CN106124744A - A kind of method testing coal tar pitch rheological characteristic - Google Patents
A kind of method testing coal tar pitch rheological characteristic Download PDFInfo
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- CN106124744A CN106124744A CN201610700878.5A CN201610700878A CN106124744A CN 106124744 A CN106124744 A CN 106124744A CN 201610700878 A CN201610700878 A CN 201610700878A CN 106124744 A CN106124744 A CN 106124744A
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- G—PHYSICS
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- 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
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Abstract
The present invention relates to a kind of method testing coal tar pitch rheological characteristic.It is characterized in that using rotational viscometer to measure coal tar pitch apparent viscosity, rotor torque percentage meter scale controls to be 40% 60%.In measurement, at interval of apparent viscosity of 3 minutes 10 minutes records, calculate the rate of change of adjacent twice apparent viscosity value.Apparent viscosity according to different temperature points measures numeric renderings temperature-vis-cosity curve, utilizes the fit curve equation formula of temperature apparent viscosity relation to calculate the coal tar pitch apparent viscosity of arbitrary temp point in the range of measurement.The present invention can improve coal tar pitch apparent viscosity measurement accuracy, reduce the difference of different experiments room apparent viscosity measured value, in producing for Carbon Materials, the determination of kneading and molding technique parameter provides the Data safeguard of science, thus is that the carbonaceous product producing high-quality provides safeguard.
Description
Technical field
The present invention relates to a kind of method testing coal tar pitch rheological characteristic.
Background technology
The method of the rheological property measuring fluid includes capillary tube method, Constructional Elements Using Falling Methods, circumgyration and vibratory drilling method etc., generally uses
The rheological property of coal tar pitch under rotational viscometer Study of Liquid state.Liquid coal Colophonium is non-newtonian liquid, shear stress with cut
Cutting speed rate is not a fixed ratio.For non-newtonian liquid, the viscosity so recorded is referred to as apparent viscosity.Along with coal tar pitch is subject to
The raising of hot temperature, apparent viscosity numerical value presents first rapid decrease, the rear rule slowly declined.But in a certain concrete measurement temperature
Degree point, the apparent viscosity of coal tar pitch is affected bigger by temperature retention time and detecting instrument rotor torque.
At certain temperature point, along with the prolongation of temperature retention time, the apparent viscosity of coal tar pitch also changes slowly.Due to
It is different that viscosity has been stablized view by different research worker, and the standard not determined causes same coal tar pitch in phase
The apparent viscosity numerical value of synthermal measurement there are differences.The research of coal tar pitch rheological property needs to measure continuously different temperature points
Apparent viscosity, the measuring method of previous temperature and result, can remote-effects to the difference of other temperature spot apparent viscosity numerical value
Different.
When measuring the apparent viscosity of coal tar pitch, rotational viscometer rotor is referred to as moment of torsion by resistance in a liquid, with
Percentage meter scale, equipment manufacturers' regulation percentage meter scale is normal value between 20%-90% or 10%-90%.But no
It is the difference that there is certain numerical value with the apparent viscosity measured under percentage meter scale.Rotor slowly runs and the testing time can be made to prolong
Long, the coal tar pitch component under long-time high temperature will change, and apparent viscosity has increase tendency, causes the difference of measured value equally
Different.
During Carbon Materials produces, need to determine kneading and molding technique parameter according to the rheological property of coal tar pitch, inaccurate
Apparent viscosity numerical value will mislead the formulation of technological parameter, causes product defects, even waste product.
Summary of the invention
It is an object of the invention to the deficiency for above-mentioned prior art, it is provided that one can improve coal tar pitch apparent viscosity and measure
Accuracy, the method reducing the test coal tar pitch rheological characteristic of the difference of different experiments room apparent viscosity measured value.
It is an object of the invention to be achieved through the following technical solutions.
A kind of method testing coal tar pitch rheological characteristic, it is characterised in that use rotational viscometer to measure coal tar pitch apparent glutinous
Degree, rotor torque percentage meter scale controls as 40%-60%.
