BG100012A - Method and device for regeneration of lubricating oils - Google Patents

Abstract

Process and plant for the regeneration of spent oils comprising: a tank (2) for the storage of spent oils; preheating means (3) for the preheating of spent oils; means (4) for the storage of a strong base; means (5) for mixing the strong base in a predetermined proportion with the spent oils; waste elimination means (10, 14).

Description

METHOD AND DEVICE FOR REGENERATION OF S.-.

OuiaCT OF TECHNIQUE

The invention relates to a method and device for the recovery of waste lubricating oils.

Lubricants generally undergo modifications and changes in their use, which often involves more or less replacement.

The removal or regeneration of these waste oils has so far been a source of significant pollution.

After use, these oils contain mainly solid wastes, impurities, combustion wastes, etc.

BACKGROUND OF THE INVENTION

Different recovery methods have been developed to date. Damaged oils are initially recovered and those different parent oils are sometimes mixed more or less with foreign products capable of disrupting regeneration methods.

So far, the most commonly used methods consist of the stage of treatment of waste and recovered oils by sulfuric acid, then their neutralization with lime and sodium carbonate, followed by discoloration with activated soil and filtration.

The apparatus and method described in document / 1 / are known. This device contains two tanks, allowing two • boots, one with soda and the other with clay and two centrifuges providing separation, one of water and the other of the spent clay of the oaraotva oil.

This type of method allows the recovery of chaot from the waste oils but releases non-recoverable wastes with highly polluting effects.

The recovery rate of industrial devices implementing these methods does not exceed $ 85 and their cost is high.

Other recovery methods are also known based on the hydrotreatment of the oil after heat treatment and its vacuum distillation. The hydrogenation of the oil is carried out with hydrodesulfurizing and hydrodesizing catalysts.

During the implementation of these methods, the catalysts are progressively depleted and finally highly contaminated non-usable products are obtained.

However, these methods are even more expensive.

Also known is the method described in document / 2 /. In this method for the recovery of waste oils, the first phase of dehydration and removal of chlorinated hydrocarbons is carried out at a temperature interval between 100 ° and <, 00 °. closed system at 300 ° C by mixing baking soda and potash. Thermal vacuum distillation is followed, reaching a temperature of 480 ° C.

SUMMARY OF THE INVENTION

The pellet of the present invention is the development of a method for the regeneration of low-contaminated or non-contaminated waste lubricating oils, which can be realized under good economic conditions.

It is also an object of the present invention to propose that a * _- * * * * · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · A method for the recovery of waste oils, allowing a high percentage of oil recovery.

To this end, the invention relates to a method for the regeneration of waste lubricating oils, which includes a strong base treatment step.

According to the invention, the method involves the following sequential processing steps:

a / an assessment of the concentration of fuel oil, fatty acid and chlorine and the removal of oils containing a very high percentage of one of these ingredients;

b / heating, wherein the regeneration oils are in the temperature range between 120 ° and 250 ° C;

c) adapting an aqueous solution on a strong basis with a ratio of 1 to 3% pure base to the weight of the lubricating oil;

d / dehydration and extraction of light hydrocarbons;

(e) extraction and gas recovery / stripping / e) extraction of impurities by fractional distillation under vacuum providing separation of lubricating oil on the one hand and a residue in which all impurities are concentrated on the other.

In the various preferred embodiments, the invention includes the following characteristics, taken in all their combinations:

- Homogeneous oils are homogenized before heating.

- During the preheat stage, regeneration oils are in the temperature range between 120 ° _and 250%. This temperature is preferably in the range between 140 ° C and 160 ° C.

- The strong base is in aqueous solution

..... 4.u * * ·· '·· *

- A strong base is added in the ratio of 1 to 3% by weight on a pure base.

The flash / flash step, performed after the addition of a strong base and before the impurity extraction, ensures the dehydration and extraction of light hydrocarbons from the treated mixture.

- The vacuum distillation column is connected to a purifier at the base of the column.

- The strong base is sodium or potassium hydroxide.

- The strong base is sodium hydroxide.

- The strong base is potassium hydroxide.

