SA95150447A - " process to re-refine used oils " - Google Patents

Abstract

A method to repeat the used oils, as the oils (A1) are first exposed to a pre-treatment process by a basic reagent (A1), then to a pre-glow process (B) to remove the water (B2) and the more volatile parts (B2) contained therein, and then again , Subjected to a combined process of partial distillation (C) and taqiyya to remove high polymers and heavy metals, and rot in a single column (21) filled with fillings, in order to obtain one or more of the recycled oily parts (C3). High polymers and heavy metals are separated by separating the high-density and viscous oils from the base (bottom) of column (21) by means of a rotating device (cyclone) (23). Recycled oils (G3) have been subjected to an appropriate color removal process (D) and can be used as base (base) oils to produce lubricants. Figure No. (1)

Description

Z Method for Refining Used Lubricating Oils Full description: : Background of the invention This invention relates to a method for refining used lubricating oils with high yield and low pollution. In this branch of technology, the term “re-creasing” means the conversion of used oils and greases from machinery and other industrial uses into basic oils. Where these base oils are used after mixing with some suitable additives as lubricating oils and new lubricants of a degree of quality so that they can be compared to those oils that are obtained ede directly from oil refineries. 1 The first manufacturer appeared to re-refining the oil for use in stencils “0”, as a result of the pique problems resulting from the disposal of the used oil - in the machine * or Ash. In the years that followed that period, and as a result of the increase in consumption on the one hand, and the high cost of clean primary oil (A), it was obtained from the primary refining processes, on the other hand; the re-refined oil became as if it increased day after day until As raw materials, and now it has become a competitor, both in terms of its availability and in terms of its cost, to the oils that Jas!

, ! ! . This is done by creating structures that collect used oils, whereby those animals oblige all users of oils to empty the oils they use. So far, this trend is still increasing ols in the AAC + countries, in contrast to the annual consumption loss ° of lubricating oils reaching about © million tons; And the amount of theoretical ip ble of recovered oils reaches a dr? Malbun ob, where, in fact, “only 1 million tons of those recovered oils are collected and transported to the refining centers.” As for the remaining amount, it is disposed of in a random manner, which causes many problems to pick up. 11 General description of the invention, and there are actually two known methods in this matter; To carry out the process of refining the oils used, the sulfuric acid + method, the SS method, and the brompane method. In both methods, the used oils are first and foremost purified from the water contained in them, and then purified after that with sulfuric acid or, in order, with propane, to get rid of other impurities present in them. These impurities are composed of compounds with a molecular weight *, Jl, which are found in the additives that are added to the oil. Or compounds of metals derived either directly from the corrosion of the intended part or indirectly (0) from the metals present in the fuel or in oil additives such as (plo) 0: 0 in petroleum.

And it was. The method of induction of sulfuric acid is the first method to be introduced — (Las) so it is used + but it is not used now due to pollution problems. Letty Tsbesa.

Jas, this method is mainly based on the following steps as shown in the diagram in Figure 1. : f Gawd! 0 under vacuum (low pressure) Coil used A 1 . This is to separate the product of the vertex + formed with | SN A3 and light pyrocarbonate A© (gas oil); About eb the base that consists of oils torino water a € . 1b- Treating the dehydrated butter 3 with sulfuric acid up 1 ¢ in an amount of about Yo / - Yo 7 by weight ¢, to obtain the five extracts, and then filtered (decantation) of eld compounds, weight fern High and heavy metals. 0 | The oily parts of the heavy and organic oils b.m. C- Equivalence of oils B © All colors with balsa C 1 of limestone and antiquity decolorizing. - filtering kel ls for ly oils to allow Jarl L LJ to contain neutral oils

"> - Colorless C © and retrieval of the rising aerosols C 2 submerged in concentrations: high for the oily parts. Distillation, separation of 0 re-refined oils D 2 into fractions of different viscosity from the side outlets of the column | for distillation ¢ and exit | vapor (Pp) heated from the base A of the column Ca. 01 0 - to obtain a lubricating base and lubricating it 7 ¢ with !a SY exhaust retrieval e + immersed in high concentrations of oily particles. , with reference to the flow rate of Jost ae J the oils used are 1 f equal to Yoo and this | far that | od LJ | because the ad of the sulfuric acid method does not add up to 0. In fact, large amounts of oils are retained in the urban sediments, and the Less cannot be easily recovered from a little bit of sulfuric acid and hydrocarbon compounds, including polyurethane compounds with a high fe weight. and biting compounds It is abundant in sulfur, chlorine, nitrogen and phosphorous, + heavy metals such as chromium,؛ sensitivity Wl

