CN1442471A - Preparation method of microporous composite additive - Google Patents
Preparation method of microporous composite additive Download PDFInfo
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- CN1442471A CN1442471A CN 03116171 CN03116171A CN1442471A CN 1442471 A CN1442471 A CN 1442471A CN 03116171 CN03116171 CN 03116171 CN 03116171 A CN03116171 A CN 03116171A CN 1442471 A CN1442471 A CN 1442471A
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- rare earth
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Abstract
A micropore-type composite additive is prepared through loading thermomedium oil in heating container, heating to 50-70 deg.C, adding dispersing, circulation stirring by gear pump, cooling to 15-30 deg.C, adding RE pwoder, fining by said gear pump, heating to 210-240 deg.C, adding perfluorohydrocarbon, mechanicochemical treating, adding assistant and graphite powder, and circulation stirring by gear pump. Its advantages are low cost, micropore structure, good dispersity in oil, and optimal extreme pressure, antiwear and energy-saving actions.
Description
Technical field
That the present invention relates to is a kind of preparation method of composite additive, and the preparation method of particularly a kind of microporous type submicron and nano combined additive belongs to the material field.
Background technology
Micron or nano material are used as solid lubricant in recent years and are widely used in the lubricating oil, find by literature search, China Patent No. is ZL98123519.0, patent name is: nano size rare earth fluoride lubricant oil additive, this patent disclosure a kind of nano lubricating oil additive, its prescription is for water-solubility rare-earth inorganic salt 10-20, dispersion agent 10-30, Si Ben-800.1-5, promotor 10-30, base oil 40-60, Sodium Fluoride 2-5, above-mentioned formula rate is weight percentage, and its preparation method comprises: according to the above ratio water-soluble inorganic salt is dissolved in the water, with dispersion agent, tensio-active agent, promotor, base oil is mixed into portion, mixes with benzene again, in stirred in water bath half hour, slowly drip Sodium Fluoride, stirred in water bath 5-10 hour, decompression removed benzene and water substance again.
This patent is by carrying out finishing to nano size rare earth fluoride, improved its dispersing property in lubricating oil, the good friction performance of utilizing rare earth fluoride itself with and the secondary microgap import feature of good friction of nanoscale, improved the wear-resistant and extreme pressure property of this additive.Yet, this additive is prepared in water-bath by chemical process, technological process is comparatively complicated, the production cost height, and resultant is single rare earth fluoride, fail to give full play to rare earth metal itself and the good tribological property of rare earth compound (or complex compound), the nano size rare earth fluoride particle that this patent is described, do not possess micropore (oil storage) structure, thereby in case be under extreme pressure or the oil-free lubricatoin state, the rolling effect of nano particle will be because of lacking the oiliness passivation, and its wear-resistant and extreme pressure effect will be restricted.In addition, owing to surface of friction pair roughness size is a submicron-scale much larger than nanoscale often, the simple nanoscale material of this patent preparation can't be given full play to its antifriction, wear-resistant and extreme pressure property.Do not see the submicron of relevant microvoid structure and the bibliographical information of nano solid lubricant in the retrieval as yet.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, the preparation method of a kind of microporous type submicron and nano combined additive is provided, make its technological process simple, reduce production costs, the additive of preparation has microvoid structure, good dispersing property is arranged in oil product, have splendid extreme pressure, antiwear and antifriction, energy-saving and environmental protection and repair simultaneously.
Component and weight percent thereof that microporous type submicron and nano combined additive comprise are: rare earth powder 1-10%, graphite powder 1-10%, dispersion agent 1-20%, heat kerosene 60-90%, perfluoroparaffin 1-20%, surplus: auxiliary agent.
