CN104059717B - Antioxidant composition, lubricant oil composite and the method for improving lubricating oil antioxygen property - Google Patents
Antioxidant composition, lubricant oil composite and the method for improving lubricating oil antioxygen property Download PDFInfo
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Abstract
The present invention provides a kind of antioxidant composition, the lubricant oil composite including the antioxidant composition and the methods for improving lubricating oil antioxygen property.Antioxidant composition of the invention includes alkylated diphenylamine, phenthazine and vulcanization hindered phenol.It is antioxidant composition and lubricant oil composite low-sulfur provided by the invention, low ash, without phosphorus, high warm volatilization loss is few, it can significantly improve oxidation stability of lubricating oil under the conditions of hot conditions and metal ion catalysis, the service life for effectively extending lubricating oil, meets the requirement of allotment top-grade lubricating oil.
Description
Technical field
The present invention relates to a kind of antioxidant composition, in particular to a kind of antioxidant composition suitable for lubricating oil.
Background technique
Lubricating oil will be subjected to examining for harsh working environment in the use process in the fields such as internal combustion engine, automatic transfer equipment
It tests.Lubricating oil eventually forms coke, colloid, asphalitine and acidity by chemical changes such as a series of oxidation, polymerization, decomposition
Substance etc., and then a series of negative consequences are generated, such as viscosity and acid value increase, generate paint film or greasy filth, engine bearing burn into
Piston glues ring etc., and the serious properties for damaging lubricating oil shorten the working life, so that the normal work of engine is influenced,
Machine can even be damaged.Good oxidation stability is a Key Performance Indicator of lubricating oil.
For a long time, zinc dialkyl dithiophosphate (ZDDP) be a kind of antioxygen widely used in lubricating oil field,
Anti- rotten, wear-resistant multipurpose additive, it can not only remove free radical, moreover it is possible to which hydroperoxides are decomposed into more stable chemical combination
Object, avoids a large amount of formation of free radical, to extend the service life of lubricating oil.But ZDDP provides more metal member
Element, and be the main source of phosphorus in lubricating oil, element sulphur.With the raising of environmental requirement, greatly develop protosulfate ash content,
Low-phosphorous, low sulfur lubricating oil has become an inexorable trend in top-grade lubricating oil research field.This just needs crankcase lubrication
Oil should have low-down phosphorus content, and therefore, usage amount of traditional antioxidant ZDDP in high-grade I. C. engine oil is strictly limited
System.
Therefore, in order to reduce P, S constituent content in lubricating oil, people continuously attempt to develop low-phosphorous, low-sulfur even without phosphorus, nothing
The antioxidant system of sulphur meets the requirement of top-grade lubricating oil.If patent US5167844 discloses a kind of lubricant oil composite, the group
Polymer component includes dialkyl dithiophosphate (ester), diphenylamines or phenthazine, hindered amine and hindered phenol, to improve lubrication
The oxidation of oil is stable.Patent GB1360981 discloses a kind of lubricant oil composite, and the composition includes by phosphorodithioate zinc
Or the antioxidant ingredients that phosphorodithioate, alkylated diphenylamine or phenthazine and hindered phenol are constituted.Patent
US5091099 discloses a kind of lubricating oil compound being made of arylamine and hindered phenol, wherein amine: phenol=2:1~6:1, can be with
Oil product aging is prevented, the formation of black greasy filth is effectively controlled.Patent EP2173803 discloses one kind by octylated/butylated two
The anti-oxidant compositions of aniline, phenthazine and (3,5- di-t-butyl -4- hydroxyphenyl) propionic acid stearyl composition, Ke Yiyou
Effect improves the oxidation stability of polyurethane high molecule material.
Although the lubricant oil composite in above-mentioned document joined other antioxidants or use other antioxidants, from
And reduce the content of P, S in lubricating oil.But due to the metal component in mechanical equipment and engine component formed it is miscellaneous
Matter, and metal ion is formed under the action of lubricating oil acidic oxidation products.The ion of these transition metal can be catalyzed hydro carbons
The free radical chain initiation reaction of molecule and the homolytic decomposition of hydroperoxides drop to accelerate oil ageing degradation rate
The oxidation stability of low oil product.Moreover, engine develops towards small size, high-power direction, load increases, and operating temperature is gradually
It increases, which further improves the oxidizing reaction rate of lubricating oil itself, shortens its service life substantially.In addition, in high temperature
Under the conditions of, the hot volatilization loss for lubricating oil antioxidant increases, this will cause the further of the high-temperature oxidation stability of lubricating oil
It reduces.
