ES2303447B1 - REGENERATION PROCEDURE OF USED MINERAL OILS AND ASPHALTIC WASTE FOR LIQUID / LIQUID EXTRACTION AND PRODUCT AS OBTAINED. - Google Patents

Abstract

Oil Regeneration Procedure used minerals and asphaltic waste by extraction liquid / liquid and product thus obtained.

Oil Regeneration Procedure used minerals and asphaltic waste by extraction liquid / liquid, by which mineral used oils are regenerated in order to obtain four lubricant bases with the same physicochemical characteristics than those of the first refining starting of used oil and one of the asphalt wastes from the Distillation of oil in difficult regeneration plants application in the market.

The procedure includes, dehydration and distillation for the elimination of water and hydrocarbons light liquid / liquid extraction with solvent (methyl ethyl ketone) at room temperature, atmospheric pressure and solvent recovery for later reuse as well such as vacuum distillation to obtain 4 lubricant bases and last and not least because of the above the solvent extraction of asphalt products obtained to obtain a heavier lubricant base minimizing the amount of them.

Description

Oil Regeneration Procedure used minerals and asphaltic waste by extraction liquid / liquid and product thus obtained.

Object of the invention

The object of the present invention patent is present a new oil regeneration procedure used minerals and asphaltic waste by extraction liquid / liquid and product thus obtained by it.

Mineral used oils are regenerated with the in order to obtain four lubricant bases with the same physicochemical characteristics than those of the first refining starting of used oil and one of the asphalt waste.

It is also the object of the invention to obtain of high base yields without producing solid waste or atmospheric emissions

Another object of the invention is regeneration. of asphalt waste from oil distillation of difficult application in the market.

The mineral oils used in the industry contain various antioxidant additives, detergents and viscosity index improvers, these additives leave deteriorating with use until the oil is not suitable for role you have to play by becoming a waste highly polluting

Background of the invention

So far there are a number of Regeneration procedures for oils and their products obtained, however, present a series of problems regarding to the process of regeneration of used mineral oils and asphaltic waste by liquid / liquid extraction and product as well obtained, object of the present invention patent. So by example we have to:

The invention patent WO 9407798 describes a typical distillation procedure that employs high temperatures in vacuum distillation and get bases with color and smell that they differ markedly from the characteristics of the first refining and contain oxygenated products.

Therefore you have to resort to a final treatment of bleaching earth with the consequent solid waste that is generated and treatment by acids that entails its subsequent neutralization with the consequent cost, reaction violent chemistry and generation of a residue hardly from manage.

As an alternative to the separation of additives by distillation, chemical demetalization has been used by reacting the metal additives of the used oil with reagents that form metal salts.

In US Patent No. US 4247389, treat used oil with ammonium phosphate solutions to temperatures of 320-420 ° C.

However, the demetalization treatment to these temperatures and the subsequent distillation of the oil Demetalized also produce smell and color, and generate products little stable, which forces to treat the bases obtained by hydrogenation or by adsorbents, with the drawbacks of these final refining processes, in addition, of the need for elimination of the additives used before distillation with the consequent energy cost.

In German patent DE 3433336 describes the treatment with alkaline hydroxides of used oils before proceed to separate additives and asphalts by distillation.

US Patents 4834868 and WO 9826031 use the alkaline treatment of the lubricant fractions obtained after separating additives and asphalts by distillation.

Patent PCT / ES02 / 00359 describes a solvent extraction and distillation procedure, thus obtaining lubricant bases that do not require final refining treatments by acid / earth or hydrogenation.

However, no background was found. of procedures that use solvent treatments mentioned and that the recovery of used mineral oil agrees with the recovery of asphalt waste in the same process.

The present invention consists of a oil lubrication base recovery procedure mineral used by solvent extraction, distillation and recovery of asphalt waste obtained under conditions such that the lubricant bases are obtained with the same characteristics than the initials from the first refining.

At no time is it reflected in the state of the technique a mineral oil regeneration procedure used and asphalt waste by liquid / liquid extraction we can recover both used mineral oil and eat asphalts from regeneration plants.

In summary, it can be seen that the use of Solvents are described in various patent documents. In the most cases are cited as a reason to substantiate these investigations the benefits it reports for the recovery of the lubricant bases but in no case for the recovery of the resulting asphalt wastes and therefore the yield of process is much superior in the case described and the generation of Waste is minimal when recovering the asphalt component. The proposed solutions vary widely, being none of the marked fully satisfactory for oil regeneration used minerals and not contemplating any of them recovery of the asphalt waste obtained (highly polluting).

Finally indicate that at present, and as described above, there is a lot of Regeneration procedures for used mineral oils, but none of them presents the particularity of the recovery back of the asphalt component for the extraction of a new lubricant base in order to minimize waste and make even more profitable if the described process fits.