The present invention is achieved by the following technical solutions, the preparation method of microporous type submicron of the present invention and nano combined additive, adopt heating container, be used to circulate, the hydraulic oil pump equipment such as (preferred toothed gear pumps) of stirring, refinement and the rubbing effect of generation extreme pressure, concrete steps are as follows:
1) heat kerosene is poured in the heating container, when being heated to 50-70 degree centigrade dispersion agent is poured in the heating agent, stop heating, stir until the dispersion agent uniform distribution by pump housing circulation;
2) treat that the heat kerosene temperature reduces to room temperature 15-30 degree centigrade, the rare earth powder evenly poured in the heat kerosene, powder is carried out the oil bath thinning processing by the engagement of pump, sampling Detection rare earth metal particulate granularity, until granularity in 500 nanometers-1 micrometer range;
3) be heated to 210-240 degree centigrade, keep temperature, add perfluoroparaffin, utilize the hyperpressure hyperthermal friction chemical reaction of the engagement simulation friction pair of toothed gear pump, rare earth powder after the refinement is carried out mechanochemistry handle, the granularity and the shape of sampling Detection rare earth compound (or complex compound) are until granularity uniform distribution between the 50-600 nanometer, be shaped as porous spherical or elliposoidal structure, stop heating;
4) add auxiliary agent and graphite powder, circulation is stirred, until being uniformly dispersed.
In the preparation process of additive of the present invention, the engagement of toothed gear pump forms the lubricated district of an instantaneous high pressure hertz, in this high-tension lubrication district, produce instantaneous pressure and high temperature because of mechanical presses around the granular thulium, thulium is with instant melting and generate rare earth compound (or complex compound), and the organic solvent around it also is vaporized simultaneously and it is produced impact, like this, when toothed gear pump broke away from high pressure hertz district, cure shrinkage formed sphere to rare earth compound (or complex compound) and produce micropore on inner and surface because temperature moment reduces.The rare earth compound (or complex compound) that above-mentioned technology forms is the porous spherical structure after testing, and granularity is uniform distribution between the 50-600 nanometer.The characteristics of this structure at first are to store finish more; under the extreme pressure state; this structure can discharge finish by distortion and play the rolling lubrication effect; secondly; because the relative solid material density of porous structure material is less; thereby good suspension property arranged; anti-deposition capability in oil product is strengthened greatly; solved dispersion and the anti-deposition capability of submicron-scale particle in oil product; in addition; because granularity uniform distribution in the 50-600 nanometer range of additive of the present invention; thereby; the particle that granularity is big can play the rolling lubrication effect on big roughness surface; reduced frictional force, when friction pair was in the extreme pressure state, big rare earth particle was because its shear-stress is less; further refinement and play the extreme pressure provide protection again, and the little particle of granularity can in time import to microgap and be filled into play in the initial crack wear-resistant; extreme pressure; repair and the effect of reinforcement matrix.In addition, nano rare earth metal and compound thereof (or complex compound) particle can form red-hot central point in oil inflame, promote abundant burning big, that cold oil drips greatly, and then improve combustion efficiency of fuel oil and reduce the nuisance growing amount, play energy-conservation and environmental-protection function.
The present invention has substantive distinguishing features and marked improvement, compares with the preparation of chemical bath method, and the method for temperature control oil bath mechanochemistry preparation of the present invention, processing units is few, and technology is simple, the amplitude broad of processing parameter, operation easily.The circulation of toothed gear pump, refinement, extreme pressure state simulation, the preparation and the organic decoration of submicron and nanometer are integrated, the additive that generates is multiple solid lubricants such as rare earth metal, rare earth fluorine, rare earth oxide and rare-earth complex, yardstick also is a uniform distribution between submicron and nanometer, and the structure of additive granules is microporous type as mentioned above, this be the chemical bath preparation method can't finish.
Embodiment
Provide following examples in conjunction with content of the present invention:
Embodiment 1
600 gram heat kerosenes are poured in the heating container, when being heated to 50 degrees centigrade 200 gram dispersion agent iso-butylene succimides are poured in the heating agent, stop heating, stir until the dispersion agent uniform distribution by pump housing circulation; Treat that the heat kerosene temperature reduces to 20 degrees centigrade of room temperatures, 10 gram lanthanums, cerium metal powder are evenly poured in the heat kerosene, by toothed gear pump powder is carried out the oil bath thinning processing, sampling Detection rare earth metal particulate granularity is until granularity during in 500 nanometers; Be heated to 240 degrees centigrade, keep temperature, add 10 gram perfluoroparaffins, rare earth powder after utilizing toothed gear pump to refinement carries out mechanochemistry to be handled, the granularity and the shape of sampling Detection rare earth compound (or complex compound), at 50 nanometer uniform distribution, be shaped as porous spherical or elliposoidal structure until granularity, stop heating; Add 80 gram auxiliary agents and 100 gram graphite, circulation is stirred, until being uniformly dispersed; Be added in the lubricating oil in 1: 50 ratio.
