CN106198799A - A kind of analysis method of PFPE relative molecular weight and its distribution - Google Patents
A kind of analysis method of PFPE relative molecular weight and its distribution Download PDFInfo
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- CN106198799A CN106198799A CN201610532964.XA CN201610532964A CN106198799A CN 106198799 A CN106198799 A CN 106198799A CN 201610532964 A CN201610532964 A CN 201610532964A CN 106198799 A CN106198799 A CN 106198799A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention discloses a kind of analysis method of PFPE relative molecular weight and its distribution, using NMR (Nuclear Magnetic Resonance) spectrum, this method identifies that the PFPE of anionic polymerization synthesis is as standard substance, being dissolved to concentration with dichloro pentafluoropropane is 10～20mg/mL, use chromatograph of gel permeation, differential refraction detector, gel chromatographic columns, flowing phase dichloro pentafluoropropane, flow velocity 0.6mL/min, column temperature is the chromatographic condition analytical standard sample one by one of 35 DEG C, make standard curve, determine standard curve equation, and measure linearly dependent coefficient, for photooxidation polymerization, PFPE molecular weight analyse prepared by photocatalysis polymerization and anionic polymerization provides effective detection method.Highly versatile of the present invention, accuracy are high, reproducible, simple to operate, can have important practical value as the enterprise-quality examination criteria of PFPE product.
Description
Technical field
The invention belongs to Analysis of Macromolecular Materials technical field, relate to a kind of gel osmoticing chromatogram analysis PFPE relative
The method of molecular weight and distribution.Can be used for the PFPE that analyzing molecules amount is 1000～8000, it is possible to as article
Enterprise-quality examination criteria.
Background technology
PFPE (Perfluoropolyether) is a kind of water white perfluoro-polymer material, only has in molecule
Tri-kinds of elements of C, F, O.Compared with hydro carbons pfpe molecule structure, PFPE instead of c h bond with C-F key, has strong electronegativity
Fluorine atom make intermolecular captivation little, there is less surface tension；C-F key makes it to the shielding action of main chain simultaneously
There is the characteristics such as the highest antioxidation, anticorrosive, radioprotective, heat-resisting and not combustion.PFPE is through end-stabilizing process
After there are the viscosity-temperature characteristics of low condensation point, low volatility and excellence, be widely used in automobile, electronics, doctor as excellent lubricant
Treat the fields such as apparatus, Aero-Space and nuclear industry.
The relative molecular mass of PFPE is one of key parameter weighing its application performance, but due to PFPE certainly
Body characteristic, needs special fluorinated organic solvent to dissolve, and boiling point is the highest, and molecular weight is mostly between 103～104Between, it is difficult to
Analyze its matter average molecular weight by mass spectrum (MS) method, often use viscosimetry, end-group analysis and nuclear magnetic resonance spectroscopy instead of.Viscous
Although degree method equipment is simple, easy to operate, but its to be confined to analyzing molecules weight range be 104～107High polymer, thus, viscosity
Method measures the molecular weight of PFPE and has bigger method error.End-group analysis is used to measure PFPE number-average molecular weight
Time, not only need to determine by other analysis means the chemical constitution of PFPE, and require the end of PFPE strand
Hold to have and be available for chemico-analytic group (such as carboxyl, ester group), high molecular PFPE indefinite for molecular structure, should
Method has bigger analytical error.Nuclear magnetic resonance spectroscopy is applicable to analyze have and determines backbone repeat unit and end-capping group
PFPE, at specified chemical displacement19The peak area ratio of F atom, can calculate the number-average molecular weight of PFPE, tool
There is higher accuracy.In actual molecular weight analyse work, anionic polymerization the PFPE being prepared from can be adopted
With nuclear magnetic resonance spectroscopy, and the PFPE that photooxidation polymerization and photocatalysis polymerization are prepared from should not use this method.
Accordingly, it would be desirable to seek more generally applicable, accurate and effective method, the relative molecular weight of PFPE is carried out detection analysis.
