CN105675440A - Detection method for rapidly determining molecular weight distribution of special fiber type polypropylene material - Google Patents
Detection method for rapidly determining molecular weight distribution of special fiber type polypropylene material Download PDFInfo
- Publication number
- CN105675440A CN105675440A CN201410667479.4A CN201410667479A CN105675440A CN 105675440 A CN105675440 A CN 105675440A CN 201410667479 A CN201410667479 A CN 201410667479A CN 105675440 A CN105675440 A CN 105675440A
- Authority
- CN
- China
- Prior art keywords
- type polypropylene
- molecular weight
- weight distribution
- dedicated material
- polypropylene dedicated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 107
- -1 polypropylene Polymers 0.000 title claims abstract description 107
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 107
- 239000000463 material Substances 0.000 title claims abstract description 100
- 238000009826 distribution Methods 0.000 title claims abstract description 84
- 238000001514 detection method Methods 0.000 title claims abstract description 43
- 239000000835 fiber Substances 0.000 title abstract 12
- 238000012360 testing method Methods 0.000 claims abstract description 71
- 238000010008 shearing Methods 0.000 claims description 27
- 238000007731 hot pressing Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 238000002513 implantation Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 230000000694 effects Effects 0.000 description 8
- 238000004154 testing of material Methods 0.000 description 7
- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000010561 standard procedure Methods 0.000 description 4
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000518 rheometry Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 241000876833 Emberizinae Species 0.000 description 1
- 206010020852 Hypertonia Diseases 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention relates to a detection method for rapidly determining molecular weight distribution of a special fiber type polypropylene material, which comprises the following steps: firstly, respectively preparing a fiber type polypropylene special material with known molecular weight distribution and a fiber type polypropylene special material with molecular weight distribution to be tested into test sample sheets; then respectively placing the test sample sheets of the fiber type polypropylene special material with known molecular weight distribution on a strain control type rheometer fixture, and measuring the modulus value G of the fiber type polypropylene special material with known molecular weight distribution, thereby determining the linear scale relation between the molecular weight distribution and the shear modulus of the fiber type polypropylene special material; then, placing the test sample wafer of the fiber type polypropylene special material with the molecular weight distribution to be tested on a strain control type rheometer fixture by the same operation, and measuring the modulus value G of the fiber type polypropylene special material with the molecular weight distribution to be tested; and finally, calculating the molecular weight distribution of the fiber type polypropylene special material according to the linear scale relation between the molecular weight distribution of the fiber type polypropylene special material and the shear modulus by utilizing the modulus value G of the fiber type polypropylene special material with the molecular weight distribution value to be measured.
Description
Technical field
The present invention relates to the detection method of a kind of chemical field, specifically a kind of detection method utilizing the linear viscoelasticity feature of polymkeric substance to determine fibrous type polypropylene dedicated material molecular weight distribution fast.
Background technology
Fibrous type polypropylene dedicated material has purposes widely in industries such as non-woven fabrics, carpet, chinampa, buntings, and domestic market demand amount is very big. Domestic Shuo Jia large-scale petrochemical company has released one after another the fibrous type polypropylene dedicated material of melting index within the scope of 10-50g/10min, but still cannot meet current domestic market demand. Its spinning processing performance and use properties are had most important impact by the molecular weight distribution of fibrous type polypropylene dedicated material. Therefore, how producing and detection molecules amount distribution rapidly and accurately during application, the control of polymerization technique and spinning processing technique is all very important.
