CN111088073A - Hydrocracking method for catalytic diesel oil - Google Patents
Hydrocracking method for catalytic diesel oil Download PDFInfo
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- CN111088073A CN111088073A CN201811244750.8A CN201811244750A CN111088073A CN 111088073 A CN111088073 A CN 111088073A CN 201811244750 A CN201811244750 A CN 201811244750A CN 111088073 A CN111088073 A CN 111088073A
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- 238000004517 catalytic hydrocracking Methods 0.000 title claims abstract description 92
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- -1 ammonium ions Chemical class 0.000 claims description 4
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- 239000000377 silicon dioxide Substances 0.000 claims description 4
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- 239000010941 cobalt Substances 0.000 claims description 3
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- VLXBWPOEOIIREY-UHFFFAOYSA-N dimethyl diselenide Natural products C[Se][Se]C VLXBWPOEOIIREY-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004821 distillation Methods 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004904 shortening Methods 0.000 abstract description 2
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- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 6
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a hydrocracking method for catalytic diesel oil, which comprises the following steps: (1) the catalytic diesel raw material enters a hydrofining reactor to contact with a hydrofining catalyst for reaction, and the reaction effluent enters a high-pressure separator; (2) the high-pressure gas obtained from the upper part of the high-pressure separator is subjected to desulfurization treatment and then circulated back to the hydrofining reactor or directly enters the hydrocracking reactor without being subjected to desulfurization treatment, and the liquid phase obtained from the middle lower part of the high-pressure separator enters the low-pressure separator; (3) the liquid phase obtained from the middle lower part of the low-pressure separator enters a fractionating tower and is fractionated to obtain dry gas, liquefied gas, light naphtha, heavy naphtha and tail oil; (4) the tail oil enters a hydrocracking reactor to contact with a hydrocracking catalyst for hydrocracking reaction, and the reaction effluent enters a high-pressure separator. H of hydrofining reactor and hydrocracking reactor through sectional control2S and NH3Concentration, thereby achieving the purposes of shortening the stable time in the initial start-up period and prolonging the running period of the device.
Description
Technical Field
The invention relates to a hydrocracking method of catalytic diesel oil, in particular to a method for producing high-octane gasoline or aromatic hydrocarbon by hydrocracking the catalytic diesel oil.
Background
The hydrocracking technology has the characteristics of high production flexibility, strong raw material adaptability and high product quality, and plays a role of a medium-flow column in the aspect of adjusting the production balance of a whole plant. The products of the hydrocracking process include natural gas, liquefied gas, naphtha, jet fuel, diesel, and tail oil. The raw oil of the traditional hydrocracking process technology is mainly conventional wax oil, and the product is mainly naphtha or middle distillate oil.
The polycyclic aromatic hydrocarbons are more and more brought by crude oil heaving and deterioration, the allowable content of the polycyclic aromatic hydrocarbons is less and less by improving the quality of diesel oil products, and how to efficiently convert the polycyclic aromatic hydrocarbons in oil products is one of the great challenges faced by the petroleum refining industry. The catalytic cracking process is one of the most important crude oil secondary processing means, and the status thereof is irreplaceable in a refining enterprise from the aspects of processing capacity and economy. In recent years, the processing capacity of a catalytic cracking unit in China exceeds 1.7 hundred million tons per year, the yield of catalytic diesel oil reaches 3500 million tons per year, and the catalytic diesel oil accounts for more than 20 percent of the yield of the diesel oil. However, the process is a process for increasing the polycyclic aromatic hydrocarbon, and the content of the polycyclic aromatic hydrocarbon in the produced diesel oil is very high (the content of the bicyclic aromatic hydrocarbon and the polycyclic aromatic hydrocarbon is generally more than 50%), so that the complete combustion performance of the produced diesel oil is poor (the density is high and the cetane number is low). The conventional hydrofining method is adopted to process the catalytic diesel oil, so that the processing difficulty is high, the diesel oil product cannot meet the five national standards, and the key problem of upgrading the product quality of a refining enterprise is how to process the catalytic diesel oil or efficiently convert the catalytic diesel oil.
