CN101381649B - Non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent and preparation method - Google Patents
Non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent and preparation method Download PDFInfo
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- CN101381649B CN101381649B CN2008100533496A CN200810053349A CN101381649B CN 101381649 B CN101381649 B CN 101381649B CN 2008100533496 A CN2008100533496 A CN 2008100533496A CN 200810053349 A CN200810053349 A CN 200810053349A CN 101381649 B CN101381649 B CN 101381649B
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Abstract
The invention belongs to the technical field of lubricating oil and discloses a non-sulfur non-phosphorus anti-wear and antifrictional multifunctional additive and a preparation method thereof. The compositions of the additive comprise a friction modifier, an antiwear agent, an antioxidant, a detergent dispersant, and an antirusting agent. Firstly, the friction modifier is synthesized, then the friction modifier, the antiwear agent, the detergent dispersant, the antioxidant, and the antirusting agent with the needed amount are orderly mixed according to the proportion, and the mixture is heated to between 50 and 70 DEG C under the stirring and then is stirred evenly. The additive can be widely applied to various lubricating oil products including lubricant base oil or lubricant oil finished products, such as internal combustion engine oil, gear oil and so on, and is added into lubricating oil of an internal combustion engine with 3 to 20 weight percentage during the use. The additive can greatly improve the abrasion resistance and the antifriction performance of oil products, can also apparently improve the initial oxidation temperature and the oxidation induction time of the oil products, effectively suppress the viscosity of the oil products from increasing, and ensure that the high-temperature antioxidation performance of the internal combustion engine oil is greatly improved.
Description
Technical field
The invention belongs to technical field of lubricating oil, particularly relate to a kind of non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent and preparation method.
Background technology
Good lubrication oil antiwear antifriction additive, can reduce equipment maintenance cost, prolong equipment duration of service, cut down the consumption of energy.For motor car engine, good IC engine oil additive not only can be protected the engine protected from wear, the burn oil phenomenon that also can avoid insufficient lubrication to cause, protection atmospheric environment.
Increasingly stringent along with environmental regulation, petrol engine has adopted three-way catalytic converter, diesel motor has increased tail gas recirculation system, this makes engine oil develop to low-sulfur and low-phosphorous direction gradually, replace or reduce the usage quantity of zinc dialkyl dithiophosphate (T 202) additive commonly used in the engine oil, become inexorable trend.Reduce discharging, improve fuel economy, prolong the direct driving force that engine oil has become the high-grade engine oil of development work-ing life.But, the minimizing of T 202 content, can reduce the extreme pressure of oil product, wear-resistant and antioxidant property again, and new ILSAC specification requirement further improves the wear-resistant and antioxygen property of oil product under the prerequisite that reduces the sulphur phosphorus content, therefore, seek of the use of new non-sulphur phosphorus additive technology, and it is significant to satisfy service requirements efficient, energy saving and environment friendly engine oil to minimizing or alternative T 202.
Summary of the invention
For this reason, we have developed a kind of non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent, and this additive not only has good wear-resistant, antifriction and antioxidant property, but also has outstanding wear-resistant and antifriction synergistic effect with multiple conventional additive.
The component and the weight percent content of non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention are as follows:
A. friction improver 35-55
B. anti-wear agent 35-55
C. oxidation inhibitor 3-8
D. detergent-dispersant additive 2-8
F. rust-preventive agent 1-3.
Described friction improver is the organic many metallic compounds of non-sulphur phosphorus, and institute's containing metal is tin, titanium and bismuth.
Described anti-wear agent is one of organic boronic ester cpds, oil soluble borate compound or their mixture.
Described oxidation inhibitor is one of shielding bisphenol cpd, dialkyl diphenylamine, methene-two (dibutyl dithiocaarbamate ester) or their mixture.
Described detergent-dispersant additive is one of alkyl sodium salicylate, polyisobutylene succinic acid imines or their mixture.
Described rust-preventive agent is dodecenylsuccinic acid.