At present, usually molecular weight distribution is recorded according to the high-temperature gel permeation chromatography standard method of ASTMD6474-1999 (2006) standard. When surveying molecular weight distribution by high-temperature gel permeation chromatography method, need to use 1,2,4-trichlorobenzene as the solvent of fibrous type polypropylene dedicated material sample, 2,6-di-tert-butyl-4-methy phenol is as oxidation inhibitor, wherein 1,2,4-trichlorobenzene is high toxicity chemical, the respiratory tract of test operator, skin and mucosal tissue etc. there is very big murder by poisoning, and waste liquid after using is very big to environmental influence; In this standard method, operation steps is complicated, and the polystyrene solution often being configured different concns is to produce standard correction curve, and operational requirement is higher; In addition, the method at least needs 3-6 hour with dissolution with solvents sample so that whole test period is relatively long; In addition, due to fibrous type polypropylene specimen consumption is less in this test, about about 20mg, is collected in sample local, the homogeneity of sample itself is proposed high requirement, otherwise the numerical value measured can not represent the characteristic of whole sample.Therefore, for the development and application of fibrous type polypropylene dedicated material, need badly a kind of can the method for Quick Measurement molecular weight distribution, carry out in time being polymerized the adjustment produced to facilitate, and and the control of spinning processing technique.
Summary of the invention
It is an object of the invention to provide a kind of detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast. Utilize the characteristic of fibrous type polypropylene dedicated material linear viscoelasticity in the molten state, merely through the mensuration of once linear visco-elasticity curve, molecular weight distribution can be obtained rapidly and accurately.
The detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast of the present invention, comprises the steps:
First fibrous type polypropylene dedicated material known molecular amount distributed and the fibrous type polypropylene dedicated material of testing molecule amount distribution make test sample respectively;
The test sample of the fibrous type polypropylene dedicated material then described known molecular amount distributed is placed on strain controlling type rheometer fixture respectively, measure the modulus value G* of the fibrous type polypropylene dedicated material of known molecular amount distribution, thus determine the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus;
The test sample of the fibrous type polypropylene dedicated material then described testing molecule amount distributed with same operation is placed on strain controlling type rheometer fixture, measures the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution;
Finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of described testing molecule amount point implantation, calculate its molecular weight distribution by the linear scale relation of described fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus.
Wherein, described test sample adopts thermocompressor compacting and becomes, first with mould, fibrous type polypropylene dedicated material sample is positioned on thermocompressor, then at the temperature of 180-200 DEG C, sample melted 2-4 minute is made, after the complete melting of sample, fusing sample is pressed into stand-by test sample under the pressure of 3-8Mpa, and thermocompressor hot pressing time controlled at 1-2 minute.
Described modulus value G* be phase angle be preferably 65-75 ° time modulus value G*.
Described dot pattern of getting is that logarithm gets a method, and each order of magnitude at least gets 3 points, and integral time is 1-3 test period under each test frequency.
Described strain controlling type rheometer torque range is 0.01 μ Nm-200mNm, and torque precision is 0.1nNm, and normal stress scope is 0.01-50N, and detection range of frequency is 10-7The condition of-628rad/s gets off to measure described modulus value G*.
Described rheometer fixture is that diameter is preferably the flat board of 15-25mm or bores the cone plate that angle is preferably 5o.
The temperature parameter control of described strain controlling type rheometer is preferably 180-220 DEG C; Described strain controlling type rheometer can apply the strain of 1%-8%; Described detection range of frequency is preferably 0.001rad/s-600rad/s.
Described fibrous type polypropylene dedicated material is resin particle or powder, and structure is line polymer.
Compared with prior art, the present invention has following useful effect: for fibrous type polypropylene dedicated material, can merely through the mensuration of once linear visco-elasticity curve, the used time is about 15-30 minute, just disposable can obtain the molecular weight distribution of this fibrous type polypropylene dedicated material sample accurately. Relative to the ordinary method of the molecular weight distribution measuring fibrous type polypropylene dedicated material, the method that the present invention relates to is fast, easy, efficient, cost is low, precision height, sample homogeneity is required low, without any need for aligning step, do not produce any environmental pollution, in industrial production testing process, there is using value.
Accompanying drawing explanation
Fig. 1 is the scale relation curve of fibrous type polypropylene dedicated material rheology modulus and molecular weight distribution, and wherein ordinate zou is the shearing modulus of phase angle when 70 °.
