Passivation method of sulfuration type hydrocracking catalyst and passivated hydrocracking catalyst
By using NH3 to passivate the sulfidation-type hydrocracking catalyst under an inert atmosphere, the risk of self-heating of the catalyst during storage, transportation and loading is solved, the passivation process is simplified, safety and economy are improved, and product quality is maintained.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-28
- Publication Date
- 2026-03-10
AI Technical Summary
Existing sulfurized hydrocracking catalysts are susceptible to oxidation during storage, transportation, and loading, leading to self-heating or combustion. Furthermore, existing passivation methods are complex, costly, or can affect product quality.
NH3 is used as a passivation gas to treat the sulfide-state hydrocracking catalyst under an inert atmosphere, forming a tight adsorption layer to prevent the active components of the catalyst from reacting with oxygen and simplifying the passivation process.
It improves the safety of catalyst storage, transportation and loading, simplifies the start-up process, reduces start-up time and cost, and maintains product quality.
Smart Images

Figure SMS_1
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of petroleum chemical industry, and particularly relates to a passivation method of a sulfided hydrocracking catalyst and the hydrocracking catalyst after passivation. BACKGROUND
[0002] In recent years, the demand for clean fuel is increasing in various countries, and the hydrogenation process is one of the most effective means for producing clean fuel, and the high-efficiency hydrogenation catalyst is the key to the process. The conventional hydrogenation catalyst is in an oxidized state, and the real active substance in actual use is in a sulfided state, so it needs to be sulfided before use. At present, the most common ones are in-situ presulfurization and ex-situ presulfurization technologies. The ex-situ presulfurization technology can be divided into two types according to the existing state of the metal on the catalyst: one is that in the ex-situ presulfurization process, the active metal on the catalyst forms a complex or an oxysulfide with a sulfiding agent, that is, the ex-situ presulfurization technology of sulfur-carrying type. The other is that the catalyst is completely sulfided outside the reactor to generate high-activity metal sulfide, and then passivated for safe storage, transportation and loading, that is, the ex-situ presulfurization technology of complete type.
[0003] The activity and stability of the sulfided catalyst are higher than those of the oxidized catalyst. The metal sulfide may produce concentrated heat release and even spontaneous combustion phenomenon when contacting with oxygen, which requires that the catalyst must be isolated from air, so the catalyst needs to be passivated after presulfurization to prevent the metal sulfide in the pores of the catalyst from being oxidized.
[0004] The passivation technology is generally divided into gas passivation and liquid passivation. The gas passivation mainly uses O2 and other oxidizing gases to oxidize the surface of the reduced catalyst at a certain temperature to form a dense oxide film to protect the inside of the catalyst from being oxidized by air. Or use mercaptan, sulfide, carbon disulfide and other gases to adsorb on the surface of the catalyst and combine with the active components of the catalyst, so as to prevent the active components of the catalyst from reacting with O2 and water in the air to release heat and deactivate. The liquid passivation mainly uses organic hydrocarbons to form a protective layer on the surface of the catalyst by spraying, dipping and stirring methods.
[0005] As disclosed in Chinese patent document CN109675643A, after the hydrogenation catalyst is sulfided, it is passivated by using distillate oil or oxygen-containing substances. The protective film formed by the liquid passivation agent can be removed during the reaction, but the recovery of the removed liquid may cause trouble to the refinery, and after being mixed with the introduced raw oil, it may affect the quality of the product.
[0006] Chinese patent document CN113509964A discloses a passivation method of sulfided hydrocracking catalyst, comprising: loading sulfur compounds and nitrogen compounds onto the sulfided hydrocracking catalyst, and then performing passivation treatment; the passivation treatment atmosphere can be an inert atmosphere or an oxygen-containing atmosphere with an oxygen content of 0.1-21% by volume or air, and the inert atmosphere is selected from an atmosphere containing one or more of nitrogen, helium and argon. Loading nitrogen compounds on the surface of the catalyst can maximize the passivation effect of nitrides, and has the advantages of resource saving, low carbon and environmental protection. However, the introduction of nitrogen compounds may introduce new impurities into the reaction system, affecting the quality of the product.
