A method of obtaining a lubricating base oil

 

(57) Abstract:

Usage: petrochemistry. Essence: conduct a preliminary removal of part of the aromatic compounds from petroleum fractions with a boiling range of lubricating oils by selective extraction with subsequent dewaxing product selective extraction. Then the product of selective extraction is directed to the following stages: (a) contacting the lubricating base oil product with a suitable solifidianism catalyst in the first stage Hydrotreating process; (b) separation effluent from stage (a) for gas and liquid fractions; (C) contacting the liquid fraction from step (b) with a catalyst comprising a component of the noble metal deposited on an amorphous refractory oxide carrier, in the presence of hydrogen in the second stage Hydrotreating; (d) the allocation of the lubricating base oil. Technical result: development of a method of producing base oils group II API from petroleum fractions with a boiling range of lubricating oils having a high content of sulfur and/or nitrogen. 8 C.p. f-crystals, 1 table.

The present invention relates to a method for lubricating the main oil having content such as base oil is sometimes referred to as substance, related to essential oils of API group II, according to API publication 1509: Engine oil licensing and certification system, "Appendix E-API base oil interchangeability guidelines for passenger car motor oil and diesel engine oils". Currently, there is increasing demand for such products related to the fact that the modern automobile engines are operated under more severe conditions that require the use of lubricating oil formed from the primary oils that meet the above technical requirements. Major oil API group II are also valuable industrial lubricants because of their superior stability associated with the inhibition of the oxidation process.

Lubricating the main oil traditionally receive from the vacuum distillate or deasphalting vacuum residue. Such distillates obtained by atmospheric distillation of crude oil, which receive the remainder, which is then subjected to distillation under reduced pressure to obtain a vacuum distillate and a vacuum residue. From the obtained vacuum distillate by selective extraction removes the aromatics, receiving a product with a low content of aromatic hydrocarbons. At a subsequent stage of the product of selective ek is initaly solvent. It was found that the above method does not provide easy access to the main oil group II API from most sources of crude oil. An overview of the main ways to get to the main oils of group I and II according to the API are listed in the Oil and gas Journal, September 1, 1997, pp. 63-70.

In the application for U.S. patent US-A-5855767 describes the method of obtaining the primary oil having a content of saturated compounds of above 90% and the viscosity index (VI) of about 100, by hydrogenation of raw materials with a total content of sulfur and nitrogen to about 5 ppm by using a catalyst containing platinum or palladium and zeolite Y. the Specified raw materials can be obtained by selective solvent extraction of oil fractions with a boiling range of lubricating oils, followed by a stage dewaxing with a solvent and combined stage hydrodesulfurization (HDS) and hydrodenitrogenation (HDN).

The disadvantage of the method disclosed in WO-A-5855767, is that when using as starting material fraction oil boiling range of lubricating oils containing significant amounts of sulfur and/or nitrogen, United HDS/HDN stage requires the application of strict conditions in order to reduce the radiation of the main oils of API group II, including stage HDS/HDN oil fraction with the boiling range of lubricating oils with 360S and a pressure of 100 bar, using a Nickel-molybdenum catalyst on alumina, the catalytic dewaxing hydrotreated product and the final Hydrotreating deparaffinizing product using a platinum-palladium catalyst on a mixed carrier of silica-alumina in 232C and pressure bar 77. At the final stage Hydrotreating the main part of aromatic compounds is subjected to saturation. Raw materials may be subjected to selective extraction before the first stage Hydrotreating, in which the coefficient of viscosity of the product of selective extraction in the 5-20 times smaller than the coefficient of viscosity desired for the base oil group II API.

The disadvantage of the method described in WO-A-9802502, is that in the first stage Hydrotreating are relatively strict reaction conditions. Another disadvantage is that due to the large differences in temperatures between the two stages Hydrotreating requires additional cooling.

In US-A-3673078 describes the way in which raw materials are obtained tapinoma method of hydrobromide. Consider the raw material contains less than 800 ppm of sulfur. In the first stage are used sulpicianus NiCoMo containing catalyst. The temperature of this stage is S, and the pressure - bar 102. In the second stage as a catalyst using platinum on alumina and the process is carried out under the same conditions as in the first stage.

The disadvantage of the method described in US-A-3673078, is the use of relatively harsh reaction conditions in the first stage Hydrotreating.