For diesel fractions, a high aromatics content is disadvantageous, but for naphtha fractions, naphtha fractions with a high aromatics content can be used as high octane gasoline blending components, and naphtha fractions with a high potential aromatics content are high quality catalytic reforming feedstocks. Therefore, if the aromatic hydrocarbon in the catalytic diesel oil can be partially converted and retained in naphtha fraction, the aromatic hydrocarbon rich in the catalytic diesel oil can be effectively utilized to produce naphtha products with high added value, the quality of the diesel oil can be improved, and the difficulty in upgrading the quality of the factory diesel oil products of refining enterprises can be reduced, so that an economic and effective processing way is provided for the high-aromatic hydrocarbon catalytic diesel oil.
At present, the hydrocracking technology is adopted to convert the catalytic cracking light cycle oil into ultra-low sulfur diesel oil and a high octane number gasoline blending component in foreign countries. Such as: NPRA annual meeting in 1995, David a. Pappal et al introduced a single stage hydrocracking process technology developed by Mobil, Akzo Nobel/Nippon Ketjen and m.w. Kellogg companies; the 2005 annual meeting of NPRA, Vasant P. Thakkar et al introduced the LCO Unicraking technology developed by UOP. Both of the above techniques have been reported to convert low value catalytic cycle oil components into high octane gasoline components and premium diesel blending components. In China, the technology of FD2G (FRIPP) for producing high-octane naphtha by catalytic diesel oil conversion is successfully applied to three sets of devices for medium petrochemical industry. Because the technology is initially applied, an industrial device usually adopts a single-stage series flow, and the conventional process flow mainly faces the following three problems. Firstly, in the initial operation stage of the catalytic diesel conversion device, the initial activity of the hydrofining catalyst is high, the aromatic saturation capacity and the desulfurization and denitrification performance are good, the hydrogenation performance of the hydrocracking agent is also good, at the moment, the aromatic content in the gasoline component is low, the octane number is not high, the production requirement cannot be met, and the gasoline component can be qualified after being stabilized for a certain time. Secondly, the temperature at the inlet and outlet of the refining reactor is not matched with the temperature at the initial and final stages of the cracking reactor. The initial activity of the hydrofining agent at the initial startup is higher, the temperature at the inlet and outlet is lower than that of normal production, and the inlet temperature of the cracking reactor is lower due to the fact that a heating device is not arranged between the refining reactor and the cracking reactor, so that the target temperature cannot be reached. However, at the end of the start-up period, the catalyst is deactivated faster than the cracking performance, so that the activity of the refining agent is insufficient. On the premise of ensuring that refined nitrogen is qualified, the outlet temperature of the refining reactor is too high, and the inlet temperature of the cracking reactor cannot be reduced to the normal reaction temperature through cold hydrogen, so that the device must be shut down. Finally, the pressure grade of the diesel catalytic device is low, and the content of sulfur and nitrogen in the catalytic diesel is high, so that the hydrogen partial pressure of a cracking reactor is low, the ammonia concentration is too high, and the activity of the hydrocracking catalyst is not favorably exerted.
In hydrocracking technology, there are many reports on hydrocracking methods and technologies, but there are few reports on the aspect of producing high-octane gasoline or aromatic hydrocarbons by hydrocracking catalytic diesel. CN 103865577A discloses a method for producing light aromatic hydrocarbon and clean fuel oil from catalytic cracking diesel oil. The method adopts a hydrocracking-hydrofining reverse process, the hydrofined catalytic diesel distillate oil is cut, wherein the distillate oil with the temperature of more than 355 ℃ is mixed with hydrogen and then returns to perform hydrocracking; extracting cut distillate oil, and taking paraffin-rich raffinate oil as a clean diesel blending component; the aromatic hydrocarbon-rich extract oil is subjected to hydrocracking reaction to produce light aromatic hydrocarbons and clean gasoline blending components. The technology can produce clean gasoline and clean diesel oil at the same time, but the middle section is fed, so that the temperature of two beds is not matched easily, the filling amount of the refining agent is small, and the processing amount is not large. The extract oil rich in aromatic hydrocarbon is completely used as hydrocracking feed, so that the hydrocracking inactivation speed is increased, and the running period of the device is influenced.