The invention also relates to a waste oil regeneration device enabling the above method to be carried out.

This device includes:

- a waste oil storage tank,

- equipment for mixing and homogenizing the oil initially stored in the tank,

- waste oil heating installations,

- strong storage facilities,

- equipment for mixing on a strong basis in a specific proportion to the waste oils,

- unit for extraction of water and light hydrocarbons by flash / flash /

- gas extraction unit / stripping /

- impurity extraction facilities including a vacuum distillation unit.

Preferably, the vacuum distillation unit is coupled to a column evaporator for purification.

• · _her. _..... · · · · · · ···· WQ *

INJURY FOR THE IMPLEMENTATION OF THE INVENTION

An embodiment of the invention will be described in more detail with respect to the only figure which is a schematic representation of the waste oil regeneration device of the invention.

The collected waste oils may have different origins, they may refer, for example, to motor oils, engine oils, hydraulic oils, turbine oils, and the like.

When these oils arrive at the regeneration unit, their suitability for treatment is checked.

In fact, the regeneration method according to the invention essentially addresses the removal of light constituents such as gasoline, gas oil and water, but does not allow the removal of heavy constituents such as oils themselves that have different physical properties. For example, the removal or treatment of fuel oil may only by the method of complete purification.

Excessive content of chlorine mixtures can provoke premature wear of the device.

Collected oils containing a very high percentage of fuel oil, fatty acids, or chlorine must be removed. In order to assess the concentration of these various ingredients, well-known tests used in this field are practiced.

Chlor Test can be cited between them, which allows the presence of chlorides to be captured. Copper wire immersed in waste oil is placed on a flame. A greenish flame indicates the presence of chlorides.

Drop Test allows you to catch the presence of fuel oil. A drop of oil is placed on the chromatographic paper. A concentric spot with a yellowish halo indicates the presence of fuel oil.

• · • »

Fast Test allows the capture of the presence of fatty acids in the oil. Heat 2 ml. waste oil in the presence of a soda tablet: when the oil thickens after cooling, it means that it has fatty acids.

The grouped waste oils 1, which have successfully passed these various tests, are assembled in tank 2.

They are mixed either inside the tank itself or during their extraction by classical means not shown in the figure.

Preheating facilities 3 contain

0 'the collected oils from tank 2 at a temperature between 120 and 250 b and preferably between 140 and 160 ° C.

The stored base in tank 4 is transferred and mixed through the facilities 5 with the heated waste oil.

Preferably, the amount of pure base added to the waste oils is in the range of 1 to 3 pounds by weight.

This percentage may be pre-specified depending on the quality of the waste oils and the nature of the base used.

The base used is a strong base preferably sodium or potassium hydroxide. It may also be contemplated to use a mixture of these bases.

Exhausted oils with a high temperature range, a strong base was added to power the unit 6 for extraction of water and light hydrocarbons by flash. In such an aggregate, the evaporation of the water is effected by gross expansion of the mixture into a balloon.

The water and light hydrocarbons are extracted and the remaining mixture is directed to unit 8 for gas oil extraction.

Stri »» π π stri · stri π π π π stri stri stri stri π stri stri stri stri stri stri stri stri / / / / stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri stri

1'azole 9 is withdrawn and the remaining mixture is directed to a distillation column 10 allowing fractionation of the mixture of basic lubricating oils and separation of the residue where all impurities are concentrated.

Base oils can be divided into different levels according to the number of parts sought.

Further results were obtained by dividing, on the one hand, a base oil of 1b0 Neutral 11 and a base oil of 400 to 500 Neutral 12.

The distillation column 10 under vacuum is a traditional vacuum column which allows the dissociation and extraction of residues that are directed to a storage bubble 14.

The waste 15 is disposed of and is suitable for use as, for example, tar or bitumen for road construction. They can also be used as fuel.

The vacuum distillation column 10 is preferably connected to a purification evaporator at the base of the column 13, which allows it to improve its operation. A portion of the energy required to raise the temperature of the exhaust oils prior to adapting to the pure base preferably originates from the energy recovered on the base oils 11,12 at the outlet of column 10.

