CN110498889A - Contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition and preparation method thereof - Google Patents
Contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition and preparation method thereof Download PDFInfo
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- CN110498889A CN110498889A CN201910749638.8A CN201910749638A CN110498889A CN 110498889 A CN110498889 A CN 110498889A CN 201910749638 A CN201910749638 A CN 201910749638A CN 110498889 A CN110498889 A CN 110498889A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/06—Organic solvent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/04—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethene-propene copolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F287/00—Macromolecular compounds obtained by polymerising monomers on to block polymers
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
- C10M143/04—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation containing propene
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/022—Ethene
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/024—Propene
Abstract
The invention discloses one kind to contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition and preparation method thereof, the composition is mainly the solid for the star-type polymer being prepared by bipolymer (I), catalyst (II), modified monomer (III), auxiliary monomer (IV) by melt polymerization process, or the liquid composition for the star-type polymer being prepared by solution polymerization process.The present invention is can to improve shear stability or cryogenic property under the premise of not reducing the oil product detergency of OCP class VII.
Description
Technical field
The invention belongs to modifying lubricating oil technical field more particularly to a kind of lubricating oil viscosity index improver composition and
Preparation method.
Background technique
Viscosity index improver (VII) is the oil-soluble high-molecular compound under a kind of room temperature in rubber-like or solid-like,
Usually the concentrate of 5-10% is diluted to come using a kind of (lubricant oil composite of Li Zhongming with the neutral oil of 150SN or 100SN
Viscosity index improver .CN 108048167A).VII is added into lubricating oil, can be obtained that cold cranking capacity is good, high temperature viscosity is suitable
Preferably, the multi-grade oil of all-season, long service life.The macromolecular chain of VII is fully extended at high temperature in lubricating oil, plays increase
Viscosity effect；Meeting shrinkage crimping, the influence to viscosity are small under low temperature.Thus, compared with the identical single-stage lubricating oil of viscosity, contain
The multi-grade oil of VII viscosity index (VI) with higher and smooth viscosity-temperature curve.
The tackifying of ethylene-propylene copolymer viscosity index improver (OCP), shear stability, viscosity temperature characteristic are preferable, and
Raw material is easy to get, simple process (Xiang Wencheng dispersion type ethylene-propylene copolymer viscosity index improver lubricating oil .1994,5:36-
42.), it is usually used in the formula of I. C. engine oil.Unfortunately the cryogenic property of OCP class viscosity index improver is poor.It grinds
Study carefully and shows that the cryogenic property of OCP class viscosity index improver is related with the structure of strand and molecular size range and distribution.Molecule
Amount is bigger, and molecular entanglement is more significant under low temperature, and under certain shear effect, flow resistance is bigger.Molecular weight distribution is got over
Narrow, long-chain and short chain molecule ratio are fewer, under certain shearing force, occur chain rupture possibility it is smaller, viscosity retention compared with
By force.In addition, propyl sequence molar ratio is bigger in ethylene-propylene copolymer strand, methyl substituents quantity is more, molecular entanglement
Effect is stronger, and shearing resistance is bigger, and low-temperature startup is poor.(Wang Guojin, Zhu Heju, Ye Yuankai, Chen Yuezhu .OCP viscosity index (VI) change
Influence lubrication and sealing 1999,6:26-29.) into agent molecule structure to cryogenic property
Currently, engine apparatus forward direction high speed, small size, high-power, environmental protection and energy saving direction develop, to being used
The thickening property of OCP class VII, shear stability, oxidation detergency, the requirement of resistance to low temperature are also further harsh.Existing OCP's
Shear stability index is 55 or less (diesel fuel nozzle 30 recycles SSI, and smaller then shear stability is better), and low temperature apparent viscosity refers to
Number CCSI is 200 or less (measuring at -20 DEG C, smaller then cryogenic property is better), and high-temperature oxydation detergency is 4.0 grades or less (heat
Pipe oxidation grading, smaller then oil product detergency are better).For meet demand, it is necessary to be modified, commonly use to ethylene-propylene copolymer
Mode be that polar monomer graft is carried out to OCP or prepares polar monomer copolymerization (Chen Dehong, Song Qingwu, Liu Jianxin dispersion is anti-
The development petroleum refining of oxygen type ethylene-propylene copolymer viscosity index improver DAOCP and chemical industry .2001,1:34-36.), although property
Can on centainly promoted, but still there are thickening property, shear stability, oil product detergency, resistance to low temperatures etc. cannot be simultaneous
The problem of Gu.
If patent application 201610522192.1 discloses a kind of method of polymer modification lubricating oil, this method comprises:
The polymer solution obtained after polymerization reaction is directly mixed with lube base oil, wherein the polymer is selected from second
At least one in third rubber, hydrogenated styrene-butadiene block polymer and hydrogenated styrene isoprene block polymer
Kind.Method provided by the invention can overcome the solid lubrication oil viscosity index modifier of the prior art to be lubricated oil base oil
Modification when, mobility of the existing modification of lubricating oils that cannot improve acquisition in ultralow temperature, and cannot be in high temperature
When higher tackifying is provided, to affect the defect of the viscosity-temperature characteristics of lubricating oil.However, the polymer can not be in low temperature
Under the conditions of improve shear stability, there is thickening property, shear stability, oil product detergency, resistance to low temperatures etc. cannot be simultaneous
The problem of Gu.
