P102, post-filter booster pump R101, fluidized bed reactor R102: fixed bed reactor R103, fixed bed reactor R104, fixed bed reactor R105, fixed bed reactor F101, reactor C101, circulating hydrogen compressor SR101: raw oil filter E101, raw oil heat exchanger E102, original oil heat exchanger E103: reaction effluent heat exchanger E104, reaction effluent heat exchanger E105, hot high-gas heat exchanger E106: hot high-gas heat exchanger DETAILED DESCRIPTION

[0026] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0027] In the present invention, unless otherwise specified, directional words such as "up, down, top, bottom, left, right" are usually used with reference to the directions shown in the drawings or are used to describe the relative positional relationships of components in the vertical, perpendicular or gravity direction.

[0028] The present invention discloses a method for starting up a fluidized bed-fixed bed system. The fluidized bed-fixed bed system comprises a reaction unit, wherein the reaction unit comprises a fluidized bed reactor and a fixed bed reactor connected to each other. The method for starting up the system comprises the following steps:

[0029] 1) loading the catalyst into the reaction unit;

[0030] 2) introducing an inert gas into the reaction unit in step 1) to displace the air, and after the replacement is qualified, continuing to introduce the inert gas to pressurize the reaction unit to make it airtight;

[0031] 3) Introduce hydrogen to increase the pressure and airtightness of the reaction unit and simultaneously increase the temperature until the pressure is increased to the operating pressure and the airtightness is qualified;

[0032] 4) Feeding start-up oil into the reaction unit to flush the catalyst bed;

[0033] 5) The catalyst in the reaction unit that has passed the flushing in step 4) is sulfurized. After the sulfurization is completed, the raw oil is cut in, and the boiling bed-fixed bed system is started.

[0034] Compared with the prior art, the start-up method of the present invention can effectively avoid the introduction of air when the catalyst is loaded; it is safe, reliable and highly operable, and can prevent the safety risks and extended start-up time brought by subsequent airtight failures in the reaction unit treatment.

[0035] In the present invention, there are two loading methods for the reaction unit, and the two loading methods each correspond to a different start-up method, one of which is: when the catalyst is loaded into the fluidized bed reactor and the fixed bed reactor in step 1), steps 2)-5) are performed in sequence; compared with the other method, the start-up steps of full-pressure airtightness and pressure relief are reduced, which can effectively reduce the start-up time, but the pressure increase process may cause catalyst wear, and is generally used for non-first start-up devices.

[0036] Another method is: when only the catalyst is loaded into the fixed bed reactor in step 1), step 2) comprises: introducing an inert gas into the reaction unit in step 1) to replace the air, and after the replacement is qualified, continuing to introduce the inert gas to pressurize the reaction unit to make it airtight (increase the pressure to 2.0-4.5MPa to check whether there is a leak point), and further comprises:

[0037] a) introducing hydrogen to increase the pressure of the reaction unit to make it airtight and simultaneously increase the temperature until the pressure reaches the operating pressure and the airtightness is qualified;

[0038] b) depressurizing the reaction unit in step a) to 2.0-5.0 MPa;

[0039] c) introducing the start-up oil to pad the ebullated bed reactor with oil. After the padding is completed, the reaction unit is depressurized to 0.5-1.0 MPa, and the catalyst is added to the ebullated bed reactor, and steps 3) to 5) are performed in sequence;

[0040] 3) Introduce hydrogen to increase the pressure and airtightness of the reaction unit and simultaneously increase the temperature until the pressure is increased to the operating pressure and the airtightness is qualified;

[0041] 4) feeding the start-up oil into the reaction unit to flush the catalyst bed;

[0042] 5) The catalyst in the reaction unit that has passed the flushing in step 4) is sulfurized. After the sulfurization is completed, the feedstock oil is cut in, and the operation of the ebullating bed-fixed bed system is completed.

[0043] The fluidized bed reactor is added with additives only after full pressure airtightness is achieved, which effectively avoids the introduction of flammable medium start-up oil before full pressure airtightness is achieved, and prevents the safety risks and extended start-up time caused by subsequent airtightness failures in the reaction unit processing.

[0044] In the present invention, there are no special requirements for the filling of the catalyst in the fixed bed reactor, and the commonly used filling forms can be used in the present invention. The following exemplary description does not limit the scope of the present invention. In some embodiments of the present invention, the fixed bed reactor adopts a dilute phase or dense phase filling method to fill the catalyst.

[0045] In the present invention, there is no special requirement for the inert gas. One or more of nitrogen, helium, neon, argon, krypton, xenon and radon can be used in the present invention. The following is an exemplary description, but the scope of the present invention is not limited thereto. In some embodiments of the present invention, the inert gas is selected from nitrogen.

[0046] To improve the replacement efficiency, in some embodiments of the present invention, in step 2), the method for replacing the reaction unit includes: introducing an inert gas to pressurize the reaction unit to 0.3-2.0 MPa, and then depressurizing it to 0.05-0.2 MPa; preferably, pressurizing it to 0.4-0.8 MPa and depressurizing it to 0.05-0.10 MPa.

[0047] To improve the replacement efficiency, in some embodiments of the present invention, in step 2), based on the above disclosure, the reaction unit is preferably repeatedly pressurized and depressurized for 2-10 times.

[0048] In some embodiments of the present invention, in step 2), the qualified replacement standard is: oxygen content < 0.5v%.

[0049] In some embodiments of the present invention, pressurizing the reaction unit to make it airtight in step 2) comprises: introducing an inert gas to pressurize the reaction unit to 2.0-4.5 MPa; preferably, releasing the pressure after the airtightness is qualified, and more preferably releasing the pressure to 0.1-0.2 MPa.

