CZ20011573A3 - Adaptable process for preparing medicinal oils and selected middle distillates as well as apparatus for making the same - Google Patents

Abstract

The invention concerns an improved method for making high-quality basic oils optionally with simultaneous production of high-quality middle distillates, comprising hydrotreatment steps, preferably hydrocracking, on Y or beta zeolite, atmospheric distillation. The effluent (which is not vacuum-distilled) is subjected to catalytic dewaxing, preferably on NU-10, EU-1, EU-13 zeolite or ferrierite. The method then comprises steps of hydrofinishing to hydrogenate the aromatics, preferably on a catalyst comprising at least one noble metal of group VIII, chlorine and fluorine, and steps of atmospheric and vacuum distillation. The properties of the oils and the middle distillates are enhanced (flow point, viscosity index, aromatic content) resulting even in to medicinal oils.

Description

The present invention relates to an improved process for producing an oil having a base of very high quality, i.e. it has high viscosity (VI) characteristics, low aroma content, good UV stability and low flow point from kerosene slices, the boiling point of this kerosene slice being above 340 ° C, and may also be the production of high quality distillation means (such as gas oil or kerosene), which means that they have a low flavor content and a low pour point.

High-quality lubricating oils are a prime consideration for the good operation of modern machines, cars and trucks.

BACKGROUND OF THE INVENTION:

These lubricating oils are most often obtained by technological refining operations that allow the properties of kerosene to be improved. In particular, the treatment of heavy paraffinic heavy paraffins with a high linear paraffin content or low branching is necessary to obtain oil with a high quality base and the best properties, which is achieved by an operation that leads to the removal of linear paraffins or not branched paraffins from the starting product. subsequently used as the base of this oil.

High molecular weight paraffins, which are linear or very branched and which are contained in oils, lead to a high creep value and hence to solidification when used at low temperature. To reduce the creep value, it must be ensured that these linear or not branched paraffins are completely or at least partially removed.

This operation can be achieved by extraction of solvents such as toluene / methyl-ethylene ketone or methyl-isobutyl ketone, with the emphasis being on the removal of paraffin from methyl ethyl ketone (MEK) or methyl. Isobutyl ketone (MIBK). However, these operations are very expensive, not always simple, and also lead to the production of by-products, the production of impure - crude paraffins.

Another process is catalytic treatment with or without hydrogen and, although of course, depending on their selective form, the zeolites that are most commonly used among catalysts.

Zeolite-based catalysts such as ZSM-5, ZSM-11, ZSM 1, ZSM-22, ZSM-23, ZSM-35 and ZSM-38 have already been used in these processes.

SUMMARY OF THE INVENTION:

The object of the invention is to improve the entire process of producing high quality lubricating oils.

SUMMARY OF THE INVENTION The present invention provides a set of processes for producing high quality oil bases and high quality distillation means (especially gas oils). The oils thus obtained are characterized by a high viscosity (VI), a low flavor content, a low volatility, a good UV stability and a low flow point of kerosene having a boiling point above 340 ° C.

In particular, and in contrast to the conventional process and the prior art solutions, this process makes it possible to achieve a high quality oil product, in particular a reasonable choice of process conditions makes it possible to obtain white, medicinal oils (that is, of truly excellent quality). More particularly, the invention relates to a process for the production of high-quality oils and, optionally, to the production of high-quality distillation means having a hydrocarbon content of at least 20%, boiling above 340 ° C, the following processes:

a) the hydroprocessing is carried out at a temperature of 330-450 ° C, under a pressure of 5-25 MPa, with a space velocity of 0.1 to ⁰ , in the presence of hydrogen with a hydrogen / hydrocarbon volume ratio of 100-2000 and in the presence of an amorphous catalyst consisting of of ······ ···*·· · • · · ·"· "" · · ·· · ····· ·· · • · · ···· ·· · • · · · · At least one Group VIII metal and at least one Group VI B metal of the Periodic Table of the Elements,

b) hydrocracking without separation of the effluent from the hydroprocessing received, is realized at a temperature from 340 to 430 ° C under a pressure of 5-25 MPa, with space velocities of 0, ^L-_l 5h, with the presence of hydrogen with a catalyst which comprises at least one zeolite as well as at least one Group VIII element and one Group VI B element of the Periodic Table of the Elements,

(c) atmospheric distillation of the obtained hydro-cleavage effluent to separate the gases from the liquid

d) catalytic dewaxing of at least one liquid portion obtained from atmospheric distillation, which consists of compounds having a boiling point above 340 ° C and dewaxing at 200-500 ° C, under a total pressure of 1-25 MPa, with a volume schedule at a rate of 0.05-50h -1, with 50-20001 hydrogen / l charge, in the presence of a catalyst also consisting of at least one part of functional hydro-dehydrogenation and at least one molecular sieve, the microporous system of which represents at least one main open channel type pores having 9 or 10 T atoms, T being selected from the group consisting of Si / Al, P, B, Ti, Fe, Ga containing the same number of oxygen atoms, the distance between two openings of accessible pores being 9 or 10 T atoms, having a maximum of 0,75 mm and the aforementioned sieve in the n-decane test has a 2-methylnonane / 5-methylnonane ratio greater than 5,

e) the dewaxed effluent is immediately subjected to a final distillation treatment at a temperature of 180-400 ° C, which is a temperature below the catalytic dewaxing temperature of at least 20 ° C and at most 200 ° C, under a total pressure of 1-25 MPa with a volumetric flow rate of 0 , 05-LOOH ^'1, in the presence of 50-2000 liters of hydrogen / liter of charge, and in the presence of an amorphous catalyst for the hydrogenation of aromatics which comprises at least part of a metal selected from the group VIII metals and group VIB metals of the periodic table, · · · · «· · · · · · · · · · · · ·

(f) the dewaxed effluent resulting from hydroprocessing is subjected to a distillation stage consisting of atmospheric distillation and vacuum distillation, in such a way as to remove at least one part of the oil having a boiling point above 340 ° C, a point below -10 ° C, aromatic compounds below 2% by weight and VI above 95, viscosity at 100 ° C at at least 3cSt (eg 3mm / s) and in such a way that eventually at least part of the distillation agent whose pour point is lower is removed or equal to -20 ° C, aromatic content not more than 2% by weight and polyaromatic content not more than 1% by weight.

The process according to the invention consists of the following stages:

Stage a): Hydro-processing

The hydrocarbon filling, from which oils, and possibly distilling agents of high quality, are produced, consists of at least 20% of the content, which boils at a temperature of at most 340 ° C.

This makes it possible to use very diverse fillings and to process them by this process.