Useful effect:
Submicron with microvoid structure among the embodiment 1 and nano combined additive adding whiteruss are carried out bite-resistant, the experiment of abrasion resistance four-ball tester, and compare with the ZDDP extreme-pressure additive, the result is as shown in table 1.
Table 1 embodiment 1 different additive Pb value and abrasion resistance (WSD) contrast
| Additive | Concentration (WT%) | Pb value (N) | ????WSD ????(mm) | Remarks |
| Whiteruss | ????100 | ????383 | ????0.69 | Four-ball tester operational conditions: load: 390N time: 30min rotating speed: 1450rpm |
| The present invention | ????2 | ????760 | ????0.42 | |
| ????3 | ????780 | ????0.38 | ||
| ????4 | ????780 | ????0.48 | ||
| ZDDP | ????1 | ????780 | ????0.50 |
Embodiment 2
900 gram heat kerosenes are poured in the heating container, when being heated to 70 degrees centigrade the high-alkali calcium mahogany sulfonate of 10 gram dispersion agents is poured in the heating agent, stop heating, stir until the dispersion agent uniform distribution by pump housing circulation; Treat that the heat kerosene temperature reduces to 15 degrees centigrade of room temperatures, 10 gram lanthanums, cerium metal powder are evenly poured in the heat kerosene, by toothed gear pump powder is carried out the oil bath thinning processing, sampling Detection rare earth metal particulate granularity is until granularity during at 1 micron; Be heated to 210 degrees centigrade, keep temperature, add 10 gram perfluoroparaffins, rare earth powder after utilizing toothed gear pump to refinement carries out mechanochemistry to be handled, the granularity and the shape of sampling Detection rare earth compound (or complex compound), until granularity uniform distribution between 400 nanometers, be shaped as porous spherical or elliposoidal structure, stop heating; Add 60 gram auxiliary agents and 10 gram graphite, circulation is stirred, until being uniformly dispersed; Be added in the lubricating oil in 1: 50 ratio.
Useful effect:
Submicron with microvoid structure among the embodiment 2 and nano combined additive adding whiteruss are carried out bite-resistant, the experiment of abrasion resistance four-ball tester, and compare with the ZDDP extreme-pressure additive, the result is as shown in table 2.
Table 2 embodiment 2 different additive Pb values and abrasion resistance (WSD) contrast
| Additive | Concentration (WT%) | Pb value (N) | ????WSD ????(mm) | Remarks |
| Whiteruss | ????100 | ????383 | ????0.69 | Four-ball tester operational conditions: load: 390N time: 30min rotating speed: 1450rpm |
| The present invention | ????2 | ????795 | ????0.40 | |
| ????3 | ????792 | ????0.35 | ||
| ????4 | ????778 | ????0.42 | ||
| ZDDP | ????1 | ????780 | ????0.50 |
Embodiment 3
700 gram heat kerosenes are poured in the heating container, when being heated to 60 degrees centigrade 50 gram dispersion agent alkyl sodium salicylates are poured in the heating agent, stop heating, stir until the dispersion agent uniform distribution by pump housing circulation; Treat that the heat kerosene temperature reduces to 30 degrees centigrade of room temperatures, 20 gram lanthanums, cerium metal powder are evenly poured in the heat kerosene, by toothed gear pump powder is carried out the oil bath thinning processing, sampling Detection rare earth metal particulate granularity is until granularity during at 0.5 micron; Be heated to 230 degrees centigrade, keep temperature, add 200 gram perfluoroparaffins, rare earth powder after utilizing toothed gear pump to refinement carries out mechanochemistry to be handled, the granularity and the shape of sampling Detection rare earth compound (or complex compound), at 300 nanometer uniform distribution, be shaped as porous spherical or elliposoidal structure until granularity, stop heating; Add 100 gram auxiliary agents and 20 gram graphite, circulation is stirred, until being uniformly dispersed; Be added in the fuel oil in 1: 5000 ratio.
