CN112485215A - Method for quantitatively analyzing ethylene content in impact-resistant polypropylene by infrared spectroscopy - Google Patents
Method for quantitatively analyzing ethylene content in impact-resistant polypropylene by infrared spectroscopy Download PDFInfo
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- CN112485215A CN112485215A CN202011259294.1A CN202011259294A CN112485215A CN 112485215 A CN112485215 A CN 112485215A CN 202011259294 A CN202011259294 A CN 202011259294A CN 112485215 A CN112485215 A CN 112485215A
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- ethylene content
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000005977 Ethylene Substances 0.000 title claims abstract description 30
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 28
- -1 polypropylene Polymers 0.000 title claims abstract description 28
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004566 IR spectroscopy Methods 0.000 title claims description 8
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 9
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 7
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 6
- 238000007731 hot pressing Methods 0.000 claims abstract description 3
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 230000008033 biological extinction Effects 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to the technical field of infrared spectrum quantitative analysis, and particularly relates to a method for measuring ethylene content in a high molecular polymer by infrared spectrum. Keeping the impact polypropylene with known ethylene content for 2min at the temperature of 175 ℃ and under the pressure of 0.5MPa by using a hot-pressing film machine to obtain a sheet with the thickness of 3 mm; carrying out infrared spectrum test on six impact resistant polypropylenes with different known ethylene contents; selecting infrared curve located at 4022.31cm‑1～4093.65cm‑1Has an average peak height of A1 and is located at 695.21cm‑1～754.14cm‑1The average peak height of (a) 2; the average peak height ratio A2/A1 is plotted on the abscissa x and the ethylene to propylene ratio of the impact polypropylene is plotted on the ordinate y. And obtaining a standard curve y which is a + bx, wherein a is the slope of the standard curve, and b is the intercept of the standard curve. The technical scheme of the invention is applied to detect the ethylene content in the impact polypropylene, the test preparation is simple, the analysis is rapid, the repetition rate is high, the contact with a solvent and radiation is not needed, and the method is environment-friendly and harmless.
Description
Technical Field
The invention belongs to the technical field of infrared spectrum quantitative analysis, and particularly relates to a method for measuring ethylene content in a high molecular polymer by infrared spectrum.
Background
The infrared spectroscopy is one of the classical chemical structure analysis and identification methods of substances, and is widely applied to the fields of scientific research and production. Infrared spectroscopy can give information on the chemical structures of functional groups, crystalline states, etc. contained in substances, reflecting the chemical structures of different substances, but in recent years infrared spectroscopy has been widely used to identify the concentrations of the components of substances.
The polypropylene is a polymer polymerized by taking propylene as a monomer and can be divided into isotactic polypropylene, syndiotactic polypropylene and atactic polypropylene, wherein the impact-resistant atactic copolymerized polypropylene is a mixture of polypropylene multiphase copolymers prepared by connecting a plurality of reactors in series, and the content of ethylene is an important control index.
The method for measuring the ethylene content comprises an infrared method, a nuclear magnetic method and a xylene soluble substance method. The nuclear magnetic method establishes a standard working curve between the absorbance ratio and the polymer composition on the basis of nuclear magnetic resonance, but nuclear magnetic equipment is expensive and harmful to human bodies; the xylene soluble substance method is characterized by large influence of manual measurement human factors, long period and harm to human bodies due to long-term exposure to toxic substances.
Disclosure of Invention
The invention mainly aims to provide a method for quantitatively analyzing the ethylene content in impact-resistant polypropylene by infrared spectroscopy, which can quickly obtain a result to meet the requirement of process control in time.
The technical scheme of the invention is as follows:
a method for quantitatively analyzing the ethylene content in impact-resistant polypropylene by infrared spectroscopy comprises the following steps:
(1) keeping the impact polypropylene with known ethylene content for 2min at the temperature of 175 ℃ and under the pressure of 0.5MPa by using a hot-pressing film machine to obtain a sheet with the thickness of 3 mm;
(2) carrying out infrared spectrum test on six impact resistant polypropylenes with different known ethylene contents;
(3) selecting an average peak height A1 of an infrared curve at 4022.31cm < -1 > to 4093.65cm < -1 > and an average peak height A2 of an infrared curve at 695.21cm < -1 > to 754.14cm < -1 >;
(4) the average peak height ratio A2/A1 is plotted on the abscissa x and the ethylene to propylene ratio of the impact polypropylene is plotted on the ordinate y. And obtaining a standard curve y which is a + bx, wherein a is the slope of the standard curve, and b is the intercept of the standard curve.
