CN107760413A - A kind of non-sulphur phosphorus oil-soluble organic molybdenum additive and its preparation method and application - Google Patents
A kind of non-sulphur phosphorus oil-soluble organic molybdenum additive and its preparation method and application Download PDFInfo
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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
- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
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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
- 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
- C10M2227/06—Organic compounds derived from inorganic acids or metal salts
- C10M2227/066—Organic compounds derived from inorganic acids or metal salts derived from Mo or W
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- 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
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- 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
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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- 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
- C10N2030/40—Low content or no content compositions
- C10N2030/42—Phosphor free or low phosphor content compositions
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- 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
- C10N2030/40—Low content or no content compositions
- C10N2030/43—Sulfur free or low sulfur content compositions
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- 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
- C10N2030/64—Environmental friendly compositions
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Abstract
The invention provides a kind of non-sulphur phosphorus oil-soluble organic molybdenum additive and its preparation method and application, its preparation method comprises the following steps：1) long-chain unsaturation acyl chlorides and pyridine are dissolved in organic solvent A in a reservoir, diethanol amine is added under the conditions of 20 30 DEG C, continue reaction 45 hours to complete reaction at a temperature of 20 30 DEG C and obtain reaction solution, by reacting liquid filtering, organic phase after filtering is washed with cushioning liquid, then is stripped, dried with ethyl acetate, rotated to remove in organic phase and obtain long-chain unsaturated amides after solvent；2) the long-chain unsaturated amides that step 1) obtains are dissolved in organic solvent B, add catalyst, controlling reaction temperature is 90 120 DEG C, add ammonium molybdate aqueous solution, then back flow reaction 78 hours at a temperature of 60 120 DEG C, filtered, vacuum distillation obtain non-sulphur phosphorus oil-soluble organic molybdenum after removing solvent.Non- sulphur phosphorus oil-soluble organic molybdenum of the present invention has good oil-soluble, corrosion resistance and anti-wear and wear-resistant performance.
Description
Technical field
The invention belongs to lube oil additive field, more particularly, to a kind of non-sulphur phosphorus oil-soluble organic molybdenum additive and its
Preparation method and application.
Background technology
As industrial expansion, the whole world are increasing to the demand of lubricating oil.According to statistics, the world moistens since nineteen ninety
The yield of lubricating oil is up to 38,000,000 tons, and the trend development to increase.Along with the high speed development of industry, the lubricating oil in China
There is very big development space in market.
Lube oil additive is the important component of lubricating oil, while is also had to the combination property of lubricating oil important
Influence.Although wherein antifriction additive usage amount is little, the energy-saving and emission-reduction to lubricating oil especially I. C. engine oil play important
Effect, conventional anti-friction agent include organic amine and its derivative, polyol ester, organic-molybdenum etc..In lubricating oil especially internal combustion engine
The friction reducing effect of organic-molybdenum is the most prominent in oil.Molybdenum dialkyl-dithiophosphate (MoDTP), molybdenum dialkyldithiocarbamacompositions
(MoDTC) and non-sulphur phosphorous organic molybdenum additive is the widely used organic molybdenum additive of in the market.According to the study：Dialkyl group
Molybdenum dithiophosphate (MoDTP), molybdenum dialkyldithiocarbamacompositions (MoDTC) this kind of oil-soluble organic molybdenum additive have excellent
Different anti-attrition, abrasion resistance, but can be produced in the production and use process containing sulphur, P elements in both compounds
Noxious pollutant, and serious corrosion can be produced to metal.Non- sulphur phosphorous organic molybdenum additive has good antioxygen, anti-attrition
Can, and not sulfur-bearing, P elements, meet environmental requirement, and this organic molybdenum additive is applied widely, it is a variety of to be added to
In lubricating oil and lubricating grease.
With environmental protection and the continuous improvement of power conservation requirement, the market potential of non-sulphur phosphorous organic molybdenum additive is increasingly
Greatly, the MOLYVAN 855 (molybdenum content 10%) of R.T.Vanderbilt in the market, Ethyl Co. HITEC4716
(molybdenum content 6%) and the Sakura-lube of Asahi Kasei Corporation 700 (molybdenum content 4.4%) represent organic molybdenum additive
Advanced level, but the existing most of organic molybdenum additive of in the market, all there is complex manufacturing, oil-soluble difference to be asked
Topic, therefore, the non-sulphur phosphorous organic molybdenum additive of Development of Novel is imperative.