Summary of the invention
The present invention provides a kind of antioxidant composition, the lubricant oil composite including the antioxidant composition and improve profit
The method of lubricating oil antioxygen property.
Antioxidant composition of the invention includes alkylated diphenylamine, phenthazine and vulcanization hindered phenol.
The structure of the alkylated diphenylamine are as follows:
Wherein R1、R2The alkyl of respectively H or C1~C20, the preferably alkyl of C2~C10, most preferably tert-butyl, iso-octyl
Or nonyl, R1And R2It is preferably placed at contraposition or the ortho position of amino.
The alkylated diphenylamine can select butyl/octyl mixing diphenylamines, such as German BASF Ciba company life
IRGANOX L57 of production, the production of Beijing Xing Pu company butyl/octyl diphenylamine T534, it is right, to '-di-iso-octyldiphenylamine,
Such as IRGANOX L01, the VANLUBE81 of Vanderbilt company of U.S. production, moral of German BASF Ciba company production
The RC7001 of Rhein Chemie Corporation of state production, dinonyldiphenylamine, such as Jinzhou Huifa Tianhe Chemical Co., Ltd.'s production
T558。
Mass fraction of the alkylated diphenylamine in antioxidant composition is 50%~85%, preferably 55%~80%, most
It is preferred that 60%~75%.
The structure of the phenthazine are as follows:
Wherein R3、R4The alkyl of the alkyl of respectively H or C1~C20, preferably H or C1~C10.The phenthazine is most preferably
3,7- diisooctyl phenthazine, structure are as follows:
3,7- diisooctyl phenthazine can be prepared by patent US2,781,318 method.
Mass fraction of the phenthazine in antioxidant composition be 3%~30%, preferably 5%~20%, most preferably 10%~
15%。
The structure of the vulcanization hindered phenol are as follows:
Wherein R5、R6、R7And R8The alkyl of respectively H or C1~C10, preferably H, methyl, tert-butyl or octyl, most preferably
Methyl or tert-butyl；M and n is respectively 0 or 1.One of described preferably following structural material of vulcanization hindered phenol is a variety of:
The vulcanization hindered phenol can select 2,2 '-thio-bis--(4- methyl-6-tert-butylphenols), such as Zibo Wanke
Antioxidant 2246-the S of Chemical Co., Ltd.'s production, 4,4'- sulphur union IIs (6- tert-butyl-2- methylphenol), such as Zibo moral hundred
The antioxidant 736 of beneficial Trade Co., Ltd.'s production, 4,4 '-thio-bis--(- 6 tert-butyl phenols of 3- methyl), such as Nanjing Holley
The antioxidant 300 of bright Chemical Co., Ltd.'s production, 2,2 '-thio-bis--(4- octyl -6- tert-butyl phenols), such as Zibo moral hundred
The antioxidant 2244S of beneficial Trade Co., Ltd.'s production, bis- (- 4 hydroxy phenyl of 3,5- di-t-butyl) thioethers can be by document
“Synthesis and Hypocholesterolemic Activityof Alkylidenedithio Bisphenols”
(M.B.Neuworth, R.J.Laufer, J.W.Barnhart, et al.Journal of Medicine Chemistry,
1970,13 (4): 722-725) disclosed in method preparation, bis- (- 4 hydroxybenzyl of 3,5- di-t-butyl) thioethers, such as Changzhou Ling Chi
The antioxidant methene 4426-S of chemical company's production.
The vulcanization hindered phenol most preferably 2,2 '-is thio-bis--(4- methyl-6-tert-butylphenol) and/or 2,2 '-thio-
Double-(4- octyl -6- tert-butyl phenol).
Mass fraction of the vulcanization hindered phenol in antioxidant composition is 5%~45%, preferably 10%~30%, most preferably
15%~25%.
