Sulfur supplementing system and sulfur supplementing method for hydrogenation device

Abstract

The invention discloses a sulfur supplementing system of a hydrogenation device. The sulfur supplementing system comprises: a sulfur injection homogenization tank in which homogenized oil, sulfur, a circulating homogeneous vulcanizing agent and a backwashing oil filtrate form a homogeneous vulcanizing agent; the sulfur injection pump is used for feeding a homogeneous sulfur injection agent into the sulfur injection mixer and / or the circulating reinjection sulfur homogenization tank; the raw oil and the homogeneous sulfur injection agent are mixed in the sulfur injection mixer to obtain sulfur injection raw oil; the homogenized oil heater is used for heating the homogenized oil; the raw oil filter is used for filtering the raw oil after sulfur injection to obtain sulfur-supplemented raw oil; and the back-flushing oil filter is used for receiving the solid particle-containing flushing oil of the raw oil filter and filtering the solid particle-containing flushing oil. According to the sulfur supplementing system, sulfur serves as a vulcanizing agent, the vulcanizing agent is continuously and smoothly conveyed to the hydrogenation reactor economically and efficiently, and stable operation of the sulfur supplementing process in production of the hydrogenation device is guaranteed.

Description

Technical Field

[0001] This invention belongs to the field of oil refining hydrogenation technology, and relates to a sulfur replenishment system and method for a hydrogenation unit. Background Technology

[0002] The active metal components of the catalyst used in hydrogenation units exhibit high activity in their sulfide state; therefore, the catalyst must maintain this sulfide state during normal operation. When the sulfur on the catalyst reaches equilibrium with the hydrogen sulfide in the circulating hydrogen during hydrogenation, the high-valence metal sulfide on the catalyst is preserved. However, when the hydrogen sulfide content in the circulating hydrogen is too low (generally less than 300 ppm), the partial pressure of hydrogen sulfide decreases, disrupting this equilibrium. Hydrogen then reduces the metal sulfides on the catalyst to lower-valence metals, or even to elemental metals, causing the catalyst to lose activity and affecting the reaction efficiency. In the hydrogenation of low-sulfur feedstocks (such as low-sulfur coal tar and wax oil), the amount of hydrogen sulfide generated during hydrogenation is relatively small, resulting in extremely low hydrogen sulfide content in the circulating hydrogen. Therefore, to prevent the reduction of the catalyst metal sulfides, the reactor needs to continuously replenish the sulfiding agent to ensure sufficient hydrogen sulfide partial pressure in the circulating hydrogen, generally maintaining a hydrogen sulfide concentration of 300-500 ppm to achieve the desired hydrogenation reaction effect.

[0003] Commonly used sulfurizing agents include carbon disulfide, dimethyl disulfide, and elemental sulfur. Dimethyl disulfide and carbon disulfide are highly toxic, pose significant risks, and are expensive. In contrast, sulfur is less toxic, easier to transport and handle, has a higher safety factor, and is readily available and inexpensive. However, using sulfur as a sulfurizing agent presents several problems. First, sulfur is solid at room temperature and pressure and requires heating to above 119°C to become liquid and fluid. If the temperature drops, the sulfur will solidify, leading to blockages or pump damage. Second, sulfur injected into pipelines cannot mix thoroughly with the oil. The oil-insoluble sulfur aggregates into large droplets that sink within the pipeline, adhering to the pipe walls and slowly depositing to form sulfur clumps, causing blockages. Therefore, developing a safe, efficient, and reliable sulfur injection system and process for hydrogenation units, ensuring the continuous and smooth delivery of the sulfurizing agent to the hydrogenation reactor, is crucial for guaranteeing the performance of the hydrogenation catalyst and the long-term stable operation of the unit.

