Asphalt containing unconventional bituminous materials

Abstract

The present invention discloses an asphalt comprising an unconventional asphalt base material. The present invention relates to an asphalt which comprises: - from 40% to 75% by weight of a first asphalt base material B1, said first asphalt base material B1 consisting of pitch obtained by solvent deasphalting of a first vacuum residue R1, said first vacuum residue R1 being produced by distillation of the effluent from the ebullated bed hydroconversion process of a heavy hydrocarbon feedstock, B1 having a softening point of from 50°C to 110°C, and - from 25% to 60% by weight of a second asphalt base material B2 and / or a flux F, F consisting of at least one heavy aromatic fraction having an initial point greater than 350°C, a 90% distillation point less than 650°C and a hydrogen content greater than 8.5% by weight according to standard ASTM D2887, B2 consisting of the second vacuum residue R2 produced by R1 or crude oil distillation, or consisting of a mixture of R1 and R2.

Description

Technical Field

[0001] The present invention relates to the field of asphalt, and in particular to asphalt compositions for road construction and public works (e.g., waterproofing asphalt). More specifically, the present invention relates to asphalt formulated from an unconventional asphalt base, particularly comprising an asphalt base composed of the final residue from an ebullated-bed hydroconversion process of a heavy liquid hydrocarbon feedstock, i.e., asphalt obtained by solvent deasphalting of the vacuum residue from the hydroconversion effluent. Background Art

[0002] Bitumen (also called asphalt binder) is a hydrocarbon mixture widely used as paving in road construction or civil engineering. Bitumen is usually formed from a mixture of "bituminous bases" which are conventionally obtained from the processing of crude oil.

[0003] Bitumen is usually produced from the residue resulting from units for the vacuum distillation (without any post-treatment) of asphaltenic crude oils, known as "bituminous crudes". However, these bituminous crudes represent about 10% of all crude oils, which constitutes a limiting factor in the production of bitumen.

[0004] There are other methods for producing bitumen, such as those based on the partial oxidation of the residue from direct distillation of crude oil (when the properties of the residue deviate too far from the specific properties of bitumen) – an operation known as "bitumenblowing" that changes the properties of the residue; or those based on the deasphalting of the residue obtained from direct distillation of crude oil, using paraffinic solvents such as propane, butane, or a mixture of the two; or those based on the use of visbroken residues, although the latter have properties that are mediocre for producing bitumen, in particular with regard to the thermooxidative stability of the bitumen. However, these production methods are either expensive (in the case of bitumen oxidation), or again depend on the bituminous crude oil (as in the case of bitumen base obtained by deasphalting bituminous crude oil), or result in bitumen of mediocre quality (as in the case of bitumen base obtained from visbroken residues).

[0005] Furthermore, the supply of the above-mentioned conventional bituminous bases (obtained from direct distillation of bituminous crude oil) depends on the number of refineries, which in certain parts of the world (such as Europe) is sometimes caused to decrease, which can therefore constitute an additional constraint on bitumen production.

[0006] There is therefore a need to produce bitumen of good quality while moving away as much as possible from the use of crude bitumen or expensive technologies aimed at modifying the properties of the bitumen base.

[0007] In addition, in refineries, there is a residue oil produced by the hydroconversion process of heavy hydrocarbon feedstocks that is difficult to increase in value for the preparation of fuel base oils. This residue oil contains high levels of impurities such as metals, sulfur, nitrogen, Conradson carbon, and heptane insolubles (also known as C7 asphaltenes). Typically, such residue oils (which are usually vacuum residue oils obtained by distilling hydroconversion effluents) are used as marine fuels with a high sulfur content. However, the commercial demand for these fuels is decreasing, especially due to the introduction of more stringent sulfur emission standards for flue gases from ships (which are the main consumers of such fuels). This is the case, for example, of the vacuum residue oil produced by atmospheric distillation followed by vacuum distillation of the hydroconversion effluent in a boiling bed hydroconversion process of the H-Oil TM type, or of the vacuum residue oil in the form of a suspension (referred to as slurry vacuum residue oil) produced by atmospheric distillation followed by vacuum distillation of the hydroconversion effluent in a transport bed (also known as slurry) hydroconversion process. The transport bed hydroconversion process is based on the use of a catalyst dispersed in the feedstock in the form of very small particles, with a size less than 500 μm, typically from 1 nm to 200 nm, and in fact even from 1 nm to 20 nm, and which leaves the hydroconversion reactor together with the hydroconversion effluent. The mixture of the hydroconversion effluent and the catalyst leaving the transport bed reactor is then referred to as the slurry hydroconversion effluent, which is itself in the form of a suspension.

[0008] Such residue oils can be used to formulate bitumen. Such residue oils are not considered conventional bitumen bases, such as those described above.

[0009] As a mixture with conventional bitumen bases, road bitumen compositions containing hydroconversion residue oil produced by a boiling bed hydroconversion process of the H-Oil TM type are thus known, as described in patent US 4 904 305. However, the residue oil content in such bitumens is low, typically from 2% to 10%, and it is not optimal in terms of increasing the value of the hydroconversion residue oil.

[0010] The use of slurry hydroconversion residue oil as a bitumen base for forming road bitumen is also known, as described in patent application US20170137718. Here again, the hydroconversion residue oil content in the bitumen composition is limited, typically from 1 wt% to 30 wt%. In addition, the presence of the catalyst dispersed in the hydroconversion residue oil limits the maximum possible content of the slurry residue oil in the bitumen and requires a filtration stage for the slurry residue oil to bring it to around 30 wt%. This is because the presence of the catalyst affects the physico-chemical properties of the bitumen and can, for example, reduce its solubility and alter its rheological properties.

[0011] Higher contents of residues from hydroconversion of heavy feedstocks in bituminous compositions are disclosed, for example, in US 4 683 005. However, in the bitumens disclosed in that patent, the hydroconverted residues must be produced by a hydroconversion process showing a conversion degree of greater than 80%, which entails non-negligible operating constraints.

[0012] The inventors have surprisingly demonstrated that relatively large amounts of heavy products resulting from the ebullated bed hydroconversion process of liquid heavy hydrocarbon feedstocks can be used to form bitumens having unexpectedly advantageous properties, in particular good thermo-oxidative stability.

[0013] In particular, the inventors have demonstrated that it is possible to start from crude oils (different from said "bitumen crudes") that are unconventional for bitumen production and form bitumens having advantageous properties, and in particular according to the criteria for construction and road paving, in particular according to European standards, and in fact even for waterproof paving, while maximizing the value of the final residues from the hydroconversion process of liquid heavy feedstocks (i.e., the pitch resulting from the deasphalting of the heavy fraction of the ebullated bed hydroconversion effluent).

[0014] Surprisingly, it has been demonstrated that the pitch (and in relatively large amounts) obtained by solvent deasphalting of the vacuum residue resulting from the ebullated bed hydroconversion process of liquid heavy feedstocks, used in the form of a mixture with another bituminous binder and / or flux, can form bitumens meeting these criteria without having to resort to techniques for modifying the bitumen properties, such as, for example, the operation of partial oxidation of the residue called bitumen oxidation, and without the need to use bitumen crudes.

[0015] The inventors have thus confirmed that it is possible, in particular, to formulate bitumens meeting these criteria starting from the ebullated bed hydroconversion residues that are usually used as fuel (high sulfur heavy fuel oil), said ebullated bed hydroconversion residues including final residues that are difficult to increase in value and whose production is usually desired to be minimized in these hydroconversion processes.

[0016] Formulating such bitumens thus constitutes another way to increase the value of these ebullated bed hydroconversion residues, since the market for high sulfur heavy fuel oil is well known to be declining due to the introduction of a 0.5% sulfur specification (effective as of January 1, 2020) for the fuel used by ships not equipped with devices (scrubbers) for removing sulfur from combustion flue gases.

[0017] The inventors have also confirmed the useful application of aromatic extracts from lubricant manufacture in the form of a mixture with such pitch obtained by deasphalting the vacuum residue resulting from the ebullated bed hydroconversion process to form bitumens meeting current standards. Summary of the Invention

[0018] The object of the present invention is to provide bitumen that complies with current standards, in particular those of European origin such as NF EN 12591 for road bitumen, while maximizing the value of the final residue of the hydroconversion process of liquid heavy feedstocks in a ebullated bed (i.e., the pitch resulting from the deasphalting of the heavy fraction of the ebullated bed hydroconversion effluent).

[0019] Another object of the present invention is to provide bitumen that complies with such standards starting from oils different from "bitumen crudes".

[0020] Yet another object of the present invention is to provide bitumen that complies with such standards and that contains a maximum of ebullated bed hydroconversion residue, including a large part of the final residue of the hydroconversion process of liquid heavy feedstocks in a ebullated bed (i.e., the pitch resulting from the deasphalting of the heavy fraction of the ebullated bed hydroconversion effluent).

[0021] Thus, in order to achieve at least one of the above - oriented objects, according to a first aspect, the present invention provides bitumen that comprises:

[0022] - 40% to 75% by weight of a first bitumen base B1, said first bitumen base B1 consisting of pitch obtained by solvent deasphalting of a first vacuum residue R1, said first vacuum residue R1 being produced by distillation of the effluent resulting from the hydroconversion of a heavy hydrocarbon feedstock in an ebullated bed, B1 having a softening point of 50°C to 110°C, and

[0023] - 25% to 60% by weight of a second bitumen base B2 and / or a flux F, F consisting of at least one heavy aromatic fraction having an initial point greater than 350°C, a 90% distillation point less than 650°C and a hydrogen content greater than 8.5% by weight according to standard ASTM D2887, B2 consisting of a second vacuum residue R2 produced by R1 or by crude oil distillation, or consisting of a mixture of R1 and R2,

[0024] It is understood that the bitumen comprises at most:

[0025] 75% by weight of B1 when the bitumen consists of B1 and F,

[0026] 50% by weight of B1 when the bitumen consists of B1 and B2, and

[0027] 70% by weight of B1 when the bitumen consists of a mixture of F and B2 and B1, and

[0028] The sum of the weight percentages of B1, B2 and F is equal to 100%.

[0029] According to one or more embodiments of the present invention, the heavy aromatic fraction is an aromatic fraction extracted from the vacuum distillate obtained in a lubricating oil manufacturing process.

[0030] According to one or more embodiments of the present invention, the heavy hydrocarbon feedstock fed to the hydroconversion process contains a hydrocarbon fraction at least 80 wt% of which has an initial boiling point of at least 300 °C and is preferably crude oil or consists of atmospheric residue and / or vacuum residue produced by atmospheric and / or vacuum distillation of crude oil, and preferably consists of vacuum residue produced by vacuum distillation of crude oil.

