CN106478851B - High molecular weight molybdenum modified succinimides dispersing agent, preparation method and application - Google Patents
High molecular weight molybdenum modified succinimides dispersing agent, preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of high molecular weight molybdenum modified succinimides dispersing agent, preparation method and applications.The preparation method includes: at least by Ashless butyl diimide dispersant, addition may be selected or the solvent and molybdenum reagent not added mixing carry out one section of molybdenumization reaction, then possible remaining unreacted reactant is removed, then carries out two sections of molybdenumizations reactions, last post-treated acquisition target product.Preparation process of the present invention is simple and fast, mild condition, it is low in cost, high production efficiency, obtained product performance is stablized, act not only as the extreme pressure anti-wear additives of function admirable, friction improver uses, also act as Viscosity Index modifying agent etc., and it with alkylated diphenylamine class antioxidant there is obvious high temperature to cooperate with antioxidation in lubricating oil, have with zinc dialkyl dithiophosphate and well cooperates with antiwear and antifriction effect, similar additive can be reduced and add dosage in lubricating oil, to reduce the phosphorus content in lubricating oil product, be conducive to improve whole fuel economy.
Description
Technical field
The present invention relates to a kind of molybdate compound lubriation material and preparation method thereof, in particular to a kind of high molecular weight molybdenum changes
Property dispersing agent, preparation method and application.
Background technique
The development trend of automobile engine oil is to extend the drain period and improve fuel economy, and improve the master of fuel economy
Wanting approach is to reduce oil viscosity and reduce the frictional dissipation between parts, and this requires lubricating oil to have excellent antifriction antiwear
Performance.
In order to improve the antifriction antiwear effect of lubricating oil, a small amount of lube oil additive is usually added in lubricating oil, is passed
The lube oil additive of system is sulphur, phosphorus and chlorine type, and this kind of material can have selectivity and corrosivity to surface of friction pair, especially
The lube oil additive of the elements such as sulfur-bearing, phosphorus or chlorine can discharge a large amount of waste water, exhaust gas and pollution in the production and use process
Object pollutes the environment.
Molybdate compound lubriation material occupies extremely important because of its excellent tribological property in numerous lubriation materials
Status, be one of the hot spot of domestic and international lube oil additive research in recent years.Existing molybdate compound additive is mainly
Oil-soluble organo-molybdenum compound, after being added in lubricating oil, in greasing, organic molybdenum is thermal decomposited simultaneously
The molybdenum disulfide of ultra-fine or approximate nanometer is generated, this molybdenum disulfide adheres to surface of friction pair, fills out coarse surface "
It is flat " and become smooth.Therefore, oil-soluble organo-molybdenum compound is as extreme pressure anti-wear additives and friction improver, in lubricating oil and profit
The friction and wear of slidingsurface can be reduced in consistent lubricant, improves load-carrying ability, while also there is fabulous collaboration oxidation resistance,
Capable of saving fuel 3%~4%.
Common are machine molybdenum compound additive is broadly divided into molybdenum dialkyl-dithiophosphate (MoDDP), dialkyl group at present
Molybdenum dithiocarbamate (MoDTC), three core molybdenums and molybdenum amine compounds etc., these products are mainly used in I. C. engine
Among lubricating oil, gear oil, hydraulic oil, intermetallic composite coating and lubricating grease.
Molybdenum modified succinimides dispersing agent is the novel molybdate compound lubriation material of one kind developed in recent years.
For example, USP8076275B2 describes a kind of molybdenum modifiers dispersants, mainly with multiple types (mono-/bis-succimide
Type) ashless dispersant reacts to be formed as basic nitrogen compound and molybdenum trioxide and water etc..USP20120190864A1 is also illustrated
A kind of molybdenum modifiers dispersants, the ashless dispersant for being mainly 500~5000 using side chain molecular weight as basic nitrogen compound and
Acrylic acid, molybdenum trioxide and water reaction obtain.USP20130261313A1 also depicts a kind of molybdenum modifiers dispersants, is mainly
Selecting side chain is the ashless dispersant of C12-C30 as basic nitrogen compound, reacts acquisition with acrylic acid, molybdenum trioxide and water.
