CN102507396B - Method for determining dispersity of ultrafine additive in lubricant - Google Patents
Method for determining dispersity of ultrafine additive in lubricant Download PDFInfo
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- CN102507396B CN102507396B CN 201110314020 CN201110314020A CN102507396B CN 102507396 B CN102507396 B CN 102507396B CN 201110314020 CN201110314020 CN 201110314020 CN 201110314020 A CN201110314020 A CN 201110314020A CN 102507396 B CN102507396 B CN 102507396B
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Abstract
The invention discloses a method for determining the dispersity of an ultrafine additive in a lubricant. The method comprises the steps of: placing each part of lubricant in one centrifugal pipe, sampling the upper layers of three parts of lubricants among the lubricants before centrifuging, dividing the rest parts into groups in a triple manner, placing the groups in respective centrifugal machines, centrifuging at the same time, taking out one group every other 5-15 minutes, sequentially determining the additive content in each sample according to a time sequence of sampling, then, respectively calculating the average concentration of each group of additives, sequentially carrying out subtraction on the average concentration of the additives of a later group and the average concentration of the additives of the former group, and dividing each subtraction result by the average concentration of the additive of the former group to sequentially obtain a relative concentration change value of every two groups in sequence, wherein the relative concentration value change value is smaller than or equal to 2%, the required centrifuging time is longer, and the dispersity is better at the same rotation speed in the same media. The method disclosed by the invention has no requirements on the shape, the granularity, the particle size distribution and the electrified condition, has wide range of measurable substances, and can be used for reflecting the dispersity of particles in the lubricant.
Description
Technical field
The present invention relates to lubricant, especially relate to the assay method of particle dispersiveness in a kind of lubricant.
Background technology
Lubricant has extremely important effect in plant equipment, single quality that improves the base oil oil product from oil refining process far can not satisfy low speed, at a high speed, the needs of the different service conditions such as top load, high-power, high temperature, low temperature, high vacuum, high radiation, must in lubricant, add the quality that the various adjuvants of people improve lubricant.In recent years, both at home and abroad with ultrafine dust particularly nano particle be applied in the lubricating system, nano material has the characteristics such as surface area is large, high diffusibility, easy-sintering, fusing point is low, hardness is large, not only can form the film that one deck is easily sheared at friction surface, reduce friction factor, and can also carry out filling up and repairing to a certain degree to friction surface.Nano lubricating oil additive has outstanding anti-extreme pressure energy and excellent resistance to abrasion, and greasy property is adapted at working under heavy duty, low speed, the high temperature preferably; Simultaneously, it combines again the advantage of fluid lubrication and solid lubrication, is different from general solid lubricant.
Because the ultrafine additive surface area is large, particle itself is reunited easily, its dispersiveness that joins in the lubricant becomes the key factor that affects its effect, and ultrafine additive degree of scatter in lubricant often differs greatly with the adjuvant initial size, can improve its dispersiveness by ultrafine additive being carried out surface modification, change addition manner etc., it is all most important to determining process conditions and final lubricant product quality therefore to estimate its dispersiveness.Compare with the nano particle technology of preparing, nanometer additive relates to reunion and the scattering problem of nano particle itself in lubricant as lubricant, property is poor, viscosity is high, complicated component because lubricant flows, the dispersiveness of ultra-fine grain adjuvant check is very difficult in the product, thereby limited its application.
At present, light transmittance ratio method commonly used is also dispersed in conjunction with sedimentation mensuration superfine particulate matter, observes the variation of certain hour internal absorbance, changes little person's good dispersion, and large or opaque lubricant system is difficult to use this method for viscosity; And in the granularity observation, using microscope or image analyzer to observe particle size and distribution, granule number is limited in the visual field, makes easily the sample distortion when spreading to film; Publication number be CN1570601 patent literature the method for nano material dispersiveness in a kind of testing rubber, the method is that the rubber that contains nanometer Zinc oxide powder is freezing, the rubber after freezing is cut into the thin slice of 50 ~ 90 nanometers, then uses scanning electron microscopic observation; A kind of method of measuring insoluble matter dispersiveness in solution that publication number has been the CN1945277A patent literature, the method are to utilize to calculate the mean concentration of pouring out suspending liquid and the dispersion degree of recently weighing insoluble matter that leaves standstill the concentration of front unit for uniform suspension; JP2008003079A has reported the method for testing of particle particle diameter in a kind of lubricant, is the solvent dilution sample of using with the lubricant base oil similar performance, and then ultrasonic dispersion measures the initial size of adding particle with particle size analyzer.
