CN104263461A - Ceramic alloy composite functional coupling agent and preparation method thereof - Google Patents
Ceramic alloy composite functional coupling agent and preparation method thereof Download PDFInfo
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- CN104263461A CN104263461A CN201410527528.4A CN201410527528A CN104263461A CN 104263461 A CN104263461 A CN 104263461A CN 201410527528 A CN201410527528 A CN 201410527528A CN 104263461 A CN104263461 A CN 104263461A
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Abstract
The invention discloses a ceramic alloy composite functional coupling agent and a preparation method of the ceramic alloy composite functional coupling agent. The coupling agent is prepared from mixed sulphur amine phosphate ester, molybdenum oxide, carbonic acid rare earth, boric acid and calcium sulfonate of 100 to 4.5-5 to 4.5-5 to 12-17 to 12-17; the mixed sulphur amine phosphate ester is prepared by reacting coconut fatty acid and triethanolamine with phosphorus pentasulfide and capryl alcohol. The addictive is an oil-soluble ceramic alloy composite functional coupling agent and can be used as a friction improver, an anti-wear agent and a clearing agent for lubricating oil specially for internal combustion engines, so that the oil-saving effect is obvious; moreover, the addictive also has the advantages of energy conservation and environmental protection because of rare earth elements and low-sulphur low-phosphorous chloride-free contents.
Description
Technical field
The invention belongs to the field of chemical synthesis, relate in particular to a kind of oil soluble ionic ceramal complex function couplant and preparation method thereof.
Background technology
Have motion just to have friction, have friction just to have lubrication, the main body of this lubrication is exactly lubricating oil and lubricating grease, and current lubricating oil, fat prod are almost applied to national economy every field, is the blood of industry park plan.From communications and transportation, intermetallic composite coating, motive power machine equipment, invariably relate to building, each electric appliances etc.Since half a century, along with the continuous renewal of mechanical means, its range of application constantly expands, and depends merely on lubricating oil, fat prod that refining of petroleum processes, can not meet requirement objectively performance far away.For this reason, in each class lubricating oil, fat prod, add additive, to improve the particular requirement under various different application situation, improve use properties.Through application and practice for many years, lubricating oil, fat additives have become the economy and effective important means that improve oil product use properties and improve oil quality.Over nearly 20 years, research that is wear-resistant for environment-friendly type, extreme-pressure additive achieves many theoretical results, as novel upgraded product organic-molybdenum, nitrogen-containing borate etc. are better than traditional zinc dialkyl dithiophosphate (ZDDP), nanometer additive etc. far away in performance.
Ceramal additive domestic, external is at present all solid nano type, and with dispersant in lubricating oil, the time has been grown and can precipitate.
Such as, Chinese invention patent publication number CN1765803 discloses a kind of metal/ceramic nano composite additive of self-rehabilitation and preparation method thereof, belong to nanoparticle suspension technology, in addition, Chinese invention patent publication number CN101186856 discloses a kind of for lubricating oil nano-stage ceramic metal additive and preparation; Chinese invention patent publication number CN1324922 discloses a kind of sintering metal lubricant and manufacture method thereof, this lubricant is made up of the slip additive of 5 ~ 15% and the carrier fluid of 85 ~ 95%, wherein slip additive is formed by Nano metal powder, nano-ceramic powder and dispersion agent Homogeneous phase mixing, these three kinds of methods remain in larger defect due to the dispersion technology of nanoparticle in lubricating oil, therefore all remain to be further improved.US Patent No. 4,844,825 disclose a kind of based on the extreme-pressure additive of chlorination petroleum wax, effectively can improve the lubrication anti-friction performance of oil engine, but in order in and the metallic corrosion that causes of muriate, a large amount of alkaline sulfonate must be added, make sulphur content cannot lower than 1%.US Patent No. 7,423,000 extreme-pressure additive disclosing a kind of not phosphorous and metallic compound, but cannot invariably use sulfur-bearing additive.US Patent No. 6,588, the 393 metal tripolyphosphate compound extreme-pressure additives disclosing a kind of low sulfur content (5-250ppm), although sulphur content is extremely low, phosphorus content cannot reach GF-4, GF-5 standard.