Further, a is (absorption coefficient of CH2 in propylene + absorption coefficient of CH3 in propylene)/absorption coefficient of CH2 in ethylene;
further, b is the total absorption/3 times the absorption of CH2 in ethylene;
further, the infrared spectrum test conditions are as follows: the scanning range is 4400-400/cm < -1 >, the resolution is 2cm < -1 >, and the scanning times are 32 times;
further, the sheet is wrinkled, bubble free.
The invention has the beneficial effects that:
the technical scheme of the invention is applied to detect the ethylene content in the impact polypropylene, the test preparation is simple, the analysis is rapid, the repetition rate is high, the contact with a solvent and radiation is not needed, and the method is environment-friendly and harmless.
Detailed Description
The following further describes embodiments of the present invention. It should be noted that the description of the embodiments is only for the purpose of understanding the present invention, and the present invention is not limited thereto.
Selecting the known ethylene content as 06%, 0.63%, 5.43%, 6.9%, 9.3%, 12.8% of impact-resistant polypropylene pellets were retained at 175 ℃ and 0.5MPa for 2min by a hot-press film machine to prepare sheets having a thickness of 3 mm. Selecting infrared curve located at 4022.31cm-1～4093.65cm-1Has an average peak height of A1 and is located at 695.21cm-1～754.14cm-1The average peak height of (a) 2; the average peak height ratio A2/A1 is plotted on the abscissa x and the ethylene to propylene ratio of the impact polypropylene is plotted on the ordinate y. And obtaining a standard curve y which is a + bx, wherein a is the slope of the standard curve, and b is the intercept of the standard curve. The accuracy of the curve determination result is shown in the table below, and it can be seen that the absolute errors are within ± 3%, and the accuracy can meet the analysis requirement of process control.
TABLE 1 comparison of actual values with measured value data
| Serial number | Actual value% | Found value% | Error value% |
| 1 | 0.6 | 0.61 | +0.01 |
| 2 | 0.63 | 0.64 | +0.01 |
| 3 | 5.43 | 5.61 | +0.18 |
| 4 | 6.9 | 6.62 | -0.28 |
| 5 | 9.3 | 9.64 | +0.34 |
| 6 | 12.8 | 12.91 | +0.11 |
TABLE 2 comparison of Infrared and Nuclear magnetic data
Claims (5)
1. A method for quantitatively analyzing the ethylene content in impact-resistant polypropylene by infrared spectroscopy is characterized by comprising the following steps:
(1) keeping the impact polypropylene with known ethylene content for 2min at the temperature of 175 ℃ and under the pressure of 0.5MPa by using a hot-pressing film machine to obtain a sheet with the thickness of 3 mm;
(2) carrying out infrared spectrum test on six impact resistant polypropylenes with different known ethylene contents;
(3) selecting infraredThe curve is located at 4022.31cm-1～4093.65cm-1Has an average peak height of A1 and is located at 695.21cm-1～754.14cm-1The average peak height of (a) 2;
(4) and taking the ratio A2/A1 of the average peak height as an abscissa x and the ratio of ethylene to propylene in the impact polypropylene as an ordinate y to obtain a standard curve y which is a + bx, wherein a is the slope of the standard curve and b is the intercept of the standard curve.
2. The method for infrared spectroscopic quantitative analysis of ethylene content in impact polypropylene according to claim 1, wherein the standard curve y is a + bx, wherein a is CH in propylene2Absorption coefficient and CH3Sum of extinction coefficients of (a) with CH in ethylene2The ratio of the absorption coefficients of (a).
3. The method for infrared spectroscopic quantitative analysis of ethylene content in impact polypropylene according to claim 1, wherein in the standard curve y ═ a + bx, b is the total absorption coefficient and 3 times the CH in ethylene2The ratio of the absorption coefficients of (a).
