CN101750456B - Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F - Google Patents

Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F Download PDF

Info

Publication number
CN101750456B
CN101750456B CN2008102436274A CN200810243627A CN101750456B CN 101750456 B CN101750456 B CN 101750456B CN 2008102436274 A CN2008102436274 A CN 2008102436274A CN 200810243627 A CN200810243627 A CN 200810243627A CN 101750456 B CN101750456 B CN 101750456B
Authority
CN
China
Prior art keywords
gas
phase
phase product
electrochemical fluorination
analysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN2008102436274A
Other languages
Chinese (zh)
Other versions
CN101750456A (en
Inventor
许文林
陶勤艳
王雅琼
李建中
司宗飞
杨升
沙红霞
瞿燕芳
赵世勇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JIANGSU GUOTAI SUPER POWER NEW MATERIALS CO., LTD.
Original Assignee
Yangzhou University
Zhangjiagang Guotai Huarong New Chemical Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yangzhou University, Zhangjiagang Guotai Huarong New Chemical Materials Co Ltd filed Critical Yangzhou University
Priority to CN2008102436274A priority Critical patent/CN101750456B/en
Publication of CN101750456A publication Critical patent/CN101750456A/en
Application granted granted Critical
Publication of CN101750456B publication Critical patent/CN101750456B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention relates to an analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F, the steps of the method are as follows: (1) the gas-phase product of the CH3SO2F electrochemical fluorination is cooled and condensed, the HF in gas-phase is condensed to the HF in liquid-phase; (2) gas-liquid separation: the gas-phase product enters into the next step; (3) chemical absorption: the chemical absorbent is adopted, the acidic gas in the gas-phase product in the last step and the generated OF2 are neutralized and then are removed; (4) the gas-liquid separation: the gas-phase further enters a sampling analyzer of the gas chromatography; (5) chromatographic analysis: the gas-phase product gained at the last step enters a sample injector of the gas chromatography for analyzing and detecting, and then the relative molar percentage content of the CH3SO2F and H2 in the gas-phase product is obtained. The advantages of the invention are as follows: the operating procedure is simple, fast, the cost is low, on-site quantitative analyzing and detecting can be conducted, and the detected data is reliable.