Exist as follows not however, the revealed molybdenum modified succinimides dispersing agent synthesis technology of these documents is substantially all
Foot, comprising: first, the reaction time is long, generally more than 24 hours, energy consumption is high, high production cost；Second, synthesized molybdenum is modified
Succinimide dispersant molecular weight is lower, and function is less.
Summary of the invention
In view of the deficiencies of the prior art, it is a primary object of the present invention to propose that a kind of modified succinyl of high molecular weight molybdenum is sub-
Amine dispersant and preparation method thereof.
Another free-revving engine of the invention is to provide the application of the high molecular weight molybdenum modified succinimides dispersing agent.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
A kind of preparation method of high molecular weight molybdenum modified succinimides dispersing agent is provided among some embodiments,
Comprising: which addition may be selected or the solvent and molybdenum reagent not added mixing carry out one section of molybdenum at least by ashless dispersant
Then reaction removes possible remaining unreacted reactant, then carry out two sections of molybdenumizations reactions, last post-treated acquisition target product.
Among some more preferred embodiments, the preparation method may include: by ashless dispersant with it is molten
Agent is uniformly mixed under conditions of temperature≤100 DEG C, then molybdenum reagent is added under conditions of temperature≤120 DEG C and may be selected to add
The promotor for adding or not adding is stirred to react under conditions of temperature≤150 DEG C reacts no more than 0.5h, then temperature rising reflux later
No more than 10h, possible remaining unreacted reactant, then the constant temperature under conditions of temperature≤200 DEG C at reduced pressure conditions are then removed
It is kept for no more 5h, last post-treated acquisition target product.
More preferred, the ashless dispersant is selected from the ashless dispersant containing basic nitrogen.
More preferred, the promotor includes C1-C13Monohydric alcohol and/or polyalcohol, water in any one or two
Kind or more combination.
More preferred, the solvent is selected from the low polar solvent that boiling range is 60~200 DEG C.
It additionally provides in some embodiments sub- by the modified succinyl of high molecular weight molybdenum of aforementioned any method preparation
Amine dispersant, weight average molecular weight Mw >=1.9 × 104, molybdenum content is 0.01~6.91wt%.
The purposes of the high molecular weight molybdenum modified succinimides dispersing agent is additionally provided among some embodiments.
For example, providing a kind of lubricant oil composite in some case study on implementation, it includes the high molecular weight molybdenums to change
Property succinimide dispersant.
Further, in some embodiments, the lubricant oil composite also may include other multiple additives.
Compared with prior art, the invention has the advantages that
(1) in preparation method of the invention, by the screening and technological operation of raw material and the adjustment of process conditions, substantially
Reaction rate is improved, the reaction time foreshortens to 4~10h；
(2) further, the present invention is by selecting polyisobutene succinimide dispersing agent as raw material, and is aided with technique
Operation and the optimization of condition, enable molybdenum during molybdenum to connect multiple isobutene succimide molecules, to can get weight
Average molecular weight is more than 1.9 × 104High molecular weight molybdenum modified succinimides dispersing agent, so that it is acted not only as function admirable
Extreme pressure anti-wear additives, friction improver use, also act as Viscosity Index modifying agent；
(3) high molecular weight molybdenum modified succinimides ashless dispersant of the invention in lubricating oil with alkylated diphenylamine
There is class antioxidant apparent high temperature to cooperate with antioxidation, and has with zinc dialkyl dithiophosphate and cooperate with well
Antiwear and antifriction effect, therefore can be reduced when being applied in lubricating oil and add dosage similar to additive, to reduce lubricating oil
Phosphorus content in product is conducive to improve whole fuel economy.
More detailed explanation will hereafter be made to technical solution of the present invention.It is understood, however, that in model of the present invention
In enclosing, above-mentioned each technical characteristic of the invention and it is ok between each technical characteristic specifically described in below (e.g. embodiment)
It is combined with each other, to form a new or preferred technical solution.Due to space limitations, I will not repeat them here.
Detailed description of the invention
Fig. 1 is mill spot photo of the obtained oil-soluble molybdenum modifiers dispersants of embodiment 1 in endurance check；
Fig. 2 is SEM-EDS energy spectrum diagram of the obtained oil-soluble molybdenum modifiers dispersants of embodiment 1 in endurance check.
Specific embodiment
As previously mentioned, in view of many deficiencies of the prior art, inventor's in-depth study and a large amount of by long-term
Practice is able to propose technical solution of the present invention, as detailed below.