Summary of the invention
Based on this, the primary purpose of the present invention is that providing one under the premise of not reducing the oil product detergency of OCP class VII
Kind improve shear stability or cryogenic property contains star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition
And preparation method thereof.
The purpose of the present invention is to provide one kind take into account tackifying (thickening ability), shear stability, oil product detergency and
Cryogenic property contains star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition and preparation method thereof, and reduces
The generation of irreversible crosslinking, improves the preparation efficiency and reliability of product.
To achieve the above object, the technical solution of the present invention is as follows:
One kind containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition, it is characterised in that described
Composition mainly passes through melt polymerization by bipolymer (I), catalyst (II), modified monomer (III), auxiliary monomer (IV)
The paste or block for the star-type polymer that method is prepared, or the star polymerization being prepared by solution polymerization process
The composition of object.
The solid is paste or block.
Wherein, according to mass fraction meter, the bipolymer (I) is not less than 96 parts, and catalyst (II) is no more than
0.3 part, modified monomer (III) be no more than 3.2 parts, auxiliary monomer (IV) be no more than 0.5 part.
Further, the line that the bipolymer (I) is minimized by the crystallinity that unit (α) and unit (β) form
Property copolymer, number-average molecular weight is 2~500,000, and the formula of unit (α) and unit (β) is
Further, the bipolymer can typically be selected from Ethylene-Propylene Block Copolymer, ethylene-propylene
Any one in random copolymer, hydrogenated polyisoprene or any combination.
The catalyst (II) is the organic compound containing formula (γ) structural unit.Wherein, R1 and R2 is respectively hydrogen original
Son and the alkyl of C1~12, naphthenic base, aryl, ketone group, carbonate group, ester group, any one in acyl group or any combination；Its
In, the alkyl, naphthenic base, aryl, ester group, carbonate group, ketone group, acyl group further can be independently selected from alkane by 1~6
Base, naphthenic base, aryl substituent group replaced, formula (γ) is as follows:
Further, the catalyst (II) can typically be selected from hydrogen peroxide, isopropyl benzene hydroperoxide, tert-butyl mistake
Hydrogen oxide, cumyl peroxide, di-t-butyl peroxide, dibenzoyl peroxide, dilauroyl peroxide, perbenzoic acid
It is the tert-butyl ester, the peroxidating trimethylacetic acid tert-butyl ester, di-isopropyl peroxydicarbonate, any one in di-cyclohexylperoxy di-carbonate
Kind.
The modified monomer (III) is the compound containing more than two (δ) or (ε) groups, the molecule of (δ) or (ε)
Formula is as follows:
Further, the modified monomer (III) typical case can be selected from trimethylolpropane trimethacrylate, trihydroxy methyl
Propane trimethyl acrylic ester, ethoxylated trimethylolpropane triacrylate, pentaerythritol triacrylate, 3 (the third oxygen
Base) glycerol triacrylate, three (2- ethoxy) isocyanuric acid triacrylates, two (trimethylolpropane) tetrapropylenes acid
Ester, pentaerythritol tetraacrylate, 4 (ethyoxyl) pentaerythritol tetraacrylates, appointing in double pentaerythritol methacrylate
It anticipates a kind of or any combination.
The auxiliary monomer (IV) is styrene, acrylamide, contains appointing in the thiuram derivative of formula (φ) structure
It anticipates one kind, wherein R3 and R4 can be the alkyl of C1~7, naphthenic base, aryl, benzyl, isobutyl group, any one in piperidyl
Or any combination, wherein formula (φ) structure is as follows:
Further, the thiuram derivative typical case can be selected from tetramethylthiuram monosulfide, tetramethyl
Thiuram, tetraethylthiuram disulfide, tetra-benzyl thiram disulfide, DMDPTD dimethyl diphenylthiuram disulfide, curing
Diisobutyl thiuram, two rings, penta methylene tetraalkylthiuram disulfide, bis-pentamethylenethiuram tetrasulfide, six vulcanizations are double
Penta-methylene thiuram etc..
A kind of melt polymerization process containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition,
Be characterized in that method includes the following steps:
(11) catalyst (II) is accurately weighed, and is dissolved in solvent, solution (A) is obtained；Solution (A) is equably sprayed into
Stirring in bipolymer pellet (B), stands, after solvent volatilizees completely, obtains mixture (C)；
(12) mixed and modified material (C) is squeezed out on extruder, control extrusion temperature is to squeeze out between 120-300 DEG C
The composition (D) being mixed by modified monomer (III) and auxiliary monomer (IV) is added dropwise in machine bringing-up section or end, is after extrusion
Obtain the star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition.
In the melt phase polycondensation, solvent used is energy catalyst-solvent but cannot dissolve bipolymer (I)
Solvent can be acetone, ethyl acetate, methanol, ethyl alcohol and other solvents for being easy to volatilize.
A kind of solution polymerization process containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition,
It is characterized in that the described method comprises the following steps:
(21) it is added in batches in the reactor of Xiang Shengyou base oil bipolymer (I), control temperature is no more than 130
DEG C, blender is started, copolymer is dissolved, mass ratio of the copolymer in base oil is no more than 30%.
(22) it is warming up to 130 DEG C~300 DEG C, then injecting catalyst (II) into reaction kettle, is reacted by 1~30min,
So that bipolymer is degraded, macromolecular radical is formed；
(23) modified monomer (III) and auxiliary monomer (IV) are reinjected, persistently stirs 10-30min, cooling discharging to get
To the star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition.