[0050] It should be noted that the tempering brittleness of the equipment should also be considered during the start-up process, and the start-up pressure increase process needs to be accompanied by temperature increase. For this reason, in some embodiments of the present invention, in step a), hydrogen is introduced to increase the pressure in the reaction unit to 3.5-5.0MPa, and the temperature of the reaction unit is synchronously controlled to 50-93°C. After the airtightness is qualified, the reaction unit is pressurized to 14.5-17.5MPa. It should be noted that in step a), the pressure is increased from 3.5-5.0MPa to 14.5-17.5MPa, and can be increased to 6.0MPa, 8.0MPa, 10.0MPa, 12.0MPa, 14.0MPa, 16.0MPa, and 17.5MPa in sequence, so that it has the advantage of reducing the safety risk caused by hydrogen leakage under high pressure.

[0051] In some embodiments of the present invention, the pressure relief conditions in step b) include: a pressure relief rate of 0.5-2.0 MPa / h, preferably 0.5-1.0 MPa / h. In this way, it is possible to prevent the pressure relief rate from being too fast, causing a large pressure difference change and causing leakage, which may lead to safety risks.

[0052] In some embodiments of the present invention, in step c), the speed of introducing the start-up oil into the ebullated bed reactor is 50-200 t / h, preferably 100-150 t / h. In this way, the start-up time can be shortened as much as possible while ensuring that the oil level of the ebullated bed reactor is highly controllable.

[0053] In some embodiments of the present invention, in step c), when the height of the start-up oil in the ebullated bed reactor is 1-100% of the tangent height of the ebullated bed reactor, the introduction of the start-up oil into the ebullated bed is stopped; this has the advantage of preventing breakage or wear during catalyst transportation.

[0054] Preferably, when the height of the start-up oil in the ebullated bed reactor is 3-50% of the tangent height of the ebullated bed reactor, the introduction of the start-up oil into the ebullated bed is stopped.

[0055] In some embodiments of the present invention, in step c), after the oil pad is completed, the pressure relief condition of the reaction unit includes: a pressure relief rate of 0.5-2.0 MPa / h, preferably 0.5-1.0 MPa / h. In this way, it is possible to prevent the pressure relief rate from being too fast and the pressure difference from changing greatly, causing leakage and leading to safety risks.

[0056] In order to avoid the loss of catalyst to the fixed bed reactor or reduce the catalyst "boiling" wear during emergency pressure relief, in some embodiments of the present invention, a delivery oil is used to deliver the catalyst to the ebullating bed reactor, wherein the flow rate of the delivery oil is 0-40m 3 / h, preferably 20-30m 3 / h. When the delivery oil is running, the delivery oil is discharged from the system synchronously.

[0057] In some embodiments of the present invention, in step 3), heating the reaction unit comprises: increasing the temperature of the feed port of the fluidized bed reactor to 150-160°C at 5-25°C / h, preferably at a heating rate of 10-20°C / h. In this way, the heating rate is too fast and the temperature difference is large, which may cause leakage and lead to safety risks.

[0058] In some embodiments of the present invention, in step 3), introducing hydrogen to increase the pressure to make it airtight includes: increasing the pressure to 3.5-5.0 MPa at a rate of 0.5-2.0 MPa / h, preferably increasing the pressure to 4.0-5.0 MPa at a rate of 0.5-1.0 MPa / h. In this way, the equipment is prevented from tempering brittleness and the start-up time is shortened as much as possible.

[0059] In some embodiments of the present invention, in step 3), the temperature of the reaction unit is synchronously controlled to 50-93°C. After the airtightness is qualified, the reaction unit is pressurized to 14.5-17.5MPa, so as to prevent the equipment from tempering brittleness while ensuring the airtightness of the reaction unit under normal operating pressure. Referring to the above, the pressure can be increased to 6.0MPa, 8.0MPa, 10.0MPa, 12.0MPa, 14.0MPa, 16.0MPa, and 17.5MPa in sequence.

[0060] In some embodiments of the present invention, in step 4), the feed amount of the start-up oil is 60-100 wt %, preferably 60-80 wt %, of the design load of the reaction unit.

[0061] In some embodiments of the present invention, in step 4), the flushing time of the catalyst bed is 3-8 hours, preferably 4-5 hours. In this way, while ensuring the flushing effect of the catalyst bed, the start-up oil consumption is reduced, thereby reducing the start-up cost.

[0062] In some embodiments of the present invention, in step 4), the initial feed rate is 0-50 t / h, the initial temperature is 90-120°C, and during the flushing process, the feed rate of the start-up oil fed into the reaction unit is gradually increased, for example, by an increase of 50 t / h.

[0063] In the present invention, there is no special requirement for the catalyst to be vulcanized, and commonly used vulcanization conditions can be used in the present invention. The following exemplary description is not intended to limit the scope of the present invention. In some embodiments of the present invention, in step 5), a vulcanizing agent is used to vulcanize the catalyst, and the vulcanizing agent is selected from at least one of dimethyl disulfide (DMDS), carbon disulfide, dibutyl polysulfide or liquid sulfur; the vulcanization conditions include: temperature 160-310° C., pressure is operating pressure, and vulcanization time 24-48 h.