[0004] CN106047403A discloses a method and equipment for injecting sulfur additive into a hydrocracking reactor in a direct coal liquefaction process. In this method, intermediate feedstock hydrogen sulfide is directly injected into the hydrocatalytic cracking reactor as a sulfurizing agent, shortening the process, reducing energy consumption, and saving the amount of hydrogen consumed in existing technologies where elemental sulfur is used as a sulfur additive to react with hydrogen in the hydrocracking reactor to produce hydrogen sulfide. However, using hydrogen sulfide as a sulfurizing agent presents significant safety hazards in terms of operation and metering.

[0005] CN215312228U discloses a coal tar hydrogenation liquid sulfur injection device, including a shell, a heating steam coil and a condensate coil installed inside the shell, the heating steam coil and the condensate coil being connected together, a dosing port being provided at the top of the shell, a submersible pump and a stirrer being connected to the top of the shell, the lower end of the submersible pump extending into the shell, and the stirring blades at the lower end of the stirrer extending into the shell, ensuring continuous and stable operation of the sulfur injection system during production, but this technology cannot guarantee that the sulfur precipitation and crystallization problems caused by temperature difference will occur after the liquid sulfur is injected into the raw material oil pipeline.

[0006] CN113897211A and CN206204237U disclose sulfur injection systems and methods for biodiesel hydrogenation and anthracene oil hydrogenation, respectively. However, neither of them considers the potential precipitation and crystallization of sulfur in the feedstock oil transportation system after sulfur injection, which could very likely cause pipeline blockage and pump damage, affecting the continuous and stable operation of the device. Summary of the Invention

[0007] The technical problem to be solved by this invention is to provide a sulfur replenishment system and method for a hydrogenation unit. This invention uses sulfur as a sulfurizing agent, and through a sulfur injection homogenization and blending system and a sulfur injection mixing and solids removal treatment, it economically and efficiently delivers the sulfurizing agent continuously and smoothly to the hydrogenation reactor, ensuring the stable operation of the sulfur replenishment process in the hydrogenation unit, and extending the service life of the hydrogenation catalyst and the operating cycle of the hydrogenation unit.

[0008] To achieve the above objectives, the first aspect of the present invention provides a sulfur replenishment system for a hydrogenation device.

[0009] Specifically, the sulfur replenishment system of the hydrogenation unit includes: A sulfur injection homogenization tank is used to receive liquid sulfur, a second homogenization oil, a first homogenized sulfurizing agent, and backwash oil filtrate, forming a homogenized sulfurizing agent therein; wherein, the sulfur injection homogenization tank includes a feed pipeline for receiving liquid sulfur, a feed pipeline for receiving the second homogenization oil, a circulation pipeline for receiving the homogenized sulfurizing agent, a feed pipeline for receiving the backwash oil filtrate, and a discharge pipeline for discharging the homogenized sulfurizing agent; Sulfur injection pumps are used to feed homogeneous vulcanizing agents to sulfur injection mixers and / or circulating sulfur homogenization tanks. The sulfur injection mixer is used to receive the feed oil and the second homogeneous sulfurizing agent and mix them to obtain the sulfur injection feed oil. A homogenizing oil heater is used to heat and raise the temperature of homogenized oil. The raw material oil filter is used to filter the raw material oil after sulfur injection; the raw material oil filter includes a first homogenization oil inlet pipeline, a sulfur injection raw material oil inlet pipeline, a pipeline for discharging supplementary sulfur raw material oil, and a discharge pipeline for discharging flushing oil containing solid particles. A backwash oil filter is used to receive and filter flush oil containing solid particles from a feed oil filter; it includes a sludge discharge line and a backwash oil filtrate discharge line.

[0010] Furthermore, the sulfur injection system also includes a sulfur melting tank in which solid sulfur is heated and melted to obtain liquid sulfur.

[0011] Furthermore, the raw sulfur in this invention can be liquid sulfur or solid sulfur. When using solid sulfur, a sulfur melting tank is set up before the sulfur injection homogenization tank to liquefy the solid sulfur before it enters the sulfur injection homogenization tank.