The base oil is mineral base oil, synthetic base oil, vegetalitas base oil, and 40 DEG C of kinematic viscosity of base oil are
5.0~160.0mm2/ s or 100 DEG C of kinematic viscosity is 1.5~34.0mm2/s。
The mineral base oil main component includes that alkane, cycloalkane, aromatic hydrocarbons, naphthenic base aromatic hydrocarbons and oxygen-containing, nitrogen, sulphur have
Machine compound；Synthetic oil can be polyalphaolefin, synthetic ester, polyethers, silicone oil, fluorine-containing oil, in phosphate any one or it is any
Combination；Vegetalitas base oil is the natural animal-plant grease in molecular structure containing ester bond.
The present invention is by being added catalyst (II), so that the upper structural unit (β) of bipolymer is degraded, molecule
(β) unit ratio is reduced on chain；Simultaneously as degradation be it is random, the molecular weight distribution of gained strand can be very wide.Further
The addition sequence and dosage for controlling catalyst (II) and modified monomer (III), enable macromolecular radical and modified monomer
(III) it reacts, forms the star copolymer of long-chain branch, improve thickening ability；The use of auxiliary monomer (IV), reduces not
The generation of reversible crosslink.
Furthermore, it is understood that strand is shunk the be formed by star-type polymer of the present invention at low temperature, but do not occur serious
It tangles, the influence to viscosity is smaller；Under high temperature, strand is unfolded, significant to lubricating oil tackifying effect, so that lubricating oil adds dosage
It is reduced, main carbochain and (β) unit are reduced in addition, help to improve shear stability.
More importantly structural unit (β) ratio is reduced and the molecular weight distribution of strand broadens, the low temperature of gained VII
Performance is significant.The preparation method of the modified copolymer overcomes the crosslinking problem in polymerization process, makes the modified copolymer
The thickening ability of the lubricating oil VII of preparation, shear stability, cryogenic property, high-temperature oxydation detergency greatly improve.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
What the present invention was realized contains star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition, mainly
By bipolymer (I), catalyst (II), modified monomer (III), auxiliary monomer (IV) by melt polymerization process prepare and
At star-type polymer paste or block, or the combination of star-type polymer being prepared by solution polymerization process
Object.In composition and preparation process, however not excluded that other auxiliary agents can be added.
Wherein, according to mass fraction meter, the bipolymer (I) is not less than 96 parts, and catalyst (II) is no more than
0.3 part, modified monomer (III) be no more than 3.2 parts, auxiliary monomer (IV) be no more than 0.5 part.
Specifically, what the bipolymer (I) was minimized by the crystallinity that unit (α) and unit (β) form
Linear copolymer, number-average molecular weight are 2~500,000, and the formula of unit (α) and unit (β) is
Further, the bipolymer can typically be selected from Ethylene-Propylene Block Copolymer, ethylene-propylene
Random copolymer, hydrogenated polyisoprene, any one in hydrogenated styrene-butadiene copolymer or any combination.
The catalyst (II) is the organic compound containing formula (γ) structural unit.Wherein, R1 and R2 is respectively hydrogen original
Son and the alkyl of C1~12, naphthenic base, aryl, ketone group, carbonate group, ester group, any one in acyl group or any combination；Its
In, the alkyl, naphthenic base, aryl, ester group, carbonate group, ketone group, acyl group further can be independently selected from alkane by 1~6
Base, naphthenic base, aryl substituent group replaced, formula (γ) is as follows:
In the specific implementation, the catalyst (II) can typically be selected from hydrogen peroxide, isopropyl benzene hydroperoxide, tertiary fourth
Base hydrogen peroxide, cumyl peroxide, di-t-butyl peroxide, dibenzoyl peroxide, dilauroyl peroxide, benzoyl peroxide
T-butyl formate, the peroxidating trimethylacetic acid tert-butyl ester, di-isopropyl peroxydicarbonate, appointing in di-cyclohexylperoxy di-carbonate
It anticipates one kind.
The modified monomer (III) is the compound containing more than two (δ) or (ε) groups, the molecule of (δ) or (ε)
Formula is as follows:
Modified monomer (III) typical case can be selected from trimethylolpropane trimethacrylate, trimethylolpropane tris
Methacrylate, ethoxylated trimethylolpropane triacrylate, pentaerythritol triacrylate, 3 (propoxyl group) the third three
Alcohol triacrylate, three (2- ethoxy) isocyanuric acid triacrylates, two (trimethylolpropane) tetraacrylates, Ji Wusi
Alcohol tetraacrylate, 4 (ethyoxyl) pentaerythritol tetraacrylates, in double pentaerythritol methacrylate any one or appoint
Meaning combination.
The auxiliary monomer (IV) is styrene, acrylamide, contains appointing in the thiuram derivative of formula (φ) structure
It anticipates one kind, wherein R3 and R4 can be the alkyl of C1~7, naphthenic base, aryl, benzyl, isobutyl group, any one in piperidyl
Or any combination, wherein formula (φ) structure is as follows:
The thiuram derivative typical case can selected from tetramethylthiuram monosulfide, tetramethylthiuram disulfide,
Tetraethylthiuram disulfide, tetra-benzyl thiram disulfide, DMDPTD dimethyl diphenylthiuram disulfide, disulfide diisobutyl
Thiuram, two rings, penta methylene tetraalkylthiuram disulfide, bis-pentamethylenethiuram tetrasulfide, six vulcanization di-penta methylene autumns
Blue nurse etc..