Embodiment
Do embodiments of the invention to illustrate in detail below: the present embodiment is implemented under premised on technical solution of the present invention, gives detailed enforcement mode and process, but protection scope of the present invention is not limited to following embodiment. The experimental technique of unreceipted concrete condition in the following example, usually conveniently condition.
Sample melted temperature:
In the present invention, sample melted temperature being not particularly limited, normally 180-200 DEG C, if temperature is higher than 200 DEG C, then easily causes sample oxidation to degrade, there is no other useful effects, temperature is too low, and sample can not be made to arrive molten state fast.
The sample melted time:
In the present invention, the sample melted time is not particularly limited, normally 2-4 minute, if overlong time, more than 4 minutes, then easily causes sample oxidation to degrade, there is no other useful effects; And the time is too short, it is less than 2 minutes, melting can be caused uneven, the incomplete possibility of melting.
Thermocompressor hot pressing pressure:
In the present invention, hot pressing pressure when fusing sample is pressed into stand-by test sample is not particularly limited, and fusing sample is normally pressed under the pressure of 3-8Mpa stand-by test sample, if hypertonia, it is greater than 8Mpa, test sample can be caused to have the possibility of crackle, there is no other useful effects; And hypotony, it is less than 3Mpa, test sample compressing tablet can be caused uneven, do not reach the requirement to test sample.
Thermocompressor hot pressing time:
In the present invention, thermocompressor hot pressing time is not particularly limited, usually controls at 1-2 minute, if hot pressing time is too high, be greater than 2 minutes, then cause sample oxidation to degrade, there is no other useful effects; Time is too short, is less than 2 minutes, hot pressing time can be caused not enough, the impact that test sample hot pressing effect is not good, the possibility that print is uneven.
The phase angle of modulus value G*:
In the present invention, the phase angle of modulus value G* being not particularly limited, the phase angle of usual modulus value G* is 65 °-75 °, if phase angle spends height or excessively little, namely be greater than 75 ° or lower than 65 °, then can not there is the linear scale relation good with molecular weight distribution in corresponding modulus value G*.
Get dot pattern:
In the present invention, being not particularly limited getting dot pattern, each order of magnitude at least gets 3 points usually, if getting o'clock less than 3 points, then causes data point less, and inaccurate so that modulus value G* and molecular weight distribution the linear scale relation of digital independent is inaccurate.
Integral time:
In the present invention, being not particularly limited integral time, 1-3 the test period being generally under each test frequency, if 3 test periods under being greater than each test frequency, then cause waveform recording less, digital independent is inaccurate.
Strain controlling type rheometer:
In the present invention, being not particularly limited by strain controlling type rheometer, usual strain controlling type rheometer torque range is 0.01 μ Nm-200mNm, and torque precision is 0.1nNm, and normal stress scope is 0.01-50N, and detection range of frequency is 10-7-628rad/s, if torque range is not at 0.01 μ Nm-200mNm, torque precision is lower than 0.1nNm, and normal stress scope is not at 0.01-50N, and detection range of frequency is not 10-7-628rad/s, then can not reach test precision, causes the linear scale relation of modulus value G* and molecular weight distribution inaccurate.
Rheometer fixture:
In the present invention, being not particularly limited by rheometer fixture, general diameter is the flat board of 15-25mm or bores the cone plate that angle is 5 °, if plate diameter is greater than 25mm, then required test sample is more, is less than 15mm, then can affect test precision.
The temperature parameter of strain controlling type rheometer:
In the present invention, the temperature parameter of strain controlling type rheometer is not particularly limited, is usually controlled to 180-220 DEG C, if temperature is higher than 220 DEG C, then easily causing sample oxidation to degrade, there is no other useful effects, temperature is too low, and sample can not be made to ensure to arrive molten state fast.