Description

Methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product
Technical field
The present invention relates to a kind of methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product belongs to the fine chemical technology field.
Background technology
Methanesulfonyl fluoride CH 3SO 2F carries out the electrochemical fluorination reaction and generates trifluoromethyl sulfuryl fluoride CF in anhydrous hydrogen fluoride HF 3SO 2F, methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination prepares trifluoromethyl sulfuryl fluoride CF 3SO 2F is important synthetic CF 3SO 2The method of F, trifluoromethyl sulfuryl fluoride CF 3SO 2F is synthetic other fine chemistry industry fluorinated organic compound important source material, trifluoromethyl sulfuryl fluoride CF 3SO 2F is the important source material of synthetic ionic liquid, fluorine surfactant and lithium-ion electrolyte etc., is with a wide range of applications development and preparation trifluoromethyl sulfuryl fluoride CF 3SO 2The new process of F and gordian technique are to construct the important research and development field of functional form, meticulous type, the meticulous fluorine chemical product of high-level efficiency; Be with a wide range of applications, the electrochemical fluorination synthetic technology is that important organic electrochemistry fluorination technology has very important application development prospect simultaneously.
Methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is meant with CH 3SO 2F is a raw material, in HF solution, carries out the electrochemical fluorination reaction, generates principal product trifluoromethyl sulfuryl fluoride CF at anode 3SO 2F generates accessory substance hydrogen H at negative electrode 2, and because the boiling point lower (19.5 ℃) of HF and with CF 3SO 2F and H 2Leave the gas phase mixture of electrochemical fluorination reactor together with gas form together, mainly contain CF 3SO 2F, H 2And HF, because water H is arranged 2O and CH 3SO 2Bond rupture and the trace impurity that produce of F in the electrochemical fluorination process is like oxygen difluoride OF 2, carbon tetrafluoride CF 4Wait the impurity of the difficult liquefaction of some low boilings.
At CH 3SO 2In the F electrochemical fluorination process, the structure of electrochemical fluorination system, operating conditions and electrochemical reactor and electrode material etc. are all to methanesulfonyl fluoride CH 3SO 2The current efficiency of the electrochemical fluorination process of F and the selectivity of electrochemical reaction have very big influence, on-site measurement methanesulfonyl fluoride CH 3SO 2The composition of the gas-phase product of F electrochemical reactor and content are to improving methanesulfonyl fluoride CH 3SO 2The electrochemical fluorination process of F has important practical value and application prospects.But, the present analysis determining method that does not still have effective electrochemical fluorination gas-phase product.Traditional method is that the gas-phase product with electrochemical reaction carries out separation and purification or with CF 3SO 2F carries out derivatization treatment, then according to obtaining trifluoromethyl sulfuryl fluoride CF 3SO 2The amount of F, thus methanesulfonyl fluoride CH obtained 3SO 2The yield of current efficiency, selectivity and the product of F electrochemical fluorination process.The used operation steps of this method is many, and required time is long, and can only obtain the average current efficient and the average yield of electrochemical fluorination process, and reliable, the effective analysis determining method of therefore inventing the online detection of a kind of ability is insurmountable technical barrier always.
Summary of the invention
The objective of the invention is deficiency, provide the on-line analysis that a kind of operating process is simple, quick, cost is low to measure methanesulfonyl fluoride CH to prior art 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product.
The technical scheme that realizes above-mentioned purpose is: a kind of methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product, said method step is following:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid phase;
(2) solution-air is separated: will go up material that step cooling condensation obtains and carry out solution-air and separate, gas-phase product gets into next step, and liquid phase is the further recycle of hydrogen fluoride HF;
(3) chemical absorbing: adopted chemical absorbent to carry out chemical absorbing, with the sour gas in the gas-phase product in a last step and the OF of generation 2Remove after the neutralization;
(4) solution-air is separated: the material after the chemical absorbing is carried out solution-air separate, gas phase further gets in the sample introduction analyzer of gas chromatography;
(5) stratographic analysis: will go up and go on foot in the injector of the gas-phase product entering gas chromatography that obtains, and carry out assay determination, and obtain CF in the gas-phase product 3SO 2F and H 2Relative molar content.
Further, the operating conditions of first step cooling condensation is-20 ℃～0 ℃, and the operation absolute pressure is 0.1MPa～1.0MPa.
Further; The absorbing agent that is adopted in the 3rd step chemical absorbing is a carbonate aqueous solution; Used concentration is 0.1mol/L～3.0mol/L; The volume ratio of the amount of used absorbing agent and gaseous substance amount 1.0: 1.0～10.0, used operating temperature are 0 ℃～40 ℃, and used operation absolute pressure is 0.1MPa～1.0MPa.
Further, the condition that gas chromatographic analysis is measured in the 5th step stratographic analysis is: the packing material of gas phase post is a carbonaceous molecular sieve, and carrier gas is N 2, detecting device is thermal conductivity detector (TCD) TCD, and the operating temperature of gas phase analysis post is 60 ℃～120 ℃, and the operating temperature of detecting device is 60 ℃～160 ℃, CF 3SO 2F and H 2Relative molar content use area normalization method.
Further, described absorbing agent carbonate aqueous solution is NaHCO 3, Na 2CO 3, KHCO 3Or K 2CO 3In the carbonate aqueous solution any one.
