MXPA97007522A - Process in several stages of conversion of a residue of petro - Google Patents

Abstract

A process of converting a heavy fraction of the hydrocarbons in which the hydrocarbon filler is treated in a hydrodemetalation section containing at least one hydrodemetalation catalyst in fixed bed is described, at least a part of the hydrotreated liquid effluent is sent out from step a) to an atmospheric distillation zone from which a distillate and an atmospheric residue are recovered, at least a part of the atmospheric waste is sent to a vacuum distillation zone, from which a distilled and a residue under vacuum, at least a part of the residue under vacuum is sent to a deasphalting section from which a cut of deasphalted hydrocarbon and residual asphalt is obtained, at least a part of the deasphalted hydrocarbon cut is sent to a hydrotreating section, from which a gas fraction, a fuel fraction is obtained after separation and a heavier liquid fraction of hydrotreated charge, said section comprising at least one three-phase reactor, containing at least one boiling bed hydrotreating catalyst, operating in updraft of liquid and gas, said reactor including at least one medium. transfer of the catalyst out of the reactor, and at least one medium of fresh catalyst supplementation in the reaction

Description

PROCESS IN SEVERAL STAGES OF CONVERSION OE A RESIDUE OF PETROLEUM DESCRIPTION OF THE INVENTION The present invention relates to the refining and conversion of heavy fractions of hydrocarbons containing, among others, asphaltenes and sulfur and metal impurities. This relates more particularly to a process that makes it possible to convert at least part of a load where the Conradson carbon ratio is greater than 10, and more frequently more than 15, and even higher than 20, for example, a vacuum residue of an oil. crude in a product that has a Conradson carbon sufficiently small and a proportion of metals and in sulfur sufficiently low that it can be used as a charge to manufacture gas oil and gasoline by catalytic disintegration in a conventional fluid bed catalytic disintegration unit and / or in a catalytic fluid bed disintegration unit that includes a double regeneration system, and eventually a catalyst cooling system at the regeneration level. The present invention also relates to a process for the manufacture of gasoline and / or gas oil that includes at least one step of catalytic disintegration in a fluidized bed. REP: 25727 As refiners increase the proportion of heavier and lower quality crude oil in the cargo to be treated, it becomes increasingly necessary to have particular processes, specially adapted to the treatment of these residual heavy petroleum fractions. , of shale oil, or similar materials containing asphaltenes and containing a large proportion of Conradson carbon. It is in this way that the European patent EP-B-435242 describes a charge treatment process of this type, comprising a hydrotreatment with the help of a single catalyst under conditions that allow to reduce the proportion of sulfur and metal impurities, the contact of the total effluent with a reduced proportion of sulfur from the hydrotreatment, with a solvent under extraction conditions of asphaltenes that allow recovering a relatively poor extract in asphaltene and metallic impurities and sending this extract to a catalytic disintegration unit with a view to producing low molecular weight hydrocarbon products. In a preferred form according to the text of this patent, a reduction in viscosity will be effected (visbrereduction) of the product from the first stage and it is the product left from the visbreaking that is sent to the solvent extraction of the asphaltenes. 'According to example 1 of this patent, the treated charge is an atmospheric waste. It seems difficult to produce according to the teaching of this patent a load that has the necessary characteristics to be treated in a reactor of classic catalytic disintegration, in order to produce a fuel from waste under vacuum to a very large proportion of metals (greater than 50 ppm, frequently higher than 100 ppm, and more frequently higher than 200 ppm), and a large proportion of Conradson carbon. In effect, the limit of the current proportion of metals in the usable industrial loads is approximately 20 to 25 ppm of metals, and the limit with respect to the Conradson carbon ratio is approximately 3% for a classical disintegration unit. catalytic, and »of about 8% in the case of a unit specially designed for the disintegration of heavy loads. The use of fillers where the proportions of metal impurities are in the upper limits or above these upper limits mentioned hereinafter, involve a very important deactivation of the catalyst, which needs a considerable complement of fresh catalyst which is very penalizing for the process and even prohibitive. In addition this process involves the use "of very important quantities of solvent for the desalination, since it is the entire hydrotreated product and preferably viscoreduced which is deasphalted. The use of a single hydrotreating catalyst limits the yields in the elimination of the metallic impurities to values lower than 75% (table I, example II) and / or in desulphurisation to values lower than or equal to 85% (table I, example II) . This technique will not allow to obtain. a treatable load in a classic FCC in which if the hydrotreated oil, optionally viscoreduced, is deasphalted with a solvent of the type of 3 carbon atoms, which limits the yield very strongly. The object of the present invention is to reduce the disadvantages