The content of the invention
In view of this, the present invention is directed to propose a kind of non-sulphur phosphorus oil-soluble organic molybdenum additive and preparation method thereof and should
With to simplify production technology, improving oil-soluble, while strengthen antifriction and abrasion resistance..
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
A kind of non-sulphur phosphorus oil-soluble organic molybdenum additive, its preparation method comprise the following steps：
1) synthesis of long-chain unsaturated amides
Long-chain unsaturation acyl chlorides and pyridine are dissolved in organic solvent A in a reservoir, diethyl is added under the conditions of 20-30 DEG C
Hydramine, continue to react 4-5 hours to complete reaction obtaining reaction solution at a temperature of 20-30 DEG C, by reacting liquid filtering, after filtering
Organic phase washed with cushioning liquid, then be stripped, dried with ethyl acetate, rotated to remove in organic phase and obtain long-chain not after solvent
Saturated amide；
2) synthesis of non-sulphur phosphorus oil-soluble organic molybdenum additive
The long-chain unsaturated amides that step 1) obtains are dissolved in organic solvent B, add catalyst, controlling reaction temperature is
90-120 DEG C, ammonium molybdate aqueous solution is added, then the back flow reaction 7-8 hours at a temperature of 60-120 DEG C, filtered, vacuum distillation
Non- sulphur phosphorus oil-soluble organic molybdenum is obtained after removing solvent.
Preferably, long-chain unsaturation acyl chlorides, pyridine, the mass ratio of diethanol amine in the step 1) are：1：(0.1-
3)：(0.1-2).
Preferably, one in the straight chain unsaturation acyl chlorides that the long-chain unsaturation acyl chlorides in the step 1) is C12-C18
Kind or two or more mixtures.
Preferably, the organic solvent A in the step 1) is benzene, toluene, dichloromethane, petroleum ether, ethyl acetate, trichlorine
The mixture of methane, acetone, one or both of tetrahydrofuran, dimethyl sulfoxide (DMSO) above.
Preferably, the cushioning liquid in the step 1) is that mass percent is 5% sodium bicarbonate aqueous solution, 5% carbonic acid
Sodium water solution, 5% wet chemical, 5% biphosphate sodium water solution, 5% potassium dihydrogen phosphate aqueous solution, 5% phosphoric acid hydrogen two
Mixture more than one or both of sodium water solution, 5% aqueous dibasic potassium phosphate solution.
Preferably, the long-chain unsaturated amides in the step 2), catalyst, the mass ratio of ammonium molybdate are：1：(0.001-
0.03):(0.05-0.5)。
Preferably, the organic solvent B in the step 2) be benzene, toluene, tetrahydrofuran, DMF, N,
Mixture more than one or both of N- dimethyl acetamides, dimethyl sulfoxide (DMSO).
Preferably, the catalyst in the step 2) be ammoniacal liquor, triethylamine, diisopropylethylamine, pyridine, sodium acid carbonate,
Sodium carbonate, potassium carbonate, one or more kinds of mixtures of sodium hydroxide.
The preparation method of above-mentioned non-sulphur phosphorus oil-soluble organic molybdenum additive, comprises the following steps：1) long-chain unsaturated amides
Synthesis
Long-chain unsaturation acyl chlorides and pyridine are dissolved in organic solvent A in a reservoir, diethyl is added under the conditions of 20-30 DEG C
Hydramine, continue to react 4-5 hours to complete reaction obtaining reaction solution at a temperature of 20-30 DEG C, by reacting liquid filtering, after filtering
Organic phase washed with cushioning liquid, then be stripped, dried with ethyl acetate, rotated to remove in organic phase and obtain long-chain not after solvent
Saturated amide；
2) synthesis of non-sulphur phosphorus oil-soluble organic molybdenum additive
The long-chain unsaturated amides that step 1) obtains are dissolved in organic solvent B, add catalyst, controlling reaction temperature is
90-120 DEG C, ammonium molybdate aqueous solution is added, then the back flow reaction 7-8 hours at a temperature of 60-120 DEG C, filtered, vacuum distillation
Non- sulphur phosphorus oil-soluble organic molybdenum is obtained after removing solvent.
Use of the above-mentioned non-sulphur phosphorus oil-soluble organic molybdenum additive as antifriction antiwear agent addition agent in lubricating oil or lubricating grease
On the way.
