CN105548401B - A method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount - Google Patents

A method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount Download PDF

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CN105548401B
CN105548401B CN201511034875.4A CN201511034875A CN105548401B CN 105548401 B CN105548401 B CN 105548401B CN 201511034875 A CN201511034875 A CN 201511034875A CN 105548401 B CN105548401 B CN 105548401B
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hexafluoropropene
hexafluoropropylene oxide
relative amount
hexafluoropropylene
measurement
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CN105548401A (en
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闫锐
冀汝南
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Tianjin Changlu Chemical New Materials Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025Gas chromatography

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  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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Abstract

A method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount, it is related to a kind of measuring method, and in particular to a method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount.The present invention analyzes the lower problem of structural fidelity to solve existing hexafluoropropene and hexafluoropropylene oxide relative amount measuring method higher cost.Step of the invention are as follows: Step 1: the measurement of standard items purity;Step 2: establishing standard curve;Step 3: sample analysis detects;Step 4: result calculates.The invention belongs to chemical fields.

Description

A method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount
Technical field
The present invention relates to a kind of measuring methods, and in particular to a kind of measurement hexafluoropropene and hexafluoropropylene oxide relative amount Method, belong to chemical field.
Background technique
Hexafluoropropylene oxide (HFPO), also known as perfluoro propene oxid have height since it contains trifluoromethyl structure Chemical activity, be a kind of important fluoro-containing intermediate, can be used for synthesizing perfluorinated ion exchange resin, fluoroplastics, fluorubber, contain The important fluorochemicals such as fluorinated surfactant, fluorine-containing lubricating oil, advanced cleaning agent, in aerospace, electronics, medicine and other fields It is widely used.In the prior art, hexafluoropropylene oxide is substantially prepared for raw material with hexafluoropropene (HFP), due to The boiling point of both substances separates band very close to (- 29.4 DEG C of hexafluoropropene, -27.0 DEG C of hexafluoropropylene oxide), thus to the later period Carry out very big technical problem.Therefore, the relative amount for rapidly and accurately measuring hexafluoropropene and hexafluoropropylene oxide, to hexafluoro ring The evaluation and control of the synthesis condition of Ethylene Oxide are of great significance.
Summary of the invention
The present invention analyzes to solve existing hexafluoropropene and hexafluoropropylene oxide relative amount measuring method higher cost The lower problem of structural fidelity, and then propose a kind of method for measuring hexafluoropropene and hexafluoropropylene oxide relative amount.
The technical solution adopted by the present invention to solve the above problem is as follows: the specific steps of the present invention are as follows:
A method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount, a kind of measurement hexafluoropropene and six The method of fluorine propylene oxide relative amount is achieved by the steps of:
Step 1: the measurement of standard items purity: the gas Chromatographic Determination of hexafluoropropene and hexafluoropropylene oxide standard items;
Step 2: establishing standard curve: a certain amount of hexafluoropropene or hexafluoropropylene oxide gas are passed through metal vacuum Line is transferred in infrared-gas pond, reads its absorbance at selected wave number with infrared spectroscopy, wherein hexafluoropropene is selected Wave number is 1795 centimetres-1, the selected wave number of hexafluoropropylene oxide is 1550 centimetres-1, gained absorbance value and corresponding hexafluoropropene Or a standard curve can be obtained between the content of hexafluoropropylene oxide;
Step 3: sample analysis detects: accurately shifting a certain amount of hexafluoropropene and Hexafluoropropylene by metal vacuum line The mixed gas of propane measures its infrared spectrum and reads the absorbance at the wave number selected by step 2;
Step 4: result calculates: the surveyed absorbance value of step 3 is compareed with the established standard curve of step 2, it can The content of hexafluoropropene or hexafluoropropylene oxide in sample is obtained, and then the phase of hexafluoropropene with hexafluoropropylene oxide is calculated To content.
The beneficial effects of the present invention are: the 1, present invention has many advantages, such as easy to operate, experimental cost is lower;2, this hair Bright detection sample used volume is less;3, operation of the present invention is easy, is easily mastered;4, detection process of the present invention only needs infrared spectroscopy The simple instrument such as instrument, at low cost, the time is short, easy to spread.
Detailed description of the invention
Fig. 1 is the gas infrared spectrum of hexafluoropropene standard sample, and Fig. 2 is that the gas of hexafluoropropylene oxide standard sample is red Outer spectrogram, Fig. 3 are the standard relationship curve synoptic diagrams between absorbance value and the pressure of hexafluoropropene standard sample, and Fig. 4 is to inhale Standard relationship curve synoptic diagram between shading value and the pressure of hexafluoropropylene oxide standard sample, Fig. 5 are hexafluoropropene and six The gas infrared spectrum of the mixed gas of fluorine propylene oxide.
Specific embodiment
Specific embodiment 1: illustrating present embodiment, a kind of measurement hexafluoro described in present embodiment in conjunction with Fig. 1 to Fig. 5 The method of propylene and hexafluoropropylene oxide relative amount is achieved by the steps of:
Step 1: the measurement of standard items purity: the gas Chromatographic Determination of hexafluoropropene and hexafluoropropylene oxide standard items;
Step 2: establishing standard curve: a certain amount of hexafluoropropene or hexafluoropropylene oxide gas are passed through metal vacuum Line is transferred in infrared-gas pond, reads its absorbance at selected wave number with infrared spectroscopy, wherein hexafluoropropene is selected Wave number is 1795 centimetres-1, the selected wave number of hexafluoropropylene oxide is 1550 centimetres-1, gained absorbance value and corresponding hexafluoropropene Or a standard curve can be obtained between the content of hexafluoropropylene oxide;