The strain that strain controlling type rheometer applies:
In the present invention, the strain that strain controlling type rheometer applies is not particularly limited, usual strain controlling type rheometer applies the strain of 1%-8%, if the strain applied is higher than 8%, then can destroy sample molecule chain structure, there is no other useful effects, if lower than 1%, then strain control accuracy is realized difficulty.
Detection range of frequency:
In the present invention, detection range of frequency is not particularly limited, usually detection range of frequency is 0.001rad/s-600rad/s, if detection range of frequency is not in 0.001rad/s-600rad/s, then can not obtain the linear scale relation of effective modulus value G* and molecular weight distribution.
Fibrous type polypropylene dedicated material:
In the present invention; fibrous type polypropylene dedicated material is not particularly limited; it is generally resin particle or powder; structure is line polymer; fibrous type polypropylene dedicated material is selected to be resin particle or powder; if structure is not linear polymer, then can not obtain the linear scale relation of effective modulus value G* and molecular weight distribution.
Embodiment 1
Fibrous type polypropylene dedicated material particulate state sample known molecular amount distributed with mould is positioned on thermocompressor, melting 3 minutes at 180 DEG C, imposes the pressure durations hot pressing 1 minute of 4Mpa subsequently, and compacting obtains stand-by test sample; It is on the plate jig of 20mm that print is placed in strain controlling type rheometer diameter, and this rheometer torque precision is 0.1nNm, and torque range is 0.01 μ Nm-200mNm, and normal stress scope is 0.01-50N, and the detection range of frequency that can apply is 10-7-628rad/s, set temperature is 180 DEG C, apply the strain of 8%, arranging detection range of frequency is 0.01-100rad/s, gets 3 data points with each order of magnitude of logarithmic mode, is set to 1 cycle integral time, recording phase angle is shearing modulus when 70 °, according to the scale relation curve of Fig. 1 fibrous type polypropylene dedicated material rheology shearing modulus and molecular weight distribution, calculate the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus, MWD=-2.272 × 10-4G*+7.399。
Then with same operation, the test sample of fibrous type polypropylene dedicated material testing molecule amount distributed is placed on strain controlling type rheometer fixture, measure the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution, finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of the testing molecule amount point implantation recorded, substitute into the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and the shearing modulus tried to achieve, i.e. MWD=-2.272 × 10-4G*+7.399, calculates its molecular weight distribution MWD, in table 1.
Embodiment 2
Fibrous type polypropylene dedicated material particulate state sample known molecular amount distributed with mould is positioned on thermocompressor, melting 2 minutes at 180 DEG C, imposes the pressure durations hot pressing 1 minute of 3Mpa subsequently, and compacting obtains stand-by test sample; It is on the plate jig of 15mm that print is placed in strain controlling type rheometer diameter, and this rheometer torque precision is 0.1nNm, and torque range is 0.01 μ Nm-200mNm, and normal stress scope is 0.01-50N, and the detection range of frequency that can apply is 10-7-628rad/s, set temperature is 180 DEG C, apply the strain of 1%, arranging detection range of frequency is 0.001-100rad/s, getting 3 data points with each order of magnitude of logarithmic mode, be set to 1 cycle integral time, recording phase angle is shearing modulus when 65 ° (see table 1), calculate the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus, MWD=-2.135 × 10-4G*+7.087。
Then with same operation, the test sample of fibrous type polypropylene dedicated material testing molecule amount distributed is placed on strain controlling type rheometer fixture, measure the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution, finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of the testing molecule amount point implantation recorded, substitute into the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and the shearing modulus tried to achieve, i.e. MWD=-2.135 × 10-4G*+7.087, calculates its molecular weight distribution MWD, in table 1.