described above and to obtain from a very strongly charged filler of metals and a large portion of Conradson carbon and sulfur, a demetalated product at more than 80% and more frequently at least 90% , desulfurized at the most 80% and more frequently at least 85% and where the Conradson carbon will be less than or equal to 8, which allows this product to be sent to a catalytic residue disintegration reactor such as a reactor with double regeneration and preferably a carbon Conradson less than or equal to about 3, which allows this product to be sent to a classic catalytic disintegration reactor. The fillers that can be treated according to the present invention usually include amounts of metals (essentially vanadium and / or nickel) different from those mentioned above, at least 0.5% by weight of sulfur, frequently more than 1% by weight of sulfur, very frequently more than 2% by weight of sulfur and most frequently up to 4%, even up to -10% by weight of sulfur, and at least 1% by weight of asphaltenes of 7 carbon atoms. The proportion of asphaltene of 7 carbon atoms of the fillers treated in the framework of the present invention is frequently greater than 2% and very frequently greater than 5% by weight, and can equal or even exceed 24% by weight. These charges are for example those where the characteristics are given in the BILLÓN article and others published in 1994 in volume 49, number 5 of the INSTITUT FRANÇAIS DU PETROLE magazine, pages 495 to 507. In its most extensive form, the present invention is defined as a conversion process of a heavy fraction of hydrocarbons having a Conradson carbon ratio of at least 10, a proportion of metals of at least 50 ppm, and frequently of at least 100 ppm, and very often of at least 200 ppm by weight, a proportion of asphaltene of 7 carbon atoms of at least 1%, frequently of at least 2%, and very frequently of at least 5% by weight, and a sulfur content of at least 0.5% , often of at least 1%, and very often of at least 2% by weight, characterized in that it comprises the following steps: a) the hydrocarbon charge is treated in a treatment section in the presence of hydrogen which * comprises at least one which comprises at least one fixed bed hydrodemetalation catalyst, and preferably at least one hydrodemetalation catalyst and at least one hydrodesulphurisation catalyst in fixed beds, under conditions that allow obtaining a liquid effluent with reduced proportion of metals and carbon Conradson and preferably also of sulfur, b) at least a part, and often all, of the hydroconverted liquid effluent from stage a) is sent to an atmospheric distillation zone from which a distillate and an atmospheric residue are recovered. , c) at least part, and often all, of the atmospheric waste obtained in step b) is sent to a vacuum distillation zone from which a distillate and a vacuum residue were recovered, d) at least a part, and preferably all of the vacuum residue obtained in step c), is sent to an asphalt removal section in which This is treated in an extraction section with the help of a solvent under the conditions that allow obtaining a deasphalted hydrocarbon cut, and residual asphalt, e) at least a part, and preferably the entire hydrocarbon cut desasfaltads obtained in step d) is sent to a hydrotreating section, preferably in mixture with at least a part of the vacuum distillate obtained in step c), even with all of this vacuum distillation, in which it is hydrotreated in the presence of hydrogen, under conditions that allow to obtain an effluent with reduced Conradson carbon ratio of metals and sulfur, and after separation of a gaseous fraction, an atmospheric distillate that can be cleaved into a gasoline fraction and into a gas oil fraction that are more often sent at least in part to the corresponding fuel combinations and a heavier liquid fraction of hydrotreated filler, said section at least one three-phase reactor, which contains at least one hydrotreating catalyst in a boiling bed, operating at upstream of liquid and gas, said reactor including at least one means for transferring the catalyst out of the reactor, and at least one medium for fresh catalyst supplementation in the reactor. According to a variant, the heavier liquid fraction of hydrotreated charge exiting from step e) is sent to a catalytic disintegration section (step f) optionally in mixture with at least a part of the vacuum distillate obtained in step c) ), in which it is treated under conditions that allow the production of a gaseous fraction, a gasoline fraction, a diesel fraction and a suspension fraction. The gas fraction contains mainly saturated and unsaturated hydrocarbons having from 1 to 4 carbon atoms in their molecules (methane, ethane, propane, butanes, ethylene, propylene, butylenes). The gasoline fraction is, for example, at least in part and preferably in its entirety sent to the fuel mixture. The diesel fraction is, for example, sent at least in part to stage a). The suspension fraction is more frequently at least in part, if not entirely, sent to the refinery's heavy fuel mixture, in general after the separation of the fine particles contained therein in suspension. the invention, this suspension fraction is at least in part, if not entirely, sent back to the input of the catalytic decay of step f) The conditions of stage a) of charge treatment in the presence The following are usually used in the dismetallation zone: at least one fixed bed of conventional hydrodemetalation catalyst, and preferably at least one of the catalysts described by the applicant, in particular at least