Step 3: sample analysis detects: accurately shifting a certain amount of hexafluoropropene and Hexafluoropropylene by metal vacuum line The mixed gas of propane measures its infrared spectrum and reads the absorbance at the wave number selected by step 2;
Step 4: result calculates: the surveyed absorbance value of step 3 is compareed with the established standard curve of step 2, it can The content of hexafluoropropene or hexafluoropropylene oxide in sample is obtained, and then the phase of hexafluoropropene with hexafluoropropylene oxide is calculated To content.
Specific embodiment 2: illustrating present embodiment, a kind of measurement hexafluoro described in present embodiment in conjunction with Fig. 1 to Fig. 5 The standard of hexafluoropropene and hexafluoropropylene oxide used in the step of method of propylene and hexafluoropropylene oxide relative amount two The purity of product is all larger than 99%.Other compositions and connection relationship are same as the specific embodiment one.
Specific embodiment 3: illustrating present embodiment, a kind of measurement hexafluoro described in present embodiment in conjunction with Fig. 1 to Fig. 5 Hexafluoropropene, hexafluoropropylene oxide and hexafluoro in the step of method of propylene and hexafluoropropylene oxide relative amount two and step 3 Absorption values of the content of the mixed gas of propylene and hexafluoropropylene oxide at selected wave number are no more than 2 and are in spike.Its It is formed and connection relationship is same as the specific embodiment one.
Specific embodiment 4: illustrating present embodiment, a kind of measurement hexafluoro described in present embodiment in conjunction with Fig. 1 to Fig. 5 Hexafluoropropene, hexafluoropropylene oxide and hexafluoro in the step of method of propylene and hexafluoropropylene oxide relative amount two and step 3 Absorption values of the content of the mixed gas of propylene and hexafluoropropylene oxide at selected wave number are not less than 0.05.Other compositions And connection relationship is same as the specific embodiment one.
Specific embodiment 5: illustrating present embodiment, a kind of measurement hexafluoro described in present embodiment in conjunction with Fig. 1 to Fig. 5 In the step of method of propylene and hexafluoropropylene oxide relative amount three in the mixed gas of hexafluoropropene and hexafluoropropylene oxide The relative scale of hexafluoropropene and hexafluoropropylene oxide should be in the section of 1.4:98.6 to 96.9:3.1.Other compositions and connection are closed It is same as the specific embodiment one.
Embodiment one:
Hexafluoropropene and hexafluoro in mixed gas after the reaction directly obtained during measurement synthesis hexafluoropropylene oxide The content of propylene oxide
Step 1: the measurement of standard items purity: using gas Chromatographic Determination hexafluoropropene and hexafluoropropylene oxide standard items Purity;
Step 2: establishing standard curve: respectively will not same amount (or pressure) hexafluoropropene (or hexafluoropropylene oxide) mark Quasi- product are transferred in infrared-gas sample cell by metal vacuum line, obtain hexafluoropropene (or hexafluoropropylene oxide) standard items Infrared spectrum;According to 1795 centimetres-1The absorbance value at place and the pressure of hexafluoropropene establish standard curve, and standard curve is such as Shown in Fig. 3;According to 1550 centimetres-1The absorbance value at place and the pressure of hexafluoropropylene oxide establish standard curve, and standard is bent Line is as shown in Figure 4.
Step 3: sample measures: accurately shifting the hexafluoropropene and hexafluoro of a certain amount of (or pressure) by metal vacuum line The mixed gas (mixed gas after the reaction directly obtained during synthesis hexafluoropropylene oxide) of propylene oxide, measures it Infrared spectrum is simultaneously read at 1795 centimetres-1Locate and 1550 centimetres-1The infrared spectrum of the absorbance value at place, sample is as shown in Figure 5.
Step 4: result calculates: the surveyed absorbance value of step 3 is compareed with the established standard curve of step 2, it can The content of hexafluoropropene and hexafluoropropylene oxide in sample is obtained, and then phase of the hexafluoropropene with hexafluoropropylene oxide is calculated To content.
Step 5: measurement result is as follows: Fig. 5 is the infrared spectrum for measuring sample, it can be seen from the figure that institute's sample exists 1795 centimetres-1The absorbance value for locating (hexafluoropropene) is 1.295, at 1550 centimetres-1Locate the absorbance value of (hexafluoropropylene oxide) It is 0.861, is calculated using pressure-absorbance standard curve of hexafluoropropene and hexafluoropropylene oxide shown in Fig. 2 and Fig. 3 The content of hexafluoropropene is 17.48 millimetress of mercury out, and the content of hexafluoropropylene oxide is 14.07 millimetress of mercury, is further calculated Show that the relative scale of hexafluoropropene and hexafluoropropylene oxide is 55.4:44.6 in the mixed gas.
Embodiment two:
Measure the content of hexafluoropropene and hexafluoropropylene oxide mixed gas
Specific steps are same as Example 1.Measurement result is as follows: institute's sample is at 1795 centimetres-1Locate (hexafluoropropene) Absorbance value is 0.050, at 1550 centimetres-1The absorbance value for locating (hexafluoropropylene oxide) is 1.861, utilizes institute in Fig. 2 and Fig. 3 The content that the hexafluoropropene of display and pressure-absorbance standard curve of hexafluoropropylene oxide calculate hexafluoropropene is 0.42 milli Meter mercury column(unit of pressure), the content of hexafluoropropylene oxide are 30.41 millimetress of mercury, further calculate obtain in the mixed gas hexafluoropropene with The relative scale of hexafluoropropylene oxide is 1.4:98.6.
Embodiment three:
Measure the content of hexafluoropropene and hexafluoropropylene oxide mixed gas
Specific steps are same as Example 1.Measurement result is as follows: institute's sample is at 1795 centimetres-1Locate (hexafluoropropene) Absorbance value is 1.895, at 1550 centimetres-1The absorbance value for locating (hexafluoropropylene oxide) is 0.050, utilizes institute in Fig. 2 and Fig. 3 The content that the hexafluoropropene of display and pressure-absorbance standard curve of hexafluoropropylene oxide calculate hexafluoropropene is 25.70 The content of millimetres of mercury, hexafluoropropylene oxide is 0.82 millimetres of mercury, further calculates and obtains hexafluoropropene in the mixed gas Relative scale with hexafluoropropylene oxide is 96.9:3.1.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., is all included in the scope of protection of the present invention.

