CN112557634B - Method for evaluating performance of diesel oil and application - Google Patents
Method for evaluating performance of diesel oil and application Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000002283 diesel fuel Substances 0.000 title claims abstract description 21
- 238000001914 filtration Methods 0.000 claims abstract description 127
- 239000012528 membrane Substances 0.000 claims abstract description 94
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 22
- 231100000719 pollutant Toxicity 0.000 claims abstract description 22
- 238000011156 evaluation Methods 0.000 claims abstract description 18
- 239000000356 contaminant Substances 0.000 claims abstract description 14
- 239000003365 glass fiber Substances 0.000 claims description 19
- 238000000967 suction filtration Methods 0.000 claims description 13
- 229920002678 cellulose Polymers 0.000 claims description 9
- 238000012360 testing method Methods 0.000 abstract description 27
- 230000008569 process Effects 0.000 abstract description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 24
- 239000003921 oil Substances 0.000 description 12
- 239000011521 glass Substances 0.000 description 10
- 238000012795 verification Methods 0.000 description 10
- 239000011148 porous material Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 6
- 238000011109 contamination Methods 0.000 description 5
- 239000000446 fuel Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000013215 result calculation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2829—Mixtures of fuels
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
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Abstract
The invention discloses a method for evaluating the performance of diesel oil and application thereof, and relates to the technical field of diesel oil performance evaluation; the evaluation step of the filtering performance comprises the following steps: theoretical filtration time t for obtaining a sample based on 1 0 Calculating the actual filtering time t 1 From the theoretical filtration time t 0 Is the difference of (2) t is; wherein, formula 1: t is t 0 = 80.07 ×v+48.46; v is the kinematic viscosity of the sample at 15-25 ℃; calculating the total contaminant content μ based on formula 3; wherein, formula 3:
m 0 for the mass, m of the filter membrane before filtration 1 For the mass of the filter membrane after filtration, ρ is the density of the sample at 15-25 ℃. The method can rapidly and effectively evaluate the filtering performance and total pollutants of the diesel oil through one test process, and compared with the prior art, the method considers the influence of the viscosity of the oil product, and the performance index of the obtained oil product is more reasonable.
Description
Technical Field
The invention relates to the technical field of diesel performance evaluation, in particular to a method for evaluating diesel performance and application thereof.
Background
Currently, the total contaminant assay is EN 12662:2014 "determination of total pollutant content in middle distillate, diesel oil and fatty acid methyl ester: about 300mL of the sample was weighed and filtered under vacuum through a pre-weighed glass fiber filter membrane having an average pore size of 0.7. Mu.m. The filter with residue was washed, dried and weighed. The total contaminant content was calculated using the mass difference of the filters and expressed in mg/kg. The method uses a large amount of solvent to wash the filter membrane, and the filter membrane is weighed after constant weight, so that the test time is long, the labor intensity is high, and a large amount of reagent is needed to influence the health of test personnel. It was determined the amount of particles in the sample having a diameter greater than 0.7 μm and insoluble in n-heptane.
The blocking tendency was measured by ASTM D2068, filter blocking tendency measurement, which measures the pressure differential across a filter and the volume of sample passing through the filter at a constant rate (20 mL/min) until the pressure applied to the filter reached 105kPa or the amount of fuel passing through the filter reached 300mL, and the pressure and flow rate were used to calculate the Filter Blocking Tendency (FBT), with lower FBT indicating better fuel. The standard comprises three methods, and the materials, sizes and areas of the filter membranes used are different. This standard has been converted in China into industry standard NB/SH/T0895-2015, middle distillate fuel and liquid fuel filter clogging tendency determination method. It reflects the amount of material in the sample with a diameter greater than 1.6 μm. In addition to inorganic substances, some organic substances such as microorganisms and wax particles can clog the filter screen.
In the use process of the oil product, besides the abrasion of the particulate matters in the oil product to the nozzle, whether impurities block the filter screen or not is also considered. In practice it was found that some oils were acceptable for FBT, but unacceptable for total contaminants. While other oils, FBT, are unacceptable, but the total contaminants are acceptable.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a method for evaluating the performance of diesel oil and application thereof.
