US1178532A - Process of obtaining ceresin and the like from residues of mineral oil. - Google Patents

Description

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JANMIJS, or BUssuM, NETHERLANDS.

PROCESS OF OBTAINING CER-ESIN AND THE LIIIIKE FROM RESIDUES F MINERAL OIL.

T 0 all whom it mag concern Be it known that I, JAN Mus, a sub e ct I of the Queen of the Netherlands, residing 1n Bussum, Netherlands, (whose post-ofiice address is Villa Omega,. Nieuwes Gravelandsche Weg -57, Bussum, Netherlands,)

chemist, have invented a certain new and useful Process of Obtaining Ceresin and the like from Residues of Mineral Oil,'of which.

the following is a specification.

The present invention relates to a process of obtaining ceresin or purified ozocerite and other solid "hydrocarbons of known kind, such as parafiins, from mineral oil residues, that is to say, the substance remaining in the still after the several fractions up to and including lubricating oils have been distilled from crude petroleum, and from the more or less soiled substance obtained during purification of various crude petroleum .distillates with sulfuric acid and the mineral oils of buttery consistency found in Russia, Roumania, India, and elsewhere. The use for such purposes of b'enzin, acetic ether or homologous esters, carbon or other halogen substitution products of saturatedand non--saturated hydrocarbons is well known, acetic acid (glacial fects attend the use of such solvents.

acetic acid), propi'onic acid, butyric acid or the like being preferably added. Great de- Tetrachlorid of carbon in particular, as Well as other compounds {containing chlorin, and also acid compounds (glacial acetic acid-or the like) damage the apparatus, attacking the metal parts so that expensive apparatus protected in a special manner from such attack must be used. Moreover, tetrachlorid I of carbon and benzin have very low boiling points and'when working with such readily volatile liquids great losses are unavoidable. Chlorin compounds such as tetrachlorid of carbon have an injurious action on the health of the persons working with them. The process constituting the subject-matter of the present invention obivates these defects' by using toluene, or more strictly speaking toluol having. a boiling point of 110 degrees (1., instead of the solvents hitherto used. This solvent is, firstly, relatively inexpensive, secondly, can be readily obtained in large quantities to be considered when working with this solvent. Furthermore, the toluene, having Specification of Letters Patent.

tetrachlorid of r and, thirdly, is v specially distinguished by a high boiling "point, so that appreciable losses hardly have Patented Apr. 11, 1916.

Application filed May 11, 1912. Serial No. 696,707.

boiling point of 110 degrees (1., can by distillation be recovered comparatively simply and almost without loss.

The applicant is Well aware that he is not the first to propose the use of toluol in preference to benzol as a solvent of paraffin, but he is the first to discover that ceresin, p'araflin and other solid hydrocarbons from mineral-oil residues, instead of being precipitated injelly-like or colloidal form as they would be on cooling from benzol solutions will, when the residues are treated with toluol having the specified boiling point, or in other words with toluene, be

precipitated in a more crystalline form.

Thereconsequently issues from his discovery the fact that toluene is better suited than the solvents heretoforeused, for obtaining from the residues in question solid hydrocarbons in excellent yield and of excellent nature.

The following example will serve to show how my process may be carried into practice in obtaining purified ozocerite or ceresin: The residues referred to in the opening'paragraph of this specification and preferably preliminarily purified in the usual manner by mixing them with a proper proportion of sulfuric acid and subsequently neutralizing them, are intimately mixed in closed mixers of ordinary construction-with approximately an equal quantity of toluene heated to about 50-80 C., but the exact amount of toluene to be added depends, in

general, on the composition of the residues. After agitating the residues for an appropriate period, for instance, about twenty minutes, with the toluene, the toluene solut1on, perature within the above limits, is allowed to cool to a temperature which is dependent on the melting point of the product to be obtained and may vary from 25 degrees to 60 degrees C., and the undissolved'constituents are separated out in any suitable known manner, for example by filter presses. The separated crude ozocerite substance is further purified by means of, first, sulfuric acid solution, as explained above, and then by magnesia hydrosilicate (fullers earth). The ceresin or ozocerite; obtained in this which has been maintained at a tem-.

manner is of a better quality than the products obtained accor'dingvto well-known processes. Particularly, the ceresin has a higher melting point and is not so sticky as that obtained 1n the manner known heretofore from the same mineral-oil residue. Lastly, the

yield of this ceresin of a. higher melting point is likewise greater. The separated solution can be at first cooled, to say 50 degrees (1., toobtain the hydrocarbons with .high melting point and then be cooled further, to say, 30 degrees (1., whereupon the hydrocarbons, with lower melting point, can

be obtained. Lastly, almost all the toluene can be recovered. The residue which is then left can be used for various technical purposes. The procedure is the same whether mineral oil residues or mineral tars are un der treatment, except that the more solid the material the larger the proportion of toluene used.

Other solid hydrocarbons, such as paraflin and the like, can also be obtained from other mineral oil residues, for example, shale oil residues, in like manner as ceresin or puri fied ozocerite from ozocerite residues.

Having now described the nature of my said mvention and the best means I know of carrying the same into practical efiect, I;

claim 1. A process of obtaining in a crystalline form ceresin (purified ozocerite), paraflin and other solid hydrocarbons from mineralconsists in first subjecting the residues to a preliminary purification, then mixing the same in closed mixers with approximately an equal quantity'of toluene, having a boiling point of 110 degrees (1., andat a temperature. in excess ofrfifty degrees C., and

then separating the toluene from the undissolved solid matterbefore it is cooled. I

- In-testimony whereof I have signed my name to this specification in the presence of two subscribing Witnesses. y

m JANMIJS. Witnesses-z v JOSEPH MILLARI),

W. I. S. MERTEN."