One aspect of the present invention provides a kind of preparation method of high molecular weight molybdenum modified succinimides dispersing agent, packet
Include three phases: one section of molybdenum, pretreatment, two sections of molybdenumization reactions.
Specifically, the preparation method include: at least by ashless dispersant, may be selected addition or the solvent not added and
The mixing of molybdenum reagent carries out one section of molybdenumization reaction, then removes possible remaining unreacted reactant, then carries out two sections of molybdenumization reactions, most
Target product is obtained by post-processing.
Among some more preferred embodiments, the preparation method may include: by ashless dispersant with it is molten
Agent is uniformly mixed under conditions of temperature≤100 DEG C, then molybdenum reagent is added under conditions of temperature≤120 DEG C and may be selected to add
The promotor for adding or not adding is stirred to react under conditions of temperature≤150 DEG C reacts no more than 0.5h, then temperature rising reflux later
No more than 10h, possible remaining unreacted reactant, then the constant temperature under conditions of temperature≤200 DEG C at reduced pressure conditions are then removed
It is kept for no more 5h, last post-treated acquisition target product.
Among some highly preferred embodiments, the preparation method may include: by ashless dispersant with it is molten
Agent is uniformly mixed under conditions of 100 DEG C of temperature <, then molybdenum reagent is added under conditions of 120 DEG C of temperature < and may be selected to add
The promotor for adding or not adding is stirred to react under conditions of 150 DEG C of temperature < reacts no more than 0.5h, then temperature rising reflux later
No more than 10h, possible remaining unreacted reactant, then the constant temperature under conditions of 200 DEG C of temperature < at reduced pressure conditions are then removed
It is kept for no more 5h, last post-treated acquisition target product.
Among some more specifically embodiments, which may include: that ashless dispersant and solvent exist
Temperature is sufficiently mixed uniformly under conditions of being 30~100 DEG C, and molybdenum reagent is added under conditions of temperature is 50~120 DEG C later
With optional addition or the promotor not added, 0.2~0.5h is then reacted under conditions of temperature is 60~150 DEG C, then rise
Then warm 4~10h of back flow reaction removes remained unreacted object, then at reduced pressure conditions under conditions of temperature is 99~200 DEG C
Constant temperature keeps 0.5~5h, last post-treated acquisition target product.
It is further preferred that the preparation method includes: the condition for being 50~80 DEG C in temperature by ashless dispersant and solvent
Lower stirring is no more than 0.5h, and molybdenum reagent is added under conditions of temperature is 60~100 DEG C later and addition may be selected or do not add
The promotor added then reacts 0.2~0.5h under conditions of temperature is 60~110 DEG C, then temperature rising reflux reacts 4~9h, so
Remove afterwards may remaining unreacted reactant, then under conditions of being at reduced pressure conditions 120~155 DEG C in temperature constant temperature keep 2~
5h, last post-treated acquisition target product.
It is further preferred that the reduced pressure refers to vacuum degree >=4KPa condition.
Further, the post-processing includes the water and solvent after removing two sections of molybdenumization reactions in obtained reaction product.
For example, among a more typical concrete case, a kind of preparation method may include: by the ashless dispersants of metering
Agent and solvent mixing, optimize Mo/N and Mo/H2The molybdenum reagent of metering is added in the ratio of O, 100 DEG C of < 120 DEG C of stirring 0.5h, <
And promotor, mixture is in 150 DEG C of stirring 0.5h of <, and then temperature rising reflux reacts < 10h again, and it is remaining not to be filtered to remove possibility
Reactant, under conditions of vacuum degree >=4KPa, constant temperature keeps < 5h under the conditions of 200 DEG C of <, removes solvent and water, can be obtained
Target product.
The definition of heretofore described ashless dispersant, molybdenum reagent and promotor be those skilled in the art
Know.
More preferred, the ashless dispersant uses the ashless dispersant containing basic nitrogen.
More preferably, the ashless dispersant can be different selected from but not limited to single polyisobutene succinimide, double focusing
Butylene succimide etc..
It is further preferred that the number-average molecular weight of polyisobutylene group is 500~5000 in the ashless dispersant.
More preferred, the molar ratio for the nitrogen that the dosage of the molybdenum reagent contains with the ashless dispersant is
1:0.1~1:10.
