CN103091476A - Rapid and comprehensive evaluation method of lubricant oil aging performance - Google Patents
Rapid and comprehensive evaluation method of lubricant oil aging performance Download PDFInfo
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Abstract
The present invention provides an evaluation method of lubricant oil aging performance. The method includes feeding air or oxygen with flow of 3-15L/h into the to-be-tested lubricant oil, under the conditions of oil temperature of 100-200 DEG C and metal catalyst, and then measuring aging performances including lubricant oil viscosity, color, acid value, demulsibility, pentane insolubles, copper corrosion, copper weight loss and sludge trend after 20-200 hours, and evaluating the lubricant oil aging performance according to the change of lubricant oil performances before and after the test. The evaluation method of lubricant oil aging performance helps to achieve rapid and comprehensive evaluation for oil.
Description
Technical field
The present invention relates to a kind of lubricants performance detection method, specifically, relate to the assessment method of the lubricating oil product ageing properties that a kind of test period is short, test item is complete.
Background technology
Due to the oil ageing complex forms, be difficult to its life-span is carried out simple and appropriate evaluation, be therefore all in equipment overhaul cycle, it to be regularly replaced in the past.Along with the development of material assessment method, make and set up a kind of quick, comprehensive, appropriate oil ageing assessment method and become possibility.This to correct evaluation lubricant life, correctly to formulate equipment overhaul cycle most important.
Base oil in lubricating oil and adjuvant are along with the variation of time can consume or go bad, be i.e. oil ageing.In addition, lubricating oil in use can accumulate the insolubles of the reason generations such as wearing and tearing, also is equivalent to the aging of broad sense.Therefore, oil ageing need by base oil rotten, adjuvant rotten, consume and accumulation three aspects of other materials are estimated.For going bad of base oil, be mainly reflected in the variation of viscosity and the generation of acidic materials, therefore can investigate by indexs such as viscosity, acid number and colourities; For the consumption of adjuvant, rotten, in most cases can not directly estimate it, but the consumption of antioxidant can cause the variation of acid number, the rotten meeting of corrosion protection abrasion resistant agent makes has mud shape thing to separate out in lubricating oil.Therefore, for the consumption of adjuvant, rotten can the investigation by indexs such as acid number, copper corrosion and pentane insolubles; The in use wearing and tearing of high temperature, high pressure and friction pair of oil product can cause the accumulation of insolubles, and this respect can be investigated by indexs such as copper sheet weightlessness and greasy filth trend.In sum, if the oil product ageing properties is more comprehensively evaluated, need to investigate following project: viscosity, colourity, acid number, pentane insolubles, copper corrosion, copper sheet weightlessness and greasy filth trend.
At present, the assessment method relevant to oil ageing is mainly the oxidation stability assay method.Existing oxidation stability assay method has multiple, its principle is basic identical, general is all directly to pass into the air of oxygen or purge drying in sample, under the effect of the catalyzer such as metal, and the variation of the indexs such as the viscosity of mensuration sample, acid number after the experience official hour under set point of temperature.Test condition is different because of oil product.China carries out oxidation test to the anti-oxidative stability of aero-turbine lubricating oil by SH/T 0450-92, is called the oxidation tube method; Combustion motor Determination of oil method has SH/T0299-92 and SH/T0192-92 standard; Steam turbine oil SH/T 0193-92 rotary oxygen bomb method is measured its antioxygenic property; The oxidation characteristic of transformer oil is undertaken by SH/T 0206-92 standard method; The Productions of middle and high grade lube oil oxidation stability is measured and to be mainly contained GB/T 12581 inhibiting mineral oil oxidation characteristic determination methods, GB/T 12709 oil ageing characteristic measurement methods (Conradson carbon residue method), SH/T 0123 extreme pressure lublicating oil oxidation stability determination method and carry out.
The above-mentioned test method major part part that all comes with some shortcomings, for example method GB/T 12581 comparatively commonly used mainly contains following aspect and is unfavorable for operation at present: (1) test period is oversize.It is 1000h that the method requires detection time, can not realize the oil product fast detecting; (2) test item is single.Only estimated the oxidation stability of oil product, the test item major part only relates to viscosity, acid number etc., and the sundry item relevant to ageing properties do not tested.
This shows, existing lubricating oil detects assessment method can not realize, comprehensively evaluation quick to the oil product ageing properties, demands setting up a kind of new oil product ageing properties assessment method urgently.
Summary of the invention
The object of the present invention is to provide a kind of quick, comprehensive oil ageing Reliable Evaluating Methods of Their Performance.