Summary of the invention
It is an object of the invention to provide a kind of analysis method of PFPE relative molecular weight and its distribution, in view of at present
There is no the fluoro containing polymers standard sample of commercialization, the molecular density of existing non-fluorine standard sample is not less than perfluor high polymer, and not
Easily being completely dissolved in fluorinated organic solvent, it is difficult to be applied to gel osmoticing chromatogram analysis, designing one can be to PFPE
The method that relative molecular weight and its distribution realizes analyzing.
In order to solve above-mentioned technical problem, adopt the following technical scheme that
A kind of analysis method of PFPE relative molecular weight and its distribution, it is characterised in that comprise the steps:
Step 1: the selection of PFPE standard sample and qualification；
Step 2: gel osmoticing chromatogram analysis PFPE relative molecular weight and its distribution.
After preferably, being chosen as of PFPE standard sample in step 1: select the perfluor that anionic polymerization is prepared from
Polyethers is as standard sample
After preferably, what in step 1, PFPE standard sample was identified concretely comprises the following steps:
1) PFPE standard sample is dissolved in phenyl-hexafluoride makes perfluoropolyether solution；
2) use19Perfluoropolyether solution to be measured is measured by F-nuclear magnetic resonance spectroscopy, obtains fluorine spectrum spectrogram；
3) by area normalization method process PFPE backbone repeat unit fluorine atom peak area with there is " end group fluorine "
The fluorine atom peak area of characteristic, tries to achieve the degree of polymerization according to the two peak area ratio, then is calculated perfluor by the degree of polymerization
The number-average molecular weight of polyethers, in this, as standard sample, is applied to gel osmoticing chromatogram analysis.
In the qualification of step 1 PFPE standard sample, PFPE standard sample has a following feature structure:
CF3CF2CF2O(CF(CF3)CF2O)nCF2CF3(n=1-48)；
After preferably, the concretely comprising the following steps of gel osmoticing chromatogram analysis PFPE relative molecular weight and its distribution in step 2:
1) preparation of standard sample solution
Choose respectively several equal molecular mass be the PFPE of 2130,2960,4786,5284,7276 as standard substance,
Being dissolved to concentration with dichloro pentafluoropropane is 10～20mg/mL, prepares standard sample solution；
2) making of standard curve
Using chromatograph of gel permeation, differential refraction detector, gel chromatographic columns, flowing is dichloro pentafluoropropane mutually, stream
Speed is 0.6～0.8mL/min, and column oven temperature is the chromatographic condition of 35 DEG C, the standard sample solution of above-mentioned preparation is carried out by
One analyzes, and makes standard curve, determines standard curve equation, and measure linearly dependent coefficient；Wherein gel chromatography column parameter is:
Column length 300mm, internal diameter 7.5mm, expanded polystyrene/divinylbenzene particle diameter 3 μm；
3) analysis of PFPE relative molecular weight and its distribution
Weigh appropriate PFPE sample, be dissolved in dichloro pentafluoropropane, be configured to the sample that concentration is 15～20mg/mL molten
Liquid, after waiting chromatographic balance and stability, is analyzed with above-mentioned chromatographiccondition, measures the relative of this PFPE sample
Molecular weight and distribution.
After preferably, in step 3) in gel osmoticing chromatogram analysis PFPE relative molecular weight and its distribution, perfluor to be measured
Polyethers sample can use photooxidation polymerization, photocatalysis polymerization or anionic polymerization to be prepared from, its relative molecular mass
Scope is 1000～8000.
Owing to using technique scheme, have the advantages that
The present invention is a kind of analysis method of PFPE relative molecular weight and its distribution, it is provided that a kind of gel infiltration color
The method of analysis of spectrum PFPE relative molecular weight and its distribution, this method highly versatile, accuracy are high, reproducible, operation letter
Single, can be applicable to the PFPE molecular weight that anionic polymerization, photooxidation polymerization and photocatalysis polymerization be prepared from and divide
Analysis, it is possible to as the enterprise-quality examination criteria of Related product, there is important practical value.