In sum, in the regeneration procedure of used mineral oils and asphaltic waste by extraction liquid / liquid object of the present invention is conjugated the recovery by regeneration of used mineral oil and the asphalt recovery of regeneration plants including its own to obtain another lubricant base heavy, characteristics that are not reflected in the current state of the  technique. However, it is unknown the existence of a Regeneration procedure of used mineral oils and asphaltic waste by liquid / liquid extraction as described in the present specification.

Description of the invention

To alleviate or, where appropriate, eliminate all problems mentioned above, this new procedure is presented of regeneration of used mineral oils and asphalt waste by liquid / liquid extraction and product thus obtained, object of The present invention patent:

For this a composite procedure is presented by different stages well differentiated.

1st stage Dehydration for the elimination of water in the presence of a caustic in order to neutralize the acidity of the oil. This stage includes the distillation of the oil for the elimination of lighter compounds (gasoline, naphtha, solvents).

2nd stage Liquid / liquid extraction with solvent (methyl ethyl ketone) at room temperature and pressure Atmospheric and solvent recovery for later reuse

3rd stage Vacuum distillation to obtain of 4 lubricant bases.

4th stage Solvent extraction of asphalt products obtained to obtain a base heavier lubricant minimizing the amount thereof.

With this new procedure management is avoided of most of the highly asphaltic component pollutant.

No high pressures and temperatures are necessary for the development of the process, raising the security of the installation and process performance thanks to recovery in the last phase of the asphalt component.

It is possible to reduce this component and even recover from other regeneration plants.

Description of the drawings

To complement the description that is being performing, and in order to help a better understanding of the characteristics of the invention, is accompanied herein descriptive, as an integral part of it, a series of figures in which, for illustrative and non-limiting purposes, has represented the following:

- Figure 1: Procedure flow chart of regeneration of used mineral oils and asphalt waste by liquid / liquid extraction and product thus obtained.

Preferred Embodiment of the Invention

As can be seen in the attached figure, the Regeneration procedure of used mineral oils and asphaltic waste by liquid / liquid extraction, and product as well obtained is composed of the following stages:

A first stage of dehydration is performed for the elimination of water in the presence of a caustic with the in order to neutralize the acidity of the oil. This stage includes the oil distillation for the removal of the most compounds Light (gasoline, gasoline, solvents).

The oil enters the line (A), is sent to the reactor with stirring (1), before reaching it, and along the line (B) 3% caustic is added to neutralize the acidity of the oil.

The oil-caustic mixture is send to the heat exchanger (2), where the temperature rises up to 130 ° C. In this changer the heat is supplied by thermal oil at 240 ° C.

The mixture at this temperature is sent to the vacuum distillation column (3), where water and water evaporate light hydrocarbons

The vacuum distillation column (3) works at Absolute 200 mm of Hg, pressure achieved by the equipment Dry system vacuum to prevent water generation residual.

Dehydrated and hydrocarbon-free oil light is extracted from the bottom of the vacuum distillation column (3) and is sent to the next stage before going through the cooler (4), where the temperature is lowered to 40 ° C.

Water and hydrocarbons come out top of the vacuum distillation column (3) towards the condenser (6), where it condenses and is sent to the separator water / light (7), and from there along lines (C) and (D) each at corresponding storage tank.

In the second stage the extraction takes place liquid / liquid with solvent (methyl ethyl ketone) at temperature ambient and atmospheric pressure and solvent recovery for its subsequent reuse.

Dehydrated oil from the first stage is introduced into the intermediate storage tank (5) and from there to the reactor with stirring (8).

In the same entry line you enter methyl ethyl ketone from the tank (9) in a 4: 1 ratio in said reactor and for the residence time, the stirrer mixes intimately the oil with the solvent starting the extraction.

The oil solvent mixture is sent to the decanter (10). In this decanter two phases are formed: bottom containing solvent and waste from deterioration of oil additives and the solvent-containing top, lubricating bases and asphalt compounds.

The lower phase is sent to the exchanger (16), where the temperature rises to 100 ° C and from there to the solvent recovery column (11).

The upper phase is sent to the exchanger (20), where the temperature rises to 100 ° C and from there to the solvent recovery column (12).

Through the third stage of vacuum distillation it is possible to obtain 4 lubricant bases.

From the solvent recovery column (12) and the result of the extraction is extracted from the bottom Free of solvent, it is sent to the exchanger (17) to raise it the temperature at 320 ° C and from this to the distillation column at empty (13).

The vacuum distillation column (13) works at 6 mm Hg and has four distillation cuts in each of the which condense the different fractions of lubricant bases (J, K, L, M) and from there they are sent to their respective tanks storage.

In the fourth stage the extraction is carried out with solvent of the asphalt products obtained for obtaining a heavier lubricant base minimizing the amount of same.

Asphalt at the bottom of the column is removed, joins in line the bottom residue of the recovery column of solvent (11), solvent 5: 1 is injected through point (P) and send to asphalt decanter (14).