Tickle iron and lead ‎Ce ', in view of the technological problems | Because of this method of waste disposal to AED!, the solution currently in existing factories is to dispose of waste in warehouses or quarries. Py The process of waste disposal is preceded by a process of reconstitution of the present sediments with lime, which relatively increases their size and the cost of their disposal, considering that one to four kilograms of lime is used for each kilogram of lime sediment. Also, the method of burning to ash is not preferred, as it requires the installation and operation of complex and expensive equipment for the disposal of 0 inputs. Resulting from the direct distillation of used oils) the installation of new re-refining plants, which use sulfurmisc acid, was stopped as soon as the well-known method 1 appeared, which uses O-propa in markets, and Figure Y shows Schematic drawing [NOR] of the second method in a similar way to that (AJ) used in the description of the first method that uses Aa

: 7 and the sulfuric + and also the squares are mentioned by reference to the flow rate of : PERN a 1 which is equal to 0001 . In the Albroyan method, it is: The treatment step is replaced by deny, by Lo all, using Albroyan Alsakl. ° In fact, it is possible to easily convert the aforementioned head roe carbon into a liquid, and it has a very reduced volume at this liquid stage. When mixed with the oils to be used, the propane sprays on it as an agent to reduce spillage and liquefaction, which makes it easily evaporated, so the first liquid part B1 with aay; The high UL content contains high polymers and sadly heavy metals

Gd Hy vo is called “asphalt” for the second liquid part 0 contains pure oils that are still free? Of course, aad is equipped to remove broyan from the liquid part B?, and to re-pass the recovered propane for use again. The next filtration step takes place C with decolorizing soil C 1 with (ova pale dust) hot treatment - so that in addition to recovering 1 consisting of a small part of the aly gaseous parts can also be recovered C M; the remaining part of the oil Vase this day.” The gas oil contained in B is in danger of distillation, 1 box with colorless oils, then it will be retrieved in V.

Z, A”, and the reactivity of this fraction is 0, and all the abs distillation d and the decolorization step e are identical to those previously described in the sulfuric acid method. The Al-Bruyan method represents some development compared to the sulfuric acid method, in terms of productivity, which increased by 18 percent, and in terms of eS 0, the contamination that was observed, Lol, decreased to a large extent, 0, and despite that, this method has some defects. For example, the As First Brewian process creates many security problems for workers, due to its high vulnerability to explosives. In addition ; In spite of the processing recessions to remove the propane, the lower heavy fraction B (Jha) 0 contains traces of propane. And this small amount of bromsan is sufficient to prevent the use of these types of asphalt in areas with special names such as roads and pavements. SEIN; On the other hand, it puts its use in one of the fields, such as the formation of aS sealing liners. In fact, it is not possible to form the Ally sealing liners using such types as the working tooth without exposure to the risk of fire.

1 q | 2 and therefore; It was lost in the propane method. The fuel used in JS is considered waste as waste, and it can be disposed of by several stages to reduce the cost: With gas oil so that it becomes sufficiently impermeable and can be used as fuel that has a high calorific value, but the rate of pollution and ignition. Examples of its uses and use include covering ovens with special devices to get rid of (ws SW) and also to get rid of the materials weld! that are in those non-filtered materials. Finally; It is from the point of view of energy; The brompesan method requires a greater amount of electrical energy and fuel to produce the attia steam and to heat the oil compared to the sulfuric filling method. In recent years, a third new method has appeared, in which the used oil is subjected, after the imitation dewatering step, to a thin-film distillation process. In that continuous process, the used oil is sent to a distillation column that rotates around its axis, and from that rotating column it is sprayed on the inner walls of the column (Aly) at high temperatures by means of a fluid flow that generates heat and enters the bottom of that column. With Gypse Sara Al-Amoud, the forehead is transformed?

Z 0: JW Gas! To evaporate from the oils at the same moment to the phase: gar + while the heavy part remains in the slag phase and collects on a base. : column; After that, the evaporated part is collected and then divided into the required parts in a fractionating column.