Summary of the invention
The object of the present invention is to provide ceramal complex function couplant that a kind of production method is simple, cost is low, oil soluble is good, productive rate is high and preparation method thereof, this additive is a kind of oil soluble ceramal complex function couplant, be the lubricating oil particularly friction improver of I. C. engine lubricating oil, anti-wear agent and purification agent, oil-saving effect is remarkable.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of ceramal complex function couplant, and described couplant is prepared from by mix sulphur phosphamide ester, molybdenum oxide, carbonated rare earth, boric acid, calcium sulphonate; Wherein the weight ratio of mix sulphur phosphamide ester and molybdenum oxide, carbonated rare earth, boric acid, calcium sulphonate is: 100:4.5 ~ 5:4.5 ~ 5:12 ~ 17:12 ~ 17, mix sulphur phosphamide ester is reacted by cocinic acid, trolamine and thiophosphoric anhydride, octanol to be made.
The mol ratio of described mix sulphur phosphamide ester component is cocinic acid: trolamine: thiophosphoric anhydride: octanol=2 ~ 3:3 ~ 5:1 ~ 1.5:2 ~ 2.5.
The raw material weight of described couplant is than being mix sulphur phosphamide ester: molybdenum oxide: carbonated rare earth: boric acid: calcium sulphonate=100:5:5:16:17; The mol ratio of mix sulphur phosphamide ester component is cocinic acid: trolamine: thiophosphoric anhydride: octanol=2:3.5:1:2.
The preparation method of above-mentioned ceramal complex function couplant, comprises the following steps:
1) synthesis of mix sulphur phosphamide ester
Cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4 ~ 5 hours under the condition of 90 DEG C ~ 100 DEG C of vacuum, then trolamine is added, between adjustment pH=7.5 ~ 8.5, under nitrogen protection condition, be 100 ~ 110 DEG C in temperature and continue reaction 3 ~ 4 hours, obtain mix sulphur phosphamide ester;
2) synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester of above-mentioned preparation is mixed with molybdenum oxide, carbonated rare earth, adds boric acid after stirring, add calcium sulphonate, under temperature 90 ~ 100 DEG C, pressure 0.2MPa condition, react 4 ~ 5 hours; Heighten temperature to 180 ~ 190 DEG C, continue reaction under pressure permanence condition 3 ~ 4 hours, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa, extract lower boiling material out; Finally filter, obtain yellow ceramal coupling recombiner.
The condition of the vacuum in mix sulphur phosphamide Lipase absobed step is 0.098 ~ 0.1MPa.
When synthesizing mix sulphur phosphamide ester, after adding trolamine, adjust pH=8.
The invention has the beneficial effects as follows: in the present invention, first react with thiophosphoric anhydride, octanol based on cocinic acid, add trolamine again, adopt the method for adjust ph, obtain the mix sulphur phosphamide ester being conducive to lower step sound response, then react with molybdenum oxide and carbonated rare earth, adopt when adding boric acid, calcium sulphonate two step pressure applications to make rare earth and boron, molybdenum content reach optimum value, rare earth and boron nitride Stability Analysis of Structures, thus make the ceramal complex function couplant with good lubricating properties and splendid resistance to abrasion.It is low-phosphorous without the efficient advantage of chlorine environmental-protecting that ceramal complex function couplant provided by the invention has energy-conservation low-sulfur.
Embodiment
Ceramal complex function couplant of the present invention, described couplant is prepared from by mix sulphur phosphamide ester, molybdenum oxide, carbonated rare earth, boric acid, calcium sulphonate; Wherein the weight ratio of mix sulphur phosphamide ester and molybdenum oxide, carbonated rare earth, boric acid, calcium sulphonate is: 100:4.5 ~ 5:4.5 ~ 5:12 ~ 17:12 ~ 17, mix sulphur phosphamide ester is reacted by cocinic acid, trolamine and thiophosphoric anhydride, octanol to be made.
The mol ratio of described mix sulphur phosphamide ester component is cocinic acid: trolamine: thiophosphoric anhydride: octanol=2 ~ 3:3 ~ 5:1 ~ 1.5:2 ~ 2.5.
The raw material weight of described couplant is than being mix sulphur phosphamide ester: molybdenum oxide: carbonated rare earth: boric acid: calcium sulphonate=100:5:5:16:17; The mol ratio of mix sulphur phosphamide ester component is cocinic acid: trolamine: thiophosphoric anhydride: octanol=2:3.5:1:2.
