Lube fraction purification process

FIELD: petroleum processing and petrochemistry.

SUBSTANCE: lube fractions are brought into contact with N-methylpyrrolidone in extraction tower according to three-step countercurrent purification scheme to form raffinate and extract solutions. When distillate fraction II (300-400°C) is purified, of sulfoxide is preliminarily added in amount of 0.1-0.5% based on the weight of solvent. Distillate fraction III (350-420°C) is then purified after addition to solvent of 0.5-1.5% of extract obtained from purification of distillate fraction II.

EFFECT: deepened purification of raffinate, increased yield of raffinate as commercial product, and enabled qualified application of extract by-product.

11 tbl, 6 ex

 

The invention relates to the field of oil and can be used for the production of refined selective treatment.

A known method of cleaning oil fractions by mixing the raw material with a solvent in the extraction column with the formation of the raffinate and extract solutions in the presence of excess freed from the solvent extract. In the countercurrent is repeated contacting of the feedstock with a solvent to form the raffinate and extract solutions with subsequent processing of the extract solution by the excess amount of the extract to replenish rafinate phase is desirable oil components /Goldberg D.O. and other "Lubricating oil from the Eastern oil fields", M.: Chemistry, 1972, p.77-78/.

A known method of cleaning oil fractions by multiple counterflow contact of the feedstock with a solvent for phenol and processing of the extract solution of phenol in water for replenishment rafinate phase is desirable oil components. However, phenolic water affects the selectivity of the solvent in the extract solution remains a valuable part of the desirable hydrocarbons, raffinato the solution remains the unwanted part. When the ratio of solvent and raw materials to 2.5:1 by volume of distillate fractions removed 55-57% resinous compounds and d is 80% polycyclic aromatics /Chernozhukov N.I. "Technology of oil and gas processing", 3, M.: Chemistry, 1978, s/.

A known method of cleaning oil fractions by adding the solvent, various additives and surface-active substances (surfactants):

- ethyl - or a mixture of isopropyl-phosphate, in an amount of 0.1 to 1.0 wt.% in the calculation of the solvent;

- Quaternary ammonium salts and alkylimidazole, in the amount of 0.001-5.0 wt.% in the calculation of the solvent;

- polymethylsiloxane, in the amount of 0.005-0.1 wt.% in the calculation of the solvent;

- mixtures of ethers, wikipaedia at temperatures of 130-150°With, in the amount of 0.3 to 1.0 wt.% in the calculation of the solvent;

etc /Patent RF №2059686 "Method of cleaning oil fractions"/.

The objective of the invention is to improve the quality of refined and increase their outputs when cleaning distillates II oil fraction (300-400° (C) and III oil fraction (350-420° (C)obtained from a mixture of sulfur crude oil, while reducing the consumption of expensive solvent.

The problem is solved by the fact that:

1) when cleaning the distillate II oil fraction (300-400° (C) in an organic pre-add oil sulfoxide in an amount of 0.1-0.5 wt.% in the calculation of the organic;

2) when cleaning the distillate III oil fraction (350-420° (C) in an organic pre-add the extract in the amount of 0.5-1.5 wt.%, received at academicist II oil fraction with sulfoxide.

This method allows you to:

to find the optimal process temperature to obtain the maximum possible output of the raffinate with the required quality;

- to increase the output of refined 2-3% without changing the temperature, the ratio of solvent or quality of the raffinate;

- enhance cleaning of the raffinate without increasing the consumption of expensive solvent;

- use the by-product of the extract to reduce costs in the cleaning process

and to increase the yield of the main product - the raffinate.

Oil sulfoxidov reduce solvent capacity of the solvent through the formation of hydrogen molecules methylpyrrolidone with oxo group of sulfoxidov that, in turn, increases the dipole moment and the polarity of the solvent, increasing its selectivity. When this change of the temperature of dissolution of groups of hydrocarbons: temperature dissolving tar and polycyclic aromatic hydrocarbons practically unchanged or slightly reduced, and the temperature of the dissolution of alkanes and naphthenes increases, the sulfoxidov introduced into the solvent in the form of a concentrate, which is presented in table 1.

Also it is well known that the introduction of additional concentrate of aromatic hydrocarbons (in our case - extra is t, obtained when cleaning II oil fraction) when the extraction creates a saturation soluble hydrocarbons from the extract solution is allocated secondary phase, increasing yield of raffinate.