The purpose of the present invention is to develop a method ensuring receipt of base oils group II API by mild hydrotreatment of petroleum fractions with a boiling range of lubricating oils having high levels of sulfur and/or nitrogen.

This goal is achieved using the method described below. This method is intended to obtain basic lubricating oils with saturated substances more than 90 wt. -%, sulfur content less than 0.03% of the mass. and having a coefficient of viscosity of 80-120 from the main lubricating oil having a saturated hydrocarbon of less than 90% of the mass. and the sulfur content in the range from 300 wt. parts/million to 2% wt., and specified major oil what ralom boiling lubricating oils by the method of selective solvent extraction with obtaining the product of selective extraction, after which the product is subjected to dewaxing.

Consider the method includes the following stages:

(a) contacting the main lubricating oil in the first stage Hydrotreating with a suitable Hydrotreating catalyst in the presence of hydrogen at a temperature of 25-350C;

(b) separation effluent from stage (a) a gaseous fraction and a liquid fraction and the liquid fraction contains sulfur in an amount of 50-1000 masses. parts/million and has a nitrogen content of less than 50 mass. parts per million;

(c) contacting the liquid fraction from step (b) in the second stage Hydrotreating in the presence of hydrogen with a catalyst comprising a noble metal deposited on an amorphous refractory oxide carrier; and

(d) isolation of the main lubricating oil with the specified properties.

The authors of the present invention have found that the base oil API group II can be obtained by two-stage method of Hydrotreating at less severe conditions in the case where the raw material is the main oil product produced by the above methods of selective extraction and dewaxing solvent. An additional advantage of the base oils, obtained by selective extraction and dewaxing. Such base oils do not need to prepare where carry out the method of the present invention. This fact is very advantageous in the case when existing gidroochistke equipment and equipment for the selective extraction and dewaxing located in different places.

Another advantage is that the performance of the first stage Hydrotreating (a) of the method of the present invention can be lower than the performance of the first stage Hydrotreating of the method according to WO-A-9802502 with the same formulation base oil group II API. This difference is due to the fact that in contrast to the method of the present invention in a known way on stage Hydrotreating is a certain amount of paraffins. Another advantage is that there is no need in an intermediate stage of cooling, because the working temperature stages (a) and (C) may have close values.

In the context of the present invention, the content of sulfur and nitrogen, expressed in weight percent or Mac. parts/million, represents the number of sulfur or nitrogen in the calculation of the total mixture, of which idet by selective solvent extraction and dewaxing solvent oil fraction with the boiling range of lubricating oils. Suitable distillirovanna oil fractions can serve fraction of the vacuum distillate, obtained from the residue of the vacuum distillation, i.e., the distillate fraction obtained by vacuum distillation tail fraction, which, in turn, is produced by distillation of crude oil under atmospheric pressure. The boiling range of such fraction of the vacuum distillate is usually 300-S, preferably 350-S. However, for this purpose can also be used neasfaltirovanyj tail oil fraction, including neasfaltirovanyj atmospheric distillation residues, and neasfaltirovanyj vacuum residues.

Selective extraction is a widely used technology used to prepare base oils, and this technique is described, for example, in "Lubricating base oil and wax processing", by Avilino Sequeira, Jr., 1994, Marcel Dekker Inc. New York, pp. 81-118. Selective extraction is conveniently conducted using as the extraction solvent, for example, N-methyl-2-pyrrolidone, furfural, phenol, and sulfur dioxide. Most commonly used N-methyl-2-pyrrolidone and furfural. During the selective extraction of aromatic compounds partially removed from a hydrocarbon mixture, thereby increasing the EU ETS sulfur and nitrogen.

Dewaxing is also a widely used technology to prepare base oils.

Possible ways dewaxing include the catalytic dewaxing and dewaxing solvent, which is described in the above mentioned book "Lubricating base oil and wax processing", by Avilino Sequeira, Jr., 1994, Marcel Dekker Inc. New York, pp. 153-224. Example catalytic deparaffinization technology described in the above-cited application WO-A-9802502. For the purposes of the present invention is of a particular type stage dewaxing used to obtain the original base lubricating oil supplied to the step (a), is not decisive. Used in the present invention, the raw materials containing relatively high quantities of sulfur, apparently, should be obtained by the method of dewaxing solvent, since most catalytic dewaxing sensitive to high concentrations of sulfur.

