CN102485839B - Preparation method of rubber oil base oil raw material - Google Patents
Preparation method of rubber oil base oil raw material Download PDFInfo
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- CN102485839B CN102485839B CN201010578975.4A CN201010578975A CN102485839B CN 102485839 B CN102485839 B CN 102485839B CN 201010578975 A CN201010578975 A CN 201010578975A CN 102485839 B CN102485839 B CN 102485839B
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Abstract
The invention relates to a preparation method of a rubber oil base oil raw material. Crude oil with a density of 950-1000 Kg / m<3> and a 100 DEG C kinematic viscosity of 200-800 mm<2> / s or cycloalkyl normal pressure residuum is used as a raw material, heated to 360-480 DEG C by a heating furnace and enters to an insulating reactor; reactants from the reactor are cooled by quenching oil to 300-380 DEG C, enters to normal and reduced pressure fractionate tower for fractionation, so as to obtain a 340-400 DEG C fraction or a 400-450 DEG C fraction, namely a rubber oil raw material fraction; the quenching oil is a fraction between 360-450 DEG C or 150-280 DEG C from a fractionate tower. The method expands source of rubber oil base oil raw material; and the rubber oil base oil product obtained from a visbreaking-hydrogenation combined technology satisfies enterprise standard of products KN4006 and KN4010 and has characteristics of moderate viscosity, shallow color, low pour point and small UV absorbance.
Description
Technical field
The present invention relates to a kind of preparation method of rubber oil base oil raw material, particularly produce a kind of preparation method of mineral rubber oil base oil raw material by conventional pyrolysis installation.
Background technology
Viscosity breaking is slight heat cracking reaction process, process the main processing technology scheme of mink cell focus and vacuum residuum as 20th century, for refinery provides the means of production of distillate and gas products, object is that the viscosity, the pour point that make oil fuel product are qualified, reduce the amount of mixing light-end products in mink cell focus, improve refinery's economic benefit.
Rubber oil is the general designation of rubber filling oil and rubber processing oil.The oil adding in SR glue production process is called rubber filling oil, as manufactures oil-filled SBR and oil-filled SBS (the vinylbenzene 2-divinyl 2-styrene block copolymer) oil that thermoplastic elastomer adopted; The oil adding in rubber item production process is called rubber processing oil or RUBBER PROCESS OIL.Because the hardness of rubber itself is higher, if add other filler or framework material, the hardness of sizing material can be higher again.In sizing material, add a certain amount of rubber oil, not only softness but also there is good elasticity of the rubber item of producing, in this sense, rubber oil is called again Rubber Softener.The massfraction of rubber filling oil in oil-extended rubber is generally 0.20%～0.50%, the massfraction of rubber processing oil in sizing material is generally 0.02%～0.17%, and concrete used in amounts is determined according to the requirement to sizing material physicals and processing characteristics and character and the consumption of weighting agent.The manufacturer that is sorted in about rubber oil is different with composition according to the molecular structure of mineral oil with the common method adopting of institutions for academic research, thereby has different characterization factor K values, and rubber oil is divided into paraffinic base, cycloalkyl and aromatic base three major types.Oxidation-resistance and the light stability of paraffinic base rubber oil are better, but emulsifying property, consistency and low temperature properties are relative poor, and therefore in a lot of application scenarios, the consistency of paraffinic base rubber oil and rubber is poor, and good processing characteristics cannot be provided.The consistency of aromatic base rubber oil and rubber is best, and the rubber product intensity of producing is high, can add-on large, cheap; But color is dark, pollution is large, toxicity is large, along with the raising day by day of environmental requirement, will progressively be restricted.Naphthenic rubber oil has the characteristic of paraffinic base and aromatic base concurrently, and its emulsifying property and consistency are better, and pollution-free, nontoxic, and the rubber glue kind of adaptation is more, be widely used, and be optimal rubber oil.
And naphthenic base crude reserves only account for 2.2% of crude oil total reserves, resource is few, and along with the exploitation of oil field progressive rolling movement, naphthenic base crude will be fewer and feweri.In recent years, China's rubber industry has entered a fast-developing period, and along with the increase of people to health environment-friendly product demand, environment protecting high-grade white rubber and plastic is by the demand of extending oil also in continuous increase, and desirable rubber oil resource will be fewer and feweri.Therefore widen rubber oil raw material and improve its complete processing, thering is very large realistic meaning.
