CN105548401A - Method for measuring relative content of hexafluoropropylene and relative content of hexafluoropropylene oxide - Google Patents
Method for measuring relative content of hexafluoropropylene and relative content of hexafluoropropylene oxide Download PDFInfo
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- CN105548401A CN105548401A CN201511034875.4A CN201511034875A CN105548401A CN 105548401 A CN105548401 A CN 105548401A CN 201511034875 A CN201511034875 A CN 201511034875A CN 105548401 A CN105548401 A CN 105548401A
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- hexafluoropropylene
- oxide
- hexafluoropropylene oxide
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- PGFXOWRDDHCDTE-UHFFFAOYSA-N hexafluoropropylene oxide Chemical compound FC(F)(F)C1(F)OC1(F)F PGFXOWRDDHCDTE-UHFFFAOYSA-N 0.000 title claims abstract description 80
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002835 absorbance Methods 0.000 claims description 27
- 238000002329 infrared spectrum Methods 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 8
- LLRDUIXNNHUYLY-UHFFFAOYSA-N 2,2,3,4,4,5-hexafluoro-3,5-bis(trifluoromethyl)oxolane Chemical compound FC(F)(F)C1(F)OC(F)(F)C(F)(C(F)(F)F)C1(F)F LLRDUIXNNHUYLY-UHFFFAOYSA-N 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 9
- 230000005477 standard model Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical class C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
Classifications
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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
- G01N30/02—Column chromatography
-
- 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
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
-
- 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
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- Physics & Mathematics (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)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention provides a method for measuring the relative content of hexafluoropropylene and the relative content of hexafluoropropylene oxide, relates to a measuring method, in particular to a method for measuring the relative content of hexafluoropropylene and the relative content of hexafluoropropylene oxide, and aims to solve the problems that an existing method for measuring the relative content of hexafluoropropylene and the relative content of hexafluoropropylene oxide is high in cost and low in accuracy of a analytic structure and belongs to the field of chemical engineering. The method includes the steps of 1 measuring the purity of a standard product; 2, establishing a standard curved line; 3, analyzing and detecting a sample; 4, calculating the result.
Description
Technical field
The present invention relates to a kind of assay method, be specifically related to a kind of method measuring hexafluoropropylene and hexafluoropropylene oxide relative content, belong to chemical field.
Background technology
Hexafluoropropylene oxide (HFPO), also known as perfluoro propene oxid, there is because it contains trifluoromethyl structure the chemical activity of height, it is a kind of important fluoro-containing intermediate, can be used for the important fluorochemicalss such as synthesis perfluorinated ion exchange resin, fluoroplastic, fluororubber, fluorochemical surfactant, fluorine-containing lubricating oil, senior clean-out system, be widely used in Aero-Space, electronics, medicine and other fields.In the prior art, substantially with hexafluoropropylene (HFP) for hexafluoropropylene oxide prepared by raw material, because the boiling point of these two kinds of materials is very close to (hexafluoropropylene-29.4 DEG C, hexafluoropropylene oxide-27.0 DEG C), is thus separated to the later stage and brings very large technical barrier.Therefore, measure the relative content of hexafluoropropylene and hexafluoropropylene oxide rapidly and accurately, to the evaluation of the synthesis condition of hexafluoropropylene oxide with control significant.
Summary of the invention
The present invention in order to solve existing hexafluoropropylene and hexafluoropropylene oxide relative content assay method cost is higher, the problem that analytical structure accuracy is lower, and then proposes a kind of method measuring hexafluoropropylene and hexafluoropropylene oxide relative content.
The present invention is the technical scheme taked that solves the problem: concrete steps of the present invention are as follows:
The mensuration of step one, standard items purity: the gas Chromatographic Determination of hexafluoropropylene and hexafluoropropylene oxide standard items;
Step 2, Criterion curve: a certain amount of hexafluoropropylene or hexafluoropropylene oxide gas are transferred in infrared-gas pond by metal vacuum line, read its absorbance at selected wave number place with infrared spectrum, a typical curve between the content of gained absorbance and hexafluoropropylene or hexafluoropropylene oxide, can be obtained;
Step 3, sample analysis detect: the mixed gas accurately being shifted a certain amount of hexafluoropropylene and hexafluoropropylene oxide by metal vacuum line, measure its infrared spectrum and read in the absorbance at wave number place selected by step 2;
Step 4, result calculate: contrasted with step 2 institute Criterion curve by absorbance that step 3 is surveyed, can obtain the content of hexafluoropropylene or hexafluoropropylene oxide in sample, and then calculate the relative content of hexafluoropropylene and hexafluoropropylene oxide.
