CN106190434A - Nitrogen molybdenum complex lube oil additive and preparation method thereof - Google Patents
Nitrogen molybdenum complex lube oil additive and preparation method thereof Download PDFInfo
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- CN106190434A CN106190434A CN201610522146.1A CN201610522146A CN106190434A CN 106190434 A CN106190434 A CN 106190434A CN 201610522146 A CN201610522146 A CN 201610522146A CN 106190434 A CN106190434 A CN 106190434A
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- additive
- nitrogen
- ester
- molybdenum
- molybdenum complex
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Classifications
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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
- C10M139/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
-
- 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
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/09—Complexes with metals
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
Abstract
The invention discloses a kind of nitrogen molybdenum complex lube oil additive and preparation method thereof, react with monoethanolamine based on Oleum Brassicae campestris, add the different monooctyl ester of SA, the method using regulation negative pressure, obtain the beneficially lower mixed amine ester walking sound response, then with amino benzoic Acid 2-aminopropane., isoamyl salicylate, molybdenum oxide reacts, adding adipic acid, two step pressure applications are used to make molybdenum content reach optimum in the case of lauryl alcohol, nitrogen molybdenum structure is stable, thus make the nitrogen molybdenum complex lube oil additive of the novel high molybdenum content with good lubricating properties and splendid wear resistence.The additive that the present invention prepares is a kind of oil-soluble nitrogen molybdenum complex, is the lubricating oil particularly friction improver of I. C. engine lubricating oil, antiwear additive and antioxidant, and oil-saving effect is notable, due to not sulfur-bearing phosphorus, the advantage that this additive also has energy-conserving and environment-protective.
Description
Technical field
The present invention relates to lube oil additive, relate in particular to a kind of oil-soluble nitrogen molybdenum complex lube oil additive and
Its preparation method.
Background technology
The research of the lube oil additives such as oil-soluble boron, molybdenum, tungsten, the most existing a lot of document introductions, this element is made
Lube oil additive can be effectively reduced friction coefficient of lubricating oil and improve its wear-resistant antifraying property that undermines, but, by
In the difference of carrier, major part is containing elements such as sulfur, phosphorus, chlorine, and when machine oil uses more than 4000 kilometers, substantial amounts of sulfur phosphorus can shape
Become corresponding acid, electromotor is caused damage.
In recent years, along with developing rapidly of auto industry, particularly energy-saving and emission-reduction, low-carbon environment-friendly cry day by day strong,
Force many petroleum additive companies, all furnish a huge amount of money for study the lube oil additive product of efficient energy-saving.
Summary of the invention
The technical problem to be solved is to provide that a kind of production method is simple, low cost, oil-soluble are good, productivity
High nitrogen molybdenum complex lube oil additive and preparation method thereof, this additive is a kind of oil-soluble molybdenum amine complex, is lubrication
The oil particularly friction improver of I. C. engine lubricating oil, antiwear additive and antioxidant, oil-saving effect is notable, owing to not containing
Sulfur phosphorus, the advantage that this additive also has energy-conserving and environment-protective.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: a kind of nitrogen molybdenum complex lubricating oil adds
The preparation method of agent, comprises the following steps:
1) synthesis of mixed amine ester: Oleum Brassicae campestris and monoethanolamine are placed in container, nitrogen protective condition lower 100 DEG C～
110 DEG C are reacted 2～3 hours, then add the different monooctyl ester of SA, under the conditions of negative pressure 50mmHg height, heighten temperature to 180 DEG C～190
DEG C, continue reaction 4～5 hours, obtain mixed amine ester, by weight Oleum Brassicae campestris: monoethanolamine: different monooctyl ester=2 of SA～3:3
～4:1～1.5；
2) synthesis of nitrogen molybdenum complex additive: by the mixed amine ester of above-mentioned preparation and amino benzoic Acid 2-aminopropane., bigcatkin willow
Isoamyl valerate, molybdenum oxide mix, and add adipic acid, under the conditions of temperature 90 DEG C～95 DEG C, negative pressure 80mmHg height, instead after stirring
Answer 4～5 hours；It is subsequently adding lauryl alcohol, adjusts negative pressure under the conditions of 50mmHg height, heighten temperature to 180 DEG C～190 DEG C, continue
Continuous reaction 3～4 hours, then cools to 100 DEG C, continues to keep negative pressure under the conditions of 50mmHg height；Finally filter, obtain reddish brown
Color novel nitrogen molybdenum complex lube oil additive；Wherein mixed amine ester and amino benzoic Acid 2-aminopropane., isoamyl salicylate, oxidation
Molybdenum, adipic acid, weight ratio=100:8～9.5:6～6.5:16～19:11～12:12～14 of lauryl alcohol.