Embodiment 3
Fibrous type polypropylene dedicated material particulate state sample known molecular amount distributed with mould is positioned on thermocompressor, melting 3 minutes at 190 DEG C, imposes the pressure durations hot pressing 2 minutes of 5Mpa subsequently, and compacting obtains stand-by test sample; It is on the plate jig of 25mm that print is placed in strain controlling type rheometer diameter, and this rheometer torque precision is 0.1nNm, and torque range is 0.01 μ Nm-200mNm, and normal stress scope is 0.01-50N, and the detection range of frequency that can apply is 10-7-628rad/s, set temperature is 200 DEG C, apply the strain of 8%, arranging detection range of frequency is 0.01-600rad/s, getting 5 data points with each order of magnitude of logarithmic mode, be set to 2 cycles integral time, recording phase angle is shearing modulus when 70 ° (see table 1), calculate the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus, MWD=-1.989 × 10-4G*+7.215。
Then with same operation, the test sample of fibrous type polypropylene dedicated material testing molecule amount distributed is placed on strain controlling type rheometer fixture, measure the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution, finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of the testing molecule amount point implantation recorded, substitute into the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and the shearing modulus tried to achieve, i.e. MWD=-1.989 × 10-4G*+7.215, calculates its molecular weight distribution MWD, in table 1.
Embodiment 4
Fibrous type polypropylene dedicated material particulate state sample known molecular amount distributed with mould is positioned on thermocompressor, melting 3 minutes at 200 DEG C, imposes the pressure durations hot pressing 1.5 minutes of 8Mpa subsequently, and compacting obtains stand-by test sample; It is on the cone board clamp of 25mm that print is placed in strain controlling type rheometer diameter, and cone angle is 5 °, and this rheometer torque precision is 0.1nNm, and torque range is 0.01 μ Nm-200mNm, and normal stress scope is 0.01-50N, and the detection range of frequency that can apply is 10-7-628rad/s, set temperature is 220 DEG C, apply the strain of 5%, arranging detection range of frequency is 0.001-100rad/s, getting 7 data points with each order of magnitude of logarithmic mode, be set to 3 cycles integral time, recording phase angle is shearing modulus when 75 ° (see table 1), calculate the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus, MWD=-2.187 × 10-4G*+7.508。
Then with same operation, the test sample of fibrous type polypropylene dedicated material testing molecule amount distributed is placed on strain controlling type rheometer fixture, measure the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution, finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of the testing molecule amount point implantation recorded, substitute into the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and the shearing modulus tried to achieve, i.e. MWD=-2.187 × 10-4G*+7.508, calculates its molecular weight distribution MWD, in table 1.
Embodiment 5
Fibrous type polypropylene dedicated material particulate state sample known molecular amount distributed with mould is positioned on thermocompressor, melting 4 minutes at 200 DEG C, imposes the pressure durations hot pressing 2 minutes of 5Mpa subsequently, and compacting obtains stand-by test sample; It is on the cone board clamp of 20mm that print is placed in strain controlling type rheometer diameter, and cone angle is 5 °, and this rheometer torque precision is 0.1nNm, and torque range is 0.01 μ Nm-200mNm, and normal stress scope is 0.01-50N, and the detection range of frequency that can apply is 10-7-628rad/s, set temperature is 210 DEG C, apply the strain of 3%, arranging detection range of frequency is 0.01-100rad/s, getting 3 data points with each order of magnitude of logarithmic mode, be set to 2 cycles integral time, recording phase angle is shearing modulus when 70 ° (see table 1), calculate the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus, MWD=-2.358 × 10-4G*+7.659。
Then with same operation, the test sample of fibrous type polypropylene dedicated material testing molecule amount distributed is placed on strain controlling type rheometer fixture, measure the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution, finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of the testing molecule amount point implantation recorded, substitute into the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and the shearing modulus tried to achieve, i.e. MWD=-2.358 × 10-4G*+7.659, calculates its molecular weight distribution MWD, in table 1.