The invention has the beneficial effects as follows: 1, the present invention has convenient to operation, the advantages such as experimental cost is lower; 2, to detect specimen in use volume less in the present invention; 3, the present invention easy and simple to handle, easily grasp; 4, testing process of the present invention only needs the simple instruments such as infrared spectrometer, and cost is low, and the time is short, is easy to promote.
Accompanying drawing explanation
Fig. 1 is the gas infrared spectrum of hexafluoropropylene standard model, Fig. 2 is the gas infrared spectrum of hexafluoropropylene oxide standard model, Fig. 3 is the standard relationship curve synoptic diagram between the pressure of absorbance and hexafluoropropylene standard model, Fig. 4 is the standard relationship curve synoptic diagram between the pressure of absorbance and hexafluoropropylene oxide standard model, and Fig. 5 is the gas infrared spectrum of the mixed gas of hexafluoropropylene and hexafluoropropylene oxide.
Embodiment
Embodiment one: composition graphs 1 to Fig. 5 illustrates present embodiment, described in present embodiment, a kind of method measuring hexafluoropropylene and hexafluoropropylene oxide relative content realizes as follows:
The mensuration of step one, standard items purity: the gas Chromatographic Determination of hexafluoropropylene and hexafluoropropylene oxide standard items;
Step 2, Criterion curve: a certain amount of hexafluoropropylene or hexafluoropropylene oxide gas are transferred in infrared-gas pond by metal vacuum line, read its absorbance at selected wave number place with infrared spectrum, a typical curve between the content of gained absorbance and hexafluoropropylene or hexafluoropropylene oxide, can be obtained;
Step 3, sample analysis detect: the mixed gas accurately being shifted a certain amount of hexafluoropropylene and hexafluoropropylene oxide by metal vacuum line, measure its infrared spectrum and read in the absorbance at wave number place selected by step 2;
Step 4, result calculate: contrasted with step 2 institute Criterion curve by absorbance that step 3 is surveyed, can obtain the content of hexafluoropropylene or hexafluoropropylene oxide in sample, and then calculate the relative content of hexafluoropropylene and hexafluoropropylene oxide.
Embodiment two: composition graphs 1 to Fig. 5 illustrates present embodiment, described in present embodiment, a kind of purity measuring the standard items of hexafluoropropylene used in the step 2 of the method for hexafluoropropylene and hexafluoropropylene oxide relative content and hexafluoropropylene oxide is all greater than 99%.Other composition and annexation identical with embodiment one.
Embodiment three: composition graphs 1 to Fig. 5 illustrates present embodiment, described in present embodiment a kind of measure the method for hexafluoropropylene and hexafluoropropylene oxide relative content step 2 and step 3 in the content of mixed gas of hexafluoropropylene, hexafluoropropylene oxide and hexafluoropropylene and hexafluoropropylene oxide be not more than 2 and in spike at the absorption values at selected wave number place.Other composition and annexation identical with embodiment one.
Embodiment four: composition graphs 1 to Fig. 5 illustrates present embodiment, described in present embodiment a kind of measure the method for hexafluoropropylene and hexafluoropropylene oxide relative content step 2 and step 3 in the content of mixed gas of hexafluoropropylene, hexafluoropropylene oxide and hexafluoropropylene and hexafluoropropylene oxide be not less than 0.05 at the absorption values at selected wave number place.Other composition and annexation identical with embodiment one.
Embodiment five: composition graphs 1 to Fig. 5 illustrates present embodiment, described in present embodiment, a kind of relative scale measuring hexafluoropropylene and hexafluoropropylene oxide in the mixed gas of hexafluoropropylene and hexafluoropropylene oxide in the step 3 of the method for hexafluoropropylene and hexafluoropropylene oxide relative content should in the interval of 1.4: 98.6 to 96.9: 3.1.Other composition and annexation identical with embodiment one.
Embodiment one:
Measure the content of hexafluoropropylene and hexafluoropropylene oxide in the reacted mixed gas directly obtained in synthesis hexafluoropropylene oxide process
The mensuration of step one, standard items purity: the purity using gas Chromatographic Determination hexafluoropropylene and hexafluoropropylene oxide standard items;
Step 2, Criterion curve: transfer in infrared-gas sample cell by hexafluoropropylene (or hexafluoropropylene oxide) standard items of difference amount (or pressure) by metal vacuum line respectively, obtain the infrared spectrum of hexafluoropropylene (or hexafluoropropylene oxide) standard items; According to 1795 centimetres
-1the absorbance at place and the pressure Criterion curve of hexafluoropropylene, its typical curve is as shown in Figure 3; According to 1550 centimetres
-1the absorbance at place and the pressure Criterion curve of hexafluoropropylene oxide, its typical curve as shown in Figure 4.