Described additive raw material weight ratio is mixed amine ester: amino benzoic Acid 2-aminopropane.: isoamyl salicylate: molybdenum oxide:
Adipic acid: lauryl alcohol=100:8.5:6:16:11:14；The weight ratio of mixed amine ester component is Oleum Brassicae campestris: monoethanolamine: certain herbaceous plants with big flowers two
Different monooctyl ester=the 2:3:1 of acid.
The nitrogen molybdenum complex lube oil additive that above-mentioned preparation method prepares.
The invention has the beneficial effects as follows: nitrogen molybdenum complex lube oil additive not sulfur-bearing phosphorus phosphorus, high containing molybdenum amount, such adds
Agent has good antiwear and antifriction and anti-oxidative stability, can be greatly improved the inefficacy load of friction pair material, this nitrogen molybdenum
Complex can form stratiform structural membrane in metal surface, it is not easy to oxidized, can be greatly prolonged the drain period of lubricating oil.Combine
Close the common denominator of conventional anti-friction agent, preferably highlight wear-resistant, antifriction and antioxygenic property, more obvious energy-saving effect,
Complementary raising can be accomplished completely.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail:
The preparation method of the nitrogen molybdenum complex lube oil additive of the present invention, comprises the following steps:
1) synthesis of mixed amine ester: Oleum Brassicae campestris and monoethanolamine are placed in container, nitrogen protective condition lower 100 DEG C～
110 DEG C are reacted 2～3 hours, then add the different monooctyl ester of SA, under the conditions of negative pressure 50mmHg height, heighten temperature to 180 DEG C～190
DEG C, continue reaction 4～5 hours, obtain mixed amine ester, by weight Oleum Brassicae campestris: monoethanolamine: different monooctyl ester=2 of SA～3:3
～4:1～1.5；
2) synthesis of nitrogen molybdenum complex additive: by the mixed amine ester of above-mentioned preparation and amino benzoic Acid 2-aminopropane., bigcatkin willow
Isoamyl valerate, molybdenum oxide mix, and add adipic acid, under the conditions of temperature 90 DEG C～95 DEG C, negative pressure 80mmHg height, instead after stirring
Answer 4～5 hours；It is subsequently adding lauryl alcohol, adjusts negative pressure under the conditions of 50mmHg height, heighten temperature to 180 DEG C～190 DEG C, continue
Continuous reaction 3～4 hours, then cools to 100 DEG C, continues to keep negative pressure under the conditions of 50mmHg height；Finally filter, obtain reddish brown
Color novel nitrogen molybdenum complex lube oil additive；Wherein mixed amine ester and amino benzoic Acid 2-aminopropane., isoamyl salicylate, oxidation
Molybdenum, adipic acid, weight ratio=100:8～9.5:6～6.5:16～19:11～12:12～14 of lauryl alcohol.
Described additive raw material weight ratio is mixed amine ester: amino benzoic Acid 2-aminopropane.: isoamyl salicylate: molybdenum oxide:
Adipic acid: lauryl alcohol=100:8.5:6:16:11:14；The weight ratio of mixed amine ester component is Oleum Brassicae campestris: monoethanolamine: certain herbaceous plants with big flowers two
Different monooctyl ester=the 2:3:1 of acid.
The nitrogen molybdenum complex lube oil additive that above-mentioned preparation method prepares.