The melting containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition that the present invention is realized
Polymerization, comprising the following steps:
(11) catalyst (II) is accurately weighed, and is dissolved in solvent, solution (A) is obtained；Solution (A) is equably sprayed into
Stirring in bipolymer pellet (B), stands, after solvent volatilizees completely, obtains mixture (C)；
(12) mixed and modified material (C) is squeezed out on extruder, control extrusion temperature is to squeeze out between 120-300 DEG C
The composition (D) being mixed by modified monomer (III) and auxiliary monomer (IV) is added dropwise in machine bringing-up section or end, is after extrusion
Obtain the star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition.
In the melt phase polycondensation, solvent used is energy catalyst-solvent but cannot dissolve bipolymer (I)
Solvent can be acetone, ethyl acetate, methanol, ethyl alcohol and other solvents for being easy to volatilize.
The solution containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition that the present invention is realized
Polymerization, it is characterised in that the described method comprises the following steps:
(21) it is added in batches in the reactor of Xiang Shengyou base oil bipolymer (I), control temperature is no more than 130
DEG C, blender is started, copolymer is dissolved, mass ratio of the copolymer in base oil is no more than 30%.
(22) it is warming up to 130 DEG C~300 DEG C, then injecting catalyst (II) into reaction kettle, is reacted by 1~30min,
So that bipolymer is degraded, macromolecular radical is formed；
(23) modified monomer (III) and auxiliary monomer (IV) are reinjected, persistently stirs 10-30min, cooling discharging to get
To the star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition.
The base oil is mineral base oil, synthetic base oil, vegetalitas base oil, and 40 DEG C of kinematic viscosity of base oil are
5.0~160.0mm2/ s or 100 DEG C of kinematic viscosity is 1.5~34.0mm2/s。
The mineral base oil main component includes that alkane, cycloalkane, aromatic hydrocarbons, naphthenic base aromatic hydrocarbons and oxygen-containing, nitrogen, sulphur have
Machine compound；Synthetic oil can be polyalphaolefin, synthetic ester, polyethers, silicone oil, fluorine-containing oil, in phosphate any one or it is any
Combination；Vegetalitas base oil is the natural animal-plant grease in molecular structure containing ester bond.
Specific embodiment is as follows:
Embodiment one:
Melt phase polycondensation:
It accurately weighs hydroperoxides catalyst (II) and (chooses hydrogen peroxide, isopropyl benzene hydroperoxide, tert-butyl hydroperoxide
One of hydrogen), and be dissolved in solvent, obtain solution (A).Solution (A) is equably sprayed into bipolymer (ethylene-propylene
Block copolymer) the middle stirring of pellet (B), a period of time is stood after solvent volatilizees completely, obtains mixture (C)；Mixing is changed
Property material (C) squeezed out on extruder, control extrusion temperature is 150 DEG C, in extruder bringing-up section or end be added dropwise it is modified single
The mixture (D) that body (III) trimethylolpropane trimethacrylate and auxiliary monomer (IV) styrene are formed obtains after extrusion
Star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition.
In dosage, standard is: according to mass fraction meter, 97.3 parts of the bipolymer (I), and catalyst (II)
0.2 part, 2.0 parts of modified monomer (III), 0.5 part of auxiliary monomer (IV).
The lubricating oil viscosity index improver composition formed in the embodiment is dissolved in 100 DEG C of movements with 10% concentration and glues
Degree is 5.1mm2100 DEG C of kinematic viscosity that (i.e. 10% concentration liquid glue, similarly hereinafter) is tested in the base oil of/s are 1401mm2/ s, shearing
Stability index SSI 24 (diesel fuel nozzle SSI), 6.0 mm of thickening ability2/s；The apparent viscosity index (VI) CCSI of low temperature up to 80 (-
Tested at 20 DEG C), high-temperature oxydation detergency is up to 3.5 grades (heat tubes).
Solution polymerization process:
Bipolymer (I) Ethylene-Propylene Block Copolymer is added in batches into the reactor for filling base oil (IV),
It controls temperature and is no more than 130 DEG C, start blender, dissolve bipolymer, quality of the bipolymer in base oil point
Number is being no more than 30%.Wherein base oil selects mineral oil, and mineral base oil main component includes alkane, cycloalkane, aromatic hydrocarbons, ring
Alkylaromatic hydrocarbon and oxygen-containing, nitrogen, sulphur organic compound.It is 5.0~160.0mm that base oil, which can be 40 DEG C of kinematic viscosity,2/ s and/
Or 100 DEG C of kinematic viscosity are 1.50~34.0mm2/s.165 DEG C are warming up to, and after reaction temperature is stablized, then to reaction kettle
Middle injection hydroperoxides catalyst (II) (hydrogen peroxide, isopropyl benzene hydroperoxide, tert-butyl hydroperoxide), by 30min
Reaction forms macromolecular radical so that bipolymer is degraded；Modified monomer (III) three is injected into reaction kettle again
Hydroxymethyl-propane triacrylate and auxiliary monomer (IV) styrene, persistently stir 10min, and macromolecular radical is made to cause more officials
Energy degree modified monomer reacts, and forms the lubricating oil viscosity index improver composition concentrated solution with hub-and-spoke configuration, cooling
Cooling discharging obtains certain density liquid concentration material.