[0031] According to one or more embodiments of the present invention, R2 is produced by atmospheric and vacuum distillation of crude oil that has already been used as a feedstock in a ebullated bed hydroconversion process.

[0032] According to one or more embodiments of the present invention, R1 comprises a residual fraction boiling at a temperature of greater than or equal to 540 °C and is obtained by atmospheric and vacuum distillation of the effluent hydroconverted by an ebullated bed hydroconversion process of a heavy hydrocarbon feedstock, the process comprising at least one hydroconversion stage and preferably two hydroconversion stages, the hydroconversion stages being carried out at an absolute pressure of 2 MPa to 38 MPa at a temperature of 300 °C to 550 °C at a space velocity HSV of 0.05 h -1 to 10 h -1 per cubic meter (m 3 of heavy hydrocarbon feedstock and at a hydrogen quantity mixed with the heavy hydrocarbon feedstock of 50 to 5000 standard cubic meters (Sm 3 ).

[0033] According to one or more embodiments of the present invention, B1 is pitch obtained by deasphalting of R1, wherein the hydrocarbon solvent mainly comprises compounds having 3 to 4 carbon atoms, preferably butane or propane or a mixture thereof, wherein the solvent / feedstock ratio (volume / volume) is 4 / 1 to 10 / 1, the temperature is 40 °C to 150 °C, and the pressure is from 2 MPa to 6 MPa.

[0034] According to one or more embodiments of the present invention, the asphalt consists of B1 and R1.

[0035] According to one or more embodiments of the present invention, the asphalt consists of B1 and F.

[0036] According to one or more embodiments of the present invention, the asphalt consists of a mixture of R1 and / or R2 and F and B1.

[0037] According to one or more embodiments of the present invention, B1 accounts for 40 wt% to 60 wt% of the asphalt, R1 and / or R2 account for 25 wt% to 45 wt% of the asphalt, and F accounts for 5 wt% to 15 wt% of the asphalt.

[0038] According to one or more embodiments of the present invention, B1 accounts for 40% to 55% by weight of the bitumen, R1 and / or R2 account for 30% to 45% by weight of the bitumen, and F accounts for 5% to 15% by weight of the bitumen.

[0039] According to one or more embodiments of the present invention, the bitumen consists of a mixture of R1 and F and B1, wherein B1 and R1 account for 85% to 95% by weight of the bitumen, and F accounts for 5% to 15% by weight of the bitumen.

[0040] The bitumen according to the present invention is preferably a road bitumen having a ring and ball softening point greater than or equal to 43 °C and less than 58 °C, and a penetration at 25 °C greater than or equal to 35 °C and less than 100 °C.

[0041] According to a second aspect, the present invention relates to a road pavement consisting of a mixture of the bitumen according to the present invention and suitable mineral aggregates.

[0042] According to a third aspect, the present invention relates to the use of pitch obtained by solvent deasphalting of a first vacuum residue R1 produced by distillation of an effluent hydrocracked by a ebullated bed hydrocracking process of a heavy hydrocarbon feedstock as a first bitumen base B1 for preparing a bitumen according to the present invention in the form of a mixture with a second bitumen base B2 and / or a flux F, B1 having a softening point of 50 °C to 110 °C and constituting 40% to 75% by weight of the bitumen, B2 and / or F constituting 25% to 60% by weight of the bitumen, B2 consisting of R1, or consisting of a second vacuum residue R2 produced by crude oil distillation, or consisting of a mixture of R1 and R2, and F consisting of at least one heavy aromatic fraction having an initial boiling point greater than 350 °C, a 90% distillation point less than 650 °C and a hydrogen content greater than 8.5% by weight according to ASTM D2887, when the bitumen consists of B1 and F, the bitumen contains at most 75% by weight of B1, when the bitumen consists of B1 and B2, the bitumen contains at most 50% by weight of B1, and when the bitumen consists of a mixture of F and B2 and B1, the bitumen contains 70% by weight of B1, and the sum of the weight percentages of B1, B2 and F is equal to 100%.

[0043] According to a fourth aspect, the present invention relates to a method for preparing a bitumen according to the present invention, the method comprising:

[0044] - The first stage a) of the hydroconversion of a heavy hydrocarbon feedstock, which is carried out in the presence of hydrogen in a first hydroconversion section comprising at least one three-phase reactor operating in a fluidized bed form and containing at least one hydroconversion catalyst, at an absolute pressure of 2 MPa to 38 MPa, at a temperature of 300 °C to 550 °C, with a space velocity of 0.05 h -1 to 10 h -1 per volume of each three-phase reactor and with a hydrogen quantity of 50 Sm 3 / m 3 to 5000 Sm 3 / m 3 to obtain a liquid hydroconversion effluent with reduced contents of C7 asphaltenes, Conradson carbon, metals, sulfur, and nitrogen;

[0045] - Optionally, stage b) of separating the hydroconversion effluent produced in the first hydroconversion stage to form at least one light fraction and one heavy fraction;

[0046] - Optionally, the second stage c) of the hydroconversion of the liquid hydroconversion effluent produced in the first hydroconversion stage a) or the heavy fraction produced in stage b), which is carried out in the presence of hydrogen in a second hydroconversion section comprising at least one three-phase reactor operating in a fluidized bed form and containing at least one hydroconversion catalyst, at an absolute pressure of 2 MPa to 38 MPa, at a temperature of 300 °C to 550 °C, with a space velocity of 0.05 h -1 to 10 h -1 per volume of each three-phase reactor and with a hydrogen quantity of 50 Sm 3 / m 3 to 5000 Sm 3 / m 3 ;

[0047] - Stage d) of the atmospheric distillation followed by vacuum distillation of part or all of the liquid hydroconversion effluent produced in the first hydroconversion stage a) or the liquid hydroconversion effluent produced in the second hydroconversion stage c), producing at least one first vacuum residue R1 boiling mainly at a temperature of 350 °C or higher, said vacuum residue containing a residual fraction boiling at a temperature of 540 °C or higher;

[0048] - Stage e) of the deasphalting of the first vacuum residue R1 produced in stage d), at a temperature of 40 °C to 150 °C and a pressure of 2 to 6 MPa, using at least one hydrocarbon solvent mainly comprising compounds having 3 to 4 carbon atoms, preferably butane or propane or a mixture thereof, and with a solvent / feedstock ratio (volume / volume) of 4 / 1 to 10 / 1, producing a deasphalted fraction DAO and pitch;

[0049] - Stage f) of preparing bitumen, including mixing part or all of the pitch produced in stage e) as the first bitumen base B1 with the second bitumen base B2 and / or the flux F, B2 being composed of part of the second vacuum residue R2 produced from the first vacuum residue R1 and / or distilled crude oil, and F being composed of at least one heavy aromatic fraction, to prepare the bitumen such that the bitumen contains 40 wt% to 75 wt% of B1 and 25 wt% to 60 wt% of B2 and / or F, where when the bitumen is composed of B1 and F, it contains at most 75 wt% of B1, when the bitumen is composed of B1 and B2, it contains at most 50 wt% of B1, and when the bitumen is composed of a mixture of F and B2 and B1, it contains at most 70 wt% of B1, and the sum of the weight percentages of B1, B2, and F is equal to 100%.

[0050] Other subjects and advantages of the present invention will become apparent upon reading the following description of specific exemplary embodiments of the invention given by way of non - limiting examples. Specific embodiments

[0051] The bitumen according to the present invention comprises:

[0052] - 40 wt% to 75 wt% of a first bitumen base B1, the first bitumen base B1 being composed of pitch obtained by solvent deasphalting of a first vacuum residue R1, the first vacuum residue R1 being produced by distilling the effluent from a fluidized - bed hydroconversion process of a heavy hydrocarbon feedstock, B1 having a softening point of 50°C to 110°C, and

[0053] - 25 wt% to 60 wt% of a second bitumen base B2 and / or a flux F composed of at least one heavy aromatic fraction having an initial point greater than 350°C, a 90% distillation point less than 650°C, and a hydrogen content greater than 8.5 wt% according to standard ASTM D2887, B2 being composed of the second vacuum residue R2 produced from R1 and / or crude oil distillation, it being understood that the bitumen contains at most:

[0054] 75 wt% of B1, when the bitumen is composed of B1 and F,

[0055] 50 wt% of B1, when the bitumen is composed of B1 and B2, and

[0056] 70 wt% of B1, when the bitumen is composed of a mixture of F and B2 and B1, and

[0057] The sum of the weight percentages of B1, B2, and F is equal to 100%.

[0058] In the following part of the specification, for simplicity of reading, the following abbreviations are used:

[0059] B1: The first bituminous base of the bitumen according to the invention, i.e. the pitch obtained by solvent deasphalting of the first reduced crude R1 resulting from the distillation of the effluent hydroconverted by a ebullated bed hydroconversion process of a heavy hydrocarbon feedstock;

[0060] B2: The second bituminous base which can participate in the bituminous composition according to the invention, which is R1 or R2 or a mixture of R1 and R2;

[0061] R1: The first reduced crude resulting from the distillation of the effluent hydroconverted by a ebullated bed hydroconversion process of a heavy hydrocarbon feedstock, which is sent to the solvent deasphalting stage for producing B1;

[0062] R2: The second reduced crude resulting from crude oil distillation, i.e. directly obtained from crude oil distillation without any other treatment;

[0063] F: The flux which can participate in the bituminous composition according to the invention, consisting of at least one heavy aromatic fraction having an initial boiling point greater than 350 °C, a 90% distillation point less than 650 °C and a hydrogen content greater than 8.5% by weight according to standard ASTM D2887, such as for example the aromatic extract resulting from solvent extraction in a lubricating oil production line (also known as oil production line).

[0064] For a better understanding of the invention, some definitions are given hereinafter.

[0065] The bitumen or bituminous binder according to the invention is a mixture of bituminous bases or a mixture of one or more bituminous bases and a flux, and corresponds to the finished product, i.e. a product having physical properties suitable for its final use, particularly in road construction and civil engineering, and preferably in the field of road construction.

[0066] In the present specification, the expression bituminous base is used to denote a component of bitumen, and more particularly a fraction of bitumen from a given source, such fraction generally having chemical and physical characteristics, that is to say a given chemical composition and given physical property characteristics of the source from which it is derived. The bituminous bases according to the invention exhibit physical properties specific to bitumen, particularly certain properties related to hardness and viscosity.

[0067] The important physical properties of bituminous bases are particularly mentioned in the regulatory literature characterizing bitumen. They are mainly the properties of hardness and viscosity. The important physical parameters characterizing road bitumen include for example the softening point (ring and ball temperature in °C) according to standard NF EN 12591 and the penetration at 25 °C (unit 1 / 10 mm), which are measured according to standardized methods. These methods are recalled at the end of the present specification (the standards of which are listed in standard NF EN 12591).

