RU2675852C1 - Method of obtaining high-index components of base oils of group iii/iii+ - Google Patents

Method of obtaining high-index components of base oils of group iii/iii+ Download PDF

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RU2675852C1
RU2675852C1 RU2018120987A RU2018120987A RU2675852C1 RU 2675852 C1 RU2675852 C1 RU 2675852C1 RU 2018120987 A RU2018120987 A RU 2018120987A RU 2018120987 A RU2018120987 A RU 2018120987A RU 2675852 C1 RU2675852 C1 RU 2675852C1
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iii
base oils
index components
hydrocracking
mpa
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RU2018120987A
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Сергей Николаевич Волобоев
Алексей Федорович Мухин
Алексей Михайлович Ткаченко
Роман Евгеньевич Пашкин
Василий Иванович Анисимов
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Общество с ограниченной ответственностью "ЛУКОЙЛ-Волгограднефтепереработка" (ООО "ЛУКОЙЛ-Волгограднефтепереработка")
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G65/00Treatment of hydrocarbon oils by two or more hydrotreatment processes only
    • C10G65/02Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only

Abstract

FIELD: technological processes.SUBSTANCE: invention relates to a method for producing high-index components of base oils III and III+ groups according to API by catalytic hydrocracking of crude oil at a pressure of at least 13.5 MPa, temperature from 380 to 430 °C, volumetric feed rate from 0.5 to 1.5 hwith a degree of conversion of at least 75 % to obtain an unconverted hydrocracking residue containing at least 90 % by weight of saturated hydrocarbons, including isoparaffin hydrocarbons of at least 30 % by weight, which, after mixing with paraffin slack, obtained in the process of solvent dewaxing from raffinates II, n, III, n, IV, n, the hydrocracking residue is subjected to successively: hydrotreating, catalytic dewaxing (hydroisomerization), hydrofinishing, rectification and vacuum distillation. Method is characterized by the fact that: the required quality of high-index components of base oils is achieved at a pressure of maintaining hydroprocesses less than 6.0 MPa; by adding slack wax, high-index components of base oils are obtained, corresponding to group III, III+ according to API.EFFECT: method allows to obtain high-index components of base oils with a viscosity index from 120 to 140 points, a sulfur content of less than 10 ppm (0,0010 wt%) and a saturated hydrocarbon content of at least 90 wt%, with kinematic viscosity at 100 °C from 4 to 6 mm/s, allowing to vary the range in the production of commercial oils.1 cl, 10 tbl

Description

The invention relates to a method for producing high-index base oil components corresponding to group III / III + by API, and can be used in the oil refining industry to obtain high-index base oil components from an unconverted hydrocracking residue using catalytic hydrotreating, catalytic dewaxing (hydroisomerization), hydrofinishing, and rectification processes and vacuum distillation.

The method allows to obtain high index components of base oils with a kinematic viscosity at 100 ° C from 4.0 mm / s to 6.0 mm / s, a viscosity index of more than 120 points, a sulfur content of less than 10 ppm (0.0010% wt.) And a content of saturated hydrocarbons not less than 90% wt.

From literature data it is known that the technology for the production of components of base oils may include:

- or a number of physico-chemical methods for cleaning raw materials from undesirable components, including selective cleaning and dewaxing processes;

- or a set of catalytic hydrofining processes (hydrocracking, hydrogenation, hydroisomerization, hydrodewaxing);

- or the combination of one or more hydroprocesses with physicochemical methods.

The main disadvantage when using only physicochemical purification methods to obtain high-index base oils is the low yield of the target product up to 50% wt. on raw materials. The combination of hydroprocesses with physico-chemical methods of purification allows you to achieve the necessary purification of oil raw materials with selective solvents to obtain components of the base oils of the required quality and higher yield of the target product.

The processes of catalytic hydrofining, as a rule, are carried out at pressures above 10.0 MPa, which requires the use of expensive equipment.

Despite the fact that a wide variety of technological schemes, operating conditions and catalysts are used in the industrial production of base components of oils, there remains a need for new methods, including methods using fuel oil hydrocracking of heavy raw materials, which can reduce costs and increase work efficiency.