[0007] Chinese patent document CN113117761A discloses a method for passivation treatment of sulfided hydrogenation catalyst, which adopts gas phase passivation and liquid phase passivation in combination. First, the sulfided hydrogenation catalyst is contacted with a liquid passivation agent, then the obtained solid material is separated and heat treated to obtain material A; the obtained material A is treated under vacuum to obtain material B; the obtained material B is further treated in the presence of ozone-containing gas, and finally the passivated catalyst is obtained after cooling under nitrogen or inert atmosphere. The liquid passivation agent is anthraquinone, furan, dihydroquinoline, tetrahydroquinoline and other organic compounds containing lone pair electrons or electron-donating groups, and the gas passivation agent is ozone. The passivation protection effect of this method is good, but two kinds of passivation agents are used, and the use cost is high.
[0008] Chinese patent document CN113117763A discloses a passivation method of sulfided hydrogenation catalyst. First, the sulfided hydrogenation catalyst is placed in a sealed container, the container is vacuumed and cooled, and then nitrogen or carbon dioxide is introduced for treatment; then the obtained material is subjected to warming treatment, and finally ozone is used as a passivation gas for passivation treatment. The passivation process is divided into two stages, wherein the first stage passivation temperature is preferably-30 to-5℃, and the ozone content in the passivation gas is preferably 1-20% by volume; the second stage passivation temperature is preferably-5 to 20℃; and the ozone content in the passivation gas is preferably 0.2-30% by volume. The method uses ozone to passivate the catalyst at low temperature, so that a dense oxidation layer is formed on the surface of the catalyst, preventing the oxygen in the air from further reacting with the metal sulfides in the pores of the catalyst, avoiding the self-heating reaction of the catalyst, and improving the safety of catalyst storage, transportation and loading. However, this passivation method is relatively complicated. SUMMARY
[0009] In view of the problems in the prior art, the present application provides a passivation method for a sulfided hydrocracking catalyst, which uses NH3 to passivate the catalyst so that the NH3 is adsorbed on the surface of the catalyst and combined with the active components of the catalyst, thereby preventing the active components of the catalyst from reacting with O2 and water in the air to release heat and deactivate, greatly avoiding the self-heating reaction of the catalyst and improving the safety of the storage, transportation and loading of the catalyst. The entire passivation process is simple in operation and low in cost, and does not affect the product quality. At the same time, the adsorbed NH3 can be removed by directly heating to the reaction temperature during the start-up of the hydrogenation device, and the NH3 only undergoes the adsorption process and can be removed by heating, without generating additional impurities. Moreover, the catalyst sulfuration and passivation processes in the existing start-up process are eliminated, the start-up time is greatly saved, the safety of the start-up is improved, the operation is simple, and the environment is friendly.
[0010] To achieve the above-mentioned purposes, the present application adopts the following technical solutions:
[0011] A passivation method for a sulfided hydrocracking catalyst, comprising the following steps:
[0012] After the sulfided hydrocracking catalyst is treated in an inert gas atmosphere, it is heated and introduced into a passivation gas for passivation treatment; the passivation gas comprises NH3.
[0013] In an optional embodiment, the passivation gas further comprises an inert gas which has no interaction with the hydrocracking catalyst and NH3.
[0014] In an optional embodiment, the volume content of NH3 in the passivation gas is 5%-50%.
[0015] In an optional embodiment, the inert gas is selected from nitrogen and / or carbon dioxide gas.
[0016] In an optional embodiment, after heating to the passivation treatment temperature, the passivation gas is introduced.
[0017] In an optional embodiment, the pressure of the passivation gas is 0.1-0.2 MPa, preferably 0.1-0.15 MPa.
[0018] In an optional embodiment, the passivation gas is flowing, and the flow rate of the passivation gas is 300-90000 mL / h, preferably 600-20000 mL / h, and more preferably 1000-10000 mL / h.
[0019] In an optional embodiment, the temperature of the passivation treatment is 40-110℃.
[0020] In an optional embodiment, the time of the passivation treatment is 20-100 min.
[0021] In an alternative embodiment, the temperature for treating the sulfided hydrocracking catalyst in the inert gas atmosphere is 20-30℃, the pressure is 0.1-0.2 MPa, and the time is 1-3 h.
[0022] In an alternative embodiment, the sulfided hydrocracking catalyst is treated in the inert gas atmosphere at a pressure of 0.1-0.15 MPa.
[0023] In an alternative embodiment, when the sulfided hydrocracking catalyst is treated in the inert gas atmosphere, the flow rate of the inert gas is 300-90000 mL / h.