> This continuous method allows it to obtain global productivity, but it requires a series of obstacles that limit its spread. match the start; This method requires pre-treatment to purify the oils to be used so that they can last for a long period of time without the need for cleaning operations. In particular, the presence of a shaft drive makes

0 of that process is a minute, las, if one takes into account the attrition of soiling, which makes the periodic ala its cost, sal lalas, in consideration of the cleaning process. On the other hand, this process requires capital © Jl and operating costs that do not make it economically competitive with the Broyan method, and finally, WILL, that the height of the thin-film distillation column must be specified.

To clean it, when LS management spe is applied as a result of the need to withdraw the process at high internal flow rates; It requires the use of [amdad].

of "parallel columns + without being able to achieve any interpretation of the dimensions. :

1 Z The inventors of this patent have stood for you, and one of their goals was to prepare a method for re-refining used or used oils with reduction or disposal

OSS Aly completely from the use of factors that are difficult to get rid of, harmful to the environment or causing dangers to human safety, it is implemented in the manufacture also reduces the consumption of geass and simple and small and does not increase the costs of production energy and can be performed in the manufacture of a completely static; The gpI components do not contain any moving parts; It is exposed to dirt problems similar to the treatment of its use; Finally; In order to increase productivity, which is still not satisfactory in the methods 1 currently presented, in terms of the quantity and quality of the recovered oils, and in terms of the possibility of using the by-products for economically beneficial uses; Al-Atjibsa was 0

JUN | To think about the current method and make it more out of place. Known, and according to this invention ¢ Those goals were achieved by using a method to re-refining the used oils, from the type in which these oils are subjected to pre-flare to get rid of water and the most volatile components present in the treatment of yo a to kill them with those oils; Then a purification process to remove the bulk polymers and metals, to a fractional distillation step to obtain oily parts * pam 0 is used as a lubricant; And news exposed to the step of color removal. The method of this invention is distinguished by what opis: Yes

! x The distillation step (JER) is carried out in a single column of the stuffed model. The purification step is done in the form of three consecutive stages, the first stage of pre-treatment, in which, before the glow treatment, an agent is added to the Ba ell) and mixed with oils; The second stage, in which the oils resulting from the glow treatment are filtered, before the fractional distillation, and the third stage, in which the heavy sap* containing high polymers and heavy metals are hatched from the base of the fractional distillation column. And the third stage, in which the heavy sludge part containing high polymers and heavy metals is discharged from the base of the partial distillation column. ye Explanation as to the drawings, and more advantages and benefits of the method of re-refining, the subject of this invention, will become clear from the following detailed description of making a favorite that is done by this method, which is shown in the attached drawings, including: Figure 1: A schematic diagram showing the method of re-refining Refining using the well-known iam 0 sulfuric acid. Figure T: A schematic diagram showing the known method of re-refining using Broyan. 0 Figure M: A schematic drawing showing the method of refining the sealing oils according to the present invention.

Figure 11: For the plant used in implementing the method of this invention: + in which hs explains the addition of the base agent and the pre-glow step in more details. Figure herein: a schematic diagram of the manufacture used in the Sis method, the subject of this invention, in which they clarify the distillation step srl and the step of separating the heavy part containing high polymers and heavy metals with more tetamysil. Description Delivery, and the method of refining the used oils differs according to this invention; . on known methods; In terms of the simplicity of the purification step, “and that the distillation steps are all done in one column (in the case of the well-known Gb, they are done in several columns. In addition to the gift of separating the heavy part containing high polymers and heavy metals.” In addition, this last separation is done By means of a spiral tool (silicone) that is placed at the lower cavity 1 of the distillation column, which is prepared so that it does not receive any moving CURDS, and therefore there are no problems of dirt or blockage “0” resulting from the high viscosity and the special composition of the materials that are processed. ‏

I 0: Pie chart of the Shall blocks that flow to and from each Ml outlet to a feed flow rate of oils to give it A 1 equal to 001 . (LS) aforementioned, the hazards of the treatment to purify the oil from high polyrates and heavy metals include a pretreatment with > a base agent. Thanks to the fact that the worker used for this purpose is a handrail, which is added in A? It is mixed with A1 oils before treatment. This pre-treatment does not directly affect the aforementioned pollutants 0+, but helps in the conversion of existing fatty acids into saponins and precipitates them. On the other hand, it works to neutralize the existing chlorine associated or alone. Attia works to convert the fatty acid into soap, in addition to facilitating the removal of the oil by slurry, which improves the flow of the system by destroying its volatilities, and thus prevents the conversion of the oil into vapor in the distillation column, thus 0 polluting the oils directly and with the contaminated parts that are associated with it. The chlorine neutralization process also protects the manufacture from the dangerous JST 0 purity, which prolongs the operating life of the manufacture. The incandescent process requires pre-treatment with the following