Preferably, addition of the described non-sulphur phosphorus oil-soluble organic molybdenum additive in lubricating oil or lubricating grease is lubrication
The 0.2%-3% of oil or lubricating grease gross mass.
Relative to prior art, non-sulphur phosphorus oil-soluble organic molybdenum additive of the present invention and its preparation method and application
Have the advantage that：
(1) non-sulphur phosphorus oil-soluble organic molybdenum of the present invention has good oil-soluble, corrosion resistance and antifriction antiwear
Performance；
(2) in the preparation method of non-sulphur phosphorus oil-soluble organic molybdenum additive of the present invention using long-chain unsaturation acyl chlorides as
Initiation material, long-chain unsaturated amides first are prepared with diethanol amine reaction, non-sulphur phosphorus oil-soluble is then obtained with ammonium molybdate reaction
Organic molybdenum additive.The synthetic reaction condition is gentle, and 90-120 DEG C can be smoothed out under catalyst, without high temperature height
Press strip part；Technique post processing is simple, and intermediate can be used in second step reaction without purification, without the separating-purifying of complexity
Process, production technology more clean, are pollution-free.The non-sulphur phosphorus oil-soluble organic molybdenum additive being prepared has well oily molten
Property, corrosion resistance and anti-wear and wear-resistant performance, solve the problems, such as existing product oil-soluble is poor, corrosivity is strong, not environmentally.
Brief description of the drawings
The embodiment 1 that Fig. 1 is 0.5% obtains non-sulphur phosphorus oil-soluble organic molybdenum with being stirred at 0.5% 60 DEG C of commercially available organic-molybdenum
Mix the dissolubility comparison diagram after 1h；
The embodiment 1 that Fig. 2 is 0.5% obtains non-sulphur phosphorus oil-soluble organic molybdenum and 0.5% commercially available organic-molybdenum is placed 10 days
Dissolubility comparison diagram afterwards；
Fig. 3 is that the I. C. engine oil of I. C. engine oil and the commercially available organic-molybdenum of addition 1% and the embodiment 1 of addition 1% obtain
Non- sulphur phosphorus oil-soluble organic molybdenum I. C. engine oil friction coefficient curve.
Embodiment
In addition to being defined, technical term used has universal with those skilled in the art of the invention in following examples
The identical meanings of understanding.Test reagent used, is routine biochemistry reagent unless otherwise specified in following examples；It is described
Experimental method, it is conventional method unless otherwise specified.
The present invention is described in detail with reference to embodiment and accompanying drawing.
Embodiment 1
A kind of non-sulphur phosphorus oil-soluble organic molybdenum additive, its preparation method comprise the following steps：
1) synthesis of coconut oleamide
Coconut oleoyl chloride 31.6g, pyridine 15g are dissolved in 100ml petroleum ethers in three-necked flask, mechanical agitation, in 20-
Under the conditions of 30 DEG C, 12g diethanol amine is added dropwise into reaction system while stirring, 20-30 DEG C of reaction temperature is kept after being added dropwise
Continue to react 4-5 hours, reacted completely using thin-layer chromatography (TLC) monitoring raw material, by reacting liquid filtering, organic phase 50ml matter
Amount fraction is that 5% sodium bicarbonate buffer solution washes twice, then with 20ml ethyl acetate strip aqueous, then with the anhydrous sulphur of 10g
Sour magnesium dries organic phase, and last vacuum rotary steam removes organic solvent and obtains coconut oleamide；
2) synthesis of non-sulphur phosphorus oil-soluble organic molybdenum additive
30g coconut oleamides are dissolved in 70mlN, are placed in dinethylformamide in 250ml three-necked flasks, are added
0.6g triethylamine, mechanical agitation, 90-120 DEG C of controlling reaction temperature, 25g mass point is added dropwise while stirring into reaction system
Number is 20% ammonium molybdate aqueous solution, then the back flow reaction 7-8 hours at 90-120 DEG C, is cooled to less than 50 DEG C, then mistake
The ammonium molybdate not reacted completely is filtered, filtrate obtains blackish green non-sulphur phosphorus oil-soluble organic molybdenum by being evaporated under reduced pressure removing solvent, should
Non- sulphur phosphorus oil-soluble organic molybdenum yield is 92.8%, molybdenum content 6.32%.