Step 3, sample determination: accurately shift the hexafluoropropylene of a certain amount of (or pressure) and the mixed gas (namely synthesizing in hexafluoropropylene oxide process the reacted mixed gas directly obtained) of hexafluoropropylene oxide by metal vacuum line, measure its infrared spectrum and read in 1795 centimetres
-1locate and 1550 centimetres
-1the absorbance at place, the infrared spectrum of sample as shown in Figure 5.
Step 4, result calculate: contrasted with step 2 institute Criterion curve by absorbance that step 3 is surveyed, can obtain the content of hexafluoropropylene and hexafluoropropylene oxide in sample, and then calculate the relative content of hexafluoropropylene and hexafluoropropylene oxide.
Step 5, measurement result are as follows: Fig. 5 is the infrared spectrum of working sample, and as can be seen from the figure, institute's test sample product are at 1795 centimetres
-1the absorbance at place's (hexafluoropropylene) is 1.295, at 1550 centimetres
-1the absorbance at place's (hexafluoropropylene oxide) is 0.861, the content utilizing the pressure-absorbance standard curve of hexafluoropropylene shown in Fig. 2 and Fig. 3 and hexafluoropropylene oxide to calculate hexafluoropropylene is 17.48 mm Hg, the content of hexafluoropropylene oxide is 14.07 mm Hg, and the relative scale calculating hexafluoropropylene and hexafluoropropylene oxide in this mixed gas is further 55.4: 44.6.
Embodiment two:
Measure the content of hexafluoropropylene and hexafluoropropylene oxide mixed gas
Concrete steps are identical with embodiment 1.Measurement result is as follows: institute's test sample product are at 1795 centimetres
-1the absorbance at place's (hexafluoropropylene) is 0.050, at 1550 centimetres
-1the absorbance at place's (hexafluoropropylene oxide) is 1.861, the content utilizing the pressure-absorbance standard curve of hexafluoropropylene shown in Fig. 2 and Fig. 3 and hexafluoropropylene oxide to calculate hexafluoropropylene is 0.42 mm Hg, the content of hexafluoropropylene oxide is 30.41 mm Hg, and the relative scale calculating hexafluoropropylene and hexafluoropropylene oxide in this mixed gas is further 1.4: 98.6.
Embodiment three:
Measure the content of hexafluoropropylene and hexafluoropropylene oxide mixed gas
Concrete steps are identical with embodiment 1.Measurement result is as follows: institute's test sample product are at 1795 centimetres
-1the absorbance at place's (hexafluoropropylene) is 1.895, at 1550 centimetres
-1the absorbance at place's (hexafluoropropylene oxide) is 0.050, the content utilizing the pressure-absorbance standard curve of hexafluoropropylene shown in Fig. 2 and Fig. 3 and hexafluoropropylene oxide to calculate hexafluoropropylene is 25.70 mm Hg, the content of hexafluoropropylene oxide is 0.82 mm Hg, and the relative scale calculating hexafluoropropylene and hexafluoropropylene oxide in this mixed gas is further 96.9: 3.1.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., be all included within protection scope of the present invention.
Claims (5)
1. measure a method for hexafluoropropylene and hexafluoropropylene oxide relative content, it is characterized in that: a kind of described method measuring hexafluoropropylene and hexafluoropropylene oxide relative content realizes as follows:
The mensuration of step one, standard items purity: the gas Chromatographic Determination of hexafluoropropylene and hexafluoropropylene oxide standard items;
Step 2, Criterion curve: a certain amount of hexafluoropropylene or hexafluoropropylene oxide gas are transferred in infrared-gas pond by metal vacuum line, read its absorbance at selected wave number place with infrared spectrum, a typical curve between the content of gained absorbance and hexafluoropropylene or hexafluoropropylene oxide, can be obtained;
Step 3, sample analysis detect: the mixed gas accurately being shifted a certain amount of hexafluoropropylene and hexafluoropropylene oxide by metal vacuum line, measure its infrared spectrum and read in the absorbance at wave number place selected by step 2;
Step 4, result calculate: contrasted with step 2 institute Criterion curve by absorbance that step 3 is surveyed, can obtain the content of hexafluoropropylene or hexafluoropropylene oxide in sample, and then calculate the relative content of hexafluoropropylene and hexafluoropropylene oxide.