Accompanying drawing explanation
The invention will be further described below in conjunction with the accompanying drawings:
Fig. 1 is PFPE prepared by anionic polymerization19F-NMR spectrogram；
Fig. 2 is the standard curve of gel osmoticing chromatogram analysis PFPE；
Fig. 3 is the GPC spectrogram of gel osmoticing chromatogram analysis PFPE sample.
Detailed description of the invention
In order to make those skilled in the art be better understood from technical scheme, below in conjunction with specific embodiment and
Scheme of the present invention is described in further detail by accompanying drawing.
Embodiment
1: the qualification of PFPE standard sample
1.1 PFPE19The mensuration of F-NMR spectrogram
Take PFPE sample that a small amount of anionic polymerization is prepared from 5mm nuclear magnetic tube, dissolve with phenyl-hexafluoride, be placed in
In nuclear magnetic resonance analyser, pulse protocol zgflqn is used to measure sample solution19F-NMR spectrogram.Observing frequency 500MHz, measures temperature
Degree 298K, spectrum width 113636.367Hz, sampled data points 131072, time delay 6.50, μ s, received gain 9, and sky sweeps number of times 4
Secondary, scanning times 256 times.
1.2 PFPE19The qualification of F-NMR spectrogram F atom signal peak
19F-NMR spectrogram is after phasing, baseline correction and chemical shift correct, according to the chemistry of F atom signal peak
Shift value, coupling split point situation and peak area, and the molecular structure identifying PFPE sample is CF3CF2CF2O(CF(CF3)
CF2O)nCF2CF3.In Fig. 1, that signal center of chemical shift-146.3ppm place represents is backbone repeat unit-(CF (CF3)
CF2O)n-CF-group in-, that signal center of chemical shift-132.0ppm place represents is end group CF3CF2CF2With CF in O-3-
-the CF being connected2-group, that signal center of chemical shift-90.8ppm ,-89.7ppm place represents is end group-CF2CF3In-
CF2-、CF3-group, that signal center of chemical shift-84.1ppm place represents is end group CF3CF2CF2CF in O-3-group, changes
That signal center of displacement study-82.4ppm place represents is-the CF in backbone repeat unit2-、-CF3Group.
1.3 PFPE averages degree of polymerization and the computational methods of number-average molecular weight
The average degree of polymerization of PFPE uses area normalization method to try to achieve, and detailed description of the invention is as follows:
1) chemical shift-132.0ppm place F atom signal peak being set to end group reference peak, its parent mass peak area is A2, return
One change peak area is A2/2
2), in backbone repeat unit, fluorine atom signal peak at chemical shift-146.3ppm and-82.4ppm two is comprised, original
Peak area is respectively A1And A3, normalization peak area is
3) average degree of polymerization:
The number-average molecular weight of PFPE is tried to achieve by following formula:
Mn=166n+304
In formula, MnFor the number-average molecular weight of PFPE, n is the degree of polymerization, and 166 is backbone repeat unit hexafluoro propoxyl group
Molecular weight, 304 is end group molecular weight sum.
2, gel osmoticing chromatogram analysis PFPE relative molecular weight and its distribution
The preparation of 2.1 standard sample solution
Choosing the number-average molecular weight identified by nuclear magnetic resonance spectroscopy respectively is 2130,2960,4786,5284,7276
PFPE is as standard substance, and being dissolved to concentration with dichloro pentafluoropropane is 10～20mg/mL
2.2 instrument and equipments and the selection of chromatographiccondition
Chromatograph: Malvern Viscotek chromatograph of gel permeation
Chromatography work station: OmniSEC 4.7
Detector: differential refraction detector
Chromatographic column: Agilent PLgel MIXED-E type chromatographic column, column length 300mm, internal diameter 7.5mm, expanded polystyrene/
Divinylbenzene particle diameter 3 μm
Flowing phase: dichloro pentafluoropropane
Flow velocity: 0.6mL/min
Column temperature: 35 DEG C
The making of 2.3 standard curves
After chromatographic is stable, with above-mentioned chromatographic condition, each standard sample solution is analyzed, one by one with retention body
Long-pending V is abscissa, and the logarithmic function LogM of number-average molecular weight is vertical coordinate, produces standard curve (see accompanying drawing 2), obtains linear
Equation, linearly dependent coefficient and standard deviation.