In the present invention, first react with monoethanolamine based on Oleum Brassicae campestris, add the different monooctyl ester of SA, use regulation
The method of negative pressure, obtains the beneficially lower mixed amine ester walking sound response, then with amino benzoic Acid 2-aminopropane., salicylic acid isoamyl
Ester, molybdenum oxide react, and use two step pressure applications to make molybdenum content reach optimum, nitrogen in the case of adding adipic acid, lauryl alcohol
Molybdenum structure is stable, thus makes the nitrogen molybdenum complex lubricating oil of the novel high molybdenum content with good lubricating properties and splendid wear resistence
Additive.
The nitrogen molybdenum complex lube oil additive that the present invention provides has the advantage of energy-saving, environment-friendly and high-efficiency, adds in lubricating oil
Add 0.5～1% (weight) additive of the present invention, i.e. can reach following effect:
1, coefficient of friction is reduced: being added to lubricating oil, grease etc., its coefficient of friction is reduced to about 0.03.
2, engine temperature is reduced: temperature more than 30% can be significantly reduced.
3, fuel oil is saved: can be with fuel-economizing more than 10%.
4, the drain period is extended: the drain period more than 50% can be extended.
5, energy-conserving and environment-protective: additive of the present invention not sulfur-bearing, phosphorus or chlorine type antiwear additive, thus avoid conventional additive
Friction pair material is had corrosivity, selectivity to problems such as environments.
Embodiment 1
1, the synthesis of mixed amine ester
Oleum Brassicae campestris and monoethanolamine being placed in container, under nitrogen protective condition, temperature 100 DEG C is reacted 2 hours, then adds
The different monooctyl ester of SA, under the conditions of negative pressure 50mmHg height, heightens temperature to 180 DEG C, continues reaction 4 hours, obtain mixed amine ester；
Oleum Brassicae campestris: monoethanolamine: the different monooctyl ester=2:3:1 of SA (weight ratio).
2, the synthesis of nitrogen molybdenum complex lube oil additive
By the mixed amine ester 50 grams of above-mentioned preparation and amino benzoic Acid 2-aminopropane. 4.5 grams, isoamyl salicylate 3 grams, oxidation
Molybdenum 9 grams mixing, adds adipic acid 5.5 grams after stirring, under the conditions of temperature 90 DEG C, negative pressure 80mmHg height, react 4 hours；So
6 grams of lauryl alcohols of rear addition, adjustment negative pressure under the conditions of 50mmHg height, is heightened temperature to 180 DEG C, is continued reaction 3 hours, then drop
Temperature, to 100 DEG C, continues to keep negative pressure under the conditions of 50mmHg height；Finally filter, obtain brownish red novel nitrogen molybdenum complex lubrication
Oil additive.
The antifriction antiwear of product and the investigation of bearing capacity: utilize four-ball tester to measure, (temperature 20 DEG C is born to set load
Lotus 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, the steel ball used by four-ball test is straight
The GCR steel ball of footpath 12.7mm, test shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly use
Lubricating oil, wear scar diameter reaches 0.70mm.In full formula SN0W/40 engine oil, add 1% (weight) the present embodiment prepare
Product, wear scar diameter reaches 0.33mm, coefficient of friction 0.039.
Embodiment 2
1, the synthesis of mixed amine ester
Oleum Brassicae campestris and monoethanolamine being placed in container, under nitrogen protective condition, temperature 110 DEG C is reacted 3 hours, then adds
The different monooctyl ester of SA, under the conditions of negative pressure 50mmHg height, heightens temperature to 190 DEG C, continues reaction 5 hours, obtain mixed amine ester；
Oleum Brassicae campestris: monoethanolamine: the different monooctyl ester=2:3:1 of SA (weight ratio).
2, the synthesis of nitrogen molybdenum complex lube oil additive
By the mixed amine ester 100 grams of above-mentioned preparation and amino benzoic Acid 2-aminopropane. 8 grams, isoamyl salicylate 6.5 grams, oxidation
Molybdenum 16 grams mixing, adds adipic acid 12 grams after stirring, under the conditions of temperature 95 DEG C, negative pressure 80mmHg height, react 5 hours；So
14 grams of lauryl alcohols of rear addition, adjustment negative pressure under the conditions of 50mmHg height, is heightened temperature to 190 DEG C, is continued reaction 4 hours, then
Cool to 100 DEG C, continue to keep negative pressure under the conditions of 50mmHg height；Finally filter, obtain brownish red novel nitrogen molybdenum complex profit
Oil additive.
