CN105547926B - A kind of method for measuring miberal powder surface free energy - Google Patents
A kind of method for measuring miberal powder surface free energy Download PDFInfo
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Abstract
The present invention relates to a kind of method for measuring miberal powder surface free energy.This method selects pentane liquid to calibrate the effective radius R of capillary firsteff, then select other three kinds of different liquid to carry out immersion test, the regression parameter drawn according to the relevant parameter of three kinds of selected liquid and immersion test, according to formula h with miberal powder respectively2/ t=(γlReffCos θ)/2 η, the contact angle of miberal powder and every kind of liquid is calculated again.WithFor abscissa, withFor ordinate, establish the linear relationship of miberal powder and three kinds of liquid, calculate intercept and slope, intercept square with slope square the sum of be the miberal powder surface free energy.The present invention solves in conventional method that used surface energy of liquid is as far as possible minimum when measuring effective radius, to ensure dipping powder more i.e. contact angle values closer to 0, but surface energy of liquid is lower, it impregnates the problem of height is faster with the time rate of climb, and data recording errors are larger.Error using this method measure miberal powder surface free energy is smaller.
Description
Technical field
The present invention relates to surface chemistry domain, more particularly to a kind of method for measuring miberal powder surface free energy.
Background technology
Surface free energy refer to keep temperature, pressure and composition it is constant under conditions of, every increase (or reduce) unit table
During area, the value added (or reduced value) of Gibbs free energy is known as surface Gibbs free energy, referred to as surface free energy or
Surface energy.The analysis pitch and the size of miberal powder interface adhesiveness that surface free energy can quantify, same bitumen is in different type
Miberal powder in the case of, the adhesion property of pitch and miberal powder depends primarily upon the surface free energy of miberal powder.
However, during measuring surface free energy using conventional method, used liquid table when measuring effective radius
Face can be as low as possible, and to ensure dipping miberal powder more i.e. contact angle values closer to 0, but surface energy of liquid is lower, it is soaked
Stain height is faster with the time rate of climb, and error is larger.
The content of the invention
In view of this, it is an object of the invention to provide a kind of method for measuring miberal powder surface free energy, using this method
The error for measuring surface free energy is smaller.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of method for measuring miberal powder surface free energy, it is concretely comprised the following steps：
A. 0.5 ± 0.02g of miberal powder to be measured no less than 2 parts is weighed；
B. the glass bottom of the tube identical with the miberal powder number to be measured that step A is weighed is sealed with one layer of filter paper；
C. every part of miberal powder to be measured weighed up is slowly put into every glass tube by dropper, and uniformly shakes glass tube；
D. the pentane liquid of 0.9-1.1cm height is added in the glass dish on iron stand；
E. glass tube is put into glass dish and be fixed on iron stand, it is immersed liquid 4-6mm described in step D；
F. record and required time during 1-5cm is risen in the miberal powder column that liquid is immersed in glass tube, record 6 groups of numbers
According to by lifting height to carry out data record in a manner of arithmetic progression in uphill process, R is calculated according to equation beloweff, and calculate
The R of gained parallel laboratory test dataeffAverage value；
G. other three kinds of different liquid is selected again respectively, immersion test described in repeat step A to step F,
The cos θ of miberal powder and three kinds of liquid are calculated according to equation below respectively：
WithFor abscissa, withFor ordinate, the linear relationship of miberal powder and three kinds of liquid is established,
Calculate intercept and slope, intercept square with slope square the sum of be the miberal powder surface free energy.