Summary of the invention
The object of the present invention is to provide a kind of method of measuring ultrafine additive dispersiveness in lubricant, the method measurement of species wide ranges, method are easy, are applicable to contain preparation technology's control, the evaluation of additive agent modified effect and the check of lubricant end product quality of the lubricant of ultrafine additive.
To achieve these goals, the assay method of dispersity of ultrafine additive in lubricant provided by the invention can be realized as follows:
(1) gets 15 ~ 30 parts of lubricants that contain the equal in quality of ultrafine additive, every part of lubricant is respectively as in the centrifuge tube, before centrifugal therein the upper strata of three parts of lubricants all get 0.1 ~ 0.4g specimen, be simultaneously centrifugal in the hydro-extractor that a group is placed on separately with per three parts of remaining lubricant, the rotating speed of hydro-extractor is 3000 ~ 30000 rev/mins;
(2) corresponding one group of sample in the hydro-extractor was taken out at every interval in 5 ~ 15 minutes, all got 0.1 ~ 0.4g specimen on the upper strata of every duplicate samples;
(3) use atomic absorption spectrography (AAS), by the additive level in every part of specimen of time order and function order sequentially determining of sampling, calculate respectively again the adjuvant mean concentration of every group of specimen, then successively the adjuvant mean concentration of the adjuvant mean concentration of rear one group of specimen and last group of specimen is done poor and divided by the adjuvant mean concentration of last group of specimen, obtain successively the relative concentration changing value between per two groups, when the relative concentration changing value is less than or equal to 2% the required centrifugal time longer, the dispersiveness in same rotating speed and medium is better.
Foundation of the present invention is the Stokes law, for the sedimentation of accelerating particle so that measure, in centrifugal field, implement sedimentation, the settling velocity of particle is relevant with particle diameter and centrifugal acceleration, replaces granularmetric analysis with the constituent analysis of the adjuvant of sampling spot, by regulating the rotating speed of hydro-extractor, realize the controllability of settling time, whether charged to the shape of particle, granularity, size-grade distribution with do not do requirement, the measurement of species wide ranges can reflect the dispersiveness of particle in lubricant.
Embodiment
The lubricant of getting 15 ~ 30 parts of equals in quality is put into the centrifuge tube of hydro-extractor, and this lubricant contains ultrafine additive, is commercially available or homemade lubricating oil, railway grease or the base oil that is added with superfine particulate matter.Additive component refers to the allotrope of graphite and adamantine carbon, the simple substance that contains soft metal and compound, carbonate, oxide and oxyhydroxide or contains the compound of boron, barium, calcium, lead, magnesium, phosphorus, potassium, sodium, elemental lithium.The simple substance of the soft metal that contains and compound refer to contain aluminium, tin, copper, nickel, zinc, silver, bismuth and plumbous simple substance and compound.Carbonate refers to calcium carbonate or magnesium carbonate.Oxide and oxyhydroxide refer to titania, zirconia, silicon dioxide, nickel hydroxide, manganous hydroxide and magnesium hydroxide.
After lubricant left standstill 3 minutes, before centrifugal, the specimen of 0.1 ~ 0.4g lubricant was all got on the upper strata of three parts of lubricants therein, and the upper strata of centrifuge tube refers to that the centrifuge tube surface is to 1/6 of centrifuge tube height.With remaining every part lubricant each as in the centrifuge tube, per three samples are one group and are placed in the hydro-extractor centrifugally that the rotating speed of setting hydro-extractor is 3000 ~ 30000 rev/mins.
The corresponding one group of sample in the hydro-extractor was taken out at every interval in 5 ~ 15 minutes, three parts every group, all got 0.1 ~ 0.4g specimen on the upper strata of every duplicate samples.Press the constituent analysis of adjuvant, constituent analysis is that the content of the contained ultimate analysis of subject additives is sign, use atomic absorption spectrography (AAS), by the additive level in every part of specimen of time order and function order sequentially determining of sampling, calculate respectively again the adjuvant mean concentration of every group of specimen, i.e. the mean value of the additive level analysis result of three duplicate samples in every group of specimen.The mean concentration of not putting into three duplicate samples of hydro-extractor is C
0, for the first time the mean concentration of three duplicate samples taken out of 5 ~ 15 minutes intervals is adjuvant mean concentration C of first group of specimen
1, for the second time the mean concentration of three duplicate samples taken out of 5 ~ 15 minutes intervals is adjuvant mean concentration C of second group of specimen
2, the like obtain second group to the adjuvant mean concentration C of the specimen of n group
3～C
9Then successively the adjuvant mean concentration of the adjuvant mean concentration of rear one group of specimen and last group of specimen is done poor and obtained successively relative concentration changing value between per two groups, that is: relative concentration changing value △ C divided by the adjuvant mean concentration of last group of specimen
1=(C
1-C
0)/C
0, △ C
2=(C
2– C
1)/C
1, △ C
3=(C
3– C
2)/C
2△ C
10=(C
10– C
9)/C
9When the relative concentration changing value is less than or equal to 2% the required centrifugal time longer, the dispersiveness in same rotating speed and medium is better.
