EP3418352B1 - Procede et systeme pour mélanger des agents d'amélioration de l'indice de viscosité dans des huiles de base - Google Patents

Procede et systeme pour mélanger des agents d'amélioration de l'indice de viscosité dans des huiles de base Download PDF

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Publication number
EP3418352B1
EP3418352B1 EP17176937.5A EP17176937A EP3418352B1 EP 3418352 B1 EP3418352 B1 EP 3418352B1 EP 17176937 A EP17176937 A EP 17176937A EP 3418352 B1 EP3418352 B1 EP 3418352B1
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EP
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Prior art keywords
boiler
inert gas
liquefaction chamber
line
base oil
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EP17176937.5A
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German (de)
English (en)
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EP3418352A1 (fr
Inventor
Gerhard Seewald
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Intervalve Research And Development GmbH
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Intervalve Research And Development GmbH
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/49—Mixing systems, i.e. flow charts or diagrams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/59—Mixing systems, i.e. flow charts or diagrams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/21—Jet mixers, i.e. mixers using high-speed fluid streams with submerged injectors, e.g. nozzles, for injecting high-pressure jets into a large volume or into mixing chambers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle
    • B01F25/53—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle in which the mixture is discharged from and reintroduced into a receptacle through a recirculation tube, into which an additional component is introduced
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02—Pour-point; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions
    • C10N2070/02—Concentrating of additives

Definitions

  • the process according to the invention serves to incorporate viscosity index improvers (VIV) into suitable base oils. Furthermore, arrangements for carrying out the method are claimed.
  • VIV viscosity index improvers
  • Viscosity index improvers made of high molecular weight polymers are generally present as granules, highlypaste polymer bales (mixed with a few percent by mass of a base oil) or as a highly viscous, but flowable fluid (mixed with a higher mass percentage of a base oil).
  • VI improvers are polyisobutylenes, polymethacrylates (PMA) and olefin copolymers (OCP), in particular olefinic ethylene-propylene copolymers.
  • the aim of the incorporation of VIV into base oils is to reduce the viscosity drop in mixtures when the temperature increases. This is achieved by the macromolecules being present as balls at low temperatures, which develop more and more at higher temperatures. Intermolecular interactions in the vicinity of the elongated macromolecules maintain the viscous properties there.
  • the resulting lubricant mixtures can thus be used over wide temperature ranges (multigrade oils) and ensure the required lubricant film thickness even at higher temperatures.
  • suitable amounts of VIV and base oil eg, 10 wt% VIV and 90 wt% base oil, with the VIV possibly broken up
  • VIV and base oil eg, 10 wt% VIV and 90 wt% base oil, with the VIV possibly broken up
  • temperatures above 130 ° C may be required.
  • the value of the process temperature is left little room for maneuver, because at too low temperatures, no completely homogeneous mixture is formed, or at too high temperatures, the base oil content is damaged.
  • mechanical mixing by means of stirrers improves.
  • the temperatures during the mixing process should be chosen to avoid significant thermal decomposition or undesired chemical reactions.
  • DE 2932459 C2 presents a method and an apparatus for mixing VIV as a granulate or as a powder in base oil.
  • the wall is constantly flushed with base oil, the VIV granulate or VIV powder weighed into it and fed the forming VIV base oil mixture in a loop of a colloid mill recycled , Due to the cyclic grinding process, the VIV content in the base oil is better pre-dissolved and the time for the mixing process, which is followed by another agitator tank, is significantly reduced.
  • this method is unsuitable for high paste viscosity improvers in bale form.
  • CN 205127860 U discloses a processing of base oils with a VIV already liquefied in advance by a base oil mixture.
  • a partial flow of the base oil and the liquefied and therefore also pumpable VIV is introduced separately into a first boiler and mixed with a stirrer.
  • the thus enriched with VIV premix is then over a mixer line in a second boiler combined with another partial stream of base oil, mixed with another agitator and so diluted to the final mixture.
  • a protective gas is used for overpressure.