The filler may be, for example, light cycle oil (LCO), distillates in a vacuum resulting from direct crude distillation or a partially converted portion such as FCC, coke or viscosity reduction, or from desulphurisation or desulphurisation or origin RAT (atmospheric residue) and / or RSV (residue in the vacuum) or may be from asphalted oil or any mixture of the aforementioned agents. However, it is also important to note that the above-mentioned compositions do not in any way limit or limit the subject matter of the invention. In most cases, the oil fillings have a boiling point above 340 ° C and most above 370 ° C.

The cartridge is first subjected to a hydrotreatment during which it comes into contact, in the presence of hydrogen, with at least one catalyst that consists of an amorphous support and At least one of the Group VI B elements and at least one of the Group VIII elements at a temperature between 330 ° C and 330 ° C. and 450 ° C most preferably between 360-420 ° C and under a pressure between 5 and 25 MPa, preferably not lower than 20 MPa and a space velocity between 0.1 and 6h ^_1, most preferably between 0,3-311 ^-1 and it should also be noted that the amount of hydrogen introduced is such as the hydrogen / hydrogen carbon volume ratio, i.e. something between 100 and 2000.

During the first stage, the utilization of the catalyst is the privilege of hydrogenation as opposed to the cleavage step, utilizing it under appropriate thermodynamic and kinetic conditions, thereby allowing a very significant reduction of the aromatic polycyclic condensed hydrocarbon content. Under these conditions, most of the nitrogenous and sulphurous fill contents are converted. Thus, this operation makes it possible, in one step, to eliminate the two types of compounds that we know are a barrier to the zeolite catalyst that is used in the next steps.

This first stage allows, while realizing the pre-cleavage of the processing charge, to adjust the properties of the oil base after the completion of the first stage so that the quality of the oil base that we want to obtain at the end of the process is achieved. Advantageously, this control is possible by the nature and quality of the catalyst used in this first stage and / or by the temperature of the first stage in such a way that the degree of viscosity in the oil base is increased and the boiling point is higher than 340 ° C. the viscosity obtained before dewaxing is preferably between 80 and 150, more preferably between 90 and 140, or even between 90 and 130.

The support is in most cases based on (most preferably made of) aluminum or amorphous silica-aluminum. However, it may also consist of boron oxide, magnesium, zirconium, titanium oxide or a combination of these oxides. The hydro-dehydrogenation function is preferably formed by at least one metal or a compound of Group VIII and VI metal, most preferably molybdenum, tungsten, nickel and cobalt.

The catalyst may contain phosphorus; Finally, it is known in the art that the compound provides two advantages to hydrotreating catalysts:

Simplicity of preparation, in particular impregnation of nickel and molybdenum solution and improved hydrogenation activity. · · · · · · · · · · · · · ·

The most preferred catalysts are NiMo and / or NiW catalysts on aluminum, as well as NiMo and / or NiW catalysts on aluminum, which is doped with at least one element from the group of atoms formed from phosphorus, boron, silicon and fluorine or still NiMo and / or NiW catalysts on silica. -aluminium or on titanium-alumina-silica doped or not doped with at least one element from the group of atoms formed from phosphorus, boron, fluorine and silicon.

The total concentration of Group VI and VIII metal oxides is between 5 and 40% by weight and the most preferred percentage is between 7 and 30% and the weight ratio expressed by the oxidizing metals between Group VI metal (s) to Group VIII metal (or metals) is most preferably between 20 and 1.25, or even between 10 and 2. The concentration of phosphorus pentoxide P2O5 will be less than 15% by weight and preferably will be 10% by weight.

The product obtained from this first stage is fed to the second catalyst in the second stage of processing, without separation of NH3 or H2S or distillation.

Stage b): hydro-cleavage

The effluent resulting from the first stage a) is completely introduced into the second stage b), i.e. the second catalyst, in the presence of hydrogen, where it is hydro-cleaved in the presence of a bifunctional catalyst comprising zeolite functions and hydro-dehydrogenation functions.

During this stage, the polyaromatic and polynaphthenoaromatic compounds are partially and / or fully hydrogenated, during which they are cleaved on the acidic network, thereby forming paraffins. These paraffins, in the presence of a bifunctional catalyst, may undergo isomerization, followed by hydro-cleavage to form isoparaffins and lighter cleavage products.

·· · · · · · · · · · · · · · · · · · · · · · · ·

The conversion of multi-core polyaromatic compounds must precede hydrogenation prior to their cleavage.

The second stage catalyst consists of zeolite, support and hydrodehydrogenation function.

The hydro-dehydrogenation function is more preferably achieved by combining Group VI B metals (e.g. molybdenum and / or tungsten) and / or Group VIII metals, with the most preferred non-noble elements (e.g. cobalt and / or nickel) from the Periodic Table of the Elements. It is also preferred that the catalyst can comprise at least one part of the initiator which is deposited on the surface of the catalyst, which is an element of the group consisting of phosphorus, boron and silicon, most preferably phosphorus.

The total concentration of metals of Group VI_ELa-VIII of the Periodic Table, expressed as metal oxides in the support ratio, is most often between 5 and 40% by weight, most preferably between 7 and 30% by weight. The weight ratio (expressed as metal oxides) of Group VIII metals and Group VI B metals is preferably between 0.05 and 0.8; most preferably between 0.13 and 0.5.

This type of catalyst may advantageously comprise phosphorus, the content of which, expressed as phosphorus pentoxide in proportion to the support, will be less than 15% by weight, most preferably less than 10% by weight.

The boron and silicon contents are less than 15% by weight and most preferably less than 10% by weight (expressed as oxide).

The amorphous or poorly crystallizing support is selected from the group consisting of aluminum, silicon, aluminum silicon, aluminum-boron oxide, magnesium, silica-magnesium, zirconium, titanium oxide, clay, either alone or in any combination thereof.

Zeolite is most preferably selected from the group consisting of zeolite Y (structural type FAU, faujasite) and zeolite beta (structural type BEA), according to the nomenclature set out in · · ···· ·· · · * · · · · · · ··· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

Atlas of structural types of zeolites, WM Meier, DH Olson and Ch. Baerlocher, 4 ^th revised Edition 1996, Elsevier.

The weight content of zeolite is between 2 and 80%, more preferably between 3 and 50% with respect to the final catalyst, and most preferably between 3 - 25%.

The zeolite may optionally be doped with metal elements such as rare metals, in particular lanthanum and cerium or Group VIII noble metals such as platinum, palladium, rutenium, rhodium, iridium, iron and other metals such as manganese, zinc and magnesium.