In order to realize the object of the invention, oil ageing Reliable Evaluating Methods of Their Performance of the present invention, it adopts in lubricating oil to be measured and passes into the air or oxygen that flow is 3-15L/h, under oil temperature 100-200 ℃, metallic catalyst condition, through 20-200 hour, then measure lubricating oil viscosity, colourity, acid number, resistance to emulsion, pentane insolubles, copper corrosion, copper sheet weightlessness and the every ageing properties of greasy filth trend, according to the variation of lubricants performance to be measured before and after test, the oil ageing performance is evaluated.
Wherein, preferred, described oil temperature is controlled at 120-180 ℃, is more preferably 150-180 ℃.
Preferably, the flow of described air or oxygen is 5-10L/h, is more preferably 5L/h.
Preferably, the described time is controlled at 160-180 hour, is more preferably 168 hours.
Preferably, described metallic catalyst is copper or iron.Can adopt copper sheet or iron plate.
Described copper sheet adopts is purity greater than 99.9% cathode copper, and the wide of described copper sheet be 12.5mm, and thick be 1.5-3.0mm, and growing is 75mm.
Described oil temperature adopts the modes such as constant temperature oven, baking oven, metal bath or oil bath to control.
The present invention is directed to the present situation that there is no at present special oil product ageing properties assessment method, existing oil oxidation stability method is improved, oil product to be measured is kept certain test temperature in special time, and pass into quantitative air, measure variation and pentane insolubles, copper corrosion, copper sheet weightlessness and the greasy filth trend of viscosity, colourity, acid number through the regular hour, realize that oil product is quick, comprehensively ageing properties evaluation.Can complete required test within a short period of time, the while is the evaluation indices relevant to the oil product ageing properties comprehensively, thereby for correctly evaluation lubricant life, formulation equipment overhaul cycle provide important references.
Description of drawings
Fig. 1 is the structural representation that the present invention is lubricated oil degradation evaluation oil product treating apparatus used.
Fig. 2 is that the oil product outward appearance is with digestion time situation of change (left-to-right: oil product A, oil product B, oil product C).
Fig. 3 is copper sheet and insolubles outward appearance situation after aging test in embodiment 2.
Embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
See also shown in Figure 1, the oil product ageing properties assessment method of preferred embodiment of the present invention, it comprises the process of tested oil product being carried out burin-in process, and the process that the indexs such as viscosity, colourity, acid number, pentane insolubles, copper corrosion, copper sheet weightlessness and greasy filth trend of the oil product after burin-in process are measured.
This method adopts oil product treating apparatus shown in Figure 1 to carry out burin-in process to tested oil product.This device comprises thermostatic container 10 and oil product container 20.
This oil product container 20 holds tested lubricating oil oil product, is arranged in thermostatic container 10.Oil product container 20 can adopt test tube.
Add tested oil product and copper sheet catalyzer in oil product container 20, copper sheet adopts is purity greater than 99.9% cathode copper, and the wide of copper sheet be 12.5mm, and thick be 1.5-3.0mm, and growing is 75mm.
One stopper 23 is set on the opening of oil product container 20, and is provided with a draft tube 21 and an escape pipe 22 on stopper 23.The bottom that draft tube 21 is inserted oil product container 20 is used for passing into air or oxygen to oil product container 20 interior tested lubricating oil oil products, and escape pipe 22 insertion is more shallow, is used for discharging the gas in oil product container 20.
Oil ageing Reliable Evaluating Methods of Their Performance of the present invention comprises the steps:
First pass into air from draft tube 21, the flow of air is 3-15L/h; Start thermostatic container and make tested oil product reach design temperature, and remaining on this design temperature, this design temperature is 100-200 ℃; After the temperature of tested oil product reaches design temperature, the beginning timing, and extract successively sample according to setting-up time, to the variation of the indexs such as its viscosity of sample determination, colourity, acid number, pentane insolubles, copper corrosion, copper sheet weightlessness and greasy filth trend extracted.Judge the aging conditions of tested sample according to the variation of above performance index.The measuring method of above-mentioned viscosity, colourity, acid number, pentane insolubles, copper corrosion, copper sheet weightlessness and greasy filth trend adopts method of the prior art to get final product.
Embodiment 1
The present embodiment is to utilize assessment method of the present invention within a short period of time that similar hydraulic oil oil product A, the oil product B of three kinds of performances and the ageing properties of oil product C are compared.
1. test condition
Test temperature is 150 ℃, and it is 5L/h that air passes into speed, adds the 5.5g copper sheet as catalyzer, and copper sheet adopts purity greater than 99.9% cathode copper, and wide be 12.5mm, and thick be 2.0mm, and growing is 75mm; Test period 120h, test item comprise viscosity, viscosity index, colourity and acid number.
2. test specimen
Oil product A: wherein base oil is comprised of API I class oil and API II class oil, and weight ratio both is 8: 1; The antiwear agent weight percentage is 1% of total amount.