A known method of producing oils by hydrofining and dewaxing of oil fractions after selective purification followed by vacuum distillation of the dewaxed product to obtain distillate and residual components of different viscosity [Zolotnikov V.Z. and others. Hydrogenation refinement of oil raw materials with the aim of improving the technology for the production of lubricating oils. Thematic review. Series: Oil refining. - M.: TSNIITneftekhim, 1986, p. 47-48].

A known method of obtaining the basic components of petroleum oils by hydrocracking straight-run vacuum distillate, with the allocation of the residual fraction of hydrocracking, which is partially sent for recycling in the feedstock in an amount of from 0.5 to 60% wt. on the raw materials of the process [RU 2109793]. By changing the amount of the residual fraction of hydrocracking going for recycling, the increase in the temperature of the end of boiling of the feed stream to 480-520 ° C and the yield of light and heavy fractions obtained by fractionation of the balance part of the residue are controlled. The light and heavy fractions are sent for dewaxing with selective solvents (MEK / toluene). The dewaxed oil is treated with clay.

The method allows to obtain base oils with kinematic viscosity at 100 ° C from 3.1 to 5.5 mm 2 / s, a viscosity index of more than 125 points.

The disadvantage of this method is the decrease in the performance of the hydrocracking unit due to the use of recycling to increase the conversion rate of (undesirable) polycyclic aromatic hydrocarbons. Clay post-treatment is not an environmentally friendly process due to the inability to regenerate the main component of the process - clay.

A known method of producing base oils from the hydrocracking residue of petroleum feedstock using solvent extraction (phenol), dewaxing processes (IEC / MIBK), followed by fractionation with the allocation of the target fraction sent for hydrotreating [US 2004245147]. Prepared a base oil viscosity index 117 points to the kinematic viscosity at 100 ° C 7.05 mm 2 / s and a pour point - minus 12 ° C.

The disadvantage of this method is to obtain one target narrow fraction with a low yield. The resulting base oil product in terms of viscosity index does not comply with the specifications established by the American Petroleum Institute (API) for group III base oils.

A known method of obtaining a lubricating base oil of low kinematic viscosity with a high viscosity index by hydrocracking of crude oil with the release of the hydrocracking residue, its subsequent dewaxing and hydrotreating [US 5460713]. As a raw material for hydrocracking, a mixture of not only vacuum gas oil and coking gas oil is used, but also gach, a paraffin product of the process of dewaxing distillate raffinates. Get the base oil with a viscosity index of more than 120 points, kinematic viscosity at 100 ° C from 3.0 to 7.5 mm 2 / s and pour point - minus 10 ° C.

The disadvantages of this method include obtaining one wide fraction of the base oil.

A known method of producing a lubricating base oil with a high viscosity index and low kinematic viscosity by hydrocracking of crude oil (a mixture of vacuum gas oil and coking gas oil) with the release of the hydrocracking residue with its subsequent dewaxing and hydrotreating [US 5462650].

The method allows to obtain a base oil with a kinematic viscosity of 3 to 5 mm 2 / s, a viscosity index of at least 120 points, and a pour point of minus 10 ° C.

Hydrocracking mixed feeds belong to the classic version of a mixture of vacuum gas oil and coking gas oil, the upper limit of the boiling point of which does not exceed 480 ° C.

A known method of producing high-quality base oil using catalytic processes of hydrocracking, hydrodewaxing (improving low-temperature indicators by changing the structure of long-chain paraffins) and hydrofining (improving color, stability) [US 5358627].

The method allows to obtain a base oil after distillation with a viscosity index in the range of 95-100 points.

The disadvantage of this method is the low viscosity index.

Closest to the proposed method is a method for producing a high index component of base oils using catalytic processes of hydrocracking, hydrotreating, hydrodewaxing, hydrofinishing, rectification and vacuum drying [RU 2604070].

The disadvantage of this method is that it does not allow you to get the base oil corresponding to group III + by API and the quality of the resulting product is highly dependent on the quality of the raw materials for hydrocracking.

The aim of the proposed technical solution of the invention is to develop a method for producing high-index components of base oils corresponding to group III and III + by API, using raw materials of the unconverted hydrocracking residue of the fuel direction in a mixture with paraffin wax obtained in the process of solvent dewaxing from selective raffinates of vacuum selective cleaning shoulder straps (hereinafter referred to as high-grade oil) of the process of primary oil refining (ABT) and from the unconverted hydrocracking residue (patent [RU 5358627]), by technological Coy scheme with successive application hydrotreating processes isodewaxing catalyst, hydrofinishing conducted at a pressure below 6.0 MPa and in the final stage - distillation and vacuum distillation.