The dewaxing solvent is carried out by cooling the raw material by the solvent, resulting in crystallization of the paraffin molecules. Then the paraffin crystals are removed by filtration and regenerate the solvent. Examples of possible solvents can serve netilat is the train propane.

Original base lubricating oil supplied to the step (a) resulting from the implementation stages of the selective solvent extraction and dewaxing (catalytic or solvent), contains less than 90% of the mass. saturated hydrocarbons and has a sulfur content in the range from 300 mass. parts/million to 2% of the mass. It was found that the method of the present invention is implemented particularly successful, in comparison with the known methods, in cases where the raw material contains a relatively high amount of sulfur, for example more than 1000 mass. parts/million nitrogen Content is preferably less than 50 mass. parts/million, the saturated hydrocarbon is preferably more than 70% of the mass. The main components of the base oil, after the saturated hydrocarbons are aromatic hydrocarbons and polar compounds. Examples of polar compounds can serve as specific gray - and nitrogen-containing compounds. The point of yield is usually less than 0C. Base oils, especially suitable for use in the present invention, are materials that are classified as base oil group I no API, according to the above-cited API publication 1509: Engine oil licensing and certificati reducing sulfur and nitrogen, therefore, this stage can be considered as known previously HDS/HDN stage. In this regard, as the catalyst for the first stage Hydrotreating can be used by any well-known specialist of the catalyst which catalyzes the reaction of HDS and HDN, such as the system described in the above-cited application US-A-5855767.

Suitable catalysts include at least one component based on the metal of group VI and at least one component based on the base metal of group VIII selected from iron, Nickel or cobalt deposited on a refractory oxide carrier. Examples of suitable metals of group VIB can serve as molybdenum (Mo) and tungsten (W). Examples of suitable base metals VIII can serve as Nickel (Ni) and cobalt (Co). Suitable catalysts are, which as a component composed of base metal of group VIII include one or more metals selected from Nickel (Ni) and cobalt (Co), in the amount of 1-25 weight percent (% wt.), preferably 2-15 wt. -%, in the calculation of the number of cells relative to the total weight of the catalyst, and as a component-based metal VIB groups include one or more of the above metals in the number of the Torah. These metal components may be present in elemental, oxidized, and/or sulfide forms deposited on refractory oxide carrier. In addition to the above metals, the catalyst can contain a noble metal of group VIII. Examples of suitable noble metals can serve as palladium and platinum.

Refractory oxide catalyst carrier used in the first stage Hydrotreating may be any inorganic oxide, aluminum silicate, or mixtures thereof, optionally in combination with an inert binder material. Examples of suitable refractory oxides include inorganic oxides like aluminum oxide, silicon oxide, titanium oxide, zirconium oxide, boron oxide, mixed aluminum oxide-silicon and mixtures of two or more of the listed substances.

The catalyst used in the first stage Hydrotreating may also include phosphorus (P), which is a well-known promoter. The preferred content of phosphorus in the calculation of the oxide is 1-10 wt. -%

The preferred catalysts, more preferably containing phosphate promoter, represent a cobalt/molybdenum on alumina is/molybdenum on alumina with Nickel oxide 1-5% of the mass. and the content of molybdenum oxide 10-30 wt. -%, moreover, an example of a catalyst of this type can serve as a commercially available catalyst C-424 Criterion Catalyst company (Houston, TX); Nickel/ultram aluminum oxide with Nickel oxide 1-5% of the mass. and the content of tungsten oxide 10-30% of the mass.

Since the base oil is subject to conversion at the stage (a), contains sulfur-containing compounds, the catalyst used in the first stage Hydrotreating at least partially subjected to preliminary acarnania to improve its serologist. Preliminary acarnania catalyst can be carried out by such known methods as disclosed in the following published patent documents: EP-A-181254, EP-A-329499, EP-A-448435, EP-A-564317, WO-A-9302793 and WO-A-9425157.