[0064] Another aspect of the present invention discloses a fluidized bed-fixed bed system, such as Figure 1 As shown, the system includes:

[0065] The reaction unit comprises a raw material subunit, a heat exchange subunit, a fluidized bed reactor subunit and a fixed bed reactor subunit which are sequentially connected in series along the material flow direction; wherein the raw material subunit is connected with an oil injection pipeline and a solvent injection pipeline, the solvent injection pipeline is used to feed a sulfiding agent into the reaction unit to sulfide the catalyst in the reaction unit, and the oil injection pipeline is used to feed a start-up oil into the reaction unit to flush the catalyst bed and provide oil for sulfidation;

[0066] An inert gas unit connected to the reaction unit and used to provide inert gas to the reaction unit;

[0067] The new hydrogen unit is connected to the heat exchange subunit and is used to provide hydrogen to the reaction unit. It should be noted that the present invention has no special requirements for the new hydrogen unit. The new hydrogen unit can be a hydrogen feed pipeline connected to the heat exchange subunit, which will not be elaborated in the present invention.

[0068] In some embodiments of the present invention, the ebullating bed-fixed bed system further comprises:

[0069] A catalyst adding and discharging unit is connected to the ebullated bed reactor subunit, and a catalyst is fed into the ebullated bed reactor subunit through the catalyst adding and discharging unit;

[0070] The separation subunit is connected to the fixed bed reactor subunit and is provided with a gas phase outlet, an oil phase outlet and a water phase outlet for separating the gas, oil and water of the output of the fixed bed reactor subunit. The separation subunit is also provided with an external discharge pipeline for open-circuit discharge during catalyst bed flushing.

[0071] In some embodiments of the present invention, the oil phase outlet is preferably connected to the catalyst addition and discharge unit through a dosing circulation pipeline.

[0072] In some embodiments of the present invention, the oil phase outlet is preferably connected to the feed of the raw material subunit to achieve a sulfurization cycle during the start-up process.

[0073] In some embodiments of the present invention, the fluidized bed-fixed bed system also includes a circulating hydrogen unit, which is connected to the gas phase outlet and the heat exchange subunit. The circulating hydrogen unit includes a circulating hydrogen compressor, a circulating hydrogen desulfurization tower and a separator tank, which are used to desulfurize and recycle the circulating hydrogen in the reaction unit; preferably, the circulating hydrogen unit is also directly connected to the fixed bed reactor subunit and the heat exchange subunit.

[0074] In some embodiments of the present invention, the fluidized bed-fixed bed system further comprises a fractionation unit, which has the following functions: first, to separate the product from the effluent of the reaction unit; second, to remove H from the sulfided oil during the sulfidation process. 2 S and H 2 , ensuring that the external sulfurized oil is safer and more environmentally friendly. Among them, the feed part of the fractionation unit is connected to the oil phase outlet of the separation subunit, which is used to further separate the oil phase material from the separation subunit.

[0075] The discharge section of the distillation unit is provided with a discharge pipeline and a circulation pipeline, wherein the discharge pipeline is used to deliver the product to a downstream device / system; the circulation pipeline is connected with the feed section of the raw material subunit, and the feed section of the distillation unit is connected with the oil phase outlet of the separation subunit, so that product separation is achieved after passing through the distillation unit.

[0076] In some embodiments of the present invention, Figure 2 As shown, the fixed bed reactor subunit includes at least one fixed bed reactor, preferably 3-5, and the multiple fixed bed reactors are connected in series; the fluidized bed reactor subunit includes at least one fluidized bed reactor, and the fluidized bed reactor is connected to the fixed bed reactor.

[0077] In order to prevent the catalyst in the ebullated bed from entering the fixed bed when the system is running after startup, in other embodiments of the present invention, the ebullated bed reactor subunit includes at least one ebullated bed reactor, an interstage separator and / or a circulating oil pump, and the interstage separator is used to separate the reaction materials from the catalyst. Specifically, the feed end of the interstage separator is connected to the ebullated bed reactor, and the discharge end of the interstage separator is connected to the elevated bed reactor of the fixed bed reactor subunit.

[0078] The present invention has no special requirements for the configuration of the heat exchange subunit, as long as it can meet the temperature requirements of the raw materials entering the reaction unit, conventional heat exchange units are applicable to the present invention. The following exemplary description does not limit the scope of the present invention. In some embodiments of the present invention, Figure 2 As shown, the heat exchange subunit may include at least two heat exchangers and a reaction furnace, which can be used for heat exchange between the feed material and the discharge material of the reaction unit.

[0079] In the present invention, for the configuration in the raw material subunit, conventional raw material feeding units are applicable to the present invention. The following is an exemplary description, but the scope of the present invention is not limited thereby. In some embodiments of the present invention, for example Figure 2 As shown, the raw material subunit includes a pre-filtration raw material tank, a heat exchanger, a raw material filter and a post-filtration raw material tank which are sequentially connected along the raw material flow direction, wherein the post-filtration raw material tank is sequentially connected to the heat exchanger and the reactor of the heat exchange subunit.

[0080] There are no special requirements for the configuration of the inert gas unit in the present invention, as long as the inert gas can be passed to the reaction unit. For example, the inert gas unit may include an inert gas source and a pipeline connecting the inert gas source to the fluidized bed reactor and the fixed bed reactor in the reaction unit.

[0081] In the present invention, there is no special requirement for the arrangement of the catalyst addition and discharge unit ( Figure 2 As long as the catalyst loading of the method 1 and the method 2 of the present invention can be realized, for example, a conventional catalyst adding and discharging unit including a catalyst tank, a catalyst adding and discharging tank, a filter, a buffer tank, a flushing oil pump, a delivery oil pump, etc. can be used in the present invention.

[0082] In the present invention, there is no special requirement for the arrangement of the separation subunit, and any conventional separation subunit capable of achieving separation of gas, oil and water is applicable to the present invention. The following is an exemplary description, but the scope of the present invention is not limited thereby. In some embodiments of the present invention, Figure 2 As shown, the separation subunit includes a hot high-pressure separator, a hot low-pressure separator, a cold high-pressure separator, and a cold low-pressure separator.