The invention is realized in the following way:
in a first aspect, an embodiment of the present invention provides a method for evaluating performance of diesel fuel, the method including performing suction filtration on a sample to be evaluated, and evaluating filtration performance and/or total pollutants of the sample to be evaluated; the evaluation step of the filtering performance comprises the following steps: obtaining theoretical filtering time t of the sample to be evaluated based on the sample 1 0 Calculating the actual filtering time t of the sample to be evaluated based on the formula 2 1 And the theoretical filtering time t 0 Is the difference of (2) t is; wherein, formula 1: t is t 0 = 80.07 ×v+48.46; v is the kinematic viscosity of the sample to be evaluated at 15-25 ℃; formula 2: t=t 1 -t 0 ；
Evaluation of total pollutants: calculating the total pollutant content mu of the sample to be evaluated based on formula 3; wherein, formula 3:
m 0 for the quality of the filter membrane before filtration of the sample to be evaluated, m 1 For the quality of the filter membrane after filtration, ρ is the density of the sample to be evaluated at 15-25 ℃.
In a second aspect, an embodiment of the present invention provides an application of a filtering device in evaluating diesel performance, where the filtering device includes a sample bottle and a suction filter, an outlet of the sample bottle is communicated with an inlet of the suction filter, and a filter membrane is disposed at the inlet of the suction filter;
the evaluating diesel performance includes evaluating total pollutants and/or evaluating filtration performance.
The invention has the following beneficial effects:
the invention provides a method for evaluating diesel performance, which comprises the steps of carrying out suction filtration on a sample to be evaluated, and evaluating the sample to be evaluatedThe filtration performance of the sample and/or total contaminants; the evaluation step of the filtering performance comprises the following steps: obtaining theoretical filtering time t of the sample to be evaluated based on the sample 1 0 Calculating the actual filtering time t of the sample to be evaluated based on the formula 2 1 And the theoretical filtering time t 0 Is the difference of (2) t is; wherein, formula 1: t is t 0 = 80.07 ×v+48.46; v is the kinematic viscosity of the sample to be evaluated at 15-25 ℃; formula 2: t=t 1 -t 0 ；
Evaluation of total pollutants: calculating the total pollutant content mu of the sample to be evaluated based on formula 3; wherein, formula 3:
m 0 for the quality of the filter membrane before filtration of the sample to be evaluated, m 1 For the quality of the filter membrane after filtration, ρ is the density of the sample to be evaluated at 15-25 ℃.
The method can rapidly and effectively evaluate the filtering performance and total pollutants of the diesel oil through one test process, and compared with NB/SH/T0895-2015, the method considers the influence of the viscosity of the oil product, and the performance index of the obtained oil product is more reasonable.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view of a filtration device provided by the present invention;
FIG. 2 is a plot of filtration time versus volume for a filter membrane used for oxidation stability versus a diesel sample in accordance with verification example 4 of the present invention;
FIG. 3 is a plot of filter membrane versus secondary filtration time-volume for oxidation stability in accordance with verification example 4 of the present invention;
FIG. 4 is a plot of filtration time versus volume for a sample of diesel fuel using a glass fiber filter in accordance with verification example 4 of the present invention;
FIG. 5 is a graph showing the secondary filtration time-volume curve of the glass fiber filter in the verification example 4 of the present invention.
Icon:
1-a sample bottle; 2-filtering membrane; 3-supporting means; 4, filtering the mixture in a suction filtration bottle; 5-buffer bottles; 6-a vacuum controller; 7-vacuum pump.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
The embodiment of the invention provides a method for evaluating the performance of diesel oil, which comprises the steps of carrying out suction filtration on a sample to be evaluated, and evaluating the filtration performance and/or total pollutants of the sample to be evaluated; the evaluation step of the filtering performance comprises the following steps: obtaining theoretical filtering time t of the sample to be evaluated based on the sample 1 0 Calculating the actual filtering time t of the sample to be evaluated based on the formula 2 1 And the theoretical filtering time t 0 Is the difference of (2) t is; wherein, formula 1: t is t 0 = 80.07 ×v+48.46; v is the kinematic viscosity of the sample to be evaluated at 15-25 ℃; formula 2: t=t 1 -t 0 ；
Evaluation of total pollutants: calculating the total pollutant content mu of the sample to be evaluated based on formula 3; wherein, formula 3:
m 0 the mass, m of the filter membrane 2 before filtration for the sample to be evaluated 1 For the mass of the filter membrane 2 after filtration, ρ is the density of the sample to be evaluated at 15-25 ℃.