According to the difference of the difference of feedstock property and rubber oil product, the production technique of rubber oil is also different.CN1570037A discloses a kind of production technique of high aromatic rubber oil, what relate to is the production technique of the black rubber oil that uses in rubber industry, adopt the catalytic cracking turning oil of slag-mixing amount 20% as raw material, the Extract of lube oil furfural refining unit carries out the method for the high aromatic oil that extracting obtains as solvent.CN101386687A discloses a kind of aromatic rubber oil and production method thereof, that to subtract three distillates be that raw material carries out solvent extraction and obtains primary purification oil and once extract oil out, carry out secondary solvent extracting and obtain secondary fine liquefaction and secondary and extract oil out once extracting oil out, secondary fine liquefaction is through the clay-filtered aromatic rubber oil that just obtains, the standby rubber oil aromaticity content of this legal system is high, PCA% is less than 3%, and nontoxic without carcinogenesis.CN101597513 discloses a kind of environment-friendly rubber oil and preparation method thereof, that to subtract three distillates be that raw material carries out solvent extraction and obtains primary purification oil and once extract oil out, primary purification oil is carried out to secondary that secondary solvent extracting obtains to be extracted oil out and is environment-friendly rubber oil, the environment-friendly rubber oil aromaticity content of this invention is high, environmental protection, nontoxic, without carcinogenesis, can be used as the substitute of existing aromatic hydrocarbon oil, there is very bright application prospect.The production technique of current high-grade rubber oil transfers high-pressure hydrogenation process to by traditional solvent treatment, sulfuric acid treatment-clay treatment technique, and quality product is greatly improved, but still has the bad problem of light and thermally stable." hydrogenation method is produced the research of white naphthenic rubber oil " [rubber industry, the 53rd the 8th phase of volume, 2006,475-478] in, adopting hydrogenation technique route is stock oil, high-pressure hydrogenation processing, hydrodewaxing, cutting, the de-aromatic hydrocarbons of high-pressure hydrogenation, product, can greatly improve sunlight stability and the ultraviolet light stability of rubber oil.
Summary of the invention
The object of this invention is to provide a kind of preparation method who prepares rubber oil base oil raw material taking naphthenic base crude inferior or time processing cycloalkyl heavy oil as raw material.The strong adaptability of the method to raw material, can use the existing oil refining process of general prepared using to produce rubber oil base oil raw material.The invention solves and be subject to cycloalkyl viscous crude to subtract two in the past, subtract the restriction that three line distillates are rubber oil base oil raw material, expand rubber oil base oil raw material source, make naphthenic base crude inferior or time processing cycloalkyl heavy oil become displaced loop alkyl viscous crude and subtract two, subtract the rubber oil base oil raw material of three line distillates, and the rubber oil base oil product obtaining through viscosity breaking-hydrogenation combination technique meets the product company standard (Q/SY KL0037-2002) of KN4006 and KN4010, this rubber oil base oil product has modest viscosity, of light color, pour point is low, the features such as ultraviolet absorptivity is little.
Technical scheme provided by the invention is:
Taking naphthenic base crude inferior or time processing cycloalkyl heavy oil as raw material, after process furnace heating, enter from the bottom to top in an in-built dispersion inner member or the adiabatic reactor without inner member, reactor reactant flow out, after quenching oil is cooling, enters normal, vacuum fractionation tower fractionation and obtains rubber oil base oil raw material cut; After this, under hydroprocessing technique condition, rubber oil base oil raw material cut removes sulphur, nitrogen, oxygen and other heteroatomic reaction in hydrogenator, and alkene and part aromatic hydrocarbons are carried out to hydrogenation saturated reaction, make stock oil upgrading, improve viscosity temperature characteristic and inner quality; Enter hydrodewaxing device from hydrotreating reactor hydrogenated oil out, improve oil low-temperature mobility, reduce oil pour point, make the requirement that touches the mark of the pour point of rubber oil base oil; Hydrodewaxing reaction generates oil and enters hydrofining reactor, remove a small amount of alkene producing in pour point depression process, and the further hydrogenation of remaining polycyclic aromatic hydrocarbons is saturated, improves the stability of oil product, and the hydrofined oil obtaining is exactly rubber oil base oil.