The spent oils are conveniently filtered during their recovery and at the outlet of the storage tank 2 in such a way as to remove the solids that they contain.

Various pumps that are not presented provide circulation of the mixture and extracts through the device described.

The method and apparatus of the invention allow the use of waste oils to produce oils of various qualities, usable waste, water, light hydrocarbons and gas oil.

All the products obtained are recoverable, so this method avoids pollution risks in principle.

This method allows a recovery rate of at least 90% to be obtained. This percentage is based on the mass of recovered oils by this industrial method with regard to laboratory recovered oils under optimum conditions, regardless of any economic considerations.

In an alternative embodiment, the disposal of the waste is carried out by means of a centrifugal device.

The two ways of removing the waste distillation column and centrifugation can be combined.

However, the preferred way of realizing the invention is to use a vacuum-distillation column with a evaporator for purification at the base of the column. Thus, it is possible to obtain a percentage of recovery with superior basic lubricating oil, to reduce the cost of investment and operation in terms of Other known methods of regeneration produce recovered oils with the same capabilities as new oils and remove almost all metals from them.

Moreover, all impurities are contained in the residues, · '«. ♦ ·· r, · ****** Μ - ·· ·· ····· which, as already stated, are easily appreciable.

The device of the invention can be put into operation easily under the most reliable conditions.

The following numbered example illustrates the implementation of the invention.

The result of the vacuum distillation of waste oils in a laboratory shall be indicated in (a), giving the ingredients and their precise characteristics.

The result of the distillation by a previous method, oe addition of a base, is presented in (b). This method, according to previous development, must be followed by chemical treatment to be completed by the traditional acid and clay method, the disadvantages of which are indicated above. of this treatment are presented in taolica in /.

E / is an oil regeneration according to an iso-industrial method.

In these tables the products are recovered ingredients.

Rdt represents their yield (the ratio by mass of the recovered amount to the starting amount of waste oil regenerated).

T.A.N. represents their acidity (content in acid number).

vis 40 ° C represents their viscosity at 40 ° C expressed in centistocks.

color is expressed in terms of the colors of standardized standards.When the numerical value is insignificant the color and appearance are better and is an indication of quality.

Ba is barium, Ca - calcium, Pb - lead, Zn zinc, P - phosphorus, Mn - chromium, Re - iron and si - silicon.

The comparison of table c / c table d / shows the high quality of the basic oil fractions obtained according to the invention. It is especially important that the metal content of the recovered oils is too low and the yield is more significant. Moreover, the complex of oil parts is easily recoverable.

The engine samples of reclaimed oils according to the invention have shown their equivalence to new oils. They are more capable than those recovered by known methods.

The indicative indications included after the technical features set forth in the claims are solely for the purpose of facilitating the understanding of the latter and in no way limit their scope.

• · · · t «r

hours ί-ι μ X υ υ CQ ο ο X X η- s Η X oh 4 Xia S S X Η = Μ

Η ος

Μ X ιη

Λ I I I I

X rfr ες X i ο n et Ρ. ΙΟ ΙΟ et «

Ct υ «5 2

X X ο ο

Я ct I Η ο ct X

X X χ Λ X

X Η υ ο

XI

<Γ C— < X Η X X Ρ [>. LO ο (Λ CD Ο ΟΟ ω · * * * and '- / X X CX)

Η In Q

X X

X X

X ο

X X χ

<

χ Π

X <

ct

X Η

X >>

XI ο X

X ο X

Μ ε

τ — i ι_η CD Ο • 4 Λ Midrange Ο ο

ο ι_η ο Ο CD ο ο ιΡ ΓΌ what IO LQ Λ Λ · \ · * • V λ Yu Yu CD ΟΟ Γ — 1 Midrange p- ! -4

X SP

C υ Ct Η and et X X O X ε; in r ° + X ο Ct H VO Λ Ct Ct et >> Γ> « K b Hrs X Ct CD CD CD o Ct X IX H Oh X cn

Distillation rate: 66.45 ct * Η ο ω ct α. yo ο

Sun.

- their holy self

I N ⁴

X O in X a NZ «h o a c o> 1O <u X B.