\o . The previous step - as in the currently known methods - is to separate the Zeytsa Mbah current by 1 ; And the stream of gas oil? And before sending the hamsa to the next line, the stream of dehydrated oils is left with the resulting puree from the treatment [ame sgn] for a period of time sufficient to obtain 0 liquor ha transformed into soap or agglomerated. After that, the treated oils stream is sent to the thermal removal line of asphalt and molecular distillation c, which includes at the same time the separation of the phase / light / d1 level on gas oil and the heavy phase c? content of 1 high polymers and heavy metals; Divide 0 oils into three thal gas m of different density. And the three parts that are purified by the separation treatment + are sent to ba, the final decolorization d known, where the ale soil of color d 1 enters, from which the dust exhaust d 7 is removed, and thus | PUREST is based on a main stream of re-refined oils D © + with a high productivity equal to about 77 m with an additional process to recover the oil that has been immersed in the oil exhausts D 2 and thus the productivity can be increased to 75 2 Yau, from that it is possible to carry out a process Decolorization of recycled oils with hydrogen treatment.

1 1 a + b c e 0 holed, bs. It will now be explained: co + with reference to the manufacture shown in each figure, p, showing squares a and b. Where oils are inserted. To the stem flare column ?1 through the pump 1 a er outlet of that pump a base agent A > ¢ is introduced with a flow rate controlled by the metering pump. As previously mentioned, it is preferred that the base worker be made up of a hand; And it is added in the form of a solution: R + an amount that allows the hydrogen number of the oil to be used to settle to 0, preferably + 13 + 01 at the outlet of the column p at a value between, and it is preferable that the flow rate be regulated in the pump 1. 7.17 and VILA between 0 automatically by means of control 2 in the hydrant number showing “. 3 At the exit of the column and the agent M1, after that the used butter is mixed well in the mixing line E; Then it is pre-heated to a temperature of about thermal + fed by the Jobe line.) through “Sare Ne. Steam cap A: The pre-flare column 7 is kept under reduced pressure and is fed by + y mm Hg, by an ejector. And then the stream is separated from the inside to

i VY: column 3 to gr vapor tones on water and gas oil; and to Tur Sakil; contains dehydrated butter; contains gil degre water and polluting materials; The vapor phase is condensed by a cold water condenser MA and then sent to a gravity separator F. The same device 4 also receives the stream of steam that comes out of the ejector ey after it condenses in the condenser A b. After the separation device, the undiscovered gaseous phase is separated - gas - which is sent to a high-temperature burner, so that any gaseous pollutants present in it are destroyed by the cyclic streams We and B0, and the water stream B1 is sent as a simple pollutant with oil. ; To make biological purification with the attia water that comes out of other parts of the factory. And this is indeed the only waste product of the method subject of this invention + which does not exceed Uy of the incoming materials and which does not Gesu of problems during its disposal. Can gas oil be used? - Excellent quality, as the oil has not been treated with polluting agents - In normal uses as fuel, the base product is condensed in the column using a 01 cooling coil; Then it is sent by pump 11 to the VY collection tank. And the dimensions of the tank 1, 3 and the positions of the entry and exit pipes were calculated so that the time for the current in m inside that tank to be on the machine with an hour. And this way

YA 1 a te) aad! plasty i” and other agglomerated fractions soha - as a result of hand processing - is able to be deposited on the base of the tank 7 cy, where it is removed periodically through the washer isbn CY with some impurities . : the figure shows e; It is based on thermal removal of asphalt and partial distillation, which is carried out by vo ladle of dewatered butter. First and foremost, those butters are heated to a temperature of about 0.21°C in a Faz Al-Mathan oven. The oils are then introduced to the base of the fractional distillation column 0 y 1 where it is under a reduced pressure of at least yom 11 mm Hg pe (at the top of the column) + as a result of the main ejector 27a; Which connects in series to secondary launchers IEEE 717 and ?2C I SAF SY RWC at Bukharamab line. Precisely, the heated oils and the fan (Lye) are sent to the top of the spiral tool (silicone) i A rr at the lower part of column 31, and it consists of an open spiral channel that Vo plugs into Jill around its concentric tube, which is centered in Joss. The base part of the column with the part directly above it. At the inlet of column 31 + the evaporation of LS approximately evaporates and the glycosidicity of SY Tr allows complete and good phase separation

Z 0 TS gas for the slick phase + which contains heavy oil fractions on the other and all the pollutants consisting of high polymers and heavy metals. SC p.