[0024] In the passivation method of the sulfided hydrocracking catalyst described above, the sulfided hydrocracking catalyst is not particularly limited and can be prepared by a conventional method, such as first preparing an oxidized hydrocracking catalyst and then sulfidizing the oxidized hydrocracking catalyst to obtain the sulfided hydrocracking catalyst. Alternatively, the sulfided hydrocracking catalyst can be directly prepared during the preparation of the hydrocracking catalyst. Generally, the hydrocracking catalyst is prepared by using an inorganic refractory oxide as a carrier and using metals of Group VIII and Group VIB as active metal components. The metal of Group VIII is selected from Ni and / or cobalt, and the metal of Group VIB is selected from Mo and / or W. The inorganic refractory oxide is generally one or more of alumina, silica, and molecular sieve. The content of the metal of Group VIII is 0.5%-12% by element, and the content of the metal of Group VIB is 5%-35% by element, based on 100% by weight of the sulfided hydrocracking catalyst. The hydrocracking catalyst can also contain an auxiliary component, which is generally one or more of phosphorus, fluorine, titanium, zirconium, and boron, and the content of the auxiliary component is generally 30 wt% or less in the sulfided hydrocracking catalyst.
[0025] The present application also provides a passivated sulfided hydrocracking catalyst obtained by the passivation method of the sulfided hydrocracking catalyst described above.
[0026] Compared with the prior art, the present application has at least the following beneficial effects:
[0027] Beneficial effect 1: the sulfided catalyst with high specific surface area has high oxygen affinity, is unstable when exposed to air, and generates SO2 and heat when encountering O2, and has a tendency to self-heat or burn below 200℃. The passivation method of the sulfided hydrocracking catalyst provided by the present application is simple and flexible to operate, and has small equipment investment. The sulfided hydrocracking catalyst obtained after passivation treatment can directly remove the adsorbed NH3 when heated to the reaction temperature in the start-up of the hydrogenation device, thereby eliminating the catalyst sulfuration and passivation process in the existing start-up process, greatly saving the start-up time, and reducing the start-up activity of the catalyst. There is no obvious heat release phenomenon during the heating process, and the operation is simple and friendly to the environment. Moreover, the passivated hydrogenation catalyst can be stably stored in air and basically does not have a self-heating / self-combustion reaction, and can be stored, transported and loaded under natural conditions, which is the same as the oxidized catalyst.
[0028] Beneficial effect 2: the passivation method of the sulfided hydrocracking catalyst provided by the present application first pretreats the sulfided hydrocracking catalyst by contacting it with nitrogen, and then reduces it to room temperature (20-30℃) under the protection of nitrogen, so that the gas in the pores continues to be adsorbed on the active sites. Then, passivation treatment is performed. The passivation treatment is only performed on the surface of the catalyst, and NH3 is adsorbed on the surface of the catalyst, first forms physical adsorption with the acid sites on the surface of the molecular sieve and reacts with the acid sites on the surface of the molecular sieve to form ionic bonds, and then gradually releases to the surface of the molecular sieve and reacts with more acid sites until it is completely released or reaches a certain stable state, completing the passivation of the acid sites. The combination of NH3 and the active sites of the catalyst is more close compared with the existing passivation gas, thereby preventing the active components of the catalyst from reacting with O2 and water in the air to release heat and deactivate; and the self-heating reaction of the catalyst is avoided to a great extent, and the safety of the storage, transportation and loading of the catalyst is improved. Moreover, the nitrogen used is an inert gas, does not react with the catalyst, and is easy to remove, and has no impact on the environment. DETAILED DESCRIPTION
[0029] The present application will be described in detail below by way of examples. It is necessary to point out here that the following examples are only used to further illustrate the present application, and cannot be understood as limiting the protection scope of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application according to the above content of the present application.
[0030] The specific experimental steps or conditions are not specified in the examples, and can be performed according to the conventional experimental steps described in the literature in the art. The reagents or instruments used are not specified by the manufacturer, and are conventional reagent products that can be obtained by purchase.
[0031] The existing vulcanization methods can meet the implementation of the technical scheme of the present application, but for the convenience of comparison, the following all adopt the hydrogen cracking catalyst PHC-05 produced industrially, and are vulcanized according to the following method:
[0032] H2S is introduced into the system, the H2S concentration is kept at about 0.6v%, the gas volume space velocity is 300h -1 The bed temperature of the hydrogen cracking catalyst is raised to 230℃ at a temperature raising rate of 10℃ / min, kept for 16h, then raised to 290℃ at a temperature raising rate of 10℃ / min, kept for 8h, and finally raised to 370℃ at a temperature raising rate of 10℃ / min, kept for 8h, that is, the pre-vulcanization of the hydrogen cracking catalyst is completed.