The present invention also provides a kind of lubricant oil composites comprising above-mentioned antioxidant composition, wherein containing above-mentioned antioxygen
Agent composition and lubricating base oil.The lubricating base oil can select one of I, II, III, IV and V class lubricating base oil
Or a variety of, preferably II class and/or Group III lubricating base oil.The antioxidant composition accounts for lubricant oil composite gross mass
0.1%~30%, preferably 0.1%~10%.The lube oil additive of other types can also be added in the lubricant oil composite, than
Such as detersive, dispersing agent, antiwear additive, viscosity index improver, pour-point depressant, antirust agent and anti-foaming agent.
Detersive, dispersing agent, oxidation and corrosion inhibitor, friction improver and viscosity can also be added in the lubricant oil composite
Preferred composition oil of gasoline engine is prepared in index improver.The preferred sulfoacid calcium of the detersive and sulfurized alkylphenol calcium it is mixed
Object is closed, the mass ratio of the two is 1:3~3:1, and additional amount is the 1.0~5.0% of composition oil of gasoline engine gross mass；Described point
Polyisobutene succinimide and/or boron of the number-average molecular weight of the part the preferred polyisobutenyl of powder (PIB) 800~2500
Change polyisobutene succinimide, additional amount is the 3.0~7.0% of composition oil of gasoline engine gross mass；The oxidation and corrosion inhibitor
It is preferred that zinc dialkyl dithiophosphate, additional amount is the 0.6~1.0% of composition oil of gasoline engine gross mass；The friction improves
The mixture of agent preferred oil-soluble organic molybdenum salt and polyol ester Ashless friction modifiers, additional amount are composition oil of gasoline engine
The 0.1~0.5% of gross mass；The viscosity index improver optimal ethylene propylene copolymer, additional amount are gasoline engine oil combination
The 3.0~10% of object gross mass；The preferred polymethacrylates of pour-point depressant, additional amount are the total matter of composition oil of gasoline engine
The 0.1~0.5% of amount.
Lubricant oil composite of the present invention is by alkylated diphenylamine, phenthazine and vulcanization hindered phenol and lubricating base oil
And the lube oil additive of non-essential other types is mixed modulation and obtains.
The present invention also provides a kind of methods for improving lubricating oil antioxygen property, which is characterized in that by the antioxidant group
Object to be closed to be added in lubricating oil, the additional amount of the antioxidant composition is the 0.1%~30% of quality of lubrication oil, preferably 0.1%~
10%。
Antioxidant composition low-sulfur provided by the invention, low ash, without phosphorus, high warm volatilization loss is few, can significantly improve
Oxidation stability of lubricating oil under the conditions of hot conditions and metal ion catalysis effectively extends the service life of lubricating oil, full
The requirement of foot allotment top-grade lubricating oil.
Antioxidant composition of the present invention can effectively delay lubricating oil at the top of engine piston skirt section, piston wall and piston ring
Deterioration by oxidation in equal high-temperature regions, can also significantly extend lubricating oil makes under the impurity catalytic condition such as metal ion in crankcase
With the service life, can be used in protecting IC engine lubricating oil, such as gasoline engine machine oil, diesel engine oil, engine of boat and ship crankcase
Oil, railway high speed diesel engine oil, motorcycle engine oil etc..Antioxidant composition of the present invention can be also used for high temperature item
The industrial lubricant to work under part, as steam turbine oil, hydraulic oil, chain oils, compressor oil, gear oil, bobbin oil, antirust oil,
Rail oil etc..
Lubricant oil composite low-sulfur provided by the invention, low ash, high-temperature oxidation stability is good, long service life.
Specific embodiment
Below by example, present invention be described in more detail, but the present invention is not limited thereto.