In dosage, standard is: according to mass fraction meter, 97.3 parts of the bipolymer (I), and catalyst (II)
0.2 part, 2.0 parts of modified monomer (III), 0.5 part of auxiliary monomer (IV).The lubricating oil viscosity index formed in the embodiment improves
100 DEG C of kinematic viscosity of agent composition concentrated solution (10% liquid glue) are 1245mm2/ the s, (diesel fuel nozzle 30 of shear stability index 19
Recycle SSI), thickening ability 6.3mm2Up to 55 (measuring at -20 DEG C), high-temperature oxydation is clear by/s, the apparent viscosity index (VI) CCSI of low temperature
Net 3.5 grades of property (heat tube).
Embodiment two:
Embodiment two is based on embodiment one and modified monomer is changed to trimethylol-propane trimethacrylate, remaining behaviour
Make step and dosage requires such as embodiment one.
10% concentration liquid of the lubricating oil viscosity index improver composition (melt polymerization product) formed in the embodiment
100 DEG C of kinematic viscosity of glue are 1255mm2/ s, shear stability index 14 (diesel fuel nozzle 30 recycles SSI), thickening ability
6.2mm2/ s, the apparent viscosity index (VI) CCSI of low temperature at -20 DEG C up to 58 (measuring), and high-temperature oxydation detergency is up to 3.5 grades of (heat pipe oxygen
Change)；The lubricating oil viscosity index improver composition concentrated solution (polymerisation in solution product, 10% liquid glue) formed in the embodiment
100 DEG C of kinematic viscosity are 1263mm2/ s, shear stability index 16 (diesel fuel nozzle 30 recycles SSI), thickening ability 6.2mm2/ s,
The apparent viscosity index (VI) CCSI of low temperature at -20 DEG C up to 72 (measuring), and 3.5 grades of high-temperature oxydation detergency (heat tube).
In other embodiments, modified monomer can be trimethylol-propane trimethacrylate, ethoxylation
Trimethylolpropane trimethacrylate, pentaerythritol triacrylate, 3 (propoxyl group) glycerol triacrylates, three (2- hydroxyl second
Base) isocyanuric acid triacrylate, two (trimethylolpropane) tetraacrylates, pentaerythritol tetraacrylate, 4 (ethyoxyls)
Any one or more in pentaerythritol tetraacrylate, double pentaerythritol methacrylate.
Embodiment three:
Embodiment three is based on embodiment one and auxiliary monomer is changed to acrylamide, remaining operating procedure and dosage require ginseng
See embodiment one.
10% concentration liquid of the lubricating oil viscosity index improver composition (melt polymerization product) formed in the embodiment
100 DEG C of kinematic viscosity of glue are 1212mm2/ s, shear stability index 15 (diesel fuel nozzle 30 recycles SSI), thickening ability
5.7mm2/ s, the apparent viscosity index (VI) CCSI of low temperature are up to 67 (measuring at -20 DEG C), 3.5 grades of (heat pipe oxygen of high-temperature oxydation detergency
Change)；The lubricating oil viscosity index improver composition concentrated solution (polymerisation in solution product, 10% liquid glue) formed in the embodiment
100 DEG C of kinematic viscosity are 1243mm2/ s, shear stability index 15 (diesel fuel nozzle 30 recycles SSI), thickening ability 5.4mm2/
Up to 69 (measuring at -20 DEG C), high-temperature oxydation detergency can reach 3.5 grades of (heat pipe oxygen by s, the apparent viscosity index (VI) CCSI of low temperature
Change).
In other embodiments, auxiliary monomer can be styrene, acrylamide, the thiuram for containing formula (φ) structure
Any one in derivative.
Example IV:
Melt phase polycondensation:
It accurately weighs in dialkyl class catalyst (II) (such as cumyl peroxide, di-t-butyl peroxide)
One kind, and be dissolved in solvent, obtain solution (A).Solution (A) is equably sprayed into bipolymer (ethylene-propylene random copolymerization
Object) the middle stirring of pellet (B), a period of time is stood after solvent volatilizees completely, obtains mixture (C)；Mixed and modified material (C) is passed through
It is squeezed out on extruder, control extrusion temperature is 300 DEG C, and in extruder bringing-up section or modified monomer (III) three is added dropwise in end
It is total to obtain the star-like binary second third after extrusion for hydroxymethyl-propane triacrylate and auxiliary monomer (VI) acrylamide
Polymers lubricating oil viscosity index improver composition.
In dosage, standard is: according to mass fraction meter, 96.4 parts of the bipolymer (I), and catalyst (II)
0.3 part, 3.0 parts of modified monomer (III), 0.3 part of auxiliary monomer (IV).
100 DEG C of concentrate (10% liquid glue) fortune of the lubricating oil viscosity index improver composition formed in the embodiment
Kinetic viscosity is 960mm2/ s, shear stability index 10 (diesel fuel nozzle 30 recycles SSI), thickening ability 4.9mm2/ s, low temperature are apparent
Viscosity index (VI) CCSI 84 (is measured) at -20 DEG C, and 3 grades of high-temperature oxydation detergency (heat tube).