X

X a χ h <υ a x

o d o i

In ο X ο

And cn

X ο a self u: ίο to CO a σι self a

id χ υ 03 s ctj X a x

Ci <x> a x X o ΙΟ to ct3 a in o3

X

X

X

X dam χ x B υ <υ

XI to

• · • · • « • * • • · ► and • « • * • »« · · • • · » • · · · • · • • • • • · • 4 • · · · · t = I X in in in ί Yes υ and and Fr. Fr. Fr. X X X X me in in in 3 in in in > x X 2 2 2 X Yes X Yes X [yes> what Ό [Yes. OO X (Yes- hh Midrange Midrange X ΓΌ Midrange Fr. Yes Fr. ες LO magazine LO LD oo Midrange Yes LD 'd ^- * X L. * LQ XI • H ^- X 00 Fr. Ο Yu <P H '4 Fr. 2 LH LD LD Fr. Fr. · * · * Yes Fr. a LD Fr. Ο Oh (Ώ X hours 4 Yes n Yes Yes Oh (Yes- oo X -R LT) ff a t (L. ** * - · * Fr. Fr. X (Ό Fr. LD - & 'Ct OO LQ T-H Fr. Yes '- ¹ oh Oh- υ Fr. 4 Fr. (Yes- U Fr. Where T-H LH X e Midrange Yes X • H ^- T-H τ-4 sch ff X ff Yes 4 Yu Yes what * h · Yes ss and Fr. from X to ^. X X Fr. X Fr. Oh Fr. t-h me CO., LTD what ιΠ ff ff Yes Yes Where t-h Fr. CO., LTD (Ό Midrange IX from * « *> X t-h LO Fr. Well Fr. Fr. Fr. t-h sch X Yes > x X X SL hours Yes Yes Fr. ОЗ Thu. ff Yes * h- X < X SL Fr. LH (Yes. ff Yes f— \ CT> <3- σ> sch > x Yes f> \ o L. L. • S · * ** X X yes-> Yu sch ff Oh Fr. X a oo Os] sch Midrange LQ < t-h * 4 " sch Mr X ОЗ Yes Yes Yes 00 Yes 03 Yes in <υ Fr. 2 X / - \ and LF • « Ct in X 2 X and in X 0> α> Fr. in in υ magazine X X e X in υ X υ ОЗ X Yes-. X a (D υ Ct Yes ОЗ X <P X ОЗ a IN Ct X and Yes X X in Yes that S Fr. X X in Fr. ОЗ in + Yes a n Yu Ct Fr. in Yes in ОЗ X 05 NW in in '-' ОЗ Ct in Ct Fr. magazine ! 4 and in X ОЗ Yes a co in Yes ct <0 <υ and Fr. magazine in in <υ <ΰ Ct υ X Uh Yes E- Fr. CQ + and Fr. Yes Yes Oh

ο \ °

Distillation Randem: 62.35

X m ff Yu LT) ff X 0) 1D / —H I — 1 Oh Mr Si Mid] 04 E- X Oh, oh • hours • hours • hours m 0 $ Oh < - · Fr. Mr Fr. Fr. d ** U5 hours Yu Si d-h 'C' sch Mr 05 CU X N. e Fr. ОЗ • hours n St from · e Fr. I X your S <—Ch S your tx • X ОЗ X JV * t * n X X X F. / —H n X and '· - / n 03 Yu Art n and magazine j) X <and n υ your X h_ / X and 05 X e cx, ОЗ X , —H and 05 f n n ОЗ P * X <and H_> X t * H-i e ОЗ 3 * X e Fr. 3 · R. X n 05 your 3 f >> Fr. Yu 03 n + Yu X Fr. Mr Rücker your AZ XI X ОЗ o5 X ОЗ 05 X that that your ОЗ X <D Fr. magazine your X J. n e and >> 03 X m X K. Si your 05 that <and <and and Fr. ОЗ and your e <υ F. The dream Fr. G- * Fr. JV magazine ОЗ that X H ^ / n G-> + magazine Fr. and m