The unconverted hydrocracking residue is mixed with paraffin wax obtained in solvent dewaxing units of oils from the selective refining of vacuum shoulder straps of the primary oil refining process (ABT) and / or from the unconverted hydrocracking residue (patent [RU 5358627]), in the ratio: paraffin wax - not more than 90% unconverted hydrocracking residue - up to 100% and is subsequently subjected to: hydrotreating, in order to saturate unsaturated hydrocarbons and remove sulfur, nitrogen and coloring compounds, then catalytic dewaxing (hydroisomerization) - in order to lower the pour point to a temperature of no higher than minus 15 ° С; further hydrofinishing - in order to saturate olefins, residual aromatic compounds and remove coloring substances in the dewaxed product. At the final stage, by distillation and vacuum distillation, the target fraction with kinematic viscosity at 100 ° C from 4.0 mm 2 / s to 6.0 mm 2 / s is isolated.

The implementation of the invention:

Hydrocarbon raw materials, which include straight-run vacuum gas oil, obtained from a mixture of low-sulfur oils, heavy coking gas oil, as well as by-products of secondary solvent processes, successively passes through the following processing stages:

a) hydrocracking of mixed hydrocarbon feedstocks at a pressure of at least 13.5 MPa, temperature from 380 ° C to 430 ° C, bulk feed rate from 0.5 to 1.5 h -1 with a degree of conversion of at least 75% with the release of unconverted the hydrocracking residue containing at least 90% wt. saturated hydrocarbons, including isoparaffin hydrocarbons, at least 30% wt;

b) mixing the unconverted residue with paraffin wax at a temperature not exceeding 90 ° C in the ratio: paraffin wax - not more than 90%; unconverted hydrocracking residue - up to 100%. Changing the amount of saccharum involved, as well as the type of squash (gach from II v / p, III v / p, IV v / p, non-converted residue) allows you to change the kinematic viscosity at 100 ° C of the resulting base oil in the range of 4.0 ... 6.0 mm 2 / s, and a viscosity index of 120 to 140 points;

c) hydrotreating a mixture of unconverted hydrocracking residue with pump in the presence of a catalyst containing at least one of the metals of groups VI and VIII of the periodic table of chemical elements, at a temperature of 300 to 400 ° C, a pressure of 3.5 to 6.0 MPa , with a volumetric feed rate of 0.5 to 1.50 h -1 and a hydrogen-containing gas circulation rate of 500 to 1100 nm 3 / m 3 ;

g) catalytic dewaxing (hydroisomerization) of a hydrotreated mixture of the unconverted hydrocracking residue with gache obtained in stage c) in the presence of a catalyst containing at least one of the metals of group VIII of the periodic table of chemical elements at a temperature of from 290 to 400 ° C, a pressure of from 3.5 to 6.0 MPa, with a volumetric feed rate of from 0.5 to 1.50 h -1 and a hydrogen-containing gas circulation ratio of from 1200 to 3800 nm 3 / m 3 ;

e) hydrofinishing a hydrotreated dewaxed mixture of the unconverted hydrocracking residue with gache obtained in step d), in the presence of a catalyst containing at least one of the metals of group VIII of the periodic table of chemical elements, at a temperature of from 180 to 300 ° C, pressure from 3, 5 to 6.0 MPa, with a volumetric feed rate of 0.5 to 1.50 h -1 and a hydrogen-gas circulation rate of 1200 to 3800 nm 3 / m 3 ;

f) distillation, at a temperature in the distillation column cube of not more than 330 ° C and a pressure of not more than 0.17 MPa, of a hydrotreated mixture of the unconverted hydrocracking residue with pump obtained in step e), with the separation of the NK-280 ° C fraction used hereinafter as a component of commercial fuels, and a fraction of 280 ° C - KK;

g) vacuum distillation, at a temperature in the cube of the vacuum column of not more than 315 ° C and a pressure of abs. not more than 0.05 MPa, fraction 260 ° С - KK obtained from a hydrotreated mixture of the unconverted hydrocracking residue with pump in step e), with the separation of 260 ° С-370 ° С fractions, which are sent as a component to commercial fuels or hydraulic oil bases , and fractions 370 ° С - КК - high index components of base oils.

