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Method for modifying paraffins
IPC classes for russian patent Method for modifying paraffins (RU 2313519):
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Method for modifying paraffins / 2313519
Invention relates to modification of oil paraffins, namely, to preparing sulfurous compounds used as additives in manufacturing bitumen in petroleum chemistry. Method involves interaction of paraffin with sulfur in the presence of alkaline metal persulfate or alkaline-earth metal persulfate, or ammonium persulfate. Invention provides preparing modified paraffins for a single step.

FIELD: chemical technology, oil products.

SUBSTANCE: invention relates to modification of oil paraffins, namely, to preparing sulfurous compounds used as additives in manufacturing bitumen in petroleum chemistry. Method involves interaction of paraffin with sulfur in the presence of alkaline metal persulfate or alkaline-earth metal persulfate, or ammonium persulfate. Invention provides preparing modified paraffins for a single step.

EFFECT: improved modifying method.

8 ex

 

The present invention relates to the field of modification of paraffin hydrocarbons, allowing to receive a direct synthesis of sulfur-containing compounds from alkanes, and can be used in the petrochemical industry for the production of bitumen from petroleum residues.

It is known that the paraffins or saturated hydrocarbons capable to oxidize fatty acids with oxygen, air and even the exhaust gases containing little oxygen. The process occurs at 100-160°in the presence of catalysts (metals, metal oxides, metal salts of fatty acids). (Carrer. The course of organic chemistry, Goskomizdat, 1960, 1216 pages). Also known reaction arylaliphatic hydrocarbons containing in the side chain four linearly related carbon atom, and sulfur to form teofanov. Personal reaction Voronkov was the response based on the interaction of elemental sulfur with arilgalogenide. /Voronkov M.G. Dragana E.N. thermal path for the synthesis of organic sulfur compounds. 3 national Symposium on organic chemistry "Strategy and tactics in organic synthesis", Yaroslavl, March 3-6, 2001, p.18/.

The closest technical solution to this problem is the method of obtaining serosoderjaschei additives with enhanced extreme-pressure, anti-wear properties, the interaction of olefins with grey pritemperature 130-150° With (U.S. Pat. Of the Russian Federation No. 2181137, 10.04.2002). The method consists in the interaction of olefins, C16-C26with sulfur at a temperature of 130-150°in the presence of a catalyst. However, paraffin hydrocarbons in the reaction with sulfur under these conditions, do not enter.

Object of the present invention is a modification of the paraffin oil by obtaining from paraffin sulfur compounds.

The technical result is achieved by reaction of paraffin with elemental sulfur in the presence of catalyst is potassium persulfate or other alkali or alkaline earth metal or ammonium.

The reaction is carried out in a mixture of paraffin, sulfur and catalyst at a temperature of 130-170°C for 2-3 hours under vigorous stirring. Modified foods are a mixture of products, since the molecular weight of medical paraffin different and in addition to direct circuits always have some amount of branched chains. In the heavy fractions of oil composition paraffins even more diverse, so the authors believe that the definition and allocation of individual connections impractical. The mixture obtained product is separated from unreacted paraffins known method of freezing GOST 11851-85 Method and characterize the General formula C43H79S2calculated on the elemental composition and molecular weight. Selected the s sulfur compounds of the General formula C 43H79S2are not mercaptans or sulfides, as the titration does not show their presence, most likely compounds are titanovyi character.

The control output is determined by the content of unreacted n-alkanes by gas chromatography using silica capillary column coated with a liquid phase SE-54 length of 30 m and an inner diameter of 0.22 mm in programming mode temperature to 2600°C at 30 C/min, the Content of components determined using the internal standard (n-16).

The calculation of the concentration of sulfur compounds by UV-spectra is carried out by the absorption band 277 MMK (Bolshakov GF, Wataga B.C., Agrest FB Ultraviolet spectra of hetero-organic compounds. Publishing house "Chemistry", 1969, s), the composition sintezirovannyh sulfur compounds is determined by the elemental composition of the reacted compounds.

The molecular weight of the reacted compounds in average remains unchanged, and the number of sulfur atoms in the molecule is 2.

Examples

1. 20 g of paraffin medical and 3% (0.6 g) of sulfur are heated to 150°C, the reaction mixture was added 0.5% (0.1 g) of potassium persulfate and stirred at this temperature for 3 hours. The output of the modified sulfur products amounted to 60%.

2. 20 g of paraffin medical and 3% (0.6 g) sulfur load, which provide up to 170° C, the reaction mixture was added 0.5% (0.1 g) of potassium persulfate and stirred at this temperature for 3 hours. The output of the modified sulfur products amounted to 64%.

3. 20 g of paraffin medical and 14% (2.8 g) of sulfur are heated to 170°C, the reaction mixture was added 0.5% (0.1 g) of potassium persulfate and stirred at this temperature for 3 hours. The output of the modified sulfur products amounted to 62%.

4. 20 g of paraffin medical and 14% (2.8 g) of sulfur are heated to 170°C, the reaction mixture was added 0.5% (0.1 g) of potassium persulfate and stirred at this temperature for 2 hours. The output of the modified sulfur products amounted to 63%.

5. 20 g of paraffin medical and 3% (0.6 g) of sulfur are heated to 170°C, the reaction mixture was added 0.5% (0.1 g) of magnesium persulfate and stirred at this temperature for 2 hours. The output of the modified sulfur products amounted to 60%.

6. 20 g of paraffin medical and 3% (0.6 g)of sulfur are heated to 170°C, the reaction mixture was added 0.5% (0.1 g) of ammonium persulfate and stirred at this temperature for 2 hours. The output of the modified sulfur products amounted to 65%.

7. 20 g of paraffin medical and 3% (0.6 g) of sulfur are heated to 170°C, the reaction mixture was added to 0.25% (0.05 g) of potassium persulfate and stirred at this temperature for 2 hours. The output of the modified sulfur products is left 40%.

Example 9. 20 g of residue Tamsagbulag oil, wikipaedia above 450°content of n-alkanes 6.3% and 3% (0.6 g) of sulfur are heated to 170°C, the reaction mixture was added 0.5% (0.1 g) of potassium persulfate and stirred at this temperature for 3 hours. The content of n-alkanes in the obtained product was 4.8%. The output of the modified n-alkanes was 24%.

Thus, the proposed method allows to obtain in a single stage modified waxes suitable for use as a raw material additives in the petrochemical industry for the production of bitumen from petroleum residues.

1. Modification paraffins sulfur in the presence of a catalyst, characterized in that the interaction of paraffin with sulfur is carried out in the presence of persulfate alkaline or alkaline-earth metal, or ammonium.

2. The method according to claim 1, characterized in that the catalyst is used in amounts of 0.25-0.5% of the reaction mass.

 
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