  • the individual components, the pre- and the final mixture have sufficiently low viscosity, so that the mixing process takes place at moderate temperatures.
  • the number of revolutions of the agitator motors are sufficiently low that no aging processes with regard to temperature or shear occur.
  • this method fails with not yet liquefied, highly pasty VIV in bale shape.
  • additives such as corrosion inhibitors, friction modifiers, antioxidants, etc.
  • additives such as corrosion inhibitors, friction modifiers, antioxidants, etc.
  • the oil additives are placed in a suitable container using a dry inert atmosphere, with stirring and at slightly elevated temperatures (at about 40 ° C - 60 ° C and preferably not higher than about 40 ° C) Base oil introduced. In this way, the oil additives dissolve more easily in the oil and the lubricant is more homogeneous.
  • VIV liquefaction of highly-viscous polymer bales and granules has reportedly commonly used a high-speed shredder or high-speed agitator for liquids to shorten the mixing process between VIV and base oil by rapidly increasing the interfacial area.
  • a protective gas atmosphere nitrogen or carbon dioxide
  • the object of the invention is to develop a process for the incorporation of viscosity index improvers, which are present as a high-paste polymer bales, in base oils. This makes it possible to carry out the mixing operations in such a way that further processing of the mixtures can follow immediately. It is also an object of the invention to develop an arrangement for carrying out the method.
  • the inventive method allows in a liquefaction chamber mixing a batch of at least 70 wt% viscosity index improver and at most 30 wt% base oil by introducing heat under inert gas at overpressure and by a fluidic circulation of the liquid components in a secondary circuit. Thereafter, the admixing of the resulting dissolved concentrate into a main stream of base oil of suitable mass corresponding to a target mixture. Liquefaction of highly viscous viscosity index improvers tends to be far more difficult as the viscosity of high viscosity VIV is several orders of magnitude higher than for VIV already liquefied with base oil.
  • the dissolved concentrate (m 1 ) consists of at least 70 wt% viscosity index improver and at most 30 wt% base oil.
  • What is essential is a combination of low-shear liquefaction by means of controlled, controllable heating of the substances and of a suitable protective gas, such as, for example, nitrogen or butane or carbon dioxide.
  • a suitable protective gas such as, for example, nitrogen or butane or carbon dioxide.
  • the temperature is chosen between 90 ° C and 100 ° C and the defined overpressure in the liquefaction chamber is chosen between 100 mbar and 50 bar to prevent outgassing during the mixing of viscosity index improver in the base oil.
  • the overpressure is preferably chosen to be less than 24 bar, more preferably the overpressure is less than 10 bar.
  • the defined overpressure prevents outgassing during the mixing of viscosity index improvers in base oil and minimizes the solubility time.
  • the pressure in the boiler is less than or equal to half the pressure in the liquefaction chamber in this embodiment.
  • the arrangement according to the invention for carrying out the method for incorporating viscosity index improvers into base oils for the production of a target mixture consists of a boiler for a base oil and a liquefaction chamber for a viscosity index improver.
  • a main circuit and a secondary circuit for a separate conditioning of mixing partners of the target mixture are arranged.
  • the main circuit is arranged for priming and conditioning with base oil and the secondary circuit for liquefaction and conditioning with a viscosity index improver and base oil concentrate.
  • the main circuit connects the boiler, at least one pump, at least one heater, and a plurality of static mixers in series via a main line.
  • the liquefaction chamber is connected via a branch line to the main circuit and via a secondary line to the secondary circuit, which leads via a pump back into the liquefaction chamber.
  • a first Suction device is connected to the liquefaction chamber and a second suction device to the boiler, wherein the suction devices are operated by a common vacuum pump.
  • a first protective gas supply is connected to the liquefaction chamber and a second protective gas supply to the boiler, wherein the protective gas feeds are connected to a common inert gas pressure vessel.
  • the first suction device of the liquefaction chamber is defined by the vacuum pump, a suction line, a three-way cock and a connection to the liquefaction chamber and the second suction device of the boiler is defined by the vacuum pump, another suction line, a three-way tap and a connection to the boiler.