Principle of work of the present invention is: according to CH 3SO 2The main composition and the character thereof of F electrochemical fluorination process gas-phase product utilize HF to be prone to and alkali compounds reaction properties and CF 3SO 2F and H 2Be insoluble in water, weak alkaline aqueous solution and difficult and alkalescent chemical reagent reaction properties, the pre-service before analyzing.And by total air flow in the gas-phase product and generation H 2Relation with contents, through measuring CF in the gas phase 3SO 2F and H 2Relative content, obtain CH 3SO 2The instantaneous current efficiency and the CF of F electrochemical fluorination process 3SO 2The selectivity of F.
The present invention adopts gas phase analysis to measure CF 3SO 2F and H 2Relative molar content usable area normalizing ratio juris be:
Realize that the main technique equipment that the present invention needs is: chemical absorbing device, gas chromatograph, detecting device TCD etc.
Adopt the benefit of technique scheme to be:
(1), operating process is simple, fast, can carry out the scene, quantitative test is measured;
(2), used analytical test reagent is simple, cost is low;
(3), measure and carry out pre-service getting into gas phase analysis, remove the HF that carries secretly in the gas-phase product, make later processing and assay determination method therefor simple;
(4), adopt carbonate aqueous solution to carry out removal of impurities, CF 3SO 2The loss amount of F is few, and determination data is reliable;
(5), adopt gas phase analysis, the expense of analytical instrument and assay determination is low; (6), adopt peak area ratio in the chromatogram as the method for quantitative test, simple, intuitive and reliable.
Description of drawings
Accompanying drawing is a process chart of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Realize that the main technique equipment that the present invention needs is: chemical absorbing device, GC-14C gas chromatograph, detecting device TCD etc.
Embodiment one
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product, said method step is following:
(1) cooling condensation: in indirect cooling heat exchanger, will mainly contain trifluoromethyl sulfuryl fluoride CF 3SO 2F, hydrogen fluoride HF and hydrogen H 2Methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the operation absolute pressure is 0.8MPa, is cooled to-9 ℃, makes the hydrogen fluoride HF in the gas phase be condensed into liquid phase;
(2) solution-air is separated: in gas-liquid separator, HF turns back to CH with liquid-phase fluorination hydrogen 3SO 2Recycle in the reaction of F electrochemical fluorination, contain trifluoromethyl sulfuryl fluoride CF 3SO 2F and hydrogen H 2Gas phase get into next step;
(3) chemical absorbing: will go up the gaseous phase materials that obtains of step through in the bubbling absorption plant, through the sodium carbonate Na of 1.0mol/L 2CO 3The WS is with the sour gas in the gas-phase product in a last step and the OF of generation 2Material after removing after the neutralization gets into next step, and the volume ratio of the amount of used absorbing agent and gaseous substance amount 1.0: 10.0, used operating temperature are 40 ℃, and used operation absolute pressure is 1.0MPa;
(4) solution-air is separated: the material after the chemical absorbing is carried out solution-air separate, gas phase further gets in the sample introduction analyzer of gas chromatography;
(5) stratographic analysis: will go up one and go on foot in the injector of the gas-phase product entering gas chromatography that obtains, and carry out assay determination, the condition of gas chromatographic analysis is that the packing material of GC-14C gas chromatograph, gas phase post is a carbonaceous molecular sieve, and carrier gas is N 2, detecting device is thermal conductivity detector (TCD) TCD, and the operating temperature of gas phase analysis post is 60 ℃, and the operating temperature of detecting device is 80 ℃, adopts area normalization method.Obtain CF in the gas-phase product 3SO 2F and H 2Relative molar content.
Embodiment two
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product, said method step is following:
(1) cooling condensation: in indirect cooling heat exchanger, will mainly contain trifluoromethyl sulfuryl fluoride CF 3SO 2F, hydrogen fluoride HF and hydrogen H 2Methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the operation absolute pressure is 0.5MPa, is cooled to-15 ℃, makes the hydrogen fluoride HF in the gas phase be condensed into liquid phase;
(2) solution-air is separated: in gas-liquid separator, HF turns back to CH with liquid-phase fluorination hydrogen 3SO 2Recycle in the reaction of F electrochemical fluorination, contain trifluoromethyl sulfuryl fluoride CF 3SO 2F and hydrogen H 2Gas phase get into next step;
(3) chemical absorbing: will go up the gaseous phase materials that obtains of step through in the bubbling absorption plant, through the soda mint NaHCO of 2.0mol/L 3The WS is with the sour gas in the gas-phase product in a last step and the OF of generation 2Material after removing after the neutralization gets into next step, and the volume ratio of the amount of used absorbing agent and gaseous substance amount 1.0: 1.0, used operating temperature are 0 ℃, and used operation absolute pressure is 0.1MPa;
(4) solution-air is separated: the material after the chemical absorbing is carried out solution-air separate, gas phase further gets in the sample introduction analyzer of gas chromatography;
(5) stratographic analysis: will go up one and go on foot in the injector of the gas-phase product entering gas chromatography that obtains, and carry out assay determination, the condition of gas chromatographic analysis is that the packing material of GC-14C gas chromatograph, gas phase post is a carbonaceous molecular sieve, and carrier gas is N 2, detecting device is thermal conductivity detector (TCD) TCD, and the operating temperature of gas phase analysis post is 80 ℃, and the operating temperature of detecting device is 100 ℃, adopts area normalization method.Obtain CF in the gas-phase product 3SO 2F and H 2Relative molar content.
Embodiment three
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product, said method step is following:
(1) cooling condensation: in indirect cooling heat exchanger, will mainly contain trifluoromethyl sulfuryl fluoride CF 3SO 2F, hydrogen fluoride HF and hydrogen H 2Methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the operation absolute pressure is 0.1MPa, is cooled to-20 ℃, makes the hydrogen fluoride HF in the gas phase be condensed into liquid phase;
(2) solution-air is separated: in gas-liquid separator, HF turns back to CH with liquid-phase fluorination hydrogen 3SO 2Recycle in the reaction of F electrochemical fluorination, contain trifluoromethyl sulfuryl fluoride CF 3SO 2F and hydrogen H 2Gas phase get into next step;
(3) chemical absorbing: will go up the gaseous phase materials that obtains of step through in the bubbling absorption plant, through the sal tartari K of 1.0mol/L 2CO 3The WS is with the sour gas in the gas-phase product in a last step and the OF of generation 2Material after removing after the neutralization gets into next step, and the volume ratio of the amount of used absorbing agent and gaseous substance amount 1.0: 5.0, used operating temperature are 20 ℃, and used operation absolute pressure is 0.5MPa;
(4) solution-air is separated: the material after the chemical absorbing is carried out solution-air separate, gas phase further gets in the sample introduction analyzer of gas chromatography;
(5) stratographic analysis: will go up one and go on foot in the injector of the gas-phase product entering gas chromatography that obtains, and carry out assay determination, the condition of gas chromatographic analysis is that the packing material of GC-14C gas chromatograph, gas phase post is a carbonaceous molecular sieve, and carrier gas is N 2, detecting device is thermal conductivity detector (TCD) TCD, and the operating temperature of gas phase analysis post is 100 ℃, and the operating temperature of detecting device is 120 ℃, adopts area normalization method.Obtain CF in the gas-phase product 3SO 2F and H 2Relative molar content.
Embodiment four
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product, said method step is following:
(1) cooling condensation: in indirect cooling heat exchanger, will mainly contain trifluoromethyl sulfuryl fluoride CF 3SO 2F, hydrogen fluoride HF and hydrogen H 2Methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the operation absolute pressure is 0.1MPa, is cooled to-20 ℃, makes the hydrogen fluoride HF in the gas phase be condensed into liquid phase;
(2) solution-air is separated: in gas-liquid separator, HF turns back to CH with liquid-phase fluorination hydrogen 3SO 2Recycle in the reaction of F electrochemical fluorination, contain trifluoromethyl sulfuryl fluoride CF 3SO 2F and hydrogen H 2Gas phase get into next step;
(3) chemical absorbing: will go up the gaseous phase materials that obtains of step through in the bubbling absorption plant, through the saleratus KHCO of 3.0mol/L 3The WS is with the sour gas in the gas-phase product in a last step and the OF of generation 2Material after removing after the neutralization gets into next step, and the volume ratio of the amount of used absorbing agent and gaseous substance amount 1.0: 3.0, used operating temperature are 10 ℃, and used operation absolute pressure is 0.3MPa;
(4) solution-air is separated: the material after the chemical absorbing is carried out solution-air separate, gas phase further gets in the sample introduction analyzer of gas chromatography;
(5) stratographic analysis: will go up one and go on foot in the injector of the gas-phase product entering gas chromatography that obtains, and carry out assay determination, the condition of gas chromatographic analysis is that the packing material of GC-14C gas chromatograph, gas phase post is a carbonaceous molecular sieve, and carrier gas is N 2, detecting device is thermal conductivity detector (TCD) TCD, and the operating temperature of gas phase analysis post is 120 ℃, and the operating temperature of detecting device is 160 ℃, adopts area normalization method.Obtain CF in the gas-phase product 3SO 2F and H 2Relative molar content.
Embodiment five
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product, said method step is following:
(1) cooling condensation: in indirect cooling heat exchanger, will mainly contain trifluoromethyl sulfuryl fluoride CF 3SO 2F, hydrogen fluoride HF and hydrogen H 2Methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the operation absolute pressure is 1.0MPa, is cooled to 0 ℃, makes the hydrogen fluoride HF in the gas phase be condensed into liquid phase;
(2) solution-air is separated: in gas-liquid separator, HF turns back to CH with liquid-phase fluorination hydrogen 3SO 2Recycle in the reaction of F electrochemical fluorination, contain trifluoromethyl sulfuryl fluoride CF 3SO 2F and hydrogen H 2Gas phase get into next step;
(3) chemical absorbing: will go up the gaseous phase materials that obtains of step through in the bubbling absorption plant, through the saleratus KHCO of 0.1mol/L 3The WS is with the sour gas in the gas-phase product in a last step and the OF of generation 2Material after removing after the neutralization gets into next step, and the volume ratio of the amount of used absorbing agent and gaseous substance amount 1.0: 8.0, used operating temperature are 30 ℃, and used operation absolute pressure is 0.8MPa;
(4) solution-air is separated: the material after the chemical absorbing is carried out solution-air separate, gas phase further gets in the sample introduction analyzer of gas chromatography;
(5) stratographic analysis: will go up one and go on foot in the injector of the gas-phase product entering gas chromatography that obtains, and carry out assay determination, the condition of gas chromatographic analysis is that the packing material of GC-14C gas chromatograph, gas phase post is a carbonaceous molecular sieve, and carrier gas is N 2, detecting device is thermal conductivity detector (TCD) TCD, and the operating temperature of gas phase analysis post is 70 ℃, and the operating temperature of detecting device is 60 ℃, adopts area normalization method.Obtain CF in the gas-phase product 3SO 2F and H 2Relative molar content.
Remove the various embodiments described above, embodiment of the present invention also have a lot, and the technical scheme that all employings are equal to or equivalence is replaced is all within protection scope of the present invention.