Claims (5)

1. a kind of method for measuring hexafluoropropene and hexafluoropropylene oxide relative amount, it is characterised in that: a kind of measurement six Fluoropropene and the method for hexafluoropropylene oxide relative amount are achieved by the steps of:
Step 1: the measurement of standard items purity: the gas Chromatographic Determination of hexafluoropropene and hexafluoropropylene oxide standard items;
Step 2: establishing standard curve: a certain amount of hexafluoropropene or hexafluoropropylene oxide gas are turned by metal vacuum line It moves on in infrared-gas pond, reads its absorbance at selected wave number with infrared spectroscopy, wherein the selected wave number of hexafluoropropene It is 1795 centimetres-1, the selected wave number of hexafluoropropylene oxide is 1550 centimetres-1, gained absorbance value and corresponding hexafluoropropene or six A standard curve can be obtained between the content of fluorine propylene oxide;
Step 3: sample analysis detects: accurately shifting a certain amount of hexafluoropropene and hexafluoropropylene oxide by metal vacuum line Mixed gas, measure its infrared spectrum and read the wave number selected by step 2 at absorbance;
Step 4: result calculates: the surveyed absorbance value of step 3 being compareed with the established standard curve of step 2, can be obtained The content of hexafluoropropene or hexafluoropropylene oxide in sample, and then the opposite of hexafluoropropene and hexafluoropropylene oxide is calculated and contains Amount.
2. a kind of method for measuring hexafluoropropene and hexafluoropropylene oxide relative amount, feature exist according to claim 1 In: the purity of hexafluoropropene used in step 2 and the standard items of hexafluoropropylene oxide is all larger than 99%.
3. a kind of method for measuring hexafluoropropene and hexafluoropropylene oxide relative amount, feature exist according to claim 1 In: the mixed gas of hexafluoropropene, hexafluoropropylene oxide and hexafluoropropene and hexafluoropropylene oxide in step 2 and step 3 Absorption values of the content at selected wave number are no more than 2 and are in spike.
4. a kind of method for measuring hexafluoropropene and hexafluoropropylene oxide relative amount, feature exist according to claim 1 In: the mixed gas of hexafluoropropene, hexafluoropropylene oxide and hexafluoropropene and hexafluoropropylene oxide in step 2 and step 3 Absorption values of the content at selected wave number are not less than 0.05.
5. a kind of method for measuring hexafluoropropene and hexafluoropropylene oxide relative amount, feature exist according to claim 1 In: in step 3 in the mixed gas of hexafluoropropene and hexafluoropropylene oxide hexafluoropropene and hexafluoropropylene oxide relative scale It should be in the section of 1.4:98.6 to 96.9:3.1.
CN201511034875.4A 2015-12-31 2015-12-31 A method of measurement hexafluoropropene and hexafluoropropylene oxide relative amount Expired - Fee Related CN105548401B (en)

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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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