Embodiment 2
1st, the synthesis of coconut oleamide
Coconut oleoyl chloride 94.8g and pyridine 45g are dissolved in 300ml tetrahydrofurans in 500ml three-necked flasks, machinery stirs
Mix, under the conditions of 20-30 DEG C, 35.8g diethanol amine is added dropwise into reaction system while stirring, reaction temperature is kept after being added dropwise
20-30 DEG C of degree continues to react 4-5 hours, is reacted completely using thin-layer chromatography (TLC) monitoring raw material, organic by reacting liquid filtering
It is mutually that 5% sodium bicarbonate buffer solution washes twice with 150ml mass fractions, then with 60ml ethyl acetate strip aqueous, then
Organic phase is dried with 20g anhydrous magnesium sulfates, last vacuum rotary steam removes solvent and obtains coconut oleamide；
2nd, the synthesis of non-sulphur phosphorus oil-soluble organic molybdenum additive
90g coconut oleamides are dissolved in 200ml toluene and are placed in 500ml three-necked flasks, mechanical agitation, add 1.8g
Sodium carbonate, control 90-120 DEG C of temperature, be added dropwise while stirring into reaction system 75g mass fractions be 20% ammonium molybdate water
Solution, then the back flow reaction 7-8 hours at 90-120 DEG C, less than 50 DEG C are cooled to, then filter the molybdic acid not reacted completely
The last filtrate of ammonium removes solvent by being evaporated under reduced pressure, and obtains blackish green non-sulphur phosphorus oil-soluble organic molybdenum, the non-sulphur phosphorus oil-soluble has
Machine molybdenum yield is 91.7%, molybdenum content 4.89%.
Embodiment 3
1st, the synthesis of ricinoleamide
Castor-oil plant oleoyl chloride 37.1g and pyridine 15g are dissolved in 100ml petroleum ethers in three-necked flask, mechanical agitation,
Under the conditions of 20-30 DEG C, 12g diethanol amine is added dropwise into reaction system while stirring, reaction temperature 20-30 is kept after being added dropwise
DEG C continue to react 4-5 hours, reacted completely using thin-layer chromatography (TLC) monitoring raw material, by reacting liquid filtering, organic phase quality
Fraction is that 50ml mass fractions are that 5% sodium bicarbonate buffer solution washes twice, then with 20ml ethyl acetate strip aqueous, then
Organic phase is dried with 10g anhydrous magnesium sulfates, last vacuum rotary steam removes solvent and obtains ricinoleamide.
2nd, the synthesis of non-sulphur phosphorus oil-soluble organic molybdenum additive
30g ricinoleamides are dissolved in 70ml toluene and are placed in 250ml three-necked flasks, mechanical agitation, add 0.6g
Sodium carbonate, control 90-120 DEG C of temperature, be added dropwise while stirring into reaction system 25g mass fractions be 20% ammonium molybdate water
Solution, then the back flow reaction 7-8 hours at 90-120 DEG C, less than 50 DEG C are cooled to, then filter the molybdic acid not reacted completely
Ammonium, last filtrate obtain blackish green non-sulphur phosphorus oil-soluble organic molybdenum by being evaporated under reduced pressure removing solvent, and the non-sulphur phosphorus oil-soluble has
Machine molybdenum yield is 90.7%, molybdenum content 5.71%.
The non-sulphur phosphorous organic molybdenum additive can be used as a kind of single dose compounding into compositions of additives, can also be direct
It is added to application and additive capacity in lubricating oil to be recommended as：
(1) addition in I. C. engine oil is：0.2wt%-1wt%；
(2) addition in gear oil is：0.05wt%-0.5wt%；
(3) addition in lubricating grease is：0.2wt%-3wt%.
Dissolubility is tested
The invention product of embodiment 1 is (industrial gear oil, interior in a kind of oil, two classes oil, three classes oil, artificial oil PAO and product oil
Combustion engine oil) in have excellent dissolubility
Cosolvent is free of in industrial gear oil, therefore industrial gear oil requires higher to the oil-soluble of organic molybdenum additive.
It is test crude oil with industrial gear oil (CKC220), is separately added into the invention of embodiment 1 production of 0.5% (mass percent, similarly hereinafter)
The commercially available organic-molybdenum of thing and 0.5% (mass percent, similarly hereinafter), 1h is stirred at 60 DEG C to uniform, the two dissolubility of observation, sees figure
1。
Can intuitively it be found out by Fig. 1, the oil sample for adding the non-sulphur phosphorus oil-soluble organic molybdenum that 0.5% embodiment 1 obtains is clarified, thoroughly
It is bright；And the oil sample for adding 0.5% commercially available organic-molybdenum is muddy, without remarkable improvement after placement 10d, Fig. 2 is seen.As can be seen here, this hair
Bright non-sulphur phosphorus oil-soluble organic molybdenum is more more excellent than the dissolubility of commercially available organic-molybdenum.