The method of non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention may further comprise the steps successively:
(1) friction improver is synthetic: with carbon chain lengths greater than 12 organic acid and trolamine according to 1.0～3.0: in 1.0～2.0 the molar ratio adding reaction flask, and then the catalyzer of adding reaction-ure mixture 5%～15%, stir, and be heated to 120 ℃～140 ℃, reacted 3～5 hours, synthetic intermediate, and then adding pink salt, the mixture of organic titanic compound and bismuth compound, adding molar ratio is 1～2.5: 2～3.5: 0.5～1.5, continue to stir, and under 180～200 ℃ temperature, reacted 4～8 hours, obtain the organic many metallic compounds of non-sulphur phosphorus at last;
(2) fused: friction improver, anti-wear agent, detergent-dispersant additive, oxidation inhibitor and the rust-preventive agent of aequum are mixed successively in proportion, and miscellany under agitation is warming up to 50～70 ℃, and stirring then gets final product.
Described organic acid is oleic acid or naphthenic acid; Catalyzer is a dialkylamine.
Non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention can be widely used in comprising in the various lubricating oil products of lubricant base or lubricated processed oil, as I. C. engine oil, gear wet goods, in use the weight percentage with 3-20 joins in the internal combustion (IC) engine lubricating oil.After in modern engine oil, adding non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention, not only can improve the wear-resistant and antifriction performance of oil product greatly, and can obviously improve initial oxidation temperature, the oxidation induction time of oil product, the viscosity that suppresses oil product effectively increases, the high temperature antioxygen property of I. C. engine oil is greatly improved, and non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention has outstanding wear-resistant, antifriction and high-temperature oxidation resistance.
Description of drawings
Fig. 1: embodiment 2 additions are to containing the influence of T 202 oil product frictional coefficient;
Fig. 2: T 202 additions are to containing the influence of embodiment 2 oil product frictional coefficient;
Fig. 3: embodiment 11 influence that oil sample viscosity increases under different oxidization times.
Embodiment
Friction improver is synthetic.0.2mol oleic acid and 0.2mol trolamine are added in the reaction flask, 4.5g dibutylamine then, stir, and be heated to 120 ℃, reacted synthetic intermediate 3 hours, and then the mixture of adding 0.05mol dibutyl tin laurate, 0.1mol tetra isopropyl titanate and 0.025mol bismuth oxide, continue to stir, and reacted 6 hours down, obtain the friction improver product at last at 180 ℃.
Again with friction improver 45%, oleic acid diethyl amide boric acid ester 45%, 2,6-ditertbutylparacresol 3%, diene base succimide 6%, dodecenylsuccinic acid 1% is mixed successively, and mixture under agitation is warming up to 50 ℃, and stirring obtains non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention.
Friction improver 50% with embodiment 1 preparation, oleic acid diethyl amide boric acid ester 40%, methene-two (dibutyl dithiocaarbamate ester) 3%, alkyl sodium salicylate 2%, diene base succimide 4%, dodecenylsuccinic acid 1% is mixed successively, and mixture under agitation is warming up to 50-60 ℃, and stirring obtains non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention.
Friction improver 55% with embodiment 1 preparation, borate (T 361) 35%, di-iso-octyldiphenylamine 3%, alkyl sodium salicylate 6%, dodecenylsuccinic acid 1% is mixed successively, and mixture under agitation is warming up to 50-60 ℃, stirring obtains non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention.
Embodiment 4
Friction improver 40% with embodiment 1 preparation, boric acid three monooctyl esters 45%, borate (T 361) 9%, 2,6 ditertiary butyl p cresol 1%, methene-two (dibutyl dithiocaarbamate ester) 2%, alkyl sodium salicylate 2%, dodecenylsuccinic acid 1% is mixed successively, and mixture under agitation is warming up to 50-60 ℃, and stirring obtains non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention.
Friction improver is synthetic.0.4mol oleic acid and 0.2mol trolamine are added in the reaction flask, 12g Di-Octyl amine then, stir, and be heated to 140 ℃, reacted synthetic intermediate, and then the mixture of adding 0.1mol stannous naphthenate, 0.3mol four isobutyl-titanic acid ester and 0.1mol naphthenic acid bismuth 5 hours, and, obtain the friction improver product at last 190 ℃ of following stirring reactions 8 hours.