Specifically, low viscosity rubber oil base plinth oil tech scheme provided by the invention is: taking density as 950Kg/m
3～1000Kg/m
3, 100 DEG C of kinematic viscosity 200～800mm
2the cycloalkyl long residuum of the crude oil of/s and long residuum thereof, >360 DEG C is raw material, be heated in the adiabatic reactor that enters in-built dispersion inner member after 360～480 DEG C through process furnace, inner member is bubble deck, valve tray, traverse baffle or non-activity packing layer, control raw material 10～180 minutes residence time in reactor, pressure 0.1～2.0MPa; Reactor reactant flow is out cooling through quenching oil, and quenching oil is the cut between 360～450 DEG C that fractionate out through separation column, or cut between 150～280 DEG C, is cooled to 300～380 DEG C; Thermally splitting generates oil and cuts out 340～400 DEG C of cuts through fractionation; The hydrogenated oil that 340～400 DEG C of cuts are obtained through conventional high-pressure hydrogenation processing, hydrodewaxing, the de-three sections of hydrogenation production technique of aromatic hydrocarbons of high-pressure hydrogenation, the distillate that obtains >360 DEG C through cutting is low viscous rubber oil oil base oil.
High viscosity rubbers oil base plinth oil tech scheme provided by the invention is: taking density as 950Kg/m
3～1000Kg/m
3, 100 DEG C of kinematic viscosity 200～800mm
2the cycloalkyl long residuum of the crude oil of/s and long residuum thereof, >360 DEG C is raw material, be heated in the adiabatic reactor that enters in-built dispersion inner member after 360～480 DEG C through process furnace, inner member is bubble deck, valve tray or non-activity packing layer, control raw material 10～180 minutes residence time in reactor, pressure 0.1～2.0MPa; Reactor reactant flow is out cooling through quenching oil, and quenching oil is the cut between 360～450 DEG C that fractionate out through separation column, or cut between 150～280 DEG C, is cooled to 300～380 DEG C; Thermally splitting generates oil and cuts out 400～450 DEG C of cuts through fractionation; The hydrogenated oil that 400～450 DEG C of cuts are obtained through conventional high-pressure hydrogenation processing, hydrodewaxing, the de-three sections of hydrogenation production technique of aromatic hydrocarbons of high-pressure hydrogenations, often vacuum fractionation tower cuts out the distillate of >400 DEG C and is full-bodied rubber oil oil base oil.
Or rather, the invention provides low viscous rubber oil base oil technical scheme is: with density at 950Kg/m
3～1000Kg/m
3, 100 DEG C of kinematic viscosity 200～800mm
2the crude oil of/s and long residuum thereof, a >360 DEG C cycloalkyl long residuum are raw material, after being heated to 390 DEG C～430 DEG C, process furnace enters in the adiabatic reactor of in-built dispersion inner member, inner member can be bubble deck, valve tray and non-activity packing layer, control raw material 20～90 minutes residence time in reactor, pressure 0.1～0.6MPa; Reactor reactant flow is out cooling through quenching oil, and quenching oil can be the cut between 360～450 DEG C that fractionate out through separation column, can be also the cut between 150～280 DEG C, is cooled to 300～330 DEG C; Thermally splitting generates oil and cuts out 340～400 DEG C of cuts through fractionation; The hydrogenated oil that 340～400 DEG C of section cuts are obtained through conventional high-pressure hydrogenation processing, hydrodewaxing, the de-three sections of hydrogenation production technique of aromatic hydrocarbons of high-pressure hydrogenation, the distillate that obtains >360 DEG C through cutting is low viscous rubber oil oil base oil.
High viscosity rubbers oil base plinth oil tech scheme provided by the invention is: with density at 950Kg/m
3～1000Kg/m
3, 100 DEG C of kinematic viscosity 200～800mm
2the crude oil of/s and long residuum thereof, a >360 DEG C cycloalkyl long residuum are raw material, after being heated to 390 DEG C～430 DEG C, process furnace enters in the adiabatic reactor of in-built dispersion inner member, inner member can be bubble deck, valve tray and non-activity packing layer, control raw material 20～90 minutes residence time in reactor, pressure 0.1～0.6MPa; Reactor reactant flow is out cooling through quenching oil, and quenching oil can be the cut between 360～450 DEG C that fractionate out through separation column, can be also the cut between 150～280 DEG C, is cooled to 300～330 DEG C; Thermally splitting generates oil and cuts out 400～450 DEG C of section cuts through fractionation; The hydrogenated oil that 400～450 DEG C of section cuts are obtained through conventional high-pressure hydrogenation processing, hydrodewaxing, the de-three sections of hydrogenation production technique of aromatic hydrocarbons of high-pressure hydrogenations, often vacuum fractionation tower cuts out the distillate of >400 DEG C and is full-bodied rubber oil oil base oil.