It is extracted from this decanter by the part top a new heavier lubricant base, heats up in the exchanger (19) and is sent to the recovery column of solvent (21), from which the top part is removed solvent, condenses on the condenser (18) and recovers the tank (9), for later reuse. On the bottom is remove the lubricant base (Y).

It is extracted from this decanter by point (O) a Asphaltic residue with solvent, heated in the exchanger (15) and sent to the solvent recovery column (22), the solvent is removed from this column from the top, it condenses on the condenser (18), and recovers the tank (9) to its reuse The residue is extracted from the bottom asphalt (Z).

The solvent of the different columns comes out on top of them, they condense on the condenser (18) and return to the storage tank for reuse

Once nature is sufficiently described of the present invention, as well as a way of bringing it to the practice, it only remains to be added that said invention can suffer certain variations in form and materials, as long as these alterations do not substantially vary the characteristics which are claimed below.

Claims (2)

1. Procedure for the regeneration of used mineral oils and asphalt waste by liquid / liquid extraction, characterized by being composed of several distinct stages. First, a first stage of dehydration is carried out for the removal of water in the presence of a caustic in order to neutralize the acidity of the oil; This stage includes the distillation of the oil for the removal of the lighter compounds (gasoline, naphtha, solvents); the oil enters through the line (A), is sent to the reactor with stirring (1), before reaching it, and 3% of caustic is added to the line (B) to neutralize the acidity of the oil; The caustic oil mixture is sent to the heat exchanger (2), where the temperature is raised to 130 ° C, in this exchanger the heat is supplied by thermal oil at 240 ° C; the mixture at this temperature is sent to the vacuum distillation column (3), where water and light hydrocarbons evaporate; the vacuum distillation column (3) works at 200 mm of absolute Hg, pressure that is achieved by the dry system vacuum equipment to avoid the generation of residual water; Dehydrated and light hydrocarbon-free oil is extracted from the bottom of the vacuum distillation column (3) and sent to the next stage before passing through the cooler (4), where the temperature is lowered to 40 ° C; water and hydrocarbons leave the top of the vacuum distillation column (3) to the condenser (6), where it condenses and is sent to the water / light separator (7), and from there through the lines (C ) and (D) each to its corresponding storage tank; in the second stage the liquid / liquid extraction with solvent (methyl ethyl ketone) occurs at room temperature and atmospheric pressure and solvent recovery for later reuse; dehydrated oil from the first stage is introduced into the intermediate storage tank (5) and from there to the reactor with stirring (8); in the same inlet line, methyl ethyl ketone from the tank (9) is introduced in a ratio of 4: 1 into said reactor and by the residence time, the agitator intimately mixes the oil with the solvent starting the extraction; The oil solvent mixture is sent to the decanter (10). In this decantation two phases are formed: the lower one containing solvent and the residues of deterioration of the oil additives and the upper one containing solvent, the lubricant bases and asphaltic compounds; the lower phase is sent to the exchanger (16), where the temperature is raised to 100 ° C and from there to the solvent recovery column (11); the upper phase is sent to the exchanger (20), where the temperature is raised to 100 ° C and from there to the solvent recovery column (12); by means of the third stage of vacuum distillation it is possible to obtain 4 lubricant bases; from the solvent recovery column (12) and the result of the solvent-free extraction is extracted from the bottom, sent to the exchanger (17) to raise the temperature to 320 ° C and from this to the vacuum distillation column ( 13); The vacuum distillation column (13) works at 6 mm Hg and has four distillation cuts in each of which the different fractions of lubricating bases (J, K, L, M) are condensed and from there they are sent to their respective storage tanks; in the fourth stage the solvent extraction of the asphalt products obtained is obtained to obtain a heavier lubricant base minimizing the amount thereof; Asphalt from the bottom of the column is removed, it is connected in line to the residue at the bottom of the solvent recovery column (11), 5: 1 solvent is injected through point (P) and sent to the asphalt decanter ( 14); a heavier new lubricant base is removed from the top of this decanter, heated in the exchanger (19) and sent to the solvent recovery column (21), from which the solvent is removed from the top, It condenses on the condenser (18) and recovers the tank (9), for later reuse. The lubricant base (Y) is removed from the bottom; an asphaltic residue with solvent is removed from this decanter at point (0), heated in the exchanger (15) and sent to the solvent recovery column (22), from this column the solvent is removed from the top , condenses on the condenser (18), and recovers the tank (9) for reuse. Asphalt residue (Z) is extracted from the bottom; The solvent of the different columns comes out from the top of them, they condense in the condenser (18) and return to the storage tank for reuse. 2. Method of regeneration of used mineral oils and asphalt waste by liquid / liquid extraction, according to claim one characterized in that different fractions of lubricating bases (J, K, L, M) are obtained.