Corrosion resistance is tested
Copper corrosion experiment is the JSR2101 types copper corrosion test in Hunan Petro-Chemical Instruments Co., Ltd., Jinshi City
Carried out on instrument.Experimental condition is：121 DEG C, testing time 3h.
The non-sulphur phosphorus oil-soluble organic molybdenum that 1% embodiment 1 is obtained respectively is added to I. C. engine oil 10W-40 and industry
In gear oil CKC220, after experiment carries out 3h, copper sheet is corrosion-free to show generation, and copper corrosion result is 1a levels, it is seen that this hair
Bright non-sulphur phosphorus oil-soluble organic molybdenum has excellent corrosion resistance.
Antifriction performance is tested
(1) antifriction performance is tested in industrial gear oil
Antifriction experiment is what is carried out on the ball frictional testing machines of MS-10A tetra- of Xiamen Tenkey Automation Co., Ltd..Experiment
Condition is：25 DEG C, rotating speed 1200r/min, load 40Kg of room temperature, testing time 32400s.In the microscope that precision is 0.01mm
The wear scar diameter of three steel balls of lower measurement, horizontal survey are averaged three times.Average friction coefficient, maximum temperature rise, average temperature rising
By direct reading on four-ball tester.
Using industrial gear oil CKC220 as test crude oil, the non-sulphur phosphorus oil-soluble organic molybdenum that 0.5% embodiment 1 is obtained
With after 0.5% zinc dialkyl dithiophosphate (ZDDP) compounding and 0.5% commercially available organic-molybdenum and 0.5% ZDDP compoundings points
It is not added in industrial gear oil, the antifriction performance of non-sulphur phosphorus oil-soluble organic molybdenum is evaluated by frictional wear experiment.Test knot
Fruit is as shown in table 1：
The non-sulphur phosphorus oil-soluble organic molybdenum antifriction performance contrast of table 1
As can be seen from Table 1, non-sulphur phosphorus oil-soluble organic molybdenum of the invention and commercially available organic-molybdenum have higher antifriction quality
Energy.
(2) antifriction performance is tested in I. C. engine oil
Experiment is carried out on the SRV5 type friction wear testing machines of German OPTIMAL companies.Experimental condition is：Pressure
200N, temperature 60 C, frequency 50HZ, stroke 2mm, testing time 7200s, the way of contact are linear contact lay.
With I. C. engine oil (SN 10W-40) for test crude oil, the non-sulphur phosphorus oil-soluble that 1% embodiment 1 is obtained is organic
Molybdenum and 1% commercially available organic-molybdenum are added separately in I. C. engine oil.Friction coefficient curve result is shown in Fig. 3, wear scar width and depth
It is shown in Table 2.
The wear scar width of table 2 and depth
| Sample | Grind spot width (mm) | Grind spot depth (um) |
| I. C. engine oil | 0.43 | 1.85 |
| The commercially available organic-molybdenum of I. C. engine oil+1% | 0.44 | 2.16 |
| The non-sulphur phosphorus oil-soluble organic molybdenum of I. C. engine oil+1% | 0.40 | 1.80 |
As seen from Figure 3, after the invention product of embodiment 1 is added to I. C. engine oil (SN 10W-40), described non-sulphur phosphorus
Oil-soluble organic molybdenum additive has the antifriction performance better than prior art.As can be known from the results of Table 2, adding 1% embodiment 1 has
After machine molybdenum, the width and depth that grind spot all decrease.The above results can illustrate that non-sulphur phosphorus oil-soluble proposed by the present invention has
Machine molybdenum has excellent antifriction, abrasion resistance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (10)
- A kind of 1. non-sulphur phosphorus oil-soluble organic molybdenum additive, it is characterised in that：Its preparation method comprises the following steps：1) synthesis of long-chain unsaturated amidesLong-chain unsaturation acyl chlorides and pyridine are dissolved in organic solvent A in a reservoir, diethanol is added under the conditions of 20-30 DEG C Amine, continue to react 4-5 hours to complete reaction obtaining reaction solution at a temperature of 20-30 DEG C, by reacting liquid filtering, after filtering Organic phase is washed with cushioning liquid, then is stripped, dried with ethyl acetate, rotated to remove in organic phase and obtain long-chain insatiable hunger after solvent And acid amides；2) synthesis of non-sulphur phosphorus oil-soluble organic molybdenum additiveThe long-chain unsaturated amides that step 1) obtains are dissolved in organic solvent B, add catalyst, controlling reaction temperature 90- 120 DEG C, ammonium molybdate aqueous solution is added, then the back flow reaction 7-8 hours at a temperature of 60-120 DEG C, filtered, vacuum distillation removes Go after solvent to obtain non-sulphur phosphorus oil-soluble organic molybdenum.