  • the pumps of the arrangement are low-shear rotary lobe pumps in this embodiment; other possible pumps are not excluded.
  • the heater is in this embodiment a Einschraubsheddingelasticity, with other heaters are conceivable.
  • the main line in the boiler ends in a dive with freely rotatable tail.
  • the main pipe in the boiler ends in a mixing nozzle.
  • the stub line below the liquefaction chamber opens into the main line and into a Venturi nozzle, which is located near the point of connection to the main line in the branch line.
  • a melting grid is arranged, wherein the secondary line above it opens into the liquefaction chamber.
  • the main pipe, the secondary pipe, the sting pipe and the boiler are thermally insulated.
  • inert gases in particular nitrogen
  • solubility temperature for the mixture of viscosity index improvers with base oils is lowered.
  • the output temperatures of the mixing partners can be reduced and saved about 50% to 60% of the electrical energy for the thermal conditioning of the substances.
  • inert gas at lower pressure and lower temperature the otherwise observed outgassing of ethylene and propylene, which are components of VIV based on olefinic copolymers, are avoided, thus maintaining miscibility with base oil.
  • shielding gases including the conditioning of the base oil, avoids aging processes such as oxidation and hydrolysis in the mixing partners.
  • FIG. 1 shows a diagram in which the dependence of the solubility temperature ⁇ L of a mixture of x wt% of a viscosity index improver (OCP base) and 100 wt% on olefin based - x wt% of a base oil at varying VIV fraction under atmospheric conditions in Warming cabinet (course with circles and Strichticianlinienzug) and under N 2 atmosphere and with overpressure (with approx. 5 bar with star, with approx. 9 bar with diamond marked) is represented.
  • OCP base viscosity index improver
  • the solubility temperature ⁇ L was 145 ° C, for mixtures with a VIV fraction above 20 wt%, the solubility temperature ⁇ L was 185 ° C ( FIG. 1 , Gradient with circles and dash-dot line).
  • FIG. 2 The arrangement according to the invention ( FIG. 2 ) for incorporation of viscosity index improvers into suitable base oils prevents these side effects.
  • FIG. 3 Another embodiment is shown in FIG. 3 shown.
  • the low-shear, without participation of oxygen and moisture functioning mixing plant consists of a main circuit I and a secondary circuit II for the separate conditioning of the mixing partners.
  • the arrangement consists of a boiler 7, which can be opened under atmospheric conditions and is first filled with the base oil.
  • a pump 10 for example, a low-shear rotary lobe pump, and a heater 9, for example, a screw-in, arranged.
  • static mixers 11 which support the mixing process.
  • About the main line 14 of the main circuit I is led by the boiler 7 via the pump 10 back to the boiler 7.
  • the main line 14 terminates in the boiler 7 in a dip tube 12 with freely rotatable tail to support the distribution of the incoming fluid into the boiler 7.
  • the rotatably mounted end of the dip nozzle 12 is rotated by the inflow into the boiler 7 in rotation and realized a Spiral mixing of the mixture flowing from the main line with the liquid in the boiler 7.
  • Via a sting line 16 is an interference of a dissolved concentrate m 1 , at least 70 wt% viscosity index improver and at most 30 wt% base oil, from the secondary circuit II in the Base oil, which flows through the main line 14 of the main circuit I.
  • a liquefaction chamber 1, which serves the liquefaction of VIV bales, is connected at its lower end via the stub line 16, in which a Venturi nozzle 6 is arranged, and via a shut-off and metering valve 5 to the main line 14.
  • a secondary line 15 branches off below the liquefaction chamber 1 from the branch line 16 and leads over a further pump 4, which is also a rotary piston pump in this embodiment, back into the liquefaction chamber 1 above a melting grate 3, which is arranged in the liquefaction chamber 1.
  • the sub-line 15 forms together with the branch line 16 the secondary circuit II (bordered with a dashed line).