The feed mixture is subjected to catalytic hydrocracking at a pressure of at least 13.5 MPa, a temperature of 380 ° C to 430 ° C, a bulk feed rate of 0.5 to 1.5 h -1 and a conversion of at least 75%.

Table 1 shows typical physicochemical characteristics of the unconverted hydrocracking residue with a sulfur mass fraction of less than 30 ppm (0.0030% wt.), Namely, 0.0024% wt., And a saturated hydrocarbon content of at least 90% wt., Including the number of isoparaffin hydrocarbons is not less than 30 wt.%, which is promising from the point of view of its use as a raw material for producing high-index components of base oils of 11+ and group III according to API classification.

Figure 00000001

Figure 00000002

The obtained unconverted hydrocracking residue containing not less than 90% wt. saturated hydrocarbons, including at least 30% by weight of isoparaffin hydrocarbons, are mixed with paraffin wax obtained in solvent dewaxing units of oils from raffinates of selective purification of vacuum shoulder straps of the process of primary oil refining (ABT); from the unconverted hydrocracking residue (patent [RU 5358627]), in the ratio: paraffin wax - not more than 90%; unconverted hydrocracking residue - up to 100%. Table 2 shows typical characteristics of paraffin wax according to STO PR 029-00148599-2011

Figure 00000003

The essence of the invention will be shown by the example of mixing the unconverted hydrocracking residue with mixed pump in ratios: 30:70, 50:50, 70:30

Table 3 shows the physicochemical characteristics of the resulting mixture of unconverted hydrocracking residue with gache.

Figure 00000004

Figure 00000005

The resulting mixture is hydrotreated in the presence of a catalyst containing at least one of the metals of groups VI and VIII of the periodic table of chemical elements, at a temperature of 300 to 400 ° C, a pressure of 3.5 to 5.3 MPa, with a volumetric feed rate raw materials from 0.5 to 1.50 h -1 and the ratio of the circulation of hydrogen-containing gas from 500 to 1100 nm 3 / m 3 .

Table 4 shows the characteristics of a hydrotreated mixture of unconverted hydrocracking residue (NOGK) with paraffin wax. Hydrotreating was carried out with the following process parameters: space velocity V = 1.5 h -1 ; pressure P = 5.0 MPa; temperature T = 320 ° C; WASH multiplicity circulation / feed = 600 nm 3 / m 3.

Figure 00000006

Further, the obtained hydrotreated mixture of the unconverted hydrocracking residue with paraffin wax undergoes catalytic dewaxing (hydroisomerization) in the presence of a catalyst containing at least one of the metals of group VIII of the periodic table of chemical elements at a temperature from 290 to 400 ° C, pressure from 3, 5 to 5.3 MPa, with a volumetric feed rate of 0.5 to 1.50 h -1 and a hydrogen-gas circulation rate of 1200 to 3800 nm 3 / m 3 and hydrofinishing in the presence of a catalyst containing at least one of metal fishing of group VIII of the periodic table of chemical elements, at a temperature of from 180 to 300 ° C, a pressure of from 3.5 to 5.3 MPa, with a volumetric feed rate of 0.5 to 1.50 h -1 and a multiplicity of hydrogen-containing gas circulation from 1200 to 3800 nm 3 / m 3 .

Tables 5, 6, 7 show the characteristics of a hydrotreated mixture of the unconverted hydrocracking residue with paraffin wax after catalytic dewaxing (hydroisomerization) and hydrofinishing.

Figure 00000007

Figure 00000008

Figure 00000009

Figure 00000010

Figure 00000011

where V is the volumetric feed rate, P is the pressure in the catalytic system, Tkd is the temperature of the catalytic dewaxing, and Tgf is the temperature of the hydrofinishing.

The rate of circulation of the WASH / raw material in all modes = 2000 nm 3 / m 3

Next, the resulting hydrofined mixture of the unconverted hydrocracking residue with paraffin wax is subjected to rectification and vacuum distillation, with the allocation of the target fraction 370 ° C - KK.

