CN104568659B - A kind of measuring method of high polymer plateau modulus - Google Patents
A kind of measuring method of high polymer plateau modulus Download PDFInfo
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- CN104568659B CN104568659B CN201310522249.4A CN201310522249A CN104568659B CN 104568659 B CN104568659 B CN 104568659B CN 201310522249 A CN201310522249 A CN 201310522249A CN 104568659 B CN104568659 B CN 104568659B
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- 229920000642 polymer Polymers 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 description 8
- 239000004793 Polystyrene Substances 0.000 description 7
- 229920002223 polystyrene Polymers 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000009514 concussion Effects 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing Methods 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
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
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- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
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Abstract
The invention discloses a kind of measuring method of high polymer plateau modulus, by the cooling scanning curve under the conditions of measurement high polymer molten, phase angle and complex modulus variation with temperature relation are obtained, and then obtains curve of the phase angle to complex modulus, the minimum point of curve is the plateau modulus of material.By the present invention in that using technology provided by the present invention, the plateau modulus of material can be obtained with less workload, it is to solve the problems, such as that prior art is relatively complicated, significant to the relative molecular weight and molecular structure of research material.
Description
Technical field
The invention belongs to the method for testing high polymer plateau modulus, more particularly, 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 which is obtained
Phase angle δ is to composite modulus G*Change curve, so as to obtain 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, therefore the research of macromolecule melt flow behavior processes most important to which.
Rheology test is that, by applying certain flow field to fluids such as polymer, and then it is dirty in specific flow field to determine which
Become the characterizing method of response, for the flow behavior of material in the structural information and the course of processing understood in the fluid such as polymer and
Its control is significant.The vGP figures of polymer fluid such as can be obtained by rheometer test, and then analysis draws polymer
Relative molecular mass size and its distribution information.VGP figures are 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, contain in vGP figures many with regard to tested
Information in terms of the molecular structure of measurement.In linear polymer, vGP figures are typically characterised by with composite modulus G*From it is little to
Greatly, phase angle δ is gradually reduced, and is gradually increasing after a minimum, phase angle minimum δ in the vGP figuresminInstitute
Corresponding composite modulus G*I.e. equal to the plateau modulus G of the polymer fluidN.Therefore, in order to obtaining 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 that obtains and obtain sample than more complete vGP
Figure, and then obtain the plateau modulus G of sampleN, thus bring many operational inconvenience.
The 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, controlling certain frequency and 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 for being obtained
It is further to process, vGP figures are drawn, phase angle minimum δ in the figure is drawnminCorresponding composite modulus G*, the G*Value is equal to
The plateau modulus G of the polymer fluidN, thus easily complete the measure 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 that heat is flat
After weighing apparatus, it is fixed value to control shear stress and frequency, is once lowered the temperature in linear viscoelastic region to test dynamic rheological property curve,
Corresponding composite modulus are mapped with phase angle, the corresponding composite modulus of selected phase angle minimum, as high polymer to be measured
Plateau modulus.
In above-mentioned measuring method, it is 1000Pa to control flow graph shear stress, and frequency is 1Hz, and it is 200 DEG C that cooling is interval
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.
Application of the measuring method described above in test polystyrene plateau modulus, error is within 2%.
The present invention provides a kind of technology for determining high polymer fluid plateau modulus during rheological behavior, with
Solve the problems, such as that prior art is 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 which 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 (are combined
Modulus) variation with temperature relation, and then curve of the phase angle to composite modulus is obtained, the minimum point of curve is the flat of material
Platform modulus.By using technology provided by the present invention, the plateau modulus of material can be obtained with less workload, to studying material
The relative molecular weight and molecular structure of material is significant.
Description of the drawings
Fig. 1 is the vGP figures 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,
▽ is that the vGP figures for obtaining are frequency scanned under the conditions of 140 DEG C.
Fig. 2 is that the vGP of the temperature-fall period of the embodiment of the present invention 1 schemes, 2 DEG C/min of its rate of temperature fall.
Fig. 3 is that the vGP of the temperature-fall period of the embodiment of the present invention 2 schemes, 4 DEG C/min of its rate of temperature fall.
Specific embodiment
Technical scheme is further illustrated with reference to specific embodiment, with the 666D that Yanshan Petrochemical company produces
As a example by type polystyrene raw material, the dynamic mechanical determining instrument for adopting is Reologica Instruments AB companies
Stress Tech rotational rheometers, basic parameter are as follows：Moment of torsion resolution be 0.001micro Nm, position resolution
0.1micro rad, 0.0001-100mNm of moment of torsion, 0.00001-100Hz of frequency, make further specifically to the present invention
It is bright：
Comparative example：0.25g polystyrene is weighed, is first measured 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 that obtains
Obtain sample to scheme than more complete vGP, the plateau modulus for obtaining are 107000Pa.