Solution polymerization process:
Bipolymer (I) ethylene-propylene random copolymer is added in batches into the reactor for fill base oil, controls
Temperature is no more than 130 DEG C, starts blender, dissolves bipolymer, mass ratio of the bipolymer in base oil does not surpass
Cross 30%.Wherein base oil select synthetic base oil, synthetic oil can be polyalphaolefin, synthetic ester, polyethers, silicone oil, fluorine-containing oil,
Any one or more in phosphate.It is 5.0~160.0mm that base oil, which can be 40 DEG C of kinematic viscosity,2/ s and/or 100 DEG C
Kinematic viscosity is 1.50~34.0 mm2/s.300 DEG C are warming up to, and after reaction temperature is stablized, then injected into reaction kettle
Catalyst (II) dialkyl (such as cumyl peroxide, di-t-butyl peroxide), reacts by 20min, so that two
Membered copolymer is degraded, and macromolecular radical is formed；Modified monomer (III) trimethylolpropane is injected into reaction kettle again
Triacrylate and auxiliary monomer (IV) styrene, persistently stir 30min, so that macromolecular radical is caused polyfunctionality modified single
Body reacts, and forms the lubricating oil viscosity index improver composition concentrated solution with hub-and-spoke configuration, and cooling down discharging is
Obtain certain density liquid concentration material.
In dosage, standard is: according to mass fraction meter, 96.4 parts of the bipolymer (I), and catalyst (II)
0.3 part, 3.0 parts of modified monomer (III), 0.3 part of auxiliary monomer (IV).
100 DEG C of the lubricating oil viscosity index improver composition concentrated solution (10% liquid glue) formed in the embodiment movements are viscous
Degree is 1245mm2/ s, shear stability index 9 (diesel fuel nozzle 30 recycles SSI), thickening ability 4.8mm2/ s, low temperature apparent viscosity
Index CCSI at -20 DEG C up to 85 (measuring), and 3 grades of high-temperature oxydation detergency (heat tube).
Embodiment five:
Embodiment five is based on example IV and modified monomer is changed to trimethylol-propane trimethacrylate, remaining behaviour
Make step and dosage standard referring to example IV.
10% concentrate 130- kinematic viscosity of the lubricating oil viscosity index improver composition formed in the embodiment is
1212mm2/ s, shear stability index 12 (diesel fuel nozzle 30 recycles SSI), thickening ability 4.8mm2/ s, low temperature apparent viscosity refer to
Number CCSI at -20 DEG C up to 87 (measuring), and 3 grades of high-temperature oxydation detergency (heat tube).
Formed in the embodiment lubricating oil viscosity index improver composition concentrated solution (polymerisation in solution product, 10%
Liquid glue) 100 DEG C of kinematic viscosity are 920mm2/ s, shear stability index 12 (diesel fuel nozzle 30 recycles SSI), thickening ability
5.8mm2/ s, the apparent viscosity index (VI) CCSI of low temperature are reachable (measuring at -20 DEG C), and 3 grades of high-temperature oxydation detergency (heat tube).
In other embodiments, modified monomer can be trimethylol-propane trimethacrylate, ethoxylation
Trimethylolpropane trimethacrylate, pentaerythritol triacrylate, 3 (propoxyl group) glycerol triacrylates, three (2- hydroxyl second
Base) isocyanuric acid triacrylate, two (trimethylolpropane) tetraacrylates, pentaerythritol tetraacrylate, 4 (ethyoxyls)
Any one or more in pentaerythritol tetraacrylate, double pentaerythritol methacrylate.
Embodiment six:
Embodiment six is based on example IV and auxiliary monomer is changed to acrylamide, remaining operating procedure and dosage standard ginseng
See example IV.
Lubricating oil viscosity index improver composition (100 DEG C of the melt polymerization product movement viscosity formed in the embodiment
Kinematic viscosity is 1221mm2/ s, shear stability index 15 (diesel fuel nozzle 30 recycles SSI), thickening ability 6.1mm2/ s, low temperature
Apparent viscosity index CCSI at -20 DEG C up to 75 (measuring), and 3 grades of high-temperature oxydation detergency (heat tube).In the embodiment
100 DEG C of kinematic viscosity of lubricating oil viscosity index improver composition concentrated solution (polymerisation in solution product, 10% liquid glue) of formation are
1156mm2/ s, shear stability index 14 (diesel fuel nozzle 30 recycles SSI), thickening ability 5.8mm2/ s, low temperature apparent viscosity refer to
Number CCSI at -20 DEG C up to 88 (measuring), and 3 grades of high-temperature oxydation detergency (heat tube).
In other embodiments, auxiliary monomer can be styrene, acrylamide, the thiuram for containing formula (φ) structure
Any one in derivative.
Embodiment seven:
Melt phase polycondensation:
Peroxyesters catalyst (II) is accurately weighed (in peroxidized t-butyl perbenzoate, the peroxidating trimethylacetic acid tert-butyl ester
One kind), and be dissolved in solvent, obtain solution (A).Solution (A) is equably sprayed into the mixture pellet (B) of bipolymer
Middle stirring stands a period of time after solvent volatilizees completely, obtains mixture (C)；By mixed and modified material (C) through being squeezed on extruder
Out, control extrusion temperature is 250 DEG C, and in extruder bringing-up section or modified monomer (IV) trimethylolpropane tris is added dropwise in end
Acrylate and auxiliary monomer acrylamide obtain the star-like binary ethylene-propylene copolymer lubricating oil viscosity after extrusion and refer to
Number improver composition.
In dosage, standard is: according to mass fraction meter, 97.5 parts of the bipolymer (I), and catalyst (II)
0.2 part, 2.0 parts of modified monomer (III), 0.3 part of auxiliary monomer (IV).The lubricating oil viscosity index formed in the embodiment improves
10% liquid glue, 100 DEG C of kinematic viscosity of agent composition are 1031mm2/ s, (diesel fuel nozzle 30 recycles shear stability index 16
SSI), thickening ability 5.0mm2/ s, the apparent viscosity index (VI) CCSI of low temperature are up to 76 (measuring at -20 DEG C), high-temperature oxydation detergency 3
Grade (heat tube).
