CN104568659A - Measurement method of high-polymer platform modulus - Google Patents
Measurement method of high-polymer platform modulus Download PDFInfo
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- CN104568659A CN104568659A CN201310522249.4A CN201310522249A CN104568659A CN 104568659 A CN104568659 A CN 104568659A CN 201310522249 A CN201310522249 A CN 201310522249A CN 104568659 A CN104568659 A CN 104568659A
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- modulus
- superpolymer
- temperature
- plateau modulus
- measuring method
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- 229920000642 polymer Polymers 0.000 title abstract description 11
- 238000000691 measurement method Methods 0.000 title abstract 4
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 11
- 238000012360 testing method Methods 0.000 claims description 10
- 239000004793 Polystyrene Substances 0.000 claims description 8
- 229920002223 polystyrene Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 3
- 239000012530 fluid Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 4
- 238000010408 sweeping Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000009514 concussion Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000005259 measurement 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
- 239000002994 raw material Substances 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000010998 test method 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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- Analytical Chemistry (AREA)
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention discloses a measurement method of high-polymer platform modulus. The measurement method comprises the following steps: a cooling scanning curve under the condition of high-polymer melt is measured, so that the change relationship of a phase angle and a complex modulus along with the temperature can be obtained and further the curve of the phase angle to the complex modulus is obtained, and the platform modulus of the material is the lowest point of the curve. Through using the technology, the platform modulus of the material can be obtained with low workload, the complicated problem of the prior art can be solved, and the measurement method has important significance on the relative molecular weight and molecular structure of the research material.
Description
Technical field
The invention belongs to the method for test superpolymer plateau modulus, more particularly, relate under certain linear-viscoelastic condition, by measuring polymer melt composite modulus G in temperature-fall period
*with the situation of change of phasing degree δ, and then obtain its phasing degree δ to composite modulus G
*change curve, thus obtain the plateau modulus G of polymkeric substance
n.
Background technology
Along with the development of material science, macromolecular material is widely used, no matter in daily life or in high-grade, precision and advanced technical fields such as space flight and aviation, macromolecular material is all indispensable, the processing of macromolecule material product and shaping significant to its application, therefore the research of macromolecule melt flow behavior is most important to its processing.
Rheology test is by applying certain flow field to fluids such as polymkeric substance, and then measure its characterizing method at specific stream rheological response after the match, for material in the structural information understood in the fluids such as polymkeric substance and process flow behavior and control significant.As can be obtained the vGP figure of polymer fluid by rheometer test, and then analysis draws the relative molecular mass size of polymkeric substance and the information of distribution thereof.VGP figure normally carries out frequency sweeping to polymer fluid within the scope of linear-viscoelastic, gets its phasing degree δ to corresponding composite modulus G
*map and obtain, in vGP figure, containing a lot of information in the molecular structure of tested measurement.In linear polymer, the characteristic feature of vGP figure is along with composite modulus G
*from small to large, phasing degree δ reduces gradually, and is increasing gradually after a minimal value, phasing degree minimal value δ in this vGP figure
mincorresponding composite modulus G
*namely the plateau modulus G of this polymer fluid is equaled
n.Therefore, in order to the numerical range of enough composite modulus can be obtained, to obtain phasing degree minimal value δ
min, generally first need measure the frequency sweeping curve under different temperatures, by time temperature superposition realize the expansion of experiment test frequency range, by time temperature superpose the principal curve obtained and obtain sample and scheme than more complete vGP, and then obtain the plateau modulus G of sample
n, bring many operational inconvenience thus.
Summary of the invention
Technical purpose of the present invention is to overcome the deficiencies in the prior art, the short-cut method of the plateau modulus of polymer fluid is measured under proposing a kind of dynamic rheological property condition, specifically in certain temperature range, control certain frequency and stress (or strain), dynamic rheological property curve in linear-viscoelastic scope build-in test temperature-fall period, and then be further processed based on obtained data, draw vGP figure, draw phasing degree minimal value δ in this figure
mincorresponding composite modulus G
*, this G
*namely value equals the plateau modulus G of this polymer fluid
n, complete the mensuration of material platform modulus thus easily, no longer need the frequency sweeping curve under measurement different temperatures.