The inventor provides a method for evaluating the total pollutants and the filtering performance of the diesel through a series of creative labor, and the calculation parameters of the total pollutants and the filtering performance can be obtained through one-time test, so that the method is simple and easy to implement.
Preferably, the step of evaluating the filtering performance further includes: the filtration performance of the samples was evaluated based on the difference t.
When t is selected 0 And t 1 When the difference value t of the sample to be evaluated is evaluated, if t is less than or equal to a first threshold value, judging that the filtering performance of the sample to be evaluated is qualified, otherwise, judging that the filtering performance of the sample to be evaluated is unqualified;
preferably, the first threshold is 80 to 160s. In some embodiments, the first threshold may be selected from any of 80s, 90s, 100s, 102s, 104s, 106s, 108s, 110s, 112s, 114s, 116s, 118s, 120s, 122s, 124s, 126s, 128s, 130s, 132s, 134s, 136s, 138s, 140s, 150s, 160s.
Preferably, ρ is any density of the sample to be evaluated at 15 ℃, 16 ℃, 17 ℃, 18 ℃, 19 ℃, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃ and 25 ℃, preferably 20 ℃, the result of calculation being more reasonable.
Preferably, the filter membrane 2 is selected from any one of a glass fiber filter membrane 2 and a cellulose ester filter membrane 2. The glass fiber filter membrane 2 is preferable, and the evaluation result using the glass fiber membrane is more accurate and stable than other filter membranes 2.
Preferably, the diameter of the filter membrane 2 is 10-100 mm, and the pore diameter is 0.1-2 μm. The diameter and the pore diameter of the filter membrane directly influence the stability of the evaluation method; preferably, the diameter of the filter membrane 2 is 30-60 mm and the pore size is 0.45-0.7 μm.
Preferably, the pressure is 1 to 10kPa when the sample to be evaluated is suction-filtered. In some embodiments, the pressure may be selected from any of 1kPa, 2kPa, 3kPa, 4kPa, 5kPa, 6kPa, 7kPa, 8kPa, 9kPa, 10kPa.
Preferably, the pressure is 3 to 7kPa. A smaller vacuum will significantly extend the test time (t for certain high viscosity diesel samples at a vacuum of 2kPa 1 Up to 30.2 minutes) while a larger vacuum also increases t significantly 1 Random error of (a)(t of certain low viscosity Diesel samples at 10kPa vacuum.) 1 Only 172 s). Within this range, the obtained evaluation effect is better.
Preferably, the volume of the sample to be evaluated is 250-350 mL. In some embodiments, the volume of the sample to be evaluated is selected from any of 250mL, 260mL, 270mL, 280mL, 290mL, 300mL, 310mL, 320mL, 330mL, 340mL, 350mL.
In addition, the embodiment of the invention provides an application of a filtering device in evaluating diesel performance, referring to fig. 1, the filtering device comprises a sample bottle 1 and a suction filter, an outlet of the sample bottle 1 is communicated with an inlet of the suction filter, and a filter membrane 2 is arranged at the inlet of the suction filter;
the evaluating diesel performance includes evaluating total pollutants and/or evaluating filtration performance.
Preferably, the step of evaluating the filtration performance includes: obtaining theoretical filtering time t of the sample to be evaluated based on the sample 1 0 Calculating the actual filtering time t of the sample to be evaluated based on the formula 2 1 And the theoretical filtering time t 0 Is the difference of (2) t is; wherein, formula 1: t is t 0 = 80.07 ×v+48.46; v is the kinematic viscosity of the sample to be evaluated at 15-25 ℃; formula 2: t=t 1 -t 0 ；
Preferably, the step of evaluating the total contaminants comprises: calculating the total pollutant content mu of the sample to be evaluated based on formula 3; wherein, formula 3:
m 0 the mass, m of the filter membrane 2 before filtration for the sample to be evaluated 1 For the mass of the filter membrane 2 after filtration, ρ is the density of the sample to be evaluated at 15-25 ℃;
preferably, the step of evaluating the filtering performance further includes: the filtration performance of the samples was evaluated based on the difference t.
When t is selected 0 And t 1 When the difference value t of the sample to be evaluated is evaluated, if t is less than or equal to a first threshold value, judging that the filtering performance of the sample to be evaluated is qualified, otherwise, judging that the filtering performance of the sample to be evaluated is unqualified.