° and the vapor phase rising from the silicon © moves to the top of the column vy; Correspondingly, four gaskets, similar to Yo adie +, are placed on top of the 320 assembly plates; They float in a well-known way - the passage of the vapor phase upwards towards the top of the column + the retention of the liquid that condenses.

Column 31 aad], the subject of this invention, has been researched

pen 0 to separate the inlet Lal into an upper part, containing the process steam - and gas oil; and three ab ug af (pled g 1/7 76 g 7/9 µg/©) of re-refined oils of different densities, ready for commercial uses; refer to the base c+ moiety previously described. To obtain this result It must be black

The coil has a very low flow resistance (ym) mm Hg at most per filling) and a large gas-liquid contact surface. Positive results have been obtained to a large extent by using metallic abrasive materials

| From metal strips stacked side by side, in the form of an accordion, ‎CORNER‎

1: aa channels that allow the vapor to rise to about several . Stetimerat. Gaskets of this type, which are made of non-ductile iron, are produced by: Glitzen Italiana - Collameoferd de Arelia (La Nina) - Italy - and is known in the market as Gem Pack. > The part of the liquid that collects the height of the apex surface +7a, which is the plate that is placed under Jol, filled with an ovo, is re-flowed by the pump mma to the area of the column located directly below that plate 0 and is sent after it has been cooled in the Machinist mm to the top of the column 711 . The part in excess of the requirements of 1 dee return machines is collected in C 1; Like gas oil to go down to the market, Masa vo Lal!, which is detailed in the previous pre-glow step. The liquid fh YE collected on plates 1, 6 and = 71 is re-flowed to the column regions below those plates tbe through the drive pumps ory and vyc respectively. pets vo sending the ash part of those but sha ate which is more than the requirements of the ester process is returned to the alia parts of the chapter column 2 which consists of three different sections, flows to one of them directly the part that collects On the base of the board 1 d.

0 z 71 more YA is done and in the three sections of the divided column |, Jalal sl line for the three parts in the reverse current aad

The steam is young and heated in the oven 01 . Finally, the tha accumulated in the column of chapter 34 is sent to the collection tanks by pumps (core.g.© d;) after cooling in 321 flee coolers. Condensation of the condensed currents from the main ejector, try, and from the secondary ejector, vy + ory c + containing process steam, non-condensable gases (0) and zyptal gas vapors, is condensed in water condensers 2 ev, and then collected in a phase separator 0 By gravity “ovr” and the separator “pies vr” fulfills the separation of the gas oil phase exiting from the top of the column 21 from the water phase and from the non-condensable gases Jb dy gas oil to c 1 and the water stream vg is re-passed, To the boilers produced in Baghdad, after they have been treated to remove their spoilage, while the non-condensable gases are sent to a “bath” and then to a combustion furnace to remove any potential Vo gases. 1: Very medium zebuts, v/v oils, V/V ads, to a final color removal, as these oils are exposed in a well-known way to inactivation.

Ty. Color removal with decolorizing soil or pydrogen; So that it becomes suitable for commercial uses. The asphalt stream can be marketed as a result of the absence of solvents, and because it contains polluting materials as a carrier and part of the heavy oils that increase viscosity in an economical way to form pneumatic mattresses in! For methods so as to give the properties of Lg po and sound insulation in particular. The method of refining the used oil, the subject of this invention, is distinct when compared to the currently known methods and techniques. And in fact, regardless of whether it is carried out in simple craftsmanship; Which requires 0 therefore Bila Spade; there is also less need for maintenance d aay yg + as a result of pre-treatment and basic purification in addition to the absence of 1 fle f a mobile. ay If we consider aS the operation; The method subject of this invention is distinct Ley as a + a from C13 in the corresponding table, and therefore the ws of the consumed products, as well as the cost of waste disposal, lye: as shown in the table, all of which are m 7 m With regard to the cost in the sulfuric acid method and 1.4 in relation to the cost in the 0 Las 'propane method, the residues of this method are mainly what Jie

