DE928060C - Process to increase the yield and improve the quality of Schieferoelschwelparaffin - Google Patents

Description

Process for increasing the yield and improving the quality of shale oil wax paraffin Shale oil wax paraffin is obtained mainly from a fral @ tion of the shale oil melt product boiling between 320 and 46o ° in the sweating process and with subsequent refining, whereby yellowish to yellow paraffin is obtained.

It has been found that there is an increase in yields and a Improving the quality of Schieferölsch.welparaffin receives when the in one Boiling range between 32o and 46o ° passing fraction of the carbonization product of a Pre-hydrogenation at medium pressures of preferably up to 25 atmospheres suitable Hydrogenation catalysts, preferably nickel-copper-magnesiumoxy.d-kieselg; ur catalysts, at temperatures from Zoo to 26o °, preferably at 2.5o °, this is subjected Product is de-oiled in a subsequent extraction or sweating process and finally a refined post-hydrogenation at hydrogen partial pressures of 50 to zoo atü, preferably 75 atü, is connected in a known manner.

Due to the pre-hydrogenation, turn mainly the unsaturated compounds hydrogenated, and the amount of recoverable paraffins increases. Since mainly the oily parts are also the color carriers and these are extremely difficult to achieve Allow to hydrogenate, it is not practical to full the feedstock in one step to hydrate out, especially because one cannot by de-oiling such products comes to fully refined paraffin.

In the process according to the invention, the product is prehydrogenated and its softening point increases by 4 to 6 ° or more. will this If the product has been de-oiled in a suitable process, the subsequent hydrogenation is limited on the amount of paraffins that can actually be obtained, this increases their yield, and only a little colored paraffin is obtained, which becomes due to the post-hydrogenation a completely colorless, odorless and tasteless, color-stable product refined will. The de-oiling can be carried out in a known manner by extraction or in the sweating process performed. #verden.

It has now been found that: by extracting the prehydrogenated product, particularly high paraffin yields, up to 85 % of the input, are achieved if lower alcohols with carbon numbers from 1 to 4, preferably i- or n-propanol, are used as solvents . The amount of solvent used, which is circulated, need not exceed four times the input product, and the cooling temperatures need not be below + 10 °.

In the sweating process, the yields are somewhat lower, and you is forced to work with a high percentage of circulating paraffin, i. H. large proportions of the oily substances removed in fractions during the sweating process Products have to come out as so-called return paraffin: subjected to the sweating process will.

Refining hydrogenation has two advantages over the otherwise usual refining methods: firstly, there are almost no losses, and secondly, a very high degree of refining is achieved, that with otherwise usual refining methods. Refining methods are not achievable and where "color-stable products are obtained. Example A fraction 32o! To 46o ° of the Schieferölschwelprod uktes (Mineralölwerk Messel),. Which is usually processed in the sweating process to obtain table paraffin, with a softening point of 47 ° and an iodine number of Hydrogenation was carried out on a Ni-Cu-Mg O-kieselguhr catalyst for 1 hour at 25o ° and 25 atmospheres H2 + N2, at a partial hydrogen pressure of 18.7 atmospheres. The hydrogenated product was lightened, the softening point rose to 50.5 ° , and the iodine number was = o.

The prehydrated product wound with i-propanol in a ratio of i Part by volume of product mixed with 2 parts by volume of alcohol at 60 °, cooled down to -E- 20 ° and ground to a pulp. After filtering off the 0l alcohol solution and the Wash out the precipitate on the filter with another 2 parts by volume of i-propanol the filter cake was freed from the alcohol residues .and weighed. The so; won The product, 82.5% of the feed, was a light yellow colored, oil-free table paraffin with a softening point of 52.8 °.

This table paraffin was hydrogenated at 250 ° and 100 atmospheres H2 + N2 = .75 atmospheres H2 on a Ni-Cu-MgO-diatomaceous earth catalyst for 2.1 / 2 hours. The hydrogenated product was a transparent, colorless, odorless and tasteless paraffin with a softening point of 52.8 °.

The same starting product with a softening point of q.7 ° wunde de-oiled without pre-hydrogenation in the sweating process, whereby about 4o '/ o of an oil-free, brown colored paraffin with a softening point of 54 °. The paraffin yield could be increased to 700/0 if one tried the Input product partly the last fractions of the previous joke process adds to oily products.

Claims (2)

PATENT CLAIMS: i. Process for increasing the yield and improving the quality of paraffins from Schieferölschwelpro, products, characterized in that the distillation product of the crude paraffin which passes over in a boiling range from 320 to 4 $ o ° is suitable for prehydrogenation at average pressures of preferably ibis to 25 atmospheres Hydrogenation catalysts, preferably Ni - Cu - Mg O - kieselguhr catalysts, at temperatures from Zoo to 26o °, preferably 25o °, with subsequent de-oiling by extraction or sweating processes and a refining post-hydrogenation to be carried out in a known manner at hydrogen pressure of 5o to 100 atmospheres, preferably 75 atmospheres. 2. The method according to claim i, characterized in that that, for (the extractive de-oiling or pre-hydrogenated products with lower alcohols Use C numbers from i to 4, preferably i- or n-propanol.