More preferred, the molybdenum reagent can be selected from molybdate compound, such as preferably certainly but be not limited to titanium dioxide
One of molybdenum, molybdenum trioxide, two water, 13 ammonium thiomolybdate, four thio ammonium molybdate, sodium molybdate, ammonium molybdate, molybdic acid are more
Kind.
More preferred, the promotor can be C1-C13Monohydric alcohol and/or polyalcohol and deionized water in it is any
One or more kinds of combinations, can accelerate two phase reaction rate.
Further, the alcohol preferably from but be not limited to methanol, ethyl alcohol, propyl alcohol, n-butanol, isobutanol, isoamyl alcohol, just
Octanol, isooctanol, ethylene glycol, cyclohexanol, cyclopentanol, the tert-butyl alcohol, any one or a variety of combinations in sec-amyl alcohol.
It is further preferred that the mass ratio of the promotor and the molybdenum reagent is 0.5~3:1.
More preferred, the solvent can be selected from the low polar solvent that boiling range is 60~200 DEG C, and particularly preferred boiling range is 65
~120 DEG C of low polar solvent, for example, can selected from but not limited to one of n-hexane, petroleum ether, toluene, dimethylbenzene or
A variety of mixtures.
It is more preferred, the solvent usage account for used reaction mass total weight among the preparation method 1/3~
2。
Another aspect of the present invention, which provides a kind of high molecular weight molybdenum modified succinimides dispersing agent, (hereafter can also claim
For oil-soluble molybdenum modifiers dispersants), at room temperature it is blackish green thick liquid, there is good oil-soluble.
Further, the molybdenum content of the high molecular weight molybdenum modified succinimides dispersing agent reach 0.01~
6.91wt%.
Further, weight average molecular weight Mw >=1.9 × 10 of the high molecular weight molybdenum modified succinimides dispersing agent4。
Further, the high molecular weight molybdenum modified succinimides dispersing agent can more than half a year room temperature storage, and nothing
Precipitation.
Another aspect of the invention provides the purposes of the high molecular weight molybdenum modified succinimides dispersing agent.
It, can be by the high molecular weight molybdenum modified succinimides dispersing agent and more for example, among some case study on implementation
Kind additive compound, formulated oil composition.
Thus, the present invention also provides a kind of lubricant oil composites, and it includes the modified succinyl of the high molecular weight molybdenum
Imine dispersants.
Further, among some embodiments, the lubricant oil composite also may include other multiple additives.
For example, the additive can be alkylated diphenylamine class antioxidant.Also, the high molecular weight molybdenum is modified
Succinimide dispersant has with alkylated diphenylamine class antioxidant cooperates with antioxidation well.
For example, the additive can be zinc dialkyl dithiophosphate.Also, the modified fourth two of the high molecular weight molybdenum
Acid imide dispersing agent and zinc dialkyl dithiophosphate have cooperates with antiwear and antifriction effect well, immediate cause may be
Contact surface forms molybdenum disulfide.
Further, the lubricant oil composite also may include one of following component or a variety of, such as lubrication oil base
Plinth oil, detersive, antiwear additive, viscosity index improver, pour-point depressant, corrosion inhibitor, antirust agent, anti-foaming agent, supplement are rubbed
Wipe or mixtures thereof modifier.
Technical solution of the present invention will be described in detail in conjunction with several embodiments as follows, but these embodiments are to pass through
Expand invention rather than limits what the mode invented proposed.
The preparation process of some high molecular weight molybdenum modified succinimides dispersing agents is related among following examples,
Employed in various reaction partners and process conditions be more typical example, but pass through inventor's a large number of experiments
Verifying, is also applicable, and also reachable in the other types of reaction partner of those listed above and other process conditions
The technical effect claimed at the present invention.If not " % " addressed in following examples is " wt% " in addition, illustrating.
Embodiment 1 is by mono butonediimide ashless dispersant agent (mono butonediimide ashless dispersant agent Mw=4002, poly- isobutyl
Alkene Mn=1300, base number=50.49mg KOH/g) 20g and toluene 40g launch into reaction flask, stir at 30~100 DEG C
0.5h, in 50~100 DEG C of addition molybdenum trioxide 2.23g, 3.86g distilled water, mixture connects in 50 DEG C~100 DEG C stirring 0.5h
Again temperature rising reflux react 4~10h.It is filtered to remove remained unreacted object, finally under conditions of vacuum degree >=4KPa, 120
DEG C~200 DEG C under the conditions of constant temperature keep 2~5h, to remove toluene and water, obtained the modified fourth of high molecular weight molybdenum of Mw=42327
Imidodicarbonic diamide dispersing agent M1, molybdenum content 6.91wt%, product storage was without sedimentation time > 6 months.