6 embodiment of the present invention below are provided:
Embodiment 1
Get the PAO10(PAO that contains the superfine cupper powder adjuvant: poly alpha olefine synthetic oil) sample 12g, totally 15 parts, every part each is as in the centrifuge tube, after leaving standstill 3 minutes, the 0.4g specimen is all got on three parts upper strata therein, be called first group of specimen, per three samples of all the other samples are placed in the hydro-extractor centrifugal, it is centrifugal to put into altogether 4 hydro-extractors, 3000 rev/mins of rotating speeds, three duplicate samples in first hydro-extractor were taken out at the interval in 10 minutes, all got the 0.1g specimen on the upper strata of this three duplicate samples, were second group of specimen; By that analogy, obtain the the 3rd, the 4th, the 5th group of specimen.Press again SH/T 0102-92(People's Republic of China (PRC) petroleum chemical industry standard) step, with the copper content in every part of specimen of aas determination, draw the mean concentration of copper content of three parts of specimen of each time point by the time order and function sequentially determining of sampling, the mean concentration of copper content of not putting into first group of specimen of hydro-extractor is C
0, for the first time the mean concentration of second group of specimen taking out in 10 minutes of interval is C
1, for the second time the mean concentration of the 3rd group of specimen taking out in 10 minutes of interval is C
2, the like the mean concentration C of the 4th, the 5th group of specimen
3, C
4Then, the relative concentration difference of respectively organizing specimen in 10 minutes counting periods obtains △ C
1, △ C
2, △ C
3, △ C
4, that is: △ C
1=(C
1-C
0)/C
0, △ C
2=(C
2– C
1)/C
1, △ C
3=(C
3– C
2)/C
2, △ C
4=(C
4– C
3)/C
3, the relative concentration difference is respectively 0.15,0.07,0.03,0.02, and the time of the poor arrival 0.02 of relative concentration is 40 minutes.
Embodiment 2
Get the PAO10 sample 12g that contains the superfine cupper powder adjuvant, totally 21 parts, every part each as in the centrifuge tube, leave standstill 3 minutes after, the 0.4g specimen is all got on three parts upper strata therein, be called first group of specimen, it is centrifugal that all the other samples are put into 6 hydro-extractors, and per three samples are placed in the hydro-extractor, 3000 rev/mins of rotating speeds, three duplicate samples in first hydro-extractor were taken out at the interval in 10 minutes, all got the 0.1g specimen on the upper strata of three duplicate samples, were second group of specimen; By that analogy, obtain the the the 3rd, the 4th, the 5th, the 6th, the 7th group of specimen.Press again SH/T 0102-92 steps, with the copper content in every part of specimen of aas determination, draw the mean concentration of copper content of three parts of specimen of each time point by the time order and function sequentially determining of sampling, do not put into the mean concentration C of copper content of first group of specimen of hydro-extractor
0, the first time, the mean concentration of second group of specimen that took out in 10 minutes at the interval was C
1, the second time, the mean concentration of the 3rd group of specimen that took out in 10 minutes at the interval was C
2, the like draw the the the 4th, the 5th, the 6th, the 7th group of specimen mean concentration be C
3, C
4, C
5, C
6Then, calculating successively, 10 minutes the relative concentration difference of respectively organizing specimen in interval obtains △ C again
1, △ C
2, △ C
3, △ C
4, △ C
5, △ C
6, that is: △ C
1=(C
1-C
0)/C
0, △ C
2=(C
2– C
1)/C
1, △ C
3=(C
3– C
2)/C
2, △ C
4=(C
4– C
3)/C
3, △ C
5=(C
5– C
4)/C
4, △ C
6=(C
6– C
5)/C
5The relative concentration difference is followed successively by 0.25,0.16,0.10,0.05,0.02,0.01, hence one can see that, the variation of the relative concentration after centrifugal 40 minutes of the copper powder among the embodiment 1 is less than 0.02, and needs 50 minutes among the embodiment 2, illustrates that the copper powder dispersiveness among the embodiment 2 is better than embodiment 1.