[0068] In the present specification, a flux is a component capable of fluidizing bitumen. The flux of the bitumen according to the invention can modify the properties of one or more bitumen bases of the bitumen according to the invention, in particular by reducing the ring and ball softening point, and / or by increasing the penetration at 25 °C, and / or by improving the oxidation stability (e.g. measuring the ring and ball softening point and the penetration at 25 °C after the RTFOT test).

[0069] According to standard ASTM D6560 (corresponding to standard NF T60-115), C7 asphaltenes (also referred to as asphaltenes in the present specification) are heptane-insoluble compounds.

[0070] In the present specification, unless otherwise stated, pressures are expressed as absolute values.

[0071] According to the invention, there is thus used as the first bitumen base B1 for preparing bitumen in the form of a mixture with B2 and / or F the pitch obtained by solvent deasphalting of the vacuum residue resulting from the distillation of the effluent hydroconverted by a fluidized bed hydroconversion process of a heavy hydrocarbon feedstock, said pitch being the "final" residue of such a process. B1 constitutes from 40% to 75% by weight of the bitumen, and the remainder of the bitumen, i.e. from 25% to 60% by weight of the bitumen, consists of B2 and / or F.

[0072] B1 has a softening point of from 50 °C to 110 °C, B2 consists of R1 and / or R2, F consists of at least one aromatic extract, and the bitumen comprises:

[0073] - at most 75% by weight of B1, when the bitumen consists of B1 and F,

[0074] - at most 50% by weight of B1, when the bitumen consists of B1 and B2, and

[0075] - at most 70% by weight of B1, when the bitumen consists of a mixture of F and B2 and B1.

[0076] Although neither bitumen base B1 nor B2 can be used alone (i.e. without another component (including the flux) participating in formulating the bitumen) to formulate a standard-compliant bitumen, in particular a bitumen compliant with the standards for road bitumen, such as those of document NF EN12591, the advantageous combination of B1 with B2 and / or F in the indicated proportions can.

[0077] The first bitumen base B1

[0078] According to the invention, there can be formulated bitumens containing a large amount, i.e. from 40% to 75%, of pitch obtained by solvent deasphalting of the vacuum residue resulting from the distillation of the effluent hydroconverted by a fluidized bed hydroconversion process of a heavy hydrocarbon feedstock, said pitch being the "final" residue of such a process.

[0079] The ebullated bed hydroconversion process and the production of this final residue involved in the bituminous composition according to the invention are described below.

[0080] The feedstock for the ebullated bed hydroconversion process to produce B1 is preferably the vacuum residue resulting from the direct distillation of crude oil, i.e., without stages other than the distillation (atmospheric and vacuum) of crude oil.

[0081] Crude oil is also understood to mean a mixture of crude oils.

[0082] According to one embodiment, the crude oil is different from asphaltic crude oil, which can, for example, eliminate the need to use highly specific crude oils (i.e., asphaltic crude oils) and can increase the value of the products (other than asphaltic crude oil used for manufacturing bitumen) produced from the treatment of crude oil by a refinery.

[0083] Asphaltic crude oil is understood to mean a crude oil, the direct distillation residue of which by vacuum distillation can have properties compatible with those required for bitumen, for example in terms of penetration or softening point. Among the approximately 1300 crude oils compiled in the world, only 10% are used by refiners for the direct preparation of bitumen bases. They relate to heavy crude oils, which have a high content (from approximately 20% to 50% by weight) of vacuum residue distilled above 500 °C (in fact even 550 °C), and the residual fractions of which have a generally higher density than 1030 kg / m 3 and a viscosity at 100 °C generally greater than 3000 mm 2 / s, a saturated hydrocarbon content generally less than 10% (wherein at most a few percent are paraffins) and a rather high to high content of heptane asphaltenes, generally greater than 10% by weight. These properties are generally associated with a high sulfur content (generally greater than 4% by weight): typical examples of asphaltic crude oils are heavy crude oils from Venezuela or Mexico, or Arabian heavy crude oil produced in Saudi Arabia.

[0084] For example, the vacuum residue generally used as the feedstock for the ebullated bed hydroconversion process comes from Ural crude oil, the direct distillation vacuum residue of which is too soft to manufacture bitumen bases. It also contains a rather high content of paraffins, approximately 15% by weight according to the fractional distillation point, and a low content of C7 asphaltenes, approximately 5% by weight according to the fractional distillation point.

[0085] On the other hand, the deasphalted pitch obtained from the unconverted vacuum residue after hydroconversion is much harder, has a very low content (negligible) of saturated hydrocarbons and a high content of aromatics, resins and asphaltenes, generally having a C7 asphaltene content of 10% to 40% by weight and a saturated hydrocarbon content of less than 6% by weight.

[0086] B1 has a softening point of from 50 °C to 120 °C. Preferably, B1 has a softening point of from 55 °C to 110 °C and more preferably from 70 °C to 100 °C.

[0087] Preferably, B1 has a penetration at 25 °C of less than 20 1 / 10 mm.

[0088] As is known to those skilled in the art, such final residues differ from conventional bituminous binders in their chemical composition and their physicochemical and rheological properties, such as atmospheric or vacuum distillation residues from crude oil, visbroken residues, or slurry residues from catalytic cracking such as fluid catalytic cracking (FCC), or ebullated bed hydroconversion vacuum residues.

[0089] Thus, the final residues used in the present invention differ from atmospheric or vacuum distillation residues from crude oil, which result from methods for separating the various hydrocarbon fractions of crude oil in which the molecules undergo no (or very little) transformation, and from the heavy hydrocarbon feedstocks in the ebullated bed hydroconversion process from which the present invention is obtained. Atmospheric or vacuum residues resulting from crude oil distillation may contain from 2% to 25% by weight of asphaltenes.

[0090] Visbroken residues, more particularly visbroken vacuum residues, are residues obtained by vacuum distillation of the products resulting from a visbreaking process. Visbreaking is known to represent the treatment of heavy hydrocarbon feedstocks which consists essentially in bringing these feedstocks in the liquid state to the cracking temperature of the heaviest hydrocarbons in a furnace. The cracking reaction may be carried out continuously in a soaker in which, without additional heating, the feedstocks move at a rate such that their residence time at the temperature considered is sufficient to obtain the desired cracking of the heavy molecules to provide lighter molecules. The temperature is generally about 400 °C to 500 °C and the pressure is about 0.2 to 3 MPa. The cracking results in a reduction in the viscosity of the treated feedstocks. The cracking products (including the gaseous products which may form) are discharged in the direction of the assembly in order to be fractionated by atmospheric distillation and then by vacuum distillation. Visbroken residues (VBR) may contain from 10% to 30% by weight of asphaltenes.

[0091] Residues from catalytic cracking (such as the FCC process) result from a process in which the molecules are cracked in the presence of a specific deterioration catalyst and optionally molecular hydrogen to provide lighter molecules. The FCC process is generally carried out under temperature conditions of 480 °C to 540 °C and pressure conditions of 0.2 MPa to 0.3 MPa. The 350 °C+ fraction may contain from 0.1% to 8% by weight of asphaltenes.

[0092] Slurry residue is the final vacuum residue produced by a slurry-phase hydroconversion process. The slurry-phase hydroconversion process is carried out under very severe conditions to convert complex heavy feedstocks such as atmospheric residue and vacuum residue, residue produced by a deasphalting unit, visbreaking (thermal cracking) effluent, 350 °C+ heavy effluent (including FCC slurry) produced by an FCC unit, shale oil, biomass or coal. The slurry-phase hydroconversion process is typically carried out at a temperature of 400 °C to 500 °C, such as 410 °C to 470 °C and at a hydrogen pressure of typically 9 MPa to 25 MPa, such as 10 to 17 MPa. The liquid hourly space velocity (the ratio of feedstock flow rate to reaction volume) is typically 0.05 to 1.5 h -1 -1. These processes are typically carried out in an isothermal bubble column reactor. After the hydroconversion stage in a reactor containing a catalyst as a slurry containing at least one metal, separation of the hydroconversion effluent is carried out, which separation comprises three sub-stages, each carried out in a distillation column: distillation of the hydroconverted slurry effluent to provide a C6- fraction and a C6+ fraction at high temperature and high pressure (about 300 °C and 15 MPa), followed by atmospheric distillation (at atmospheric pressure) of the C6+ fraction at high temperature (about 300 °C) to obtain a 350 °C+ fraction, and subsequently vacuum distillation of the 350 °C+ fraction at high temperature (greater than 300 °C) to form a 525 °C- fraction and a 525 °C+ fraction corresponding to the final slurry residue. The slurry residue can contain a significant amount of asphaltenes, such as 15% to 50% asphaltenes, depending on the source of the feedstock. However, due to the slurry technology based on the use of extremely small-sized catalysts, slurry residues differ from other residues in that they contain a variable content of catalyst particles, such as up to 5 wt% of the residue.

[0093] The vacuum residue of the ebullated bed hydroconversion process is from the atmospheric distillation and subsequent vacuum distillation of the effluent produced by one or more ebullated bed hydroconversion stages as described hereinafter for the hydroconversion process (which is the source of B1 and R1). Such residues have a variable asphaltene content, also depending on the source of the feedstock, and are for example greater than 5 wt% and less than 10 wt%. Different from slurry residues, they do not contain a significant amount of catalyst.

[0094] Second asphaltic base B2

[0095] According to the invention, the bitumen can contain a second asphaltic base B2 which is a vacuum residue produced by the same hydroconversion process (same treated feedstock and same process) as the source of B1 or another vacuum residue R2 produced by direct distillation of crude oil, in the presence or absence of F in the bitumen. The second asphaltic base can also consist of a mixture of R1 and R2.

[0096] First vacuum residue R1

[0097] The source of R1 is described in detail below in the context of describing a ebullated bed hydroconversion process. R1 and B1 are from the same ebullated bed hydroconversion process.

[0098] Thus, for B1, the feedstock for the ebullated bed hydroconversion process is preferably the vacuum residue produced by directly distilling crude oil (or a mixture of crude oils), and the crude oil can be different from asphaltic crude oil, as described above for B1.

[0099] R1 does not contain catalyst particles, or may be in trace amounts (< 100 mg / kg) form.

[0100] R1 can have a C7 asphaltene content greater than 5% and less than 10 wt%.

[0101] R1 can have a saturate hydrocarbon content greater than 10 wt%.

[0102] R1 preferably has a softening point less than 50 °C. Preferably, R1 has a softening point less than 45 °C and more preferably less than 40 °C. R1 preferably has a softening point greater than 28 °C.