Oil product B: wherein base oil is comprised of API I class oil and API II class oil, and weight ratio both is 5: 1; The antiwear agent weight percentage is 1% of total amount.
Oil product C: wherein base oil is comprised of API I class oil and API II class oil, and weight ratio both is 1: 8; The antiwear agent weight percentage is 1% of total amount.
According to the API criteria for classification, API I class base oil is low than API II class base oil hydrogenation degree, and its antioxygenic property is slightly poor.Formed and can be found out by above A, B, C oil product, three kinds of main difference of oil product are that API I class is different with the ratio of API II class base oil, and wherein oil product C API II class base oil ratio is the highest, and oil product B is placed in the middle, and oil product A is minimum.Can infer that thus three kinds of oil product ageing resistances are: oil product C＞oil product B＞oil product A.
3. test findings
Table 1 has been showed and has been utilized above-mentioned test method obtained experimental result.
The test result of table 1 oil product
In analytical table 1, data can be found out, three kinds of oil products through colourity after aging test, variation are occuring obviously, and oil product A and oil product B change more obvious.In addition, oil product A acid number changes than other two kinds of oil products variations obviously.And the performance of oil product C property indices is stable.Above test findings shows, oil product C ageing resistance is better than other two kinds of oil products, consistent with aforementioned deduction conclusion.
Adopt the advantage of this method to be, realized the trade-off to different oil product ageing properties within a short period of time, provide reference timely to selection and the evaluation of oil product.In addition, can adjust according to actual needs test condition, increase test item, oil product is more comprehensively estimated.
Embodiment 2
The present embodiment is to utilize assessment method of the present invention to carry out comprehensive ageing properties relatively to three kinds of oil products.
1. test condition
(1) test temperature: 150 ℃;
(2) test source of the gas: pressurized air, flow are 5L/h;
(3) catalyzer: copper sheet, purity is greater than 99.9% cathode copper, and wide is 12.5mm, and thick is 1.5-3.0mm, longly is 75mm;
(4) test period: 168 hours;
(5) analysis project: viscosity, colourity, acid number, resistance to emulsion, pentane insolubles, copper corrosion, copper sheet weightlessness and greasy filth trend.
2. test specimen
Oil product A, oil product B and oil product C, oil product is with embodiment 1.
3. test findings
3.1 oil product outward appearance
Fig. 2 has showed that the oil product outward appearance increases situation about changing with digestion time.
As seen from Figure 2, oil product A outward appearance changes the most obvious with digestion time, becomes black general through oil product after 48h; Oil product B is not obvious with interior change color at 48h, but the rapid blackening of oil product color afterwards, the oil product color is substantially close to oil product A when 144h; Oil product C is relatively stable, and particularly after oil product process 168h high-temperature oxydation, other products all become black, and oil product C color is brown but the clear that remains unchanged.Above test findings tentatively shows, oil product C hydraulic oil ageing resistance is better than other two kinds of products.For further confirming the oil product ageing resistance, sample after aging test has been carried out further physical and chemical performance analysis.
3.2 basic physical and chemical index
In order further to determine the oil product degree of aging, at first we carried out basic physical and chemical performance analysis to oil product, analyzes data and see Table 2.
The basic physical and chemical performance analysis data of table 2 sample
Can be found out by data in table 2, variation is obviously occuring through colourity after aging test in three kinds of oil products, and this is consistent with viewed oil product appearance results; The indexs such as oil product A viscosity, acid number, resistance to emulsion and pentane insolubles change obviously, and wherein after resistance to emulsion and oxidation, two indexs of acid number are obviously defective.In addition, the pentane insolubles index value is higher, illustrates that this oil product has occured significantly aging; Oil product B is through after aging test, and resistance to emulsion is defective, pentane insolubles numerical value is higher simultaneously, illustrates that to a certain degree aging occured this oil product; Oil product C is after aging test, and indices is all qualified, shows that this oil product has ageing resistance preferably.
3.3 copper sheet weightlessness and greasy filth trend
In order further to investigate the ageing resistance of oil product, this paper is investigating outside basic physical and chemical index, also increased with use procedure in the investigation of more closely-related indexs, comprise that copper sheet is weightless, greasy filth trend and filterableness.Fig. 3 has showed through copper sheet outward appearance after aging test and the situation that leaches insolubles.
As seen from Figure 3, oil product is through after aging test, and three kinds of oil products are similar to the corrosion condition of copper sheet, but two kinds of oil products generation insolubless of oil product A and oil product B are comparatively serious.This result shows that tentatively oil product C ageing stability is better than other two kinds of products.In order to confirm conclusions, we have carried out the investigation of insolubles and copper sheet mass change to aged product, analyze data and see Table 3.