Claims (4)

1. methanesulfonyl fluoride CH 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product is characterized in that said method step is following:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid phase;
(2) solution-air is separated: will go up material that step cooling condensation obtains and carry out solution-air and separate, gas-phase product gets into next step, and liquid phase is the further recycle of hydrogen fluoride HF;
(3) chemical absorbing: adopted chemical absorbent to carry out chemical absorbing, with the sour gas in the gas-phase product in a last step and the OF of generation 2Remove after the neutralization;
(4) solution-air is separated: the material after the chemical absorbing is carried out solution-air separate, gas phase further gets in the sample introduction analyzer of gas chromatography;
(5) stratographic analysis: will go up and go on foot in the injector of the gas-phase product entering gas chromatography that obtains, and carry out assay determination, and obtain CF in the gas-phase product 3SO 2F and H 2Relative molar content, the condition that gas chromatographic analysis is measured in this step stratographic analysis is: the packing material of gas phase post is a carbonaceous molecular sieve, and carrier gas is N 2, detecting device is thermal conductivity detector (TCD) TCD, and the operating temperature of gas phase analysis post is 60 ℃～120 ℃, and the operating temperature of detecting device is 60 ℃～160 ℃, CF 3SO 2F and H 2Relative molar content use area normalization method.
2. methanesulfonyl fluoride CH according to claim 1 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product is characterized in that: the operating conditions of first step cooling condensation is-20 ℃～0 ℃, and the operation absolute pressure is 0.1MPa～1.0MPa.
3. methanesulfonyl fluoride CH according to claim 1 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product; It is characterized in that: the absorbing agent that is adopted in the 3rd step chemical absorbing is a carbonate aqueous solution; Used concentration is 0.1mol/L～3.0mol/L; The volume ratio of the amount of used absorbing agent and gaseous substance amount 1.0: 1.0～10.0, used operating temperature are 0 ℃～40 ℃, and used operation absolute pressure is 0.1MPa～1.0MPa.
4. methanesulfonyl fluoride CH according to claim 3 3SO 2The analysis determining method of F electrochemical fluorination gas-phase product is characterized in that: described absorbing agent carbonate aqueous solution is NaHCO 3, Na 2CO 3, KHCO 3Or K 2CO 3In the carbonate aqueous solution any one.
CN2008102436274A 2008-12-11 2008-12-11 Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F Active CN101750456B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2008102436274A CN101750456B (en) 2008-12-11 2008-12-11 Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2008102436274A CN101750456B (en) 2008-12-11 2008-12-11 Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F

Publications (2)

Publication Number Publication Date
CN101750456A CN101750456A (en) 2010-06-23
CN101750456B true CN101750456B (en) 2012-05-16

Family

ID=42477750

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2008102436274A Active CN101750456B (en) 2008-12-11 2008-12-11 Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F

Country Status (1)

Country Link
CN (1) CN101750456B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107110744A (en) * 2014-12-21 2017-08-29 山西省化工研究所（有限公司） It was found that the method for fluorochemical
CN111398481A (en) * 2020-04-22 2020-07-10 上海汽车集团股份有限公司 Analysis test method of perfluorosulfonyl fluoroolefin ether

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1106077A (en) * 1993-08-31 1995-08-02 美国3M公司 Process for preparating fluorochemicals
EP1258470A2 (en) * 2001-05-18 2002-11-20 Takasago International Corporation Process for producing optically active alcohol