[0103] Preferably, R1 has a penetration at 25 °C greater than 60 1 / 10 mm. R1 preferably has a penetration at 25 °C less than 400 1 / 10 mm.

[0104] Second vacuum residue R2

[0105] R2 is the second vacuum residue produced by direct distillation of crude oil, i.e., there is no stage other than crude oil distillation. R2 is thus different from R1.

[0106] R2 is obtained by atmospheric distillation of crude oil followed by vacuum distillation.

[0107] Preferably, the crude oil is different from asphaltic crude oil, as explained above, since there is no constraint to use a specific crude oil (such as asphaltic crude oil) which constitutes a small part of the world crude oil production, which provides an advantage.

[0108] R2 can be from the distillation of crude oil that is different from the crude oil that can be used to form the vacuum residue which is the feedstock for the ebullated bed hydroconversion process that provides R1 and B1.

[0109] Advantageously, the crude oil is the same as the crude oil that produces the vacuum residue which is the feedstock in the ebullated bed hydroconversion process (which is the source of R1 and B1). Thus, the asphalt according to the present invention can be formed from a single and same crude oil, which is preferably different from asphaltic crude oil.

[0110] R2 can have an asphaltene content of 5 wt% to 20 wt%.

[0111] R2 preferably has a softening point of less than 50 °C. Preferably, R2 has a softening point of less than 45 °C and more preferably less than 40 °C. R2 preferably has a softening point of greater than 28 °C.

[0112] Preferably, R2 has a penetration at 25 °C of greater than 60 1 / 10 mm. R2 preferably has a penetration at 25 °C of less than 400 1 / 10 mm.

[0113] Flux F

[0114] According to the invention, the bitumen can contain the flux F in the form of a mixture with the first bituminous base B1 or in the form of a mixture with B1 and the second bituminous base B2.

[0115] F consists of at least one heavy aromatic fraction having an initial point of greater than 350 °C, a 90% distillation point of less than 650 °C and a hydrogen content of greater than 8.5% by weight according to standard ASTM D2887, and preferably consists of said heavy aromatic fraction (i.e. only one heavy aromatic fraction).

[0116] F is advantageously a fraction of petroleum origin having a low content of saturated hydrocarbons, usually less than 10% by weight, and a high aromaticity tendency.

[0117] Preferably, the heavy aromatic fraction is an aromatic fraction extracted from a vacuum distillate, which is advantageously obtained during the manufacture of lubricating oils, such as the aromatic extract resulting from the solvent extraction of a vacuum distillate obtained in a lubricating oil manufacturing process. Generally, the aromatic extract produced by this type of process has a density of 1000 g / l to 1050 g / l, a saturated hydrocarbon content of less than 10% by weight, an aromatic compound content of greater than 50% by weight and a hydrogen content of 8.5% to 11% by weight.

[0118] Bitumen composition

[0119] According to the invention, the bitumen is a binary composition, a ternary composition or a quaternary composition.

[0120] According to one embodiment of the invention, the bitumen is a binary composition and consists of B1 and F or B1 and R1.

[0121] When the bitumen according to the invention consists of B1 and F, it contains 40% to 75% by weight of B1.

[0122] When the bitumen according to the invention consists of B1 and B2, it contains 40% to 50% by weight of B1, and B2 preferably consists of R1.

[0123] According to another embodiment, the bitumen is a ternary composition and consists of B1, B2 (consisting of R1 or R2) and F.

[0124] When the bitumen according to the invention consists of a mixture of F and B2 and B1, it contains 40% to 70% by weight of B1.

[0125] According to one embodiment, the ternary composition bitumen according to the invention contains 40% to 60% by weight of B1, 25% to 45% by weight of B2 (consisting of R1 or R2), and 5% to 15% by weight of F. More preferably, such ternary composition bitumen contains 40% to 55% by weight of B1, 30% to 45% by weight of B2 (consisting of R1 and / or R2), and 5% to 15% by weight of F.

[0126] According to one embodiment of the invention, the bitumen is a quaternary composition and consists of B1, B2 (consisting of R1 and R2), and F.

[0127] It should be remembered that the sum of the weight percentages of B1, B2, and F is always equal to 100%.

[0128] The bitumen according to the ternary composition preferably consists of B1, R1, and F, which particularly has the following advantages: The two bitumen bases B1 and B2 (B2 consists of R1) are derived from the same ebullated bed hydroconversion process for treating the same heavy hydrocarbon feedstock.

[0129] Thus, the bitumen according to the invention can advantageously be formulated solely or almost solely from the residue oil from the ebullated bed hydroconversion process: This is the case where the binary composition of the bitumen according to the invention consists of B1 and R1. This is also the case where the ternary composition of the bitumen according to the invention consists of B1, R1, and F, where B1 and R1 can, for example, account for 85% to 95% by weight of the bitumen, and F can account for 5% to 15% by weight of the bitumen.

[0130] The bitumen according to the invention is advantageously a road bitumen, which has a ring and ball softening point greater than or equal to 43 °C and less than 58 °C, and a penetration at 25 °C greater than or equal to 35 °C and less than 100 °C.

[0131] The bitumen according to the invention can be a bitumen of grades 35 - 50 to 70 - 100 according to standard FR EN 12591.

[0132] The bitumen according to the invention can be a bitumen of PG 58 - 16 grade according to the North American Superpave system.

[0133] The invention thus also relates to a road pavement consisting of a mixture of the bitumen according to the invention and suitable inorganic aggregates (such as aggregates, namely pebbles, gravel, or sand).

[0134] Fluidized bed hydroconversion process

[0135] The fluidized bed hydroconversion process for the hydroconversion of heavy hydrocarbon feeds (such as the H-Oil TM type) is a process known to those skilled in the art. Such processes are based on the hydroconversion of heavy hydrocarbon feeds in one or more three-phase hydroconversion reactors that can be connected in series and / or in parallel, typically using the technology of the H-Oil TM process and carried out under its conditions, as described in the following: Patent US 4 521 295 or US 4 495 060 or US 4 457 831 or US 4 354 852, or the paper AIChE, March 19 - 23, 1995, Houston, Texas, paper No. 46d, “Second generation ebullated bed technology”, or Chapter 3.5 “Hydroprocessing and Hydroconversion of Residue Fractions” of the book “Catalysis by Transition Metal Sulphides” published by Éditions Technip in 2013. According to this embodiment, each three-phase reactor operates in a fluidized bed form, called an ebullated bed. Each reactor advantageously includes a recycle pump that can maintain the catalyst in the form of an ebullated bed by continuously recycling at least a portion of the liquid fraction, advantageously withdrawn at the top of the reactor and reinjected at the bottom of the reactor.

[0136] The method for preparing B1 and R1 participating in the asphalt composition according to the present invention and the feedstock treated in the method are described in more detail below.

[0137] Heavy hydrocarbon feedstock for a fluidized bed hydroconversion process

[0138] The feedstock treated in the fluidized bed hydroconversion process is a heavy hydrocarbon feedstock. Advantageously, the feedstock is a feedstock containing hydrocarbon fractions produced in a refinery. The feedstock according to the present invention includes feedstocks containing hydrocarbon fractions (at least 80% by weight of which have a boiling point greater than 300 °C), atmospheric residue and / or vacuum residue, atmospheric and / or vacuum residue from hydrotreating, from hydrocracking and / or from hydroconversion, fresh or refined vacuum distillates, steam cracking residue, fractions from cracking units such as FCC, coking or visbreaking, aromatic fractions extracted from units for preparing lubricants, deasphalted oil from a deasphalting unit, tar from a solvent deasphalting unit or similar hydrocarbon feedstocks, or combinations of these fresh feedstocks and / or refined effluents. The feedstock may also contain, by thermal methods with or without hydrogen, with or without a catalyst (such as by H-CoalTM residual fractions produced by direct liquefaction of coal, in the case of atmospheric residue and / or vacuum residue produced by the process), vacuum distillates produced by direct liquefaction of coal (such as, for example, the H-Coal TM process), or residual fractions produced by direct liquefaction of lignocellulosic biomass alone or in mixture with coal and / or fresh and / or refined petroleum fractions.

[0139] Preferably, the heavy hydrocarbon feedstock sent to the ebullated bed hydroconversion process contains a hydrocarbon fraction and preferably consists of a hydrocarbon fraction, at least 80% by weight of which has an initial boiling point of at least 300 °C, preferably at least 350 °C and preferably at least 375 °C.

[0140] The feedstock preferably consists of crude oil or one or more atmospheric residues and / or one or more vacuum residues produced by atmospheric and / or vacuum distillation of crude oil, and preferably consists of one or more vacuum residues produced by vacuum distillation of crude oil, preferably having an initial boiling point of at least 450 °C, more preferably at least 500 °C and even more preferably at least 540 °C.

[0141] All of the above feedstocks contain impurities such as metals, sulfur, nitrogen, Conradson carbon and C7 asphaltenes. This is because these types of feedstocks are usually rich in impurities, with a metal content greater than or equal to 20 ppm, and in fact even greater than or equal to 100 ppm. The sulfur content is greater than or equal to 0.5% by weight, and in fact even greater than or equal to 1% by weight and even greater than or equal to 2% by weight. The C7 asphaltene content is at least 1% by weight and is usually greater than or equal to 3% by weight. C7 asphaltenes are compounds known to inhibit the conversion of residual fractions, both through their ability to form heavy hydrocarbon residues (commonly known as coke) and through their tendency to produce deposits that greatly limit the operability of hydrotreating and hydroconversion units. The Conradson carbon content is greater than or equal to 3% by weight, and in fact even greater than or equal to 5% by weight. The Conradson carbon content is defined by standard ASTM D 482 and, for a person skilled in the art, represents a well-known evaluation of the amount of carbon residue produced after pyrolysis under standard temperature and pressure conditions.

[0142] Stages of the fluidized bed hydroconversion process

[0143] The ebullated bed hydroconversion process as a source of B1 and R1 includes stages a), optional b) and c), as well as stages d) and e), described in detail below.

[0144] First stage a) of the hydroconversion of the heavy hydrocarbon feedstock

[0145] The first stage of the hydroconversion of a heavy hydrocarbon feedstock a) is carried out in the presence of hydrogen in a first hydroconversion section comprising at least one three-phase reactor operating in a fluidized bed form and containing at least one hydroconversion catalyst.

[0146] The absolute pressure in this stage a) process is from 2 MPa to 38 MPa, the temperature is from 300 °C to 550 °C, and the space velocity per volume of each three-phase reactor is 0.05 h -1 to 10 h -1 , and the hydrogen quantity is 50 Sm 3 / m 3 to 5000 Sm 3 / m 3 .