Table 8 shows the material balances of the fractions obtained from the hydrotreated mixture of the unconverted hydrocracking residue with praffin pump at various ratios and modes of catalytic dewaxing (hydroisomerization) and hydrofinishing processes.

Figure 00000012

where V is the volumetric feed rate, P is the pressure in the catalytic system, Tkd is the temperature of the catalytic dewaxing, and Tgf is the temperature of the hydrofinishing.

The rate of circulation of the WASH / raw material in all modes = 2000 nm 3 / m 3

Table 9 shows the quality indicators of the target fraction of 370 ° C - KK obtained from a hydrotreated mixture of the unconverted hydrocracking residue with praffin gum at various ratios and modes of catalytic dewaxing (hydroisomerization) and hydrofinishing processes

Figure 00000013

Figure 00000014

Table 10 summarizes the API classification requirements for base oils.

Figure 00000015

An analysis of the data presented in tables 9 and 10 shows that the viscosity index of the obtained components of base oils under various modes of catalytic dewaxing (hydroisomerization) and hydrofinishing processes ranged from 125 to 137 points, the content of saturated compounds was not less than 90.0% wt., sulfur - less than 10 ppm (0.0010% wt.), which meets the quality requirements for base oils of group III and III + by API.

EFFECT: obtaining high-index components of base oils from an unconverted hydrocracking residue corresponding to API requirements for oils of groups III and III +, at a hydraulic process pressure of less than 6.0 MPa. The production of high-index base oils with a high level of saturated compounds provides an improvement in the operational characteristics of commercial oils, which is not achieved either by the use of new multifunctional additives or by thickening the oils.

Claims (3)

  1. A method for producing high-index components III base oils and Group III + according to API by catalytic hydrocracking of petroleum feedstock at a pressure of at least 13.5 MPa, a temperature of from 380 to 430 ° C, feed space velocity of from 0.5 to 1.5 h -1 with the degree of conversion of not less than 75% to obtain an unconverted hydrocracking residue containing at least 90 wt.% saturated hydrocarbons, including isoparaffin hydrocarbons of at least 30 wt.%, which after mixing with paraffin wax obtained in the process of solvent dewaxing from raffinates II to /P, III v / p, IV v / p, the hydrocracking residue is subjected to successively: hydrotreating, catalytic dewaxing (hydroisomerization), hydrofinishing, distillation and vacuum distillation, characterized in that:
  2. - the required quality of high-index components of base oils is achieved at a hydraulic process pressure of less than 6.0 MPa;
  3. - due to the addition of paraffin wax, high-index base oil components are obtained corresponding to group III, III + by API.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2726619C1 (en) * 2019-08-06 2020-07-15 Общество с ограниченной ответственностью "ЛУКОЙЛ-Волгограднефтепереработка" (ООО "ЛУКОЙЛ-Волгограднефтепереработка") Method for producing medium viscosity white oils

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5460713A (en) * 1992-10-02 1995-10-24 Mitsubishi Oil Co., Ltd. Process for producing low viscosity lubricating base oil having high viscosity index
US20040245147A1 (en) * 2003-06-06 2004-12-09 Boucher Ashe Heather A. Process to manufacture high viscosity hydrocracked base oils
RU2604070C1 (en) * 2015-08-20 2016-12-10 Общество с ограниченной ответственностью "ЛУКОЙЛ-Волгограднефтепереработка" (ООО "ЛУКОЙЛ-Волгограднефтепереработка") Method of producing high-index components of base oils

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5460713A (en) * 1992-10-02 1995-10-24 Mitsubishi Oil Co., Ltd. Process for producing low viscosity lubricating base oil having high viscosity index
US20040245147A1 (en) * 2003-06-06 2004-12-09 Boucher Ashe Heather A. Process to manufacture high viscosity hydrocracked base oils
RU2604070C1 (en) * 2015-08-20 2016-12-10 Общество с ограниченной ответственностью "ЛУКОЙЛ-Волгограднефтепереработка" (ООО "ЛУКОЙЛ-Волгограднефтепереработка") Method of producing high-index components of base oils

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2726619C1 (en) * 2019-08-06 2020-07-15 Общество с ограниченной ответственностью "ЛУКОЙЛ-Волгограднефтепереработка" (ООО "ЛУКОЙЛ-Волгограднефтепереработка") Method for producing medium viscosity white oils

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