The preparation method of above-mentioned ceramal complex function couplant, comprises the following steps:
1) synthesis of mix sulphur phosphamide ester
Cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4 ~ 5 hours under the condition of 90 DEG C ~ 100 DEG C of vacuum, then trolamine is added, between adjustment pH=7.5 ~ 8.5, under nitrogen protection condition, be 100 ~ 110 DEG C in temperature and continue reaction 3 ~ 4 hours, obtain mix sulphur phosphamide ester;
2) synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester of above-mentioned preparation is mixed with molybdenum oxide, carbonated rare earth, adds boric acid after stirring, add calcium sulphonate, under temperature 90 ~ 100 DEG C, pressure 0.2MPa condition, react 4 ~ 5 hours; Heighten temperature to 180 ~ 190 DEG C, continue reaction under pressure permanence condition 3 ~ 4 hours, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa, extract lower boiling material out; Finally filter, obtain yellow ceramal coupling recombiner.
The condition of the vacuum in mix sulphur phosphamide Lipase absobed step is 0.098 ~ 0.1MPa.
When synthesizing mix sulphur phosphamide ester, after adding trolamine, adjust pH=8.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
1, the synthesis of mix sulphur phosphamide ester
Cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4 hours under 100 DEG C of vacuum (pressure=0.10MPa) condition, then add trolamine, adjustment pH=8, under nitrogen protection condition, at 100 DEG C, continue reaction 3 hours, obtain mix sulphur phosphamide ester;
Cocinic acid: trolamine: thiophosphoric anhydride: octanol=2:3.5:1:2 (mol ratio).
2, the synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester 50 grams of above-mentioned preparation is mixed with molybdenum oxide 2.5 grams, carbonated rare earth 2.5 grams, after stirring, adds boric acid 8 grams, add 8 grams of calcium sulphonate, react 4 hours under temperature 90 DEG C, pressure 0.2MPa condition; Heighten temperature to 180 DEG C, continue reaction under pressure permanence condition 3 hours.Then lower the temperature 100 DEG C, being evacuated to pressure is 0.1MPa, extracts lower boiling material out; Finally filter, obtain yellow ceramal complex function couplant product.
The antifriction antiwear of product and the investigation of supporting capacity: utilize four-ball tester to measure, setting load (temperature 20 DEG C, load 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, four-ball test steel ball used is the GCR steel ball of diameter 12.7mm, and test shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm.Add 1% (weight) the present embodiment preparing product in lubricating oil, wear scar diameter reaches 0.34mm, frictional coefficient 0.02.
Embodiment 2
1, the synthesis of mix sulphur phosphamide ester
Cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4 hours under 100 DEG C of vacuum (pressure=0.10MPa) condition, then add trolamine, adjustment pH=8, under nitrogen protection condition, at 100 DEG C, continue reaction 3 hours, obtain mix sulphur phosphamide ester;
Cocinic acid: trolamine: thiophosphoric anhydride: octanol=2:3:1:2.5 (mol ratio).
2, the synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester 100 grams of above-mentioned preparation is mixed with molybdenum oxide 4.5 grams, carbonated rare earth 4.5 grams, after stirring, adds boric acid 17 grams, add 17 grams of calcium sulphonate, react 5 hours under temperature 90 DEG C, pressure 0.2MPa condition; Heighten temperature to 180 DEG C, continue reaction under pressure permanence condition 4 hours.Then lower the temperature 100 DEG C, being evacuated to pressure is 0.1MPa, extracts lower boiling material out; Finally filter, obtain yellow ceramal complex function couplant product.
The antifriction antiwear of product and the investigation of supporting capacity, with embodiment 1, by contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm, add product prepared by 1% (weight) the present embodiment in lubricating oil, wear scar diameter reaches 0.32mm, frictional coefficient 0.018.
Embodiment 3
1, the synthesis of mix sulphur phosphamide ester
Cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4.5 hours under 100 DEG C of vacuum (pressure=0.10MPa) condition, then add trolamine, adjustment pH=8.5, under nitrogen protection condition, at 100 DEG C, continue reaction 3 hours, obtain mix sulphur phosphamide ester;
Cocinic acid: trolamine: thiophosphoric anhydride: octanol=2:3.5:1:2 (mol ratio).