[0083] In the present invention, there is no special requirement for the configuration of the fractionation unit, as long as the product separation of the effluent from the reaction unit and / or the removal of H from the sulfided oil in the sulfidation process can be achieved. 2 S and H 2 That is, the following exemplary description is not intended to limit the scope of the present invention. In some embodiments of the present invention, the fractionation unit includes a fractionation tower, a side-line tower, and the like.

[0084] It is understandable that the fluidized bed-fixed bed system of the present invention is also provided with valves, instruments, pumps and other components commonly used in the chemical industry. The present invention has no special requirements for this and will not be described in detail.

[0085] The ebullating bed-fixed bed system of the present invention can be used for the hydrogenation reaction of crude oil, and the crude oil can be one or more of residual oil, heavy oil, asphalt, coal tar and catalytic oil slurry.

[0086] The specific implementation of the present invention is described in detail below in conjunction with the accompanying drawings. It should be understood that the specific implementation described here is only used to illustrate and explain the implementation of the present invention, and is not used to limit the implementation of the present invention.

[0087] Example 1

[0088] use Figure 2 As shown, the ebullated bed-fixed bed system is started up, wherein the reaction unit comprises an ebullated bed reactor and three fixed bed reactors connected in series, and the start-up is carried out in mode 2, including:

[0089] (1) loading catalyst into the fixed bed reaction subunit;

[0090] (2) Nitrogen from the inert gas unit is introduced to replace the gas phase in the system (including the reaction unit, heat exchange subunit, fluidized bed reactor subunit, fixed bed reactor subunit, separation unit, circulating hydrogen unit and catalyst addition and discharge unit), the reaction unit is pressurized to 0.4 MPa, the pressure is released from the separation subunit to 0.05 MPa, and the reaction unit is pressurized again. This pressurization-pressure release is repeated twice until the gas phase is basically replaced by nitrogen. The replaced gas phase is discharged to the outside of the system through the separation subunit. The oxygen content in the system is detected to be less than 0.5v%, and the nitrogen replacement is qualified;

[0091] (3) Nitrogen is introduced from the inert gas unit to increase the pressure of the reaction unit to 4.0 MPa at a pressure increase rate of 0.5 MPa / h and make it airtight. After the airtightness is qualified, the reaction unit is depressurized to 0.1 MPa at a pressure release rate of 0.5 MPa / h.

[0092] (4) Introduce hydrogen from the new hydrogen unit, increase the pressure of the reaction unit to 4.0 MPa at a pressure increase rate of 0.5 MPa / h, and simultaneously control the temperature of the reaction unit to 50°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0 MPa, 8.0 MPa, 10.0 MPa, 12.0 MPa, and 14.5 MPa in sequence and made airtight;

[0093] (5) After the airtightness is qualified, the reaction unit is depressurized to 5.0 MPa at a depressurization rate of 0.5 MPa / h, and the start-up oil is introduced at 100 t / h through the raw material subunit to pad the ebullated bed reactor with oil. When the height of the start-up oil in the ebullated bed reactor is 3% of its tangent height, the introduction of the start-up oil into the ebullated bed is stopped;

[0094] (6) Depressurize the reaction unit to 0.5 MPa at a pressure relief rate of 0.5 MPa / h, start the circulating hydrogen compressor, and control the oil delivery system of the catalyst addition and discharge unit by 20m 3 / h, the catalyst is transported to the ebullated bed reactor. When the oil level in the ebullated bed reactor is full to the liquid phase outlet, the oil (diesel) is transported to overflow to the fixed bed reactor sub-unit, and then circulated back to the catalyst addition and discharge sub-unit through the heat exchange sub-unit and the separation unit.

[0095] (7) After the addition of the ebullated bed reaction subunit is completed, the oil circulation is stopped. The hydrogen from the new hydrogen unit is introduced to increase the pressure of the reaction unit to 4.0MPa at a pressure increase rate of 0.5MPa / h, and the temperature of the reaction unit is simultaneously controlled to 50°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0MPa, 8.0MPa, 10.0MPa, 12.0MPa, and 14.5MPa in sequence and airtight;

[0096] (8) After the airtightness is qualified, the start-up oil is introduced into the reaction unit through the raw material subunit at an increase of 50 t / h. When the start-up oil feed amount reaches 60% by weight of the design load, the catalyst bed of the ebullated bed reaction subunit and the fixed bed reaction subunit is flushed for 4 hours; the temperature of the synchronous point reactor is increased, and the inlet temperature of the ebullated bed reaction subunit is increased to 150°C at a rate of 10°C / h;

[0097] (9) injecting the vulcanizing agent dimethyl disulfide into the raw material subunit for vulcanization, the final vulcanization temperature is 310°C, the pressure is the operating pressure, and the vulcanization time is 24 hours;

[0098] (10) Switch to residual oil and complete the start-up.

[0099] Results: There was no leakage in the airtight process, the catalyst wear rate was 0, and the start-up time was 15 days.

[0100] Example 2

[0101] use Figure 2 As shown, the ebullated bed-fixed bed system is started up, wherein the reaction unit comprises an ebullated bed reactor and three fixed bed reactors connected in series, and the start-up is carried out in mode 2, including:

[0102] (1) loading catalyst into the fixed bed reaction subunit;

[0103] (2) Nitrogen from the inert gas unit is introduced to replace the gas phase in the system (including the reaction unit, heat exchange subunit, fluidized bed reactor subunit, fixed bed reactor subunit, separation unit, circulating hydrogen unit, and catalyst addition and discharge unit), the reaction unit is pressurized to 0.8 MPa, the pressure is released from the separation subunit to 0.1 MPa, and the reaction unit is pressurized again, and this is repeated 10 times until the gas phase is basically replaced by nitrogen. The replaced gas phase is discharged to the outside of the system through the separation subunit. The oxygen content is detected to be less than 0.5v%, and the nitrogen replacement is qualified;

[0104] (3) Nitrogen is introduced from the inert gas unit to increase the pressure of the reaction unit to 5.0 MPa at a pressure increase rate of 1.0 MPa / h and make it airtight. After the airtightness is qualified, the reaction unit is depressurized to 0.2 MPa at a pressure release rate of 1.0 MPa / h.