[0012] Furthermore, the sulfur homogenization tank is equipped with heating and heat tracing facilities, and preferably a heating tank with a stirring device is provided.

[0013] Furthermore, the sulfur injection mixer is a liquid-liquid mixer, preferably a pipeline mixer.

[0014] Furthermore, the raw oil filter is a filter with a backwashing function.

[0015] Furthermore, it is preferable to have two or more sets of the raw oil filter for switching between them.

[0016] Furthermore, the sulfur replenishment feedstock pipeline of the feedstock oil filter is preferably connected to the inlet pipeline of the feedstock oil hydrotreating booster pump.

[0017] Furthermore, the sulfur replenishment system also includes a sulfur injection regulating valve. This valve is located on the second sulfur injection agent pipeline at the outlet of the sulfur injection pump and is used to control the injection volume of homogeneous sulfurizing agent. The sulfur injection regulating valve controls the injection volume of sulfurizing agent based on the data signal from the hydrogen sulfide detector in the circulating hydrogen.

[0018] A second aspect of the present invention provides a method for replenishing sulfur in a hydrogenation device, wherein the sulfur replenishment system for the hydrogenation device described above is applied.

[0019] The sulfur replenishment method for the hydrogenation unit of the present invention includes the following steps: (1) Liquid sulfur first enters the sulfur homogenization tank and is fully mixed with the second homogenization oil to form a homogeneous sulfurizing agent. Then, after being pressurized by the sulfur injection pump, it is divided into two paths: the first path is circulated back into the sulfur homogenization tank to enhance the mixing and homogenization effect of liquid sulfur and homogenization oil; the second path enters the sulfur injection mixer through the sulfur injection regulating valve to control the flow rate. (2) Step (1) The homogeneous sulfurizing agent entering the sulfur injection mixer is mixed with the feed oil in the sulfur injection mixer and then enters the feed oil filter for treatment. The particulate impurities in the feed oil and some of the sulfur that precipitates during cooling are intercepted by the filter. The filtered oil enters the hydrogenation unit through the subsequent sulfur replenishment feed oil pipeline. (3) The particles trapped in the raw material oil filter in step (2) are periodically backwashed by the first homogenization oil. The flushing liquid (oil) enters the backwash oil filter. The trapped material in the backwash oil filter is treated as sludge discharge. The filtrate is returned to the sulfur injection homogenization tank for recycling.

[0020] Furthermore, when using solid sulfur, a sulfur melting tank is installed before the sulfur injection homogenization tank to liquefy the solid sulfur before it enters the sulfur injection homogenization tank.

[0021] Furthermore, the operating temperature of the sulfur homogenization tank in step (1) is 120-160℃.

[0022] Furthermore, the temperature of the homogenized oil after heat treatment in step (1) is 120-160℃.

[0023] Furthermore, in step (1), the mass ratio of homogenized oil to liquid sulfur is 2 / 1 to 20 / 1.

[0024] Furthermore, in step (1), the second-path sulfur injection regulating valve is controlled by the feedback signal of the hydrogen sulfide content in the circulating hydrogen of the reaction system, maintaining the hydrogen sulfide content in the circulating hydrogen of the reaction system at 300-1000 ppm, preferably 300-500 ppm.

[0025] Furthermore, the filtration accuracy of the raw oil filter in step (2) is 1 to 100 μm, preferably 2 to 50 μm.

[0026] Furthermore, in step (2), it is preferable to set two or more sets of raw oil filters and switch them according to the pressure difference between the inlet and outlet of the filter. When the pressure difference reaches the set value, such as when the pressure difference between the inlet and outlet is ≥0.05MPa, preferably 0.05~0.5MPa, the raw oil filter is backwashed, and the raw oil is switched to another raw oil filter.

[0027] Furthermore, the particles retained in the raw oil filter in step (3) are particulate impurities in the raw oil and are treated as waste oil sludge; the filtrate in the raw oil filter is homogenized oil and liquid sulfur, which are returned to the sulfur injection homogenization tank for recycling.