one of those described in US Pat. European patents EP-B-113297 and EP-B-113284. It is usually operated under an absolute pressure of 5 to 35 mPa, and more frequently of 10 to 20 mPa at a temperature from about 300 to about 500 ° C, and frequently from about 350 to about 450 ° C. The WH and hydrogen partial pressure are important factors that are chosen according to the characteristics of the load to be treated and the desired conversion. Most often the WH is in a range from about 0.1 to about 5, and preferably from about 0.15 to about 2. The amount of hydrogen blended with the filler is usually from about 100 to about 5000 normal cubic meters (Nm3) per cubic meter (3) of liquid charge, and more frequently from approximately 500 to approximately 3000 Nm3 / m3. It is usefully operated in the presence of sulfurized hydrogen, and the partial pressure of hydrogen sulfide is usually about 0.002 times a. about 0.1 times, and preferably about 0.0005 times to about 0.05 times the total pressure. In the hydrodesulfurization zone, the ideal catalyst must have a strong hydrogenating power, in order to carry out a deep refining of the products coming from the dismetalation, and obtain an important reduction of the sulfur, carbon Conradson and the proportion of asphaltenes. It will be possible, for example, to use one of the catalysts described by the applicant in the European patents EP-B-113297 and EP-B-113284. In the case where the hydrodesulfurization zone is different from the hydrodemetalation zone, it will be possible to operate at a relatively low temperature, that is to say substantially lower than the temperature at the hydrodemetalation zone which goes in the direction of a deep hydrogenation and a limitation of coking. It will not be outside the scope of the present invention to use the same catalyst in the two zones, nor to regroup these two zones so that only one area in which hydrodesmetalation and hydrodesulphurization will be formed, simultaneously or in a manner successive with a single catalyst or with several different catalysts. In this step a) at least one catalyst can be used, while ensuring both demetalation and desulphurisation, under conditions which make it possible to obtain a liquid charge with a reduced content of metals, Conradson carbon and sulfur. at least two catalysts, one of them that ensures mainly the demetalation., and the other mainly the desulphurization under conditions that allow to obtain a liquid charge with a reduced content of metals, Conradson carbon and sulfur In the area of atmospheric distillation of step b), the conditions are generally chosen so that the cut-off point is from about 300 to about 400 ° C, and preferably from 340 to about 380 ° C. The distillate obtained in this way is usually sent more after the separation into a fraction of gasoline and a fraction of gas oil, to the corresponding combined fuels. A particular embodiment, at least a part, is that the whole of the gas oil fraction of the atmospheric distillate can be sent to step e) of hydrotreating. Atmospheric waste can be sent at least in part to the refinery's fuel mix. In the vacuum distillation zone in the stage. c), where the atmospheric waste obtained in step b) is treated, the conditions are generally chosen so that the cut-off point is about 450 to 600 ° C, and more frequently about 500 to 550 ° C. The distillate obtained in this way is usually sent at least in part to step e) of hydrotreating, and the residue under vacuum is at least in part sent to step d) of removing asphalts. In a particular embodiment of the invention, at least part of the vacuum residue is sent to the refinery's heavy fuel combination. It is also possible to recycle at least a part of the residue under vacuum in step a). The vacuum distillate can also, more frequently after separation in a gasoline fraction and a gas oil fraction, be at least in part sent to the corresponding fuels. This distillate or one of these fractions can also be at least partly sent to stage f) of catalytic disintegration. Step d) of removing asphalt, with the aid of a solvent, is carried out under the conventional conditions well known to the person skilled in the art. Reference can also be made to the article by BILLÓN and others published in 1994 in volume 49, number 5 of the journal INSTITUT FRAN? AIS DU PETROLE, pages 495 a., 507, or even the description given in the French patent description FR-B-2480773 or in the French patent description FR-B-2681871 in the name of the applicant, or even in the description of US patent US-A-4715946 in the name of the applicant, whose descriptions are considered as incorporated in the present by the mere fact of this mention. The removal of asphalt or deasphalting is usually carried out at a temperature of 60 to 250 ° C with at least one hydrocarbon solvent having from 3 to 7 carbon atoms, optionally added with at least one additive. Usable solvents and additives are mainly described in the documents cited above and in U.S. Pat. US-A-1948296, US-A-2081473, US-A-2587643, US-A-2882219, US-A-3278415 and US-A-3331394 for example. It is also possible to effect the recovery of the solvent according to the opticritic process, that is, using a solvent under supercritical conditions. This process allows in particular to improve mainly the overall economy of the process. This removal of asphalt can be done in a mixer-decanter or in an extraction column. Within the framework of the present invention, the technique using at least one extraction column is preferred. Step e) of hydrotreating the deasphalted hydrocarbon cutting is