[0147] This stage produces a liquid hydroconversion effluent with reduced contents of C7 asphaltenes, Conradson carbon, metals, sulfur, and nitrogen.

[0148] In this stage, the feedstock is converted under the specific hydroconversion conditions as described above.

[0149] Stage a) is carried out under the following preferred conditions:

[0150] An absolute pressure of 2 MPa to 35 MPa, more preferably 5 MPa to 25 MPa and in a more preferred manner 6 MPa to 20 MPa, and at a temperature of 350 °C to 500 °C, more preferably 370 °C to 430 °C and even more preferably 380 °C to 430 °C;

[0151] Preferably 100 Sm 3 / m 3 to 2000 Sm 3 / m 3 And in a very preferred manner 200 Sm 3 / m 3 to 1000 Sm 3 / m 3 of the hydrogen quantity mixed with the feedstock.

[0152] According to one embodiment, the space velocity of the reactor or "HSV" (usually referred to as "LHSV" for "liquid hourly space velocity") is 0.1 h -1 to 10 h -1 、preferably 0.1 h -1 to 5 h -1 and more preferably 0.15 h -1 to 2 h -1 . According to another embodiment, the HSV is 0.05 h -1 to 0.09 h -1 , and preferably 0.05 h-1 to 0.08 h -1 It relates to the HSV with respect to the reactor, which is defined as the ratio of the volumetric flow rate of the liquid feedstock entering the reactor measured under ambient conditions, also known as standard conditions (usually at 15 °C and 1 atm, i.e., 0.101325 MPa), to the volume of the reactor.

[0153] One or more three-phase reactors are reactors operating in a fluidized bed form. The reactors can be in series and / or in parallel. A liquid heavy hydrocarbon feedstock, a hydrogen gas phase dispersed in the form of bubbles, and a catalyst itself dispersed in the form of particles with a size generally from 0.4 mm to 4.4 mm are placed in the reactor.

[0154] According to one embodiment, the hydroconversion reactor (or each reactor if there are several reactors) advantageously includes a recycle pump, which can keep the catalyst in the fluidized bed form by continuously recycling at least a portion of the liquid fraction, advantageously withdrawn at the top of the reactor and reinjected at the bottom of the reactor.

[0155] The liquid recycle ratio (defined as the ratio of the recycled liquid flow rate to the incoming liquid feedstock flow rate) is generally from 1 to 10.

[0156] The hydroconversion catalyst for the hydroconversion stage a) contains one or more elements of Groups 4 to 12 of the Periodic Table, which may or may not be deposited on a support. Catalysts containing the following can be advantageously used: a support (preferably an amorphous support such as silica, alumina, silica-alumina, titanium dioxide or a combination of these structures, and very preferably alumina) and at least one metal of Group VIII (which is selected from nickel and cobalt, and preferably nickel), and the elements of Group VIII are preferably used in combination with at least one metal of Group VIb (which is selected from molybdenum and tungsten, and the metal of Group VIb is preferably molybdenum).

[0157] In this specification, the groups of chemical elements are given according to the CAS classification (CRC Handbook of Chemistry and Physics, published by CRC Press, edited by D.R. Lide, 81st edition, 2000 - 2001). For example, Group VIII according to the CAS classification corresponds to the metals in columns 8, 9 and 10 according to the new IUPAC classification.

[0158] Advantageously, the hydroconversion catalyst in stage a) is a catalyst comprising an alumina support and at least one Group VIII metal selected from nickel and cobalt, preferably nickel, said Group VIII element being used in combination with at least one Group VIb metal selected from molybdenum and tungsten; preferably, the Group VIb metal is molybdenum. Preferably, the hydroconversion catalyst comprises nickel as the Group VIII element and molybdenum as the Group VIb element. Advantageously, the nickel content is from 0.5% to 10% by weight, expressed as the weight of nickel oxide (NiO), relative to the weight of the catalyst, and preferably from 1% to 6% by weight, and the molybdenum content is from 1% to 30% by weight, expressed as the weight of molybdenum trioxide (MoO3), and preferably from 4% to 20% by weight.

[0159] The catalyst is advantageously used in the form of extrudates or beads. For example, the beads have a diameter of from 0.4 mm to 4.0 mm. The extrudates have, for example, the shape of a cylinder with a diameter of from 0.5 mm to 4.0 mm and a length of from 1 mm to 5 mm. The extrudates can also be objects with different shapes, such as regular or irregular trilobal, quadrilobal or other multilobal shapes. Other forms of the catalyst can also be used.

[0160] The size of these various forms of catalyst can be characterized by the equivalent diameter. The equivalent diameter is defined as the ratio of the particle volume to the particle external surface area multiplied by six. The catalyst used in the form of extrudates, beads or other forms thus has an equivalent diameter of from 0.4 mm to 4.4 mm, preferably from 0.5 mm to 4.4 mm. These catalysts are well known to those skilled in the art.

[0161] According to the method, the spent hydroconversion catalyst can be partially replaced with fresh catalyst by: preferably at regular time intervals and in a preferred manner intermittently or substantially continuously, (preferably at the bottom of the reactor), removing and introducing at the top or bottom of the reactor fresh catalyst and / or spent catalyst and / or regenerated catalyst and / or rejuvenated catalyst. The replacement of the catalyst can be carried out completely or partially with spent catalyst and / or regenerated catalyst and / or rejuvenated catalyst from the same reactor and / or another reactor from any hydroconversion stage. The catalyst can be added together with the metal in the form of a metal oxide, with the metal in the form of a metal sulfide or after pretreatment. For each reactor, the extent of replacement of the spent hydroconversion catalyst with fresh catalyst is advantageously from 0.01 kg to 10 kg per cubic meter of feedstock treated, and preferably from 0.1 kg to 3 kg per cubic meter of feedstock treated. This removal and this replacement are advantageously carried out using a device that enables the hydroconversion stage to operate continuously.

[0162] The spent catalyst removed from the reactor can also be sent to a regeneration zone where the carbon and sulfur contained therein are removed, and then the regenerated catalyst is returned to the hydroconversion stage. The spent catalyst removed from the reactor can also be sent to a recovery zone where most of the deposited metals are removed, and then the spent catalyst and the catalyst with restored activity are sent to the regeneration zone where the carbon and sulfur contained therein are removed, and then the regenerated catalyst is returned to the hydroconversion stage.

[0163] Stage b) of separating the hydroconversion effluent produced in stage a)

[0164] This stage is optional. The method preferably includes stage b).

[0165] According to this stage b), the hydroconversion effluent produced in the first hydroconversion stage a) is separated to form at least one light fraction and one heavy fraction.

[0166] Preferably, at least a part of the hydroconversion effluent produced in the first stage a) is sent to the separation stage b).

[0167] This separation stage is carried out with the aim of advantageously obtaining at least one light liquid fraction preferably boiling mainly at a temperature below 350 °C, and at least one heavy liquid fraction preferably boiling mainly at a temperature greater than or equal to 350 °C.

[0168] This separation stage b) thus produces at least two fractions, including a heavy liquid fraction, and one or more other fractions are light and intermediate fractions.

[0169] The light fraction separated in this way preferably contains dissolved light gases (H2 and C1-C4), naphtha (the fraction boiling at a temperature below 150 °C), kerosene (the fraction boiling at 150 °C to 250 °C), and at least a part of the gas oil (the fraction boiling at 250 °C to 375 °C).

[0170] At least a part of the light fraction can be sent to a fractionation unit where, for example, the light gases (H2 and C1-C4) can be extracted from the light fraction by passing through a flash drum. The gaseous hydrogen recovered in this way can be advantageously recycled to the inlet of the first hydroconversion stage a).

[0171] The fractionation unit into which the light fraction can be sent can also include a distillation column. In this case, the naphtha, kerosene, and gas oil fractions of the light fraction fed into the column are separated.

[0172] The heavy liquid fraction produced in separation stage b) (preferably boiling mainly at a temperature of 350 °C or higher) preferably contains at least one fraction boiling at a temperature of 540 °C or higher (also referred to as the 540 °C+ fraction), which is the untransformed fraction. In addition to the 540 °C+ fraction, the heavy liquid fraction may also contain fractions boiling between 375 °C and 540 °C, referred to as vacuum distillates. It may also optionally contain a portion of the gas oil fraction boiling between 250 °C and 375 °C.

[0173] This heavy liquid fraction can then be sent completely or partially to the second hydroconversion stage c) described below.

[0174] Separation stage b) can be implemented by including any separation method known to those skilled in the art.

[0175] Separation can thus be carried out in one or more of the following separation equipment items: one or more flash drums arranged in series, one or more steam and / or hydrogen stripping towers, an atmospheric distillation column, or a vacuum distillation column.

[0176] Preferably, this separation stage b) is carried out by one or more flash drums arranged in series.

[0177] According to a preferred embodiment, separation stage b) is carried out by a single flash drum. Preferably, the flash drum is at a pressure and temperature close to the operating conditions of the reactor in hydroconversion stage a) (the final hydroconversion reactor if several hydroconversion reactors are used in stage a). This embodiment is preferred, especially because the number of equipment items can be reduced, thereby reducing the capital investment.

[0178] According to another embodiment, separation stage b) is carried out by a series of several flash drums, which operate under operating conditions different from those of the reactor in hydroconversion stage a) and result in at least obtaining a light liquid fraction that can subsequently be sent at least partially to a fractionation unit, and at least obtaining a heavy liquid fraction that can subsequently be sent at least partially to the second hydroconversion stage c).

[0179] In another embodiment, separation stage b) is carried out by one or more steam and / or hydrogen stripping.

[0180] In another embodiment, separation stage b) is carried out in an atmospheric distillation column, which separates the liquid effluent produced in the first hydroconversion stage a). The heavy liquid fraction recovered from the atmospheric distillation column can then be sent at least partially to the second hydroconversion stage c).

[0181] In another embodiment, the separation stage b) is carried out by an atmospheric distillation column (separating the liquid effluent produced in the first hydroconversion stage a)) and by a vacuum distillation column which receives the residue from the atmospheric distillation column and produces a liquid heavy fraction which is then at least partially sent to the second hydroconversion stage c).

[0182] The separation stage b) can also be composed of a combination of the various embodiments described above in a different order than that described.

[0183] Optionally, before being sent to the second hydroconversion stage c), the liquid heavy fraction can be subjected to a steam and / or hydrogen stripping stage using one or more stripping columns in order to remove compounds having a boiling point of less than 540 °C from the heavy fraction.

[0184] Second hydroconversion stage c)

[0185] This stage is optional. However, the process preferably includes this second hydroconversion stage c).