Conventional de-three sections of hydrogenation manufacturing conditions of aromatic hydrocarbons of high-pressure hydrogenation processing, hydrodewaxing, high-pressure hydrogenation are: to preparing low viscous rubber oil oil base oil, that 340～400 DEG C of cuts are entered to hydrotreatment reaction bed with after hydrogen mixing preheating, to preparing full-bodied rubber oil oil base oil, that 400～450 DEG C of section cuts are entered to hydrotreatment reaction bed with after hydrogen mixing preheating, controlling afterwards reaction bed temperature is 250 DEG C～400 DEG C, hydrogen dividing potential drop is 5.0～20MPa, and volume space velocity is 0.2～2.0h
-1, hydrogen to oil volume ratio 300:1～1500:1; Enter hydrodewaxing reactor from top from reactor hydrogenated oil out and contact and react with hydrogen with catalyzer, controlling reaction bed temperature is 200 DEG C～350 DEG C, and hydrogen dividing potential drop is 5.0～20MPa, and volume space velocity is 0.2～2.0h
-1, hydrogen to oil volume ratio 300:1～1500:1; Hydrodewaxing reaction generates oil and enters hydrofining reaction bed again, and controlling reaction bed temperature is 200 DEG C～350 DEG C, and hydrogen dividing potential drop is 5.0～20MPa, and volume space velocity is 0.5～2.0h
-1, hydrogen to oil volume ratio 300:1～1000:1; Be low viscous rubber oil oil base oil from the oily distillate that obtains >360 DEG C through cutting of reactor hydrofining generation out, or be the oily base oil of full-bodied rubber oil from the oily distillate that obtains >400 DEG C through cutting of reactor hydrofining generation out.
The catalyzer that hydrogenation combination technique of the present invention uses is conventional catalyst.Use hydrotreating catalyst at the first hydrotreatment reaction bed, the active metal component of catalyzer is W, Ni, and Co, a kind of or its combination in Mo, accounts for 10～40% of catalyst weight in oxide compound active metallic content, and carrier is Al
2o
3, before use, carry out sulfidizing; Use hydrodewaxing catalyzer at the second reaction bed, the active metal component of catalyzer is Ni, and a kind of or its combination in Zn, accounts for 1～10% of catalyst weight in oxide compound active metallic content, and carrier is mordenite or ZSM-5 molecular sieve and Al
2o
3mixture (50:50 weight ratio), before use, can carry out sulfidizing also can be without sulfidizing.Use Hydrobon catalyst at the 3rd reaction bed, the active metal component of catalyzer is W, Ni, and Co, one or two or more kinds combination in Mo, accounts for 10～40% of catalyst weight in oxide compound active metal component content, and carrier is Al
2o
3or Al
2o
3-SiO
2, before use, carry out sulfidizing.
The invention solves the single and resource in the rubber oil base oil raw material source Current Situation such as less, widen rubber oil base oil raw material source, make naphthenic base crude inferior or time processing cycloalkyl heavy oil become displaced loop alkyl second line of distillation, subtract the raw material of three lines, and by adopting thermally splitting-hydrogenation combination technique, produce the rubber oil base oil product of the product standard (Q/SY KL0037-2002) that meets KN4006 and KN4010.
Embodiment
Further set forth technical solution of the present invention and effect below in conjunction with embodiment.
Embodiment 1
Taking the normal residual oil of cycloalkyl as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 2, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 2, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material passes through the rubber oil base oil product that hydrotreatment, hydrodewaxing and hydrofining technology obtain, and meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Embodiment 2
Taking naphthenic base crude as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 2, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 2, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material obtains rubber oil base oil product through hydrogenation, pour point depression and process for refining, meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Embodiment 3
To surpass viscous crude long residuum as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 2, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 2, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material obtains rubber oil base oil product through hydrogenation, pour point depression and process for refining, meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Embodiment 4
Taking high viscous crude as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 2, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 2, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material obtains rubber oil base oil product through hydrogenation, pour point depression and process for refining, meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Embodiment 5
Taking naphthenic base crude as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 3, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 3, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material obtains rubber oil base oil product through hydrogenation, pour point depression and process for refining, meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Embodiment 6
Taking high viscous crude as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 3, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 3, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material obtains rubber oil base oil product through hydrogenation, pour point depression and process for refining, meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Embodiment 7
To surpass viscous crude long residuum as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 3, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 3, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material obtains rubber oil base oil product through hydrogenation, pour point depression and process for refining, meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Embodiment 8
Taking cycloalkyl long residuum as raw material, feedstock property, in table 1, carries out thermocracking process, thermocracking process operational condition, in table 3, obtains rubber oil base oil raw material through cut cutting, and property analysis is in table 3, hydrogenation technique operating parameters and character are in table 4, table 5, and hydrogenation catalyst property analysis is in table 6.Raw material obtains rubber oil base oil product through hydrogenation, pour point depression and process for refining, meets the product standard (Q/SY KL0037-2002) of KN4006 and KN4010.