YY of oils in linear pre-glow. And that water, S52, is very small, about m, of the substance A1;

Ye: : Cd — products, method, sulfuric acid, propane, this invention, consumables, 1, natural gas, VY Y ToS, 11, 11, 8, e, 11, 11, 8, 10, 101 Y, 7, 1, oAsoY, 101 Y ,-! Additives USD 0A vote aldose Joly kg - - t EE \Y Broyan PEN - ° - Jo kg VYASY - - nitrogen kg or in TiVo decolorizing dust kg AAR 11.4 Dram Yr A - Filters and Others USD 1 Yor A 7 Items | To get rid of its dead: & m dust, kg, kg for another, YY, and 14) acid sediment + kg, 1 t) E70 - -

0_0 dzi Yo Total cost 1. yoo Ye. per ton of oil used $ 7717 7174 Productivity 4 Arm m

AY 1 ¢o veg Total cost, per ton US dollars (refined oil produced)

PRY SE ES | ! values

IVA Veo / natural gas $ - 08 electric current $ / kWh - - 1 factors $ / kg ato propane $ / kg a1 Y fuel $ / kg

YY nitrogen $ / kg - ether decolorizing $ / kg One $ 1 / kg as 1 exhaust disposal -

YA Disposal of particulate sediment in dollars / kg

Claims (1)

Z | 71. © 1 secret - 1 way to recycle used oils; of the type in which it is exposed Those bots with (a 1) refer to the pre-treatment (B) To remove the water (B.) 1 and the most volatile parts (B”) present Then to purification hazel to remove high polymers and heavy metals 0 > Then the used oils are subjected to a fractional distillation process (c) to obtain 1 One or more parts of the oil for use in lubricating and lubricating ,: and finally to the treatment to remove the color (D); The advantage of this method is that 0 v 1 The partial distillation process (C) takes place in one spe (TV) of the meteorite 4 > Filled with fillings. 1 The purification step takes place in three stages: a first stage of pre-treatment (a) 11, in which a high-alkali agent (orl) is added before the incandescent treatment (b). 1" and mixed with oils (A1); a second stage in which reflux is done before distillation (b +) resulting from the pre-luminescence (b (wed] tamsriq (=) iy content (v2) and a third stage in which the heavy gypsum is discharged before ( CTY) Said] and on high polymers The aforementioned and heavy metals from a column, in which the fractionation column is 1 method, as in the element - 1. It does not exceed mm Hg (Gal). It is a four-stage column with a resistance (11). z 0 y 1 method as in element ? 1 In it, the fragmentation column Y (71) is a four-stage column with a resistance to flow that does not exceed 0 and 1 mm HgBg. 35) For the column (71) of adjacent strips of metal and folded in the shape of a cord. 1E A method as in item 1, in which oils (B©) resulting from pre-flaring (B) are inserted into a helical tool 33 (silicone) placed at “the lower part of the chamfering column (71) E. In it, those oils 8 are separated into a gaseous fraction, which is sent to the upper part of the column (1?) and the lower part 0 is heavy (c “) containing high polymers and heavy metals, which 1 is discharged from the column. oq 1 method as in item 1 + and its subsection The hash column (YY) 1 does not contain any parts. moving ; Even in the lower part where D1D oil circulation occurs. 1x 0 method as in item 1 where the factor is highly alkaline (rl) and | He r a hand. YA: A 1 method as in item 7), in which the agent (A 2) enters in an amount of 0 sufficient to retain the hydrogen number of dehydrated oils, as YI from the step »| Pre-glow in the range between AY + 01 and preferably between 0. 17 rum 3 VISA 1 4- A method as in item 1, in which the process of liquefaction takes place in Kharran 0 (? 1); A position between the pre-flare column (1) and the fragmentation column (71) ( ) 1 with a residence time of at least any hour. / J + 7 + + ) which is dragged into the fragmentation column (71) in the va separation column) before being processed ALY color 1 (D1 . Where the color removal process (D 1 method as in item - 11 1 1) is carried out using color removing dust (E 11 - The same method in item 1, in which the color removal step (D) is a treatment with Hyde Rogaine.