CN109443956A - A method of measurement polymer average molecular weight - Google Patents
A method of measurement polymer average molecular weight Download PDFInfo
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- CN109443956A CN109443956A CN201811205791.6A CN201811205791A CN109443956A CN 109443956 A CN109443956 A CN 109443956A CN 201811205791 A CN201811205791 A CN 201811205791A CN 109443956 A CN109443956 A CN 109443956A
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- molecular weight
- flow rate
- average molecular
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- melt flow
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/30—Investigating strength properties of solid materials by application of mechanical stress by applying a single impulsive force, e.g. by falling weight
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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
Abstract
The present invention relates to a kind of methods for measuring polymer average molecular weight.First in the notch impact strength z of impact test airborne measurements polymer, the melt flow rate (MFR) x of polymer is measured on Melt Flow Rate Measurer, is in power function relationship: z=C0 × x between the notch impact strength z and melt flow rate (MFR) x of polymerC(I), C and C0 is constant in formula, is in power function relationship: M=10 between the weight average molecular weight M and melt flow rate (MFR) x of polymer5×D0×xD(II), D and D0 is constant in formula, will can obtain M=10 after formula (I) and formula (II) abbreviation5×D0×(z/C0)D/C；Notch impact strength z is brought into, polymer average molecular weight M is solved to obtain, the present invention only needs to measure the weight average molecular weight for obtaining polymer by common Melt Flow Rate Measurer and impact strength machine, and this method is quick, environmentally friendly and accurate.
Description
Technical field
The present invention relates to a kind of methods for measuring polymer (high molecular material) weight average molecular weight, more particularly to mechanics side
The impact strength and melt flow rate (MFR) of method test polymer, and weight average molecular weight is solved with non-linear fitting method.
Background technique
The method of measurement high molecular material molecular weight is mainly GPC method, including high temperature GPC method at present.Due to not ready-made
Instrument, equipment or suitable solvent, so that the molecular weight for obtaining polymer becomes difficult.Rheological method can be estimated indirectly
The molecular weight parameter of high molecular material, such as application No. is the patents of 200910095287.X and 201310147593.X to give
The method for measuring linear polymeric molecular weight with rheological method, but need rheometer.And the application does not have to rheometer, it is only necessary to
Simpler common Melt Flow Rate Measurer and impact strength machine can measure the weight average molecular weight for obtaining polymer.
Summary of the invention
Object of the present invention is to provide in order to solve the above problem and a kind of measure polymeric material indirectly using mechanical measuring and calculation method
Expect weight average molecular weight method.
To achieve the goals above, the present invention is implemented as follows:
The first step, in the notch impact strength z of impact test airborne measurements polymer.
Second step measures the melt flow rate (MFR) x of polymer on Melt Flow Rate Measurer.
Third step measures N group data, analyzes data, makees notch impact strength z and intends with what melt flow rate (MFR) x changed
Close curve.Studies have shown that being in power function relationship between the notch impact strength z and melt flow rate (MFR) x of polymer:
Z=C0 × xC (1)
C and C0 is constant in formula (1).
It in the prior art, is in certain relationship between the weight average molecular weight M and melt flow rate (MFR) x of polymer.I.e.
Lgx=A-BlgM (2)
A, B are constant in formula (2).
Or
Lgx=A-BlgM+Flg (M/Mn) (2 ')
Mn is number-average molecular weight, i.e. the weight average molecular weight M and molecular weight distribution of melt flow rate (MFR) x and polymer are related
System.
Make the matched curve that weight average molecular weight M changes with melt flow rate (MFR) x, studies have shown that the Weight-average molecular of polymer
It can also be indicated with power function between amount M and melt flow rate (MFR) x, it may be assumed that
M=105×D0×xD (3)
D and D0 is constant in formula (3)；
Using formula 1 and formula 3, can be obtained after abbreviation
M=105×D0×(z/C0)D/C (4)
The notch impact strength z of certain polymer is brought into formula (4), the weight average molecular weight M to emergencing copolymer is obtained after solution.
Compared with prior art, the invention has the benefit that
The present invention is not required to dissolve in polymer from the angle of mechanical meaurement, overcome traditional test mode cannot or
It is difficult to measure insoluble or indissoluble object weight average molecular weight limitation；Method of the invention can it is cheap, quickly, environmental protection, more reliably
Measure the weight average molecular weight of polymer.
Figure of description
Fig. 1 is the curve of weight average molecular weight M Yu melt flow rate (MFR) x (190 DEG C, 2.16kg)；
Fig. 2 is the notch impact strength and MFR relation curve of high density polyethylene (HDPE) A；
Fig. 3 is the notch impact strength and MFR relation curve of high density polyethylene (HDPE) B；
Fig. 4 is the notch impact strength and MFR relation curve of high density polyethylene (HDPE) C.