[0105] (4) Introduce hydrogen from the new hydrogen unit, increase the pressure of the reaction unit to 5.0 MPa at a pressure increase rate of 1.0 MPa / h, and simultaneously control the temperature of the reaction unit to 93°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0 MPa, 8.0 MPa, 10.0 MPa, 12.0 MPa, 14.0 MPa, 16.0 MPa, and 17.5 MPa in sequence and made airtight;

[0106] (5) After the airtightness is qualified, the reaction unit is depressurized to 3.0 MPa at a depressurization rate of 0.5 MPa / h, and the start-up oil is introduced through the raw material subunit at 150 t / h to pad the ebullated bed reactor with oil. When the height of the start-up oil in the ebullated bed reactor is 50% of its tangent height, the introduction of the start-up oil into the ebullated bed is stopped;

[0107] (6) Depressurize the reaction unit to 1.0 MPa at a rate of 0.5 MPa / h, start the circulating hydrogen compressor, and control the oil delivery system of the catalyst addition and discharge unit to 25 m 3 / h, the catalyst is transported to the ebullated bed reactor. When the oil level in the ebullated bed reactor is full to the liquid phase outlet, the oil (diesel) is transported to overflow to the fixed bed reactor sub-unit, and then circulated back to the catalyst addition and discharge sub-unit through the heat exchange sub-unit and the separation unit.

[0108] (7) After the addition of the ebullated bed reaction subunit is completed, the oil circulation is stopped. The hydrogen from the new hydrogen unit is introduced to increase the pressure of the reaction unit to 5.0MPa at a pressure increase rate of 1.0MPa / h, and the temperature of the reaction unit is simultaneously controlled to 93°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0MPa, 8.0MPa, 10.0MPa, 12.0MPa, 14.0MPa, 16.0MPa, 17.5MPa in sequence and airtight;

[0109] (8) After the airtightness is qualified, the start-up oil is introduced into the reaction unit through the raw material subunit at an increase of 50 t / h. When the start-up oil feed amount reaches 80% by weight of the design load, the catalyst bed of the ebullated bed reaction subunit and the fixed bed reaction subunit is flushed for 5 hours; the temperature of the synchronous point reactor is increased, and the inlet temperature of the ebullated bed reaction subunit is increased to 160°C at a rate of 20°C / h;

[0110] (9) injecting the vulcanizing agent carbon disulfide into the raw material subunit for vulcanization, the final vulcanization temperature is 310°C, the pressure is the operating pressure, and the vulcanization time is 36 hours;

[0111] (10) Switch to residual oil and complete the start-up.

[0112] Results: There was no leakage in the airtight process, the catalyst wear rate was 0, and the start-up time was 15 days.

[0113] Example 3

[0114] use Figure 2 The ebullated bed-fixed bed system shown in the figure has a reaction unit including one ebullated bed reactor and four fixed bed reactors connected in series. The ebullated bed-fixed bed system is started up in mode 1, including:

[0115] (1) loading catalyst into the ebullated bed reaction subunit and the fixed bed reaction subunit;

[0116] (2) Nitrogen from the inert gas unit is introduced to replace the gas phase in the system (including the heat exchange subunit, the fluidized bed reactor subunit, the fixed bed reactor subunit, the separation unit, the circulating hydrogen unit, and the catalyst addition and discharge unit), the reaction unit is pressurized to 0.6 MPa, the pressure is reduced to 0.08 MPa from the separation subunit, and the reaction unit is pressurized again. This is repeated 5 times until the gas phase is basically replaced by nitrogen. The replaced gas phase is discharged to the outside of the system through the separation subunit. The oxygen content is <0.5v% after detection, and the nitrogen replacement is qualified; (3) Nitrogen from the inert gas unit is introduced to increase the pressure of the reaction unit to 4.5 MPa at a pressure increase rate of 0.8 MPa / h and make it airtight. After the pressure is airtight, the reaction unit is depressurized to 0.15 MPa at a pressure reduction rate of 0.8 MPa / h.

[0117] (4) Introduce hydrogen from the new hydrogen unit, pressurize the reaction unit to 4.5 MPa at a pressure increase rate of 0.8 MPa / h, and simultaneously control the temperature of the reaction unit to 75°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0 MPa, 8.0 MPa, 10.0 MPa, 12.0 MPa, 14.0 MPa, and 16.0 MPa in sequence and made airtight;

[0118] (5) After the airtightness is qualified, the start-up oil (diesel) is introduced into the reaction unit through the raw material subunit at an increase of 50 t / h. When the start-up oil feed amount reaches 70% by weight of the design load, the catalyst bed of the ebullated bed reaction subunit and the fixed bed reaction subunit is flushed for 4.5 hours; the temperature of the synchronous point reactor is increased, and the inlet temperature of the ebullated bed reaction subunit is increased to 155°C at a rate of 15°C / h;

[0119] (6) injecting liquid sulfur as a vulcanizing agent into the raw material subunit for vulcanization, with the final vulcanization temperature being 310°C, the pressure being the operating pressure, and the vulcanization time being 24 hours;

[0120] (7) Switch to residual oil and complete the start-up.