The particularly preferred acid zeolite HY is characterized by various specificities: the S1O2 / Al2O3 molar ratio is between 6 and 70 and most preferably is between 12 and 50: the sodium content is less than 0.15% by weight determined on the calcium zeolite at 1100 ° C; the crystalline parameter has an elementary chain link between 24.58 x 10 ^-10 m and 24.24 x 10 ^-10 m and most preferably between 24.38 x 10 ^-10 m and 24.26 x 10 ^-10 m; a Cna capacity in grams of sodium, expressed in grams of Na per 100 grams of altered zeolite, neutral subsequently calcium, greater than about 0.85; BET specific surface area greater than about 400 m ² / g and most preferably greater than 550 m ² / g, water vapor adsorption capacity at 25 ° C for a partial pressure of 2,6 tors (about 34,6 MPa), greater than about 6%, a pore spacing determined by physicorption of nitrogen of between 5 and 45%, most preferably between 5 and 40% of the pore total volume of the zeolite contained in the pores with a diameter of between 20 x 10 ^-10 and 80 x 10 ^-10 m, and between 5 and 45% and most preferably between 5 and 40% of the pore volume of the zeolite contained in the pores with a diameter greater than 80 x 10 ^-10 m, and in most cases lower than 1000 x 10 ^-10 m, the remainder of the pore volume being contained in pores with a diameter lower than 20 x 10 ^'10 m.

The most preferred catalyst also comprises at least one Group VI metal and / or at least one Group VIII non-noble metal, zeolite Y and aluminum.

An even more preferred catalyst comprises nickel, molybdenum, zeolite Y as mentioned above, and aluminum.

· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

Of course, the operating conditions in which this second stage b) is implemented are also very important.

The pressure should be between 5 and 25 MPa, more preferably between 2 and 20 MPa and most preferably between 7 and 15 MPa, space velocity between 0.1 h ^-1 and 5 h ^-1 and most preferably between 0.5 and 4.0 h ' ¹ .

It is also important to adjust the temperature of this second stage in such a way as to obtain a suitable viscosity of V.I. It should be between 340 and 430 ° C and in most cases most preferred, between 370 and 420 ° C.

These two stages a) and b) can be carried out on two types of catalyst in (two or more) different reactors or, and particularly preferably, on at least two catalyst beds installed in the same reactor.

The final hydro-cleavage effluent, where hydrogen is separated, is subjected to direct atmospheric distillation (step c) in such a way as to remove the resulting gas (such as ammonia and H2S formed, or other light gases to be mentioned, possibly hydrogen ...). Thus, at least one liquid portion is obtained which contains products having a boiling point above 340 ° C.

It is also possible to advantageously distil at atmospheric pressure in order to obtain other parts (essence, kerosene, for example gas oil) with a boiling point of at most 340 ° C and parts (called residues) with an initial boiling point higher than 340 ° C (and preferably greater than 370 ° C).

This part consists of VI, before dewaxing, between 95 and 165, preferably at least 110.

According to the invention, this part (residue) is subsequently treated in the catalytic dewaxing stage, i.e. it does not undergo a vacuum distillation.

······ · · ·· ·· · · · · ··· · · · · ·. · · · · · · · · · · · · · · · · · · · · · · ·

According to another variant of the process, this residue undergoes, prior to catalytic dewaxing, the extraction of aromatic compounds (which constitute stage c ').

This extraction is carried out by all available means, the most widely used being furfurol and N-methylpyrrolidone solutions.

The naphthenoaromatic compounds are also extracted, and the obtained raffinate carries a higher degree of viscosity than the residue initially prepared to pass through this step. By this operation, we increase the VI of the product that came from the finishing stage.

According to a further embodiment of the invention which is more in line with the production of distillation means, the cleavage point is reduced and instead of cleavage at 340 ° C as mentioned above, for example, gas oil and possibly kerosene may be mentioned. a boiling point lower than 340 ° C. For example, it is possible to achieve a boiling point of at least 150 ° C.

On the other hand, the residue may undergo extraction of the aromatic compounds prior to catalytic dewaxing. This extraction is carried out by all known means, furfurol being most commonly used. It should also be stressed that the operating conditions are envisaged and are therefore included.

The raffinate obtained has higher viscosity characteristics than the residue entering this stage. We also increase the VI of the finished product.

The part thus obtained, which consists of the aforementioned compounds, undergoes a direct treatment by catalytic dewaxing, with the other parts (150 ° C) being treated separately or not in this catalytic dewaxing, according to this embodiment.

Generally, the distillation means herein is a portion or portions having an initial boiling point of at least 150 ° C and an endpoint warns just before the boiling point of the residue, i.e. up to 340 ° C, or preferably up to 370 ° C.

• · ·· · · · · · · · · · · · · · · · · · · · · ·

The advantage of this described conversion process (hydroprocessing and hydro-cleavage) (using the zeolite catalyst) is in most cases the possibility of producing lubricating oil bases, having a higher degree of viscosity than that obtained using an amorphous catalyst in the same conversion process. During the hydro-cleavage process, the viscosity at 100 ° C of the boiling point of more than 340 ° C is constant, and most preferably 370 ° C is achieved, and thus the descending level of conversion obtained is achieved.

When this conversion level is higher (over 70%), the viscosity of the residue obtained with the amorphous catalyst is such that it cannot be used to produce a higher degree of viscosity of the lubricating oil (500 N and Bright Stock). This limitation is eliminated when using the zeolite catalyst described above.

However, the viscosity at 100 ° C of the hydro-cleavage residue at 370 ° C +, which is obtained by the process using only non-zeolite catalysts (α) and-viscosity at 100 ° C of the hydro-cleavage residue under the same conditions, i.e. 370 ° C + in our process (Viooz); at the same conversion, they form a difference (Viooa / Viooz) which is less than 1, most preferably between 0.95 and 0.4.

Stage d): Catalytic hydro-dewaxing (HDPC)

The part consisting of the compounds having a boiling point above 340 ° C as mentioned above and which comes from the second stage and the atmospheric distillation c) is subjected, at least in part, most preferably all, to a catalytic dewaxing stage in the presence of hydrogen and a hydro-dewaxing catalyst which is partly acidic and partly metal hydrodehydrogenation and at least one matrix.

It should also be noted that compounds with a boiling point above 340 ° C still undergo catalytic dewaxing.

The acidic portion is provided by at least one molecular sieve whose microporous system represents the main type of channels, the openings of which are formed by rings which consist of: T atoms are constitutional tetrahedral atoms of the molecular sieve and may be of the particles contained in the following atoms (Si, Al, P, B, Ti, Fe, Ga).

