CN114235735A - Method for quantitatively analyzing content of transparent agent in industrial transparent polypropylene by infrared spectroscopy - Google Patents
Method for quantitatively analyzing content of transparent agent in industrial transparent polypropylene by infrared spectroscopy Download PDFInfo
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- CN114235735A CN114235735A CN202111417999.6A CN202111417999A CN114235735A CN 114235735 A CN114235735 A CN 114235735A CN 202111417999 A CN202111417999 A CN 202111417999A CN 114235735 A CN114235735 A CN 114235735A
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 64
- -1 polypropylene Polymers 0.000 title claims abstract description 64
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 64
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004566 IR spectroscopy Methods 0.000 title description 7
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 20
- 238000002835 absorbance Methods 0.000 claims abstract description 11
- 239000008187 granular material Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 239000000314 lubricant Substances 0.000 claims abstract description 6
- 238000007731 hot pressing Methods 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical group [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000037303 wrinkles Effects 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 5
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000007734 materials engineering Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
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Abstract
The invention belongs to the technical field of infrared spectrum quantitative analysis, and particularly relates to a method for determining the content of a transparent agent in a transparent high-molecular polymer by using an infrared spectrum method. Blending the transparent agent, the antioxidant, the lubricant and the polypropylene material with known content at high speed, extruding and granulating by a double-screw extruder to obtain anti-reflection blending modified polypropylene granules, preparing slices with certain thickness from the anti-reflection polypropylene granules by using a hot-pressing film making machine under certain conditions, and carrying out infrared spectrum test on the transparent agent modified polypropylene material and the unmodified polypropylene material: infrared spectrograms of standard polypropylene samples with different concentrations of the transparent agent are determined according to 628cm of characteristic peak of the transparent agent‑1The linear relation between the absorbance and the concentration is established, and a standard curve is established to pass through an infrared spectrogram 628cm‑1The absorbance of (b) can be quantitatively analyzed for the clearing agent. The technical scheme of the invention is applied to the quantitative analysis of the transparent agent in the anti-reflection polypropylene for detection, and the experimental preparation is simpleThe method is convenient and fast in experimental analysis and high in repetition rate, and is a rapid and effective infrared quantitative analysis method.
Description
Technical Field
The invention belongs to the technical field of infrared spectrum quantitative analysis, and particularly relates to a method for determining the content of a transparent agent in a transparent high polymer by using an infrared spectrum method in industry.
Background
The infrared spectroscopy is one of the classic test methods for chemical structure analysis and identification, and is widely applied to scientific research and production of high molecular materials and chemical engineering. In recent years, infrared spectroscopy is widely used for concentration measurement for identifying substances and for quantitative analysis of the substances. The current methods commonly used for qualitative and quantitative analysis of substances mainly include: nuclear magnetic method, gas chromatography, liquid chromatography, ultraviolet spectroscopy, etc. Relatively speaking, the infrared spectroscopy is a relatively efficient, convenient and environment-friendly method for qualitatively and quantitatively analyzing the polymers and additives commonly used in the industry.
The polypropylene is a high molecular polymer material polymerized by taking propylene as a monomer, the polypropylene used herein is atactic polypropylene, is a mixture of polypropylene multiphase copolymers prepared by a plurality of reactors through series reaction, and the content of a transparent agent is an important control index for judging the performance of the anti-reflection polypropylene material.
The liquid chromatogram and the ultraviolet-visible spectrophotometer can carry out quantitative analysis on the liquid chromatogram and the ultraviolet-visible spectrophotometer, compared with the infrared spectrum quantitative analysis, the infrared spectrum quantitative analysis has higher efficiency and stronger safety, and the infrared spectrum analysis does not contact with a solvent, thereby conforming to the safety production standard of a chemical plant.
Disclosure of Invention
The invention aims to provide a method for measuring the content of a transparent agent in a transparent polypropylene material by infrared spectroscopy, wherein the known content is usedBlending a transparent agent, an antioxidant, a lubricant and a polypropylene material at a high speed, extruding and granulating by a double-screw extruder to obtain anti-reflection blended modified polypropylene granules, preparing slices with a certain thickness from the anti-reflection polypropylene granules by using a hot-pressing film making machine under a certain condition, and carrying out infrared spectrum test on the transparent agent modified polypropylene material and the unmodified polypropylene material: firstly, carrying out qualitative analysis on polypropylene with a clearing agent at 628cm-1Has a unique characteristic absorption peak, and the polypropylene does not absorb a vibration peak in the area, so that the transparent agent can be proved to be blended into the polypropylene; then carrying out quantitative analysis on the transparent polypropylene, and establishing a standard curve y ═ ax + b according to the linear relation between the absorbance and the concentration of the transparent agent characteristic peak 628cm < -1 > in the infrared spectrogram of the transparent agent standard polypropylene sample with different concentrations, wherein a is the slope of the standard curve and b is the intercept of the standard curve. Passing infrared spectrogram 628cm-1The absorbance of (b) can be quantitatively analyzed for the clearing agent.