Solution polymerization process:
Bipolymer (I) hydrogenated polyisoprene is added in batches into the reactor for filling base oil (IV), controls
Temperature is no more than 130 DEG C, starts blender, dissolves bipolymer, mass ratio of the bipolymer in base oil does not surpass
Cross 30%.Wherein base oil selects vegetalitas base oil, and vegetalitas base oil is the natural dynamic plant in molecular structure containing ester bond
Object grease.It is 28.0~160.0mm that base oil, which can be 40 DEG C of kinematic viscosity,2/ s and/or 100 DEG C of kinematic viscosity is 1.50~
34.0mm2/s.212 DEG C are warming up to, and after reaction temperature is stablized, then injecting catalyst (II) peroxyester into reaction kettle
Class (peroxidized t-butyl perbenzoate, the peroxidating trimethylacetic acid tert-butyl ester) reacts (peroxidized t-butyl perbenzoate by 30/10min
When for initiator, reaction time 30min；When the peroxidating trimethylacetic acid tert-butyl ester is initiator, reaction time 10min), so that binary
Copolymer is degraded, and macromolecular radical is formed；Modified monomer (IV) trimethylolpropane tris third is injected into reaction kettle again
Olefin(e) acid ester and auxiliary monomer contain the thiuram derivative of formula (φ) structure, persistently stir 20min, cause macromolecular radical
Polyfunctionality modified monomer reacts, and being formed, there is the profit lubricating oil viscosity index improver composition of hub-and-spoke configuration to be concentrated
Liquid, cooling down discharging obtain certain density liquid concentration material.
In dosage, standard is: according to mass fraction meter, 96 parts of the bipolymer (I), and catalyst (II) 0.3
Part, 3.2 parts of modified monomer (III), 0.5 part of auxiliary monomer (IV).
100 DEG C of the lubricating oil viscosity index improver composition concentrated solution (10% liquid glue) formed in the embodiment movements are viscous
Degree is 1123mm2/ s, shear stability index 16 (diesel fuel nozzle 30 recycles SSI), thickening ability 5.2mm2/ s, low temperature apparently glue
Spend index CCSI up to 81 (measuring at -20 DEG C), 3.5 grades of high-temperature oxydation detergency (heat tube).
Embodiment eight:
Embodiment eight is based on embodiment seven and modified monomer is changed to trimethylol-propane trimethacrylate, remaining behaviour
Make step and dosage standard referring to embodiment seven.
The 100 DEG C of kinematic viscosity of lubricating oil viscosity index improver composition (melt polymerization product) formed in the embodiment
For 1134mm2/ s, shear stability index 13 (diesel fuel nozzle 30 recycles SSI), thickening ability 5.6mm2/ s, low temperature apparent viscosity
Index CCSI82 (is measured) at -20 DEG C, and 3 grades of high-temperature oxydation detergency (heat tube).
Formed in the embodiment lubricating oil viscosity index improver composition concentrated solution (polymerisation in solution product, 10%
Liquid glue) 100 DEG C of kinematic viscosity of kinematic viscosity be 1411mm2/ s, shear stability index 14 (diesel fuel nozzle 30 recycles SSI) are thick
Change ability 6.7mm2/ s, the apparent viscosity index (VI) CCSI of low temperature are up to 50 (measuring at -20 DEG C), 3 grades of (heat pipes of high-temperature oxydation detergency
Oxidation).
In other embodiments, modified monomer can be trimethylol-propane trimethacrylate, ethoxylation
Trimethylolpropane trimethacrylate, pentaerythritol triacrylate, 3 (propoxyl group) glycerol triacrylates, three (2- hydroxyl second
Base) isocyanuric acid triacrylate, two (trimethylolpropane) tetraacrylates, pentaerythritol tetraacrylate, 4 (ethyoxyls)
Any one or more in pentaerythritol tetraacrylate, double pentaerythritol methacrylate.
Embodiment nine:
Embodiment nine is based on embodiment seven and auxiliary monomer is changed in acrylamide, remaining operating procedure and dosage standard
Referring to embodiment seven.
The 100 DEG C of kinematic viscosity of lubricating oil viscosity index improver composition (melt polymerization product) formed in the embodiment
For 1282mm2/ s, shear stability index 18 (diesel fuel nozzle 30 recycles SSI), thickening ability 5.9mm2/ s, low temperature apparent viscosity
Index CCSI 69 (is measured) at -20 DEG C, and 3.5 grades of high-temperature oxydation detergency (heat tube).The profit formed in the embodiment
100 DEG C of kinematic viscosity of oil viscosity index improver composition concentrate (polymerisation in solution product, 10% liquid glue) are 887mm2/ s,
Shear stability index 13 (diesel fuel nozzle 30 recycles SSI), thickening ability 4.7mm2/ s, the apparent viscosity index (VI) CCSI 71 of low temperature
(being measured at -20 DEG C), 3 grades of high-temperature oxydation detergency (heat tube).