2. a kind of method measuring hexafluoropropylene and hexafluoropropylene oxide relative content according to claim 1, is characterized in that: the purity of hexafluoropropylene used in step 2 and the standard items of hexafluoropropylene oxide is all greater than 99%.
3. a kind of method measuring hexafluoropropylene and hexafluoropropylene oxide relative content according to claim 1, is characterized in that: in step 2 and step 3, the content of the mixed gas of hexafluoropropylene, hexafluoropropylene oxide and hexafluoropropylene and hexafluoropropylene oxide is not more than 2 and in spike at the absorption values at selected wave number place.
4. a kind of method measuring hexafluoropropylene and hexafluoropropylene oxide relative content according to claim 1, is characterized in that: in step 2 and step 3, the content of the mixed gas of hexafluoropropylene, hexafluoropropylene oxide and hexafluoropropylene and hexafluoropropylene oxide is not less than 0.05 at the absorption values at selected wave number place.
5. a kind of method measuring hexafluoropropylene and hexafluoropropylene oxide relative content according to claim 1, is characterized in that: in step 3 hexafluoropropylene and hexafluoropropylene oxide mixed gas in the relative scale of hexafluoropropylene and hexafluoropropylene oxide should in the interval of 1.4:98.6 to 96.9:3.1.
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| CN201511034875.4A CN105548401B (en) | 2015-12-31 | 2015-12-31 | A method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044475A (en) * | 2019-12-19 | 2020-04-21 | 天津市长芦化工新材料有限公司 | Method for measuring relative content of hexafluoropropylene oxide and hexafluoroacetone |
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| CN1049661A (en) * | 1989-08-25 | 1991-03-06 | 纳幕尔杜邦公司 | The three-phase liquid phase epoxidation method of perfluoroolefine class |
| CN1512962A (en) * | 2001-06-05 | 2004-07-14 | ͬ�Ϳ�ҵ��ʽ���� | Method of separating acid |
| CN102140057A (en) * | 2010-01-28 | 2011-08-03 | 中国中化股份有限公司 | Method for preparing hexafluoroacetone |
| CN102731441A (en) * | 2011-03-31 | 2012-10-17 | 大金工业株式会社 | Method for cleaning hexafluoropropylene oxide |
| CN102822155A (en) * | 2010-03-29 | 2012-12-12 | 大金工业株式会社 | Method for producing carbonyl fluoride and hexafluoropropylene oxide |
-
2015
- 2015-12-31 CN CN201511034875.4A patent/CN105548401B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049661A (en) * | 1989-08-25 | 1991-03-06 | 纳幕尔杜邦公司 | The three-phase liquid phase epoxidation method of perfluoroolefine class |
| CN1512962A (en) * | 2001-06-05 | 2004-07-14 | ͬ�Ϳ�ҵ��ʽ���� | Method of separating acid |
| CN102140057A (en) * | 2010-01-28 | 2011-08-03 | 中国中化股份有限公司 | Method for preparing hexafluoroacetone |
| CN102822155A (en) * | 2010-03-29 | 2012-12-12 | 大金工业株式会社 | Method for producing carbonyl fluoride and hexafluoropropylene oxide |
| CN102731441A (en) * | 2011-03-31 | 2012-10-17 | 大金工业株式会社 | Method for cleaning hexafluoropropylene oxide |
Non-Patent Citations (4)
| Title |
|---|
| LABELLE, CB; KARECKI, SM; REIF, R: "Fourier transform infrared spectroscopy of effluents from pulsed plasmas of 1,1,2,2-tetrafluoroethane, hexafluoropropylene oxide, and difluoromethane", 《JOURNAL OF VACUUM SCIENCE & TECHNOLOGY A-VACUUM SURFACES AND FILMS》 * |
| WROBLEWSKA, AGNIESZKA; MILCHERT, EUGENIUSZ; MEISSNER, EGBERT: "Oxidation of Hexafluoropropylene with Oxygen to Hexafluoropropylene Oxide", 《ORGANIC PROCESS RESEARCH & DEVELOPMENT》 * |
| 曾昌华: "六氟环氧丙烷及六氟丙酮的色谱分析方法研究", 《有机氟工业》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044475A (en) * | 2019-12-19 | 2020-04-21 | 天津市长芦化工新材料有限公司 | Method for measuring relative content of hexafluoropropylene oxide and hexafluoroacetone |
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