[0033] Example 1
[0034] The hydrogen cracking catalyst PHC-05 produced industrially is vulcanized according to the above method, and the obtained vulcanized hydrogen cracking catalyst is placed in a closed container, vacuumed, and then the gas is switched to nitrogen and the closed container is cooled to 20℃, the nitrogen gas pressure is controlled to be 0.15MPa, the flow rate is 6000mL / h, and the treatment is carried out for 3h; the nitrogen is closed. The temperature is raised to 100℃, nitrogen containing 5% NH3 is introduced (passivation gas), the passivation gas pressure is controlled to be 0.15MPa, the flow rate is 600mL / h, and the passivation is kept for 0.5h, and the passivated vulcanized hydrogen cracking catalyst A is obtained. After replacement with nitrogen, it is taken out and used.
[0035] Example 2
[0036] The hydrogen cracking catalyst PHC-05 produced industrially is vulcanized according to the above method, and the obtained vulcanized hydrogen cracking catalyst is placed in a closed container, vacuumed, and then the gas is switched to nitrogen and the closed container is cooled to 25℃, the nitrogen gas pressure is controlled to be 0.12MPa, the flow rate is 9000mL / h, and the treatment is carried out for 2h; the nitrogen is closed. The temperature is raised to 80℃, carbon dioxide containing 15% NH3 is introduced (passivation gas), the passivation gas pressure is controlled to be 0.12MPa, the flow rate is 1000mL / h, and the passivation is kept for 0.6h, and the passivated vulcanized hydrogen cracking catalyst B is obtained. After replacement with nitrogen, it is taken out and used.
[0037] Example 3
[0038] Take the industrial production of hydrocracking catalyst PHC-05, according to the above method vulcanization, the vulcanized state of the hydrocracking catalyst obtained in a sealed container, vacuum after switching gas for nitrogen and the sealed container to 30 ℃, control the nitrogen gas pressure of 0.2 MPa, flow 9000 mL / h, 2.5 hours after treatment; nitrogen. Increase the temperature to 60 ℃, introduce 30% NH3containing nitrogen (passivation gas), control the passivation gas pressure of 0.2 MPa, flow 1000 mL / h, keep 0.8 h, the passivated vulcanized type hydrocracking catalyst C, nitrogen replacement after switching in it is taken out for use.
[0039] Example 4
[0040] Take the industrial production of hydrocracking catalyst PHC-05, according to the above method vulcanization, the vulcanized state of the hydrocracking catalyst obtained in a sealed container, vacuum after switching gas for nitrogen and the sealed container to 30 ℃, control the nitrogen gas pressure of 0.2 MPa, flow 9000 mL / h, 2.5 hours after treatment; nitrogen. Increase the temperature to 60 ℃, introduce 30% NH3containing nitrogen (passivation gas), control the passivation gas pressure of 0.2 MPa, flow 1000 mL / h, keep 0.8 h, the passivated vulcanized type hydrocracking catalyst C, nitrogen replacement after switching in it is taken out for use.
[0041] Example 5
[0042] Take the industrial production of hydrocracking catalyst PHC-05, according to the above method vulcanization, the vulcanized state of the hydrocracking catalyst obtained in a sealed container, vacuum after switching gas for nitrogen and the sealed container to 30 ℃, control the nitrogen gas pressure of 0.2 MPa, flow 9000 mL / h, 2.5 hours after treatment; nitrogen. Increase the temperature to 60 ℃, introduce 30% NH3containing nitrogen (passivation gas), control the passivation gas pressure of 0.2 MPa, flow 1000 mL / h, keep 0.8 h, the passivated vulcanized type hydrocracking catalyst C, nitrogen replacement after switching in it is taken out for use.
[0043] Example 6
[0044] Take the industrial production of hydrocracking catalyst PHC-05, according to the above method vulcanization, the resulting vulcanized state of the hydrocracking catalyst placed in a sealed container, vacuum after switching to nitrogen gas and the sealed container to 25 ℃, control the pressure of nitrogen gas 0.11 MPa, flow 6000 mL / h, 3 hours after treatment; nitrogen. Elevated temperature to 80 ℃, introducing 45% NH3 containing nitrogen (passivation gas), control passivation gas pressure of 0.17 MPa, flow 5000 mL / h, 0.5 h, the resulting passivated vulcanized hydrocracking catalyst F, nitrogen replacement after switching it out for standby.