CN 104611050A discloses a catalytic cracking diesel oil conversion method. The method adopts a single-stage series process, and the effluent of the hydrofining reaction directly enters a hydrocracking reactor and contacts and reacts with a graded catalyst bed layer in the hydrocracking reactor; the hydrogenation activity of the hydrocracking catalyst is in a decreasing trend according to the flow direction of the reaction materials. The method can ensure the hydrocracking effect of the diesel oil, reduce the excessive hydrogenation and secondary cracking of the cracked naphtha and reduce the chemical hydrogen consumption, thereby improving the octane number and the liquid yield of the naphtha. However, the problem of high catalyst activity at the initial stage of the operation of the apparatus is not considered, and the apparatus adjustment time cannot be shortened.
CN 106669861A discloses a hydrocracking catalyst grading method and a catalytic diesel oil hydroconversion process. The invention improves the hydrogenation selectivity of diesel oil/gasoline components in the conversion process, improves the yield of high-octane gasoline products, can reduce the amount of cold hydrogen and realize stable transition of temperature by grading and filling catalysts with different reaction performances in a cracking reactor, but can not solve the problem of unmatched temperature at the final stage of start-up.
CN 107304373A discloses a catalytic diesel hydroconversion process, in which a hydrocracking reactor is provided with an upper catalyst bed and a lower catalyst bed, the hydrocracking catalyst of the upper bed is loaded with Co and Mo active metals, and the hydrocracking catalyst of the lower bed is loaded with Ni and Mo metals. On the premise of better meeting the conversion rate of catalytic diesel, the process further improves the liquid yield of the device, reduces the hydrogenation saturation of the generated gasoline component, and improves the octane number of the gasoline component, but still can not solve the problem of the initial and final stages of the start-up of the device.
Therefore, in order to solve the above problems, it is necessary to change the conventional process flow and operation method to realize independent control of the hydrofining and cracking reactors, so as to achieve the purposes of reducing the initial adjustment time of the catalytic diesel conversion device and prolonging the operation period.
For the catalytic diesel hydrocracking technology, the traditional single-stage series process flow cannot solve the problem that the temperature of a refining reactor is not matched with that of a cracking reactor. The two-stage hydrocracking process is generally provided with two heating furnaces which can control the inlet temperatures of the two reactors respectively. The separator is arranged between the two reactors, and the outlet material of the refining reactor enters the cracking reactor after being saturated by the desulphurization and denitrification aromatic hydrocarbons, so that the performance of the cracking agent can be fully exerted. However, the conventional two-stage hydrocracking process is mainly designed to process high-sulfur, high-nitrogen and high-water-content raw materials to prevent H from being generated2S、NH3And water can reduce the cracking performance of the hydrocracking agent. The traditional process technology can not realize the targeted control of H of the refining reactor and the cracking reactor2S and NH3Concentration, thereby realizing the activity control of the hydrofining agent and the hydrocracking agent.
Disclosure of Invention
The invention aims to overcome the defects of the prior catalytic diesel hydrocracking process technology and provide a catalytic diesel hydrocracking method, which controls H of a hydrofining reactor and a hydrocracking reactor in a sectional manner2S and NH3Concentration, thereby achieving the purposes of shortening the stable time in the initial start-up period and prolonging the running period of the device.
The hydrocracking method of the catalytic diesel comprises the following steps:
(1) the catalytic diesel raw material enters a hydrofining reactor to contact with a hydrofining catalyst for reaction, and the reaction effluent enters a high-pressure separator;
(2) the high-pressure gas obtained from the upper part of the high-pressure separator is subjected to desulfurization treatment and then circulated back to the hydrofining reactor or directly enters the hydrocracking reactor without being subjected to desulfurization treatment, and the liquid phase obtained from the middle lower part of the high-pressure separator enters the low-pressure separator;
(3) the liquid phase obtained from the middle lower part of the low-pressure separator enters a fractionating tower and is fractionated to obtain dry gas, liquefied gas, light naphtha, heavy naphtha and tail oil;
(4) the tail oil enters a hydrocracking reactor to contact with a hydrocracking catalyst for hydrocracking reaction, and the reaction effluent enters a high-pressure separator.
In the hydrocracking method, the distillation range of the catalytic diesel raw material in the step (1) is generally 200-380 ℃, the sulfur content in the raw material oil is less than or equal to 3000 mu g/g, the nitrogen content is less than or equal to 1000 mu g/g, the density (20 ℃) is less than or equal to 0.95g/cm3, and the aromatic hydrocarbon content (mass fraction) is less than or equal to 85.0%.