In experimentation, weigh more than a miberal powder to be measured and tested, be easy for doing parallel test, reduce the mistake of experiment
Difference.Glass bottom of the tube is sealed using filter paper, is to prevent that leakage influence experimental result causes experimental error under miberal powder, while in order to protect
Hold the uniformity of experiment, all Feng Youyi layers of filter paper of glass tube of every group of experiment.In addition, that is mentioned in step B is wrapped up in one layer of filter paper
Firmly glass bottom of the tube, and filter paper cannot be too big, prevents from influencing reading.Liquid is recorded in step F to immerse in the miberal powder column in glass tube
Rise to required time during 1-5cm, record 6 groups of data, in uphill process according to lifting height arithmetic progression mode into
Row data record, refers to rise to respectively in the miberal powder column that liquid is immersed in glass tube needed for the level altitude in the range of 1-5cm
The time wanted, such as 1cm, 1.5cm, 2cm, 2.5cm, 3cm, 3.5cm ..., recorded in the range of 1-5cm 6 groups of lifting heights with it is required
The time corresponding data wanted.Herein, 6-8 group data can also be recorded.In step D, in addition to pentane liquid, also may be used
To carry out this experiment close to 0 liquid with other contact angles between miberal powder.The R mentioned in step GeffIt is capillary
Effective radius, η be liquid viscosity, contact angles of the θ between liquid and miberal powder, γlFor the surface free energy of liquid, h is liquid
Body lifting height, t are dip time,For the polar component of liquid,For the dispersive component of liquid.In entirely experiment process
In, glass tube is in vertical state all the time, prevents from rising the uneven influence reading of liquid level.So need iron stand to consolidate, and cannot
Iron stand is collided in liquid level uphill process, in case influencing the change of climbing speed causes the error entirely tested.
Further, temperature is 24-26 DEG C in experimentation.Because liquid tension force at different temperatures and viscosity can all have
Changed, so controlling room temperature in certain temperature range.
Further, it is assay balance that miberal powder instrument to be measured is weighed described in step A.So operation is conducive to reduce and misses
Difference.
Further, it is specifically to cling filter in bottom side with double faced adhesive tape to seal glass bottom of the tube with filter paper described in step B
Paper.
Further, the degree shaken described in step C is concussion untill the miberal powder column in glass tube is no longer decreased obviously.
Further, during earthquake glass pipe outer wall is tapped with glass bar.So operation is to further make to treat
It is closely knit in glass tube to survey miberal powder.
Further, a diameter of 7.2-8cm of glass dish described in step D, is highly 1.5cm.
Further, it is to put glass tube into glass dish center to put glass tube in glass dish into described in step E.So
Operation is conducive to reduce error.
The method have the benefit that：
Error using this method measure miberal powder surface free energy is smaller.
Brief description of the drawings
Fig. 1 is the Experimental equipment of the present invention, wherein 1 be iron stand, 2 be glass dish, 3 be pentane liquid or other three
The different liquid of kind, 4 be miberal powder to be measured, and 5 be glass tube；
Fig. 2 is the linear relationship chart of embodiment 1；
Fig. 3 is the linear relationship chart of embodiment 2；
Fig. 4 is the linear relationship chart of embodiment 3.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, the embodiment of the present invention is carried out below detailed
Thin description.