carried out. in the conventional boiling-bed hydrotreating conditions, of a liquid hydrocarbon fraction. It is usually operated under an absolute pressure of 2 to 25 MPa, and more frequently of 5 to 15 MPa at a temperature of about 300 to about 550 ° C, and frequently of about 350 to about 500 ° C. The space velocity per hour (WH) and the partial pressure of hydrogen are important factors that are chosen according to the characteristics of the load to be treated and the desired conversion. More often the WH is located with a range from about 0.1 h "1 to about 10 h" 1, and preferably from about 0.2 h to about 5 h "1. The amount of hydrogen mixed with the filler is usually from about 50 to about 5000 normal cubic meters (Nm3) per cubic meter (m3) of liquid filler, and more often from about 100 to about 3000 Nm3 / m3 A classic granular hydrotreating catalyst can be used. a catalyst comprising group VIII metals, for example nickel and / or cobalt, more frequently in association with at least one metal of group VIB, for example molybdenum, For example, a catalyst comprising from 0.5 to 10% by weight can be used. of nickel and preferably from 1 to 5% by weight of nickel (expressed in NiO nickel oxide) and from 1 to 30% by weight of molybdenum, preferably from 5 to 20% by weight of molybdenum no (expressed in molybdenum oxide Mo03) on a support, for example an alumina support. This catalyst is most frequently in the form of extrudate or spheres. The catalyst used is partly replaced with a fresh catalyst by means of racking in the lower part of the reactor and introduction of fresh or new catalyst in the upper part of the reactor, at regular intervals of time, ie for example by pumping almost continuously. It is possible, for example, to introduce a fresh catalyst every day. The rate of replacement of the catalyst used by the fresh catalyst can be, for example, from about 0.05 kilogram to about 10 kilograms per cubic meter of charge. This transfer and this replacement are carried out with the help of devices that allow the continuous operation of this hydrotreating stage. The unit usually includes a recirculation pump which allows the maintenance of the boiling bed catalyst by continuous recycling of at least a part of the liquid taken up in the upper part of the reactor, and reinjected into the bottom of the reactor. More frequently this step e) of hydrotreating is put into operation under the conditions of the T-STAR process as described for example in the article Heavy Oil Hydroprocessing, published by Aiche, March 19-23, HOUSTON, Texas, document number 42d . The products obtained in the course of this step e) are usually sent to a separation zone from which a gaseous fraction and a liquid fraction that can be even sent to a second separation zone in which it can be recovered are recovered. split in light fractions, for example gasoline and diesel fuel that can be sent at least in part to the combined fuels, and in a heavier fraction. Usually this heavier fraction has an initial boiling point of at least 340 ° C and more frequently of at least 370 ° C. This heavier fraction can, at least in part, be sent to the refinery's combination of heavy fuel and very low sulfur content (usually less than 0.5% by weight). In a particular embodiment of the. invention, it is advantageous to provide at least one means for improving the viscosity of the overall filler which is treated in step a) of treatment in the presence of hydrogen. In effect, a low viscosity makes it possible to reduce the load losses in the reactor (s) of this treatment section. This is particularly important when the section contains several reactors, since in this case the global load losses at the level of the whole section become important and are penalizing for the start-up of the process. There is a drop in the partial pressure of hydrogen in the reactors, which is very unfavorable for the operation of this treatment stage in the presence of hydrogen, and on the other hand it involves a malfunction of the compressors of hydrogen recycling in the reactors. The improvement of the fluidity of the load also makes it possible to lower the temperature of the furnace or furnaces and thus obtain smaller surface temperatures, which either allows the use of less expensive steels or obtain longer life times for the most important furnaces. for a furnace constructed of a given alloy According to this particular embodiment, at least a part of the distillate obtained by atmospheric distillation in step b), and / or at least one part of the distillate obtained by vacuum distillation in step c), and / or at least part of the fuel fraction (atmospheric distillate) obtained in step e) Finally, according to the variant mentioned above in a disintegration stage f) catalytic, at least a part of the heaviest fraction of the hydrotreated charge obtained in step e) can be sent to a classical catalytic disintegration section, in which this is des catalytically integrated in a conventional manner under conditions well known to those skilled in the art, to produce a fuel fraction (comprising a gasoline fraction and a gas oil fraction) which is usually sent at least in part to the combined fuels, and a fraction in suspension that will be for example at least in part, if not in its entirety, sent to the combined heavy fuel, or recycled at least in part, if not entirely, to stage f) of catalytic disintegration. In a particular embodiment of the invention, a part of the gasoline fraction, obtained in the course of this step f), is recycled to either stage a), or to stage e), or to step f) in mixture with the charge introduced in this stage f) of disintegration.