According to the hydrocracking method, the hydrofining reactor in the step (1) is filled with a hydrofining catalyst which is conventional in the field, and the hydrofining catalyst comprises a carrier and hydrogenation active metal; wherein the carrier is inorganic refractory oxide, generally selected from one or more of alumina, amorphous silicon-aluminum, silicon dioxide or titanium oxide, etc.; the hydrogenation active metal comprises metal components of VIB and/or VIII groups, wherein the VIB group is selected from tungsten and/or molybdenum and calculated by oxide is 10-35%, preferably 15-30%, and the VIII group is selected from nickel and/or cobalt and calculated by oxide is 1-7%, preferably 1.5-6%. The carrier is inorganic refractory oxide, and is generally selected from alumina, amorphous silica-alumina, silica, titanium oxide and the like. The hydrofining catalyst can be selected from conventional hydrocracking pretreatment catalysts, wherein the conventional hydrocracking pretreatment catalysts can be selected from various existing commercial catalysts, such as hydrotreating catalysts developed and developed by the Fushu petrochemical industry research institute (FRIPP), such as 3936, 3996, FF-36, FF-46, FF-56 and FF-66; it can also be prepared according to the common knowledge in the field, if necessary.
In the hydrocracking method of the present invention, the reaction conditions in the hydrogenation refining reactor in step (1) are generally as follows: the reaction pressure is 5.0-35.0 MPa, preferably 6.0-19.0 MPa; the average reaction temperature is 200-480 ℃, and preferably 270-450 ℃; the volume space velocity is 0.1-15.0 h-1Preferably 0.2 to 3.0 hours-1(ii) a The volume ratio of hydrogen to oil is 100: 1-2500: 1, preferably 400: 1-2000: 1.
according to the hydrocracking method, in the step (1), before the octane number of the gasoline fraction (65-205 ℃) separated by the fractionating tower is not more than 90, nitrides are injected into the raw material, wherein the nitrides comprise one or more of n-butylamine, cyclohexylamine, pyridine and quinoline, and the adding amount enables the content of ammonium ions in mixed water separated by the high-pressure separator and the low-pressure separator to be 500-10000 ppm, preferably 1000-8000 ppm.
According to the hydrocracking method, before the octane number of the gasoline fraction (65-205 ℃) separated from the fractionating tower is not more than 90, the desulfurization treatment degree of the high-molecular gas is controlled to ensure that the concentration of hydrogen sulfide in recycle hydrogen of a hydrofining reactor is 10-200 ppm, preferably 20-150 ppm; when the octane number of the gasoline fraction (65-205 ℃) separated by the fractionating tower is more than 90, the high-gas-separation desulfurization treatment degree is controlled so that the concentration of hydrogen sulfide in recycle hydrogen of a hydrofining reactor is 200-3000 ppm, preferably 500-1000 ppm.
According to the hydrocracking method, when the average reaction temperature of the hydrofining reactor or the cracking reactor is higher than 405 ℃, the high-pressure gas obtained from the upper part of the high-pressure separator directly enters the hydrocracking reactor without being subjected to desulfurization treatment, sulfide can be injected into the high-pressure gas to enable the concentration of hydrogen sulfide to be 1000-6000 ppm, preferably 2000-5000 ppm, and CS is a commonly used vulcanizing agent2、C2H6S2(DMDS), SulfrZol 54, and the like.
In the process of the present invention, the hydrocracking catalyst generally comprises a cracking component, a hydrogenation component and a binder. Such as any suitable hydrocracking catalyst including those known in the art. The cracking component typically comprises amorphous silica-alumina and/or molecular sieves, typically molecular sieves such as Y-type or USY-type molecular sieves. The binder is typically alumina or silica. The hydrogenation component is a metal, a metal oxide or a metal sulfide of a metal in a VI group, a VII group or a VIII group, and more preferably one or more of iron, chromium, molybdenum, tungsten, cobalt, nickel or sulfides or oxides thereof. The hydrogenation component content is usually 5 to 40wt% based on the weight of the catalyst. Specifically, the existing hydrocracking catalyst may be selected, or a specific hydrocracking catalyst may be prepared as required. Commercial hydrocracking catalysts are mainly: HC-12, HC-14, HC-24, HC-39, etc. by UOP, 3905, 3955, FC-12, FC-16, FC-24, FC-32, 3971, 3976, FC-26, FC-28, etc. by FRIPP, and ICR126, ICR210, etc. by CHEVRON.