2, the synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester 70 grams of above-mentioned preparation is mixed with molybdenum oxide 3.4 grams, carbonated rare earth 3.4 grams, after stirring, adds boric acid 11 grams, add 11 grams of calcium sulphonate, react 4 hours under temperature 90 DEG C, pressure 0.2MPa condition; Heighten temperature to 180 DEG C, continue reaction under pressure permanence condition 4 hours.Then lower the temperature 100 DEG C, being evacuated to pressure is 0.1MPa, extracts lower boiling material out; Finally filter, obtain ceramal complex function couplant product.
The antifriction antiwear of product and the investigation of supporting capacity, with embodiment 1, by contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm, add product prepared by this 1% (weight) embodiment in lubricating oil, wear scar diameter reaches 0.33mm, frictional coefficient 0.025.
Embodiment 4
1, the synthesis of mix sulphur phosphamide ester
Cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4 hours under 100 DEG C of vacuum (pressure=0.10MPa) condition, then add trolamine, adjustment pH=7.5, under nitrogen protection condition, at 100 DEG C, continue reaction 3 hours, obtain mix sulphur phosphamide ester;
Cocinic acid: trolamine: thiophosphoric anhydride: octanol=3:3.5:1:2 (mol ratio).
2, the synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester 200 grams of above-mentioned preparation is mixed with molybdenum oxide 10 grams, carbonated rare earth 10 grams, after stirring, adds boric acid 34 grams, add 33 grams of calcium sulphonate, react 5 hours under temperature 100 DEG C, pressure 0.2MPa condition; Heighten temperature to 180 DEG C, continue reaction under pressure permanence condition 4 hours.Then lower the temperature 100 DEG C, being evacuated to pressure is 0.1MPa, extracts lower boiling material out; Finally filter, obtain yellow ceramal complex function couplant product.
The antifriction antiwear of product and the investigation of supporting capacity, with embodiment 1, by contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm, add product prepared by 1% (weight) the present embodiment in lubricating oil, wear scar diameter reaches 0.36mm, frictional coefficient 0.028.
Embodiment 5
1, the synthesis of mix sulphur phosphamide ester
Castor-oil plant cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4 hours under 100 DEG C of vacuum (pressure=0.10MPa) condition, then trolamine is added, adjustment pH=8.5, under nitrogen protection condition, at 100 DEG C, continue reaction 4 hours, obtain mix sulphur phosphamide ester;
Cocinic acid: trolamine: thiophosphoric anhydride: octanol=1:3:1:2 (mol ratio).
2, the synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester 100 grams of above-mentioned preparation is mixed with molybdenum oxide 5 grams, carbonated rare earth 5 grams, after stirring, adds boric acid 16 grams, add 17 grams of calcium sulphonate, react 4 hours under temperature 90 DEG C, pressure 0.2MPa condition; Heighten temperature to 180 DEG C, continue reaction under pressure permanence condition 3 hours.Then lower the temperature 100 DEG C, being evacuated to pressure is 0.1MPa, extracts lower boiling material out; Finally filter, obtain yellow ceramal complex function couplant product.
The antifriction antiwear of product and the investigation of supporting capacity are with embodiment 1, and by contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm.Add 1% (weight) the present embodiment preparing product in lubricating oil, wear scar diameter reaches 0.30mm, frictional coefficient 0.017.
Ceramal complex function couplant of the present invention is dissolved in various lubricant in liquid form, under lubricating component nominal situation, is formed a kind ofly have antifriction, the physics of wear-resistant effect, chemisorbed film at friction surface; Under the operating mode that high speed, high temperature, high pressure etc. are harsh, chemical alloying reaction film is formed at surface of friction pair, metallic surface is stacked and placed on stratiform microlitic structure, under suitable friction condition, multiple element interacts, make frictional diffusion, play " friction catalysis " effect, and form multiple element friction co-penetration layer, and then accelerate its scattering and permeating, engaging friction secondary surface, improve the grain boundary structure of original metallic substance, occupy the sites of surface metal, generate displacement or gap Solid solution, at the pervious course that metallic surface formative tissue structure is different from matrix.This osmotic layer configurations, belongs to advanced precedent in the world.