Then with the friction improver 40% for preparing, oleic acid diethyl amide boric acid ester 45%, 2,6-ditertbutylparacresol 1%, di-iso-octyldiphenylamine 3%, methene-two (dibutyl dithiocaarbamate ester) 2%, diene base succimide 7%, dodecenylsuccinic acid 2% is mixed successively, and mixture under agitation is warming up to 70 ℃, and stirring obtains non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention.
Friction improver is synthetic.0.4mol naphthenic acid and 0.3mol trolamine are added in the reaction flask, 9g Di-Octyl amine then, stir, and be heated to 140 ℃, reacted synthetic intermediate, and then the mixture of adding 0.15mol dibutyl tin laurate, 0.2mol tetra isopropyl titanate and 0.08mol naphthenic acid bismuth 4 hours, and, obtain the friction improver product at last 200 ℃ of following stirring reactions 6 hours.
To prepare then friction improver 50%, oleic acid diethyl amide boric acid ester 35%, di-iso-octyldiphenylamine 6%, methene-two (dibutyl dithiocaarbamate ester) 2%, diene base succimide 4%, dodecenylsuccinic acid 3% is mixed successively, and mixture under agitation is warming up to 50-60 ℃, and stirring obtains non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention.
The result as can be seen from table, after the non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of different ratios and T 202 and T 203 are composite, its wear scar diameter is all less than single agent, show that additive of the present invention and zinc dialkyl dithiophosphate have extraordinary wear-resistant synergistic effect, especially T 202 is under low concentration, and oil product also has outstanding abrasion resistance.
Table 1
Embodiment 8
The non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of embodiment 2 is joined in 150SN (commercially available) base oil with different concentration expressed in percentage by weight ratios with zinc dialkyl dithiophosphate (T 202), utilize four-ball tester to estimate the antifriction performance of oil product under the different loads condition.Test conditions: room temperature, GCr15 steel ball, 1450 rev/mins of rotating speeds, 20 minutes frictional coefficient test durations.Experimental result is seen Fig. 1 and Fig. 2.
Therefrom as can be seen, after embodiment 2 and T 202 are composite, under three kinds of loads (392N, 588N, 686N), the test frictional coefficient of oil product all obviously reduces, shown good antifriction synergism, especially when embodiment 2 concentration reach 4.0%, can also effectively reduce the frictional coefficient of oil product, this provides new prescription for the sulphur phosphorus content that reduces in the oil product.
Embodiment 9
Embodiment 4 is joined in the internal combustion (IC) engine lubricating oil of the different trades mark with 5.0% concentration expressed in percentage by weight, the abrasion resistance of oil product that evaluation is joined, used I. C. engine oil is respectively SJ 15W/50 (commercially available), SH 15W/50 (commercially available), eastern precious SJ 15W/40 and Dong Bao CD lubricating oil.Adopt four-ball tester to estimate the abrasion resistance of oil product under the different loads condition, test conditions: room temperature, GCr15 steel ball, 1450 rev/mins of rotating speeds, 30 minutes time.Experimental result sees Table 2.From the table the result as can be seen, the adding of non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent can obviously improve the abrasion resistance of commercially available internal combustion (IC) engine lubricating oil.
Table 2
| The precious SJ15W/40+ |
0.36 | 0.42 | 0.47 |
| The precious CD in east | 0.44 | 0.69 | Card is stung |
| The |
0.40 | 0.48 | 0.55 |
Table 3
| Lubricating oil | Initial oxidation temperature, ℃ | Oxidation induction time, minute |
| The 500SN base oil | 201.4 | 5.8 |
| Add component shown in the embodiment 9 | 215.8 | 25.2 |
Embodiment 11
As can be seen from the figure, after in the 150SN base oil, adding non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent, at different oxidization times, the viscosity increased value of this oil sample all is lower than the not added-time, illustrate to add the increase that non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent of the present invention can reduce oil viscosity effectively, play good antioxidant effect.