Usually preliminary acarnania carried out by Konstantinovna azulfidinee catalyst with such a suitable sulfiding agent like sulfide, elemental sulfur, suitable polysulfide, a hydrocarbon oil containing significant amounts of sulfur-containing substances, or a mixture of two or more of the following sulfiding agents. If sulfatirovnie in situ as sulfidity the substances. Then this oil is brought into contact with the catalyst at a constant temperature rise from ambient to a temperature in the range 150-S. The catalyst should be maintained at this temperature for 10-20 hours. Next, the temperature is gradually increased to the working value. Especially attractive presulfiding agent-based hydrocarbon oils can serve as the base oil itself, which contains significant amounts of sulfur-containing compounds. In this case azulfidinee catalyst may be brought into contact with raw materials, for example, under operating conditions, which ensures acarnania catalyst. Typically, in order to the original base oil can be used as the sulfiding agent, it must contain at least 0.5% mass sulfur-containing compounds, and the specified mass percentage refers to the amount of elemental sulfur based on the total amount of raw materials.

The first stage Hydrotreating is conducted under relatively mild conditions. Operating temperature is 250-350C. The actual temperature will largely depend on the content of sulfur and/or nitrogen in the raw material and the desired degree of restore is to be 10-250 bar, preferably 20-100 bar. Average hourly feed rate (WHSV) may be 0.1 to 10 kg of oil per liter of catalyst per hour (kg/LCAS), with a preferred value of 0.2-5 kg/LCAS.

Effluent from the first stage Hydrotreating stage (b), preferably at high pressure is separated into a liquid fraction and a gaseous fraction. The sulfur content in the resulting liquid fraction is 50-1000 masses. parts/million, and the nitrogen content in the specified fraction is a value less than 50 mass. parts/million Gaseous fraction will contain hydrogen sulfide and ammonia as S - and N is the reaction product formed by reacting HDS and HDN. The gas fraction also contains some hydrogen excess, unreacted in the first stage Hydrotreating, and a number of light hydrocarbons. Split system gas - liquid can be carried out using any known means of separation system gas - liquid, for example a Stripping column pressure.

The hydrogen sulfide and ammonia are removed from the gas fraction obtained in stage (b), to obtain a purified hydrogen-containing gas, which is preferably recycled to the first stage Hydrotreating. Examples of jobs such suitable absorption solvents, as solvents based on one or more alkanolamines (for example, monoethanolamine, diethanolamine, methyldiethanolamine and Diisopropylamine).

In the second stage Hydrotreating (C) the liquid fraction obtained after stage separation system gas - liquid (b), in the presence of hydrogen is brought into contact with a catalyst comprising a noble metal deposited on an amorphous refractory oxide carrier. At the stage (C) the fraction of aromatic compounds is subjected to hydrogenation to saturated compounds. Consider the catalyst preferably includes at least one component based on a noble metal of group VIII deposited on an amorphous refractory oxide carrier. Suitable components based on the noble metals of group VIII can serve as platinum and palladium. Consider the catalyst preferably comprises platinum, palladium or both of the metal. The total number of components on the basis of a noble metal of group VIII is 0.1-10 wt. -%, preferably, 0.2 to 5 wt. -%, moreover, these weight percentages refer to the amount of metal (per element) relative to the total weight of the catalyst.

It was found that the most important circumstance of having the amorphous refractory oxides include inorganic oxides, as aluminum oxide, silicon oxide, titanium oxide, zirconium oxide, boron oxide, a mixed oxide of silicon, aluminum, fluorinated alumina, fluorinated silicon oxide-aluminum and mixtures of two or more of these substances. Among these materials, preferred carrier is a mixed oxide of aluminum-silicon, and particularly preferred is a mixed oxide containing 5-75% of the mass. aluminum oxide. Examples of suitable carrier materials based on oxides of silicon and aluminum are disclosed in WO-A-9410263. Examples of suitable catalysts can serve as a catalyst containing platinum or palladium on an amorphous medium from mixed oxide of silicon-aluminum. More preferably, the catalyst contains platinum and palladium in an amorphous medium from mixed oxide of silicon-aluminum. The most preferred catalyst comprises an alloy of palladium with platinum, preferably deposited on an amorphous carrier oxide of aluminum, an example of which can be commercially available catalysts With-624 and 634 Criterion catalyst company (Houston, TX). Consider platinum/palladium catalyst has the advantage of less deactivation in the case of relatively high sulfur content of talization, used in stage (C), preferably does not contain zeolite materials, more preferably does not contain a celite-Y, such as catalytic components can give rise to undesirable cracking reactions.