[0028] Furthermore, the homogenizing oil is an organic solvent or oil product that has sulfur-dissolving properties and does not introduce impurities into the hydrogenation process, such as benzene compounds, diesel oil, or fractionation tail oil. Preferably, the homogenizing oil is fractionation tail oil produced by the hydrogenation unit itself.

[0029] The sulfur replenishment system and method for hydrogenation units proposed in this invention can be used for sulfur replenishment in hydrogenation unit production, and is especially suitable for sulfur replenishment in the production process of low-sulfur and low-sulfur high-nitrogen feedstock oil hydrogenation, such as coal tar hydrogenation, wax oil hydrogenation, anthracene oil hydrogenation and other units.

[0030] The technical principle of sulfur replenishment in the hydrogenation unit proposed in this invention is as follows: Based on extensive experimental research, the inventors of this application discovered that feedstock oil has a certain solubility for sulfur. For the low-sulfur and high-nitrogen feedstock oil system such as coal tar, wax oil, and anthracene oil described in this invention, the solubility of sulfur in the feedstock oil at different temperatures was measured to be 0.5–8 g (sulfur) / 100 g (feedstock oil). To maintain the hydrogen sulfide content in the circulating hydrogen of the subsequent hydrogenation unit reaction system at 300–1000 ppm, only 0.06–0.21 g (sulfur) / 100 g (feedstock oil) needs to be injected to meet production requirements. Therefore, the sulfur-dissolving capacity of the feedstock oil can meet the actual sulfur demand. However, complete sulfur dissolution requires a certain amount of time, and when liquid sulfur at temperatures above 120°C is injected into a low-temperature (approximately 50°C) feedstock oil system, even with a high solubility in the feedstock oil, a certain proportion of sulfur will still precipitate out due to rapid cooling. Therefore, this invention, on the one hand, regulates the amount of sulfur injected through a sulfur injection homogenization and blending system to ensure that the amount of sulfur dissolved in the feedstock oil meets the sulfur replenishment requirements of the hydrotreating unit; on the other hand, through sulfur injection mixing and solids removal treatment, the low-temperature sulfur that has precipitated is first filtered by the feedstock oil filter, and then the feedstock oil filter is backwashed with high-temperature recycled homogenized oil to reuse the retained sulfur. This economically and efficiently delivers sulfur in dissolved form to the hydrotreating reactor continuously and smoothly, ensuring the long-term stable operation of the sulfur replenishment process in the hydrotreating unit.

[0031] Compared with the prior art, the present invention has the following beneficial effects: 1. This invention uses sulfur as a sulfurizing agent. Through a sulfur injection homogenization and blending system and sulfur injection mixing and solids removal treatment, the sulfurizing agent is continuously and smoothly transported to the hydrogenation reactor in an economical and efficient manner, ensuring the stable operation of the sulfur replenishment process in the hydrogenation unit, and extending the service life of the hydrogenation catalyst and the operating cycle of the hydrogenation unit.

[0032] 2. This invention utilizes a crude oil filter to first intercept particulate impurities and sulfur precipitated during cooling in the crude oil. Then, backwashing is used to separate the particulate impurities and sulfur from the crude oil. The homogenized oil and liquid sulfur are returned to the sulfur injection homogenization tank as filtrate for recycling. This solves the problem of solid particulate impurities in the crude oil while preventing lumpy sulfur from entering the subsequent system, ensuring long-term continuous and stable operation of the device.

[0033] 3. This invention controls and adjusts the injection amount of sulfiding agent by real-time monitoring of the hydrogen sulfide concentration in the circulating hydrogen, enabling precise online real-time sulfur replenishment of the hydrogenation unit. This avoids the risk of hydrogenation catalyst being reduced by hydrogen and has the advantages of flexible and accurate operation compared with traditional periodic sulfur replenishment. Attached Figure Description

[0034] Figure 1 This is a schematic diagram of the sulfur replenishment system of the hydrogenation device of the present invention.