-catalytic. In the present description, the term a part of the gas oil fraction must be understood as a fraction less than 100%. It will not be outside the scope of the present invention to recycle a part of the gas oil fraction in stage a), another part in stage f) and a third part in stage e), not necessarily representing all three parts together the entire diesel fraction. It is also possible within the framework of the present invention to recycle all the gas oil obtained by catalytic disintegration or cleavage either in stage a), or in step f) or in step e), or a fraction in each of these steps, representing the sum of these fractions 100% of the gas oil fraction obtained in step f). It is also possible to recycle at least part of the fraction of "gasoline obtained in this step f) of catalytic disintegration in step f), for example, a summary description of catalytic disintegration (where the first industrial start-up dates back to 1936 (HOUDRY process) or to 1942 for the use of the fluidized bed catalyst) in ULLMANS ENCYCLOPEDIA OF INDUSTRIAL CHEMISTRY VOLUME A 18, 1991 pages 61 to 64. A classical catalyst is usually used. comprising a matrix, optionally an additive and at least one zeolite. The amount of zeolite is variable, but usually from about 3 to 60% by weight, frequently from about 6 to 50% by weight, and more often from about 10 to 45% by weight. The zeolite is usually dispersed in the matrix. The amount of additive is usually from about 0 to 30% by weight, and frequently from about 0 to 20% by weight. The amount of matrix represents the complement at 100% by weight. The additive is generally chosen from the group consisting of the oxides of the group IIA metals of the periodic classification of the elements, such as, for example, magnesium oxide or calcium oxide, the rare earth oxides and the titanates of the metals of group IIA. The matrix is most often a silica, an alumina, a silica-alumina, a silica-magnesium, a clay, or a mixture of two or more of these products. The most commonly used zeolite is zeolite Y. Disintegration is carried out in a substantially vertical reactor, either in ascending mode (riser) or in descending mode (dropper). The choice of the catalyst and the operating conditions are functions of the products sought, depending on the load treated as that described, for example, in the article by MARCILLY pages 990-991 published in the journal of the French Institute of Oil November-December 1975, pages 969-1006. It is usually operated at a temperature of about 450 ° C to about 600 ° C and residence times in the lower reactor of 1 minute, frequently from * about 0.1 to about 50 seconds. Stage f) of catalytic disintegration can * • also be a stage of catalytic disintegration in fluidized bed, for example according to the process set up by the applicant, called R2R. This step can be executed in a conventional manner known to the person skilled in the art, under the appropriate conditions of disintegration of the waste in order to produce hydrocarbon products of lower molecular weight. The descriptions of the operation and of the catalysts which can be used in the context of the fluidized-bed disintegration in this step f) are described, for example, in patent documents US-A-4695370, EP-B-184517, US-A -4959334, EP-B-323297, US-A-4965232, US-A-5120691, US-A-5344554, US-A-5449496, EP-A-485259, US-A-5286690, US-A-5324696 and EP-A-699224 where the descriptions are considered as incorporated herein by reference only. In this particular embodiment, it is possible to introduce in this stage f) catalytic disintegration at least a part of the atmospheric residue obtained in step b). The fluidized bed catalytic disintegration reactor can operate in updraft or downflow. Although this is not a preferred embodiment of the present invention, it is equally advisable to carry out the catalytic disintegration in a mobile bed reactor. Particularly preferred catalytic disintegration catalysts are those which contain at least one zeolite, usually in admixture with an appropriate matrix such as for example alumina, silica, or silica-alumina. According to a particular embodiment, when the treated load is a vacuum residue left from the vacuum distillation of an atmospheric distillation residue of a crude oil, it is advantageous to recover the vacuum distillate to send it at least in part , if not in its entirety, to stage e) in which it is hydrotreated in mixture with the deasphalted hydrocarbon cut obtained in step d). When the vacuum distillate is sent only partly in step e), the other part is preferably sent to stage a) of treatment in the presence of hydrogen. According to another variant, a part of the deasphalted hydrocarbon cut obtained in step d) can be recycled to step a) of hydrotreating. In a preferred form of the invention, the residual asphalt obtained in step d) is sent to an oxivapogasification section in which it is transformed into a gas containing hydrogen and carbon monoxide. This gaseous mixture can be used for the synthesis of methanol or for the synthesis of hydrocarbons by the Fischer-Tropsh reaction. This mixture within the framework of the present invention is preferably sent to a section of conversion with steam (shit conversion in English) in which in the presence of water vapor is converted into hydrogen and carbon dioxide. The hydrogen obtained can be used in steps a) and e) of the process according to the invention. The residual asphalt can also be used as a solid fuel or after the flow as a liquid fuel.

