RU2012148118A - METHOD FOR HYDROCONVERSION OF OIL FRACTIONS BY SLURRY-TECHNOLOGY, PROVIDING THE REMOVAL OF METALS OF THE CATALYST AND RAW MATERIALS, INCLUDING A WASHING STAGE - Google Patents

METHOD FOR HYDROCONVERSION OF OIL FRACTIONS BY SLURRY-TECHNOLOGY, PROVIDING THE REMOVAL OF METALS OF THE CATALYST AND RAW MATERIALS, INCLUDING A WASHING STAGE Download PDF

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RU2012148118A
RU2012148118A RU2012148118/04A RU2012148118A RU2012148118A RU 2012148118 A RU2012148118 A RU 2012148118A RU 2012148118/04 A RU2012148118/04 A RU 2012148118/04A RU 2012148118 A RU2012148118 A RU 2012148118A RU 2012148118 A RU2012148118 A RU 2012148118A
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stage
liquid
metals
fraction
hydroconversion
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RU2567232C2 (en
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Жан-Филипп ЭРО
Фредерик МОРЕЛЬ
Ален КИНЬЯР
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Ифп Энержи Нувелль
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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
    • C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
    • C10G49/10—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 with moving solid particles
    • C10G49/12—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 with moving solid particles suspended in the oil, e.g. slurries
    • 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
    • C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
    • C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
    • C10G65/12—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including cracking steps and other hydrotreatment steps
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/32—Selective hydrogenation of the diolefin or acetylene compounds
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    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/44—Hydrogenation of the aromatic hydrocarbons
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
    • 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
    • C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
    • C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
    • C10G65/04—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only refining steps
    • 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
    • C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
    • C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
    • C10G65/10—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only cracking steps
    • 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
    • C10G67/04—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 including solvent extraction as the refining step in the absence of hydrogen
    • C10G67/0454—Solvent desasphalting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/88—Molybdenum
    • B01J23/883—Molybdenum and nickel
    • 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
    • C10G2300/1077—Vacuum residues
    • 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
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/202—Heteroatoms content, i.e. S, N, O, P
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
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    • C10G2300/201—Impurities
    • C10G2300/205—Metal content
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    • 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
    • C10G2300/20—Characteristics of the feedstock or the products
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/30—Physical properties of feedstocks or products
    • C10G2300/301—Boiling range
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    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/40—Characteristics of the process deviating from typical ways of processing
    • C10G2300/44—Solvents
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    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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Abstract

1. Способ гидроконверсии тяжелых нефтяных фракций, содержащих металлы, включающий:a. стадию гидроконверсии сырья по меньшей мере в одном реакторе, содержащем суспендированный катализатор, содержащий по меньшей мере один металл и необязательно твердую добавку,b. стадию разделения потоков, выходящих из гидроконверсии без уменьшения давления, с получением фракции, называемой легкой, содержащей соединения, кипящие при температуре не более 500°C, и остаточной фракции,b'. необязательно стадию фракционирования, включающую отделение в вакууме указанной остаточной фракции, полученной на стадии b), с получением остатка вакуумной перегонки с высоким содержанием металлов,c. стадию экстракции жидкость/жидкость растворителем насыщенной природы указанной остаточной фракции, полученной на стадии b), и/или указанного остатка вакуумной перегонки, полученного на стадии b'), с получением твердого экстракта с высоким содержанием металлов и рафината,d. стадию