In the method of the invention, the hydrocracking operation conditions comprise: the reaction pressure is 5.0-35.0 MPa, preferably 6.0-19.0 MPa; the average reaction temperature is 200-480 ℃, preferably 270-450 ℃; the volume space velocity is 0.1-15.0 h-1Preferably 0.2 to 3.0 hours-1(ii) a The volume ratio of hydrogen to oil is 100: 1-2500: 1, preferably 400: 1-2000: 1.
the research result shows that NH in the reaction system3And H2The S concentration has a great influence on the activity of the hydrofining agent and the hydrocracking agent. When H is in the reaction system2When the concentration of S is too high, the hydrogen partial pressure in the reaction system can be reduced, the ultra-deep desulfurization of the hydrofining agent can be influenced, and the hydrofining reaction is not facilitated. But when H is in the reaction system2When the concentration of S is too low, the sulfuration state active metal on the surface of the catalyst can generate sulfur loss reduction reaction, and the loss of hydrogenation activity is large. When NH is in the reaction system3When the concentration is too high, for the hydrofining catalyst, ammonia molecules and raw oil sulfide and nitride generate competitive adsorption reaction, so that the hydrofining activity is reduced; in the case of hydrocracking catalysts, ammonia molecules are adsorbed on the acidic core, which is detrimental to the activity of the catalyst. According to the technical characteristics of catalytic diesel hydrocracking, NH in two-stage reactors is respectively regulated and controlled at the initial and final stages of the operation of the device3And H2And the concentration of S is used for realizing the control of the activity of the hydrofining agent and the cracking agent.
The method of the invention arranges a lateral line from the front of the recycle hydrogen desulfurization tower to the front of the hydrocracking reactor, and adds a nitrogen injection point at the inlet of the refining reactor. In the initial start-up period, nitride is injected into the inlet of the raw material tank, so that the nitride and aromatic hydrocarbon, sulfide, nitride and the like in the raw material are subjected to competitive adsorption reaction in the hydrogenation activity center of the hydrofining agent, the hydrogenation activity of the hydrofining agent is inhibited, and the aromatic hydrocarbon content in the refined oil is greatly reserved. And starting the recycle hydrogen desulfurization tower, and controlling the concentration of hydrogen sulfide at the outlet of the recycle hydrogen desulfurization tower, so that the concentration of hydrogen sulfide in the hydrocracking reactor is too low, the vulcanization degree of a hydrocracking agent is reduced, the hydrogenolysis reaction is increased, and the aromatic hydrocarbon content of the product is increased. And after the octane number of the gasoline product is qualified, stopping injecting nitrogen, and properly increasing the inlet concentration of the recycle hydrogen compressor. And at the end of the operation of the device, opening the recycle hydrogen desulfurization tower to the lateral line of the cracking reactor, increasing the concentration of hydrogen sulfide in the cracking reactor, improving the hydrogenation activity of the hydrocracking agent, reducing the hydrogenolysis reaction, slowing down the coking of the cracking agent and prolonging the service cycle of the device.
Compared with the prior art, the method has the advantages that:
(1) the two-stage hydrocracking method is adopted to process the catalytic diesel oil, so that the independent control of the temperatures of the hydrofining reactor and the hydrocracking reactor can be realized, and the problem of unmatched temperature of the two reactors in the initial and final stages of the operation of the device is effectively avoided.
(2) A nitrogen injection point is arranged at the outlet of the raw material tank, a sulfur injection point is arranged at the inlet of the cracking reactor, a lateral line is arranged between the front part of the recycle hydrogen desulfurization tower and the hydrocracking reactor, and the two reactors H are subjected to catalytic activity characteristics at the initial and final stages of the operation of the device2S and NH3The concentration is independently regulated and controlled to achieve the purposes of adjusting time in the initial stage of pressure reduction start-up work and prolonging the running period of the device.
