SU1203102A1 - Method of removing heteroatomic compounds from petroleum and petroleum products - Google Patents

Description

one.

This invention relates to methods.

CLEANING of petroleum and petroleum products from sulfur and nitrogenous compounds and can be used in the petroleum refining and petrochemical industries.

The aim of the invention is to increase the degree of purification of petroleum and petroleum products from heteroatomic compounds with the production of high purity aromatic hydrocarbon concentrates.

Example,}. 10 g of sulfur-aromatic concentrate (SAA) of the IZO-aSO C fraction of Kichik-Belskaya oil (Medium n Asia) is dissolved in 10 mp of benzene (or chloroform) and 9 g (0.1 mol) of GPTB and 0.1 g (0.37 mmol) of Mo.Clf. The mixture is kept under stirring for 2 hours at and washed down until the hydroperoxide is completely removed. The organic layer is dried with calcium chloride, the solvent is distilled off.

The oxidation products are separated by liquid adsorption chromatography using silica gel ASK as the adsorbent, and pentane is used as eluents. The pentane eluate contains a purified concentrate of aromatics, the yield of which is 1.85 g (18.5%).

The concentrate of oxidized heteroatomic compounds is eluted with methanol or ethanol.

The conditions and ratios of the initial reagents are given in the table, 1p and the results on the purification of petroleum products - in table. 2

Example2. A 5 g sulfur-aromatic concentrate of the 350-oil fraction from the Samotlor field (AVb-t formation) is added with 0.728 g (0.007 mol) of HPTA and 0.0082 g (0.030 mmol) of MoClg-. The oxidation and isolation of hydrocarbon raffinate is carried out as in Example 1, the yield of raffinate is 4.4 g (88%).

Example The COG of the sulfur-aromatic concentrate of the West-Siberian crude oil from a mixture of 10 ml of benzene (or chloroform) was added 2 g (0.022 mol) of GPTB and 0.0232 g (0.085 mmol) of MoClg-. Oxidation is carried out for 1 h at 60 ° C. The hydrocarbon raffinate is injected by the JAH method, the yield is 4.67 g (46.7%),

;

0

five

five

02-2

EXAMPLE 4 Oxidation of 20 g of the 350-540 0 fraction of the West-Siberian crude oil team after removal of the basic nitrogen is carried out in the presence of 2.3 g (0.022 mol) GPTA and 0.0221 g (0.081 mmol) MoClj at 2 hours, the separation of the purified fraction was carried out similarly to the example, raffinate yield 1.2 g 56%, Example 3. The oil of the Samotlor field (reservoir), after removal of the basic nitrogen in the amount of 20 g, is oxidized by 2 g (0.022 mol) GPTV in the presence of 0.0221 g (0.081 mmol) MoCl at 2 hours. The hexane eluate after the HPAH on silica gel contains refined heteroatomic compounds oil, yield 12.8 g (64%).

Approximately .. K20g of Samotlor oil (potted BBg) dissolved in 20 ml of benzene is added 0.728 g (0.007 mol) of HPTA and 0.082 g (0.030 mmol) of MoClj. The oxidation is carried out for 2 hours at 40 ° C. The separation of the raffinate oil is carried out as in Example 1. The output of the raffinate is 14.0 g (70%).

From the table. 2 data shows that the obtained hydrocarbons with a high degree of purity. The degree of purification of petroleum to petroleum products reaches 78sO-100% of sulfur compounds and almost 100% of nitrogen compounds, which is by 11.5% better than sulfurous compounds and 37.5% better than sulfur compounds. cleaning 6t „nitrogen compounds. The overall degree of purification is improved by 30%. Proposed purification method Prost proceeds under mild conditions, the purification time at the oxidation stage is 12 times less compared with the known method. The selected chromatographic separation of hydrocarbon raffinates allows for a high degree of purification, while sulfuric acid extraction (a known method) causes pitch and contamination of petroleum products, as well as an increase in the cost of cleaning due to the non-regenerability of sulfuric acid.

The advantage of the proposed method is its high oxidizing ability to condensed compounds containing a thiophenic cycle. which cannot be achieved by oxidation with hydrogen peroxide and tertiary butyl hydroperoxide in acetic acid in a manner known per se.

SAC, fractions 120-350 ° C (Kichik-Bel)

2. SAC, fractions 350-400 with (Samotlor AB.)

3. SAC, fractions 350-540 ° С (West-Siberian oil is collected)

4. Fraction 350-540 ° С (assembled in West-Siberian commodity)

5. Oil AVB-g reservoir (Samotlor, after removal of basic nitrogen).

6. Oil reservoir BBg (Samotlor)

By the known method Fractions 350-540 ° C (collected commodity West-Siberian)

Fractions 350-540 ° С (Compiled from West Siberian Commodity)

Table 1

12.90 0.15

10.46 0.11

18.5

2.15 Footprints

2.02 Traces 88.0

3.57 0.33

3.30 0.31

46.7

G, 71 0.06

1.30 0.06

56

1.57, 0.09 1.31 0.09 64 ", 07 0.14 1.07 0.14 70

1.71 0.06

1.30 0.06

45

3, NAO, fractions 350-540 ° С (West-Siberian oil is collected)

4, Fractions 350-540 s (assembled in West Siberian Commodity)

5, AVb-7 oil reservoir (Samotlor, - after removal of basic nitrogen)

6, BBg oil (Samotlor)

By the known method Fractions 350-540 ° C (collected commodity West-Siberian)

Fraction 350-540 ° C

(Collected goods West-52

Siberian)

Editor H, Egorova

Order 8387/3 Circulation 545 Subscription

VNIIPI USSR State Committee.

for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5

Branch PPP Patent, Uzhgorod, st. Project, 4

Continuation of table 2

84.2 93.5

100 77.8

18

0.05

37.5

63

Compiled by N, Bogdanova

Tehred T. Dubinchak Proofreader A. Obruchar

Claims (1)

'METHOD FOR CLEANING OIL AND OIL PRODUCTS FROM HETERATOMIC COMPOUNDS by oxidizing the feedstock with tertiary butyl hydroperoxide or tertiary amyl hydroperoxide followed by separation of the oxidation products, characterized in that, in order to increase the degree of purification and reduce the process time, the process is carried out at a molar ratio of the amount of tertiary butyl hydroperoxide or tertiary butyl hydroperoxide and tertiary hydroperoxide the total sulfur content in raw materials 1: (2.0-2.5) and in the presence of molybdenum pentachloride in a molar ratio of it and tertiary butyl hydroperoxide and whether hydroperoxide _of tertiary amyl 1: (233-275) ® at 40-60 ° C for 1-2 hours. If