Embodiment 6
Fibrous type polypropylene dedicated material pulverized specimen known molecular amount distributed with mould is positioned on thermocompressor, melting 4 minutes at 200 DEG C, imposes the pressure durations hot pressing 2 minutes of 5Mpa subsequently, and compacting obtains stand-by test sample; It is on the cone board clamp of 15mm that print is placed in strain controlling type rheometer diameter, and cone angle is 5 °, and this rheometer torque precision is 0.1nNm, and torque range is 0.01 μ Nm-200mNm, and normal stress scope is 0.01-50N, and the detection range of frequency that can apply is 10-7-628rad/s, set temperature is 210 DEG C, apply the strain of 3%, arranging detection range of frequency is 0.01-100rad/s, getting 3 data points with each order of magnitude of logarithmic mode, be set to 2 cycles integral time, recording phase angle is shearing modulus when 70 ° (see table 1), calculate the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus, MWD=-2.401 × 10-4G*+7.603。
Then with same operation, the test sample of fibrous type polypropylene dedicated material testing molecule amount distributed is placed on strain controlling type rheometer fixture, measure the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution, finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of the testing molecule amount point implantation recorded, substitute into the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and the shearing modulus tried to achieve, i.e. MWD=-2.401 × 10-4G*+7.603, calculates its molecular weight distribution MWD, in table 1.
Embodiment 7
Fibrous type polypropylene dedicated material pulverized specimen known molecular amount distributed with mould is positioned on thermocompressor, melting 4 minutes at 200 DEG C, imposes the pressure durations hot pressing 2 minutes of 5Mpa subsequently, and compacting obtains stand-by test sample; It is on the plate jig of 20mm that print is placed in strain controlling type rheometer diameter, and this rheometer torque precision is 0.1nNm, and torque range is 0.01 μ Nm-200mNm, and normal stress scope is 0.01-50N, and the detection range of frequency that can apply is 10-7-628rad/s, set temperature is 190 DEG C, apply the strain of 7%, arranging detection range of frequency is 0.001-600rad/s, getting 11 data points with each order of magnitude of logarithmic mode, be set to 1 cycle integral time, recording phase angle is shearing modulus when 72 ° (see table 1), calculate the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus, MWD=-2.467 × 10-4G*+7.424。
Then with same operation, the test sample of fibrous type polypropylene dedicated material testing molecule amount distributed is placed on strain controlling type rheometer fixture, measure the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution, finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of the testing molecule amount point implantation recorded, substitute into the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and the shearing modulus tried to achieve, i.e. MWD=-2.467 × 10-4G*+7.424, calculates its molecular weight distribution MWD, in table 1.
Table 1 is modulus value (G*), the molecular weight distribution (MWD) of the fibrous type polypropylene dedicated material that each embodiment method that the present invention relates to records, and the molecular weight distribution (MWD0) that same sample records according to the high-temperature gel permeation chromatography standard method of ASTMD6474-1999 (2006) standard, relatively visible, the data accuracy that the method for the present invention relates to records is very high, for fibrous type polypropylene dedicated material material system, molecular weight distribution can be obtained as a kind of fast and convenient measuring method, substitute traditional detection method.
With the present invention relates to method and the contrast of standard method test data in each embodiment of table 1
Claims (10)
1. determine a detection method for fibrous type polypropylene dedicated material molecular weight distribution fast, there are following steps:
First fibrous type polypropylene dedicated material known molecular amount distributed and the fibrous type polypropylene dedicated material of testing molecule amount distribution make test sample respectively;
The test sample of the fibrous type polypropylene dedicated material then described known molecular amount distributed is placed on strain controlling type rheometer fixture respectively, measure the modulus value G* of the fibrous type polypropylene dedicated material of known molecular amount distribution, thus determine the linear scale relation of fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus;
The test sample of the fibrous type polypropylene dedicated material then described testing molecule amount distributed with same operation is placed on strain controlling type rheometer fixture, measures the modulus value G* of the fibrous type polypropylene dedicated material of testing molecule amount distribution;
Finally utilize the modulus value G* of the fibrous type polypropylene dedicated material of described testing molecule amount point implantation, calculate its molecular weight distribution by the linear scale relation of described fibrous type polypropylene dedicated material molecular weight distribution and shearing modulus.
2. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 1, it is characterised in that:
Described test sample adopts thermocompressor compacting and becomes, first with mould, fibrous type polypropylene dedicated material sample is positioned on thermocompressor, then at the temperature of 180-200 DEG C, sample melted 2-4 minute is made, after the complete melting of sample, fusing sample is pressed into stand-by test sample under the pressure of 3-8Mpa, and thermocompressor hot pressing time controlled at 1-2 minute.
3. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 2, is characterized in that, described modulus value G* is phase angle is modulus value G* when 65 °-75 °.
4. according to the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast described in any one in claims 1 to 3, it is characterized in that, getting dot pattern is that logarithm gets a method, and each order of magnitude at least gets 3 points, and integral time is 1-3 test period under each test frequency.
5. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 4, it is characterized in that, described strain controlling type rheometer torque range is 0.01 μ Nm-200mNm, and torque precision is 0.1nNm, normal stress scope is 0.01-50N, and detection range of frequency is 10-7The condition of-628rad/s gets off to measure described modulus value G*.
6. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 5, is characterized in that, the flat board of described rheometer fixture to be diameter be 15-25mm or cone angle are the cone plate of 5 °.
7. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 5, is characterized in that, the temperature parameter of described strain controlling type rheometer is controlled to 180-220 DEG C.
8. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 5, is characterized in that, described strain controlling type rheometer applies the strain of 1%-8%.
9. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 5, is characterized in that, described detection range of frequency is 0.001rad/s-600rad/s.
10. the detection method determining fibrous type polypropylene dedicated material molecular weight distribution fast according to claim 5, is characterized in that, described fibrous type polypropylene dedicated material is resin particle or powder, and structure is line polymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410667479.4A CN105675440A (en) | 2014-11-20 | 2014-11-20 | Detection method for rapidly determining molecular weight distribution of special fiber type polypropylene material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410667479.4A CN105675440A (en) | 2014-11-20 | 2014-11-20 | Detection method for rapidly determining molecular weight distribution of special fiber type polypropylene material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105675440A true CN105675440A (en) | 2016-06-15 |
Family
ID=56957978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410667479.4A Pending CN105675440A (en) | 2014-11-20 | 2014-11-20 | Detection method for rapidly determining molecular weight distribution of special fiber type polypropylene material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105675440A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6064945A (en) * | 1998-02-20 | 2000-05-16 | Waters Investments Limited | System and method for determining molecular weight and intrinsic viscosity of a polymeric distribution using gel permeation chromatography |
| CN101178348A (en) * | 2006-11-10 | 2008-05-14 | 朗盛德国有限责任公司 | Method for determining the molecular weight distribution in a polymer |
| JP2009110228A (en) * | 2007-10-30 | 2009-05-21 | Japan Science & Technology Agency | Molecular motion analyzing method for high molecular compound in which solid particle is dispersed and analysis program |
| CN101458246A (en) * | 2009-01-08 | 2009-06-17 | 浙江大学 | Method for measuring molecular weight distribution of linear polymer |
| CN102053044A (en) * | 2009-10-30 | 2011-05-11 | 中国石油天然气股份有限公司 | Method for rapidly determining viscous flow activation energy of polyolefin |
| CN102341447A (en) * | 2009-01-09 | 2012-02-01 | 帝人芳纶有限公司 | Ultra-high molecular weight polyethylene comprising refractory particles |