Stage 1. The impact of adding sulfoxide in an organic at constant temperature mode of extraction:

Example 1. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction II oil fraction organic, containing 0.1 wt.% sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw materials to 2.5:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 51°C, the temperature at the second stage of extraction (the middle of the extraction columns) 56°C, the temperature at the third stage extraction (top of the extraction column) 61°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The results are shown in tables 3, 4, 5.

Example 2. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction II oil fraction organic, containing 0.3 wt.% sulfoxide. Conditions for extraction were selected taking into account the industry is slowly clearing. The multiplicity ratio of solvent and raw materials to 2.5:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 51°C, the temperature at the second stage of extraction (the middle of the extraction columns) 56°C, the temperature at the third stage extraction (top of the extraction column) 61°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The results are shown in tables 3, 4, 5.

Example 3. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction II oil fraction organic, containing 0.5 wt.% sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw materials to 2.5:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 51°C, the temperature at the second stage of extraction (the middle of the extraction columns) 56°C, the temperature at the third stage extraction (top of the extraction column) 61°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The results are shown in tables 3, 4, 5.

On the basis of the obtained data shows that a significant increase in the concentration of oil sulfoxidov in its solvent dissolving capacity at posto is nom temperature decreases, that is unacceptable for economic reasons, the increase of the temperature profile or temperature gradient of the process necessary to improve the quality of the raffinate, is also inappropriate. At low concentrations of sulfoxidov in its solvent selectivity increases slightly, which allows, without changing the mode and ratio of solvent to obtain a greater quantity of raffinate (increase of the yield of the target product is 2.36% for light oil distillates), working on the same raw material, at a constant quality of the target product. Experimentally it was found that the optimum amount of additive concentration is the concentration of 0.1%.

Stage 2. The impact of adding sulfoxide in an organic at variable temperature extraction. When adding a polar solvent other functional groups that differ chemically and dipole moment, its selective ability increases in contrast to the solvent, which in turn affects the critical temperature of dissolution, with the greatest increase occurs when the change in concentration from zero to the minimum value of concentration (if sulfoxide concentration of 0.1% is an increase in crown-rump length 5.7°compared with the pure solvent). Accordingly, when a higher value of the CTD can be achieved over the high degree of purification, but it is necessary to raise the temperature of the extraction. But with the increase in the temperature regime of the process will decrease the yield of raffinate, as the dissolving capacity of the solvent increases.

Example 4. According to the three-step purification scheme, in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction II oil fraction organic, not containing sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw materials to 2.5:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 46°C, the temperature at the second stage of extraction (the middle of the extraction columns) 51°C, the temperature at the third stage extraction (top of the extraction column) 56°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The results are summarized in tables 6, 7, 8.

Example 5. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction II oil fraction organic, containing 0.1 wt.% sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw materials to 2.5:1 by volume. The temperature at the first stage of extraction (bottom extraction is Olonne) 51° With temperatures in the second stage of extraction (the middle of the extraction columns) 56°C, the temperature at the third stage extraction (top of the extraction column) 61°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The results are summarized in tables 6, 7, 8.

Example 6. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction II oil fraction organic, containing 0.3 wt.% sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw materials to 2.5:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 52°C, the temperature at the second stage of extraction (the middle of the extraction columns) 57°C, the temperature at the third stage extraction (top of the extraction column) 62°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The results are summarized in tables 6, 7, 8.

Based on these results, we make the following conclusions: with increasing concentration of sulfoxide in the solvent and the corresponding change in temperature mode is a significant change in the yield of raffinate with changes in the concentration of sulfoxide from zero to the minimum value (output reduces the W 1.24%), then the output of the raffinate varies slightly, but the quality of the raffinate, on the contrary, improves almost linearly. Process temperature changes similar to the output of the raffinate increases by 5°With changes in the concentration of sulfoxide from zero to the minimum value, then increases the temperature by 1°C. Dissolving capacity decreases due to the formation of hydrogen bonds of molecules N-methylpyrrolidone with oxo group of sulfoxidov. The selective ability of the solvent with the sulfoxide increases because the formed hydrogen bonds increase the dipole moment and the polarity of the solvent, respectively change and temperature of the dissolution of the group of hydrocarbons, the temperature of dissolution of tar and polycyclic aromatic hydrocarbons practically unchanged or slightly reduced, and the temperature of the dissolution of alkanes and naphthenes increases.