Embodiment 3
Get the 500SN(SN that contains the ultra-fine lead oxide adjuvant: paraffinic base neutral oil) sample 8g, totally 30 parts, every part each is as in the centrifuge tube, after leaving standstill 3 minutes, the 0.2g specimen is all got on three parts upper strata therein, be called first group of specimen, it is centrifugal that all the other samples are put into 9 hydro-extractors, per three samples are placed in the hydro-extractor, 5000 rev/mins of rotating speeds, and three duplicate samples in first hydro-extractor were taken out at the interval in 5 minutes, the 0.1g specimen is all got on upper strata in this three duplicate samples, be called second group of specimen, by that analogy, obtain the 3rd, the 4th, the 5th, the 6th, the 7th, the 8th, the 9th, the tenth group of specimen.Press again SH/T 0617-95 steps, replace the oxidation lead amount with the lead element content in every part of specimen of aas determination, draw the mean concentration of lead element content of three parts of specimen of each time point by the time order and function sequentially determining of sampling, the mean concentration of copper content of not putting into first group of specimen of hydro-extractor is C
0, for the first time the mean concentration of second group of specimen taking out in 10 minutes of interval is C
1, the like the mean concentration of other several groups of specimen is respectively C
2～C
9, calculating successively, 5 minutes the relative concentration difference of respectively organizing specimen in interval gets △ C
1, △ C
2, △ C
3, △ C
4, △ C
5, △ C
6, △ C
7, △ C
8, △ C
9Be respectively 0.35,0.26,0.15,0.12,0.08,0.06,0.04,0.02,0.01, the poor time less than 2% of relative concentration is 40 minutes.
Because the 500SN Basic oil Viscosity greater than PAO10, in order to shorten the test duration, has improved the rotating speed of hydro-extractor.
Embodiment 4
Get the 500SN sample 8g that contains the copper powder adjuvant, totally 30 parts, every part each as in the centrifuge tube, leave standstill 3 minutes after, the 0.2g specimen is all got on three parts upper strata therein, be called first group of specimen, it is centrifugal that all the other samples are put into 9 hydro-extractors, and per three samples are placed in the hydro-extractor, 5000 rev/mins of rotating speeds, three duplicate samples were taken out at every interval in 5 minutes, and the 0.1g specimen is all got on the upper strata, obtained the 3rd to the tenth group of specimen.Press again SH/T 0102-92 steps, with the copper content in every part of specimen of aas determination, draw the mean concentration of copper content of three parts of specimen of each time point by the time order and function sequentially determining of sampling, the mean concentration of copper content of not putting into first group of specimen of hydro-extractor is C
0, by that analogy, the mean concentration that obtains second to the tenth group of specimen is C
2～C
9Calculate again successively 5 minutes the relative concentration difference △ C in interval
1～△ C
9Be respectively 0.25,0.20,0.18,0.15,0.10,0.06,0.03,0.03,0.02, the poor time less than 2% of relative concentration is 90 minutes.The dispersiveness of good dispersion massicot in embodiment 3 of copper powder among the embodiment 4 is described.
Embodiment 5
Get the urea-base grease sample 4g that contains the ultra-fine lead oxide adjuvant, totally 24 parts, every part each as in the centrifuge tube, leave standstill 3 minutes after, the 0.1g specimen is got on three parts upper strata therein, be called first group of specimen, it is centrifugal that all the other samples are put into supercentrifuge, and rotating speed is 30000 rev/mins, and three duplicate samples were taken out at every interval in 15 minutes, the 0.1g specimen is all got on the upper strata, obtains the 3rd to the 7th group of specimen.Press again SH/T 0617-95 steps, replace the oxidation lead amount with aas determination lead element content wherein, draw the mean concentration of lead content of three parts of specimen of each time point by the time order and function sequentially determining of sampling, the mean concentration of lead content of not putting into first group of specimen of hydro-extractor is C
0, for the first time the mean concentration of second group of specimen taking out in 15 minutes of interval is C
1, for the second time the mean concentration of the 3rd group of specimen taking out in 15 minutes of interval is C
2, the like the mean concentration C of the 4th to the 7th group of specimen
3～C
7Then, calculate the successively poor △ C of getting of 15 minutes the relative concentration in interval
1, △ C
2, △ C
3, △ C
4, △ C
5, △ C
6, △ C
7Be respectively 0.19,0.15,0.11,0.09,0.05,0.04,0.02, the poor time less than 2% of relative concentration is 105 minutes.