| CN102466604A (en) * | 2010-11-04 | 2012-05-23 | 中国石油天然气股份有限公司 | Method for measuring molecular weight of polyethylene |
| CN103234868A (en) * | 2013-04-25 | 2013-08-07 | 常州大学 | Method for measuring weight-average molecular weight of linear polymers |
-
2014
- 2014-11-20 CN CN201410667479.4A patent/CN105675440A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6064945A (en) * | 1998-02-20 | 2000-05-16 | Waters Investments Limited | System and method for determining molecular weight and intrinsic viscosity of a polymeric distribution using gel permeation chromatography |
| CN101178348A (en) * | 2006-11-10 | 2008-05-14 | 朗盛德国有限责任公司 | Method for determining the molecular weight distribution in a polymer |
| JP2009110228A (en) * | 2007-10-30 | 2009-05-21 | Japan Science & Technology Agency | Molecular motion analyzing method for high molecular compound in which solid particle is dispersed and analysis program |
| CN101458246A (en) * | 2009-01-08 | 2009-06-17 | 浙江大学 | Method for measuring molecular weight distribution of linear polymer |
| CN102341447A (en) * | 2009-01-09 | 2012-02-01 | 帝人芳纶有限公司 | Ultra-high molecular weight polyethylene comprising refractory particles |
| CN102053044A (en) * | 2009-10-30 | 2011-05-11 | 中国石油天然气股份有限公司 | Method for rapidly determining viscous flow activation energy of polyolefin |
| CN102466604A (en) * | 2010-11-04 | 2012-05-23 | 中国石油天然气股份有限公司 | Method for measuring molecular weight of polyethylene |
| CN103234868A (en) * | 2013-04-25 | 2013-08-07 | 常州大学 | Method for measuring weight-average molecular weight of linear polymers |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Airey et al. | The influence of geometry and sample preparation on dynamic shear rheometer testing | |
| WO2015085812A1 (en) | Apparatus for measuring cell internal resistance online and measurement method therefor | |
| CN105911512A (en) | Intelligent electric energy meter constant test system and test method thereof | |
| CN204008572U (en) | A kind of compound substance step bar | |
| CN103900955A (en) | Device for quantitatively testing initial viscosity of adhesive and test method | |
| CN105675439A (en) | Detection method for rapidly determining melt index and molecular weight of special material for fiber type polypropylene | |
| CN102661930B (en) | A kind of method for quick for thermosets degree of cure | |
| CN203772717U (en) | Quantitative test device for initial viscosity of adhesive | |
| CN103759651B (en) | A kind of alternating temperature of monitoring in real time variable-pressure laser speckle measurement system | |
| CN208109585U (en) | Concrete static(al) compression elasticity modulus test automatic acquisition device and system | |
| CN105675440A (en) | Detection method for rapidly determining molecular weight distribution of special fiber type polypropylene material | |
| CN109975243A (en) | The quickly method of measurement polyacrylonitrile solid content | |
| CN202522693U (en) | Device for detecting measure accuracy degree of electric energy meter | |
| CN103454202A (en) | Testing method of aggregating specific surface area of bituminous mixture | |
| CN104075988A (en) | Method for testing dispersity of wet chopped strands of glass fibers in water | |
| CN105259074A (en) | Rheological evaluation method of polyethylene for medical instruments | |
| CN101782492A (en) | Method for determining volume fraction of single component in two-component mixed solution through density detection | |
| CN103837170B (en) | Rate-adaptive pacemaker class sensor automatic frequency compensation circuit and method | |
| CN101871971A (en) | Method for measuring frequency-phase characteristic of electrical network | |
| CN104568623A (en) | Method for measuring hardness of biomass material | |
| CN206132591U (en) | Pitch and adhesion nature tester that gathers materials | |
| CN204630542U (en) | Based on the pressure vessel ellipsoidal head testing instruments of ellipsograph | |
| CN110018083B (en) | Characterization method for rheological property of prepreg | |
| CN204044108U (en) | A kind of high-abrasive material Element detection instrument | |
| CN206431049U (en) | A kind of Filming kinetics tester |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160615 |
|
| RJ01 | Rejection of invention patent application after publication |