[0121] Results: There was no leakage in the airtight process, the catalyst wear rate was 5-20%, and the start-up time was 8 days.

[0122] Example 4

[0123] use Figure 2 As shown, the ebullated bed-fixed bed system is started up, wherein the reaction unit comprises an ebullated bed reactor and three fixed bed reactors connected in series, and the start-up is carried out in mode 2, including:

[0124] (1) loading catalyst into the fixed bed reaction subunit;

[0125] (2) Nitrogen from the inert gas unit is introduced to replace the gas phase in the system (including the reaction unit, heat exchange subunit, fluidized bed reactor subunit, fixed bed reactor subunit, separation unit, circulating hydrogen unit, and catalyst addition and discharge unit), the reaction unit is pressurized to 0.3 MPa, the pressure is released from the separation subunit to 0.2 MPa, and the reaction unit is pressurized again, and this is repeated twice until the gas phase is basically replaced by nitrogen. The replaced gas phase is discharged to the outside of the system through the separation subunit. The oxygen content is detected to be less than 0.5v%, and the nitrogen replacement is qualified;

[0126] (3) Nitrogen is introduced from the inert gas unit to increase the pressure of the reaction unit to 3.5 MPa at a pressure increase rate of 2.0 MPa / h and make it airtight. After the airtightness is qualified, the reaction unit is depressurized to 0.1 MPa at a pressure release rate of 2.0 MPa / h.

[0127] (4) Introduce hydrogen from the new hydrogen unit, increase the pressure of the reaction unit to 3.5 MPa at a pressure increase rate of 2.0 MPa / h, and simultaneously control the temperature of the reaction unit to 50°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0 MPa, 8.0 MPa, 10.0 MPa, 12.0 MPa, 14.0 MPa, 16.0 MPa, and 17.5 MPa in sequence and made airtight;

[0128] (5) After the airtightness is qualified, the reaction unit is depressurized to 2.0 MPa at a depressurization rate of 0.5 MPa / h, and the start-up oil is introduced through the raw material subunit at a rate of 125 t / h to pad the ebullated bed reactor with oil. When the height of the start-up oil in the ebullated bed reactor is 100% of its tangent height, the introduction of the start-up oil into the ebullated bed is stopped;

[0129] (6) Depressurize the reaction unit to 1.0 MPa at a rate of 0.5 MPa / h, start the circulating hydrogen compressor, and control the oil delivery system of the catalyst addition and discharge unit to 40m 3 / h, the catalyst is transported to the ebullated bed reactor. When the oil level in the ebullated bed reactor is full to the liquid phase outlet, the oil (diesel) is transported to overflow to the fixed bed reactor sub-unit, and then circulated back to the catalyst addition and discharge sub-unit through the heat exchange sub-unit and the separation unit.

[0130] (7) After the addition of the ebullated bed reaction subunit is completed, the oil circulation is stopped. The hydrogen from the new hydrogen unit is introduced to increase the pressure of the reaction unit to 3.5MPa at a pressure increase rate of 2.0MPa / h, and the temperature of the reaction unit is simultaneously controlled to 50°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0MPa, 8.0MPa, 10.0MPa, 12.0MPa, 14.0MPa, 16.0MPa, 17.5MPa in sequence and airtight;

[0131] (8) After the airtightness is qualified, the start-up oil is introduced into the reaction unit through the raw material subunit at an increase of 50 t / h. When the start-up oil feed amount reaches 100% by weight of the design load, the catalyst bed of the ebullated bed reaction subunit and the fixed bed reaction subunit is flushed for 8 hours; the temperature of the synchronous point reactor is increased, and the inlet temperature of the ebullated bed reaction subunit is increased to 150°C at a rate of 25°C / h;

[0132] (9) injecting the vulcanizing agent dimethyl disulfide into the raw material subunit for vulcanization, the final vulcanization temperature is 310°C, the pressure is the operating pressure, and the vulcanization time is 24 hours;

[0133] (10) Switch to residual oil and complete the start-up.

[0134] Results: There was leakage of high-pressure flange in the airtight process due to excessive pressure increase, the wear rate of the catalyst was 0, and the start-up time was 17 days.

[0135] Comparative Example 1

[0136] The method disclosed in CN 108070402B was used to start up a fluidized bed reactor and three fixed bed reactors connected in series. During the first emergency pressure relief, the catalyst in the fluidized bed reactor "boiled", resulting in wear, including:

[0137] (1) loading catalyst into the ebullated bed reaction subunit and the fixed bed reaction subunit;

[0138] (2) Introducing hydrogen from the new hydrogen unit, and increasing the pressure of the reaction unit to 17.5 MPa at a pressure increase rate of 1.5 MPa / h;

[0139] (3) Conduct emergency pressure relief test;

[0140] (4) Introducing hydrogen from the new hydrogen unit, and increasing the pressure of the reaction unit to 17.5 MPa at a pressure increase rate of 1.5 MPa / h;

[0141] (5) introducing process oil (diesel) into the reaction unit through the raw material subunit to wet the catalysts of the ebullated bed reaction subunit and the fixed bed reaction subunit; synchronously raising the temperature of the reaction furnace to increase the inlet temperature of the ebullated bed reaction subunit to 155° C. at a rate of 15° C. / h;

[0142] (6) injecting a vulcanizing agent, dimethyl disulfide, into the raw material subunit for vulcanization;

[0143] (7) Switch to residual oil and complete the start-up.