[0035] In the diagram, the numbers correspond to: 1-Sulfur injection pipeline, 2-Sulfur injection homogenization tank, 3-Sulfur injection pump, 4-Sulfur injection mixer, 5-Hybridization oil heater, 6-1# feed oil filter, 7-2# feed oil filter, 8-Backflushing oil filter, 9-Sulfur injection regulating valve, 10-Feed oil pipeline, 11-Sulfur replenishment feed oil pipeline, 12-Hybridization oil supply pipeline, 13-First homogenization oil pipeline, 14-Second homogenization oil pipeline, 15-First sulfur injection agent pipeline, 16-Second sulfur injection agent pipeline, 17-Backflushing oil filtrate, 18-Sludge discharge pipeline. Detailed Implementation

[0036] The sulfur replenishment system and method of the hydrogenation device of the present invention will be described in detail below with reference to the accompanying drawings and embodiments, but this does not limit the present invention. Example 1

[0037] This embodiment provides a detailed description of the sulfur replenishment system of the hydrogenation device of the present invention.

[0038] like Figure 1 As shown, the present invention provides a sulfur replenishment system for a hydrogenation unit. The system includes a sulfur injection homogenization tank 2, a sulfur injection pump 3, a sulfur injection mixer 4, a homogenization oil heater 5, a No. 1 feed oil filter 6, a No. 2 feed oil filter 7, a backflushing oil filter 8, and a sulfur injection regulating valve 9.

[0039] The inlet of the sulfur homogenizing tank 2 is connected to the sulfur injection pipeline 1, and the outlet of the sulfur homogenizing tank 2 is connected to the inlet of the sulfur injection pump 3. The outlet of the sulfur injection pump 3 is divided into two paths: the first path, the sulfur injection agent pipeline 15, is connected to the sulfurizing agent circulation inlet of the sulfur homogenizing tank 2, and the second path, the sulfur injection agent pipeline 16, is connected to the sulfurizing agent inlet of the sulfur injection mixer 4.

[0040] The raw material oil inlet of the sulfur injection mixer 4 is connected to the raw material oil pipeline 10, and the outlet of the sulfur injection mixer 4 is connected to the sulfur replenishment raw material oil pipeline 11 after passing through the raw material oil filter 6 or 7.

[0041] The inlet of the homogenizing oil heater 5 is connected to the homogenizing oil supply pipeline 12; the outlet of the homogenizing oil heater 5 is divided into two paths: the first homogenizing oil pipeline 13 is connected to the backwash inlet of the raw material oil filter, and the second homogenizing oil pipeline 14 is connected to the homogenizing oil inlet of the sulfur injection homogenizing tank 2.

[0042] The backwash outlets of the raw material oil filters 6 and 7 are connected to the inlet of the backwash oil filter 8. The filtrate outlet of the backwash oil filter 8 is connected to the sulfur injection homogenization tank 2 via the backwash oil filtrate pipeline 17. The filter residue outlet of the backwash oil filter 8 is connected to the sludge discharge pipeline 18.

[0043] The sulfur injection regulating valve 9 is installed on the second sulfur injection agent 16 pipeline at the outlet of the sulfur injection pump 3. It is used to control and regulate the injection amount of homogeneous sulfurizing agent. The sulfur injection regulating valve controls the injection amount of homogeneous sulfurizing agent according to the data signal of the hydrogen sulfide detector in the circulating hydrogen. Example 2

[0044] This embodiment provides a detailed description of the sulfur replenishment method for the hydrogenation device of the present invention.

[0045] Combination Figure 1 The working process of the sulfur replenishment method for the hydrogenation device provided by the present invention is as follows: Liquid sulfur first enters the sulfur homogenization tank 2 and mixes thoroughly with the homogenization oil to form a homogeneous sulfurizing agent at 120-160℃. Then, it is pressurized by the sulfur injection pump 3 and divided into two paths: the first path is circulated back into the sulfur homogenization tank through the first sulfur injection agent pipeline 15 to enhance the mixing and homogenization effect of liquid sulfur and homogenization oil; the second path enters the sulfur injection mixer 4 through the second sulfur injection agent pipeline 16 and the flow rate is controlled by the sulfur injection regulating valve 9.