[0186] According to stage c), the hydroconversion of the hydroconverted liquid effluent produced in the first hydroconversion stage a) or of the heavy fraction produced in stage b) (if such a stage is used) is carried out in the presence of hydrogen in a second hydroconversion section comprising at least one three-phase reactor operating in a fluidized bed form and containing at least one hydroconversion catalyst.

[0187] The first hydroconversion stage and the second hydroconversion stage are separate stages carried out in different hydroconversion sections.

[0188] As described above for stage a), the second hydroconversion section of the second hydroconversion stage comprises at least one three-phase reactor containing at least one hydroconversion catalyst.

[0189] The second hydroconversion stage c) is carried out in a manner similar to that described for the first hydroconversion stage a), and its description is not repeated here. This applies in particular to the operating conditions, the items of equipment used, and the one or more hydroconversion catalysts used, except for the specifications given below.

[0190] In stage c), the operating conditions can be more severe than in the first hydroconversion stage a), in particular by using a higher reaction temperature (maintained in the range of 300 °C to 550 °C, preferably 350 °C to 500 °C and more preferably 370 °C to 450 °C), or by reducing the amount of hydrogen introduced into the reactor (maintained at 50 Sm 3 / m 3 to 5000 Sm 3 / m 3 of liquid feedstock, preferably 100 Sm 3 / m3 Up to 2000 Sm 3 / m 3 And more preferably 200 Sm 3 / m 3 Up to 1000 Sm 3 / m 3 (within the range). Other pressure and HSV parameters are within the same ranges as those described in the first hydroconversion stage a).

[0191] Stage d) of fractionating the hydroconversion effluent

[0192] Stage d) of fractionating part or all of the liquid hydroconversion effluent produced in the first hydroconversion stage a) or the liquid hydroconversion effluent produced in the second hydroconversion stage c) (if stage c) is employed) is carried out particularly by atmospheric distillation followed by vacuum distillation.

[0193] Thereby producing at least a first vacuum residue R1, which preferably boils mainly at a temperature of greater than or equal to 350 °C, and R1 preferably contains a residual fraction that boils at a temperature of greater than or equal to 540 °C.

[0194] Fractionation stage d) is carried out in an atmospheric distillation column and a vacuum column for receiving the atmospheric residue. According to one embodiment, stage d) also includes using one or more flash drums upstream of the atmospheric distillation column.

[0195] The purpose of carrying out fractionation stage d) is to separate the effluents with different fractionation points and advantageously obtain at least one liquid heavy fraction (referred to herein as the first vacuum residue R1), which is the un-converted vacuum residue, commonly also referred to as UCO (un-converted oil), and preferably boils mainly at a temperature of greater than or equal to 350 °C, more preferably greater than or equal to 500 °C and even more preferably greater than or equal to 540 °C.

[0196] Stage e) of deasphalting R1 produced in stage d)

[0197] In stage e) of the process, solvent deasphalting (SDA) of R1 produced in stage d) is carried out.

[0198] Solvent deasphalting is well known to those skilled in the art. Reference may thus be made to the paper by Billon et al., published in 1994, Revue de l'Institut Français du Pétrole, Volume 49, Number 5, pages 495 to 507, to the book “Raffinage et conversion des produits lourds du pétrole” [Refining and conversion of heavy petroleum products] by JF Le Page, SG Chatila and M Davidson, published by Technip, pages 17–32, or to patents US 4 239 616, US 4 354 922, US 4 354 928, US 4 440 633, US 4 536 283 and US 4 715 946. Deasphalting is a liquid–liquid extraction which is generally carried out using at least one hydrocarbon solvent having from 3 to 7 carbon atoms, preferably an alkane solvent, at an average temperature of from 60 °C to 250 °C.

[0199] Stage e) is preferably carried out at a temperature of from 40 °C to 150 °C, preferably from 45 °C to 130 °C, and a pressure of from 2 MPa to 6 MPa, and more preferably from 3 MPa to 6 MPa.

[0200] Deasphalting is advantageously carried out using at least one hydrocarbon solvent which mainly comprises (preferably more than 80%) compounds having from 3 to 4 carbon atoms, such as butane or propane or a mixture thereof.

[0201] At least one additive may optionally be added to one or more solvents. The solvents and additives which can be used are widely described in the literature.

[0202] The solvent / feed ratio (volume / volume) entering the deasphalting unit is preferably from 4 / 1 to 10 / 1, preferably from 5 / 1 to 10 / 1 and more preferably from 5 / 1 to 9 / 1.

[0203] This stage e) gives a deasphalted fraction generally called DAO (deasphalted oil) and a tar sometimes called deasphalting pitch.

[0204] Deasphalting can be carried out in one or more mixer-settlers or in one or more extraction columns. The deasphalting unit thus comprises at least one mixer-settler or at least one extraction column.

[0205] Moreover, it is possible and advantageous to recover the solvent according to the opti-critical method, i.e. by using the solution under supercritical conditions in the separation section, which is the section that can be used to implement the integrated sub-stage for separating the fraction containing DAO and the solvent or solvent mixture. This critical method can notably improve the overall economy of the process.

[0206] In the context of the present invention, it is preferred to adopt the technique of using at least one extraction column, and preferably only one extraction column (such as the Solvahl TM process).

[0207] Depending on the operating conditions and the solvent used, and on the feedstock sent to the deasphalting unit, and in particular on the quality of the vacuum residue R1 produced in fractionation stage d), the DAO yield is generally between 30% and 95% by weight.

[0208] Table 1 below gives the ranges of the operating conditions generally used for deasphalting as a function of the solvent:

[0209] Table 1

[0210] Solvent Propane Butane Pressure (MPa) 3 – 6 3 – 6 Average temperature (°C) 45 – 90 80 – 130 Solvent / feedstock ratio (v / v) 6 – 10 5 – 8

[0211] The deasphalting conditions are adapted to the quality of the DAO to be obtained, to the feedstock entering the deasphalting, and also to the quality of the pitch (depending on the use for which the pitch is intended), the pitch becoming harder as the molecular weight of the paraffinic solvent increases.

[0212] Stage e) produces a DAO substantially free of C7 asphaltenes and a pitch concentrated with most of the impurities of the vacuum residue R1.

[0213] Advantageously, the deasphalted hydrocarbon fraction DAO obtained exhibits a C7 asphaltene content of less than 0.5% by weight, preferably less than 0.1% by weight, and more preferably less than 0.08% by weight or less than 0.07% by weight, relative to the total weight of the fraction.

[0214] Advantageously, the pitch obtained exhibits a C7 asphaltene content of between 10% and 40% by weight and generally a saturated hydrocarbon content of less than 6% by weight, relative to the total weight of the pitch.

[0215] In one embodiment, all or preferably a part of the deasphalted fraction DAO is recycled in stage a) and / or in stage c).

[0216] Method for preparing pitch

[0217] The bitumen according to the invention is prepared by implementing stages a) to e) of the above-described ebullated bed hydroconversion process and mixing, in accordance with stage f) for preparing bitumen, part or all of the pitch resulting from stage e) as B1 with B2 and / or F, B2 consisting of part of R1 resulting from stage d) or of a second vacuum residue R2 resulting from the distillation of crude oil or of a mixture of R1 and R2, and F consisting of at least one heavy aromatic fraction.

[0218] The mixture is such that the bitumen contains from 40% to 75% by weight of B1 and from 25% to 60% by weight of B2 and / or F, with at most 75% by weight of B1 when the bitumen consists of B1 and F, at most 50% by weight of B1 when the bitumen consists of B1 and B2, and at most 60% by weight of B1 when the bitumen consists of a mixture of F and B2 and B1.

[0219] The mixing in stage f) can be carried out, in particular with stirring, at a temperature sufficient to provide a homogeneous mixing of B1 with B2 and / or F, at a temperature of at least 100 °C higher than the softening point of each of the bases used (for example at a temperature between 150 °C and 250 °C).

[0220] The methods (NF EN 12591) for measuring the main standardized physical properties of the bitumen according to the invention and of the bitumen bases constituting the bitumen according to the invention are summarized below.

[0221] The penetration at 25 °C is the penetration measured in accordance with standard EN 1426 (or equivalent standard ASTM D5). The penetration is the depth of penetration (expressed in tenths of a millimeter) of a standard needle of 1 mm in diameter under a load of 100 g applied for 5 s on a bitumen sample normally maintained at 25 °C or maintained at 15 °C. At the given temperature, the harder the bitumen, the weaker its penetration. The penetration is used to classify the various grades of bitumen in the European system (NF EN 12591).

[0222] Like all residual fractions consisting of tens of thousands of molecules and having a very low content of straight-chain paraffins, and unlike waxes and paraffins, bitumen does not have a sharp melting point. For this reason, a standardized method has been developed for bitumen, called the softening point or ring and ball temperature (RBT). The RBT is measured according to standard EN 1427 (or the equivalent standard ASTM D36): a small steel ball with a diameter of 9.5 mm and a mass of 3.5 g is placed on a bitumen disk that has been previously poured into a ring with an inner diameter of 19.8 mm, and the ring itself is placed on a standardized support. The assembly is placed in a water bath, the initial and stable temperature of which is 5 °C. The lower surface of the bitumen ring is 25.4 mm from the upper surface of the plate at the bottom of the support, which corresponds to the distance the ball will fall during the test. The bath is heated at a constant rate of 5 °C / min with stirring, and the ring and ball softening point (expressed as RBT) is the temperature at which the bitumen pocket formed during the fall of the ball touches a reference plate placed 25.4 mm below the bitumen ring. In this test, the higher the softening point, the harder the bitumen.

[0223] According to standard NF EN 13607-1 (or the equivalent standard ASTM D2872), the test for resistance to hardening under the action of heat and air, called the RTFOT (Rotating Thin Film Oven Test) method, allows the combined action of heat and air on a continuously renewed film of bitumen to be measured. It simulates the hardening that bitumen undergoes during kneading in mixing equipment that usually operates at 150 °C to 180 °C. The continuously renewed film of bitumen is heated in an oven at 163 °C for 75 minutes and is simultaneously continuously flushed with hot air. The hardening of the bitumen due to the combined action of the evaporation of the lighter fractions and the oxidation that hardens the bitumen is measured by measuring the decrease in penetration (EN 1426) and the increase in softening point (EN 1427) before and after the test. Depending on the bitumen grade, this δ is limited in the European specifications (NF EN 12591). The change in sample weight (expressed as a percentage) is also measured, and the change in dynamic viscosity before and after being placed in the oven can also be measured (EN 12596).