Specific embodiment
Embodiment 1
The first step, in the notch impact strength z of impact test airborne measurements polymer samples；(standard is GB/T 1843-
2008)
Second step measures the melt flow rate (MFR) x of polymer samples on Melt Flow Rate Measurer；(standard GB/
T3682-2000)。
According to above-mentioned steps, the weight average molecular weight M of several high density polyethylene (HDPE) samples (such as A, B, C, D etc.) is measured respectively
(MA, MB, MC, MD) and melt flow rate (MFR) x (xA, xB, xC, xD) (190 DEG C, 2.16kg) data, make weight average molecular weight M with molten
The matched curve of body flow rate x variation, the relation curve are as shown in Figure 1；
Relationship between the two can use M=10 as can be seen from Figure 15×D0×xDFormula (II) expression,
Wherein D=-0.24, D0=1.477.
The weight average molecular weight M of high density polyethylene (HDPE) sample A to known toAWith melt flow rate (MFR) xA(190 DEG C, 2.16kg)
Relationship；
Two kinds of polymer material is taken, such as high density polyethylene (HDPE) A and high density polyethylene (HDPE) A1, squeezed by mixer or twin-screw
(such as 30/70,50/50,70/30) is blended using different proportion in two kinds of materials by machine out, obtains A/A1Intermingling material is surveyed respectively
Measure A/A1Intermingling material, pure material A and pure material A1Z and x value.
Make the matched curve that above-mentioned notch impact strength z changes with melt flow rate (MFR) x, notch impact strength z and molten
The half interval contour of body flow rate x is as shown in Figure 2；
Relationship can use z=C0 × x between the twoCFormula (I) expression,
Wherein C=-0.74, C0=54.3.
It will can be obtained after formula (I) and formula (II) abbreviation
M=105×D0×(z/C0)D/C(Ⅲ)
In the case where each constant known, it is only necessary to measure the notch impact strength z of materials A, can be obtained by formula (III)
Obtain the information of weight average molecular weight.
According to above-mentioned steps, the notch impact strength for measuring high density polyethylene (HDPE) A is 38KJ/m2, high-density polyethylene can be obtained
The weight average molecular weight of alkene A is 1.32 × 105。
Traditional high temperature GPC method is used to measure its weight average molecular weight as 1.5 × 10 high density polyethylene (HDPE) A5, it is seen that with this
The weight average molecular weight that the method for invention acquires differs smaller with gpc measurement value.
Embodiment 2
The first step, in the notch impact strength z of impact test airborne measurements polymer samples；(measurement standard GB/T
1843-2008)
Second step measures the melt flow rate (MFR) x of polymer samples on Melt Flow Rate Measurer；(measurement standard GB/
T3682-2000)。
According to above-mentioned steps, the weight average molecular weight M of several high density polyethylene (HDPE) samples (such as A, B, C, D etc.) is measured respectively
(MA, MB, MC, MD) and melt flow rate (MFR) x (xA, xB, xC, xD) (190 DEG C, 2.16kg) data, make weight average molecular weight M with molten
The matched curve of body flow rate x variation, the relation curve are as shown in Figure 1；
Relationship between the two can use M=10 as can be seen from Figure 15×D0×xD(II) it indicates,
Wherein D=-0.24, D0=1.477.
The weight average molecular weight M of high density polyethylene (HDPE) sample B to known toBWith melt flow rate (MFR) xB(190 DEG C, 2.16kg)
Relationship；
Two kinds of polymer material is taken, such as high density polyethylene (HDPE) B and high density polyethylene (HDPE) B1, squeezed by mixer or twin-screw
(such as 30/70,50/50,70/30) is blended using different proportion by two kinds in machine out, obtains B/B1Intermingling material measures B/B respectively1
Intermingling material, pure material B and pure material B1Z and x value.
Make the matched curve that above-mentioned notch impact strength z changes with melt flow rate (MFR) x, notch impact strength z and molten
The half interval contour of body flow rate x is as shown in Figure 3.
Relationship can use z=C0 × x between the twoC(I) it indicates,
Wherein C=-0.49, C0=20.67.
It will can be obtained after formula (I) and formula (II) abbreviation
M=105×D0×(z/C0)D/C(Ⅲ)
In the case where each constant known, it is only necessary to measure the notch impact strength z of material B, can be obtained by formula (III)
Obtain weight average molecular weight information.
According to above-mentioned steps, the notch impact strength for measuring high density polyethylene (HDPE) B is 10.39KJ/m2, it is poly- that high density can be obtained
The weight average molecular weight of ethylene B is 1.05 × 105。
High density polyethylene (HDPE) B is measured into its weight average molecular weight using traditional high temperature GPC method, the result finally measured is
0.94×105.It can be seen that the weight average molecular weight acquired with method of the invention differs smaller with gpc measurement value.
Embodiment 3
The first step, in the notch impact strength z of impact test airborne measurements polymer samples；(measurement standard GB/T
1843-2008)
Second step measures the melt flow rate (MFR) x of polymer samples on Melt Flow Rate Measurer；(measurement standard GB/
T3682-2000)；
According to above-mentioned steps, the weight average molecular weight M of several high density polyethylene (HDPE) samples (such as A, B, C, D etc.) is measured respectively
(MA, MB, MC, MD) and melt flow rate (MFR) x (xA, xB, xC, xD) (190 DEG C, 2.16kg) data, make weight average molecular weight M with molten
The matched curve of body flow rate x variation, the relation curve are as shown in Figure 1；
Relationship between the two can use M=10 as can be seen from Figure 15×D0×xD(II) it indicates,
Wherein D=-0.24, D0=1.477.