Embodiment 2 is by double Ashless butyl diimide dispersants (double Ashless butyl diimide dispersant Mw=6537, poly- isobutyl
Alkene Mn=1000, base number=22.62mg KOH/g) 20g and dimethylbenzene 40g launch into reaction flask, stir at 30 DEG C~100 DEG C
0.5h is mixed, in 50 DEG C~100 DEG C addition molybdenum trioxide 1.22g, 2.09g distilled water, mixture is stirred at 50 DEG C~100 DEG C
0.5h, then temperature rising reflux reacts 4~10h again.It is filtered to remove remained unreacted object, finally in vacuum degree >=4KPa condition
Under, constant temperature keeps 2~5h under the conditions of 120 DEG C~200 DEG C, to remove removal xylene and water, has obtained the high score of Mw=19503
Son amount molybdenum modified succinimides dispersing agent M2, molybdenum content 3.15%, the product are stored without sedimentation time > 6 months.
Embodiment 3 is by mono butonediimide ashless dispersant agent (mono butonediimide ashless dispersant agent Mw=7845, poly- isobutyl
Alkene Mn=2300, base number=20.91mg KOH/g) 20g and petroleum ether 60g launch into reaction flask, stir at 30 DEG C~100 DEG C
0.5h is mixed, in 50 DEG C~100 DEG C addition molybdenum dioxide 1.09g, 3.27g distilled water, mixture is in 60 DEG C of stirring 0.5h, then again
Temperature rising reflux reacts 4~10h.It is filtered to remove remained unreacted object, finally under conditions of vacuum degree >=4KPa, in 155 DEG C of items
Constant temperature keeps 2~5h to obtain the high molecular weight molybdenum modified succinimides of Mw=26755 to remove petroleum ether and water under part
Dispersing agent M3, molybdenum content 2.35%, the product are stored without sedimentation time > 6 months.
Embodiment 4 is by double Ashless butyl diimide dispersants (double Ashless butyl diimide dispersant Mw=4817, poly- isobutyl
Alkene Mn=2300, base number=44.18mg KOH/g) 20g and dimethylbenzene and hexane mixture 50g (mass ratio 1:1) dispensing arrive
In reaction flask, in 30 DEG C~100 DEG C stirring 0.5h, in 50 DEG C of addition four thio ammonium molybdate 2.19g, 1.09g distilled water, mixture
In 100 DEG C of stirring 0.5h, then temperature rising reflux reacts 4~10h again.Be filtered to remove remained unreacted object, finally vacuum degree >=
Under conditions of 4KPa, constant temperature keeps 2~5h under the conditions of 120 DEG C~200 DEG C, to remove removal xylene, n-hexane and water, obtains
The high molecular weight molybdenum modified succinimides dispersing agent M4 of Mw=30703, molybdenum content 5.98%, when product storage is without precipitating
Between > 6 months.
Embodiment 5 is by mono butonediimide ashless dispersant agent (mono butonediimide ashless dispersant agent Mw=4002, poly- isobutyl
Alkene Mn=1300, base number=50.49mg KOH/g) 20g and toluene 20g launch into reaction flask, 30~100 DEG C of stirring 0.5h,
50~100 DEG C of addition ammonium molybdate 1.22g, 3.66g distilled water and n-butanol mixture (mass ratio 1:1), mixture is 50~100
DEG C stirring 0.5h, then again temperature rising reflux react 2~10h, pretreatment, remaining unreacted reactant is filtered to remove, finally in vacuum
Under conditions of degree >=4kPa, constant temperature keeps 2~5h under the conditions of 120 DEG C~200 DEG C, removes toluene and water, obtains the modified fourth two of molybdenum
Acid imide dispersing agent M5, molybdenum content 4.63%, the product are stored without sedimentation time > 6 months.