дробления твердого экстракта с высоким содержанием металлов, полученного на стадии экстракции жидкость/жидкость,e. стадию промывки измельченного экстракта в присутствии воды, растворителя насыщенной природы и ПАВ, с получением твердого экстракта и промывочного раствора,f. стадию сжигания в присутствии кислорода указанного твердого экстракта, полученного на стадии промывки, с получением шлаков с высоким содержанием металлов,g. стадию экстракции металлов из шлаков, полученных на стадии сжигания,h. стадию приготовления раствора или растворов металла или металлов, содержащих по меньшей мере металл катализатора, которые рециркулируют в качестве катализатора на стадию гидроко�1. A method for the hydroconversion of heavy petroleum fractions containing metals, including: a. a step of hydroconverting the feed in at least one reactor containing a slurry catalyst containing at least one metal and optionally a solid additive, b. a stage of separating the streams leaving the hydroconversion without reducing the pressure, with obtaining a fraction called light, containing compounds boiling at a temperature of not more than 500 ° C, and a residual fraction, b '. optionally a fractionation step comprising vacuum separation of said residual fraction obtained in step b) to obtain a vacuum residue with a high metal content, c. a step of liquid / liquid extraction with a solvent of the saturated nature of said residual fraction obtained in step b) and / or said vacuum distillation residue obtained in step b ') to obtain a solid extract with a high content of metals and raffinate, d. a stage of crushing the solid extract with a high metal content obtained from the liquid / liquid extraction stage, e. the stage of washing the crushed extract in the presence of water, a solvent of a saturated nature and a surfactant, to obtain a solid extract and a washing solution, f. a stage of combustion in the presence of oxygen of said solid extract obtained in the washing stage to obtain slags with a high metal content, g. a stage for extracting metals from slags obtained in the combustion stage, h. a step of preparing a solution or solutions of a metal or metals containing at least a catalyst metal, which are recycled as a catalyst to the hydroco

Claims (15)

1. Способ гидроконверсии тяжелых нефтяных фракций, содержащих металлы, включающий:1. The method of hydroconversion of heavy oil fractions containing metals, including: a. стадию гидроконверсии сырья по меньшей мере в одном реакторе, содержащем суспендированный катализатор, содержащий по меньшей мере один металл и необязательно твердую добавку,a. a step for hydroconversion of the feed in at least one reactor containing a suspended catalyst containing at least one metal and optionally a solid additive, b. стадию разделения потоков, выходящих из гидроконверсии без уменьшения давления, с получением фракции, называемой легкой, содержащей соединения, кипящие при температуре не более 500°C, и остаточной фракции,b. the step of separating the streams leaving the hydroconversion without reducing the pressure to obtain a fraction called light, containing compounds boiling at a temperature of not more than 500 ° C, and a residual fraction, b'. необязательно стадию фракционирования, включающую отделение в вакууме указанной остаточной фракции, полученной на стадии b), с получением остатка вакуумной перегонки с высоким содержанием металлов,b '. optionally a fractionation step comprising vacuum separating said residual fraction obtained in step b) to obtain a high metal content vacuum distillation residue, c. стадию экстракции жидкость/жидкость растворителем насыщенной природы указанной остаточной фракции, полученной на стадии b), и/или указанного остатка вакуумной перегонки, полученного на стадии b'), с получением твердого экстракта с высоким содержанием металлов и рафината,c. a liquid / liquid extraction step with a saturated solvent of the indicated residual fraction obtained in step b) and / or the indicated vacuum distillation residue obtained in step b ') to obtain a solid extract with a high content of metals and raffinate, d. стадию дробления твердого экстракта с высоким содержанием металлов, полученного на стадии экстракции жидкость/жидкость,d. a stage for crushing a solid extract with a high metal content obtained in the liquid / liquid extraction stage, e. стадию промывки измельченного экстракта в присутствии воды, растворителя насыщенной природы и ПАВ, с получением твердого экстракта и промывочного раствора,e. the stage of washing the crushed extract in the presence of water, a solvent of a saturated nature and a surfactant, to obtain a solid extract and a washing solution, f. стадию сжигания в присутствии кислорода указанного твердого экстракта, полученного на стадии промывки, с получением шлаков с высоким содержанием металлов,f. a burning step in the presence of oxygen of said solid extract obtained in the washing step to obtain high metal slag, g. стадию экстракции металлов из шлаков, полученных на стадии сжигания,g. a step for extracting metals from slag obtained in the burning step, h. стадию приготовления раствора или растворов металла или металлов, содержащих по меньшей мере металл катализатора, которые рециркулируют в качестве катализатора на стадию гидроконверсии.h. the stage of preparation of the solution or solutions of the metal or metals containing at least a catalyst metal, which are recycled as a catalyst to the hydroconversion stage. 