In the orifices of the base ring channels, the T atoms mentioned above alternate with the same number of oxygen atoms. Thus, it can be said that these openings consist of rings that also have 10 or 9 oxygen atoms or consist of rings that also have 10 or 9 T atoms.

The molecular sieve that enters the hydro-dewaxing catalyst compound may also consist of other channel types, but whose openings are formed by rings that consist of 10 T atoms or oxygen atoms.

Molecular sieve which enter into compounds includes addition, the width of the bridge, the distance between two pore openings as mentioned above, which is at most 0.75 nm (LNM = 10 ^-9 m), preferably being between 0 and 0.50 nm, , 75 nm, or even 0.52 nm and 0.73nm.

The patent application also discloses that one of the determining factors for obtaining good catalytic properties in the third stage (hydro-dewaxing stage) is the use of a molecular sieve having a bridge width of at most 0.75 nm, preferably between 0.50 nm and 0.75 nm, or even 0.52 nm and 0.73nm.

The bridge width value is realized using graphitic aids and molecular modeling, such as Hyperchem or Biosym, which allows to assemble the surface of molecular sieves and, by keeping the number of ionic particle diameters contained in the sieve structure, to measure the bridge width.

A suitable catalyst for this process is selected by a catalytic test, called the standard n-decane conversion test, which is carried out under a partial pressure of 450 kPa of hydrogen and a partial pressure of n-C10, 1.2 kPa or a total pressure of 451.2 kPa at fixed bedding. constant effluent of n-C10, 9.5 ml / h, and a total effluent of 3.6 l / h and a catalytic amount of 0.2 g. The reaction is carried out in a descending stream. The rate of conversion is controlled by the temperature at which the reaction proceeds. The catalyst undergoing this test is pure pressed zeolite and is comprised of 0.5% platinum.

N-decane in the presence of molecular sieves and hydrodehydrogenation undergoes a hydroisomerization reaction that produces 10-carbon isomeric products and the hydro-cleavage reaction results in the formation of products having less than 10 carbon atoms.

Under these conditions, the molecular sieve used in the hydro-dewaxing stage of the invention must have the physicochemical properties described above to achieve, with the efficacy of the z-isomerized n-C 10 products, representing 5% by weight (conversion rate controlled by temperature), 2- methylnonane / 5-methylnonane greater than 5 and preferably greater than 7.

The use of such selected molecular sieves, under the conditions described above, among a large number of pre-existing molecular sieves, will allow, in particular, the production of products with a low pour point, a high degree of viscosity and good effects throughout the process according to the invention.

The molecular sieves that may enter the catalytic catalytic dewaxing catalyst assembly are, by way of example only, the following zeolites: ferrite, NU-10, EU-13, EU-1 and other zeolites with the same structure.

The most preferred molecular sieves entering the hydro-dewaxing catalyst assembly are in the EU-1 ferrite and zeolite group.

The molecular weight content of the molecular sieve in the hydro-deparaffinizing catalyst is between 1 and 90%, preferably between 5 and 90% and most preferably between 10 and 85%.

The catalyst support forms utilized herein are given by way of example only, in a non-limiting manner, and are: aluminum jellies, aluminum, magnesium, amorphous silicon-aluminum, and mixtures thereof. Techniques such as compression or granulation can be used to carry out the molding operation.

···············

The catalyst also consists of a secure hydro-dehydrogenation function, for example, using at least one Group VIII particle and preferably at least one particle in the group consisting of platinum and palladium. The Group VIII non-noble metal weight content, in contrast to the final catalyst, is between 1 and 40%, preferably between 10 and 30%. In these cases, the noble metal is associated with at least one Group VIB metal (preferably Mo and W).

When it is at least one noble Group VIII metal, the weight ratio, unlike the final catalyst, is less than 5%, preferably less than 3%, and most preferably less than 1.5%.

In the case of the use of noble metals of Group VIII, platinum and / or palladium are preferably located on the mold as mentioned above.

The hydro-dewaxing catalyst according to the invention may contain, inter alia, 0 to 20%, preferably 0 to 10% by weight (expressed as oxide) of phosphorus. The combination of Group VIB metal (s) and Group VIII metal (s) with phosphorus is particularly preferred.

The residue from the hydro cleavage (i.e. the portion with an initial boiling point higher than 340 ° C) which was obtained in step c) of the entire process according to the invention and which is to be treated in this step d) hydro-dewaxing bears the following characteristics: higher than 340 ° C, preferably higher than 370 ° C, pour point at least 15 ° C, nitrogen content less than 10 ppm by weight, sulfur content less than 50 ppm by weight or better 10 ppm by weight, viscosity grade 35 to 165 (before dewaxing) preferably at least equal to 110 and most preferably less than 150, aromatic content less than 10% by weight, viscosity at 100 ° C greater than or equal to 3 cSt (mm ² / s).

These properties are also borne by the residue obtained from the atmospheric distillation of a sample from a liquid part containing compounds having a boiling point above 340 ° C, said part having an initial boiling point lower than or equal to 340 ° C and undergoing catalytic dewaxing at this stage. .

4 · · · 4 4 4 4 4 a a a a 4 a <<<<<<<<<<<<<<<<<< «

The operating conditions under which the dewaxing step of the process according to the invention takes place are as follows:

the reaction temperature is between 200 and 500 ° C and preferably between 250 and 470 ° C, most preferably between 270 and 430 ° C;

a pressure between 0.1 and 25 MPa (10 ⁶ Pa) and preferably between 1.0 and 20 MPa;

the volumetric scheduling rate (vvh expressed in volume of injected charge per unit catalyst volume per hour) is between about 0.05 and about 50, preferably between about 0.1 and about 20 h ^-1 , most preferably between 0.2 and 1 Oh ¹ .

These conditions are selected to obtain the desired pour point.

Contact between the dewaxing charge and the catalyst is made in the presence of hydrogen. The ratio of hydrogen used is expressed in liters of hydrogen to liter of charge and is between about 50 and 2000 liters of hydrogen per liter of charge, and between 100 and 1500 liters of hydrogen per liter of charge is preferred.

The skilled artisan will appreciate that the improvement in the flow point of the oil bases achieved by this solvent dewaxing process (DPS) or catalytic hydro-dewaxing (HDPC) process may result in a decrease in the viscosity level (VI).

One feature of the process of the invention is that:

- the variation VI at the catalytic hydro-dewaxing (HDPC) stage is preferably greater than or equal to 0 for the same pour point, or

- when we observe the reduction of VI in the catalytic hydro-deparaffinization (HDPC) stage, this reduction is lower than that observed in the case of solvent dewaxing (DPS) to obtain the same flow point. Similarly, there is a difference between the fluctuations of VI, the base of the oil, when the catalytic phase takes place

5 · «···

The dewaxing, and fluctuation of the VI, of the oil base, during the dewaxing stage of the solvent, AVIhdpc / AVIdps is strictly less than 1 for the same pour point.