Example A heavy vacuum residue (RSV) of Safaniya origin is treated. Its characteristics are presented in table 1 column 1. All performances are-calculated from a base 100 (in mass) of RSV. This Safaniya vacuum residue is treated in a catalytic hydrotreating reaction. The unit put into operation is a pilot that simulates the operation of a HYVAHL® industrial unit. The pilot unit includes two reactors in series that operate in a downward flow. The reactors are each charged with 7 1. HMC841 hydrodemetalation catalyst, manufactured by the company Procatalyse and loaded in fixed beds. The operating conditions carried out are as follows: WH - 0.5 H "1 P = 150 barias Hydrogen recycling = 1000 1H2 / 1 load Temperature = 380 ° C The characteristics of the total liquid effluent of more than 5 carbon atoms, of the reactor, are presented in table 1, in column 2. The product is then fractionated successively in an atmospheric distillation column at the bottom of which an atmospheric residue (RA) is recovered after this RA is in turn fractionated in a vacuum distillation column leading to a vacuum distillation fraction (DSV) and a vacuum residue (RSV). The yields and characteristics of these products are presented in Table 1, respectively in columns 3, 5 and 4. In the atmospheric distillation, the distillate that is sent to the combined fuels after the separation in a gasoline fraction is recovered. and a fraction of diesel. The vacuum residue is then deasphalted in a pilot unit that simulates the SOLVAHL® process of deasphalting or asphalt removal. The pilot unit works with a vacuum waste of 5 1 / h, the solvent used is a cut of pentane put into operation with. a proportion of 5/1 in volume in relation to the load. A deasphalted oil cut (DAO) is thus obtained where the performance and characteristics are presented in table 1 column 6, and a residual asphalt. This DAO cut is immediately mixed again with the DSV cut from the previous stage. The DSV + DAO mixture is then hydrotreated catalytically in a pilot unit operating in a boiling bed. The reactor is tubular in shape and has a volume of 3 liters. The catalyst put into operation is that described in Example 2 of the. US-A-4652545 under the reference HDS-1443 B. The operating conditions are as follows: WH = 2 in relation to the catalyst P = 80 bars T = 420 ° C. * Recycling of hydrogen - 400 1H2 / 1 load Catalyst replacement ratio: 0.3 Kg / m3 Table 1 gives the characteristics of the DSV + DAO mixture (column 7) used and the characteristics of the product obtained at the hydrotreatment outlet (column 8). This preheated load at 149 ° C is placed in contact at the bottom of a vertical pilot reactor, with a hot regenerated catalyst from a pilot regenerator. The inlet temperature in the reactor of the "catalyst is 740 ° C. The ratio of the cost of the catalyst to the charge is 6.64. The caloric input of the catalyst at 740 ° C allows the vaporization of the load and the Disintegration or cleavage reaction, which is endothermic The average residence time of the catalyst in the reaction zone is about 3 seconds The operating pressure is 1.8 bar absolute The catalyst temperature, measured at the outlet of the. The fluidized bed reactor, riser, is 520 ° C. The disintegrated hydrocarbons and the catalyst are separated by cyclones located in a stripper zone where the catalyst is purified, the catalyst that has been coked during The reaction and purification in the purification zone is then sent to the regenerator.The proportion of the coke of the solid (delta coke) at the regenerator inlet is approx. This coke is burned by the air injected into the regenerator. Very exothermic combustion raises the temperature of the solid from 520 ° C to 740 ° C. The regenerated and hot catalyst leaves the regenerator and is sent back to the lower part of the reactor.