2. Способ по п.1, в котором указанную фракцию, называемую легкой, полученную на стадии b) разделения без уменьшения давления, подвергают по меньшей мере одной стадии гидроочистки и/или гидрокрекинга.2. The method according to claim 1, in which the specified fraction, called light, obtained in stage b) separation without reducing pressure, is subjected to at least one stage of hydrotreating and / or hydrocracking. 3. Способ по любому из предшествующих пунктов, в котором указанную остаточную фракцию, полученную на стадии разделения без уменьшения давления, подвергают вакуумной перегонке, с получением по меньшей мере одной фракции вакуумного дистиллята и одной фракции остатка вакуумной перегонки, причем по меньшей мере часть, предпочтительно, вся указанная фракция остатка вакуумной перегонки поступает на стадию экстракции жидкость/жидкость, и по меньшей мере часть, предпочтительно, вся указанная фракция вакуумного дистиллята поступает по меньшей мере на одну стадию гидроочистки и/или гидрокрекинга.3. The method according to any one of the preceding claims, wherein said residual fraction obtained in the separation step without pressure reduction is subjected to vacuum distillation to obtain at least one fraction of a vacuum distillate and one fraction of a vacuum distillation residue, at least a portion, preferably , all of the specified fraction of the remainder of the vacuum distillation enters the stage of extraction of the liquid / liquid, and at least part, preferably at least part of the specified fraction of the vacuum distillate enters at least Leray one stage hydrotreating and / or hydrocracking. 4. Способ по п.1, в котором стадию экстракции жидкость/жидкость осуществляют при температуре, составляющей от 50° до 300°C, предпочтительно от 120° до 250°C.4. The method according to claim 1, wherein the liquid / liquid extraction step is carried out at a temperature of from 50 ° to 300 ° C, preferably from 120 ° to 250 ° C. 5. Способ по п.1, в котором стадию экстракции жидкость/жидкость осуществляют при отношении растворитель/сырье от 1/1 до 10/1, предпочтительно от 2/1 до 7/1.5. The method according to claim 1, wherein the liquid / liquid extraction step is carried out at a solvent / feed ratio of from 1/1 to 10/1, preferably from 2/1 to 7/1. 6. Способ по п.1, в котором размер частиц указанного твердого экстракта с высоким содержанием металлов, выходящего со стадии экстракции жидкость/жидкость, полученного дроблением, составляет менее 6 мм, предпочтительно, менее 4 мм.6. The method according to claim 1, in which the particle size of the specified solid extract with a high content of metals leaving the stage of extraction of the liquid / liquid obtained by crushing is less than 6 mm, preferably less than 4 mm 7. Способ по п.1, в котором стадия промывки включает7. The method according to claim 1, wherein the washing step comprises a. стадию приготовления эмульсии, содержащей измельченный экстракт, полученный на стадии дробления, указанную воду, указанный ПАВ и указанный растворитель насыщенной природы, причем отношение вода/сырье составляет от 0,5/1 до 5/1, предпочтительно, от 1/1 до 2/1, отношение растворитель/сырье составляет от 2/1 до 6/1, предпочтительно, от 3/1 до 4/1, и концентрация ПАВ составляет от 0,05% масс. до 2% масс., предпочтительно, от 0,1% масс. до 1% масс., в расчете на воду,a. the stage of preparation of the emulsion containing the crushed extract obtained at the stage of crushing, the specified water, the specified surfactant and the specified solvent is saturated in nature, and the ratio of water / raw materials is from 0.5 / 1 to 5/1, preferably from 1/1 to 2 / 1, the ratio of solvent / raw material is from 2/1 to 6/1, preferably from 3/1 to 4/1, and the concentration of surfactant is from 0.05% of the mass. up to 2% of the mass., preferably from 0.1% of the mass. up to 1% of the mass., calculated on water, b. стадию созревания указанной эмульсии при температуре от 20° до 120°C, предпочтительно, от 60° до 70°C, необязательно в течение периода времени, составляющего от 5 мин до 3 ч,b. the stage of maturation of the specified emulsion at a temperature of from 20 ° to 120 ° C, preferably from 60 ° to 70 ° C, optionally for a period of time of 5 minutes to 3 hours, c. стадию декантации при сохранении температуры, необязательно в течение периода от 15 мин до 30 ч, с получением твердого экстракта и промывочного раствора.c. the stage of decantation while maintaining the temperature, optionally for a period of from 15 minutes to 30 hours, to obtain a solid extract and a washing solution. 