In some embodiments, the sample bottle 1 may be a graduated glass, and the suction filter may specifically include: filter membrane 2, strutting arrangement 3 (can set up stainless steel mesh support sieve in it), suction flask 4, buffer bottle 5, vacuum controller 6 and vacuum pump 7.
The support device 3 is used for supporting the filter membrane 2, the inlet of the support device is connected with the sample bottle 1, the outlet of the support device is connected with the suction filter bottle 4, the suction filter bottle 4 is connected with the vacuum controller 6 through the buffer bottle 5, and the vacuum pump 7 is connected with the vacuum controller 6.
Alternatively, the support means 3 may be a funnel.
Preferably, the filter membrane 2 is selected from any one of a glass fiber filter membrane 2 and a cellulose ester filter membrane 2.
Preferably, the diameter of the filter membrane 2 is 10-100 mm, and the pore diameter is 0.1-10 μm.
Example 1
The invention provides a filtering device for evaluating diesel oil products, which comprises: sample bottle 1 and suction filter, please refer to fig. 1.
In this embodiment, the sample bottle 1 is a graduated cylinder, which can hold 350mL of sample, and has a score line at least every 50mL.
The suction filter comprises: filter membrane 2, support device 3 (in which stainless steel mesh support sieve plate is arranged) for supporting filter membrane 2, suction filtration bottle 4, buffer bottle 5, precision vacuum controller 6 and vacuum pump 7. The support device 3 is arranged at the bottleneck at the top end of the suction filtration bottle 4 and connected with the outlet at the bottom end of the sample bottle 1, and the filter membrane 2 is arranged at the support device 3; the inlet of the buffer bottle 5 is communicated with the outlet of the filter bottle, and the outlet of the buffer bottle 5 is communicated with the vacuum controller 6; a vacuum pump 7 is connected with the vacuum controller 6.
Wherein the filter membrane 2 is a glass fiber filter membrane 2, the diameter is 47mm, and the nominal pore diameter is 0.7 μm. The support means 3 is a funnel. The buffer bottle 5 is a sealable glass bottle, the inlet of which is communicated with the outlet of the filter bottle, and the outlet of which is communicated with the vacuum controller 6. The controllable vacuum degree of the precise vacuum controller 6 is 3 kPa-99 kPa, and the highest control precision is not lower than +/-0.1 kPa.
In other embodiments, the materials of the sample bottle 1, the filter flask 4 and the buffer bottle 5 are not limited to the most, and may be selected from other materials, such as plastic, wood or metal.
Example 2
A method of evaluating diesel fuel performance using the filtration device provided in example 1, the method comprising: instrument preparation, sample suction filtration, filter membrane 2 washing weighing and result calculation.
(1) Instrument preparation
1.1, ensuring the interior and exterior of the filter device to be clean.
1.2, other parts of the filter device except the filter membrane 2 are assembled as shown in fig. 1, the inside of the filter device is cleaned by n-heptane, the sealing between the sample bottle 1 and the suction filter bottle 4 is ensured, and the tightness among the plug, the hose and the bottle body is ensured by using a proper sealing material.
1.3, placing the filter membrane 2 on a support sieve plate of a pre-cleaned instrument, ensuring that the filter membrane 2 is placed in the center of the support sieve plate and cannot damage the filter membrane 2, flushing the filter membrane 2 with n-heptane under vacuum, slowly releasing the vacuum, carefully removing the filter membrane 2 from the support sieve plate with tweezers, placing the filter membrane 2 in a culture dish, covering the culture dish, and placing the culture dish in an oven at 110+/-5 ℃ for at least 45min.
1.4, taking the petri dish with the filter membrane 2 out of the oven, covering a cover, and putting the petri dish into a dryer for cooling for about 45min.
1.5, before testing, the filter membrane 2 was taken out of the petri dish, and immediately the mass of the filter membrane 2 was weighed with an analytical balance to the nearest 0.1mg, the mass recorded as m 0 。
1.6, directly placing the weighed filter membrane 2 on a pre-cleaned supporting plate, clamping the upper and lower parts of the supporting sieve plate and the funnel by using clamps, and fixing the filter membrane 2. The filter membrane 2 was immersed in n-heptane to ensure that the filter membrane 2 was bubble free and firmly secured between the polished surfaces of the filter device.
(2) Sample suction filtration
2.1, the vacuum pump 7 was turned on with the control value of the vacuum controller 6 set to 5.0kPa.
2.2, 300mL of sample was quickly poured into the cartridge of the filter device at one time, and timing was started.