The antifriction antiwear of product and the investigation of bearing capacity, with embodiment 1, by contrast, directly use lubricating oil, mill
Spot diameter reaches 0.70mm.In full formula SN0W/40 engine oil, add 1% (weight) the present embodiment prepare product, grind speckle
Diameter reaches 0.30mm, coefficient of friction 0.033.
Embodiment 3
1, the synthesis of mixed amine ester
Oleum Brassicae campestris and monoethanolamine being placed in container, under nitrogen protective condition, temperature 100 DEG C is reacted 3 hours, then adds
The different monooctyl ester of SA, under the conditions of negative pressure 50mmHg height, heightens temperature to 185 DEG C, continues reaction 4.5 hours, obtain mixed amine ester；
Oleum Brassicae campestris: monoethanolamine: the different monooctyl ester=2:3:1 of SA (weight ratio).
2, the synthesis of nitrogen molybdenum complex lube oil additive
By the mixed amine ester 70 grams of above-mentioned preparation and amino benzoic Acid 2-aminopropane. 5.8 grams, isoamyl salicylate 4.3 grams, oxygen
Changing molybdenum 12 grams mixing, add adipic acid 8 grams after stirring, under the conditions of temperature 100 DEG C, negative pressure 80mmHg height, reaction 4.5 is little
Time；Being subsequently adding 9 grams of lauryl alcohols, adjustment negative pressure under the conditions of 50mmHg height, is heightened temperature to 185 DEG C, is continued reaction 4 hours,
Then cool to 100 DEG C, continue to keep negative pressure under the conditions of 50mmHg height；Finally filter, obtain brownish red novel nitrogen molybdenum complexation
Thing lube oil additive.
The antifriction antiwear of product and the investigation of bearing capacity, with embodiment 1, by contrast, directly use lubricating oil, mill
Spot diameter reaches 0.70mm.In full formula SN0W/40 engine oil, add 1% (weight) the present embodiment prepare product, grind speckle
Diameter reaches 0.35mm, coefficient of friction 0.037.
Embodiment 4
1, the synthesis of mixed amine ester
Oleum Brassicae campestris and monoethanolamine are placed in container, under nitrogen protective condition, temperature 105 DEG C reaction 3.5 hours, then
Add the different monooctyl ester of SA, under the conditions of negative pressure 50mmHg height, heighten temperature to 180 DEG C, continue reaction 5 hours, obtain mixed amine ester；
Oleum Brassicae campestris: monoethanolamine: the different monooctyl ester=2:3:1 of SA (weight ratio).
2, the synthesis of nitrogen molybdenum complex lube oil additive
By the mixed amine ester 200 grams of above-mentioned preparation and amino benzoic Acid 2-aminopropane. 17 grams, isoamyl salicylate 12.8 grams, oxygen
Change molybdenum 36 grams mixing, add adipic acid 23 grams after stirring, under the conditions of temperature 110 DEG C, negative pressure 80mmHg height, react 5 hours；
Being subsequently adding 26 grams of lauryl alcohols, adjustment negative pressure under the conditions of 50mmHg height, is heightened temperature to 190 DEG C, is continued reaction 4.5 hours,
Then cool to 100 DEG C, continue to keep negative pressure under the conditions of 50mmHg height；Finally filter, obtain brownish red novel nitrogen molybdenum complexation
Thing lube oil additive.
The antifriction antiwear of product and the investigation of bearing capacity, with embodiment 1, by contrast, directly use lubricating oil, mill
Spot diameter reaches 0.70mm.In full formula SN0W/40 engine oil, add 1% (weight) the present embodiment prepare product, grind speckle
Diameter reaches 0.34mm, coefficient of friction 0.030.