  • the arrows on main line 14, sub-line 15 and stub line 16, horizontal and vertical, indicate the flow direction of the fluids in main circuit I and secondary circuit II. All pipe sections and the boiler 7 are thermally insulated.
  • the liquefaction of VIV bales in the liquefaction chamber 1 takes place by heating on a melting grid 3.
  • the melting grid 3 has a grid support with a triangular cross-section and serves for inhomogeneous temperature field generation, whereby the concentrate m 1 is heated to an average temperature T m1 during the conditioning phase.
  • the melt grid 3, with the VIV bales applied is constantly flushed with the introduced base oil.
  • the pump 4 provides for a circulation of the liquid components in the liquefaction of the concentrate m 1 in the secondary circuit II.
  • the first protective gas supply 8a of the liquefaction chamber 1 takes place via an inert gas pressure container 81, a protective gas line 821 and a protective gas line 823, a metering valve 822, the three-way valve 23 and the connection to the liquefaction chamber 1.
  • the second protective gas supply 8b of the boiler 7 takes place via the protective gas pressure container 81, a Inert gas line 831 and a protective gas line 833, a metering valve 832, the three-way valve 25 and the connection to the boiler 7.
  • the arrows, horizontal and vertical, indicate the flow direction of the protective gas in the suction and filling mode.
  • the liquefaction chamber 1 is thus connected to the shielding gas pressure vessel 81 via the suction device 2a and the protective gas supply 8a and the boiler 7 via the suction device 2b and protective gas supply 8b.
  • the suction devices 2a, 2b and the protective gas supplies 8a, 8b are used in addition to the protective gas purging and protective gas filling the gas space of the liquefaction chamber 1 and the boiler 7 and the setting of a suitable, defined overpressure, the overpressure in the liquefaction chamber 1 is designated by p m1 and the overpressure in the boiler 7 with p 2 .
  • the shut-off and metering valve 5 of the secondary circuit II remains closed during filling and during the conditioning phase and is only opened during the mixing process between the concentrate m 1 and the base oil in such a way that the partial flow of the concentrate m 1 from the secondary circuit II to the main flow of the base oil from the main circuit I at most stoichiometrically, according to the target mixture m 2 , is set.
  • a veturizing nozzle 6 is arranged near the connection point to the main line 14.
  • Veturidüse 6 is for mixing the concentrate m 1 from the secondary circuit II in the base oil, which flows through the main circuit I, at the point of Meeting the stitch line 16 with the main line 14 of the partial flow of the secondary circuit II sucked into the partial flow of the main circuit I.
  • a Einschraubdistributing Moment 9 is arranged for heating the base oil to an average temperature T 2 of 60 ° C to 90 ° C during the conditioning phase.
  • a sight glass In the branch line 16, between the liquefaction chamber 1 and the branch to the sub-line 15 is a sight glass and in the liquefaction chamber 1 itself, a sight glass is also arranged. Both sight glasses are used to control the Schlieren freedom of the concentrate m 1 and the control of mass transport from the liquefaction chamber. 1
  • FIG. 3 shows the inventive device for incorporation of viscosity index improvers in suitable base oils in another embodiment.
  • the dip tube 12 is replaced by a mixing nozzle 13.
  • the flowing from the main line 14 via the mixing nozzle 13 in the boiler 7 liquid simultaneously sucks through lateral openings of the mixing nozzle 13, according to the ejector principle, liquid from the boiler 7 in the mixing nozzle 13 and mixes both liquid streams in the mixing nozzle 13th to a liquid free jet, which emerges from the mixing nozzle 13 below the liquid level in the boiler 7.
  • the liquefaction chamber 1 shut off from the main circuit I becomes at least 70 wt% viscosity index improver and at most 30 wt% base oil with a suitable mass of base oil and a suitable number of 25 kg bales of the viscosity index improver according to the composition of the desired concentrate ml (macromolecular copolymers) under atmospheric conditions and laboratory temperature equipped and sealed.