Embodiment 6 is by mono butonediimide ashless dispersant agent (mono butonediimide ashless dispersant agent Mw=4002, poly- isobutyl
Alkene Mn=1300, base number=50.49mg KOH/g, N%=2.17%) 20g and dimethylbenzene 20g launch into reaction flask, 30~
100 DEG C of stirring 0.5h, 50~100 DEG C of addition ammonium molybdate 12.2g, 6.1g distilled water and carbinol mixture (mass ratio 1:1), mixing
Object is in 50~100 DEG C of stirring 0.5h, and then temperature rising reflux reacts 2~10h again, and pretreatment is filtered to remove remaining unreacted reactant,
Finally under conditions of vacuum degree >=4kPa, constant temperature keeps 2~5h under the conditions of 120 DEG C~200 DEG C, removes removal xylene and water, obtains
To molybdenum modified succinimides dispersing agent M6, molybdenum content 5.37%, which is stored without sedimentation time > 6 months.
Also anti-oxidant and antiwear and friction reduction property is carried out to the performance of the obtained dispersing agent M1 of embodiment 1 as follows to test, wherein
The additive sample of certain mass is is dissolved in the oil sample configured in base oil 150N by the experiment oil sample used.
Antioxygenic property tests (PDSC method): executing (3.5 ± 0.2MPa of pressure, flow velocity according to SH/T 0719-2002
100 ± 10mL/min), test result is shown in Table 1.
Antiwear and friction reduction property test (four ball frictional testing machines): according to SH/T 0189-92 execute (revolving speed 1200rpm ±
60rpm, 75 DEG C ± 2 DEG C of temperature, time 60min ± 1min), test result is shown in Table 2.
Table 1: anti-oxidant (PDSC method) result of the collaboration of 1 dispersing agent M1 of embodiment
Table 2: 1 dispersing agent M1 of embodiment cooperates with four ball test result of antifriction antiwear with zinc dialkyl dithiophosphate
The SEM-EDS test result that Fig. 2 is 1 dispersing agent M1 of embodiment is please referred to again, from SEM-EDS energy spectrum analysis it is found that S
Distribution height overlapping with Mo on mill spot surface, and it is distributed more widely, illustrate after the test of four balls, S shape in conjunction with Mo atom
At a large amount of molybdenum disulfide, this may be also that dispersing agent M1 has the main reason for preferable antifriction antiwear.
In summary, oil-soluble molybdenum modifiers dispersants of the invention in lubricating oil with alkylated diphenylamine class antioxidant
Antioxidation is cooperateed with apparent high temperature, has with zinc dialkyl dithiophosphate and cooperates with antiwear and antifriction effect well,
So present invention use in lubricating oil can reduce similar to additive plus dosage, so that the phosphorus reduced in lubricating oil product contains
Amount is conducive to improve whole fuel economy.
The above is only part preferred embodiment of the invention, it is noted that for the ordinary skill people of the art
Member, without departing from the principle of the present invention, can also make several variations in detail, these variations in detail also should be regarded as this hair
Bright protection scope.
Claims (10)
1. a kind of preparation method of high molecular weight molybdenum modified succinimides dispersing agent, characterized by comprising: at least by fourth two
Acid imide ashless dispersant, may be selected addition or the solvent and molybdenum reagent not added mixing carry out one section of molybdenumization reaction, so
Possible remaining unreacted reactant is removed afterwards, then carries out two sections of molybdenumizations reactions, last post-treated acquisition target product.