Table 1

The quality of the oil concentrate sulfoxide.
IndicesThe quality indicators
Density at 20°C, kg/cm31020
Kinematic viscosity is ri 50° C, mm2/s18,9
Pour point, °-30
Sulfur content, % (mass.):
- total11,35
- sulfoxide10,66
Table 2

Characteristics of distillate II oil fraction.
The refractive index at 50°The kinematic viscosity at 50°mm2/sMelting point, °The color on the colorimeter CNT, % CNTThe flash point in closed crucible, °
1,48598,72411,52,0owed 161.1
Table 3

Material balances process.
The number sulfoxide in a solvent, %00,10,30,5
The yield of raffinate %50,4552,8153,2153,66
The extract yield, %49,2646,9946,3046,18
Loss, %0,290,200,490,16
Table 4

Characterization of II refined oil fraction.
The number sulfoxide in a solvent, %00,10,30,5
The refractive index at 50°1,45701,45701,45811,4583
The kinematic viscosity at 50 mm2/s7,4287,4267,4307,431
Melting point, °of 17.016,916,916,8
Table 5

Feature extracts II oil fraction.
The number sulfoxide in a solvent, %00,1 0,30,5
The refractive index at 50°1,51221,51221,51201,5120
The kinematic viscosity at 50°mm2/s9,8709,8129,7909,732
Melting point, °a 3.9the 4.7a 4.95,2
Table 6

Material balances process.
The number sulfoxide in a solvent, %00,10,3
The yield of raffinate %50,4549,2148,63
The extract yield, %49,2650,5551,19
Loss, %0,290,240,18

Table 7
Characterization of II refined oil fraction.
The number sulfoxide in a solvent, %00,10,3
The refractive index at 50°1,45701,45681,4565
The kinematic viscosity at 50 mm2/s7,4287,4127,410
Melting point, °of 17.017,4of 17.5
Table 8

Feature extracts II oil fraction.
The number sulfoxide in a solvent, %00,10,3
The refractive index at 50°1,51221,51151,5112
The kinematic viscosity at 50 mm2/s9,8709,8659,864
Melting point, °a 3.94,04,2

Stage 3. The impact of adding the extract obtained when cleaning II oil fraction organic, containing 0.1 wt.% sulfoxide - cleaning III oil fraction at a constant temperature of extraction. The quality of the distillate III oil fraction are shown in table 9. The quality of the extract when cleaning II mA what Laney fractions are given in table 10.

Example 7. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction III oil fraction organic, containing 0.1 wt.% sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw material 2:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 65°C, the temperature at the second stage of extraction (the middle of the extraction columns) 70°C, the temperature at the third stage extraction (top of the extraction column) 75°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The results are shown in table 11.

Example 8. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction III oil fraction organic, containing 0.1 wt.% sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw material 2:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 65°C, the temperature at the second stage of extraction (the middle of the extraction columns) 70°C, the temperature at the third stage extraction (top of the extraction column) 75°C. Is the forest raffinate and extract solutions were selected with 5 series of countercurrent purification. The concentration of extract in the organic amounted to 0.5 wt.%. The results are shown in table 11.

Example 9. According to the three-step purification scheme in countercurrent method prototechno-periodic extraction (Nash and hunter) was carried out by extraction III oil fraction organic, containing 0.1 wt.% sulfoxide. Conditions for extraction were selected based industrial cleaning. The multiplicity ratio of solvent and raw material 2:1 by volume. The temperature at the first stage of extraction (the bottom of the extraction column) 65°C, the temperature at the second stage of extraction (the middle of the extraction columns) 70°C, the temperature at the third stage extraction (top of the extraction column) 75°C. Equilibrium raffinate and extract solutions were selected with 5 series of countercurrent purification. The concentration of extract in the organic amounted to 1.5 wt.%. The results are shown in table 11.

The method of cleaning oil fractions by contacting them with N-organic in the extraction column according to the scheme of the three-step cleaning in countercurrent with the formation of the raffinate and extract solutions, characterized in that the purification of the distillate II oil fraction (300-400° (C) N -, an organic pre-add the oil sulfoxide in an amount of 0.1-0.5 wt.% in the calculation of the solvent, further, when cleaning the distillate III oil fraction (350-420° (C) N -, an organic pre-add the extract in the amount of 0.5-1.5 wt.%, obtained by purification of the distillate II oil fraction with sulfoxide.



 

Same patents:

FIELD: petroleum processing and lubricants.

SUBSTANCE: lubricating oil fraction is preliminarily combined with low-boiling hydrocarbon solvent and stepwise extraction is then conducted at 40-55°C using dimethylsulfoxide as selective solvent.

EFFECT: increased degree of purification without using surfactants complicating and raising in price purification process, reduced consumption of solvent (by 30-40%) and power.