Table 1 stock oil property analysis
| Project | Cycloalkyl long residuum | Naphthenic base crude | Super viscous crude long residuum | High viscous crude |
| Density, kg/m 3 | 962.5 | 951.7 | 998.1 | 956.0 |
| Viscosity, mm 2／s,100℃ | 382.6 | 288.27 | 1500 | 350.1 |
| Condensation point, DEG C | 3 | -2 | 6 | 4 |
Table 2 thermally splitting operating parameters and property analysis
Table 3 thermally splitting operating parameters and property analysis
Table 4 hydrotreatment-hydrodewaxing-hydrofining test conditions and property analysis
Table 5 hydrotreatment-hydrodewaxing-hydrofining test conditions and property analysis
The analysis of table 6 catalyst property
Claims (2)
1. the preparation method of a rubber oil base oil raw material, it is characterized in that: taking naphthenic base crude inferior or time processing cycloalkyl heavy oil as raw material, after process furnace heating, enter from the bottom to top in an in-built dispersion inner member or the adiabatic reactor without inner member, reactor reactant flow out after quenching oil is cooling, enter normal, the fractionation of vacuum fractionation tower obtains 340～400 DEG C of cuts or 400～450 DEG C of cuts are rubber oil feedstock fraction;
Described naphthenic base crude inferior is: density 950Kg/m
3～1000Kg/m
3, 100 DEG C of kinematic viscosity 200～800mm
2the crude oil of/s; Described time processing cycloalkyl heavy oil is: the cycloalkyl long residuum of crude oil after normal pressure fractionation;
Entering the processing condition of carrying out heat cracking reaction in adiabatic reactor is: temperature in is 360 DEG C～480 DEG C, 10～180 minutes residence time, and pressure 0.1～2.0MPa, quenching oil is cooled to 300～380 DEG C;
Described quenching oil is the cut between cut between 360～450 DEG C that fractionate out through separation column or 150～280 DEG C.
2. according to the preparation method of rubber oil base oil raw material claimed in claim 1, it is characterized in that: entering the processing condition of carrying out thermal response in adiabatic reactor is: temperature in is 390 DEG C～430 DEG C, 20～90 minutes residence time, pressure 0.1～0.6MPa, quenching oil is cooled to 300～330 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104178215A (en) * | 2013-05-27 | 2014-12-03 | 任相坤 | Viscosity-reduced heavy oil and coal co-processing technology |
| CN103242905B (en) * | 2013-05-27 | 2014-12-24 | 中国海洋石油总公司 | High-aromatic hydrocarbon environmental-friendly rubber oil and preparation method thereof |
| CN104560118B (en) * | 2014-12-10 | 2016-08-17 | 辽宁石油化工大学 | A kind of photocatalysis auxiliary thermal reaction method for residual oil |
| CN105907421B (en) * | 2016-06-21 | 2017-08-29 | 中国海洋石油总公司 | A kind of preparation method of low-viscosity environment-friendly rubber oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86102643A (en) * | 1985-05-13 | 1986-11-12 | 东洋工程株式会社 | The treating processes of heavy oil residue |
| CN1472282A (en) * | 2002-07-30 | 2004-02-04 | 中国石油化工股份有限公司 | Method for removing calcium from petroleum |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61151296A (en) * | 1984-12-25 | 1986-07-09 | Mikami Junichi | Fractionator for rubber oil |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86102643A (en) * | 1985-05-13 | 1986-11-12 | 东洋工程株式会社 | The treating processes of heavy oil residue |
| CN1472282A (en) * | 2002-07-30 | 2004-02-04 | 中国石油化工股份有限公司 | Method for removing calcium from petroleum |
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