A kind of method testing coal tar pitch rheological characteristic of the present invention, it is characterised in that measure the apparent viscosity of a certain temperature spot
Time, at interval of apparent viscosity of 3 minutes-10 minutes records, when adjacent twice apparent viscosity rate of change is not more than 2%, note
Record is the apparent viscosity of Current Temperatures point.
A kind of method testing coal tar pitch rheological characteristic of the present invention, it is characterised in that according to the apparent viscosity of different temperature points
Measure numeric renderings temperature-apparent viscosity curve, use excel or Origin etc. to have the software of data processing function, utilize soft
Curve matching function in part, does 3-6 order polynomial matchings to the temperature-apparent viscosity curve drawn, and obtains temperature-apparent glutinous
The matched curve of degree relation and equation y=ax thereof6+bx5+cx4+dx3+ex2+ fx+g, wherein y is apparent viscosity, mPas；X is
Test temperature-softening point temperature, DEG C；A, b, c, d, e, f and g are that (Colophonium owing to producing under different process system exists constant
Composition difference, therefore the constant of different pitches is different numerical value), wherein goodness of fit R2More than 0.98.
The present invention a kind of method testing coal tar pitch rheological characteristic, it is characterised in that be to utilize temperature-apparent viscosity to close
The fit curve equation formula of system calculates the coal tar pitch apparent viscosity of arbitrary temp point in the range of measurement.
For a kind of method testing coal tar pitch rheological characteristic of the present invention, research worker sticks according to the apparent of different temperature points
Number of degrees value, draws matched curve by the Arrhenius Equation, establishes arbitrary temp point and apparent viscosity pair in the range of measurement
(see accompanying drawing 1) should be related to.From the figure, it can be seen that low-temperature zone measured value and match value differ greatly, along with temperature raises, both
Difference diminish.
A kind of method testing coal tar pitch rheological characteristic of the present invention, can improve coal tar pitch apparent viscosity measurement accuracy, subtract
The difference of few different experiments room apparent viscosity measured value, the determination offer section of kneading and molding technique parameter in producing for Carbon Materials
The Data safeguard learned, thus be that the carbonaceous product producing high-quality provides safeguard.
Accompanying drawing explanation
Fig. 1 is arbitrary temp point in the range of measuring and apparent viscosity corresponding relation figure.
Fig. 2 is the apparent viscosity numeric renderings temperature-viscosity curve figure in embodiment 1 according to different temperature points.
Fig. 3 is the apparent viscosity numeric renderings temperature-viscosity curve in embodiment 2 according to different temperature points.
Fig. 4 is the apparent viscosity numeric renderings temperature-viscosity curve in embodiment 3 according to different temperature points.
Fig. 5 is higher than 48 DEG C of-98 DEG C of intervals of softening point temperature value (i.e. 150 DEG C-200 DEG C) in embodiment 3, draws temperature
Degree-viscosity curve figure.
Detailed description of the invention
A kind of method testing coal tar pitch rheological characteristic, uses the apparent viscosity rotating the viscosity apparatus lower coal tar pitch of measurement temperature.
During the measurement of viscosity, rotor inserts in the sample cylinder filling coal tar pitch.In coal tar pitch, institute is rotated by measuring rotor
The moment of torsion produced measures the comparative resistance of rotation, and moment of torsion determines coal tar pitch apparent viscosity with the ratio of speed.In measurement, need
Control rotor torque percentage meter scale, at 40%-60%, at interval of apparent viscosity of 3 minutes-10 minutes records, calculates adjacent
Twice apparent viscosity rate of change.When adjacent twice apparent viscosity rate of change is not more than 2%, it is recorded as the apparent of Current Temperatures point
Viscosity.
Apparent viscosity value input excel or Origin etc. measured at a temperature of temperature and this there is the soft of data processing function
In part, x-axis represents that temperature, y-axis represent k value, draws temperature-apparent viscosity curve.Utilize curve matching function in software,
Temperature-apparent viscosity the curve drawn is done 3-6 order polynomial matchings, obtains the matched curve of temperature-apparent viscosity relation
And equation y=ax6+bx5+cx4+dx3+ex2+ fx+g, wherein y is apparent viscosity, mPas；X is test temperature-softening point temperature
Degree, DEG C；A, b, c, d, e, f and g are constants, wherein goodness of fit R2More than 0.98.Utilize the matching of temperature-apparent viscosity relation
Fitting equation calculates the coal tar pitch apparent viscosity of arbitrary temp point in the range of measurement.