(3) The hydrocracking method has strong raw material adaptability, and can be used for processing catalytic diesel oil with high nitrogen content, high sulfur content and high oxygen content. The heavy naphtha product has high octane number and low sulfur and nitrogen content, can be used as a high-quality reforming raw material, and is also a high-quality blending component of the national Wu gasoline.
Drawings
FIG. 1 is a flow diagram of a catalytic diesel hydrocracking process of the present invention. The method comprises the following steps of 1, 2, 3, 4, 5, 6, 7, 15, 16, 19, 20, 21, 22 and 24, wherein 1 is a nitrogen injection point, 2 is a raw material tank, 3 is a raw material pump, 4 is mixed hydrogen, 5 is a hydrofining reactor, 6 is hydrofining produced oil, 7 is a high-pressure separator, 8 is high-pressure gas, 9 is a recycle hydrogen desulfurization system, 10 is a side control valve, 11 is a low-pressure separator, 12 is low-pressure gas, 13 is low-pressure oil, 14 is a fractionating tower, 15 is fractionating tower top gas, 16 is light naphtha, 17 is heavy naphtha, 18 is tail oil, 19 is acid water, 20 is a hydrocracking reactor, 21 is hydrocracking produced oil, 22, 23 and 24 are recycle hydrogen sampling points, 25 is a recycle hydrogen compressor, 26 is a control valve, 27 is new hydrogen, 28 is a sulfur injection point and 29 is new hydrogen.
Detailed Description
The process of the present invention will be further illustrated with reference to the following examples, but the invention is not limited thereto.
Raw oil in a raw material tank 2 is mixed with mixed hydrogen 4 through a pump 3 and then enters a hydrofining reactor 5, sequentially passes through a hydrofining catalyst bed layer from top to bottom, is mixed with hydrofining produced oil 6 and hydrocracking produced oil 21 and then enters a high-pressure separator 7, and high-fraction gas 8 obtained at the upper part enters a recycle hydrogen desulfurization system 9 or directly enters a hydrocracking reactor 20 through a control valve 10; the liquid phase obtained from the middle lower part of the high-pressure separator 7 enters a low-pressure separator 11, the low-fraction gas 12 discharged from the upper part is subjected to subsequent treatment, the liquid phase 13 obtained from the middle lower part enters a subsequent fractionation system 14 to obtain a fractionation tower top gas 15, light naphtha 16 and heavy naphtha 17, and tail oil 18 enters a hydrocracking reactor 20; the mixed acid water 19 discharged from the bottom of the high-pressure separator and the mixed acid water 19 discharged from the bottom of the low-pressure separator 11 is subjected to subsequent processing. The gas phase passing through the recycle hydrogen desulfurization system passes through a recycle hydrogen compressor 25, is mixed with fresh hydrogen 29 and then returns to the hydrofining reactor 5, when a control valve 26 is opened, the pressurized recycle hydrogen is mixed with fresh hydrogen 27 and then returns to the hydrocracking reactor 20, when the concentrations of hydrogen sulfide and ammonia in the reaction system are adjusted, nitride is injected through a nitrogen injection point 1, and sulfide is injected through a sulfur injection point 28.
Example 1
The catalytic diesel oil is used as a raw material, an industrial hydrofining agent FF-66 and a hydrocracking agent FC-52 system are selected, the operation flow of FIG. 1 is selected, and the implementation process conditions are shown in Table 3. In the initial stage of the operation of the device, cyclohexylamine is injected into the raw material tank, the concentration of acidic water is controlled to be 1000-8000 ppm, and the concentration of hydrogen sulfide at the inlet of the recycle hydrogen compressor is controlled to be 20-150 ppm. And after the product is qualified, closing the side line control valve 10 of the recycle hydrogen desulfurization tower, opening the control valve 26, and controlling the concentration of recycle hydrogen at the outlet position of the recycle hydrogen desulfurization tower to be 500-1000 ppm. At the end of the operation of the device, the control valve 10 is opened, the control valve 26 is closed, the concentration of the hydrogen sulfide at the position point 23 is controlled to be between 2000 and 5000 ppm, and the concentration of the hydrogen sulfide at the position point 24 is controlled to be between 300 and 1000 ppm.