[0045] Example 7
[0046] Take the industrial production of hydrocracking catalyst PHC-05, according to the above method vulcanization, the resulting vulcanized state of the hydrocracking catalyst placed in a sealed container, vacuum after switching to nitrogen gas and the sealed container to 25 ℃, control the pressure of nitrogen gas 0.11 MPa, flow 6000 mL / h, 3 hours after treatment; nitrogen. Elevated temperature to 80 ℃, introducing 45% NH3 containing nitrogen (passivation gas), control passivation gas pressure of 0.17 MPa, flow 5000 mL / h, 0.5 h, the resulting passivated vulcanized hydrocracking catalyst F, nitrogen replacement after switching it out for standby.
[0047] Comparative Example 1
[0048] This example is similar to example 2, the only difference is the use of different passivation gas, the passivation gas used in this example is 2% oxygen containing carbon dioxide, the final passivated vulcanized hydrocracking catalyst H.
[0049] Comparative Example 2
[0050] This example is similar to example 2, the only difference is the use of different passivation gas, the passivation gas used in this example is 0.5% oxygen containing nitrogen, the final passivated vulcanized hydrocracking catalyst I.
[0051] Experimental Example 1 Exothermicity Evaluation Test
[0052] The catalysts obtained in examples 1-7 and comparative examples 1-2, and catalyst 1# (not passivated, only according to the above method vulcanized catalyst PHC-05) were subjected to exothermic test under air, the specific process as follows:
[0053] Take catalyst 25g, put into self-heat material tester, heat to 150℃, constant temperature 3 hours, investigate the exothermic situation of catalyst in air, the result is listed in table 1, wherein catalyst 2# represents catalyst without passivation treatment.Self-heat material tester is the device for measuring the oxidation exothermic of material, the measuring chamber keeps adiabatic state, the oxidation exothermic of material can be monitored by the thermocouple inserted therein.The more temperature increases, the more exothermic.
[0054] Table 1 exothermic result of catalyst
[0055] Catalyst No. Temperature, °C Catalyst 1 0.8 Catalyst A — Catalyst B — Catalyst C — Catalyst D — Catalyst E — Catalyst F — Catalyst G — Catalyst H 0.15 Catalyst I 0.25
[0056] From the data in the above table, the passivated sulfided hydrocracking catalyst obtained by the passivation method provided by the application does not increase temperature after constant temperature at 150℃ for 3 hours, which shows that the passivated catalyst obtained by the passivation method provided by the application is well protected, thereby preventing the reaction of catalyst active components with O2 and water in air to generate exothermic and deactivation, avoiding the self-heating reaction of catalyst to a great extent, and improving the safety of catalyst storage, transportation and loading.The passivation method is relatively mild, and does not generate other impurities.In addition, it also reduces the start-up activity.
[0057] Without passivation (catalyst 1#), or using carbon dioxide containing 2% oxygen as passivation gas for passivation (comparative example 1), or using nitrogen containing 0.5% oxygen as passivation gas for passivation (comparative example 2), all have exothermic phenomenon after constant temperature at 150℃ for 3 hours, which shows that the catalyst without passivation, using conventional passivation gas for passivation or omitting the inert gas treatment step is not safe in the process of storage, transportation and loading.
[0058] Experimental example 2 activity evaluation of catalyst
[0059] The activity and stability of the passivated catalysts obtained by conventional sulfidation passivation catalyst 2# and examples 1-7 and comparative examples 1-2 are evaluated, and the evaluation test is carried out on a 200mL fixed bed hydrogenation treatment device.The raw material oil for evaluation is the hydrogenation cracking raw material of a certain petrochemical company (distillation range 224-556℃, density (20℃) 0.9066g / cm 3 , S content 6500μg / g, N content 1620μg / g), the process conditions are as follows: reaction pressure 15.0MPa, volume space velocity 1.5h -1 , cracking reaction temperature 372℃, hydrogen / oil ratio 1200.The evaluation results are shown in table 2.