Useful effect:
To carry out 72 hours blank contrast combustion experiments of Industrial Boiler in submicron with microvoid structure among the embodiment 3 and the nano combined additive adding residual oil fuel, the result is as shown in table 3.
72 hours blank contrast results of combustion tests of table 3 embodiment 3 Industrial Boilers
| Blank test | Add the agent test | |
| Oil tank liquid level starting altitude (m) | ????4.25 | ????4.23 |
| Oil tank liquid level (m) during off-test | ????2.10 | ????2.37 |
| Oil fuel reduces number (ton) | ????38.24 | ????33.38 |
| Quantity of steam (ton) takes place | ????529.13 | ????495.48 |
| The quantity of steam S that the unit residual oil combustion obtains | ????13.84 | ????14.84 |
| Funnel temperature (℃) | ????344.4 | ????333.1 |
| The rate of economizing gasoline of oil fuel | ??(13.84/13.84-1)*100％＝7.2％ | |
Embodiment 4
750 gram heat kerosenes are poured in the heating container, when being heated to 60 degrees centigrade 100 gram dispersion agent calcium sulfenyl phenolates are poured in the heating agent, stop heating, stir until the dispersion agent uniform distribution by pump housing circulation; Treat that the heat kerosene temperature reduces to 20 degrees centigrade of room temperatures, 100 gram lanthanums, cerium metal powder are evenly poured in the heat kerosene, by toothed gear pump powder is carried out the oil bath thinning processing, sampling Detection rare earth metal particulate granularity is until granularity during in 900 nanometers; Be heated to 220 degrees centigrade, keep temperature, add 30 gram perfluoroparaffins, rare earth powder after utilizing toothed gear pump to refinement carries out mechanochemistry to be handled, the granularity and the shape of sampling Detection rare earth compound (or complex compound), at 600 nanometer uniform distribution, be shaped as porous spherical or elliposoidal structure until granularity, stop heating; Add 5 gram auxiliary agents and 15 gram graphite, circulation is stirred, until being uniformly dispersed; Be added in the fuel oil in 1: 5000 ratio.
Useful effect:
To carry out 72 hours blank contrast combustion experiments of Industrial Boiler in submicron with microvoid structure among the embodiment 4 and the nano combined additive adding residual oil fuel, the result is as shown in table 4.
72 hours blank contrast results of combustion tests of table 4 embodiment 4 Industrial Boilers
| Blank test | Add the agent test | |
| Oil tank liquid level starting altitude (m) | ????4.25 | ????4.25 |
| Oil tank liquid level (m) during off-test | ????1.63 | ????2.00 |
| Oil fuel reduces number (ton) | ????48.14 | ????40.40 |
| Quantity of steam (ton) takes place | ????650.05 | ????590.83 |
| The quantity of steam S that the unit residual oil combustion obtains | ????13.50 | ????14.62 |
| Funnel temperature (℃) | ????348.4 | ????332.0 |
| The rate of economizing gasoline of oil fuel | ????(14.62/13.5-1)*100％＝12％ | |
Energy-conservation and the environment protecting of diesel engine bench experiment:
The submicron with microvoid structure in embodiment 1 and 3 and nano combined additive are used for the machine oil and the diesel oil of C498QD engine respectively by corresponding proportion, carry out energy-conservation and the blank contrast properties experiment of environmental protection, the result is as shown in table 5.
Energy-conservation and the blank contrast properties experimental result of environmental protection of table 5
| Rate of economizing gasoline (%) | ??2000rpm | ????2.3 |
| ??2500rpm | ????2.0 | |
| ??3000rpm | ????2.4 | |
| ??3500rpm | ????2.5 | |
| ??4000rpm | ????2.6 | |
| Idle exhaust emission reduced rate (%) | ??CO | ????34.4 |
| ??HC | ????27.7 |
| Remarks: | ??QC/T524-1999，GB/T3845-1993 |
The petrol motor real vehicle is repaired experiment effect:
2VQS engine with the submicron with microvoid structure in embodiment 2 and 4 and nano combined additive are used for having worn and torn by corresponding proportion respectively experimentizes to its repairing performance, and the result is as shown in table 6.