Randem regeneration rate: 55,21¾

Recovery rate: 83.09% (calculated on distillation in a laboratory without pre-treatment)

d) Oil regeneration in a production plant according to the invention

λ · · • • • · • · · « • · · · "· u-4 «* - • • · * » • · « ♦ »» * »· · « * » • · • * · · · · · * « • • • * • · η X PC -X X X and m « X " + + + 1 1 X 0 <l <3 \ o in in X ΓΌ Midrange r- RR X T— | 04 in in Midrange LT) cf. o « Λ * » 1 co LQ LQ x t-H Midrange CsJ 0? • 4 Λ £ o o t — 1 <D 4 • 'i xO vO and Fr. Fr. X LQ U1 Cf. o · * * 4 Oh a Oh a o N $ X X / Xj Xi n x + -> LO CD I ^- 1 magazine o 00 CD Fr. in Λ • · » 1 a '- / xO o Fr. that co Ό x LT) LO Lf) pq o 4 4 CD xO e 04 in o nC o X T-H Γ — i i — i cf. X M Xi N ND n U / —- s Fr. 00 x \ x X o x o MS r — t r — 4 « X B4 o Oh Oh o QO And B0 *> • 4 1 ς 00 LJ J. o o o o Midrange Midrange xO X 4 N 04 'X ς 05 t — 4 r — 1 r — 1 XT B4 XI x | 04 <o “Τη <ζ 2 Μ X X / —S CD Oh X X o \ => r- cd • = d- ND a < / * Λ * 05 0 <l Ox] Cxi oq x Lf) m Oh T-H X N V M that r — i rT 04 T “4 t-l X 4 o3 B CD s o3 B X n * CD in X <D CD X B CD co X Η in 03 X X r — 4 in ca. from · B CD X o5 6 B o 4 JT B And Yu and CD υ aS X o 03 B + > 4 CD CD o5 3 * B ο B <l in o3 05 in B S ' A CL, co X and B Yes 05 d a3 o B x Ci CD CD in o CO., LTD B ffl oS B B oS X Η o « + in '- / B J. cn B CD <D o3 o H X o

Randem Recovery Rate: 62.76¾

Recovery rate: 94,45¾ (calculated for distillation in a laboratory without preliminary treatment)

Claims (8)

1. A method for the regeneration of waste lubricating oils, comprising a strong-base treatment step, characterized in that it consists of the following successive treatment steps: a / an assessment of the concentrations of fuel oil, fatty acid and chlorine and the removal of oils containing a very high percentage of one of these ingredients; b / heating, wherein the regeneration oils are in the temperature range between 120 ° and 250 ° C; c) adding an aqueous solution of a strong base with a ratio of 1 to 3% pure base to the mass of the lubricating oil; d / dehydration and extraction of light hydrocarbons; e / gas extraction and recovery / stripping /; e / extraction of the impurities by fractional distillation in vacuo providing separation of the main lubricating oils on the one hand and a residue concentrating all the impurities on the other. 2. The method of regeneration of waste lubricating oils according to claim 1, characterized in that the dehydration and extraction step of light hydrocarbons is carried out by flash. 3. A method for regenerating waste lubricating oils according to any one of claims 1 and 2, characterized in that the vacuum distillation column is connected to a purifying evaporator at the base of the column. «· · · · · · · 4. A method for regenerating waste lubricating oils according to any one of claims 1 to 3, characterized in that the strong base is sodium and / or potassium hydroxide. 5. A method for regenerating waste lubricating oils according to claim 4, characterized in that the strong base is sodium hydroxide. 6. The method of regeneration of waste lubricating oils according to claim 4, characterized in that the strong base is potassium hydroxide. 7. A device for the regeneration of waste oils, including: - reservoir / 2 / for storage of waste oils, - Exhaust oil heating installations (3), - strong storage facilities (4), - mixing plants (5) on a strong basis in a specific ratio to the waste oils, - water and light hydrocarbon extraction unit (6 / / flash), - oil extraction unit / 8 / / stripping / s - impurity extraction facilities / 10,14 / including a vacuum distillation unit / 10 /. 8. A waste oil regeneration device according to claim 7, characterized in that the vacuum distillation unit (10) is connected to a purification evaporator (13) at the base of the column.