Technical purpose of the present invention is achieved by following technical proposals:
A kind of measuring method of superpolymer plateau modulus, superpolymer to be measured is heated on melt temperature, after realizing thermal equilibrium, control shear stress and frequency are fixed value, once lower the temperature in linear viscoelastic region to test dynamic rheological property curve, map to corresponding composite modulus with phasing degree, the composite modulus that selected phase angle minimal value is corresponding, as the plateau modulus of superpolymer to be measured.
In above-mentioned measuring method, controlling flow graph shear stress is 1000Pa, and frequency is 1Hz, and be 200 DEG C to 80 DEG C between cooling area, rate of temperature fall is 4 DEG C/below min, preferably 2 DEG C/below min, 0.5-1 DEG C/min.
Measuring method described above is in the application of test polystyrene plateau modulus, and error is within 2%.
The invention provides a kind of technology for determining superpolymer fluid plateau modulus in rheological behavior process, to solve the comparatively loaded down with trivial details problem of prior art, do not need frequency sweep experiment at different temperatures, use the plateau modulus method of testing of the fluids such as superpolymer provided by the invention, its corresponding plateau modulus can be determined in the rheological behavior of one group of temperature-fall period.Namely by measuring the cooling scanning curve under high polymer molten condition, obtain phasing degree and complex modulus variation with temperature relation, and then obtain the curve of phasing degree to complex modulus, the minimum point of curve is the plateau modulus of material.The technology that the application of the invention provides, available less workload obtains the plateau modulus of material, to the relative molecular weight of research material and molecular structure significant.
Accompanying drawing explanation
Fig. 1 is the vGP figure of the temperature-fall period of comparative example of the present invention, and wherein is 200 DEG C, zero is 180 DEG C, △ is 160 DEG C, ▽ is that 140 DEG C of condition lower frequencies scan the vGP figure obtained.
Fig. 2 is the vGP figure of the temperature-fall period of the embodiment of the present invention 1, its rate of temperature fall 2 DEG C/min.
Fig. 3 is the vGP figure of the temperature-fall period of the embodiment of the present invention 2, its rate of temperature fall 4 DEG C/min.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with specific embodiment, for the 666D type polystyrene raw material that Yanshan Petrochemical company produces, the dynamic mechanical determining instrument adopted is the StressTech rotational rheometer of Reologica InstrumentsAB company, basic parameter is as follows: moment of torsion resolution is 0.001micro Nm, position resolution 0.1microrad, moment of torsion 0.0001-100mNm, frequency 0.00001-100Hz, the present invention is described in further detail:
Comparative example: take 0.25g polystyrene, the frequency sweeping curve under different temperatures is first measured according to 200 DEG C, 180 DEG C, 160 DEG C, 140 DEG C, by time temperature superposition realize the expansion of experiment test frequency range, by time temperature superpose the principal curve obtained and obtain sample and scheme than more complete vGP, the plateau modulus obtained is 107000Pa.
Embodiment 1: take 0.25g polystyrene, reinforced on flow graph under 200 DEG C of conditions, select P20ETC parallel-plate annex, be added to by polystyrene on parallel-plate, after its heating 3min melting, adjust parallel-plate spacing is 0.8mm, thermal equilibrium 5min, controlling flow graph shear stress is 1000Pa, and frequency is 1Hz, does concussion scanning in its linear viscoelastic region, be 200 DEG C to 80 DEG C between cooling area, rate of temperature fall is 2 DEG C/min.Phasing degree parameter in the data obtained and corresponding complex modulus parameter are mapped, obtain the vGP figure of its temperature-fall period, the complex modulus that in figure, minimum point is corresponding is its plateau modulus, the plateau modulus obtained is 107100Pa, as Fig. 2, the plateau modulus that original method obtains is 107000Pa, and error is 0.1%.