1 tbl, 4 ex

The invention relates to the extraction methods of cleaning oil from sulfur compounds

FIELD: petroleum processing.

SUBSTANCE: invention, in particular, relates to purification of vacuum gas oils, mazuts, and/or dewaxed products used further as feedstock for hydrocracking and catalytic cracking as well as high-quality fuel oils and marine oils. Purification contemplates removal of polycyclic aromatic hydrocarbons, heteroatomic compounds, resins, asphaltenes, and heavy metal compounds. Process consists in liquid extraction of undesired components with two mutually immiscible solvents: polar N-methylpyrrolidone with 3-5% water at 40-60°C and nonpolar n-undecane or undecane fraction forming azeotropic mixtures with N-methylpyrrolidone having minimal boiling temperature (about 179°C). Weight ratio of nonpolar solvent to raw material is (0.4-0.5):1.

EFFECT: increased selectivity of process in reduced risk of thermooxidative and hydrolytic decomposition of N-methylpyrrolidone as well as corrosion of equipment.

1 dwg, 4 tbl, 4 ex

The invention relates to the extraction methods of cleaning oil from sulfur compounds

The invention relates to the refining industry and can be used for cleaning vacuum gas oil from aromatic hydrocarbons, heteroatomic compounds and heavy metals with the aim of obtaining high-quality raw materials for the process of hydrocracking and catalytic cracking

The invention relates to a process for recovering organic acids including naphthenic acids, heavy metals and sulfur from the source of crude oil

The invention relates to a process for recovering organic acids from the source of crude oil

The invention relates to the refining industry and can be used when cleaning the raw material for hydrocracking and catalytic cracking from polycyclic aromatic hydrocarbons, heteroatomic compounds and heavy metals

The invention relates to the refining industry and can be used for simultaneous receipt of hydrotreated diesel fraction environmentally friendly diesel fuel that meets the requirements for the content of aromatic hydrocarbons, and aromatic solvents "type Nefras AR" and "Solvent oil with a content of aromatic hydrocarbons of not less than 98 wt.%

The invention relates to the refining industry and can be used to remove aromatic hydrocarbons from hydrotreated oil fraction with the aim of obtaining high-quality jet fuel with simultaneous extraction of aromatic solvent

The invention relates to the cleaning of oil fractions of crude oil and can be used in the refining industry

The invention relates to methods of cleaning oil from sulphides and can be used in refining and petrochemical industries

FIELD: petroleum processing.

SUBSTANCE: invention, in particular, relates to purification of vacuum gas oils, mazuts, and/or dewaxed products used further as feedstock for hydrocracking and catalytic cracking as well as high-quality fuel oils and marine oils. Purification contemplates removal of polycyclic aromatic hydrocarbons, heteroatomic compounds, resins, asphaltenes, and heavy metal compounds. Process consists in liquid extraction of undesired components with two mutually immiscible solvents: polar N-methylpyrrolidone with 3-5% water at 40-60°C and nonpolar n-undecane or undecane fraction forming azeotropic mixtures with N-methylpyrrolidone having minimal boiling temperature (about 179°C). Weight ratio of nonpolar solvent to raw material is (0.4-0.5):1.

EFFECT: increased selectivity of process in reduced risk of thermooxidative and hydrolytic decomposition of N-methylpyrrolidone as well as corrosion of equipment.

1 dwg, 4 tbl, 4 ex

FIELD: petroleum processing and petrochemistry.

SUBSTANCE: lube fractions are brought into contact with N-methylpyrrolidone in extraction tower according to three-step countercurrent purification scheme to form raffinate and extract solutions. When distillate fraction II (300-400°C) is purified, of sulfoxide is preliminarily added in amount of 0.1-0.5% based on the weight of solvent. Distillate fraction III (350-420°C) is then purified after addition to solvent of 0.5-1.5% of extract obtained from purification of distillate fraction II.

EFFECT: deepened purification of raffinate, increased yield of raffinate as commercial product, and enabled qualified application of extract by-product.

11 tbl, 6 ex

FIELD: oil and gas production.

SUBSTANCE: invention refers to procedure of clarification of oil distillate under effect of magnetic field consisting in clarification of oil distillate with N-methyl-pyrrolidone, also, oil distillate is subjected to effect of constant magnetic field with induction 0.05-0.25 tesla. Force lines of constant magnetic field are directed perpendicular to vector of flow of oil distillate, while linear rate of flow in an active gap of a magnetizator amounts to 0.01-03 m/sec, whereupon oil distillate is mixed with N-methyl-pyrrolidone.