The invention has the technical effects that:
the technical scheme of the invention is applied to the detection of the quantitative analysis of the transparent agent in the anti-reflection polypropylene, the experimental preparation is simple, the experimental analysis is convenient and fast, the repetition rate is high, and the method is a rapid and effective infrared quantitative analysis method.
Drawings
FIG. 1 is an infrared spectrum of an unmodified and antireflective modified polypropylene material of the invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by examples below.
The method for quantitatively analyzing the content of the transparent agent in the transparent polypropylene by the infrared spectroscopy comprises the following operation steps:
(1) blending the determined amount of the transparent agent with different concentrations with the random polypropylene, the antioxidant and the lubricant, mixing at a high speed of 2000rpm/s, and discharging after 1 minute. Polypropylene materials without a clearing agent are used as a comparison test;
(2) extruding and granulating the blend prepared in the step 1) by a double screw to obtain polypropylene granules with different concentrations of the transparent agent. Preparing a sheet with the thickness of 0.05mm by the granular materials through a plastic hot film laminating machine;
(3) carrying out infrared spectrum test on the polypropylene sheet prepared in the step 2);
(4) selecting the infrared spectrum curve 620-630cm in the step 3)-1Determine the peak at 628cm-1The peak of (A) is a characteristic peak of the clearing agent, and the clearing agent is qualitatively analyzed and blended into the polypropylene material;
(5) correcting the infrared spectrum curve of the transparent agent modified polypropylene material with different concentrations measured in the step 3), wherein the infrared spectrum curve is 2719cm-1Is a unique characteristic peak of polypropylene and is measured by 2719cm-1And the peak value of the peak is taken as a reference to be corrected, so that the error of experimental data caused by the tiny difference of the polypropylene sheets is reduced. After the curve is corrected, carrying out quantitative analysis of infrared spectrum on the polypropylene material modified by the transparent agent with different concentrations;
(6) selecting the infrared spectrum curve of the step 5) according to the length of 628cm-1Making a standard fitting curve by taking the characteristic peak absorbance peak value as an abscissa and the concentration of the clearing agent as an ordinate, and making the standard fitting curve y as ax + b, wherein a is the slope of the standard curve and b is the intercept of the standard curve by taking the characteristic peak absorbance peak value as the abscissa and the concentration of the clearing agent as the ordinate;
(7) selecting the standard fitting curve determined in the step 6), and calculating the concentration of the transparency of the sample to be measured through the standard fitting curve.
Example 1
(1) Blending transparent agent NX8000 with determined amount concentration of 0%, 0.1%, 0.2%, 0.5%, 1%, 2%, 5% with random polypropylene, antioxidant 1010, antioxidant 168, lubricant calcium stearate, mixing at 2000rpm/s at high speed, discharging after 1 minute;
(2) extruding and granulating the blend prepared in the step 1) by a double screw extruder, wherein the temperature of the double screw extruder is set with six sections of temperature parameters: obtaining polypropylene granules with different concentrations of the clearing agent at 200 ℃, 230 ℃, 220 ℃, 210 ℃. Heating the granules by a plastic hot film laminating machine at 175 ℃, under 0.5MPa and for 2min to prepare a polypropylene sheet with the thickness of 0.05 mm;
(3) performing infrared spectrum test on the polypropylene sheet prepared in the step 2), wherein the scanning range is 4400-400/cm < -1 >, the resolution is 2cm < -1 >, and the scanning times are 32 times;
(4) selecting the peak at the position of 630-1 of the infrared spectrum curve 620-containing material in the step 3), shifting the infrared spectrogram of the polypropylene material due to the addition of the transparent agent, actually, showing that the characteristic peak of the transparent agent is at the position of 620.74cm-1 from the infrared spectrogram, and qualitatively analyzing that the transparent agent is blended into the polypropylene material;
(5) correcting the infrared spectrum curve of the transparent agent modified polypropylene material with different concentrations, which is measured in the step 3), wherein the infrared spectrum curve 2719cm-1 is a unique characteristic peak of polypropylene, and the peak value at 2719cm-1 is used as a reference for correction, so that the error of experimental data caused by tiny difference of polypropylene slices is reduced. After the curve is corrected, carrying out quantitative analysis of infrared spectrum on the polypropylene material modified by the transparent agent with different concentrations;
(6) selecting the infrared spectrum curve in the step 5), taking the absorbance peak value of the characteristic peak at 620.74cm & lt-1 & gt as the abscissa, and measuring the absorbance peak value of the characteristic peak. The peak value is an abscissa X, the concentration of the added modifier is known as an ordinate Y, a standard fitting curve Y is obtained by calculation, wherein a is the slope of the standard curve, b is the intercept of the standard curve, the accuracy of the measurement result of the standard curve is as shown in the following table, the theoretical and actual calculation results are within a reasonable error range, and the accuracy can meet the analysis requirement of process control.