Example 2
The catalytic diesel oil is used as a raw material, an industrial hydrofining agent FF-66 and a hydrocracking agent FC-52 system are selected, the operation flow of FIG. 1 is selected, and the implementation process conditions are shown in Table 3. In the initial operation stage of the device, n-butylamine is injected into the raw material tank, the concentration of acidic water is controlled to be 1000-8000 ppm, and the concentration of hydrogen sulfide at the inlet of the recycle hydrogen compressor is controlled to be 20-150 ppm. And after the product is qualified, closing the side line control valve 10 of the recycle hydrogen desulfurization tower, opening the control valve 26, and controlling the concentration of recycle hydrogen at the outlet position of the recycle hydrogen desulfurization tower to be 500-1000 ppm. At the end of the plant run, control valve 10 is opened and control valve 26 is closed to control the hydrogen sulfide concentration at point 23 to be between 2000 and 5000 ppm, and if the hydrogen sulfide concentration is too low, sulfide can be injected at point 28. The hydrogen sulfide concentration at point 24 was controlled to be between 300 and 1000 ppm.
Comparative example 1
The catalytic diesel oil is used as a raw material, an industrial hydrofining agent FF-66 and a hydrocracking agent FC-52 system are selected, the operation flow of FIG. 1 is selected, and the implementation process conditions are shown in Table 3. And (3) at the initial stage of the operation of the device, the nitride is not injected into the raw material tank, the side line control valve 10 of the recycle hydrogen desulfurization tower is closed, the control valve 26 is opened, and the inlet concentration of the recycle hydrogen compressor is controlled to be 500-1000 ppm.
Comparative example 2
The catalytic diesel oil is used as a raw material, an industrial hydrofining agent FF-66 and a hydrocracking agent FC-52 system are selected, the operation flow of FIG. 1 is selected, and the implementation process conditions are shown in Table 3. In the initial stage of the operation of the apparatus, no nitride is injected into the raw material tank, the control valve 10 on the side line of the recycle hydrogen desulfurization tower is closed, the control valve 26 is opened, and the concentration of recycle hydrogen at the outlet of the recycle hydrogen desulfurization tower is controlled to be 500-1000 ppm. At the end of the operation of the device, the control valve 10 is opened to control the concentration of hydrogen sulfide at the position 23 to 2000 ppm, and if the concentration of hydrogen sulfide at the position is low, sulfide can be injected at the position 28.
Comparative example 3
The catalytic diesel oil is used as a raw material, an industrial hydrofining agent FF-66 and a hydrocracking agent FC-52 system are selected, the operation flow of FIG. 1 is selected, and the implementation process conditions are shown in Table 3. In the initial stage of the operation of the device, nitride is injected into the raw material tank, the concentration of the acidic water is controlled to be 1000-8000 ppm, after the product is qualified, the side line control valve 10 of the recycle hydrogen desulfurization tower is closed, the control valve 26 is opened, and the concentration of the recycle hydrogen at the outlet position of the recycle hydrogen desulfurization tower is controlled to be 500-1000 ppm until the final stage of the operation of the device.
The properties of the catalysts used in the examples are listed in table 1. The properties of the raw oils used are shown in Table 2.
TABLE 1 physicochemical Properties of the catalyst
TABLE 2 raw oil Properties Table
TABLE 3 Process operating conditions
TABLE 4 comparison of the operating results of the comparative examples and examples
Processing the raw oil from full load to gasoline fraction octane number of more than 90 at 65-205 ℃;
time from full load processing of the feedstock to an average reaction temperature in the hydrofinishing or cracking reactor of more than 405 ℃.
From the above examples, the method of the present invention is characterized by long adjustment time in the initial startup period of the catalytic diesel hydrocracking unit and short operation period of the unit. Comparing the comparative examples with the examples, it can be seen that the initial adjustment time can be effectively reduced by using the method of implanting nitride and reducing the hydrogen sulfide concentration in the system. The operation method of opening a lateral line in the recycle hydrogen desulfurization tower and increasing the concentration of hydrogen sulfide in the hydrocracking reactor can effectively increase the running period of the device. It can be seen from comparison between example 1 and example 2 that the apparatus operation cycle is longer in the case of injecting n-butylamine than in the case of injecting cyclohexylamine, although the initial adjustment time at the start of the apparatus is longer.