Embodiment 1
The measure of miberal powder surface free energy is carried out under the conditions of 25 DEG C, it is concretely comprised the following steps：
A. two parts of the limestone mineral powder 0.52g that specification is 300 mesh is weighed with assay balance；
B. two glass bottom of the tube are sealed with one layer of filter paper respectively, and filter paper is clung in bottom side with double faced adhesive tape；
C. the limestone mineral powder weighed up is slowly put into glass tube by dropper, and uniformly shakes glass tube, concussion
During tap the concussion of glass pipe outer wall until miberal powder is highly no longer decreased obviously with glass bar untill；
D. in the glass dish on iron stand add 1cm height pentane liquid, the glass dish it is a diameter of
7.5cm, is highly 1.5cm；
E. put glass tube into glass dish center and be fixed on iron stand, it is immersed pentane liquid 5mm；
F. record pentane liquid infiltration to glass tube in limestone mineral powder rise to respectively 1cm, 1.5cm, 2cm,
2.5cm, 3cm, 3.5cm required time, 6 times of record are respectively：7.38s、15.38s、26.11s、37.92s、
51.63s, 67.58s, by data processing, obtain h2The slope of the linear equation of/t is 0.2288；Experiment process more than repeating,
The data of one group of pentane liquid and limestone mineral powder are measured again, and 6 times of record are respectively：7.36s、15.99s、
26.15s, 38.05s, 52.08s, 69.18s, after data processing, obtain h2The slope of the linear equation of/t is 0.2244；According to
Two obtained slope numerical value, are calculated the effective radius value of limestone mineral powder.The wherein surface free energy of pentane liquid
γlFor 15.49mJm-2, viscosities il 0.224mNm-2·s-1.The average value for trying to achieve effective radius is Reff=(0.6617+
0.649)/2=0.6554 μm；
G. dipping experiment described in repeat step A to F, distilled water, toluene and first are substituted for by steeping liq pentane successively
Three kinds of liquid of acid amides, that is, obtain 6 h2The value of/t.Table 1 is 6 h of three kinds of liquid2/ t numerical value；Table 2 is the parameter of three kinds of liquid
Component.
Table 1
| Liquid | Distilled water | Toluene | Formamide |
| h2/t(1) | 0.122 | 0.1482 | 0.0428 |
| h2/t(2) | 0.1226 | 0.1476 | 0.0422 |
Table 2
By the data drawn, with reference to the surface free energy parameter of steeping liq, every kind of steeping liq and stone are tried to achieve respectively
The contact angle values of limestone miberal powder.It is as follows：
Distilled water：θ (1)=arcos (2k η/γ 1Reff)=arccos (2*0.122*0.89*100/72.8/0.6554)
=62.9 °
θ (2)=arcos (2k η/γ 1Reff)=arccos (2*0.1226*0.89*100/72.8/0.6554)=
62.8°
Contact angle average θ=(θ (1)+θ (2))/2=(62.9 °+62.8 °)/2=62.85 °
Toluene：θ (1)=arcos (2k η/γ 1Reff)=arccos (2*0.1482*0.56*100/27.7/0.6554)
=23.9 °
θ (2)=arcos (2k η/γ 1Reff)=arccos (2*0.1476*0.56*100/27.7/0.6554)=
24.4°
Contact angle average θ=(θ (1)+θ (2))/2=(23.9 °+24.4 °)/2=24.15 °
Formamide：θ (1)=arcos (2k η/γ 1Reff)=arccos (2*0.0428*3.343*100/58/0.6554)
=41.2 °
θ (2)=arcos (2k η/γ 1Reff)=arccos (2*0.0422*3.343*100/58/0.6554)=42.1 °
Contact angle average θ=(θ (1)+θ (2))/2=(41.2 °+42.1 °)/2=41.65 °
By the contact angle values of the limestone mineral powder that draws under every kind of steeping liq, with reference to the surface energy parameter of steeping liq
Component, according to formulaEstablish the graph of a relation of y and x, slope square by survey interface
Polar component, intercept square by survey interface dispersive component, the sum of polar component and dispersive component are to survey the table of miberal powder
Face free energy.Result of calculation is as follows：
Distilled water：
Toluene：
Formamide：
Three groups of coordinate values more than, establish the graph of a relation of y and x, as shown in Figure 2.Table 3 is the final experiment number calculated
According to.