  • a rough vacuum is generated in the gas space of the liquefaction chamber 1 via the suction device 2a.
  • the gas space of the liquefaction chamber 1 is filled with inert gas via the protective gas supply 8a. This process of inert gas purging is repeated several times.
  • the overpressure p m1 in the liquefaction chamber 1 can be between 100 mbar and 50 bar.
  • the overpressure p m1 is preferably less than 24 bar, in which case it is less than 10 bar in the specific case.
  • the conditioning phase more and more liquefied constituents dissolve out of the VIV bales until the batch is present as concentrate m 1 at a temperature T m1 above the solubility temperature (for example about 100 ° C. or 337 K at 9 bar overpressure).
  • T m1 above the solubility temperature (for example about 100 ° C. or 337 K at 9 bar overpressure).
  • the built-in sight glasses made of borosilicate glass are provided.
  • a mass of base oil suitable for the target mixture m 2 at room temperature is filled into the vessel 7.
  • a coarse vacuum is also generated several times alternately by means of the suction device 2b and then filled with inert gas via the protective gas supply 8b.
  • the gas space of the boiler 7 is filled with protective gas up to an overpressure p 2 of p 2 ⁇ p m1 .
  • the base oil is pumped by the pump 10 through the main circuit I and temperature controlled by a heater 9 to the temperature T 2 (of approx. 90 ° C or 363 K).
  • the base oil from the boiler 7 passes through the static mixer 11 introduced at regular intervals in the main line 14 of the main circuit I and finally reaches the boiler 7 via the dip tube 12.
  • the protective gas While in the liquefaction chamber 1 of the secondary circuit II, the protective gas is used with an overpressure p m1 , takes place in the boiler 7 of the main circuit II, the application of the inert gas with a lower pressure p 2 .
  • the static pressure difference p m1 - p 2 is essentially distributed as a fluid-mechanical energy loss via the static mixer 11 mounted in the main circuit I at regular intervals.
  • the static mixers 11 mounted in the main line 14 ensure a shallow mixing of the fluid flow by generating swirl and transverse components in the velocity field. Shear-induced aging processes are avoided.
  • both mixing partners concentrate m 1 in the liquefaction chamber 1 of the secondary circuit II and base oil in the boiler 7 of the main circuit I
  • the shut-off and metering valve 5 of the liquefaction chamber 1 is opened, so that the partial flow of the concentrate is brought together in a suitable manner with the main flow of the base oil via the Venturi nozzle 6.
  • the pressure p m1 in the liquefaction chamber 1, the pressure p 2 ( p m1 > p 2 ) in the boiler 7 and the delivery pressure p P of the pump 10 in the main circuit I, before the confluence of the partial flows, are selected such that, on the one hand Outflow of the concentrate m 1 is ensured from the liquefaction chamber 1, and on the other hand, the pressure difference p m1 - p 2 is realized via the pressure drop of the total flow at a mixing temperature T m via the static mixer 11.
  • the volume flows V ⁇ 2 , V ⁇ m are to be measured before and after the confluence.
  • the system is carefully returned to normal pressure, but without Oxygen supply. Due to the significantly lower viscosity of the target mixture m 2 at the mixture temperature T m over the concentrate, the degassing of the additional inert gas succeeds within a very short time.
  • a rough vacuum can optionally be applied (eg p 2 ⁇ - 0.5 bar).
  • the suction device 2b can be used.