Stage e): Hydroconfiguration

The final effluent from the catalytic hydro-dewaxing stage is wholly, and without distillation, placed on the hydrotreating catalyst in the presence of hydrogen in such a way as to effect the hydrogenation of the extruding aromatic compounds which are detrimental to the stability of the oils and distillates. The acidity of the catalyst must be sufficiently weak so that it does not lead to the formation of a cleavage product with a boiling point below 340 ° C and does not degrade the ultimate efficiency, especially of oils.

The catalyst used in this stage consists of at least one Group VIII metal and / or at least one Group VIB rubber of the Periodic Table. Heavy metal functions: platinum and / or palladium, or a combination of nickel with tungsten, nickel with molybdenum, are very advantageous to use and to achieve hydrogenation that destroys aromatics.

These metals are deposited and dispersed to support an amorphous oxide or crystal type such as aluminum, silica, silica-aluminum.

The hydrotreating catalyst (HDF) may also comprise at least one element of Group VIIA of the Periodic Table. It therefore preferably contains fluorine and / or chlorine.

The metal content is between 10 and 30% in the case of non-noble metals, and below 2%, preferably between 0.1 and 1.5%, most preferably between 0.1 and 1.0% in the case of noble metals.

The total content of the halogen element is between 0.02 and 30% by weight, preferably between 0.01 and 15%, or between 0.01 and 10%, most preferably between 0.01 and 5%.

It is possible to cite here among the catalysts used in this stage of HDF, which leads to excellent results, in particular to obtaining medical oils, catalysts which contain: At least one noble Group VIII noble metal (for example platinum) and at least one halogen element (chlorine and / or fluorine), it is preferred to use a combination of fluorine and chlorine.

The operating conditions according to the invention in which this stage of hydropening takes place are as follows:

a reaction temperature between 180 and 400 ° C, preferably between 210 and 350 ° C, most preferably between 230 and 320 ° C;

a pressure between 0.1 and 25 MPa (10 ⁶ Pa) and preferably between 1.0 and 20 MPa;

- the volumetric scheduling rate (vvh expressed by the injected charge per unit of catalyst volume per hour) is between about 0.05 and about 100 and __. preferably between 0.1 and 30 h * ¹ .

Contact between the charge and the catalyst is made in the presence of hydrogen. The ratio of hydrogen utilized is expressed in liters of hydrogen per liter of charge, and most preferably is between 100 and 1500 liters of hydrogen per liter of charge.

One of the properties of the process according to the invention is the temperature of the HDF stage, which is lower than the temperature of the catalytic hydro-dewaxing (HDPC) stage. The difference T _H dpc - Thdf is in most cases between 20 and 200 and preferably between 30 and 100 ° C.

The effluent from the end of the HDF stage is then subjected to distillation, which includes atmospheric distillation and vacuum distillation, which separates the transformed products having a boiling point below 340 ° C and more preferably below 370 ° C (and particularly includes those formed during the stage catalytic hydro-dewaxing (HDPC)), and an oil-based part, the starting point of which warns above 340 ° C and more preferably 370 ° C.

On the other hand, this portion, in which the vacuum distillation takes place, makes it possible to separate different degrees of oil.

• ·

The oils obtained with the base according to the process have a pour point less than -10 ° C, a flavor content less than 2%, a VI greater than 95, more preferably greater than 110 and most preferably greater than 120, a viscosity of at least 3.0 cSt at 100 ° C , an ASTM color less than 1 and a UV stability such that the ASTM color increase is between 0 and 4, preferably between 0.5 and 2.5.

The UV stability test, adapted according to the procedures of ASTM D925-55 and D1148-55, is a rapid method for comparing the stability of lubricating oils that are exposed to ultraviolet light sources. The chamber, which has metal walls and where the test is being run, is equipped with a rotating plate on which the oil samples are deposited. One bulb, which produces ultraviolet rays, the same as that of the sun, is placed on the upper part of this chamber and is suspended downwards - toward the sample. Standard oil with known U.V properties is inserted between the samples. The color of ASTM D1 500 samples is observed at t = 0 and then at 45 h exposure at 55 ° C. The results are described for the standard sample and test samples as the following:

(a) initial color ASTM D1500

(b) final color ASTM D 1500

(c) color increase

d) turbidity

(e) clotting

A further advantage of the process according to the invention is that it is possible to obtain a very low aromatic content, less than 2% by weight, preferably less than 1% and even more preferably less than 0.5% by weight, thus producing white medical oils having aromatic content less than 0,01% by weight. These oils have UV absorption values of 275, 295 and 300 nanometers, respectively, are less than 0.8, 0.4 and 0.3 (ASTM D2008 method) and a Saybolt color of between 0 and

30.

Thus, in a particularly interesting way, this process also makes it possible to obtain white medical oils. White medical oils are mineral oils, which are obtained after the pressed refining of kerosene, and their quality is influenced by various regulations which lead to the guarantee of their harmlessness in the pharmaceutical use, while being free of any

They are characterized by toxicity and are characteristic of its density and viscosity. White medical oils contain particularly saturated hydrocarbon, are chemically inactive and have a low aromatic hydrocarbon content. Particular attention is paid to aromatic compounds, and in particular to 6 polycyclic aromatic hydrocarbons (P.A.H. Anglo-Saxon abbreviation polycyclic aromatic hydrocarbons), which are toxic and represent one part of the mass billion of the aromatic compound in white oils. The total flavor content can be checked by the ASTM D 2008 method, and this UV adsorption test of 275, 292 and 300 nanometers allows the absorption of less than 0.8, 0.4, and 0.3 to be checked (i.e., white oils have an aromatic content (less than 0.01% by weight). These calculations are carried out at a concentration of 1 g oil per liter, in a 1 cm container. White commercial oils differ in their viscosity, but also in their original rawness, which is paraffinic or naphthenic, and these two aspects demonstrate variation in the physico-chemical properties of white oils, but also in their chemical composition.

Part of the oils which come either from the direct distillation of crude kerosene and the subsequent solvent extraction of the aromatic compounds or from the catalytic hydrotreatment or hydro-cleavage process also contain a not negligible amount of the aromatic compounds. In the current legislative framework of most industrialized countries, white oils, called medical oils, must have a flavor content lower than the legal limits of all these countries. The absence of these aromatic compounds in oils is demonstrated by a Saybolt specific color, which must be at least 30 (+30), the maximum U.V. adsorption specification. it shall be less than 1,60 to 270 nm per net product in a 1 cm container and a maximum absorption specification of the extracted DMSO products, which shall be less than 0,1 for the US store (Food and Drug Administration, number 1211145). This last test consists of the specific extraction of polycyclic aromatic hydrocarbons with the aid of a polar solvent, mostly DMSO, and the control of their content in the extract by calculating the UV absorption in the 260-350 nm region.