[0144] Results: During the emergency pressure relief test, the catalyst in the fluidized bed reactor will be in a "boiling" state, causing catalyst wear, which will reduce the catalyst strength. The powder produced will become scale for the normal operation of the device, blocking the pipeline or causing the subsequent fixed bed reactor to increase the pressure drop, affecting the long cycle of the device. The catalyst wear rate is 5-20%, and the start-up time is 10 days.

[0145] Comparative Example 2

[0146] use Figure 2 As shown, the fluidized bed-fixed bed system is started, wherein the reaction unit includes an fluidized bed reactor and four fixed bed reactors connected in series, and the reaction system is not fully airtight, that is, the fluidized bed reactor is used to transport the catalyst with diesel, and a subsequent level of airtightness is not passed, and the pressure needs to be released and the diesel in the reaction system needs to be drained to replace the gasket, including:

[0147] (1) loading catalyst into the fixed bed reaction subunit;

[0148] (2) Nitrogen from the inert gas unit is introduced to replace the gas phase in the system (including the reaction unit, heat exchange subunit, fluidized bed reactor subunit, fixed bed reactor subunit, separation unit, circulating hydrogen unit, and catalyst addition and discharge unit), the reaction unit is pressurized to 0.8 MPa, the pressure is released from the separation subunit to 0.1 MPa, and the reaction unit is pressurized again, and this is repeated 10 times until the gas phase is basically replaced by nitrogen. The replaced gas phase is discharged to the outside of the system through the separation subunit. The oxygen content is detected to be less than 0.5v%, and the nitrogen replacement is qualified;

[0149] (3) Nitrogen is introduced from the inert gas unit to increase the pressure of the reaction unit to 1.0 MPa at a pressure increase rate of 1.0 MPa / h to make it airtight, the circulating hydrogen compressor is started, and the oil delivery system of the catalyst addition and discharge unit is controlled to 30m 3 / h, the catalyst is transported to the ebullated bed reactor. When the oil level in the ebullated bed reactor is full to the liquid phase outlet, the oil (diesel) is transported to overflow to the fixed bed reactor sub-unit, and then circulated back to the catalyst addition and discharge sub-unit through the heat exchange sub-unit and the separation unit.

[0150] (4) After the addition of the ebullated bed reaction subunit is completed, the oil circulation is stopped. The nitrogen from the inert gas unit is introduced to increase the pressure of the reaction unit to 5.0 MPa at a pressure increase rate of 1.0 MPa / h and make it airtight. After the airtightness is qualified, the reaction unit is depressurized to 0.2 MPa at a pressure release rate of 1.0 MPa / h.

[0151] (5) Introduce hydrogen from the new hydrogen unit, increase the pressure of the reaction unit to 5.0 MPa at a pressure increase rate of 1.0 MPa / h, and simultaneously control the temperature of the reaction unit to 93°C. After the airtightness is qualified, the reaction unit is pressurized to 6.0 MPa, 8.0 MPa, 10.0 MPa, 12.0 MPa, 14.0 MPa, 16.0 MPa, and 17.5 MPa in sequence and made airtight;

[0152] (6) After the airtightness is qualified, the start-up oil is introduced into the reaction unit through the raw material subunit at an increase of 50 t / h. When the start-up oil feed amount reaches 80% by weight of the design load, the catalyst bed of the ebullated bed reaction subunit and the fixed bed reaction subunit is flushed for 5 hours; the temperature of the synchronous point reactor is increased, and the inlet temperature of the ebullated bed reaction subunit is increased to 160°C at a rate of 20°C / h;

[0153] (7) injecting the vulcanizing agent carbon disulfide into the raw material subunit for vulcanization, the final vulcanization temperature is 310°C, the pressure is the operating pressure, and the vulcanization time is 36 hours;

[0154] (8) Switch to residual oil and complete the start-up.

[0155] Results: The flammable medium start-up oil was introduced before full pressure gas tightness, which caused safety risks to the reaction unit treatment and extended start-up time due to subsequent gas tightness failure. The catalyst wear rate was 0 and the start-up time was 18 days.

[0156] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. A method for starting a fluidized bed-fixed bed system, It is characterized in that The ebullated bed-fixed bed system comprises a reaction unit, wherein the reaction unit comprises an ebullated bed reactor and a fixed bed reactor connected to each other, and the start-up method comprises the following steps: 1) loading the catalyst into the reaction unit; 2) introducing an inert gas into the reaction unit in step 1) to displace the air, and after the replacement is qualified, continuing to introduce the inert gas to pressurize the reaction unit to make it airtight; 3) Introduce hydrogen to increase the pressure and airtightness of the reaction unit and simultaneously increase the temperature until the pressure is increased to the operating pressure and the airtightness is qualified; 4) feeding the start-up oil into the reaction unit to flush the catalyst bed; 5) The catalyst in the reaction unit that has passed the flushing in step 4) is sulfurized. After the sulfurization is completed, the feedstock oil is cut in, and the operation of the ebullating bed-fixed bed system is completed.

2. The start-up method according to claim 1, in, The catalyst loading method in step 1) includes: Mode 1: When the catalyst is loaded into the ebullating bed reactor and the fixed bed reactor in step 1), steps 2) to 5) are performed in sequence; or Mode 2: When only the catalyst is loaded into the fixed bed reactor in step 1), step 2) further comprises: a) introducing hydrogen to increase the pressure of the reaction unit to make it airtight and simultaneously increase the temperature until the pressure reaches the operating pressure and the airtightness is qualified; b) depressurizing the reaction unit in step a) to 2.0-5.0 MPa; c) Introducing start-up oil to pad the ebullated bed reactor with oil. After the padding is completed, the reaction unit is depressurized to 0.5-1.0 MPa, and a catalyst is added to the ebullated bed reactor, and steps 3) to 5) are performed in sequence.