Embodiment 1：0.25g polystyrene is weighed, is fed on flow graph under the conditions of 200 DEG C, it is parallel from P20ETC
Plate adnexa, polystyrene is added on parallel-plate, adjusts parallel-plate spacing for 0.8mm, thermal balance after which heats 3min meltings
5min, it is 1000Pa to control flow graph shear stress, 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 for obtaining and corresponding composite modulus parameter
Mapping, obtains the vGP figures of its temperature-fall period, and in figure, the corresponding composite modulus of minimum point are its plateau modulus, the platform for obtaining
Modulus is 107100Pa, such as Fig. 2, and the plateau modulus that original method is obtained are 107000Pa, and error is 0.1%.
Embodiment 2：0.25g polystyrene is weighed, is fed on flow graph under the conditions of 200 DEG C, it is parallel from P20ETC
Plate adnexa, polystyrene is added on parallel-plate, adjusts parallel-plate spacing for 0.8mm, thermal balance after which heats 3min meltings
5min, it is 1000Pa to control flow graph shear stress, 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 for obtaining and corresponding composite modulus parameter
Mapping, obtains the vGP figures of its temperature-fall period, and in figure, the corresponding composite modulus of minimum point are its plateau modulus, the platform for obtaining
Modulus is 109000Pa, such as Fig. 3, and the plateau modulus that original method is obtained are 107000Pa, and error is 1.8%.
Exemplary description is done above to the present invention, it should explanation, 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 (4)
1. a kind of measuring method of high polymer plateau modulus, it is characterised in that high polymer to be measured is heated on melt temperature,
After realizing thermal balance, it is fixed value to control shear stress and frequency, is once lowered the temperature to test dynamic in linear viscoelastic region
Corresponding composite modulus are mapped by rheological curve with phase angle, the corresponding composite modulus of selected phase angle minimum, as to be measured
The plateau modulus of high polymer.
2. a kind of measuring method of high polymer plateau modulus according to claim 1, it is characterised in that control shear stress
For 1000Pa, frequency is 1Hz, and it is 200 DEG C to 80 DEG C that cooling is interval, and rate of temperature fall is 4 DEG C/below min.
3. a kind of measuring method of high polymer plateau modulus according to claim 2, it is characterised in that the rate of temperature fall
For 2 DEG C/below min.
4. a kind of measuring method of high polymer plateau modulus according to claim 3, it is characterised in that the rate of temperature fall
For 0.5-1 DEG C/min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310522249.4A CN104568659B (en) | 2013-10-29 | 2013-10-29 | A kind of measuring method of high polymer plateau modulus |
| CN201610898205.5A CN106404602A (en) | 2013-10-29 | 2013-10-29 | Method used for measuring polystyrene platform modulus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310522249.4A CN104568659B (en) | 2013-10-29 | 2013-10-29 | A kind of measuring method of high polymer plateau modulus |
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| CN201610898205.5A Division CN106404602A (en) | 2013-10-29 | 2013-10-29 | Method used for measuring polystyrene platform modulus |
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| CN104568659A CN104568659A (en) | 2015-04-29 |
| CN104568659B true CN104568659B (en) | 2017-04-05 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458246A (en) * | 2009-01-08 | 2009-06-17 | 浙江大学 | Method for measuring molecular weight distribution of linear polymer |
| CN103353433A (en) * | 2013-07-03 | 2013-10-16 | 天津大学 | Method for testing wall slip length of polymer under dynamic rheological conditions |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200936619A (en) * | 2007-11-15 | 2009-09-01 | Univation Tech Llc | Polymerization catalysts, methods of making, methods of using, and polyolefin products made therefrom |
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2013
- 2013-10-29 CN CN201310522249.4A patent/CN104568659B/en active Active
- 2013-10-29 CN CN201610898205.5A patent/CN106404602A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458246A (en) * | 2009-01-08 | 2009-06-17 | 浙江大学 | Method for measuring molecular weight distribution of linear polymer |
| CN103353433A (en) * | 2013-07-03 | 2013-10-16 | 天津大学 | Method for testing wall slip length of polymer under dynamic rheological conditions |
Non-Patent Citations (3)
| Title |
|---|
| 《SBS改性沥青低温粘度的动态剪切流变测试方法》;陈华鑫 等;《同济大学学报（自然科学版）》;20090430;第37卷(第4期);第505-509页 * |
| 《Van Gurp-Palmen-plot:》;Stefan Trinkle et al.;《Rheologica Acta》;20010731;第40卷(第4期);第322-328页 * |
| 《聚合物长支链的流变学表征方法》;娄立娟;《高分子通报》;20091031(第10期);第15-23页 * |
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| CN104568659A (en) | 2015-04-29 |
| CN106404602A (en) | 2017-02-15 |
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