Prove through the foregoing embodiment as a result: the present invention is by being added catalyst (II), so that bipolymer is upper
Structural unit (β) is degraded, and (β) unit ratio is reduced on strand；Simultaneously as degradation is random, gained strand
Molecular weight distribution can be very wide.The addition sequence and dosage for further controlling catalyst (II) and modified monomer (III) make big
Molecular radical can react with modified monomer (III), form the star copolymer of long-chain branch, improve thickening ability；It is auxiliary
The use for helping monomer (IV) reduces the generation of irreversible crosslinking.
Strand is shunk the be formed by star-type polymer of the present invention at low temperature, but does not occur seriously to tangle, to viscosity
Influence it is smaller；Under high temperature, strand is unfolded, plus dosage significant to lubricating oil tackifying effect is reduced, in addition main carbochain and
(β) unit is reduced, and helps to improve shear stability.The more importantly molecule of the reduction of structural unit (β) ratio and strand
Amount distribution broadens, and the cryogenic property of gained VII is significant.The preparation method of the modified copolymer overcomes in polymerization process
Crosslinking problem, thickening ability, shear stability, cryogenic property, the high-temperature oxydation of the lubricating oil VII for preparing the modified copolymer
Detergency greatly improves.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. one kind contains star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition, it is characterised in that the group
Object is closed, melt polymerization is mainly passed through by bipolymer (I), catalyst (II), modified monomer (III), auxiliary monomer (IV)
The solid for the star-type polymer that method is prepared, or the liquid group of star-type polymer being prepared by solution polymerization process
Close object.
2. contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition as described in claim 1, it is special
Sign is that according to mass fraction meter, the bipolymer (I) is not less than 96 parts, and catalyst (II) is no more than 0.3 part, is modified
Monomer (III) is no more than 0.5 part no more than 3.2 parts, auxiliary monomer (IV).
3. contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition as described in claim 1, it is special
Sign is the linear copolymer that the bipolymer (I) is minimized by the crystallinity that unit (α) and unit (β) form,
Its number-average molecular weight is 2~500,000, and the formula of unit (α) and unit (β) is
4. contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition as described in claim 1, it is special
Sign is that the catalyst (II) is the organic compound containing formula (γ) structural unit, wherein R1 and R2 is respectively hydrogen atom
With any one in the alkyl of C1~12, naphthenic base, aryl, ketone group, carbonate group, ester group, acyl group or any combination；Formula (γ)
It is as follows:
5. contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition as described in claim 1, it is special
Sign is that the modified monomer (III) is the compound containing more than two (δ) or (ε) groups, the molecular formula of (δ) or (ε)
It is as follows:
6. contain star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition as described in claim 1, it is special
Sign is that the auxiliary monomer (IV) is any in styrene, acrylamide, the thiuram derivative containing formula (φ) structure
One kind, wherein R3 and R4 be the alkyl of C1~7, naphthenic base, aryl, benzyl, isobutyl group, in piperidyl any one or it is any
Combination, wherein formula (φ) structure is as follows:
7. a kind of melt polymerization process containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition, special
Sign be method includes the following steps:
Catalyst (II) is accurately weighed, and is dissolved in solvent, solution (A) is obtained；Solution (A) is equably sprayed into bipolymer
Stirring in pellet (B), stands, after solvent volatilizees completely, obtains mixture (C)；
Mixed and modified material (C) is squeezed out on extruder, control extrusion temperature is between 120-300 DEG C, in extruder bringing-up section
In or end the composition (D) that is mixed by modified monomer (III) and auxiliary monomer (IV) is added dropwise, obtained after extrusion described in
Star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition.
8. containing the melting of star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition as claimed in claim 7
Polymerization, it is characterised in that in the melt phase polycondensation, solvent used is energy catalyst-solvent but cannot dissolve binary
The solvent of copolymer (I) is any one of acetone, ethyl acetate, methanol, ethyl alcohol.
9. a kind of solution polymerization process containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition, special
Sign is the described method comprises the following steps:
(1) it is added in batches in the reactor of Xiang Shengyou base oil bipolymer (I), control temperature is no more than 130 DEG C, starts
Blender dissolves copolymer, and mass ratio of the copolymer in base oil is no more than 30%.
(2) it is warming up to 130 DEG C~300 DEG C, then injecting catalyst (II) into reaction kettle, is reacted by 1~30min, so that two
Membered copolymer is degraded, and macromolecular radical is formed；
(3) modified monomer (III) and auxiliary monomer (IV) are reinjected, persistently stirs 10-30min, cooling discharging is to get described in
Star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition.
10. molten containing star-like binary ethylene-propylene copolymer lubricating oil viscosity index improver composition as claimed in claim 9
Liquid polymerization, it is characterised in that the base oil be mineral base oil, synthetic base oil, vegetalitas base oil, base oil
40 DEG C of kinematic viscosity are 5.0~160.0mm2/ s or 100 DEG C of kinematic viscosity is 1.5~34.0mm2/s；The mineral base oil master
Wanting ingredient includes alkane, cycloalkane, aromatic hydrocarbons, naphthenic base aromatic hydrocarbons and oxygen-containing, nitrogen, sulphur organic compound；Synthetic oil is poly- α alkene
Hydrocarbon, synthetic ester, polyethers, silicone oil, fluorine-containing oil, any one or any combination in phosphate；Vegetalitas base oil is molecule knot
Natural animal-plant grease in structure containing ester bond.
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| PCT/CN2019/125749 WO2021027209A1 (en) | 2019-08-14 | 2019-12-16 | Composition containing star-shaped binary ethylene-propylene copolymer for improving lubricating oil viscosity index and preparation method thereof |
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