Used raw material and source:
Butyl/octyl mixes diphenylamines, butyl/octyl diphenylamine T534 of Beijing Xing Pu company production；
It is right, to '-di-iso-octyldiphenylamine, the IRGANOX L01 of BASF Aktiengesellschaft's production；
Dinonyldiphenylamine, the T558 of Jinzhou Huifa Tianhe Chemical Co., Ltd.'s production；
3,7- diisooctyl phenthazine are prepared by patent US2781318 method；
Without alkyl-substituted phenthazine, it is purchased from Wuxi City auxiliary chemicals factory；
2,2 '-thio-bis--(4- methyl-6-tert-butylphenols), the 2246-S of Wanke Chemical Co., Ltd., Zibo's production；
2,2 '-thio-bis--(4- octyl -6- tert-butyl phenols), the 2244S of the beneficial Trade Co., Ltd.'s production of Zibo moral hundred；
II class lubricating base oil 150N, Jingmen petrochemical industry；Group III lubricating base oil 150N, the double dragons of South Korea；
Antioxidant involved in comparative example includes:
(3,5- di-t-butyl -4- hydroxyphenyl) propionic acid stearyl, the bright Chemical Co., Ltd.'s production of Nanjing Holley
1076, structure are as follows:
2,2 '-thiobis [3- (3,5- di-tert-butyl-hydroxy phenyl) ethyl propionate], Nanjing Milan Chemical Co., Ltd.
The 1035 of production, structure are as follows:
The pungent primary alkyl zinc dithiophosphate of fourth, the T202 of Beijing Xing Pu company production.
The allotment of the antioxidant of above-mentioned different structure is prepared for the embodiment 1-8 of antioxidant composition of the present invention and right respectively
Ratio 1-8, composition are shown in Table 1, table 2 respectively.
Table 1
Table 2
Comparative example 1 is three component antioxidant compositions (preparing by patent EP2173803 method)；Comparative example 2 is bi-component
Antioxidant composition (is prepared) by patent US5091099 method, and wherein amine and the mass ratio of two component of phenol are 9:2；Comparative example 3 is
Traditional phosphorous bi-component antioxidant composition；Comparative example 4-6 is independent a kind of antioxidant in three component antioxidant of the invention；
Comparative example 7,8 is two kinds of antioxidant in three component antioxidant of the invention.
These antioxidant compositions are added to II class respectively to add in hydrogen lubricating base oil, lubricating oil of the present invention is prepared
The embodiment 9-16 and comparative example 9-16 of composition, formula composition are shown in Table 3 and table 4 respectively.
Table 3
Table 4
Embodiment 9~16 and comparative example 9~16 to lubricant oil composite have carried out Pressurized Differential scanning amount heat examination respectively
Test (PDSC, Pressure Differential Scanning Calorimetry) and thin layer oxygen uptake oxidation test (TFOUT,
Thin-Film Oxygen Uptake), specific test result is shown in Table 5.PDSC test is mainly used for evaluating lubricating oil in high temperature work
Oxidation stability under the conditions of work, test temperature are 210 DEG C, pressure 0.5MPa, oxygen gas flow rate 100mL/min.TFOUT's
Test temperature is 160 DEG C, using IIIE catalyst, the working environment of main analog engine crankcase, has metal suitable for simulation
Ion, NOX, harsh conditions in the presence of the impurity such as fuel after oxidation, be a kind of Fast Evaluation I. C. engine oil oxidation stability
Method.
Table 5
| Lubricant oil composite | PDSC oxidation induction period/min | TFOUT oxidation induction period/min |
| Embodiment 9 | 15.5 | 45 |
| Embodiment 10 | 31.8 | 93 |
| Embodiment 11 | 59.2 | 108 |
| Embodiment 12 | 41.3 | 88 |
| Embodiment 13 | 38.4 | 108 |
| Embodiment 14 | 33.5 | 74 |
| Embodiment 15 | 70.7 | 134 |
| Embodiment 16 | 68.5 | 104 |
| Comparative example 9 | 12.6 | 25 |
| Comparative example 10 | 24.8 | 53 |
| Comparative example 11 | 19.8 | 81 |
| Comparative example 12 | 11.3 | 29 |
| Comparative example 13 | 18.4 | 42 |
| Comparative example 14 | 23.5 | 38 |
| Comparative example 15 | 41.4 | 80 |
| Comparative example 16 | 42.0 | 92 |
As can be seen from Table 5, antioxidant composition of the present invention significantly improves the PDSC and TFOUT of lubricant oil composite
Oxidation induction period, and longer oxidation induction period can be possessed simultaneously in two kinds of simulation tests of PDSC and TFOUT.