Table 6 2VQS engine repairing performance experimental result
| Average cylinder prepareding gap (micron) | ||
| Before adding agent | ????250 | |
| Move after adding agent | ??100Km | ????245 |
| ??300Km | ????242 | |
Above-mentioned experimental result explicit declaration, microporous type submicron of the present invention and nano combined additive have splendid extreme pressure, antiwear and antifriction, energy-saving and environmental protection and repairing effect, industrial very big application prospect are arranged.
Claims (4)
1, a kind of preparation method of microporous type composite additive is characterized in that, adopt heating container and be used to circulate, the toothed gear pump of stirring, refinement and the rubbing effect of generation extreme pressure, concrete steps are as follows:
1) heat kerosene is poured in the heating container, when being heated to 50-70 degree centigrade dispersion agent is poured in the heating agent, stop heating, stir until the dispersion agent uniform distribution by pump housing circulation;
2) treat that the heat kerosene temperature reduces to room temperature 15-30 degree centigrade, the rare earth powder evenly poured in the heat kerosene, powder is carried out the oil bath thinning processing by the engagement of pump, sampling Detection rare earth metal particulate granularity, until granularity in 500 nanometers-1 micrometer range;
3) be heated to 210-240 degree centigrade, keep temperature, add perfluoroparaffin, utilize the hyperpressure hyperthermal friction chemical reaction of the engagement simulation friction pair of toothed gear pump, rare earth powder after the refinement is carried out mechanochemistry handles, the granularity of sampling Detection rare earth compound or complex compound and shape, until granularity between the 50-600 nanometer, be shaped as porous spherical or elliposoidal structure, stop heating;
4) add auxiliary agent and graphite powder, circulation is stirred, until being uniformly dispersed.
2, the preparation method of microporous type composite additive according to claim 1 is characterized in that, is used to circulate, the hydro-pump of stirring, refinement and the rubbing effect of generation extreme pressure, is preferably toothed gear pump.
3, the preparation method of microporous type composite additive according to claim 1, it is characterized in that, the engagement of toothed gear pump forms the lubricated district of an instantaneous high pressure hertz, in this high-tension lubrication district, produce instantaneous pressure and high temperature because of mechanical presses around the granular thulium, the thulium instant melting also generates rare earth compound or complex compound, and the organic solvent around it also is vaporized simultaneously and it is produced impact, when toothed gear pump broke away from high pressure hertz district, cure shrinkage formed sphere and produce micropore on inner and surface because temperature moment reduces for rare earth compound or complex compound.
According to the preparation method of claim 1 or 3 described microporous type composite additives, it is characterized in that 4, the rare earth compound of formation or complex compound are the porous spherical structure, granularity is uniform distribution between the 50-600 nanometer.
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| CN 03116171 CN1442471A (en) | 2003-04-03 | 2003-04-03 | Preparation method of microporous composite additive |
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| CN 03116171 CN1442471A (en) | 2003-04-03 | 2003-04-03 | Preparation method of microporous composite additive |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100395320C (en) * | 2006-03-15 | 2008-06-18 | 华东理工大学 | Fluorine-containing rare earth nano lubricating oil additive and preparation process thereof |
| CN115717089A (en) * | 2022-11-14 | 2023-02-28 | 上海锱碳节能环保技术有限公司 | Method and system for improving fuel energy efficiency and fuel thereof |
-
2003
- 2003-04-03 CN CN 03116171 patent/CN1442471A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100395320C (en) * | 2006-03-15 | 2008-06-18 | 华东理工大学 | Fluorine-containing rare earth nano lubricating oil additive and preparation process thereof |
| CN115717089A (en) * | 2022-11-14 | 2023-02-28 | 上海锱碳节能环保技术有限公司 | Method and system for improving fuel energy efficiency and fuel thereof |
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