3. The start-up method according to claim 1 or 2, in, In step 2), The method for replacing the reaction unit includes: introducing the inert gas to pressurize the reaction unit to 0.3-2.0 MPa, and then reducing the pressure to 0.05-0.2 MPa; Preferably, the pressure is charged to 0.4-0.8 MPa and the pressure is released to 0.05-0.10 MPa; and / or Preferably, the reaction unit is repeatedly pressurized and depressurized for 2 to 10 times; and / or The standard for qualified replacement is: oxygen content <0.5v%.

4. The method for starting a work according to any one of claims 1 to 3, in, In step 2), pressurizing the reaction unit to make it airtight comprises: The inert gas is introduced to pressurize the reaction unit to 2.0-4.5 MPa; It is preferred to release the pressure after the airtightness is qualified, and more preferably the pressure is released to 0.1-0.2MPa.

5. The method for starting a work according to any one of claims 1 to 4, in, In step a), hydrogen is introduced to increase the pressure in the reaction unit to 3.5-5.0 MPa, and the temperature of the reaction unit is simultaneously controlled to 50-93° C. After the airtightness is qualified, the reaction unit is pressurized to 14.5-17.5 MPa; and / or The pressure relief conditions in step b) include: a pressure relief rate of 0.5-2.0 MPa / h, preferably 0.5-1.0 MPa / h.

6. The method for starting a work according to any one of claims 1 to 5, in, In step c), The speed of introducing the start-up oil into the ebullated bed reactor is 50-200 t / h, preferably 100-150 t / h; and / or When the height of the start-up oil in the ebullated bed reactor is 1-100% of the tangent height of the ebullated bed reactor, the introduction of the start-up oil into the ebullated bed reactor is stopped; Preferably, when the height of the start-up oil in the ebullated bed reactor is 3-50% of the tangent height of the ebullated bed reactor, the introduction of the start-up oil into the ebullated bed reactor is stopped; and / or After the oil pad is completed, the pressure relief conditions of the reaction unit include: a pressure relief rate of 0.5-2.0 MPa / h, preferably 0.5-1.0 MPa / h; and / or The catalyst is transported into the fluidized bed reactor using a transport oil, wherein the flow rate of the transport oil is 0-40m 3 / h, preferably 20-30m 3 / h.

7. The method for starting a work according to any one of claims 1 to 6, in, In step 3), Heating the reaction unit comprises: increasing the feed inlet temperature of the ebullated bed reactor to 150-160°C at a rate of 5-25°C / h, preferably at a rate of 10-20°C / h; and / or The step of introducing hydrogen to increase the pressure to make it airtight comprises: increasing the pressure to 3.5-5.0 MPa at a rate of 0.5-2.0 MPa / h, preferably increasing the pressure to 4.0-5.0 MPa at a rate of 0.5-1.0 MPa / h; and / or The temperature of the reaction unit is synchronously controlled at 50-93°C. After the airtightness is qualified, the reaction unit is pressurized to 14.5-17.5MPa.

8. The method for starting a work according to any one of claims 1 to 7, in, In step 4), The feed amount of the start-up oil is 60-100 wt %, preferably 60-80 wt % of the design load of the reaction unit; and / or The catalyst bed is flushed for 3-8 hours, preferably 4-5 hours; and / or The feed rate of the start-up oil fed into the reaction unit is gradually increased, wherein the initial feed rate of the start-up oil is 0-50 t / h and the initial temperature is 90-120°C.

9. The method for starting a work according to any one of claims 1 to 8, in, In step 5), the catalyst is vulcanized with a vulcanizing agent, wherein the vulcanizing agent is selected from at least one of dimethyl disulfide, carbon disulfide, dibutyl polysulfide or liquid sulfur; and / or The vulcanization conditions include: temperature of 160-310° C., pressure of operating pressure, and vulcanization time of 24-48 hours.

10. A fluidized bed-fixed bed system, It is characterized in that The system comprises: The reaction unit comprises a raw material subunit, a heat exchange subunit, a fluidized bed reactor subunit and a fixed bed reactor subunit which are sequentially connected in series along the material flow direction; wherein the raw material subunit is connected to an oil injection pipeline and a liquid injection pipeline, the liquid injection pipeline is used to feed a sulfiding agent to the reaction unit to sulfide the catalyst in the reaction unit, and the oil injection pipeline is used to feed a start-up oil to the reaction unit to flush the catalyst bed; an inert gas unit, connected to the reaction unit, and used to provide an inert gas to the reaction unit; The new hydrogen unit is connected to the heat exchange subunit and is used to provide hydrogen to the reaction unit.

11. The system according to claim 10, It is characterized in that The system further comprises: A catalyst adding and discharging unit is connected to the ebullated bed reactor subunit, and a catalyst is fed into the ebullated bed reactor subunit through the catalyst adding and discharging unit; A separation subunit is connected to the fixed bed reactor subunit and is provided with a gas phase outlet, an oil phase outlet and a water phase outlet, and is used to separate the output of the fixed bed reactor subunit into gas, oil and water; Preferably, the oil phase outlet is connected to the catalyst addition and discharge unit via a dosing circulation pipeline; and / or Preferably, the oil phase outlet is connected to the feed of the raw material subunit to realize the sulfurization cycle during the start-up process.

12. The system according to claim 11, It is characterized in that The system further comprises a circulating hydrogen unit, which is connected to the gas phase outlet and the heat exchange subunit, and comprises a circulating hydrogen compressor, a circulating hydrogen desulfurization tower and a liquid separator, and is used for desulfurizing, deliquating and recirculating the circulating hydrogen in the reaction unit; Preferably, the circulating hydrogen unit is also directly connected to the fixed bed reactor subunit.

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