Standard curve equation is: logM=437.02-162.34 × V+20.33 × V2-0.85124×V3, linear correlation system
Number is 0.9996, and standard deviation is 0.01095.
The analysis of 2.4 PFPE relative molecular weight and its distributions
Weighing the PFPE sample of appropriate photooxidation polymerization synthesis, be dissolved in dichloro pentafluoropropane, being configured to concentration is
The testing sample solution of 15～20mg/mL, is placed in magnetic stirring apparatus stirring 20min, treats that sample dissolves completely, by organic facies one
Secondary property syringe-driven filter filtered sample solution.After chromatographic balance and stability, it is analyzed with above-mentioned chromatographiccondition, surveys
The relative molecular mass obtaining PFPE sample is 4072.
The GPC spectrogram of PFPE sample is shown in accompanying drawing 3, and as seen from the figure, the chromatogram of PFPE sample just presents
State is distributed, and relatively small molecular weight part is also efficiently separated.
2.5 repeatability experiments
Weighing the PFPE sample of appropriate photooxidation polymerization synthesis, be dissolved in dichloro pentafluoropropane, being configured to concentration is
The testing sample solution of 15～20mg/mL, is placed in magnetic stirring apparatus stirring 20min, treats that sample dissolves completely, by organic facies one
Secondary property syringe-driven filter filtered sample solution, is respectively placed in five sample bottles (being respectively labeled as 1#, 2#, 3#, 4#, 5#), color
After spectrum system balance and stability, being analyzed with above-mentioned chromatographiccondition, concrete determination data is shown in Table 1.
Table 1 PFPE sample repeatability experimental result
Found out by table 1 data, record equal relative standard deviation RSD of number of PFPE sampleMn, the equal relative standard deviation of matter
RSDMwWith polydispersity coefficient relative standard deviation RSDPDIIt is respectively less than in gel osmoticing chromatogram analysis specification 5% required, this is described
Method is reproducible, and precision is high.
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with this
Based on bright, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done ground simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (6)
1. the analysis method of a PFPE relative molecular weight and its distribution, it is characterised in that comprise the steps:
Step 1: the selection of PFPE standard sample and qualification；
Step 2: gel osmoticing chromatogram analysis PFPE relative molecular weight and its distribution.
A kind of analysis method of PFPE relative molecular weight and its distribution, it is characterised in that: institute
State being chosen as of PFPE standard sample in step 1: select the PFPE that anionic polymerization is prepared from as standard
Sample.
A kind of analysis method of PFPE relative molecular weight and its distribution, it is characterised in that: institute
State the qualification of PFPE standard sample in step 1 to concretely comprise the following steps:
1) PFPE standard sample is dissolved in phenyl-hexafluoride makes perfluoropolyether solution；
2) use19Perfluoropolyether solution to be measured is measured by F-nuclear magnetic resonance spectroscopy, obtains fluorine spectrum spectrogram；
3) by area normalization method process PFPE backbone repeat unit fluorine atom peak area with there is " end group fluorine " characteristic
Fluorine atom peak area, try to achieve the degree of polymerization according to the two peak area ratio, then be calculated PFPE by the degree of polymerization
Number-average molecular weight, in this, as standard sample, be applied to gel osmoticing chromatogram analysis.
A kind of analysis method of PFPE relative molecular weight and its distribution, it is characterised in that: institute
Stating in the qualification of PFPE standard sample, PFPE standard sample structure is as follows: CF3CF2CF2O(CF(CF3)CF2O)nCF2CF3(n=1-48).