2. preparation method according to claim 1, it is characterised in that:
The preparation method include: ashless dispersant is uniformly mixed under conditions of temperature≤100 DEG C with solvent, then temperature≤
The promotor that molybdenum reagent is added under conditions of 120 DEG C and addition may be selected or do not add, later in the condition of temperature≤150 DEG C
Under be stirred to react no more than 0.5h, then temperature rising reflux reaction is no more than 10h, then remove may remaining unreacted reactant, then
Constant temperature is kept for no more 5h under conditions of temperature≤200 DEG C under reduced pressure, last post-treated acquisition target product；
Preferably, which includes: and is uniformly mixed ashless dispersant under conditions of 100 DEG C of temperature < with solvent, then
The promotor that molybdenum reagent is added under conditions of 120 DEG C of temperature < and addition may be selected or do not add, later in temperature < 150
It is stirred to react under conditions of DEG C and is no more than 10h no more than 0.5h, then temperature rising reflux reaction, then removing may remaining unreacted
Object, then constant temperature is kept for no more 5h under conditions of 200 DEG C of temperature < at reduced pressure conditions, last post-treated acquisition target produces
Object；
Preferably, which includes: to be sufficiently mixed ashless dispersant and solvent under conditions of temperature is 30~100 DEG C
Uniformly, the promotor for molybdenum reagent being added under conditions of temperature is 50~120 DEG C later and addition may be selected or do not add, and
0.2~0.5h is reacted under conditions of temperature is 60~150 DEG C afterwards, then temperature rising reflux reacts 4~10h, then removes residual not
Reactant, then constant temperature keeps 0.5~5h under conditions of being at reduced pressure conditions 99~200 DEG C in temperature, it is last post-treated to obtain
Obtain target product；
It is further preferred that the preparation method includes: to stir ashless dispersant and solvent under conditions of temperature is 50~80 DEG C
It mixes and is no more than 0.5h, molybdenum reagent is added under conditions of temperature is 60~100 DEG C later and addition may be selected or do not add
Promotor then reacts 0.2~0.5h under conditions of temperature is 60~110 DEG C, then temperature rising reflux reacts 4~9h, then removes
Go may remaining unreacted reactant, then constant temperature keeps 2~5h under conditions of being at reduced pressure conditions 120~155 DEG C in temperature, most
Target product is obtained by post-processing；
Still more preferably, the reduced pressure refers to vacuum degree >=4KPa condition.
3. preparation method described in any one of -2 according to claim 1, it is characterised in that:
The ashless dispersant is selected from the ashless dispersant containing basic nitrogen；
Preferably, the ashless dispersant includes single polyisobutene succinimide and/or double polyisobutene succinimides；
It is further preferred that the number-average molecular weight of polyisobutylene group is 500~5000 in the ashless dispersant.
4. preparation method according to any one of claim 1-3, it is characterised in that the dosage of the molybdenum reagent and institute
Stating the molar ratio between the nitrogen that ashless dispersant contains is 1:0.1~1:10.
5. preparation method described in any one of -4 according to claim 1, it is characterised in that the molybdenum reagent, which is selected from, contains molybdenum
Object is closed, the molybdate compound includes molybdenum dioxide, molybdenum trioxide, two water, 13 ammonium thiomolybdate, four thio ammonium molybdate, molybdic acid
Sodium, ammonium molybdate, any one or two or more combinations in molybdic acid.
6. the preparation method according to any one of claim 2-5, it is characterised in that:
The promotor includes C1-C13Monohydric alcohol and/or polyalcohol and deionized water in any one or it is two or more
Combined mixture, the alcohol includes methanol, ethyl alcohol, propyl alcohol, n-butanol, isobutanol, isoamyl alcohol, n-octyl alcohol, isooctanol, second
Glycol, cyclohexanol, cyclopentanol, the tert-butyl alcohol, any one or two or more combinations in sec-amyl alcohol；
Preferably, the mass ratio of the promotor and the molybdenum reagent is 0.5:1~3:1.
7. preparation method according to claim 1 to 6, it is characterised in that:
The solvent is selected from the low polar solvent that boiling range is 60~200 DEG C；
Preferably, the solvent is selected from the low polar solvent that boiling range is 65~120 DEG C；
It is further preferred that the solvent include in n-hexane, petroleum ether, toluene or dimethylbenzene any one or it is two or more
Combination；
It is further preferred that the dosage of the solvent is 1/3~2 of reaction mass total weight employed in the preparation method.
8. the high molecular weight molybdenum modified succinimides dispersing agent prepared by any one of claim 1-7 the method, heavy
Average molecular weight Mw >=1.9 × 104, molybdenum content is 0.01~6.91wt%.
9. a kind of lubricant oil composite, it is characterised in that include high molecular weight molybdenum modified succinimides according to any one of claims 8
Dispersing agent.
10. lubricant oil composite according to claim 9, it is characterised in that also include alkylated diphenylamine class antioxidant
And/or zinc dialkyl dithiophosphate.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050209111A1 (en) * | 2002-05-31 | 2005-09-22 | Chevron Oronite Company Llc | Reduced color molybdenum-containing composition and a method of making same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050209111A1 (en) * | 2002-05-31 | 2005-09-22 | Chevron Oronite Company Llc | Reduced color molybdenum-containing composition and a method of making same |
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