8. Способ по п.1, в котором растворитель насыщенной природы, использованный на стадии экстракции жидкость/жидкость и на стадии промывки, является идентичным и предпочтительно выбран из группы, состоящей из гексана, гептана, легкой нафты насыщенной природы, по отдельности или в смеси в равных или разных пропорциях.8. The method according to claim 1, wherein the saturated solvent used in the liquid / liquid extraction step and the washing step is identical and is preferably selected from the group consisting of hexane, heptane, saturated light naphtha, individually or in a mixture in equal or different proportions. 9. Способ по п.1, в котором стадию сжигания осуществляют при давлении от -0,1 до 1 МПа, предпочтительно, от -0,1 до 0,5 МПа, и при температуре от 200 до 700°C, предпочтительно, от 400 до 550°C в присутствии воздуха.9. The method according to claim 1, in which the stage of combustion is carried out at a pressure of from -0.1 to 1 MPa, preferably from -0.1 to 0.5 MPa, and at a temperature of from 200 to 700 ° C, preferably from 400 to 550 ° C in the presence of air. 10. Способ по п.1, в котором стадия экстракции металлов g) включает промывку по меньшей мере одним кислым и/или основным раствором.10. The method according to claim 1, wherein the step of extracting the metals g) comprises washing with at least one acidic and / or basic solution. 11. Способ по п.1, в котором тяжелая нефтяная фракция представляет собой углеводородную фракцию, содержащую по меньшей мере 50% масс. продукта, кипящего при температуре более 250°C, и по меньшей мере 25% масс., кипящего при температуре более 350°C, и содержит по меньшей мере 50 млн-1 металлов, по меньшей мере 0,5% масс. серы и по меньшей мере 1% масс. асфальтенов (гептановых асфальтенов).11. The method according to claim 1, in which the heavy oil fraction is a hydrocarbon fraction containing at least 50% of the mass. Product boiling at a temperature greater than 250 ° C, and at least 25 wt.%, boiling at a temperature greater than 350 ° C, and contains at least 50 million -1 metals, at least 0.5% by weight. sulfur and at least 1% of the mass. asphaltenes (heptane asphaltenes). 12. Способ по п.1, в котором тяжелая нефтяная фракция выбрана из нефтяных остатков, сырой нефти, нефти с отобранными наиболее легкими фракциями, деасфальтированных масел, асфальтов после деасфальтизации, производных процессов конверсии нефти, битуминозных песков или их производных, битуминозных хвостов или их производных, или из смесей таких видов сырья.12. The method according to claim 1, in which the heavy oil fraction is selected from oil residues, crude oil, oil with the selected lightest fractions, deasphalted oils, asphalts after deasphalting, derivatives of oil conversion processes, tar sands or their derivatives, tar sands or their derivatives, or from mixtures of these types of raw materials. 13. Способ по п.1, в котором стадию гидроконверсии осуществляют при давлении от 2 до 35 МПа, предпочтительно, от 10 до 25 МПа, парциальном давлении водорода от 2 до 35 МПа, предпочтительно, от 10 до 25 МПа, температуре в интервале от 300°C до 500°C, предпочтительно, от 420°C до 480°C, и времени контакта от 0,1 ч до 10 ч, предпочтительно, от 0,5 ч до 5 ч.13. The method according to claim 1, in which the hydroconversion stage is carried out at a pressure of from 2 to 35 MPa, preferably from 10 to 25 MPa, a partial pressure of hydrogen from 2 to 35 MPa, preferably from 10 to 25 MPa, a temperature in the range from 300 ° C to 500 ° C, preferably 420 ° C to 480 ° C, and a contact time of 0.1 hours to 10 hours, preferably 0.5 hours to 5 hours 14. Способ по п.1, в котором суспендированный катализатор представляет собой сульфированный катализатор, содержащий по меньшей мере один элемент, выбранный из группы, состоящей из Mo, Fe, Ni, W, Co, V, Ru.14. The method according to claim 1, in which the suspended catalyst is a sulfonated catalyst containing at least one element selected from the group consisting of Mo, Fe, Ni, W, Co, V, Ru. 15. Способ по п.1, в котором добавку выбирают из группы, состоящей из минеральных оксидов, отработанных нанесенных катализаторов, содержащих по меньшей мере один элемент группы VIII и/или по меньшей мере один элемент группы VIB, твердых карбоидов с низким содержанием водорода или из смесей таких добавок, причем указанная добавка имеет размер частиц менее 1 мм. 15. The method according to claim 1, in which the additive is selected from the group consisting of mineral oxides, spent supported catalysts containing at least one element of group VIII and / or at least one element of group VIB, solid carbides with a low hydrogen content or from mixtures of such additives, said additive having a particle size of less than 1 mm.
RU2012148118/04A 2010-04-13 2011-03-22 METHOD OF HYDROCONVERSION OF OIL FRACTIONS USING Slurry TECHNOLOGY ENSURING EXTRACTION OF METALS OF CATALYST AND RAW MATERIALS, INCLUDING WASHING STAGE RU2567232C2 (en)

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