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1106077A (en) * 1993-08-31 1995-08-02 美国3M公司 Process for preparating fluorochemicals
EP1258470A2 (en) * 2001-05-18 2002-11-20 Takasago International Corporation Process for producing optically active alcohol

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
NikolaiV.Ignat’ev等.Electrochemical fluorination of N,N-dimethylperfluoroacylamides.《Journal of Fluorine Chemistry》.2002,第113卷(第2期),201-205. *
NikolaiV.Ignat’ev等.ElectrochemicalfluorinationofN N-dimethylperfluoroacylamides.《Journal of Fluorine Chemistry》.2002
R.D.Howells等.Trifluoromethanesulfonic acid and derivatives.《Chemical Reviews》.1977,第77卷(第1期),69-92. *
范春雷等.三氟甲烷磺酸酐的合成研究.《有机氟工业》.2005,(第4期),6,44. *

Also Published As

Publication number Publication date
CN101750456A (en) 2010-06-23

Similar Documents

Publication Publication Date Title
CN101672775A (en) Seawater total organic carbon automatic on-line monitoring instrument
CN106289433A (en) Method for measuring volume of each component gas in secondary battery
CN101750456B (en) Analyzing and detecting method of electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F
CN104914172A (en) Method for measuring fluorine gas content in fluorine-containing mixing gas through gas chromatography method
CN108956815A (en) The test method of chloride ion content in a kind of sea sand
CN113030287B (en) Method for measuring TSED-2 in lithium ion battery electrolyte containing lithium hexafluorophosphate
CN108287157A (en) A kind of fluorine gas analysis reforming unit
CN112782306B (en) Method for detecting purity of fluorosulfonic acid
CN103472146A (en) Method for measuring content of chloridion and fluorinion in solid biomass fuel
CN201555755U (en) Device for automatically monitoring total organic carbon in seawater
CN106645499B (en) The disposable method for measuring nine kinds of halogen acetic acids in air or exhaust gas simultaneously
CN104267092A (en) Method for testing hafnium isotope by using mass spectrometer
CN102539569B (en) Detecting method of ammonia and hydrogen sulfide in wet ammonia-containing acidic gas
CN102507804B (en) Sample pre-treatment method for detecting content of chloride ions in methyl carbonate solution
CN100587487C (en) Combined detection method for high-purity SO3 gas and impurity SO2 gas therein
CN108241025B (en) A method of with the double fluorine sulfimide purity of ion-chromatographic determination
CN202837136U (en) Acid salt content analysis device
CN101477087B (en) Quantitative measuring method for trace amount of foreign gas in chlorine
CN203299029U (en) Analyzing and measuring device adopting gas absorption and reaction tube
CN116338057B (en) Detection and analysis method of difluoro sodium phosphate
Santoyo et al. Capillary electrophoretic analysis of inorganic anions in atmospheric hailstone samples
JPS6267452A (en) Apparatus for measuring organic carbon in water
CN106248845B (en) A kind of method of unsaturated aldehyde content in measure liquid phase mixture
CN209372769U (en) A kind of gas phase chromatographic device for analytical industry acetylene gaseous mixture
CN116223644A (en) Method for determining trace nitric acid in dimethyl oxalate synthesis gas

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
ASS Succession or assignment of patent right

Owner name: JIANGSU GUOTAI CHAOWEI NEW MATERIAL CO., LTD.

Free format text: FORMER OWNER: GUOTAI HUARONG CHEMICAL NEW MATERIAL CO., LTD., ZHANGJIAGANG CITY

Effective date: 20141211

Free format text: FORMER OWNER: YANGZHOU UNIVERSITY

Effective date: 20141211

C41 Transfer of patent application or patent right or utility model
COR Change of bibliographic data

Free format text: CORRECT: ADDRESS; FROM: 215633 SUZHOU, JIANGSU PROVINCE TO: 215634 SUZHOU, JIANGSU PROVINCE

TR01 Transfer of patent right

Effective date of registration: 20141211

Address after: 215634, No. 4, No. two, A, building 8, Guangdong Road, Suzhou Road, Zhangjiagang Free Trade Zone, Jiangsu, China

Patentee after: JIANGSU GUOTAI SUPER POWER NEW MATERIALS CO., LTD.

Address before: 2198 room 215633, international commodity exhibition center, Zhangjiagang Free Trade Zone, Jiangsu

Patentee before: Guotai Huarong Chemical New Material Co., Ltd., Zhangjiagang City

Patentee before: Yangzhou University