4. The method for infrared quantitative analysis of ethylene content in impact polypropylene according to claim 1, wherein the infrared spectrum is measured under the following conditions: the scanning range is 4400-400/cm-1Resolution of 2cm-1The number of scans was 32.
5. The method for infrared spectroscopic quantitative analysis of ethylene content in impact polypropylene according to claim 1, wherein the flakes are wrinkled, bubble free.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011259294.1A CN112485215A (en) | 2020-11-12 | 2020-11-12 | Method for quantitatively analyzing ethylene content in impact-resistant polypropylene by infrared spectroscopy |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011259294.1A CN112485215A (en) | 2020-11-12 | 2020-11-12 | Method for quantitatively analyzing ethylene content in impact-resistant polypropylene by infrared spectroscopy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114235735A (en) * | 2021-11-26 | 2022-03-25 | 北方华锦化学工业股份有限公司 | Method for quantitatively analyzing content of transparent agent in industrial transparent polypropylene by infrared spectroscopy |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260483A (en) * | 2000-01-24 | 2000-07-19 | 中国石化集团扬子石油化工有限责任公司 | Quick determination method for ethylene content in ethylene-propylene copolymerization of polypropylene |
| JP2002022658A (en) * | 2000-07-10 | 2002-01-23 | Sumitomo Wiring Syst Ltd | Method for analyzing ethylene-vinylacetate copolymer and ethylene-ethylacetate copolymer mixture |
| JP2002202255A (en) * | 2000-12-27 | 2002-07-19 | Sumitomo Chem Co Ltd | Infrared autoanalysis system, method of infrared autoanalysis, and device therefor |
| CN101255255A (en) * | 2007-02-28 | 2008-09-03 | 住友化学株式会社 | Polypropylene resin composition and molded article |
| CN106248612A (en) * | 2015-06-10 | 2016-12-21 | 中国石油天然气股份有限公司 | The assay method of co-monomer content in second the third fourth ternary polymerized polypropylene |
| CN107036996A (en) * | 2017-03-29 | 2017-08-11 | 神华集团有限责任公司 | The assay method of ethylene contents in COPP rubber phase |
| CN108362658A (en) * | 2018-03-07 | 2018-08-03 | 苏州艾驰博特检测科技有限公司 | Talcum powder content analysis and analysis method in a kind of polypropylene plastics |
-
2020
- 2020-11-12 CN CN202011259294.1A patent/CN112485215A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260483A (en) * | 2000-01-24 | 2000-07-19 | 中国石化集团扬子石油化工有限责任公司 | Quick determination method for ethylene content in ethylene-propylene copolymerization of polypropylene |
| JP2002022658A (en) * | 2000-07-10 | 2002-01-23 | Sumitomo Wiring Syst Ltd | Method for analyzing ethylene-vinylacetate copolymer and ethylene-ethylacetate copolymer mixture |
| JP2002202255A (en) * | 2000-12-27 | 2002-07-19 | Sumitomo Chem Co Ltd | Infrared autoanalysis system, method of infrared autoanalysis, and device therefor |
| CN101255255A (en) * | 2007-02-28 | 2008-09-03 | 住友化学株式会社 | Polypropylene resin composition and molded article |
| CN106248612A (en) * | 2015-06-10 | 2016-12-21 | 中国石油天然气股份有限公司 | The assay method of co-monomer content in second the third fourth ternary polymerized polypropylene |
| CN107036996A (en) * | 2017-03-29 | 2017-08-11 | 神华集团有限责任公司 | The assay method of ethylene contents in COPP rubber phase |
| CN108362658A (en) * | 2018-03-07 | 2018-08-03 | 苏州艾驰博特检测科技有限公司 | Talcum powder content analysis and analysis method in a kind of polypropylene plastics |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114235735A (en) * | 2021-11-26 | 2022-03-25 | 北方华锦化学工业股份有限公司 | Method for quantitatively analyzing content of transparent agent in industrial transparent polypropylene by infrared spectroscopy |
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Application publication date: 20210312 |