The hydrocarbons separated from the catalyst leave the "purification zone, they are cooled by the exchangers and sent to a stabilization column that separates the gas and liquids, the liquid (+ 5 carbon atoms) is also taken and then is fractionated in another column in order to recover a fraction of gasoline, a fraction of diesel and a fraction of heavy fuel or suspension (a + of 360 ° C.) Tables 2 and 3 give the yields in gasoline and diesel and The main characteristics of these products obtained in the whole process.

Table No. 1 Performance and qualities of the cargo and the products Table No. 2 Balance and characteristics of the gasoline produced Table No. 3 Balance and characteristics of the gas oil produced It is noted that in relation to this date, the best method known to the applicant to carry out the aforementioned invention, is that which is clear from the present description of the invention.

Having described the invention as above, property is claimed as contained in the following

Claims (20)

1. A conversion process of a heavy fraction of hydrocarbons having a Conradson carbon ratio of at least 10, a proportion of metals of at least 50 ppm by weight, a ratio of asphaltene of 7 carbon atoms of at least 1%, and a sulfur content of at least 0.5%, characterized in that it comprises the following steps: a) the hydrocarbon filler is treated in a treatment section in the presence of hydrogen, comprising at least one reactor containing at least one hydrodemetallation catalyst in a fixed bed, under the conditions that allow to obtain a liquid effluent with a reduced proportion of metals and carbon Conradson, b) at least part of the effluent * liquid hydroconverted from stage a) is sent to an atmospheric distillation zone from which a distillate and an atmospheric residue is recovered, c) at least a part of the atmospheric waste obtained in stage b) is sent to a waste area. vacuum tillage, from which a distillate and a vacuum residue are recovered, d) at least a part of the vacuum residue obtained in step c) is sent to a section of deasphalting or removal of asphalt, in which This is treated in an extraction section with the help of a solvent, under conditions that allow obtaining a cut of deasphalted hydrocarbon and residual asphalt, e) at least a part of the deasphalted hydrocarbon cut obtained in step d) is sent towards a section of hydrotreatment, in the presence of hydrogen, in which it is hydrotreated under conditions that allow obtaining products with a reduced proportion of Conradson carbon, of metals and sulfur, and then the separation of a gas fraction, a fuel fraction and a heavier liquid fraction of hydrotreated filler, said section comprising at least one three-phase reactor, containing at least one hydrotreating catalyst in the ebull bed The reactor, which operates in updraft of liquid and gas, the reactor comprises at least one means for transferring the catalyst out of said reactor, and at least one means for complementing fresh catalyst in the reactor.

2. The process according to claim 1, characterized in that at least a part of the heavy liquid fraction obtained in step e) is sent to a section of catalytic disintegration (step f) in which it is treated under conditions "that allow to produce a gas fraction, a gasoline fraction, a gas oil fraction and a suspension fraction.

3. The process according to any of claims 1 or 2, characterized in that in the course of step a), the treatment in the presence of hydrogen is carried out under an absolute pressure of 5 to 35 MPa, at a temperature of about 300 to 500 ° C with a space velocity per hour of approximately 0.1 to 5 '1.

4. The process according to claim 2 to 3, characterized in that at least a part of the gas oil fraction recovered in step f) of catalytic disintegration is sent back to stage a).