[0224] According to the standardization method mentioned in Standard NF EN 12591, other parameters appearing in Standard NF EN 12591 can be measured. The following parameters, among others, and their associated standards may be mentioned: flash point (Cleveland method, EN ISO 2592), solubility (in perchloroethylene C2Cl4, EN 12592), paraffin content (EN 12606-2), dynamic viscosity at 60 °C (referred to as "VD60", EN 125956), kinematic viscosity at 135 °C (referred to as "VC135", EN 125956), Fraass point (referred to as "FRAASS", EN 12593). Their descriptions are not elaborated herein, and those skilled in the art can consult the said regulatory literature for any necessary measurements. Example

[0225] The following examples illustrate, without limitation, asphalt formulations according to the invention (Examples 2 and 3) and the use of unconventional bases for formulating such asphalts.

[0226] The properties of the asphalt bases and asphalts mentioned in the examples are those described above, based on the measurements also described above.

[0227] Example 1: Asphalt Base and Flux

[0228] The following five asphalt bases and the following fluxes were used in the examples of asphalt formulations provided below.

[0229] Three asphalt bases, pitch 1VR1, VR1, and VRSR, were obtained from the vacuum residue of the straight-run primary fractionation (VRSR) of Ural crude oil. Ural crude oil is not an asphalt crude oil, but has been the subject of many exploration and development studies and is one of the most widely used feedstocks in the H-Oil TM type of ebullated bed hydroconversion process.

[0230] Two asphalt bases, pitch 1VR3 and VR3, were obtained from the vacuum residue of the primary fractionation (VRSR) of a mixture of Arabian Heavy (AH) and Arabian Light (AL) crude oils.

[0231] The asphalt bases pitch 1VR1, VR1, pitch 1VR3, and VR3 are from the following H-Oil TM type of ebullated bed hydroconversion process.

[0232] Base pitch 1VR1: An example of asphalt base B1. This asphalt base is obtained by the H-Oil of a feedstock consisting of the vacuum residue of Ural crude oil TMPitch obtained by dewaxing the residue VR1 produced by vacuum distillation of the distillate from hydroconversion in a hydroconversion method of the boiling bed type. The degree of conversion of the feedstock in the hydroconversion method is moderate, at 55%.

[0233] Binder pitch 1 VR3: An example of binder pitch B1. This binder pitch is obtained by propane dewaxing of the residue VR3 produced by vacuum distillation of the effluent from hydroconversion in a hydroconversion method of the boiling bed type using a feedstock consisting of a vacuum residue of an AH / AL (75 / 25) mixture. The degree of conversion of the feedstock in the hydroconversion method is high, at 80%.

[0234] Binder VR1: An example of binder pitch B2 = R1. This binder pitch is the vacuum residue VR1 produced by vacuum distillation of the effluent from hydroconversion in a hydroconversion method of the H-Oil TM type of the boiling bed type using a feedstock consisting of a vacuum residue of Ural crude oil. It is the same hydroconversion method as that for producing binder pitch 1 VR1 (degree of conversion of the hydroconversion method: 55%).

[0235] Binder VR3: An example of binder pitch B2 = R1. This binder pitch is the vacuum residue VR3 produced by vacuum distillation of the effluent from hydroconversion in a hydroconversion method of the H-Oil TM type of the boiling bed type using a feedstock consisting of a vacuum residue of an AH / AL (75 / 25) mixture. It is the same hydroconversion method as that for producing binder pitch 1 VR3 (degree of conversion of the hydroconversion method: 80%).

[0236] Binder VRSR: An example of binder pitch B2 = R2. This binder pitch is obtained by atmospheric and vacuum distillation of Ural crude oil. The Ural crude oil is the same crude oil as that from which the vacuum residue is produced and used as the feedstock for the hydroconversion methods for producing binder pitch asphalt 1 VR1 and VR1.

[0237] Flux Fs: An example of flux F. Flux Fs is the aromatic extract produced in the manufacture of lubricating oil.

[0238] The five binder pitches, asphalt 1 VR1, asphalt 1 VR3, VR1, VR3, and VRSR, cannot by themselves (independently) form an asphalt that meets the road asphalt standard, especially according to the standard NF EN 12591.

[0239] The main characteristics of the feedstocks used in the hydroconversion method of the boiling bed type are given in Table 2 below.

[0240] The abbreviation "HPLC" for the measurement of saturated hydrocarbons, aromatics, and resins refers to the method of separation by high performance liquid chromatography.

[0241] The aim of the separation method used is to quantitatively fractionate an oil sample with an initial boiling point greater than 350 °C into four classes, called: saturates, aromatics, resin fraction and asphaltene fraction. It breaks down into two stages:

[0242] The first stage of the method consists of precipitating the asphaltenes from an excess of n-heptane. After precipitation, the sample is filtered to extract the asphaltenes and dried, and then weighed. Subsequently, the n-heptane present in the filtrate is evaporated under vacuum. The filtered sample free of n-heptane is called petrolatum. This first stage refers to the method for measuring C7 asphaltenes according to standard ASTM D6560 (corresponding to standard NF T60-115).

[0243] The second stage consists of weighing a portion of the petrolatum and injecting it into a chromatographic column filled with a mixture of silica and alumina. The saturate fraction is eluted by circulating n-heptane. The aromatic fraction is eluted with a mixture of n-heptane and toluene. Finally, the resin is eluted with a mixture of dichloromethane, toluene and methanol. All the substances eluted at the column outlet are collected to capture the various fractions separately. The contents of saturates, aromatics and resin are determined by weighing the collected material after complete evaporation of the solvent.

[0244] Table 2

[0245] Feedstock for the hydroconversion process (sent to the first hydroconversion stage) VR SR Ural VR SR (AH / AL) Density <![CDATA[kg / m 3 > 1004 1042 Dynamic viscosity at 100 °C MPa.s 436 3307 Hydrogen content wt% 10.8 10.2 Conradson carbon wt% 15.4 21.6 Saturates HPLC wt% 12.3 9.5 Aromatics HPLC wt% 43.1 39.5 Resins HPLC wt% 39.3 37.4 <![CDATA[C7 asphaltene]]> wt% 5.1 13.6 Penetration range of bitumen (NF EN 12591) 1 / 10 mm 250-350 70-100 RBT range of bitumen (NF EN 12591) ℃ 30-38 43-51

[0246] The composition and main characteristics of each bitumen base are given in Table 3 below (chemical composition of bitumen bases - see VRSR = VR SR Ural in Table 2) and Table 4 (physical parameters of bitumen bases), respectively.

[0247] Table 3

[0248] 。

[0249] Table 4

[0250] 。

[0251] The composition of the flux Fs is given in Table 5 below.

[0252] Table 5

[0253] Unit Flux Fs Density <![CDATA[Kg / m 3 > 1020 Kinematic viscosity at 100 °C <![CDATA[mm 2 / s]]> 95.0 Hydrogen content wt% 10.2 Conradson carbon wt% 8.1 Saturates HPLC wt% 8.3 Aromatics HPLC wt% 68.8 Resins HPLC wt% 23.8 <![CDATA[C7 asphaltene]]> wt% 0.1 Simulated distillation Initial point ℃ 383 10% distillation ℃ 503 50% distillation ℃ 549 90% distillation ℃ 576 Final point ℃ -

[0254] The ebullated bed hydroconversion process for obtaining bitumen bases bitumen 1VR1, VR1, bitumen 1VR3 and VR3 includes the hydroconversion stages a), b), c), d) and e) as described in the general description, the specific characteristics of which are given in the table below.

[0255] In the hydroconversion stage, reactors operating as ebullated beds are each used, and the reactor contains a NiMo / alumina hydroconversion catalyst exhibiting a NiO content of 4 wt% and a MoO3 content of 10 wt%, the percentages being expressed relative to the total weight of the catalyst.

[0256] Table 6

[0257] 。

[0258] Table 7

[0259] 。

[0260] Table 8

[0261] 。

[0262] Example 2: Bitumen according to a binary formulation

[0263] Two bitumens according to the invention are formulated from the following binary mixtures.

[0264] Mixture Mixture 1 (Mix 1): Bitumen 1 VR1 / VR1 mixture (40 / 60, by weight%)

[0265] Mixture Mixture 2 (Mix 2): Bitumen 1 VR1 / flux Fs mixture (60 / 40, by weight%)

[0266] The main properties of bitumen mixtures 1 and 2 are given in Table 9 below.

[0267] Table 9

[0268] Bitumen base Unit Mixture 1 Mixture 2 Ring and Ball softening point (RBT) ℃ 44.8 43.4 Penetration at 25 °C 1 / 10 mm 75.3 100 RBT after RTFOT ℃ 53 49.2 Penetration at 25 °C after RTFOT 1 / 10 mm 38 52 ΔRBT ℃ 8.2 5.8 % Penetration retained at 25 °C % 50 52 Penetration range of bitumen before RTFOT 1 / 10 mm 70-100 70-100

[0269] Example 3: Bitumen according to a ternary formulation

[0270] Three bitumens according to the invention are formulated from the following ternary mixtures.

[0271] Mixture Mixture 3 (Mix3): A mixture of 90.9 wt% of bitumen 1 VR1 / VR1 (60 / 40) and 9.1 wt% of Fs.

[0272] Mixture Mixture 4 (Mix4): A mixture of 90.9 wt% of bitumen 1 VR1 / VRSR (60 / 40) and 9.1 wt% of Fs.

[0273] Mixture Mixture 5 (Mix5): A mixture of 87.7 wt% of bitumen 1 VR3 / VR3 (60 / 40) and 12.3 wt% of Fs.

[0274] The main characteristics of asphalt mixtures 3 to 5 are given in Table 10 below.

[0275] Table 10

[0276] Bitumen base Unit Mixture 3 Mixture 4 Mixture 5 Ring and Ball softening point (RBT) ℃ 46.0 50.4 51.6 Penetration at 25 °C 1 / 10 mm 62 40 29 RBT after RTFOT ℃ 63.2 58.4 57.6 Penetration at 25 °C after RTFOT 1 / 10 mm 13 25 17 ΔRBT ℃ 7.8 8 6 % Penetration retained at 25 °C % 53 63 59 Penetration range of bitumen before RTFOT 1 / 10 mm 50-70 35-50 20-30 ΔRBT maximum, according to NF EN 12591 ℃ 9 8 11 % Penetration retained at 25 °C minimum, according to NF EN 12591 % 50 53 55

[0277] Example 4: Asphalt according to a binary formulation (not according to the present invention)

[0278] Two asphalts not according to the present invention were prepared according to the following binary mixtures.

[0279] Mixture Mixture 6 (Mix6): Asphalt 1 VR1 / VR1 mixture (60 / 40, by weight%)

[0280] Mixture Mixture 7 (Mix7): Asphalt 1 VR1 / flux Fs mixture (80 / 20, by weight%)

[0281] The main characteristics of asphalt mixtures 6 and 7 are given in Table 11 below.