2.3, stop timing when 300mL sample just filtered. The time is recorded as t 1 。
2.4, when the method is only used for judging whether the oil product has quality problems, if the filtering time of the sample is 120s longer than the theoretical filtering time calculated by the formula 2 before 300mL of the sample is filtered, the test can be stopped. If the filtration time does not exceed the theoretical filtration time of 120s after 300mL filtration is completed, then a filter membrane 2 rinse weighing step is performed.
(3) Filter membrane 2 flushing and weighing
3.1, the control value of the vacuum controller 6 was set to 95kPa, the precipitate in the measuring cylinder was rinsed onto the filter membrane 2 with n-heptane in the wash bottle, the inner wall and bottom of the measuring cylinder were carefully rinsed with n-heptane, and the washing solution was filtered. This washing operation was repeated twice.
3.2, flushing the inner wall of the filter funnel and the filter membrane 2 with n-heptane in the wash bottle, and sucking to dryness. The washing operation should be repeated at least twice with a gentle stream of solvent, moving the wash funnel circumferentially.
3.3 carefully remove the funnel and rinse filter membrane 2 from edge to center with a gentle stream of n-heptane under vacuum. Note that the particles on the surface of the filter membrane 2 are not washed away, and the vacuum pumping is continued until 10 s-15 s after the washing is finished or until the washing liquid on the filter membrane 2 is completely pumped away.
3.4, slowly releasing the vacuum, carefully removing the filter membrane 2 from the support sieve plate with clean tweezers, placing the filter membrane 2 in a petri dish, drying in a 110 ℃ oven at 5 ℃ for 45min (without covering the cover during drying), taking out, covering the cover, and cooling in a dryer for about 45min.
3.5, taking the filter membrane 2 out of the culture dish, weighing the filter membrane 2 by an analytical balance to the accuracy of 0.1mg, and recording the mass as m 1 。
(4) Result calculation
4.1, evaluating the filtration performance:
calculating the theoretical filtration time t of the sample according to the formula 1 0 (s)；
Formula 1: t is t 0 ＝80.07×v+48.46；
Wherein v is the followingThe kinematic viscosity of the sample to be evaluated at 20℃in mm 2 /s。
The difference t(s) between the actual filtering time t1 and the theoretical filtering time t0 of the sample is calculated according to the formula 2:
formula 2: t=t 1 -t 0 ；
When the difference t is less than or equal to 120s (first threshold), the sample is reported to be qualified in filtration performance, and when the difference t is greater than 120s, the sample is reported to be unqualified in filtration performance.
4.2, evaluating total contamination:
calculating the total pollution amount mu of the sample according to a formula 3;
formula 3:
wherein m is 0 For the quality of the filter membrane 2 before filtration of the sample to be evaluated, mg, m 1 For the mass of the filter membrane 2 after filtration, mg, ρ is the density of the sample to be evaluated at 20℃g/cm 3 。
Verification example 1
The method of example 2 was used to determine various diesel fuels, and the information and evaluation results of the diesel fuels are shown in Table 1.
Table 1 verification experiment
Remarks: the kinematic viscosity was that at 20 ℃.
As can be seen from Table 1, the FBT is measured as NB/SH/T0895-2015, and the limit value of FBT is usually 2-3, if FBT is 2.0, the threshold value of T is 87s; if FBT is set equal to 2.5, t is set to a threshold of 120s; if FBT is set equal to 3.0, t is thresholded to 152s.
In foreign standards, some FBT limits are 2.0 and others are 3.0. Considering the diesel oil condition in China and the influence of test errors, the threshold value of t is preferably set to 120s.
The threshold setting of t was verified and the results are shown in table 1.
As can be seen from Table 1, for the high contamination samples, the filtration time difference was much less than 120 when the obstruction was small (< 1.9), and much greater than 120 when the obstruction was large (. Gtoreq.1.9). For the vehicle diesel oil samples, the filtering time difference is far less than 120 and is only 55s at maximum, which indicates that the selected threshold value is reasonable and the distinguishing property is obvious. Some samples have negative differences in filtration time, which may be due to test errors on the one hand, and higher temperatures at the time of testing than when calculating theoretical filtration time, resulting in lower viscosity at the time of filtration.
Verification example 2
The reproducibility of the test using the method of example 2 was verified.
The method of example 2 was used to determine different diesel oils and the test was repeated 2 times, the test results are shown in Table 2.