Embodiment 2: take 0.25g polystyrene, reinforced on flow graph under 200 DEG C of conditions, select P20ETC parallel-plate annex, be added to by polystyrene on parallel-plate, after its heating 3min melting, adjust parallel-plate spacing is 0.8mm, thermal equilibrium 5min, controlling flow graph shear stress is 1000Pa, and frequency is 1Hz, does concussion scanning in its linear viscoelastic region, be 200 DEG C to 80 DEG C between cooling area, rate of temperature fall is 4 DEG C/min.Phasing degree parameter in the data obtained and corresponding complex modulus parameter are mapped, obtain the vGP figure of its temperature-fall period, the complex modulus that in figure, minimum point is corresponding is its plateau modulus, the plateau modulus obtained is 109000Pa, as Fig. 3, the plateau modulus that original method obtains is 107000Pa, and error is 1.8%.
Above to invention has been exemplary description; should be noted that; when not departing from core of the present invention, any simple distortion, amendment or other those skilled in the art can not spend the equivalent replacement of creative work all to fall into protection scope of the present invention.
Claims (5)
1. the measuring method of a superpolymer plateau modulus, it is characterized in that, superpolymer to be measured is heated on melt temperature, after realizing thermal equilibrium, control shear stress and frequency are fixed value, once lower the temperature to test dynamic rheological property curve, map with phasing degree to corresponding composite modulus in linear viscoelastic region, the composite modulus that selected phase angle minimal value is corresponding, as the plateau modulus of superpolymer to be measured.
2. the measuring method of a kind of superpolymer plateau modulus according to claim 1, is characterized in that, control shear stress is 1000Pa, and frequency is 1Hz, and be 200 DEG C to 80 DEG C between cooling area, rate of temperature fall is 4 DEG C/below min.
3. the measuring method of a kind of superpolymer plateau modulus according to claim 2, is characterized in that, described rate of temperature fall is preferred 2 DEG C/below min.
4. the measuring method of a kind of superpolymer plateau modulus according to claim 3, is characterized in that, described rate of temperature fall is 0.5-1 DEG C/min.
5. the measuring method as described in one of claim 1-4 is in the application of test polystyrene plateau modulus.
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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 |
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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 true CN104568659A (en) | 2015-04-29 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009064452A2 (en) * | 2007-11-15 | 2009-05-22 | Univation Technologies, Llc. | Ethylene polymers |
| 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 |
-
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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009064452A2 (en) * | 2007-11-15 | 2009-05-22 | Univation Technologies, Llc. | Ethylene polymers |
| 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 |
|---|
| STEFAN TRINKLE ET AL.: "《Van Gurp-Palmen-plot:》", 《RHEOLOGICA ACTA》 * |
| 娄立娟: "《聚合物长支链的流变学表征方法》", 《高分子通报》 * |
| 陈华鑫 等: "《SBS改性沥青低温粘度的动态剪切流变测试方法》", 《同济大学学报（自然科学版）》 * |
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| CN104568659B (en) | 2017-04-05 |
| CN106404602A (en) | 2017-02-15 |
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Application publication date: 20150429 Assignee: TIANJIN YEJIAN SPECIAL MATERIAL CO.,LTD. Assignor: Tianjin Bohua Xinchuang Technology Co.,Ltd. Contract record no.: X2023980049327 Denomination of invention: A measurement method for the modulus of polymer platforms Granted publication date: 20170405 License type: Common License Record date: 20231130 |
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Application publication date: 20150429 Assignee: TIANJIN TIAN YUAN ELECTRICAL MATERIALS CO.,LTD. Assignor: Tianjin Bohua Xinchuang Technology Co.,Ltd. Contract record no.: X2024980003329 Denomination of invention: A measurement method for the modulus of polymer platforms Granted publication date: 20170405 License type: Common License Record date: 20240322 Application publication date: 20150429 Assignee: Tianjin aisida New Material Technology Co.,Ltd. Assignor: Tianjin Bohua Xinchuang Technology Co.,Ltd. Contract record no.: X2024980003327 Denomination of invention: A measurement method for the modulus of polymer platforms Granted publication date: 20170405 License type: Common License Record date: 20240322 |
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