5. The process according to any of claims 1 to 4, characterized in that the removal of asphalt or deasphalting is carried out at a temperature of 60 to 250 ° C, with at least one hydrocarbon solvent having 3 to 7 atoms of carbon.

6. The process according to any of claims 1 to 5, characterized in that the distillate obtained by vacuum distillation in stage c) is at least in part sent to stage e) of hydrotreatment.

7. The process according to any of claims 1 to 6, characterized in that the step e) of hydrotreating is carried out under an absolute pressure of about 2 to 25 MPa, at a temperature of about 300 to 550 ° C with a speed per hour from approximately 0.1 to 10 h "1, and the amount of hydrogen mixed with the charge is approximately 50 to 5000 NmVpi3.

8. The process according to any of claims 2 to 7, characterized in that the step f) of catalytic disintegration is carried out under conditions that allow producing a fraction of gasoline which is at least partly sent to the fuel mixture, a gas oil fraction which is sent at least in part to the diesel fuel in a fraction of the suspension which is at least in part sent to the heavy fuel combi.

9. The process according to any of claims 1 to 8, characterized in that at least a part of the vacuum residue obtained in step c) is recycled in step a).

10. The process according to any of claims 1 to 9, characterized in that at least part of the heavier liquid fraction of hydrotreated charge obtained in step e), is sent to the combined heavy fuel with very low * proportion of sulfur .

11. The process according to any of claims 2 to 10, characterized in that at least a portion of the gas oil fraction and / or fraction of gasoline obtained in step f) of catalytic disintegration, is recycled at the entrance of this stage f).

12. The process according to any of claims 2 to 11, characterized in that at least a part of the suspension fraction obtained in step f) of catalytic disintegration is recycled at the entrance to this stage f).

13. The process according to any of claims 1 to 12, characterized in that a portion of the deasphalted hydrocarbon cutting obtained in step d) is recycled to stage a) of hydroconversion.

14. The process according to any of claims 1 to 13, characterized in that the treated charge is a vacuum residue left from the vacuum distillation of an atmospheric distillation residue * - ... of a crude oil, and the distillate The vacuum is at least in part sent to step e) of hydrotreating.

15. The process according to any of claims 1 to 14, characterized in that »the distillates obtained in step b) and / or in step e) are split into a gasoline fraction and a gas oil fraction, which are at least partly sent to their respective fuel mixes.

16. The process according to any of claims 2 to 15, characterized in that the distillate obtained in stage c) or one of the fractions of that distillate is at least in part sent to the stage f ") of catalytic disintegration.

17. The process according to any of claims 1 to 16, characterized in that the atmospheric distillate obtained in step b) is split into a gasoline fraction and a gas oil fraction where at least a part is sent to stage e) of hydrotreating.

18. The process according to any of claims 1 to 17, characterized in that the distillate obtained by atmospheric distillation in stage b) is at least in part sent to stage a) hydroconversion.

19. The process according to any of claims 1 to 18, characterized in that the distillate obtained by vacuum distillation in stage c) is at least in part sent to stage a) hydroconversion.

20. The process according to any of claims 1 to 19, characterized in that the fuel fraction obtained in step e) is at least partly sent to stage a) hydroconversion. SUMMARY OF THE INVENTION A process of converting a heavy fraction of the hydrocarbons in which the hydrocarbon charge is treated in a hydrodesmetallation section containing at least one hydrodemetalation catalyst in fixed bed is described, at least a part of the hydrotreated liquid effluent is sent out from stage a) to an atmospheric distillation zone from which a distillate and a residue are recovered, atmospheric, at least a part of the atmospheric waste is sent to a vacuum distillation zone, from which a distillate and a vacuum residue are recovered, at least a part of the residue under vacuum is sent to a section of deasphalting from which a cut of deasphalted hydrocarbon and residual asphalt is obtained, at least a portion of the deasphalted hydrocarbon cut is sent to a hydrotreating section, from which a gaseous fraction is obtained after separation , a fuel fraction and a heavier liquid fraction of hydrotreated filler, said section comprising at least one three-phase reactor, containing at least one boiling bed hydrotreating catalyst, operating in updraft of liquid- and gas, including said At least one catalyst decanting medium is removed from the reactor, and at least one medium of fresh catalyst supplementation in the reactor ctor