EFFECT: improved quantitative and qualitative indices of finish product, reduced critical temperature of oil distillate dissolving in N-methyl-pyrrolidone and reduced temperature of extraction.

2 cl, 4 ex, 2 tbl

FIELD: oil-and-gas production.

SUBSTANCE: invention relates to method whereby initial hydrotreated diesel fraction is separated by rectification into light and heavy components. Heavy component is subjected to liquid extraction with subsequent regeneration of solvent from refined and extracted solutions and blending of obtained refined product with light component of diesel fraction. Note here that solvent in liquid extraction is N-methylpyrrolidone. Hydrotreated diesel fractions with final boiling point approximating to 300°C are used as light component. Hydrotreated diesel fractions with initial boiling point approximating to 260°C are used as heavy component. Weight ratio between hydrotreated diesel fraction heavy component and N-methylpyrrolidone varies from 1:0.5 to 1:2. Temperature in liquid extraction is kept varying from 40°C to 70°C.

EFFECT: better ecological properties.

1 tbl, 2 ex

FIELD: oil-and-gas production.

SUBSTANCE: invention relates to production of diesel fuel. Proposed method comprises oil desalting, extraction of diesel fractions, their mixing and mix hydrofining. In distillation in atmospheric column, two diesel fractions are run off that boil away at 171-341°C and 199-360°C, 199-360°C-fraction is directed to fluid extraction to remove benzalkylthiophens at the stock-to-extragent ratio of 1:1 to 1:4. Note that said extragent represents the product of interaction of organic amine with organic acid, that is amide. Thereafter, fractions 171-341°C and 199-360°C are mixed after purification in percentage composition of 70-85% and 15-30%, respectively. Note here that said mix at distillation by ASTM D-86 method features dry point of 360°C. Produced mix is subjected to hydrofining to get diesel fuel.

EFFECT: diesel fuel with sulfur content not exceeding 10 ppm.

1 tbl, 6 ex

FIELD: oil and gas industry.

SUBSTANCE: task is settled by extraction of nitrogen-containing compounds from hydrocarbon phase into ion fluid (process solution). Process solution represents ion fluid, for example, on the base of alkilimidazol cation and tetrafluoroborate anion or chloride, that contains diluted compounds of transition metals selected from the group including complexes of cobalt (II) and cuprum (I) with 4,5- dicarboxyphtalocianin. Method includes further separation of hydrocarbon fracture from ion fluid and electrochemical regeneration of ion fluid. Ion fluid regeneration is done by electrochemical oxidation of nitrogen-containing compounds.

EFFECT: improvement of hydrocarbon raw materials quality.

3 cl, 1 tbl, 15 ex

FIELD: oil and gas industry.

SUBSTANCE: invention refers to diesel fuel denitration. The invention is related to the method of diesel fuel denitration which includes contact of diesel fuel containing one or several nitrogen-containing compounds with acid ionic liquid at mass ration of diesel fuel and acid ionic liquid equal from 1:0.2 up to 1:2 in at least one extraction zone for selective removal of nitrogenous compounds and production of effluent of denitrated diesel fuel that contains denitrated diesel fuel and acid ionic liquid with nitrogen-containing molecules and extraction of denitrated diesel fuel from effluent of denitrated diesel fuel; at that acid ionic liquid is hydrosulphate butyl methyl imidazoline (BMIMHSO4) or methyl sulphate butyl methyl imidazoline (BMIMCH3SO4).

EFFECT: production of the product with low content of nitrogen.

8 cl, 8 dwg, 7 tbl, 6 ex

FIELD: oil and gas industry.

SUBSTANCE: invention relates to the method of treatment of light hydrocarbon fractions containing sulphureous compounds and carbon dioxide, by means of contact in a counterflow absorber within a single stage with a circulating modified aqueous solution of alkanolamine regenerated to preserve a modifying additive by means of temperature desorption of carbon dioxide and sulphureous compounds. The modifying additive is sodium hydroxide in the amount of 0.005-1%, which after regeneration together with the absorbent is returned into the process. Absorbent supply into the absorber column is carried out by two flows into the upper and medium part of the column, the flow of saturated absorbent is discharged accordingly from the medium and the lower part of the absorber, flows are combined and sent for regeneration into a desorber.

EFFECT: high extent of treatment from carbon dioxide, hydrogen sulfide and other sulphureous compounds.

1 tbl, 2 ex

Up!