Table 3
| Slope | Intercept | Dispersive component/mJm-2 | Polar component/mJm-2 | Surface free energy/mJm-2 |
| 4.0582 | 5.1205 | 26.2195 | 16.4690 | 42.6885 |
Embodiment 2
The measure of miberal powder surface free energy is carried out under the conditions of 24 DEG C, it is concretely comprised the following steps：
A. two parts of the basalt miberal powder 0.5g that specification is 500 mesh is weighed with assay balance；
B. two glass bottom of the tube are sealed with one layer of filter paper respectively, and filter paper is clung in bottom side with double faced adhesive tape；
C. the basalt miberal powder weighed up is slowly put into glass tube by dropper, and uniformly shakes glass tube, concussion
During tap the concussion of glass pipe outer wall until miberal powder is highly no longer decreased obviously with glass bar untill；
D. in the glass dish on iron stand add 0.9cm height pentane liquid, the glass dish it is a diameter of
7.2cm, is highly 1.5cm；
E. put glass tube into glass dish center and be fixed on iron stand, it is immersed pentane liquid 6mm；
F. record pentane liquid infiltration to glass tube in basalt miberal powder rise to respectively 1cm, 1.5cm, 2cm,
2.5cm, 3cm, 3.5cm required time, 6 times of record are respectively：38.28s、42.37s、46.86s、52.06s、
59.27s, 67.75s, by data processing, obtain h2The slope of the linear equation of/t is 0.0517；Experiment process more than repeating,
The data of one group of pentane liquid and basalt miberal powder are measured again, and 6 times of record are respectively：37.93s、42.01s、
47.61s, 51.93s, 58.49s, 66.90s, after data processing, obtain h2The slope of the linear equation of/t is 0.0519；According to
Two obtained slope numerical value, are calculated the effective radius value of basalt miberal powder.The wherein surface free energy of pentane liquid
γlFor 15.49mJm-2, viscosities il 0.224mNm-2·s-1.The average value for trying to achieve effective radius is Reff=(0.1495+
0.1501)/2=0.0.1498 μm；
G. dipping experiment described in repeat step A to F, distilled water, toluene and first are substituted for by steeping liq pentane successively
Three kinds of liquid of acid amides, that is, obtain 6 h2The value of/t.Table 4 is 6 h of three kinds of liquid2/ t numerical value；The parametric component of three kinds of liquid with
Table 2 is identical.
Table 4
| Liquid | Distilled water | Toluene | Formamide |
| h2/t(1) | 0.0345 | 0.0318 | 0.0113 |
| h2/t(2) | 0.0345 | 0.0323 | 0.0114 |
By the data drawn, with reference to the surface free energy parameter of related steeping liq, every kind of steeping liq is tried to achieve respectively
With the contact angle values of basalt miberal powder.It is as follows：
Distilled water：θ (1)=arcos (2k η/γ 1Reff)=55.7 °, θ (2)=arcos (2k η/γ 1Reff)=
55.7°
Contact angle average θ=(θ (1)+θ (2))/2=55.7 °
Toluene：θ (1)=arcos (2k η/γ 1Reff)=30.9 °, θ (2)=arcos (2k η/γ 1Reff)=29.3 °
Contact angle average θ=(θ (1)+θ (2))/2=30.1 °
Formamide：θ (1)=arcos (2k η/γ 1Reff)=29.6 °, θ (2)=arcos (2k η/γ 1Reff)=
28.7°
Contact angle average θ=(θ (1)+θ (2))/2=29.1 °
By the contact angle values of the basalt miberal powder that draws under every kind of steeping liq, with reference to the surface energy parameter of steeping liq
Component, according to formulaThe graph of a relation of y and x are established, slope square is is surveyed interface
Polar component, intercept square by survey interface dispersive component, the sum of polar component and dispersive component be survey miberal powder
Surface free energy.Result of calculation is as follows：
Distilled water：
Toluene：
Formamide：
Three groups of coordinate values more than, establish the graph of a relation of y and x, as shown in Figure 3.Table 5 is the final experiment number calculated
According to.