  • the mixing operations are carried out at a temperature (about 100 ° C) at which a further processing of the mixtures can follow immediately, without having to dissipate excess heat energy.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Claims (14)

  1. Procédé d'introduction avec mélange d'agents d'amélioration d'indice de viscosité (VIV) dans des huiles de base dans un dispositif de mélange d'agents d'amélioration d'indice de viscosité dans des huiles de base, le procédé comprenant les étapes suivantes :
    a) remplir une chaudière (7) avec de l'huile de base et balayer plusieurs fois, avec un gaz de protection, un espace de gaz de la chaudière (7) avec alternance d'une génération d'un vide grossier au moyen d'un dispositif d'aspiration (2b) et d'un remplissage de l'espace de gaz avec un gaz de protection au moyen d'une alimentation en gaz de protection (8b) ;
    b) remplir une chambre de liquéfaction (1), fermée par un circuit principal (I), avec une quantité définie d'un agent d'amélioration d'indice de viscosité et une quantité définie d'huile de base correspondant à la composition d'un concentré souhaité (m1) dans des conditions atmosphériques et à la température du laboratoire ;
    c) balayer plusieurs fois, avec un gaz de protection, à partir d'un espace de gaz de la chambre de liquéfaction (1) avec alternance d'une génération d'un vide grossier au moyen d'un dispositif d'aspiration (2a) et d'un remplissage de l'espace de gaz avec du gaz de protection au moyen d'une alimentation en gaz de protection (8a) ;
    d) remplir ensuite l'espace de gaz de la chambre de liquéfaction (1) avec du gaz de protection jusqu'à une surpression définie (pm1) ;
    e) liquéfier l'agent d'amélioration d'indice de viscosité dans la chambre de liquéfaction (1) et inonder simultanément avec de l'huile de base, introduite dans la chambre de liquéfaction (1), dans une circulation continue de l'huile de base par le biais d'un circuit secondaire (II) par introduction de chaleur à une température (Tm1) au-dessus d'une température de solubilité jusqu'à ce que le concentré souhaité (m1) soit atteint ;
    f) introduire avec mélange le concentré (m1) dans l'huile de base de la chaudière (7) par le biais du circuit principal (I) jusqu'à atteindre le mélange cible (m2),
    g) ramener le dispositif à la pression normale sans apport d'oxygène ni dégazage du mélange cible (m2) dans la chaudière (7) par application d'un vide grossier approprié.
  2. Procédé selon la revendication 1, caractérisé en ce que le concentré dissous (m1) comprend au moins 70 % en poids d'agent d'amélioration d'indice de viscosité et au plus 30 % en poids d'huile de base.
  3. Procédé selon la revendication 1, caractérisé en ce que de l'azote, du butane ou du dioxyde de carbone est utilisé comme gaz de protection.
  4. Procédé selon la revendication 1, caractérisé en ce que la température (Tm1) du concentré dans la chambre de liquéfaction (1) est inférieure à 120 °C et en ce que la surpression (pm1) dans la chambre de liquéfaction (1) est comprise entre 100 mbar et 50 bars, de préférence est inférieure à 24 bars, encore plus préférablement inférieure à 10 bars, en ce que la température (Tm2) du mélange cible dans la chaudière (7) est inférieure à 100 °C et en ce que la surpression (p2) dans la chaudière (7) est p2 <= pm1/2.
  5. Dispositif destiné à mettre en oeuvre le procédé selon les revendications 1 à 4 et à introduire avec mélange des agents d'amélioration de l'indice de viscosité dans des huiles de base, le dispositif comprenant une chaudière (7) destinée à une huile de base et une chambre de liquéfaction (1) destinée à un agent d'amélioration d'indice de viscosité pour produire un mélange cible (m2), caractérisé en ce que un circuit principal (I) et un circuit secondaire (II) sont prévus pour conditionner séparément des agents participant au mélange cible (m2) .
  6. Dispositif selon la revendication 5, caractérisé en ce que le circuit principal (I) est relié à la chaudière (7) par une conduite principale (14) dans laquelle au moins une pompe (10), au moins un élément chauffant (9) et plusieurs mélangeurs statiques (11) sont disposés, en ce que la chambre de liquéfaction (1) est reliée par le biais d'une conduite d'embranchement (16) au circuit principal (I) et par le biais d'une ligne secondaire (15) au circuit secondaire (II) qui retourne par le biais d'une pompe (4) dans la chambre de liquéfaction (1), et en ce qu'un premier dispositif d'aspiration (2a) est relié à la chambre de liquéfaction (1) et un deuxième dispositif d'aspiration (2b) est relié à la chaudière (7), les dispositifs d'aspiration (2a, 2b) fonctionnant par le biais d'une pompe à vide commune (21), et en ce qu'une première alimentation en gaz de protection (8a) est reliée à la chambre de liquéfaction (1) et une deuxième alimentation en gaz de protection (8b) est reliée à la chaudière (7), les alimentations en gaz de protection (8a, 8b) étant reliées à un réservoir de gaz de protection sous pression commun (81).