A kind of analysis method of PFPE relative molecular weight and its distribution, it is characterised in that: institute
State concretely comprising the following steps of gel osmoticing chromatogram analysis PFPE relative molecular weight and its distribution in step 2:
1) preparation of standard sample solution
Choose PFPE that several equal molecular mass is 2130,2960,4786,5284,7276 respectively as standard substance, with two
It is 10～20mg/mL that chlorine pentafluoropropane is dissolved to concentration, prepares standard sample solution；
2) making of standard curve
Using chromatograph of gel permeation, differential refraction detector, gel chromatographic columns, flowing is dichloro pentafluoropropane mutually, and flow velocity is
0.6～0.8mL/min, column oven temperature is the chromatographic condition of 35 DEG C, divides the standard sample solution of above-mentioned preparation one by one
Analysis, makes standard curve, determines standard curve equation, and measure linearly dependent coefficient；Wherein gel chromatography column parameter is: column length
300mm, internal diameter 7.5mm, expanded polystyrene/divinylbenzene particle diameter 3 μm；
3) analysis of PFPE relative molecular weight and its distribution
Weigh appropriate PFPE sample, be dissolved in dichloro pentafluoropropane, be configured to the sample solution that concentration is 15～20mg/mL,
After waiting chromatographic balance and stability, it is analyzed with above-mentioned chromatographiccondition, measures relatively dividing of this PFPE sample
Protonatomic mass and distribution.
A kind of analysis method of PFPE relative molecular weight and its distribution, it is characterised in that:
Described step 3) in gel osmoticing chromatogram analysis PFPE relative molecular weight and its distribution, PFPE sample can use light oxygen
Changing polymerization, photocatalysis polymerization or anionic polymerization to be prepared from, its relative molecular mass scope is 1000～8000.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107044994A (en) * | 2017-01-09 | 2017-08-15 | 南京工业大学 | Method for measuring and calculating molecular weight and distribution of crystalline polymer by using calorimetric analysis |
| CN109358084A (en) * | 2018-10-23 | 2019-02-19 | 衢州氟硅技术研究院 | A method of measurement perfluoropropylvinylether and its content of isomer |
| CN109580798A (en) * | 2017-09-29 | 2019-04-05 | 贵州中烟工业有限责任公司 | A kind of method of remaining inflating medium in detection pipe tobacco |
| CN109655480A (en) * | 2018-12-19 | 2019-04-19 | 万华化学集团股份有限公司 | A kind of assay method of polyether polyol |
| CN110068617A (en) * | 2018-01-22 | 2019-07-30 | 中昊晨光化工研究院有限公司 | With the extraordinary fluoropolymer-containing method of gel osmoticing chromatogram analysis |
| CN110389147A (en) * | 2018-04-18 | 2019-10-29 | 中昊晨光化工研究院有限公司 | A method of structure and molecular weight based on nuclear magnetic resonance measuring perfluoropolyether |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107044994A (en) * | 2017-01-09 | 2017-08-15 | 南京工业大学 | Method for measuring and calculating molecular weight and distribution of crystalline polymer by using calorimetric analysis |
| CN107044994B (en) * | 2017-01-09 | 2019-07-19 | 南京工业大学 | Method for measuring and calculating molecular weight and distribution of crystalline polymer by using calorimetric analysis |
| CN109580798A (en) * | 2017-09-29 | 2019-04-05 | 贵州中烟工业有限责任公司 | A kind of method of remaining inflating medium in detection pipe tobacco |
| CN109580798B (en) * | 2017-09-29 | 2023-04-07 | 贵州中烟工业有限责任公司 | Method for detecting residual expanding medium in cut tobacco |
| CN110068617A (en) * | 2018-01-22 | 2019-07-30 | 中昊晨光化工研究院有限公司 | With the extraordinary fluoropolymer-containing method of gel osmoticing chromatogram analysis |
| CN110389147A (en) * | 2018-04-18 | 2019-10-29 | 中昊晨光化工研究院有限公司 | A method of structure and molecular weight based on nuclear magnetic resonance measuring perfluoropolyether |
| CN109358084A (en) * | 2018-10-23 | 2019-02-19 | 衢州氟硅技术研究院 | A method of measurement perfluoropropylvinylether and its content of isomer |
| CN109358084B (en) * | 2018-10-23 | 2021-09-07 | 衢州氟硅技术研究院 | Method for measuring perfluoro-n-propyl vinyl ether and isomer content thereof |
| CN109655480A (en) * | 2018-12-19 | 2019-04-19 | 万华化学集团股份有限公司 | A kind of assay method of polyether polyol |
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Application publication date: 20161207 |