[0060] The preparation method of the above conventional sulfidation passivated catalyst 2# includes the following steps:
[0061] The industrial production of hydrocracking catalyst PHC-05 is loaded into a reactor, and after air tightness is qualified, the pressure is increased to 3.0 MPa, the temperature is increased to 150 ℃ at a rate of 30 ℃ / h, the sulfurizing oil is introduced, the sulfurizing oil is catalytic gasoline, and CS2 is used as the sulfurizing agent, the sulfurizing agent content in the sulfurizing oil is 2 wt%, the distillation range is 40-200 ℃, the temperature is continuously increased to 230 ℃, and the temperature is kept constant for 3 h, then the temperature is increased to 350 ℃, and the temperature is kept constant for 3 h, to obtain the sulfided state hydrocracking catalyst a. The sulfided state hydrocracking catalyst a is sprayed with dodecene under the protection of nitrogen, the amount of dodecene is 30% (V) of the catalyst, the temperature is increased to 150 ℃, nitrogen is used for blowing, the flow rate of nitrogen is 50 L / h, after blowing for 5 h, the temperature is decreased to room temperature, the container containing the catalyst is vacuumized, the vacuum degree is -0.05 MPa, then the temperature is slowly decreased to 0 ℃, the ozone-containing gas (the ozone-containing gas is nitrogen containing 2% ozone) is introduced, the gas pressure is 1.0 MPa, the flow rate is 10 L, and the ozone-containing gas is kept for 0.5 h, to obtain the conventional sulfided and passivated catalyst 2#.
[0062] Table 2 evaluation results of the catalyst
[0063]
[0064] From the data in the above table, it can be seen that the catalytic performance of the passivated catalyst obtained by the passivation method provided by the present application is not affected. In comparison, the overall product yield, especially the light and heavy naphtha product yield, of the catalysts H and I obtained by using carbon dioxide containing 2% oxygen as the passivation gas (comparative example 1) and by using nitrogen containing 0.5% oxygen as the passivation gas (comparative example 2) is slightly lower, which indicates that the passivation method provided by the present application also has certain benefits in improving the cracking activity. By using NH3 to passivate the catalyst and adsorbing it on the surface of the catalyst, the active components in the catalyst are combined together, so that the reaction of the active components in the catalyst with O2 and water in the air is prevented, the exothermic and deactivation of the catalyst is avoided to a great extent, the self-heating reaction of the catalyst is avoided to a great extent, and the safety of storage, transportation and loading of the catalyst is improved. The whole passivation process is simple in operation and low in cost, and the product quality is not affected, the reaction activity of the catalyst is high, and the catalyst does not need to be sulfided or activated when the hydrocracking device is started, and the catalyst can be directly used for oil start-up, which simplifies the start-up steps and shortens the start-up time of the hydrogenation device.
[0065] Of course, the present application also has other various embodiments and deformations, and those skilled in the art can make various corresponding changes and deformations according to the present application without departing from the spirit and essence of the present application, but these corresponding changes and deformations should belong to the protection scope of the claims of the present application.
Claims
1. A method for passivating a sulfided hydrocracking catalyst, characterized in that, The method comprises the following steps: The sulfided hydrocracking catalyst is treated in an inert gas atmosphere, heated and introduced into a passivation gas for passivation treatment; the passivation gas comprises NH3.
2. The passivation method according to claim 1, characterized in that, The passivation gas further comprises an inert gas; The inert gas is selected from nitrogen and / or carbon dioxide gas.
3. The passivation method according to claim 2, wherein The volume content of NH3 in the passivation gas is 5%-50%.
4. The passivation method of claim 1, wherein, After heating to the passivation treatment temperature, the passivation gas is introduced again.
5. The passivation method of claim 1, wherein, The pressure of the passivation gas is 0.1-0.2 MPa, preferably 0.1-0.15 MPa.
6. The passivation method of claim 1, wherein, The passivation gas is flowing, and the flow rate of the passivation gas is 300-90000 mL / h, preferably 600-20000 mL / h, more preferably 1000-10000 mL / h.
7. The passivation method of claim 1, wherein, The temperature of the passivation treatment is 40-110℃; The time of the passivation treatment is 20-100 min.
8. The passivation method of claim 1, wherein, The sulfided hydrocracking catalyst is treated in an inert gas atmosphere at a temperature of 20-30℃, a pressure of 0.1-0.2 MPa and a time of 1-3 h.
9. The passivation method of claim 1 wherein, When treated in the inert gas atmosphere, the flow rate of the inert gas is 3000-20000 mL / h.
10. A passivated sulfided hydrocracking catalyst obtained after the passivation method of the sulfided hydrocracking catalyst according to any one of claims 1-9.
Citation Information
Patent Citations
Preparation method of vulcanized catalyst, vulcanized catalyst and application of vulcanized catalyst
CN109675643A
Method for passivating sulfurized hydrogenation catalyst
CN113117761A
Passivation method of sulfuration type hydrogenation catalyst
CN113117763A
Passivation method of sulfuration type hydrocracking catalyst
CN113509964A