DE725001C - Process for refining mineral oils - Google Patents

Description

Process for refining mineral oils In dry refining of mineral oils with sulfuric acid, the procedure is as a rule that one after the Acidification of the oil with sulfuric acid. acidic contained in the acidified oil Shares neutralized with an excess of dry lime and the so neutralized Oil without prior separation of the lime for further cleaning and lightening Subjected by treating with active fuller's earth. This way of working goes the lime used to neutralize the acidified oil partly in its original, partly in converted form as lime salt (soap) into the bleaching earth, so that the resulting oil-containing used bleaching earth still all of the applied Lime contains the corresponding amount of converted lime compounds.

If you want this used fuller's earth after removing the adhering Oil and the coloring substances regenerate, so it turns out that the bleaching earth only up to a lower bleaching power corresponding to the content of lime compounds can be revived, since the -lime compounds are inactive to the bleaching process, yes, even have an activity-inhibiting effect. The removal of the lime compounds is due its insolubility so costly and encounters such great technical difficulties, that a regeneration of such calcareous soils is not carried out with advantage can be.

It is known to treat acidified oils with fuller's earth and immediately to regenerate the used fuller's earth using ammonia. One way neutralized to avoid the aforementioned disadvantages in the bleaching earth treatment Oils are not given here. It has already been suggested that after the treatment to make bleaching earth that accumulates in neutralized oils recyclable by the absorbed impurities were extracted with organic solvents, two different solvents were also used. In this way could However, the fuller's earth cannot be regenerated to such an extent that a frequent Reuse without impairing the effect was possible. It is also known from the used bleaching earth the oil contained therein with hot water and, if necessary with Displacement of steam and a solvent extraction to follow this treatment. Such treatment with water leads to hydrolysis of the bleaching earth acid resin components, which make them gasoline-soluble, so dal.t at the extraction with organic solvents gives impure oils. To neutralize Of the acidic oils, caustic soda has also been proposed without this measure but would have been associated with a special: @rt of regeneration.

It has now been found that by a special combination known: measures a practically complete regeneration of used Bleaching earth is made possible, whereby the refining of the: mineral oils is essential cheaper.

According to the invention, the acidified oil is made in a known manner with basic reacting compounds in water or neutral organic Solvents form soluble salts, and then treated with fuller's earth. The used bleaching earths are successively with organic solvents and Stripped of water.

: organic compounds with a basic reaction come from organic ones Bases, such as aniline, toluidine, amines, etc., in question, as inorganic basic reacting Compounds alkalis, carbonates and primarily ammonia. Do you want the principle sustained during dry refining, gaseous ammonia can be used: A concentrated solution of aqueous ammonia is also suitable.

The use of ammonia has the advantage over lime that the acid resin components still contained in the acidified oil from the acidification are lightened so that the used fuller's earth, which is deeply dark in the lime neutralization colored, when using: Imtnoniak a light yellow to brown color shows. The raffinates obtained from ammonia neutralization are those from lime neutralization equal.

The oil components contained in it can be extracted from the bleaching earth by extraction with gasoline, the resin components with a mixture of a neutral solvent, such as gasoline or benzene, in connection with a polar solvent such as alcohol, Remove acetone etc. completely. : Mixtures of gasoline with about 10% alcohol work very advantageous. If you treat the deoiled earth with hot water, that can be weakly mineral acid, the fuller's earth shows its original adsorbent Power that is not lost even after repeated regeneration.

The invention can be carried out with any type of fuller's earth.

1Ian sometimes receives soils that can be regenerated better, if one follows the Acidification and before the neutralization of the oil by adding substances that cause a precipitation accelerate the acid resin, e.g. B. lime, water, cement, etc., as completely as possible Brings about removal of the acid resin. Asphalt or resin-like deposits then settle Stolte who would otherwise go into the earth during the next stages of treatment, easily and can be removed from the oil beforehand.

It is not necessary to use the bases in Fortn of liquids, they can also be used in a gaseous state (e.g. ammonia) or in solid form (e.g. B. Soda) apply.

It has also proven beneficial to use a slightly damp fuller's earth to use: the water added in the oil after (learning of the oven) can be used as moisture The amount of water left behind or the amount of water added to the soil in some other way Serve water. Example i A heavy machine oil distillate was made with sulfuric acid acidified: after (learning to mix, water was added (about ro ° / "of the used Sulfuric acid), stirred and allowed to settle.

After settling, the oil was neutralized with ammonia and treated with soil. As can be seen from the table, the soil had retained its old bleaching power after being regenerated four times. Neutral color un ion emulsifying action sations- @. @ r the after after h @@ rkcit number treatment; Hours io hours of steam 4 °,! "H_ S o-1 (+ H. @ a)............ - - - - - refined with N H .., and 31) / " Earth - - - - - with fresh earth. . . . . . . . . . . . . . 0.03 - 2 '/ 2 + = 1; `=; 3 ioo " with earth regenerated four times ... 0.03 -2 '-, - z' - + 3 '/, c90 " Example 2 50 tons of a heavy machine oil redistillate were, as usual, acidified with 40 ° sulfuric acid at about 40 °. After thorough mixing, water (about 100% of the sulfuric acid used) was added. After brief mixing and allowing to settle, the acid tar which had settled was drawn off and the oil was neutralized with 0.60/0 magnesite at 70 ° and bleached with 3% earth.

The used earth was regenerated four times. The following results were obtained from the refining of the heavy machine oil: Neutral- Color Union Emulsifying- Sations- treatment before l according to bility number treatment 5 hours to hours with steam 4% HZ S 04 (+ H20). . . . . . . . . . . - - - - - neutralized with magnesite and bleaches with 3 0 / a earth. . . . . . . . . - - - - - with fresh earth. . . . . . . . . . . . . . 0.03 -21/2 + 2 '/. 2 -; - 3 zoo " with earth regenerated four times ... 0.03 -2, / 2 + 2 '/.= - 3 @ / 2 90 1 /

Claims (1)

PATENT CLAIM Process for refining mineral oils by neutralizing them of the acidified oils, treatment with bleaching earth and reuse of the regenerated ones Bleaching earths, characterized in that the following are known per se in combination Measures the acidified oil with basic reacting compounds that exist in water or neutral organic solvents form soluble salts, and then with fuller's earth is treated and then the used bleaching earths successively with organic Solvents and water can be extracted and reused.