Table 5
| Slope | Intercept | Dispersive component/mJm-2 | Polar component/mJm-2 | Surface free energy/mJm-2 |
| 4.7402 | 5.078 | 25.7861 | 24.4695 | 48.2556 |
Embodiment 3
The measure of miberal powder surface free energy is carried out under the conditions of 26 DEG C, it is concretely comprised the following steps：
A. two parts of the pick base miberal powder 0.48g that specification is 400 mesh is weighed using assay balance；
B. two glass bottom of the tube are sealed with one layer of filter paper, and filter paper is clung in bottom side with double faced adhesive tape；
C. the pick base miberal powder weighed up is slowly put into glass tube by dropper, and uniformly shakes glass tube, the mistake of concussion
The concussion of glass pipe outer wall is tapped untill miberal powder height is no longer decreased obviously with glass bar in journey；
D. in the glass dish on iron stand add 1.1cm height pentane liquid, the glass dish it is a diameter of
8cm, is highly 1.5cm；
E. put glass tube into glass dish center and be fixed on iron stand, it is immersed pentane liquid 4mm；
F. record pentane liquid infiltration to glass tube in pick base miberal powder rise to respectively 1cm, 1.5cm, 2cm,
2.5cm, 3cm, 3.5cm required time, 6 times of record are respectively：27.95s、37.65s、45.30s、53.11s、
57.02s, 64.12s, by data processing, obtain h2The slope of the linear equation of/t is 0.0535；Experiment process more than repeating,
One group of pentane liquid is measured again with digging the data of base miberal powder, 6 times of record is respectively：27.16s、36.18s、
45.18s, 52.17s, 58.14s, 64.98s, after data processing, obtain h2The slope of the linear equation of/t is 0.0536；According to
Two obtained slope numerical value, are calculated the effective radius value of pick base miberal powder.The wherein surface free energy γ of pentane liquidl
For 15.49mJm-2, viscosities il 0.224mNm-2·s-1.The average value for trying to achieve effective radius is Reff=(0.1547+
0.1550)/2=0.1549 μm；
G. dipping experiment described in repeat step A to F, distilled water, toluene and first are substituted for by steeping liq pentane successively
Three kinds of liquid of acid amides, that is, obtain 6 h2The value of/t.Table 6 is 6 h of three kinds of liquid2/ t numerical value；The parametric component of three kinds of liquid with
Table 2 is identical.
Table 6
| Liquid | Distilled water | Toluene | Formamide |
| h2/t(1) | 0.0274 | 0.0326 | 0.0101 |
| h2/t(2) | 0.0267 | 0.0331 | 0.0101 |
By the data drawn, with reference to the surface free energy energy parameter of related steeping liq, every kind of maceration extract is tried to achieve respectively
The contact angle values of body and pick base miberal powder.It is as follows：
Distilled water：θ (1)=arcos (2k η/γ 1Reff)=64.4 °, θ (2)=arcos (2k η/γ 1Reff)=
65.1°
Contact angle average θ=(θ (1)+θ (2))/2=64.7 °
Toluene：θ (1)=arcos (2k η/γ 1Reff)=31.7 °, θ (2)=arcos (2k η/γ 1Reff)=30.2 °
Contact angle average θ=(θ (1)+θ (2))/2=30.94 °
Formamide：θ (1)=arcos (2k η/γ 1Reff)=41.26 °, θ (2)=arcos (2k η/γ 1Reff)=
41.26°
Contact angle average θ=(θ (1)+θ (2))/2=41.26 °
By the contact angle values of the pick base miberal powder that draws under every kind of steeping liq, with reference to the surface energy parameter point of steeping liq
Amount, according to formulaEstablish the graph of a relation of y and x, slope square by survey interface pole
Property component, intercept square by survey interface dispersive component, the sum of polar component and dispersive component are to survey the surface of miberal powder
Free energy.Result of calculation is as follows：
Distilled water：
Toluene：
Formamide：
Three groups of coordinate values more than, establish the graph of a relation of y and x, as shown in Figure 4.Table 7 is that the correlation calculated is final real
Test data.