The weight average molecular weight M of high density polyethylene (HDPE) sample C is known from Fig. 1CWith melt flow rate (MFR) xC(190 DEG C, 2.16kg)
Relationship；
Choose high density polyethylene (HDPE) C and high density polyethylene (HDPE) C1Material, crosses mixer or double screw extruder adopts two kinds
(such as 30/70,50/50,70/30) is blended with different proportion, obtains C/C1Intermingling material measures C/C1Intermingling material, pure material C and
Pure material C1Z and x value.
Make the matched curve that above-mentioned notch impact strength z changes with melt flow rate (MFR) x, notch impact strength z and molten
The half interval contour of body flow rate x is as shown in Figure 4.
Relationship can use z=C0 × x between the twoC(I) it indicates,
Wherein C=-0.76, C0=37.9.
It will can be obtained after formula (I) and formula (II) abbreviation
M=105×D0×(z/C0)D/C(Ⅲ)
In the case where each constant known, it is only necessary to measure the notch impact strength z of material C, can be obtained by formula (III)
Obtain weight average molecular weight information.
According to above-mentioned steps, the notch impact strength for measuring high density polyethylene (HDPE) C is 24.3KJ/m2, it is poly- that high density can be obtained
The weight average molecular weight of ethylene C is 1.26 × 105。
High density polyethylene (HDPE) C is measured into its weight average molecular weight using traditional high temperature GPC method, the result finally measured is
1.1×105.It can be seen that the weight average molecular weight acquired with method of the invention differs smaller with gpc measurement value.
The foregoing is merely several specific embodiments of the invention, it is noted that for the ordinary skill of this field
For personnel, many variations and modifications can also be made, it is all to be regarded as without departing from modification or improvement described in claim
Protection scope of the present invention.
Claims (1)
1. a kind of method for measuring polymer average molecular weight, which is characterized in that the measuring process is as follows:
The first step, in the notch impact strength z of impact test airborne measurements polymer；
Second step measures the melt flow rate (MFR) x of polymer on Melt Flow Rate Measurer；
Third step makees the matched curve that notch impact strength z changes with melt flow rate (MFR) x, obtains the notch shock of polymer
It is in power function relationship between intensity z and melt flow rate (MFR) x:
Z=C0 × xC (Ⅰ)
C and C0 is constant in formula (I)；
4th step makees the matched curve that weight average molecular weight M changes with melt flow rate (MFR) x, obtains the weight average molecular weight M of polymer
It is in power function relationship between melt flow rate (MFR) x:
M=105×D0×xD (Ⅱ)
D and D0 is constant in formula (II)；
5th step will obtain after formula (I) and formula (II) abbreviation:
M=105×D0×(z/C0)D/C (Ⅲ)
6th step brings notch impact strength z into formula (III), solves to obtain polymer average molecular weight M.
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| US20070111127A1 (en) * | 2005-11-14 | 2007-05-17 | Xerox Corporation | Toner having crystalline wax |
| CN103234868A (en) * | 2013-04-25 | 2013-08-07 | 常州大学 | Method for measuring weight-average molecular weight of linear polymers |
| CN105189639A (en) * | 2013-05-22 | 2015-12-23 | 陶氏环球技术有限责任公司 | Low density ethylene-based compositions with improved melt strength, output, and mechanical properties |
| CN105675439A (en) * | 2014-11-20 | 2016-06-15 | 中国石油天然气股份有限公司 | Detection method for rapid determination of melt index and molecular weight of fiber-type polypropylene special-purpose material |
| CN106062065A (en) * | 2013-11-28 | 2016-10-26 | 阿布扎比聚合物有限公司(博禄) | Multimodal polymer |
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2018
- 2018-10-17 CN CN201811205791.6A patent/CN109443956A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070111127A1 (en) * | 2005-11-14 | 2007-05-17 | Xerox Corporation | Toner having crystalline wax |
| CN103234868A (en) * | 2013-04-25 | 2013-08-07 | 常州大学 | Method for measuring weight-average molecular weight of linear polymers |
| CN105189639A (en) * | 2013-05-22 | 2015-12-23 | 陶氏环球技术有限责任公司 | Low density ethylene-based compositions with improved melt strength, output, and mechanical properties |
| CN106062065A (en) * | 2013-11-28 | 2016-10-26 | 阿布扎比聚合物有限公司(博禄) | Multimodal polymer |
| CN105675439A (en) * | 2014-11-20 | 2016-06-15 | 中国石油天然气股份有限公司 | Detection method for rapid determination of melt index and molecular weight of fiber-type polypropylene special-purpose material |
Non-Patent Citations (2)
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| 廖华勇 等: "高密度聚乙烯共混物的抗冲击强度与熔体流动速率", 《高分子材料科学与工程》 * |
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