Table 2 experimental results
Remarks: the kinematic viscosity was that at 20 ℃.
Verification example 3
The vacuum level selected in the support screen plate and the suction filtration process provided in example 2 in the filtration apparatus of example 1 of the present invention was verified.
The verification example adopts a glass sand core and a stainless steel net to respectively measure some samples, and the measured pollution degree has no systematic difference.
Then, diesel oil samples with total pollutant content near the limit value and relatively clean were prepared, a glass sand core supporting sieve plate and a stainless steel supporting plate were respectively adopted, and vacuum degrees of 5kPa and 10kPa were respectively adopted for suction filtration for measurement, and the results are shown in Table 3.
TABLE 3 filtration results of glass sand core support plates at different vacuum degrees
As can be seen from Table 3, if a glass core support plate is used, a time of 547s is required to filter 250mL even for a relatively clean sample at a vacuum of 5 kPa. For a sample with a contamination level of 26mg/kg, 250mL was filtered for up to 1508s. When the vacuum degree is 10kPa, the time for filtering 250mL of a sample with the pollution degree of 26mg/kg is 948s, and the time for filtering 250mL of a relatively clean oil product is only about 172 s.
If a stainless steel mesh is used to support the screen plate, 300mL of sample is filtered for 426s when the vacuum is 5 kPa. For a sample with a contamination level of 22mg/kg, 300mL was filtered for 590s. When the vacuum degree is 10kPa, 300mL of the sample with the pollution degree of 22mg/kg is filtered for 359s, and 300mL of the sample is filtered for 250s in comparison with a clean oil product.
From the above results, it was found that the glass sand core support plate was suitable for a vacuum of 10kPa, while the stainless steel mesh support plate was suitable for a vacuum of 5 kPa. For this reason, because the glass sand core support plate has a pore size of 30 μm and is thick, and thus a pressure drop occurs, we measure the vacuum level (10 kPa) in the suction flask, and the actual vacuum level at the filter membrane should be much lower than 10kPa. The stainless steel net is thin and the mesh is large, and the vacuum degree in the suction filter bottle is the same as that at the filter membrane. In order to avoid the influence of the difference of different glass sand cores on the vacuum degree, a stainless steel net is recommended to be used for supporting the sieve plate.
Verification example 4
1. The test was performed with the cellulose ester filter used for oxidation stability.
1.1 filtration test of samples.
Table 4 viscosity and total contamination of formulated samples
TABLE 5 filtration results of oxidation-stable filter membrane on samples (unit: s)
300mL of the sample in Table 4 was taken respectively using a filter membrane (nominal pore size 0.8 μm) for oxidation stability, and was put into a graduated glass cylinder of the filter apparatus provided in example 1, and the time was started and recorded as t 0 Time, then every 50mL of sample was filtered, record time until filtration was completed. During the test, the vacuum was maintained at 5.0kPa. The test results are shown in FIG. 2 and Table 5.
As can be seen from FIG. 2, samples were sequenced in order of 3#, 1#, 2#, 6#, 4#, 5#, 7#, 8# according to the length of the filtration time, and the total pollutant content in Table 8 was greatly different.
1.2, secondary filtration test
The filtered oil was filtered again in the same manner as the sample filtered in the previous paragraph, and the test results are shown in fig. 3 and table 6.
TABLE 6 filtration results of oxidation-stable filter membrane on secondary samples (unit: s)
Since the contaminants in the sample are not much, the viscosity of the sample before and after filtration is considered to be unchanged. Since the samples have been filtered through the membrane, most of the contaminants having a diameter greater than 0.8 μm having been removed at the time of the first filtration, it is considered that the samples no longer or less contain macromolecular substances that have an effect on the filtration performance of the membrane, and the filtration times of these samples should be relatively close. However, as can be seen from FIG. 3, the filtering times of 6# -2 and 7# -2 are greatly different from those of other samples.
2. The test was performed with a glass fiber filter membrane for total contaminants.
2.1 sample filtration test
300mL of the sample in Table 4 was taken using a glass fiber filter membrane (nominal pore size 0.7 μm) for the total contaminants, and the samples were filtered according to the procedure in step 1.1, and the test results are shown in FIG. 4 and Table 7.
TABLE 7 filtration results of glass fiber filters on samples (unit: s)
As can be seen from fig. 4 and table 7, the order of the samples in order of the filtration time is completely identical to the order of the total contaminant content in table 4.
