CN106404602A - Method used for measuring polystyrene platform modulus - Google Patents
Method used for measuring polystyrene platform modulus Download PDFInfo
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- CN106404602A CN106404602A CN201610898205.5A CN201610898205A CN106404602A CN 106404602 A CN106404602 A CN 106404602A CN 201610898205 A CN201610898205 A CN 201610898205A CN 106404602 A CN106404602 A CN 106404602A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
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Abstract
The invention discloses a method used for measuring polystyrene platform modulus. According to the method, cooling scanning curve of a high polymer under melting conditions is measured so as to obtain the relationship of changing of phase angle and complex modulus with the temperature, a phase angle-complex modulus curve is obtained, and the lowest point of the phase angle-complex modulus curve is the material platform modulus. Material platform modulus can be obtained under relatively less workload via the method, a problem of the prior art that conventional methods are complex is solved, and the method possesses significant importance on study of the relative molecular weight and molecular structures of materials.
Description
The present invention is a kind of divisional application of parent application " measuring method of high polymer plateau modulus ", and parent application number is
2013105222494, parent application day is on October 29th, 2013.
Technical field
The invention belongs to the method for test high polymer plateau modulus, more particularly, it is related in certain linear-viscoelastic
Under the conditions of, by measuring polymer melt composite modulus G in temperature-fall period*With the situation of change of phase angle δ, and then obtain it
Phase angle δ is to composite modulus G*Change curve, thus obtaining the plateau modulus G of polymerN.
Background technology
With the continuous development of material science, macromolecular material is widely used, either in daily life
Or in the high-grade, precision and advanced technical field such as space flight and aviation, macromolecular material is all indispensable, the processing of macromolecule material product
It is applied to significant with molding, the research of therefore macromolecule melt flow behavior is processed most important to it.
Rheology test is by applying certain flow field to fluids such as polymer, and then it is dirty in specific flow field to measure it
Become the characterizing method of response, the flow behavior for material in the structural information understanding in the fluid such as polymer and the course of processing and
Its control is significant.As can be obtained the vGP figure of polymer fluid by rheometer test, and then analysis draws polymer
Relative molecular mass size and its distribution information.VGP figure is typically carried out to polymer fluid in the range of linear-viscoelastic
Frequency scanning, takes its phase angle δ to corresponding composite modulus G*Map and obtain, vGP in figure contains much with regard to tested
The information of the molecular structure aspect of measurement.In linear polymer, the typical characteristic of vGP figure is as composite modulus G*From little to
Greatly, phase angle δ is gradually reduced, and is being gradually increased after a minimum, this vGP in figure phase angle minimum δminInstitute
Corresponding composite modulus G*It is equal to the plateau modulus G of this polymer fluidN.Therefore, in order to obtain enough composite modulus
Numerical range, to obtain phase angle minimum δmin, typically need to first measure the frequency scanning curve under different temperatures, by when
The extension of experiment test frequency range is realized in temperature superposition, by when temperature be superimposed the principal curve obtaining and obtain sample than more complete vGP
Figure, and then obtain the plateau modulus G of sampleN, thus bring many operational inconvenience.
Content of the invention
The technical purpose of the present invention is to overcome the deficiencies in the prior art, proposes measurement polymerization under the conditions of a kind of dynamic rheological property
The short-cut method of the plateau modulus of logistics body, specifically within the scope of certain temperature, controls certain frequency and the stress (or should
Become), the dynamic rheological property curve in temperature-fall period of linear-viscoelastic scope build-in test, and then carried out based on the data being obtained
Further process, draws vGP figure, draws this in figure phase angle minimum δminCorresponding composite modulus G*, this G*Value is equal to
The plateau modulus G of this polymer fluidN, thus easily complete the mensure of material platform modulus it is no longer necessary to measure not equality of temperature
Frequency scanning curve under degree.
The technical purpose of the present invention is achieved by following technical proposals：
A kind of measuring method of high polymer plateau modulus, high polymer to be measured is heated on melt temperature, realizes heat flat
After weighing apparatus, control shear stress and frequency to be fixed value, once lowered the temperature to test dynamic rheological property curve in linear viscoelastic region,
With phase angle, corresponding composite modulus are mapped, the corresponding composite modulus of selected phase angle minimum, as high polymer to be measured
Plateau modulus.
In above-mentioned measuring method, control flow graph shear stress is 1000Pa, and frequency is 1Hz, and cooling is interval to be 200 DEG C
To 80 DEG C, rate of temperature fall is 4 DEG C/below min, preferably 2 DEG C/below min, 0.5 1 DEG C/min.
, in the application of test polystyrene plateau modulus, error is within 2% for measuring method described above.
The present invention provides a kind of technology for determining high polymer fluid plateau modulus during rheological behavior, with
Solve the problems, such as prior art relatively complicated it is not necessary to frequency sweep experiment at different temperatures, provided using the present invention
The plateau modulus method of testing of the fluids such as high polymer, can determine that it is corresponding in the rheological behavior of one group of temperature-fall period
Plateau modulus.I.e. by the cooling scanning curve under the conditions of measurement high polymer molten, obtain phase angle and complex modulus with temperature
Variation relation, and then obtain the curve to complex modulus for the phase angle, the minimum point of curve is the plateau modulus of material.Pass through
Using technology provided by the present invention, less workload is can use to obtain the plateau modulus of material, relatively dividing to research material
Son amount and molecular structure are significant.
Brief description
Fig. 1 is the vGP figure of the temperature-fall period of comparative example of the present invention, wherein is 200 DEG C, zero is 180 DEG C, △ is 160 DEG C,
For frequency scanning the vGP figure obtaining under the conditions of 140 DEG C.