The average distillate obtained has an improved pour point (less than or equal to -20 ° C), a low flavor content (not more than 2% by weight), a polyaromatic content (di and above) of less than 1% and a gaseous oil grade of greater than 50 and also higher than 52.

··························· · f · · ·· ···

A further advantage of the process according to the invention is that the total pressure can be the same in all reactors where there is the possibility of series work and the use of a single unit and thus a considerable cost reduction.

List of drawings:

The whole process is shown in the attached Figures 1 and 2, wherein Figure 1 shows the total treatment of the liquid part by hydro-dewaxing and Figure 2 shows the residue from the hydro-cleavage.

Detailed description of the invention:

Figure 1 shows a charge between a channel (1) in a hydroprocessing zone (2) (which may be comprised of one or more reactors and contain one or more catalytic beds of one or more catalysts) into which hydrogen enters (e.g. )) and where stage a) hydroprocessing is realized.

The hydroprocessed feed is passed through a channel (4) to the hydroprocessing zone (5) (which may comprise one or more reactors and consist of one or more catalytic beds of one or more catalysts) where it proceeds, in the presence of hydrogen, step b) of the hydro cleavage.

The effluent from zone 5 is led through a channel (6) to the drum (7) to separate the hydrogen which is discharged through the channel (8), whereby the effluent is subsequently distilled at atmospheric pressure in the gas compartment (9) from which the gas portion is extracted. which is discharged through the channel (10). Phase c) of the whole process is thus realized.

At the bottom of the drum, a liquid portion is obtained which contains compounds having a boiling point higher than 340 ° C. This portion is led through a channel (11) to the catalytic dewaxing zone (12).

• · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

The catalytic dewaxing zone (12) (which comprises one or more reactors, one or more catalytic beds of one or more catalysts) also receives hydrogen from the channel (13), and thus process step d) of the process can be realized.

The effluent formed in this zone is discharged through the channel (14) and is routed directly to the hydronic termination zone (15) (which comprises one or more reactors, one or more catalytic beds of one or more catalysts), from where it is discharged through the channel (16). It is also possible, if necessary, to add hydrogen to the hydrotreating zone (15) where process step e) takes place.

The effluent obtained is separated in a distillation process (process step f), which includes, inter alia, a drum (17) separating hydrogen through the channel (18), an atmospheric distillation compartment (19) and an air-empty compartment (20) that processes the remainder of the atmospheric distillation. which was fed through the channel (21), the residue having an initial boiling point greater than 340 ° C.

In the distillation process, a portion of the oil (channel 22) and parts with a lower degree of cooking such as gaseous oil (channel 23), kerosene (channel 24) are obtained as the product; the light gases are eliminated through the atmospheric compartment channel (26) and the gases are eliminated by the distillation compartment in the vacuum (27).

For the sake of simplicity, the recycling of hydrogen, which takes place at the level of the drum (7) towards the hydroprocessing and / or hydro cleavage and / or at the level of the drum (17) towards the dewaxing and / or hydrotreating, has not been illustrated.

In Figure 2, the planes of Figure 1 are shown. The difference between these figures is in the distillation of the effluent from step b) of the hydro cleavage which is discharged through the channel (6). After the hydrogen has been separated in the drum (7), this effluent is separated by atmospheric distillation in the gas compartment (9), which is extracted with the channel (10). The distillation is controlled in such a way as to obtain a residue with an initial boiling point greater than 340 ° C from channel (11) and to obtain part of the gaseous oil (sewer 28), kerosene (sewer 29) and essence (sewer 30).

• · · · · · · · · · · · · · · ·

Only this residue is treated in the dewaxing zone (12).

The recycling described below can also take place elsewhere.

The figures show a plant with 2 reactors without recycling the effluent resulting from hydro-cleavage (5).

It is also possible to recycle part of this outflow towards the hydroprocessing stage in zone (2) and / or towards the hydroprocessing stage in zone (5).

A person skilled in the art can adapt the recycling ratio according to which products are required to select the production of oil or distillation means.

It is also very common that the hydroprocessing and hydrofission zones are located in the same reactor. In this case, the hydroprocessing effluent is transferred directly without the use of a channel (4). Outflow recycling is possible either towards the hydroprocessing zone (upstream of the catalytic bed) or towards the hydro-cleavage zone.

According to another embodiment of this conversion stage (two-stage hydro-cleavage), the residue from the channel (11) having an initial boiling point above 340 ° C (as shown in Figure 2) is diverted, at least in part, to the replacement hydro-cleavage zone. (32) which differs from the hydro-cleavage zone (5) (comprising one or more reactors, one or more catalytic beds of one or more catalysts). This replacement hydro-cleavage portion may comprise the same catalyst as the hydro-cleavage zone (5) or a completely different catalyst.

The resulting effluent is recycled towards the atmospheric distillation stage.

Another part of the residue with an initial boiling point higher than 340 ° C is transferred to the catalytic dewaxing stage.

• · · · ·

Figure 3 shows possible methods of the whole apparatus, while maintaining the same planes as Figure 2, which will not be described here.

The remainder coming from the compartment (9) through the conduit (11) is led to a replacement hydro-cleavage zone (32) from where it flows through the sewer (33), which is recycled in the compartment (9). A duct (34) connected to the duct (11) exits a residue which is led to a dewaxing zone (12).

Figure 3 shows the implementation of the same reactor (31) of the hydroprocessing part (2) and the hydro cleavage (5), but the divided parts shown can be combined in any way with a spare hydro cleavage zone (32).

The apparatus of Figure 3 may also replace the apparatus of Figure 2, the hydro-dewaxing stages, the hydrotreating stage, and the distillation fixed compartment. All additional options (hydrogen recycling ...) can be used elsewhere.

According to another embodiment of the variant of Figures 2 or 3, the residue resulting from the sewer (11) is fed to an aromatic compound extraction unit (35) equipped with a solvent inlet (36), a solvent outlet (37) and a channel (38) by means of which the raffinate flows out into the catalytic dewaxing zone (12).

This variant (which corresponds to stage c ') of the process) is shown in Figure 4.

The processing of the upper flow and the flow direction is controlled by a process which is only exemplified in Figures 2 or 3.