[0046] The homogeneous sulfurizing agent (temperature 120-160℃) entering the sulfur injection mixer 4 is mixed with the feed oil (temperature around 50℃), and the resulting sulfur injection feed oil enters the feed oil filter 6 for treatment. Particulate impurities in the feed oil and some sulfur precipitated during cooling are retained by the feed oil filter 6, and the filtered oil enters the sulfur replenishment feed oil pipeline 11 to enter the subsequent hydrogenation unit for sulfur replenishment. The retained particles in the feed oil filter 6 are periodically backwashed by the homogenization oil (temperature 120-160℃) of the first homogenization oil pipeline 13, and the flushing liquid enters the backflushing oil filter 8. The retained material in the backflushing oil filter 8 is treated as waste oil sludge, and the filtrate is returned to the sulfur injection homogenization tank 2 for recycling via the backflushing oil filtrate pipeline 17.

[0047] In the above process, the homogeneous sulfiding agent is prepared by mixing homogenizing oil and liquid sulfur at a mass ratio of 2 / 1 to 20 / 1. The injection amount of the sulfiding agent is adjusted by controlling the sulfur injection regulating valve 9 according to the hydrogen sulfide concentration data detected in the circulating hydrogen of the hydrogenation unit, maintaining the hydrogen sulfide content in the circulating hydrogen of the hydrogenation system at the operating requirement of 300–1000 ppm.

[0048] The above process utilizes the solubility of sulfur in the feedstock oil. Through the sulfur injection homogenization and blending system and the sulfur injection mixing and solids removal treatment, the amount of dissolved sulfur meets the sulfur replenishment requirements of the hydrogenation catalyst, while solving problems such as blockage caused by sulfur agglomeration during the sulfur injection process. It economically and efficiently delivers the sulfurizing agent continuously and smoothly to the hydrogenation reactor, ensuring the stable operation of the sulfur replenishment process in the hydrogenation unit.

[0049] Comparative Example 1 Sulfur is used as a sulfiding agent. After being melted, it is injected into the feedstock pipeline. The feedstock oil after sulfur injection is then pumped into the subsequent hydrotreating unit system. Directly injecting liquid sulfur at 120–160°C into the feedstock oil system at approximately 50°C will cause some sulfur crystallization due to the sudden temperature difference. The injected sulfur cannot be completely supplied smoothly to the subsequent hydrotreating unit. Furthermore, due to the lack of solids removal facilities, during long-term operation, the sulfur crystals will settle in the pipeline and slowly accumulate into clumps, easily causing blockage or even damage to the feedstock oil booster pump, affecting the continuous and stable operation of the unit.

Claims

1. A sulfur make-up system for a hydrogenation unit, characterized by, The supplementing sulfur system comprises: a sulfur injection homogenizing tank for receiving liquid sulfur, second route homogenized oil, first route homogenous sulfurizing agent and backwash oil filtrate, forming homogenous sulfurizing agent therein; wherein the sulfur injection homogenizing tank comprises a feed line for receiving liquid sulfur, a feed line for receiving second route homogenized oil, a circulation line for receiving homogenous sulfurizing agent, a feed line for receiving backwash oil filtrate, and a discharge line for discharging homogenous sulfurizing agent; a sulfur injection pump for feeding homogenous sulfurizing agent to a sulfur injection mixer and / or circulating back to the sulfur injection homogenizing tank; a sulfur injection mixer for receiving raw oil and homogenous sulfurizing agent and mixing to obtain sulfur-injected raw oil; a homogenized oil heater for heating homogenized oil; a raw oil filter for filtering sulfur-injected raw oil; the raw oil filter comprises a first route homogenized oil feed line, a sulfur-injected raw oil feed line, a line for discharging sulfur-supplemented raw oil, and a discharge line for discharging solid particle-containing flushing oil; a backwash oil filter for receiving and filtering solid particle-containing flushing oil from the raw oil filter; the backwash oil filter comprises a dirty oil discharge line and a backwash oil filtrate discharge line.