Claims (5)
1. non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent is characterized in that:
The weight percent of its raw material and component is:
Component title %
A. friction improver 35～55
B. anti-wear agent 35～55
C. oxidation inhibitor 3～8
D. detergent-dispersant additive 2～8
F. rust-preventive agent 1～3;
Friction improver is synthetic: with carbon chain lengths greater than 12 organic acid and trolamine according to 1.0～3.0: in 1.0～2.0 the molar ratio adding reaction flask, and then the catalyzer of adding reaction-ure mixture 5%～15%, stir, and be heated to 120 ℃～140 ℃, reacted 3～5 hours, synthetic intermediate, and then adding pink salt, the mixture of organic titanic compound and bismuth compound, adding molar ratio is 1～2.5: 2～3.5: 0.5～1.5, continue to stir, and under 180～200 ℃ temperature, reacted 4～8 hours, obtain the organic many metallic compounds of non-sulphur phosphorus at last;
Fused: friction improver, anti-wear agent, detergent-dispersant additive, oxidation inhibitor and the rust-preventive agent of aequum are mixed successively in proportion, and miscellany under agitation is warming up to 50～70 ℃, and stirring then gets final product;
Described catalyzer is a dialkylamine;
Described organic acid is oleic acid or naphthenic acid.
2. non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent according to claim 1 is characterized in that: described anti-wear agent is one of organic boronic ester cpds, oil soluble borate compound or their mixture.
3. non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent according to claim 1 is characterized in that: described oxidation inhibitor is one of shielding bisphenol cpd, dialkyl diphenylamine or their mixture.
4. non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent according to claim 1 is characterized in that: described detergent-dispersant additive is one of alkyl sodium salicylate, polyisobutylene succinic acid imines or their mixture.
5. non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent according to claim 1 is characterized in that: described rust-preventive agent is dodecenylsuccinic acid.
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| CN101864336A (en) * | 2010-06-23 | 2010-10-20 | 北京泽华化学工程有限公司 | Additive composite of lubricating oil for industrial gears |
| CN102492526A (en) * | 2011-12-02 | 2012-06-13 | 赵醒翩 | Multifunctional lubricating oil compound additive |
| CN103897773A (en) * | 2012-12-28 | 2014-07-02 | 哈尔滨商业大学 | Phosphorus-free low-ash antioxidative anti-wear complex additive and preparation method thereof |
| CN103333729A (en) * | 2013-05-06 | 2013-10-02 | 辽宁汽众润滑油生产有限公司 | Novel metal magnetic lubricating oil additive and preparation method thereof |
| CN103710113B (en) * | 2013-12-25 | 2016-08-17 | 烟台德高石油有限公司 | A kind of lubricating oil reinforcing agent and preparation method thereof |
| CN111500348A (en) * | 2020-04-26 | 2020-08-07 | 中国石油化工股份有限公司 | Fully-synthetic elevator gear oil composition and preparation method thereof |
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| US4834893A (en) * | 1987-12-31 | 1989-05-30 | Mobil Oil Corporation | Substituted phosphorodithioates and their metal salts as multifunctional additives |
| EP1136496A1 (en) * | 2000-03-23 | 2001-09-26 | Ethyl Corporation | Oil soluble organic molybdenum complexes and their use as multifunctional additives for lubricating compositions |
| CN1424387A (en) * | 2002-12-31 | 2003-06-18 | 上海大学 | Modified castor lubricant and its preparation |
| CN1632084A (en) * | 2004-11-18 | 2005-06-29 | 上海大学 | Method for preparing polyisobutylene base oil soluble organic molybdenum lubricating additives |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4834893A (en) * | 1987-12-31 | 1989-05-30 | Mobil Oil Corporation | Substituted phosphorodithioates and their metal salts as multifunctional additives |
| EP1136496A1 (en) * | 2000-03-23 | 2001-09-26 | Ethyl Corporation | Oil soluble organic molybdenum complexes and their use as multifunctional additives for lubricating compositions |
| CN1424387A (en) * | 2002-12-31 | 2003-06-18 | 上海大学 | Modified castor lubricant and its preparation |
| CN1632084A (en) * | 2004-11-18 | 2005-06-29 | 上海大学 | Method for preparing polyisobutylene base oil soluble organic molybdenum lubricating additives |
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