The present invention also relates to an installation for producing high quality oil and possibly high quality distillation means comprising:

At least one hydroprocessing zone (2) comprising at least one hydroprocessing catalyst having at least one filling production channel (1) and at least one hydrogen production channel (3);

At least one hydro-cleavage zone (5) comprising at least one hydro-cleavage catalyst for treating the hydroprocessed effluent resulting from zone (2), wherein the hydro-cleavage effluent leaves the zone (5) through the channel (6); an effluent which must be equipped with at least one gas outlet port (10), at least one liquid outlet port (11) containing compounds having a boiling point above 340 ° C, at least one channel (28, 29) or 30) providing an outlet for the at least one distillate, • at least one aromatic compound extraction unit (35) for processing the residue, at least one solvent conduit (35), at least one outlet conduit (36) and at least one conduit (38) for the raffinate outlet, • at least one catalytic dewaxing zone (12) comprising at least one dewaxing and a catalytic dewaxing zone (12) is also provided with at least one dewaxed effluent outlet channel (14), at least one hydrotreating zone (15) for dewaxed effluent treatment a at least one distillation zone comprising at least one atmospheric distillation compartment (19), which is equipped with at least one air-empty compartment (20), the compartment the atmospheric distillation (19) being equipped with at least one light gas outlet channel (26), at least one (23, 24 or 25) outlet channel for the at least one distillate and at least one uniform residue outlet channel (21), the air-empty compartment (20) contains at least one • · • «• ·

a channel (22) for outputting the oil portion and at least one channel (27) for outputting the other compounds.

According to another embodiment, the invention also relates to a device in which the zones (2) and (3) are placed in the same reactor equipped with at least one charge-in channel (1), at least one hydrogen-inlet channel (3) and at least one channel (6) for the outlet of the hydro-split effluent, said device comprising, inter alia, at least one spare hydro-cleavage zone (32), which is equipped with at least one channel (11) for receiving the residue resulting from the atmospheric distillation compartment (9) and at least one a channel (33) for the outlet of such a split cleavage, said channel (33) opening into a channel (6) for recycling the aforementioned effluent and in addition the device comprises at least one channel (34) located on the transfer channel (11) the residue into the aromatic compound extraction unit (35).

Example 1:

The residue from the hydro cleavage is obtained by hydro cleavage of the distillate in a vacuum, the compound of which is shown in Figure 1.

In a reactor containing an amorphous catalytic bed (15% MoO3, 5% NiO, 80% aluminum) is charged with the charge shown in Figure 1 and hydrogen under 14 MPa and H2 / HC = 100ONi / Ni by volume ratio. The space velocity of the amorphous catalyst is 0.751 &quot;. The reaction temperature is 380 ° C.

A catalyst with 12% MoO3, 4% NiO, 20% zeolite Y on aluminum is charged to the second reactor downstream of the first reactor. The product resulting from the first reactor is charged to the second reactor. The pressure is 14 MPa and the product circulates at a space velocity of 1.5b ^-1 . The effluent is grouped and then distilled in a vacuum. The properties of the residue at 375 ° C ⁺ are shown in Figure 1.

· · * * * * * * * * * * * * * * * * * * * * * * * * * ·· ·· ♦

Example 2

The residue obtained at 375 ^° C ⁺ from Example 1 is then charged to a reactor containing a hydro-dewaxing bed (0.5% Pt, 80% ferrite, the remainder being Al 2 O 3) and hydrogen at a pressure of 14 MPa and a H 2 / HC = 1000 Ni volume ratio / Ni. The space velocity is on this catalyst 1h ' ¹ . The reaction temperature is 315 ° C.

In a second reactor downstream of this first reactor, a catalyst containing 1% Pt, 1% Cl on aluminum is charged. The product resulting from the first reactor is placed in a second reactor which is maintained at 220 ° C. The pressure is 14 MPa and the product circulates at a space velocity of 0.5 h ^-1 . The effluent grouped is then distilled in a vacuum. The properties of this residue at 375 ° C ⁺ are shown in Figure 1.

The test of carbonaceous material on the dewaxing and hydrotreating residue produced in Example 2 satisfies the requirements of the standards.

On the other hand, the UV absorption of 275 nm on a clean product, in a 1 cm beaker, is 1.2, ie below the standard.

In view of these results, the dewaxed and hydrotreated residue of Example 2 is a medical oil.

Table 1

Example 1 Example 2 Cartridge the remainder from the hydro cleavage the remainder from dewaxed and hydrated cleavage First catalyst / 380 ° C 315 ° C

• · · ·

(reaction temperature Second catalyst (reaction temperature / 380 ° C 220 DEG Conversion (% by weight) / 80 Material balance (% by weight) / (% fill weight) (% by weight of hydro-cleavage residue) h ₂ s + nh ₃ / 3.26 0 C1-C4 / 1.70 12.15 C5-150 / 28,00 7.80 150-380 / 49.07 5.90 375+ 100 ALIGN! 20.47 75.20 Total 100 ALIGN! 102.50 101.05 Residue 375 ° C + charge dl 5/4 0.9377 0.8415 / V @ 100 ° C (mm ² / sec) 11.15 5,525 / Sulfur (ppm weight) 29600 6 / Nitrogen (ppm weight) 1170 3 / Color ASTMD 1500 / 2.5 / Flow point (° C) +39 +35 / The dewaxed residue 375 ° C + Dewaxed solvent Dewaxed solvent Catalytically dewaxed and hydrotreated dl 5/4 0.9479 0.8408 0.8413 V @ 40 ° C (mm ² / sec) 181 29.98 35.49 V @ 100 ° C (mm ² / sec) 12.87 5.67 6.28 VI 44 132 127 Flow point (° C) -21 -18 -18 Color Saybolt / / +30 UV absorption (D2008) /

• ·

260-280 nm / / 0.0008 280-190 nm / / 0.0007 290-300 nm / / 0.0003 300-360 nm / / 0.0002 360-400 nm / / <0.0001 300-300 nm / / 0.0002 330-350 nm / / <0.0001

Claims (13)