Ceramal complex function couplant of the present invention is that be the liquefied compound of ionic, oil soluble is good, precipitates never rare earth element together with boron nitride, molybdenum oxide, low-sulfur, low-phosphorous organic synthesis.Experimental data shows, this ceramal complex function couplant is added in engine oil, frictional coefficient can be reduced to less than 0.03 (frictional coefficient of conventional engine oil is more than 0.08), the long experiment that rubs in 60 minutes of four-ball tester 40 kgf, wear scar diameter only has 0.34mm (wear scar diameter of conventional engine oil is about 0.50), temperature reaches 50 degree, no longer continues to raise.The experiment of small friction machine modularized experiment machine can sustain 16 pieces of stone rollers above (can only the sustaining 2 pieces of stone rollers of conventional engine oil), so use ceramal complex function couplant can reach following effect
1, frictional coefficient is reduced: can more than 60% be reduced.
2, reduce engine temperature: when adopting common lubricant oil additive, engine temperature can reach about 170 DEG C, adds additive of the present invention, the temperature of engine just no longer raises to 50 degree.
3, fuel oil is saved: can fuel-economizing more than 10%.
4, the drain period is extended: 10000 kilometers or more more oil changes can be extended to.
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (6)
1. a ceramal complex function couplant, is characterized in that, described couplant is prepared from by mix sulphur phosphamide ester, molybdenum oxide, carbonated rare earth, boric acid, calcium sulphonate; Wherein the weight ratio of mix sulphur phosphamide ester and molybdenum oxide, carbonated rare earth, boric acid, calcium sulphonate is: 100:4.5 ~ 5:4.5 ~ 5:12 ~ 17:12 ~ 17, mix sulphur phosphamide ester is reacted by cocinic acid, trolamine and thiophosphoric anhydride, octanol to be made.
2. ceramal complex function couplant according to claim 1, is characterized in that, the mol ratio of described mix sulphur phosphamide ester component is cocinic acid: trolamine: thiophosphoric anhydride: octanol=2 ~ 3:3 ~ 5:1 ~ 1.5:2 ~ 2.5.
3. ceramal complex function couplant according to claim 2, is characterized in that, the raw material weight of described couplant is than being mix sulphur phosphamide ester: molybdenum oxide: carbonated rare earth: boric acid: calcium sulphonate=100:5:5:16:17; The mol ratio of mix sulphur phosphamide ester component is cocinic acid: trolamine: thiophosphoric anhydride: octanol=2:3.5:1:2.
4. a preparation method for the ceramal complex function couplant as described in any one of claim 1-3, is characterized in that, comprise the following steps:
1) synthesis of mix sulphur phosphamide ester
Cocinic acid and thiophosphoric anhydride, octanol are placed in container, react 4 ~ 5 hours under the condition of 90 DEG C ~ 100 DEG C of vacuum, then trolamine is added, between adjustment pH=7.5 ~ 8.5, under nitrogen protection condition, be 100 ~ 110 DEG C in temperature and continue reaction 3 ~ 4 hours, obtain mix sulphur phosphamide ester;
2) synthesis of ceramal complex function couplant
The mix sulphur phosphamide ester of above-mentioned preparation is mixed with molybdenum oxide, carbonated rare earth, adds boric acid after stirring, add calcium sulphonate, under temperature 90 ~ 100 DEG C, pressure 0.2MPa condition, react 4 ~ 5 hours; Heighten temperature to 180 ~ 190 DEG C, continue reaction under pressure permanence condition 3 ~ 4 hours, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa, extract lower boiling material out; Finally filter, obtain yellow ceramal coupling recombiner.
5. the preparation method of ceramal complex function couplant according to claim 4, is characterized in that, the condition of the vacuum in mix sulphur phosphamide Lipase absobed step is 0.098 ~ 0.1MPa.
6. the preparation method of ceramal complex function couplant according to claim 4, is characterized in that, when synthesizing mix sulphur phosphamide ester, adjusts pH=8 after adding trolamine.
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CN106167730A (en) * | 2016-07-13 | 2016-11-30 | 蚌埠市华科机电有限责任公司 | A kind of environmental protection wearproof lubricant |
CN106190476A (en) * | 2016-07-13 | 2016-12-07 | 蚌埠市华科机电有限责任公司 | A kind of bearing oil |
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CN106167730A (en) * | 2016-07-13 | 2016-11-30 | 蚌埠市华科机电有限责任公司 | A kind of environmental protection wearproof lubricant |
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