Fig. 2 is the vGP figure of the temperature-fall period of the embodiment of the present invention 1,2 DEG C/min of its rate of temperature fall.
Fig. 3 is the vGP figure of the temperature-fall period of the embodiment of the present invention 2,4 DEG C/min of its rate of temperature fall.
Specific embodiment
Further illustrate technical scheme with reference to specific embodiment, the 666D producing with Yanshan Petrochemical company
As a example type polystyrene raw material, the dynamic mechanical determining instrument of employing is Reologica Instruments AB company
Stress Tech rotational rheometer, basic parameter is as follows：Moment of torsion resolution is 0.001micro Nm, position resolution
0.1micro rad, moment of torsion 0.0001 100mNm, frequency 0.00001 100Hz, make further specifically to the present invention
Bright：
Comparative example：Weigh 0.25g polystyrene, first measure under different temperatures according to 200 DEG C, 180 DEG C, 160 DEG C, 140 DEG C
Frequency scanning curve, by when temperature superposition realize the extension of experiment test frequency range, by when temperature be superimposed the principal curve obtaining
Obtain sample to scheme than more complete vGP, the plateau modulus obtaining are 107000Pa.
Embodiment 1：Weigh 0.25g polystyrene, feed on flow graph under the conditions of 200 DEG C, parallel from P20ETC
Plate adnexa, polystyrene is added on parallel-plate, and heating adjustment parallel-plate spacing after 3min melting after it is 0.8mm, thermal balance
5min, control flow graph shear stress is 1000Pa, and frequency is 1Hz, does concussion scanning in its linear viscoelastic region, and cooling interval is
200 DEG C to 80 DEG C, rate of temperature fall is 2 DEG C/min.By the phase place angular dimensions in the data obtaining and corresponding complex modulus parameter
Mapping, obtains the vGP figure of its temperature-fall period, and the corresponding complex modulus of in figure minimum point are its plateau modulus, the platform obtaining
Modulus is 107100Pa, such as Fig. 2, and the plateau modulus that original method obtains are 107000Pa, and error is 0.1%.
Embodiment 2：Weigh 0.25g polystyrene, feed on flow graph under the conditions of 200 DEG C, parallel from P20ETC
Plate adnexa, polystyrene is added on parallel-plate, and heating adjustment parallel-plate spacing after 3min melting after it is 0.8mm, thermal balance
5min, control flow graph shear stress is 1000Pa, and frequency is 1Hz, does concussion scanning in its linear viscoelastic region, and cooling interval is
200 DEG C to 80 DEG C, rate of temperature fall is 4 DEG C/min.By the phase place angular dimensions in the data obtaining and corresponding complex modulus parameter
Mapping, obtains the vGP figure of its temperature-fall period, and the corresponding complex modulus of in figure minimum point are its plateau modulus, the platform obtaining
Modulus is 109000Pa, such as Fig. 3, and the plateau modulus that original method obtains are 107000Pa, and error is 1.8%.
Above the present invention is done with exemplary description it should illustrate, in the situation of the core without departing from the present invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent of creative work equal
Fall into protection scope of the present invention.
Claims (3)
1. a kind of method of test polystyrene plateau modulus it is characterised in that be heated to molten by high polymer polystyrene to be measured
Melt on temperature, after realizing thermal balance, control shear stress and frequency to be fixed value, once lowered the temperature in linear viscoelastic region
To test dynamic rheological property curve, with phase angle, corresponding composite modulus are mapped, the corresponding compound die of selected phase angle minimum
Amount, as the plateau modulus of high polymer polystyrene to be measured, control shear stress is 1000Pa, and frequency is 1Hz, and cooling interval is
200 DEG C to 80 DEG C, rate of temperature fall is 4 DEG C/below min.
2. a kind of method of test polystyrene plateau modulus according to claim 1 is it is characterised in that described cooling is fast
Rate is 2 DEG C/below min.
3. a kind of method of test polystyrene plateau modulus according to claim 1 is it is characterised in that described cooling is fast
Rate is 0.5 1 DEG C/min.
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| CN201610898205.5A CN106404602A (en) | 2013-10-29 | 2013-10-29 | Method used for measuring polystyrene platform modulus |
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| CN201610898205.5A CN106404602A (en) | 2013-10-29 | 2013-10-29 | Method used for measuring polystyrene platform modulus |
| CN201310522249.4A CN104568659B (en) | 2013-10-29 | 2013-10-29 | A kind of measuring method of high polymer plateau modulus |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TW200936619A (en) * | 2007-11-15 | 2009-09-01 | Univation Tech Llc | Polymerization catalysts, methods of making, methods of using, and polyolefin products made therefrom |
| CN101458246B (en) * | 2009-01-08 | 2012-01-11 | 浙江大学 | Method for measuring molecular weight distribution of linear polymer |
| CN105352848B (en) * | 2013-07-03 | 2017-11-28 | 天津大学 | High polymer dynamic rheological property condition lower wall slides the method for testing of length it is determined that application in the true rheological curve of high polymer fluid |
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Non-Patent Citations (3)
| Title |
|---|
| 周持兴 等: "《聚合物流变实验与应用》", 30 April 2003, 上海交通大学出版社 * |
| 杨鸣波 等: "流延聚丙烯流变性能的研究", 《2002年中国工程塑料加工应用技术研讨会论文集》 * |
| 苏家齐: "《塑料工业辞典》", 31 December 1989, 化学工业出版社 * |
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| CN104568659A (en) | 2015-04-29 |
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Application publication date: 20170215 |