Respectively by these antioxidant compositions and detersive, dispersing agent, oxidation and corrosion inhibitor, friction improver, viscosity index (VI)
Modifier, pour-point depressant and formulation of base oil are prepared the low-phosphorous low ash of SL/GF-3 that viscosity grade is 5W/30 and divide gasoline engine
The embodiment 17-21 and comparative example 17-19 of machine lubricant oil composite, formula composition are shown in Table 6.
Pressurized Differential scanning calorimetric test (PDSC) is carried out respectively to embodiment 17-21 and comparative example 17-19, thin layer is inhaled
Oxygen oxidation test (TFOUT) and viscosity build test (VIT).The test temperature of PDSC is 220 DEG C, and the test temperature of TFOUT is
160℃.VIT test temperature is 160 DEG C, oxygen flow 5L/h, calculates the viscosity build change rate (time that Δ v) is 375%.
Test result is listed in table 7.
As can be seen from Table 7, three component antioxidant compositions of the invention effectively increase petrol engine lubricating oil
Oxidation stability, oil product service life are significantly extended, compared to comparative example, PDSC oxidation induction period extends 20%~
90%, TFOUT oxidation induction period extend 20%~60%.In terms of controlling viscosity build, slightly it is better than comparative example.Three groups of the present invention
Antioxidant composition is divided to can satisfy the needs for deploying high-grade I. C. engine oil.
Table 6
Table 7
| Composition oil of gasoline engine | PDSC/min | TFOUT/min | VIT- Δ v(375%)/h |
| Embodiment 17 | 39.5 | 169 | 96 |
| Embodiment 18 | 34.3 | 174 | 94 |
| Embodiment 19 | 39.8 | 175 | 95 |
| Embodiment 20 | 43.2 | 195 | 98 |
| Embodiment 21 | 45.6 | 210 | 99 |
| Comparative example 17 | 24.7 | 138 | 88 |
| Comparative example 18 | 28.4 | 133 | 84 |
| Comparative example 19 | 23.9 | 141 | 90 |
Claims (10)
1. a kind of antioxidant composition, including alkylated diphenylamine, phenthazine and vulcanization hindered phenol；The alkylated diphenylamine exists
Mass fraction in antioxidant composition is 55%~80%, and mass fraction of the phenthazine in antioxidant composition is
5%~20%, mass fraction of the vulcanization hindered phenol in antioxidant composition is 10%~30%；
The structure of the vulcanization hindered phenol are as follows:
And/or
Wherein R5、R6、R7And R8The alkyl of respectively H or C1~C10；M and n is respectively 0 or 1.
2. antioxidant composition described in accordance with the claim 1, which is characterized in that the structure of the alkylated diphenylamine are as follows:
Wherein R1、R2The alkyl of respectively H or C1~C20.
3. antioxidant composition according to claim 2, which is characterized in that the R1、R2The alkyl of C2~C10 respectively, R1
And R2Contraposition or ortho position positioned at amino.
4. antioxidant composition described in accordance with the claim 1, which is characterized in that the structure of the phenthazine are as follows:
Wherein R3、R4The alkyl of respectively H or C1~C20.
5. antioxidant composition according to claim 4, which is characterized in that the R3、R4The alkane of respectively H or C1~C10
Base.
6. antioxidant composition described in accordance with the claim 1, which is characterized in that wherein R5、R6、R7And R8Respectively H, methyl,
Tert-butyl or octyl.
7. antioxidant composition described in accordance with the claim 1, which is characterized in that the alkylated diphenylamine is butyl/octyl
Diphenylamines, right is mixed, to '-one of di-iso-octyldiphenylamine and dinonyldiphenylamine or a variety of, the phenthazine is 3,7-
Diisooctyl phenthazine, the vulcanization hindered phenol are one of following structural material or a variety of:
8. a kind of lubricant oil composite, including antioxidant composition and lubricating base oil described in one of claim 1-7.
9. a kind of composition oil of gasoline engine, including antioxidant composition, detersive described in one of claim 1-7, dispersing agent,
Antiwear additive, viscosity index improver, pour-point depressant and lubricating base oil.
10. a kind of method for improving lubricating oil antioxygen property, which is characterized in that by antioxidant described in one of claim 1-7
Composition is added in lubricating oil.
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