[0282] Table 11

[0283] ​ ​ ​ ​ ​ ℃ 53.4 54.2 ​ ​ 26 24 ​ ℃ 62.4 63.2 ​ ​ 16 13 ​ ℃ 9.2 9 ​ % 62 54 ​ ​ 20-30 20-30 ​ ℃ 8 8 ​ % 55 55

[0284] Example 5: Asphalt according to a ternary formulation (not according to the present invention)

[0285] Three asphalts not according to the present invention were prepared according to the following ternary mixtures.

[0286] Mixture Mixture 8 (Mix8): A mixture of 90.9 wt% of asphalt 1 VR1 / VR1 (80 / 20) and 9.1 wt% of Fs.

[0287] Mixture Mixture 9 (Mix9): A mixture of 90.9 wt% of asphalt 1 VR1 / VRSR (80 / 20) and 9.1 wt% of Fs.

[0288] The main characteristics of asphalt mixtures 8 and 9 are given in Table 12 below.

[0289] Table 12

[0290] ​ ​ ​ ​ ​ ℃ 53.6 55.8 ​ ​ 25 20 ​ ℃ 62.2 64.8 ​ ​ 15 12 ​ ℃ 8.6 9 ​ % 60 60 ​ ​ 20-30 20-30 ​ ℃ 8 8 ​ % 55 55

Claims

1. Bitumen, which comprises: - 40% to 75% by weight of a first bitumen base B1, said first bitumen base B1 consisting of pitch obtained by solvent deasphalting of a first vacuum residue R1, said first vacuum residue R1 being produced by distillation of the effluent from the ebullated bed hydroconversion process of a heavy hydrocarbon feedstock, B1 having a softening point of 50°C to 110°C, and - 25% to 60% by weight of a second bitumen base B2 and / or a flux F, F consisting of at least one heavy aromatic fraction having an initial boiling point greater than 350°C, a 90% distillation point less than 650°C, and a hydrogen content greater than 8.5% by weight according to ASTM D2887, B2 consisting of R1 or a second vacuum residue R2 produced by crude oil distillation, or consisting of a mixture of R1 and R2, Among them, The bitumen comprises at most: 75% by weight of B1, when the bitumen consists of B1 and F, 50% by weight of B1, when the bitumen consists of B1 and B2, and 70% by weight of B1, when the bitumen consists of a mixture of F and B2 and B1, and the sum of the weight percentages of B1, B2 and F is equal to 100%.

2. The bitumen according to claim 1, wherein the heavy aromatic fraction is an aromatic fraction extracted from the vacuum distillate obtained in the lubricating oil manufacturing process.

3. The bitumen according to any one of claims 1 - 2, wherein the heavy hydrocarbon feedstock fed to the hydroconversion process contains a hydrocarbon fraction, at least 80% by weight of which has an initial boiling point of at least 300°C.

4. The bitumen according to any one of claims 1 - 2, wherein R2 is produced by atmospheric and vacuum distillation of crude oil that has been used as a feedstock in the ebullated bed hydroconversion process.

5. The bitumen according to one of claims 1-2, wherein R1 comprises a residual fraction boiling at a temperature greater than or equal to 540 °C and is obtained by atmospheric and vacuum distillation of the effluent hydroconverted by a fluidized bed hydroconversion process of a heavy hydrocarbon feedstock, said process comprising at least one hydroconversion stage carried out at an absolute pressure of 2 MPa to 38 MPa at a temperature of 300 °C to 550 °C with a space velocity HSV of -1 from 0.05 h -1 to 10 h per volume of each three-phase reactor and at a hydrogen quantity of 50 to 5000 normal cubic meters per cubic meter of heavy hydrocarbon feedstock mixed with the heavy hydrocarbon feedstock.

6. The asphalt according to claim 5, wherein the ebullated bed hydroconversion method of the heavy hydrocarbon feedstock comprises two hydroconversion stages, and the hydroconversion stages are carried out at an absolute pressure of 2 MPa to 38 MPa at a temperature of 300 °C to 550 °C with a space velocity HSV of 0.05 h -1 to 10 h -1 and are carried out with a hydrogen gas amount of 50 to 5000 standard cubic meters mixed with the heavy hydrocarbon feedstock per cubic meter of the heavy hydrocarbon feedstock.

7. The bitumen according to any one of claims 1 - 2, wherein B1 is pitch obtained by deasphalting of R1, wherein the hydrocarbon solvent mainly comprises compounds having 3 to 4 carbon atoms, wherein the solvent / feedstock volume ratio is 4 / 1 to 10 / 1, the temperature is 40°C to 150°C, and the pressure is 2 MPa to 6 MPa.

8. The bitumen according to claim 7, wherein the hydrocarbon solvent is butane or propane or a mixture thereof.

9. The bitumen according to any one of claims 1 - 2, which consists of B1 and R1.

10. The bitumen according to any one of claims 1 to 2, which consists of B1 and F.

11. The bitumen according to any one of claims 1 to 2, which consists of a mixture of R1 and / or R2 and F and B1.

12. The bitumen according to claim 11, wherein B1 accounts for 40% to 60% by weight of the bitumen, R1 and / or R2 accounts for 25% to 45% by weight of the bitumen, and F accounts for 5% to 15% by weight of the bitumen.

13. The bitumen according to claim 11, wherein B1 accounts for 40% to 55% by weight of the bitumen, R1 and / or R2 accounts for 30% to 45% by weight of the bitumen, and F accounts for 5% to 15% by weight of the bitumen.

14. The bitumen according to claim 11, which consists of a mixture of R1 and F and B1, and wherein B1 and R1 account for 85% to 95% by weight of the bitumen, and F accounts for 5% to 15% by weight of the bitumen.

15. The bitumen according to one of claims 1 - 2, which is a road bitumen having a ring and ball softening point of greater than or equal to 43 °C and less than 58 °C, and a penetration at 25 °C of greater than or equal to 35 °C and less than 100 °C.

16. The bitumen according to claim 3, wherein the heavy hydrocarbon feedstock fed to the hydroconversion process is crude oil, or consists of atmospheric residue and / or vacuum residue produced by atmospheric and / or vacuum distillation of crude oil.

17. A road pavement, which consists of a mixture of the bitumen according to one of claims 1 - 16 and mineral aggregates.

18. Use of pitch obtained by solvent deasphalting of a first vacuum residue R1 produced by distillation of the effluent hydroconverted by a fluidized bed hydroconversion process of a heavy hydrocarbon feedstock as a first bitumen base B1 for preparing the bitumen according to one of claims 1 to 16 in the form of a mixture with a second bitumen base B2 and / or a flux F, B1 having a softening point of 50 °C to 110 °C and constituting 40% to 75% by weight of the bitumen, B2 and / or F constituting 25% to 60% by weight of the bitumen, B2 consisting of R1, or a second vacuum residue R2 produced by distillation of crude oil, or a mixture of R1 and R2, and F consisting of at least one heavy aromatic fraction having an initial boiling point of greater than 350 °C, a 90% distillation point of less than 650 °C and a hydrogen content of greater than 8.5% by weight according to ASTM D2887, when the bitumen consists of B1 and F, the bitumen contains at most 75% by weight of B1, when the bitumen consists of B1 and B2, the bitumen contains at most 50% by weight of B1, and when the bitumen consists of a mixture of F and B2 and B1, the bitumen contains at most 70% by weight of B1, the sum of the weight percentages of B1, B2 and F being equal to 100%.

19. A method for preparing the bitumen according to one of claims 1 to 16, the method comprising: - First stage a) of the hydroconversion of a heavy hydrocarbon feedstock, which is carried out in the presence of hydrogen in a first hydroconversion section in a three-phase reactor comprising at least one hydroconversion catalyst operating in a fluidized bed form, at an absolute pressure of 2 MPa to 38 MPa and a temperature of 300 °C to 550 °C, with a space velocity of 0.05 h -1 to 10 h -1 per volume of each three-phase reactor and with a hydrogen quantity of 50 Sm 3 / m 3 to 5000 Sm 3 / m 3 to obtain a liquid hydroconversion effluent with reduced contents of C7 asphaltenes, Conradson carbon, metals, sulfur and nitrogen; - Optionally, a stage b) of separating the hydroconversion effluent produced in the first hydroconversion stage to form at least one light fraction and one heavy fraction; - Optionally, the liquid hydroconversion effluent produced in the first hydroconversion stage a) or the second hydroconversion stage c) of the hydroconversion of the heavy fraction produced in stage b), which is carried out in the presence of hydrogen in a second hydroconversion section in a three-phase reactor comprising at least one hydroconversion catalyst operating in a fluidized bed form, at an absolute pressure of 2 MPa to 38 MPa and at a temperature of 300 °C to 550 °C, with a space velocity relative to the volume of each three-phase reactor of 0.05 h -1 to 10 h -1 and at a hydrogen quantity of 50 Sm 3 / m 3 to 5000 Sm 3 / m 3 ; - A stage d) of atmospheric distillation followed by vacuum distillation of a part or all of the liquid hydroconversion effluent produced in the first hydroconversion stage a) or the liquid hydroconversion effluent produced in the second hydroconversion stage c), producing at least one first vacuum residue R1 boiling mainly at a temperature of greater than or equal to 350 °C, the first vacuum residue R1 containing a residual fraction boiling at a temperature of greater than or equal to 540 °C; - Stage e) of deasphalting the first vacuum residue R1 produced in stage d), at a temperature of 40 °C to 150 °C and a pressure of 2 to 6 MPa, using at least one hydrocarbon solvent mainly comprising compounds having 3 to 4 carbon atoms, and a solvent / feedstock volume ratio of 4 / 1 to 10 / 1, to produce a deasphalted fraction DAO and pitch; - Stage f) of preparing the bitumen, comprising mixing a part or all of the pitch produced in stage e) as the first bitumen base B1 with a second bitumen base B2 and / or a flux F, B2 being composed of a part of the first vacuum residue R1 and / or a second vacuum residue R2 produced from the distilled crude oil, and F being composed of at least one heavy aromatic fraction having an initial point greater than 350 °C, a 90% distillation point less than 650 °C, and a hydrogen content greater than 8.5 wt% according to standard ASTM D2887, to prepare the bitumen such that the bitumen contains 40 wt% to 75 wt% of B1 and 25 wt% to 60 wt% of B2 and / or F, wherein when the bitumen is composed of B1 and F, it contains at most 75 wt% of B1, when the bitumen is composed of B1 and B2, it contains at most 50 wt% of B1, and when the bitumen is composed of a mixture of F and B2 and B1, it contains at most 70 wt% of B1, and the sum of the weight percentages of B1, B2, and F is equal to 100%.