Table 7
| Slope | Intercept | Dispersive component/mJm-2 | Polar component/mJm-2 | Surface free energy/mJm-2 |
| 4.0624 | 5.0332 | 25.3331 | 16.5031 | 41.8362 |
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, this area it is general
Lead to it will be appreciated by the skilled person that can be to technical solution technical scheme is modified or replaced equivalently, without departing from technical solution of the present invention
Objective and scope, it should all cover among scope of the presently claimed invention.
Claims (8)
- A kind of 1. method for measuring miberal powder surface free energy, it is characterised in that concretely comprise the following steps：A. 0.5 ± 0.02g of miberal powder to be measured no less than 2 parts is weighed；B. the glass bottom of the tube identical with the miberal powder number to be measured that step A is weighed is sealed with one layer of filter paper；C. every part of miberal powder to be measured weighed up is put into every glass tube by dropper, and uniformly shakes glass tube；D. the pentane liquid of 0.9-1.1cm height is added in the glass dish on iron stand；E. glass tube is put into glass dish and be fixed on iron stand, it is immersed liquid 4-6mm described in step D；F. record and required time during 1-5cm is risen in the miberal powder column that liquid is immersed in glass tube, record 6 groups of data, on Data record is carried out in a manner of lifting height is arithmetic progression during rising, R is calculated according to equation beloweff, and it is flat to calculate gained The R of row experimental dataeffAverage value；<mrow> <msub> <mi>R</mi> <mrow> <mi>e</mi> <mi>f</mi> <mi>f</mi> </mrow> </msub> <mo>=</mo> <mfrac> <mrow> <mn>2</mn> <msup> <mi>&eta;h</mi> <mn>2</mn> </msup> </mrow> <msub> <mi>&gamma;</mi> <mi>l</mi> </msub> </mfrac> </mrow>G. other three kinds of different liquid, immersion test described in repeat step A to step F, respectively according to as follows are selected again respectively Formula calculates the cos θ of miberal powder and three kinds of liquid：<mrow> <mi>c</mi> <mi>o</mi> <mi>s</mi> <mi>&theta;</mi> <mo>=</mo> <mfrac> <mrow> <mn>2</mn> <msup> <mi>&eta;h</mi> <mn>2</mn> </msup> </mrow> <mrow> <msub> <mi>R</mi> <mrow> <mi>e</mi> <mi>f</mi> <mi>f</mi> </mrow> </msub> <msub> <mi>&gamma;</mi> <mi>l</mi> </msub> <mi>t</mi> </mrow> </mfrac> </mrow>WithFor abscissa, withFor ordinate, the linear relationship of miberal powder and three kinds of liquid is established, is calculated Intercept and slope, intercept square with slope square the sum of be the miberal powder surface free energy；Wherein, ReffIt is the effective radius of capillary, η is the viscosity of liquid, contact angles of the θ between liquid and miberal powder, γlFor liquid The surface free energy of body, h are liquid lifting height, and t is dip time,For the polar component of liquid,For the dispersion of liquid Component.
- 2. according to the method described in claim 1, it is characterized in that：Temperature is 24-26 DEG C in experimentation.
- 3. according to the method described in claim 1, it is characterized in that：Miberal powder instrument to be measured is weighed described in step A as analysis Balance.
- 4. according to the method described in claim 1, it is characterized in that：It is specific that with filter paper glass bottom of the tube is sealed described in step B To cling filter paper in bottom side with double faced adhesive tape.
- 5. according to the method described in claim 1, it is characterized in that：The degree shaken described in step C is in concussion to glass tube Miberal powder column be no longer decreased obviously untill.
- 6. according to the method described in claim 5, it is characterized in that：Tapped during earthquake with glass bar outside glass tube Wall.
- 7. according to the method described in claim 1, it is characterized in that：A diameter of 7.2-8cm of glass dish described in step D, height For 1.5cm.
- 8. according to the method described in claim 1, it is characterized in that：It is by glass to put glass tube in glass dish into described in step E Glass pipe puts glass dish center into.
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