Table 3 sample insolubles and copper sheet mass change situation
Can be found out by data in table 3, three kinds of oil products are similar to the extent of corrosion of copper sheet.But two kinds of oil products of oil product A and oil product B are through producing more insolubles after aging test, wherein oil product A is especially serious.In addition, the filterableness test findings shows, and is defective through oil product A after aging test and two kinds of oil product filterableness indexs of oil product B, and oil product C still satisfies index request.
4. conclusion
Above result shows that oil product C ageing resistance is better than other two kinds of oil products, and its result with aforementioned deduction is consistent, this shows,, comprehensively evaluation quick to oil product that the lubricating oil product ageing resistance assessment method that the present invention sets up can be realized.
Embodiment 3
For relatively test method that the present invention sets up and existing method in the difference aspect evaluation lubricating oil ageing resistance, utilize respectively test method of the present invention and at present in the industry the most common method (GB/T 12581-2006 inhibiting mineral oil oxidation characteristic determination method) ageing resistance of A, B, three kinds of oil products of C (oil product is with embodiment 1) is estimated.
GB/T 12581 methods are that sample is having under water and copper-iron catalyst existence condition, at 95 ℃ and oxygen reaction, utilize acid number to reach the 2.0mgKOH/g required time or changing to characterize the oxidation stability of oil product through the acid number after certain reaction time for certain oil product.For oil product that this patent is investigated, according to the GB requirement, the reaction time is 1000h, and the acid number after utilization reaction 1000h is investigated the oxidation stability of oil product.
In addition, utilize simultaneously test method of the present invention that oil product is estimated, test condition is set as follows: test temperature is 150 ℃, it is 5L/h that air passes into speed, add the 5.5g copper sheet as catalyzer, test period 168h, test item comprise viscosity, colourity, acid number, pentane insolubles, copper corrosion, copper sheet weightlessness and greasy filth trend.
The test findings of utilizing two kinds of test methods to obtain sees Table 4.
The test result of table 4 oil product
Above result shows, after utilizing GB/T 12581 methods that three kinds of oil products are evaluated, before and after three kinds of oil tests, acid number changes not obvious, and be that three kinds of oil products are specification product (GB/T 11118.1 regulations by the evaluation result that the method obtains, after process 1000h, acid number is not more than 2.0mgKOH/g and both had been specification product).
After utilizing test method of the present invention that three kinds of oil products are evaluated, the projects such as the viscosity of oil product A, acid number, pentane insolubles and greasy filth trend all have obvious variation, illustrate that this oil product is obviously aging; Oil product B has comparatively significantly on two of pentane insolubles and greasy filth trend and changes, and illustrates that to a certain degree aging also occured this oil product; Oil product C by aging test all cash in every respect relatively stable.By comprehensive investigation of above test, difference that can clear and definite three kinds of oil product ageing resistances, namely oil product C is best, and A is the poorest for oil product, and oil product B is placed in the middle.
Can find out by comparing two kinds of test methods, adopt GB/T 12581 can not reach thoroughly evaluating oil product ageing resistance, thereby reach the purpose of distinguishing the oil product quality, and adopt the self-built test method of this patent within a short period of time oil product comprehensively to be estimated, reach the purpose of distinguishing the product quality.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements, all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (8)
1. oil ageing Reliable Evaluating Methods of Their Performance, it is characterized in that, it adopts in lubricating oil to be measured and passes into the air or oxygen that flow is 3-15L/h, under oil temperature 100-200 ℃, metallic catalyst condition, through 20-200 hour, then measure lubricating oil viscosity, colourity, acid number, resistance to emulsion, pentane insolubles, copper corrosion, copper sheet weightlessness and the every ageing properties of greasy filth trend, according to the variation of lubricants performance to be measured before and after test, the oil ageing performance is evaluated.
2. method according to claim 1, is characterized in that, described oil temperature is controlled at 150-180 ℃, preferably 150 ℃.
3. method according to claim 1, is characterized in that, the flow of described air or oxygen is 5-10L/h, preferably 5L/h.
4. method according to claim 1, is characterized in that, the described time is controlled at 120-180 hour, preferably 168 hours.
5. according to claim 1-4 described methods of any one, is characterized in that, described metallic catalyst is copper or iron.
6. method according to claim 5, is characterized in that, described metallic catalyst is copper sheet or iron plate.
7. method according to claim 6, is characterized in that, described copper sheet adopts is purity greater than 99.9% cathode copper, and the wide of described copper sheet be 12.5mm, and thick be 1.5-3.0mm, and growing is 75mm.
8. method according to claim 1 and 2, is characterized in that, described oil temperature adopts constant temperature oven, baking oven, metal bath or oil bath mode to control.
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