Embodiment 1
After one coal tar pitch is processed except water, make powder, and the softening point analyzing coal tar pitch is 103.5 DEG C.
Measuring coal tar pitch apparent viscosity according to rotating viscosity apparatus rule of operation, the selected scope of initial temperature is softening point temperature
Angle value increases by 10 DEG C-30 DEG C (i.e. 113.5 DEG C-143.5 DEG C), and this initial temperature is set to 120 DEG C.Regulation rotor torque percentage
Meter scale controls at 40%-60%, apparent viscosity of every 5 minutes records, calculates adjacent twice apparent viscosity rate of change.Work as table
See viscosity rate of change and be less than 1%, be recorded as the apparent viscosity of 120 DEG C.Improve 5 DEG C of apparent viscosities doing next temperature spot to measure,
Repeating aforesaid operations, maximum temperature increases to 200 DEG C.Coal tar pitch apparent viscosity analytical data sees attached list 1.
Apparent viscosity numeric renderings temperature-viscosity curve (see accompanying drawing 2) according to different temperature points, utilizes 5 order polynomials
To its matching (dotted line in figure), the temperature obtained-apparent viscosity governing equation is y=-0.0004x5+0.1339x4-
16.886x3+1038x2-31282x+375224, R2=0.9974.Any temperature in the range of equation can be utilized to calculate measurement
The coal tar pitch apparent viscosity of degree point.
Embodiment 2
After one coal tar pitch is processed except water, make powder, and the softening point analyzing coal tar pitch is 100 DEG C.
Measuring coal tar pitch apparent viscosity according to rotating viscosity apparatus rule of operation, the selected scope of initial temperature is softening point temperature
Angle value increases by 10 DEG C-30 DEG C (i.e. 110 DEG C-130 DEG C), and this initial temperature is set to 120 DEG C.Regulation rotor torque percentage meter mark
Degree controls at 40%-60%, apparent viscosity of every 3 minutes records, calculates adjacent twice apparent viscosity rate of change.When apparent glutinous
Degree rate of change, less than 0.6%, is recorded as the apparent viscosity of 120 DEG C.Improve 5 DEG C of apparent viscosities doing next temperature spot to measure, weight
Multiple aforesaid operations, maximum temperature increases to 200 DEG C.Coal tar pitch apparent viscosity analytical data sees attached list 2.
Apparent viscosity numeric renderings temperature-viscosity curve (see accompanying drawing 3) according to different temperature points, utilizes 5 order polynomials
To its matching (dotted line in figure), the temperature obtained-apparent viscosity governing equation is y=-0.0005x5+0.1662x4-
22.374x3+1474.2x2-47750x+614139, R2=0.998.Any temperature in the range of equation can be utilized to calculate measurement
The coal tar pitch apparent viscosity of degree point.
Embodiment 3
After one coal tar pitch is processed except water, make powder, and the softening point analyzing coal tar pitch is 102 DEG C.
Measuring coal tar pitch apparent viscosity according to rotating viscosity apparatus rule of operation, the selected scope of initial temperature is softening point temperature
Angle value increases by 10 DEG C-30 DEG C (i.e. 112 DEG C-132 DEG C), and this initial temperature is set to 120 DEG C.Regulation rotor torque percentage meter mark
Degree controls at 40%-60%, apparent viscosity of every 10 minutes records, calculates adjacent twice apparent viscosity rate of change.When apparent
Viscosity rate of change is less than 2%, is recorded as the apparent viscosity of 120 DEG C.Improve 5 DEG C of apparent viscosities doing next temperature spot to measure, weight
Multiple aforesaid operations, maximum temperature increases to 200 DEG C.Coal tar pitch apparent viscosity analytical data sees attached list 3.