2.2 secondary filtration test
The above filtered samples were collected and the filtered oil was re-filtered according to the same procedure, and the test results are shown in fig. 5 and table 8.
TABLE 8 filtration results of glass fiber filters on secondary samples (unit: s)
As can be seen from fig. 5 and table 8, the filtration times of the secondary samples were relatively close.
Comparing the test results of the glass fiber filter membrane and the cellulose ester filter membrane, the regularity of the result of the glass fiber filter membrane is far better than that of the cellulose ester filter membrane for a primary sample; for the secondary samples, the regularity of the results, which are also for glass fiber filters, is better than for cellulose ester filters. This demonstrates that the consistency between the glass fiber filters used is better than that of the cellulose ester filters. The following test was performed using only glass fiber membrane filters.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A method for evaluating the performance of diesel oil, which is characterized by comprising the steps of carrying out suction filtration on a sample to be evaluated and evaluating the filtration performance of the sample to be evaluated;
the evaluation step of the filtering performance comprises the following steps: obtaining theoretical filtering time t of the sample to be evaluated based on the sample 1 0 Calculating the actual filtering time t of the sample to be evaluated based on the formula 2 1 And the theoretical filtering time t 0 Is the difference of (2) t is; wherein, formula 1:
the method comprises the steps of carrying out a first treatment on the surface of the v is the kinematic viscosity of the sample to be evaluated at 15-25 ℃; formula 2:
；
the step of filtering performance further comprises: evaluating the filtering performance of the sample based on the difference t; when t is selected 0 And t 1 When the difference value t of the sample to be evaluated is evaluated, if t is less than or equal to a first threshold value, judging that the filtering performance of the sample to be evaluated is qualified, otherwise, judging that the filtering performance of the sample to be evaluated is unqualified; the first threshold value is 80-160 s;
the filtering membrane is selected from any one of a glass fiber filtering membrane and a cellulose ester filtering membrane, the diameter of the filtering membrane is 10-100 mm, the aperture is 0.1-2 mu m, the pressure is 1-10 kPa when the sample to be evaluated is subjected to suction filtration, and the volume of the sample to be evaluated is 250-350 mL.
2. The method of claim 1, further comprising the step of evaluating total contaminants of the sample, the total contaminants being evaluated: calculating the total pollutant content [ mu ] of the sample to be evaluated based on the formula 3; wherein, formula 3:
；m 0 for the quality of the filter membrane before filtration of the sample to be evaluated, m 1 And for the quality of the filtered filter membrane, ρ is the density of the sample to be evaluated at 15-25 ℃.
3. The application of the filtering device in evaluating the performance of diesel oil is characterized in that the filtering device comprises a sample bottle and a suction filter, wherein the outlet of the sample bottle is communicated with the inlet of the suction filter, and a filter membrane is arranged at the inlet of the suction filter;
the evaluation of the diesel performance comprises the evaluation of total pollutants of a sample to be evaluated and/or the evaluation of filtering performance;
the evaluation step of the filtering performance comprises the following steps: obtaining theoretical filtering time t of the sample to be evaluated based on the sample 1 0 Calculating the actual filtering time t of the sample to be evaluated based on the formula 2 1 And the theoretical filtering time t 0 Is the difference of (2) t is; wherein, formula 1:
the method comprises the steps of carrying out a first treatment on the surface of the v is the kinematic viscosity of the sample to be evaluated at 15-25 ℃; formula 2:
；
the step of evaluating the filtering performance further comprises: evaluating the filtering performance of the sample based on the difference t;
the filtering membrane is selected from any one of a glass fiber filtering membrane and a cellulose ester filtering membrane, the diameter of the filtering membrane is 10-100 mm, the aperture is 0.1-2 mu m, the pressure is 1-10 kPa when the sample to be evaluated is subjected to suction filtration, and the volume of the sample to be evaluated is 250-350 mL.
4. The use of claim 3, wherein said evaluating diesel fuel performance further comprises evaluating total pollutants, said evaluating step comprising: calculating the total pollutant content [ mu ] of the sample to be evaluated based on the formula 3; wherein, formula 3:
；m 0 for the quality of the filter membrane before filtration of the sample to be evaluated, m 1 And for the quality of the filtered filter membrane, ρ is the density of the sample to be evaluated at 15-25 ℃. />
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