Because railway grease viscosity is large, for shortening the test duration, improved the rotating speed of hydro-extractor.
Embodiment 6
Get the urea-base grease sample 4g that contains the nickel hydroxide adjuvant, totally 30 parts, every part each is as in the centrifuge tube, after leaving standstill 3 minutes, the 0.1g sample is all got on three parts upper strata therein, it is centrifugal that all the other samples are put into supercentrifuge, rotating speed is 30000 rev/mins, three duplicate samples in first hydro-extractor were taken out at every interval in 15 minutes, the 0.1g sample is got on the upper strata, press SH/T 0617-95 steps, with the every nickel element content wherein of aas determination, calculate successively 15 minutes the relative concentration difference △ C in every interval
1, △ C
2, △ C
3, △ C
4, △ C
5, △ C
6, △ C
7, △ C
8, △ C
9Be respectively 0.12,0.10,0.10,0.09,0.08,0.06,0.05,0.03,0.02, the poor time less than 2% of relative concentration is 150 minutes.The massicot of good dispersion in embodiment 5 of nickel hydroxide among the embodiment 6 is described.
Because the sedimentation of superfine particulate matter is relevant with the viscosity of medium, the system that viscosity is large should improve rotating speed, to shorten the test duration.In same medium, use same rotational speed, measure the shortest time that concentration change tends towards stability, the time, longer explanation dispersiveness was better.
Claims (4)
1. the assay method of a dispersity of ultrafine additive in lubricant is characterized in that may further comprise the steps:
(1) gets 15 ~ 30 parts of lubricants that contain the equal in quality of ultrafine additive, every part of lubricant places a centrifuge tube, before centrifugal therein the upper strata of three parts of lubricants all get 0.1 ~ 0.4g specimen, be simultaneously centrifugal in the hydro-extractor that a group is placed on separately with per three parts of remaining lubricant, the rotating speed of hydro-extractor is 3000 ~ 30000 rev/mins;
(2) corresponding one group of sample in the hydro-extractor was taken out at every interval in 5 ~ 15 minutes, all got 0.1 ~ 0.4g specimen on the upper strata of every duplicate samples;
(3) use atomic absorption spectrography (AAS), by the additive level in every part of specimen of time order and function order sequentially determining of sampling, calculate respectively again the adjuvant mean concentration of every group of specimen, then successively the adjuvant mean concentration of the adjuvant mean concentration of rear one group of specimen and last group of specimen is done poor and divided by the adjuvant mean concentration of last group of specimen, obtain successively the relative concentration changing value between per two groups, when the relative concentration changing value is less than or equal to 2% the required centrifugal time longer, the dispersiveness in same rotating speed and medium is better.
2. the assay method of a kind of dispersity of ultrafine additive in lubricant according to claim 1, it is characterized in that: the upper strata of described centrifuge tube refers to that the centrifuge tube surface is to 1/6 place of centrifuge tube height.
3. the assay method of a kind of dispersity of ultrafine additive in lubricant according to claim 1, it is characterized in that: described lubricant refers to commercially available or homemade lubricating oil, railway grease or the base oil that is added with superfine particulate matter.
4. the assay method of a kind of dispersity of ultrafine additive in lubricant according to claim 1, it is characterized in that: described additive component is the allotrope of carbon, the simple substance that contains soft metal and compound, carbonate, oxide and oxyhydroxide or the compound that contains boron, barium, calcium, lead, magnesium, phosphorus, potassium, sodium, elemental lithium.
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|---|---|---|---|
| CN 201110314020 CN102507396B (en) | 2011-10-17 | 2011-10-17 | Method for determining dispersity of ultrafine additive in lubricant |
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| US7150182B2 (en) * | 2003-10-31 | 2006-12-19 | Chevron Oronite Company, Llc | High throughput screening methods for lubricating oil compositions |
| JP2008003079A (en) * | 2006-05-22 | 2008-01-10 | Minebea Co Ltd | Evaluation method for lifetime of grease composition |
| CN101413867B (en) * | 2008-10-27 | 2011-05-25 | 大连大学 | Intelligent tester of magnetic lubricating oil nano granule space distribution rule |
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