Apparent viscosity numeric renderings temperature-viscosity curve (see accompanying drawing 4) according to different temperature points, utilizes 6 order polynomials
To its matching (dotted line in figure), the temperature obtained-apparent viscosity governing equation is the temperature-apparent viscosity relation equation obtained
Formula is y=0.000007x6-0.002891x5+0.457208x4-37.706975x3+1716.274855x2-41224.581186x
+ 415491.012556, R2=0.999098.Equation can be utilized to calculate the coal tar pitch of arbitrary temp point in the range of measurement
Apparent viscosity.
Higher than 48 DEG C of-98 DEG C of intervals of softening point temperature value (i.e. 150 DEG C-200 DEG C), draw temperature-viscosity curve (see attached
Fig. 5), utilizing 3 order polynomials is the temperature obtained to its matching (dotted line in figure), the temperature obtained-apparent viscosity governing equation
Degree-apparent viscosity governing equation is y=-0.0299x3+7.6232x2-652.2x+18939, R2=0.9972.Can utilize
Equation calculates the coal tar pitch apparent viscosity of arbitrary temp point in the range of said temperature.
Table 1
Table 2
Table 3
Claims (4)
1. the method testing coal tar pitch rheological characteristic, it is characterised in that use rotational viscometer to measure coal tar pitch apparent viscosity,
Rotor torque percentage meter scale controls as 40%-60%.
A kind of method testing coal tar pitch rheological characteristic the most according to claim 1, it is characterised in that measure a certain temperature spot
Apparent viscosity time, at interval of 3 minutes-10 minutes record apparent viscosity, when adjacent twice apparent viscosity rate of change is little
In 2% time, it is recorded as the apparent viscosity of Current Temperatures point.
3. according to a kind of method testing coal tar pitch rheological characteristic described in claim 1 and 2, it is characterised in that according to different temperatures
The apparent viscosity of point measures numeric renderings temperature-apparent viscosity curve, uses excel or Origin data processing software, utilizes
Curve matching function in software, does 3-6 order polynomial matchings to the temperature-apparent viscosity curve drawn, and obtains temperature-apparent
The matched curve of viscosity relation and equation y=ax thereof6+bx5+cx4+dx3+ex2+ fx+g, wherein y is apparent viscosity, mPas；x
It is test temperature-softening point temperature, DEG C；A, b, c, d, e, f and g are constants, wherein goodness of fit R2More than 0.98.
A kind of method testing coal tar pitch rheological characteristic the most according to claim 1 it is characterized in that utilizing temperature-apparent
The fit curve equation formula of viscosity relation calculates the coal tar pitch apparent viscosity of arbitrary temp point in the range of measurement.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108627425A (en) * | 2017-03-25 | 2018-10-09 | 北京世通科创技术有限公司 | Temperature compensation parameter generation method and its system and device |
| CN114609932A (en) * | 2022-05-10 | 2022-06-10 | 北京橡鹭科技有限公司 | Material delivery control method, device, storage medium and program product |
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| CN101812235A (en) * | 2010-04-23 | 2010-08-25 | 中南大学 | Method for improving rheological property of coal pitch and increasing coking value of coal pitch and modifier thereof |
| CN101985526A (en) * | 2010-10-21 | 2011-03-16 | 武汉科技大学 | Composite modified asphalt for high-grade road and preparation method thereof |
| CN102653631A (en) * | 2012-04-16 | 2012-09-05 | 交通运输部公路科学研究所 | Mixed asphalt for pavements and preparation method for mixed asphalt |
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Patent Citations (3)
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| CN101812235A (en) * | 2010-04-23 | 2010-08-25 | 中南大学 | Method for improving rheological property of coal pitch and increasing coking value of coal pitch and modifier thereof |
| CN101985526A (en) * | 2010-10-21 | 2011-03-16 | 武汉科技大学 | Composite modified asphalt for high-grade road and preparation method thereof |
| CN102653631A (en) * | 2012-04-16 | 2012-09-05 | 交通运输部公路科学研究所 | Mixed asphalt for pavements and preparation method for mixed asphalt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108627425A (en) * | 2017-03-25 | 2018-10-09 | 北京世通科创技术有限公司 | Temperature compensation parameter generation method and its system and device |
| CN114609932A (en) * | 2022-05-10 | 2022-06-10 | 北京橡鹭科技有限公司 | Material delivery control method, device, storage medium and program product |
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Application publication date: 20161116 |