Claims (10)
1. A hydrocracking method of catalytic diesel oil is characterized in that: the method comprises the following steps:
(1) the catalytic diesel raw material enters a hydrofining reactor to contact with a hydrofining catalyst for reaction, and the reaction effluent enters a high-pressure separator;
(2) the high-pressure gas obtained from the upper part of the high-pressure separator is subjected to desulfurization treatment and then circulated back to the hydrofining reactor or directly enters the hydrocracking reactor without being subjected to desulfurization treatment, and the liquid phase obtained from the middle lower part of the high-pressure separator enters the low-pressure separator;
(3) the liquid phase obtained from the middle lower part of the low-pressure separator enters a fractionating tower and is fractionated to obtain dry gas, liquefied gas, light naphtha, heavy naphtha and tail oil;
(4) the tail oil enters a hydrocracking reactor to contact with a hydrocracking catalyst for hydrocracking reaction, and the reaction effluent enters a high-pressure separator.
2. The method of claim 1, wherein: in the step (1), the distillation range of the catalytic diesel raw material is 200-380 ℃, the sulfur content in the raw material oil is less than or equal to 3000 mu g/g, and the nitrogen content is less than or equal to 1000 mu g/g.
3. The method of claim 1, wherein: the hydrorefining catalyst in the step (1) comprises a carrier and hydrogenation active metal; the carrier is one or more of alumina, amorphous silicon-aluminum, silicon dioxide or titanium oxide; the hydrogenation active metal comprises VIB and/or VIII group metal components, wherein the VIB group is selected from tungsten and/or molybdenum and accounts for 10-35% of the oxide, and the VIII group is selected from nickel and/or cobalt and accounts for 1-7% of the oxide.
4. The method of claim 1, wherein: the reaction conditions in the hydrogenation refining reactor in the step (1) are as follows: the reaction pressure is 5.0-35.0 MPa; the average reaction temperature is 200-480 ℃; the volume space velocity is 0.1-15.0 h-1(ii) a The volume ratio of hydrogen to oil is 100: 1-2500: 1.
5. the method of claim 1, wherein: and (2) before the octane number of the gasoline fraction separated by the fractionating tower in the step (1) is not more than 90, injecting nitride into the raw material, wherein the nitride comprises one or more of n-butylamine, cyclohexylamine, pyridine and quinoline, and the adding amount enables the content of ammonium ions in the mixed water separated by the high-pressure separator and the low-pressure separator to be 500-10000 ppm.
6. The method of claim 1, wherein: and before the octane number of the gasoline fraction separated by the fractionating tower is not more than 90, controlling the desulfurization treatment degree of the high-molecular gas to ensure that the concentration of hydrogen sulfide in the recycle hydrogen of the hydrofining reactor is 10-200 ppm.
7. The method of claim 1, wherein: when the octane number of the gasoline fraction separated by the fractionating tower is more than 90, the desulfurization treatment degree of the high-molecular gas is controlled, so that the concentration of hydrogen sulfide in the recycle hydrogen of the hydrofining reactor is 200-3000 ppm.
8. The method of claim 1, wherein: when the average reaction temperature of the hydrofining reactor or the cracking reactor is higher than 405 ℃, the high-pressure gas obtained from the upper part of the high-pressure separator directly enters the hydrocracking reactor without desulfurization treatment.
9. The method of claim 8, wherein: injecting sulfide into the high-molecular gas to ensure that the concentration of hydrogen sulfide is 1000-6000 ppm, wherein the sulfide is CS2、C2H6S2(DMDS), SulfrZol 54.
10. The method of claim 1, wherein: the hydrocracking operating conditions include: the reaction pressure is 5.0-35.0 MPa; the average reaction temperature is 200-480 ℃; the volume space velocity is 0.1-15.0 h-1(ii) a The volume ratio of hydrogen to oil is 100: 1-2500: 1.
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| GB1315559A (en) * | 1970-08-10 | 1973-05-02 | Exxon Research Engineering Co | Hydrocracking process for high end point feeds |
| CN101294107A (en) * | 2007-04-24 | 2008-10-29 | 中国石油化工股份有限公司 | Method for preparing fuel oil with coal oil hydrogenation |
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