The conditions at stage (C) sufficiently comparable with the working conditions in the first zone of the hydrotreatment. The working temperature should not exceed 350C and is preferably 150 to 350C, preferably 180-S. The operating pressure may range 10-250 bar and preferably from 20 to 100 bar. WHSV can be 0.1-10 kg of oil per liter of catalyst per hour (kg/LCAS), preferably 0.5 to 6 kg/LCAS.

Further, the present invention is illustrated by the following examples without limiting the scope of the invention.

Example 1

Base oil obtained by solvent extraction of vacuum distillate furfural followed by dewaxing using a methyl ethyl ketone/toluene as solvent, having the characteristics listed in the table, during the first stage Hydrotreating (a) brought into contact with hydrogen and industrial NiMo catalyst on aluminum oxide

(catalyst C-424 firm Criterion Catalyst Company (Houston, TX). Used SL is for 1000 nl/kg and temperature S.

After this effluent, obtained by the above method, were divided into liquid and gas fractions in the high pressure separator (stage (b)). The liquid fraction had a sulfur content 360 mass. ppm, a nitrogen content was 4.5 wt. parts/million

After that, the liquid fraction, providing fresh hydrogen was subjected to the second stage Hydrotreating (C) using commercial PtPd on amorphous medium of the mixed silica-alumina (catalyst C-624 firm Criterion Catalyst company (Houston, TX). Used too partial pressure and the speed of the recirculation gas, which is at the stage (a). The temperature was 280S.

Effluent from stage (C) was identified as the final product. The table shows the properties of the final product.

Example 2

Repeating the procedure of example 1 except that the temperature in stage (C) was C. The final product had a content of saturated hydrocarbons to 91.1% of the mass. and a content of aromatics of 8.9% of the mass.

Example 3

Repeating the procedure of example 1 except that the temperature in stage (C) was 300C. The final product had a content of saturated hydrocarbons 93.7% of the mass. and aderant more than 90 wt.%, a sulfur content of less than 0.03 wt.% and having a coefficient of viscosity of 80-120, of the lubricating base oil product having a content of saturated hydrocarbons less than 90 wt.% and the sulfur content in the range from 300 wt.h./million to 2 wt.%, moreover, the specified base oil product is obtained by first removing from the oil fraction with the boiling range of lubricants parts of aromatic compounds by the method of selective solvent extraction to produce the selective extraction followed by dewaxing product selective extraction, including the implementation of the following stages: (a) contacting the lubricating base oil product of the first stage Hydrotreating with a suitable solifidianism a catalyst for Hydrotreating in the presence of hydrogen at a temperature of 25-350C; (b) separation effluent from stage (a) a gaseous fraction and a liquid fraction and the liquid fraction contains sulfur in an amount of 50-1000 wt.h./million and has a nitrogen content of less than 50 wt.h./million; (c) contacting the liquid fraction from step (b) in the second stage Hydrotreating in the presence of hydrogen with a catalyst comprising a noble metal deposited on an amorphous refractory Oxydry 2. The method according to p. 1, wherein the Hydrotreating catalyst in stage (a) includes at least one component on the base metal of group VIB and a metal selected from iron, Nickel and cobalt, as well as refractory oxide carrier.

3. The method according to p. 2, characterized in that the catalyst of stage (a) is a Nickel/molybdenum on alumina and has a Nickel content in the form of oxide 1-5 wt.% and the content of molybdenum oxide 10-30 wt.%.

4. The method according to any of paragraphs.1-3, characterized in that the catalyst of stage (C) include platinum and palladium, as well as amorphous media from oxides of silicon/aluminum, in which the total amount of platinum and palladium is 0.2-5 wt.%.

5. The method according to p. 4, characterized in that palladium and platinum are present in the form of alloy.

6. The method according to any of paragraphs.1-5, characterized in that the temperature in stage (C) is 150 to 350C.

7. The method according to any of paragraphs.1-6, characterized in that the pressure in the stages (a) and (C) is from 20 to 100 bar.

8. The method according to any of paragraphs.1-7, characterized in that the product of the lubricating base oil is produced by the method of selective extraction of oil fractions with a boiling range of lubricating oils, followed d the th lubricating oil is a base oil API group I, and the product obtained in stage (d) is a base oil group II API.

 

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