- 2. non-sulphur phosphorus oil-soluble organic molybdenum additive according to claim 1, it is characterised in that：Length in the step 1) Chain unsaturation acyl chlorides, pyridine, the mass ratio of diethanol amine are：1：(0.1-3)：(0.1-2).
- 3. non-sulphur phosphorus oil-soluble organic molybdenum additive according to claim 2, it is characterised in that：Length in the step 1) Mixture more than one or both of straight chain unsaturation acyl chlorides that chain unsaturation acyl chlorides is C12-C18.
- 4. non-sulphur phosphorus oil-soluble organic molybdenum additive according to claim 2, it is characterised in that：Having in the step 1) Solvent A is benzene, toluene, dichloromethane, petroleum ether, ethyl acetate, chloroform, acetone, tetrahydrofuran, in dimethyl sulfoxide (DMSO) One or more kinds of mixtures.
- 5. non-sulphur phosphorus oil-soluble organic molybdenum additive according to claim 2, it is characterised in that：It is slow in the step 1) It is that mass percent is 5% sodium bicarbonate aqueous solution, 5% aqueous sodium carbonate, 5% wet chemical, 5% phosphoric acid to rush solution In dihydro sodium water solution, 5% potassium dihydrogen phosphate aqueous solution, the 5% disodium hydrogen phosphate aqueous solution, 5% aqueous dibasic potassium phosphate solution One or more kinds of mixtures.
- 6. non-sulphur phosphorus oil-soluble organic molybdenum additive according to claim 1, it is characterised in that：Length in the step 2) Chain unsaturated amides, catalyst, the mass ratio of ammonium molybdate are：1：(0.001-0.03):(0.05-0.5).
- 7. non-sulphur phosphorus oil-soluble organic molybdenum additive according to claim 6, it is characterised in that：Having in the step 2) Solvent B is one in benzene, toluene, tetrahydrofuran, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO) Kind or two or more mixtures.
- 8. non-sulphur phosphorus oil-soluble organic molybdenum additive according to claim 6, it is characterised in that：Urging in the step 2) Agent is ammoniacal liquor, triethylamine, diisopropylethylamine, pyridine, sodium acid carbonate, sodium carbonate, potassium carbonate, one kind of sodium hydroxide or two The mixture of the kind above.
- 9. a kind of preparation method of non-sulphur phosphorus oil-soluble organic molybdenum additive, it is characterised in that the preparation method includes as follows Step：1) synthesis of long-chain unsaturated amidesLong-chain unsaturation acyl chlorides and pyridine are dissolved in organic solvent A in a reservoir, diethanol is added under the conditions of 20-30 DEG C Amine, continue to react 4-5 hours to complete reaction obtaining reaction solution at a temperature of 20-30 DEG C, by reacting liquid filtering, after filtering Organic phase is washed with cushioning liquid, then is stripped, dried with ethyl acetate, rotated to remove in organic phase and obtain long-chain insatiable hunger after solvent And acid amides；2) synthesis of non-sulphur phosphorus oil-soluble organic molybdenum additiveThe long-chain unsaturated amides that step 1) obtains are dissolved in organic solvent B, add catalyst, controlling reaction temperature 90- 120 DEG C, ammonium molybdate aqueous solution is added, then the back flow reaction 7-8 hours at a temperature of 60-120 DEG C, filtered, vacuum distillation removes Go after solvent to obtain non-sulphur phosphorus oil-soluble organic molybdenum.
- 10. any described non-sulphur phosphorus oil-soluble organic molybdenum additives of claim 1-9 are as antifriction in lubricating oil or lubricating grease The purposes of antiwear additive；Addition of the described non-sulphur phosphorus oil-soluble organic molybdenum additive in lubricating oil or lubricating grease is lubricating oil Or the 0.2%-3% of lubricating grease gross mass.
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