2. The sulfur makeup system of claim 1, wherein, The supplementing sulfur system further comprises a molten sulfur tank for heating and melting solid sulfur to obtain liquid sulfur.

3. The sulfur makeup system of claim 1, wherein, The sulfur injection homogenizing tank is provided with heating and heat tracing facilities, preferably a heating tank with stirring equipment.

4. The sulfur makeup system of claim 1, wherein, The sulfur injection mixer is a pipeline mixer; and / or The raw oil filter is a backwash filter.

5. The sulfur makeup system of claim 4, wherein, The raw oil filter is provided with two or more groups for switching use.

6. The sulfur supplementation system of claim 1, wherein, The sulfur-injected raw oil outlet line of the sulfur injection mixer is connected to the raw oil hydrogenation booster pump inlet line.

7. The sulfur supplementation system of claim 1, wherein, The supplementing sulfur system further comprises a sulfur injection regulating valve arranged on the second route sulfur injection agent line at the outlet of the sulfur injection pump for controlling the injection amount of homogenous sulfurizing agent.

8. A method of sulfur make-up for a hydrogenation unit, characterized by, The supplementing sulfur system of any one of claims 1-7 is applied.

9. The method of supplementing sulfur according to claim 8, wherein, The method comprises the following steps: (1) Liquid sulfur first enters the sulfur injection homogenizing tank, is fully mixed with homogenized oil to form homogenous sulfurizing agent, and is then boosted by the sulfur injection pump and divided into two routes: the first route is circulated back to the sulfur injection homogenizing tank to strengthen the mixing and homogenizing effect of liquid sulfur and homogenized oil; the second route enters the sulfur injection mixer through the sulfur injection regulating valve to control the flow rate; (2) The homogenous sulfurizing agent entering the sulfur injection mixer in step (1) is mixed with raw oil in the sulfur injection mixer and then enters the raw oil filter for treatment; the particulate impurities in the raw oil and part of the sulfur precipitated by cooling are intercepted by the filter, and the filtered oil enters the sulfur-injected raw oil line for subsequent treatment; (3) The intercepted particles in the raw oil filter in step (2) are periodically treated by backwashing with homogenized oil; the flushing liquid enters the backwash oil filter; the intercepted substances in the backwash oil filter are treated as dirty oil for discharge; and the filtrate is returned to the sulfur injection homogenizing tank for circulation.

10. The method of supplementing sulfur according to claim 9, wherein The operating temperature of the sulfur injection homogenizing tank in step (1) is 120-160°C; and / or The temperature of the homogenized oil after heating treatment in step (1) is 120-160°C.

11. The method of supplementing sulfur according to claim 9, wherein The mass ratio of homogenized oil to liquid sulfur in step (1) is 2 / 1-20 / 1.

12. The method of supplementing sulfur according to claim 9, wherein The sulfur injection regulating valve of the second route in step (1) is controlled by feedback of the hydrogen sulfide content signal in the reaction system circulating hydrogen to maintain the hydrogen sulfide content in the reaction system circulating hydrogen at 300-1000 ppm, which is the operation requirement.

13. The method of supplementing sulfur according to claim 9, wherein The filtering precision of the raw oil filter in step (2) is 1-100 microns.

14. The method of supplementing sulfur according to claim 9, wherein The homogenized oil is an organic solvent or oil product that has the property of dissolving sulfur and does not introduce impurities into the hydrogenation process.

15. The method of making sulfur supplements of claim 14, wherein, The homogenized oil is a self-produced fractionation tail oil of the hydrogenation device.

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