PATENT CLAIMS A process for the production of medical oils and possibly high-quality distillation agents, characterized in that they consist of a hydrocarbon filling having at least 20% by volume boiling at a temperature of above 340 ° C, wherein the medical oils contain a Saybolt color of at least 30, the UV absorption value less than 1,60 to 270 nm per net product in a 1 cm beaker and a maximum absorption value of the extracted DMSO products of less than 0,1, the process consisting of the following consecutive stages: (a) hydrotreating, which takes place at a temperature of 330 to 450 ° C, under a pressure of 5-25 MPa, with a space velocity of 0,1 -'h ¹ , in the presence of hydrogen in a hydrogen / hydrogen carbonate ratio of 100-2000 and in the presence of an amorphous catalyst containing at least one Group VIII metal and at least one Group VI B metal of the Periodic Table of the Elements, (b) hydro-cleavage, without separation of effluent obtained from hydroprocessing, the hydro-cleavage being carried out at a temperature of 3440-430 ° C, under a pressure of 5 to 25 MPa, with a space velocity of 0,1-5 h ^-1 , in the presence of hydrogen; presence of a catalyst comprising at least one zeolite as well as at least one Group VIII element and at least one Group VI B element of the Periodic Table of the Elements, (c) atmospheric distillation of the effluent obtained from hydro-cleavage for the separation of gases and liquids, d) catalytic dewaxing of at least one liquid part obtained by atmospheric distillation and containing compounds having a boiling point above 340 ° C, the dewaxing being carried out at a temperature of 200-500 ° C, under a complete pressure of 1 - 25 MPa, with a scheduling volume velocity of 0.05- 50 h ^-1 , with 50-20001 hydrogen / 1 charge, in the presence of a catalyst also comprising at least one hydrodehydrogenation element and at least one molecular sieve whose micropore system has at least one major type of pore hole channels having 9 or 10 T atoms wherein T is selected from the group consisting of Si / Al, P, B, Ti, Fe, Ga alternating with the same number of oxygen atoms, wherein the distance between two pore openings containing 9 or 10 T atoms is at most 0.75 mm and this molecular sieve provides the n-decane test with a 2-methylnonane / 5-netylnonane ratio greater than 5, e) the dewaxed effluent is directly subjected to a hydrotreating treatment which takes place at a temperature of 180-400 ° C, which is lower than the catalytic dewaxing by at least 20 ° C and at most 200 ° C, at a total pressure of 1-25 MPa, s a schedule at a rate of 0,05-100h ^_1 in the presence of an amorphous catalyst for the hydrogenation of aromatics comprising at least one metal of group VIII metals and the metals of group VI B of the periodic table, (f) - the effluent resulting from the hydroprocessing treatment is then subjected to a distillation stage consisting of atmospheric distillation and vacuum distillation, in order to separate at least a part of the oil having a boiling point above 340 ° C having a drain point below -10 ° C Aromatic compound content by weight of less than 2% and an VI content of more than 95, a viscosity at 100 ° C of at least 3cSt (3mm / s) and possibly separating at least a portion of distillation means having a run-off point of , a flavoring content of not more than 2% by weight and a polyaromatic content of not more than 1% by weight. Method according to claim 1, characterized in that the molecular sieve of the dewaxing stage d) is selected from the group consisting of zeolite ferrates, NU-10, EU-1, EU-13. Method according to one of the preceding claims, characterized in that the dewaxing stage d) catalyst comprises a hydrodehydrogenating element selected from the group consisting of Group VIII elements and Group VI B elements of the Periodic Table of the Elements, the aforementioned the catalyst consists, inter alia, of phosphorus. «· · ·················· Method according to one of the preceding claims, characterized in that the hydrotreating catalyst of step e) comprises amorphous support, at least one noble element of Group VIII of the Periodic Table, chlorine or fluorine. Production method according to one of the preceding claims, characterized in that the hydroprocessing steps a) and the hydro cleavage b) are carried out in the same reactor. Method according to one of Claims 1 to 4, characterized in that the hydroprocessing steps a) and the hydro cleavage b) are carried out in the same reactor. Method according to one of the preceding claims, characterized in that in step c) atmospheric distillation a residue is obtained with an initial boiling point higher than 340 ° C, which is subsequently subjected to catalytic dewaxing in step d). A process according to claim 7, characterized in that the hydro-cleaved residue is recycled at least in part in the hydrotreating step and / or in the hydro-cleaving step. Method according to claim 7, characterized in that one part of the residue of the hydro-cleavage undergoes a substitute stage of hydro-cleavage that differs from step b), the effluent obtained from step c) of atmospheric distillation is recycled, and the other part of the residue is treated in step d) dewaxing. Method according to one of Claims 7 to 9, characterized in that the residue from the atmospheric distillation of step c) is subjected to the extraction of aromatic compounds (step c ') and the obtained raffinate is catalytically dewaxed in step d). • · • * Method according to one of the preceding claims, characterized in that the white oils have a flavoring content of less than 0.01% by weight. 12. Installations for the production of high-quality oils and, where appropriate, high-quality distillation means, characterized in that it comprises: • at least one hydrotreating zone (2) comprising at least one hydrotreating catalyst having at least one filling production channel (1) and at least one hydrogen production channel (3), • at least one hydro-cleavage zone (5) containing at least one hydro-cleavage catalyst for treating the hydroprocessed effluent from zone (2), wherein the hydro-cleavage effluent leaves the zone (5) through a channel (6L) _: • at least one compartment of atmospheric distillation (9) for hydroprocessing effluent treatment, for gas outlet, at least one liquid outlet port (11) containing compounds having a boiling point above 340 ° C, at least one outlet (28, 29 or 30) providing outlet for at least one distillate, • at least one extraction unit of aromatic compounds (35) for processing the residue, at least one channel (35) for conducting the solvent, at least one outlet channel (36) and at least one raffinate outlet channel (38), • at least one catalytic dewaxing zone (12) comprising at least one dewaxing catalyst into which the raffinate enters and at least one channel (13) ) for hydrogen, wherein the catalytic dewaxing zone (12) is also provided with at least one dewaxed effluent outlet channel (14), • at least one hydrotreating zone (15) for treating the dewaxed effluent with a hydrotreating catalyst, which must also include at least one channel (16) at least one distillation zone comprising at least one atmospheric distillation compartment (19) provided with at least one air-empty compartment (20), the atmospheric distillation compartment (19) being equipped with at least one conduit (26) for light gas outlet through at least one channel (23, 24 or 25) for the outlet of at least one distillate and at least one residue collection channel (21), wherein the air-empty compartment (20) comprises at least one oil portion outlet channel (22) and at least one other compound outlet channel (27). Apparatus according to claim 12, characterized in that the zones (2) and (3) are located in the same reactor equipped with at least one filling inlet channel (1), at least one channel (3) for the inlet of hydrogen and at least one channel (6) for the outlet of the hydro-cleaved effluent, said device comprising, inter alia, at least one spare hydro-cleavage zone (32) which is equipped with at least one channel (11) for atmospheric distillation (9) and at least one channel (33) for the outlet of the thus-split effluent, said channel (33) opening into a channel (6) for recycling said effluent, and in addition the device consists of at least one channel (34) located on the channel (11) for transferring the residue to the aromatic compound extraction unit (35).