In sum, present disclosure is not limited in the above embodiments, and the knowledgeable people in same area can
Can propose other embodiment within technological guidance's thought of the present invention easily, but this embodiment is included in this
Within the scope of bright.
Claims (3)
1. the preparation method of a nitrogen molybdenum complex lube oil additive, it is characterised in that comprise the following steps:
1) synthesis of mixed amine ester: Oleum Brassicae campestris and monoethanolamine are placed in container, lower 100 DEG C～110 DEG C of nitrogen protective condition
React 2～3 hours, then add the different monooctyl ester of SA, under the conditions of negative pressure 50mmHg height, heighten temperature to 180 DEG C～190 DEG C, continue
Continuous reaction 4～5 hours, obtains mixed amine ester, by weight Oleum Brassicae campestris: monoethanolamine: different monooctyl ester=2 of SA～3:3～4:1
～1.5；
2) synthesis of nitrogen molybdenum complex additive: by different to the mixed amine ester of above-mentioned preparation and amino benzoic Acid 2-aminopropane., salicylic acid
Pentyl ester, molybdenum oxide mix, and add adipic acid after stirring, and under the conditions of temperature 90 DEG C～95 DEG C, negative pressure 80mmHg height, react 4
～5 hours；It is subsequently adding lauryl alcohol, adjusts negative pressure under the conditions of 50mmHg height, heighten temperature to 180 DEG C～190 DEG C, continue anti-
Answer 3～4 hours, then cool to 100 DEG C, continue to keep negative pressure under the conditions of 50mmHg height；Finally filter, obtain brownish red new
Type nitrogen molybdenum complex lube oil additive；Wherein mixed amine ester and amino benzoic Acid 2-aminopropane., isoamyl salicylate, molybdenum oxide,
Adipic acid, weight ratio=100:8～9.5:6～6.5:16～19:11～12:12～14 of lauryl alcohol.
The preparation method of nitrogen molybdenum complex lube oil additive the most according to claim 1, it is characterised in that described interpolation
Agent raw material weight is than for mixed amine ester: amino benzoic Acid 2-aminopropane.: isoamyl salicylate: molybdenum oxide: adipic acid: lauryl alcohol=
100:8.5:6:16:11:14；The weight ratio of mixed amine ester component is Oleum Brassicae campestris: monoethanolamine: the different monooctyl ester=2:3:1 of SA.
3. the nitrogen molybdenum complex lube oil additive that a preparation method as claimed in claim 1 or 2 prepares.
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| CN106833814A (en) * | 2017-03-27 | 2017-06-13 | 苏州金钼润成润滑科技有限公司 | A kind of environmentally friendly organic tungsten lubricant and preparation method thereof |
| CN106957708A (en) * | 2017-04-18 | 2017-07-18 | 北京千泓祺科技有限公司 | A kind of repairing type energy saving environment protection engine protective agent and preparation method thereof |
| CN107750269A (en) * | 2015-06-17 | 2018-03-02 | 雪佛龙奥伦耐有限责任公司 | Multi-functional molybdate compound, its preparation and application and the lubricant oil composite containing it |
| CN109536254A (en) * | 2018-11-27 | 2019-03-29 | 苏州金钼润成润滑科技有限公司 | Golden steel alkane nitrogen molybdenum lubricant and preparation method thereof |
| CN112080331A (en) * | 2020-09-24 | 2020-12-15 | 苏州金钼润成润滑科技有限公司 | Organic nitrogen zirconium fullerene lubricant and preparation method thereof |
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| CN107750269A (en) * | 2015-06-17 | 2018-03-02 | 雪佛龙奥伦耐有限责任公司 | Multi-functional molybdate compound, its preparation and application and the lubricant oil composite containing it |
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| CN109536254A (en) * | 2018-11-27 | 2019-03-29 | 苏州金钼润成润滑科技有限公司 | Golden steel alkane nitrogen molybdenum lubricant and preparation method thereof |
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| CN112080331A (en) * | 2020-09-24 | 2020-12-15 | 苏州金钼润成润滑科技有限公司 | Organic nitrogen zirconium fullerene lubricant and preparation method thereof |
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