Table 1: comparison of theoretical and actual calculated value data
| Serial number | Theoretical value% | Actual calculated value% | Error value% |
| 1 | 0.1 | 0.11 | 0.01 |
| 2 | 0.2 | 0.23 | 0.03 |
| 3 | 0.5 | 0.49 | -0.01 |
| 4 | 1 | 0.97 | -0.03 |
| 5 | 2 | 2.21 | 0.21 |
| 6 | 5 | 4.79 | -0.21 |
As can be seen from FIG. 1, the infrared spectrogram of the unmodified and anti-reflection modified polypropylene material shows that the anti-reflection modified polypropylene material has a characteristic peak of the transparent agent at 620.74cm-1, and the blending modification of the transparent agent into the polypropylene material can be qualitatively judged.
Claims (5)
1. A method for infrared spectrum quantitative analysis of the content of a transparent agent in industrial polypropylene is characterized by comprising the following steps:
(1) blending the determined amount of the transparent agent with different concentrations with the random polypropylene, the antioxidant and the lubricant, mixing at a high speed of 2000rpm/s, discharging after 1 minute, and taking the polypropylene material without the transparent agent as a comparison test;
(2) extruding and granulating the blend prepared in the step 1) by a double-screw extruder to obtain polypropylene granules of the transparent agent with different concentrations; preparing a sheet with the thickness of 0.05mm by the granules through a plastic hot-pressing film making machine;
(3) carrying out infrared spectrum test on the polypropylene sheet prepared in the step 2);
(4) selecting the infrared spectrum curve 620-630cm in the step 3)-1Determine the peak at 628cm-1The peak of (A) is a characteristic peak of the clearing agent, and the clearing agent is qualitatively analyzed and blended into the polypropylene material;
(5) correcting the infrared spectrum curve of the transparent agent modified polypropylene material with different concentrations measured in the step 3), wherein the infrared spectrum curve is 2719cm-1Is a unique characteristic peak of polypropylene and is measured by 2719cm-1Correcting the peak value of the peak as a reference, reducing the error of experimental data caused by the tiny difference of the polypropylene sheets, and after a curve is corrected, carrying out infrared spectrum quantitative analysis on the polypropylene materials modified by the transparent agent with different concentrations;
(6) selecting the infrared spectrum curve of the step 5) according to the length of 628cm-1The absorbance peak value of the characteristic peak is an abscissa, the concentration of the clearing agent is an ordinate, a standard fitting curve y is made as ax + b, the absorbance peak value of the characteristic peak is an abscissa, the concentration of the clearing agent is an ordinate, wherein a is the slope of the standard curve, and b is the intercept of the standard curve;
(7) selecting the standard fitting curve determined in the step 6), and calculating the concentration of the transparency of the sample to be measured through the standard fitting curve.
2. The method for infrared spectrum quantitative analysis of the content of the transparent agent in the industrial polypropylene according to claim 1, wherein the transparent agent in the step 1) is Milliken NX8000, the antioxidant is 1010 antioxidant or 168 antioxidant, and the lubricant is calcium stearate.
3. The method for infrared spectrum quantitative analysis of the content of the transparent agent in the industrial polypropylene as claimed in claim 1, wherein the temperature parameters of the twin-screw extruder in the step 2) are set as follows: setting six sections of temperature parameters: 200 deg.C, 230 deg.C, 220 deg.C, 210 deg.C; the preparation conditions of the hot-pressing film making machine are as follows: the heating temperature is 175 ℃, the pressure is 0.5MPa, the film-making time is 2min, and the film has no wrinkles and no bubbles.
4. The method for infrared spectrum quantitative analysis of the content of the transparent agent in the industrial polypropylene according to claim 1, wherein the infrared spectrum test conditions in the step 3) are as follows: the scanning range is 4400--1Resolution of 2cm-1The number of scans was 32.
5. The method for infrared spectrum quantitative analysis of the content of the transparent agent in the industrial polypropylene according to claim 1, wherein the abscissa of the standard fitting curve in the step 6) is the peak value of the absorbance of the characteristic peak of the transparent agent, and the ordinate is the concentration of the transparent agent.
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| CN116087135A (en) * | 2022-11-17 | 2023-05-09 | 广东广麟材耀新能源材料有限公司 | Evaluation test method and tool for performance of inner glue of aluminum plastic film |
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