  7. Dispositif selon la revendication 6, caractérisé en ce que le premier dispositif d'aspiration (2a) de la chambre de liquéfaction (1) est défini par la pompe à vide (21), une conduite d'aspiration (22), un robinet à trois voies (23) et une liaison à la chambre de liquéfaction (1) et le deuxième dispositif d'aspiration (2b) de la chaudière (7) est défini par la pompe à vide (21), une conduite d'aspiration (24), un robinet à trois voies (25) et une liaison à la chaudière (7).
  8. Dispositif selon la revendication 6, caractérisé en ce que la première alimentation en gaz de protection (8a) de la chambre de liquéfaction (1) est effectuée par le biais du réservoir de gaz de protection sous pression (81), d'une conduite de gaz de protection (821) et d'une conduite de gaz de protection (823), d'une vanne de dosage (822), d'un robinet à trois voies (23) et d'une liaison à la chambre de liquéfaction (1) et la deuxième alimentation en gaz de protection (8b) de la chaudière (7) est effectuée par le biais du réservoir à gaz de protection (81), d'une conduite de gaz de protection (831) et d'une conduite de gaz de protection (833), d'une vanne de dosage (832), d'un robinet à trois voies (25) et d'une liaison à la chaudière (7).
  9. Dispositif selon l'une des revendications précédentes 6 à 8, caractérisé en ce que les pompes (4 ; 10) sont des pompes à piston rotatif à faible cisaillement.
  10. Dispositif selon l'une des revendications précédentes 6 à 8, caractérisé en ce que l'élément chauffant (9) est un corps chauffant vissé.
  11. Dispositif selon l'une des revendications précédentes 6 à 8, caractérisé en ce que la conduite principale (14) se termine dans la chaudière (7) par un tube plongeur (12) à embout pouvant tourner librement ou par une buse mélangeuse (13).
  12. Dispositif selon l'une des revendications précédentes 6 à 8, caractérisé en ce que la conduite d'embranchement (16) débouche dans la conduite principale (14) au-dessous de la chambre de liquéfaction (1) et en ce qu'une buse à effet Venturi (6) est disposée dans la conduite d'embranchement (16) près du point de liaison à la conduite principale (14).
  13. Dispositif selon l'une des revendications précédentes 6 à 12, caractérisé en ce qu'une grille de fusion (3) est disposée dans la chambre de liquéfaction (1) et la conduite secondaire (15) débouche dans la chambre de liquéfaction (1) au-dessus de ladite grille de fusion.
  14. Dispositif selon l'une des revendications précédentes 6 à 13, caractérisé en ce que la conduite principale (14), la conduite secondaire (15) et la conduite d'embranchement (16) et la chaudière (7) sont isolés thermiquement.
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CN112342074B (zh) * 2020-12-21 2022-06-28 山东恒利热载体工程技术有限公司 一种再生基础油润滑油抗光热稳定剂的生产工艺
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DE2309039B2 (de) * 1973-02-23 1974-12-19 Chemische Werke Huels Ag, 4370 Marl Verfahren zur Herstellung von homogenen Polyolefinkautschuk-Öl-Mischun-
DE2932459C2 (de) 1979-08-10 1985-10-31 Mobil Oil Ag In Deutschland, 2000 Hamburg Vorrichtung zum Lösen eines granulatförmigen Feststoffes in einer Flüssigkeit
US4464493A (en) * 1982-09-13 1984-08-07 Copolymer Rubber & Chemical Corp. Process for dissolving EPM and EPDM polymers in oil
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