CN102351636A - Novel technology for preparing pentafluoroethyl iodide by one-step method - Google Patents
Novel technology for preparing pentafluoroethyl iodide by one-step method Download PDFInfo
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- CN102351636A CN102351636A CN2011102466801A CN201110246680A CN102351636A CN 102351636 A CN102351636 A CN 102351636A CN 2011102466801 A CN2011102466801 A CN 2011102466801A CN 201110246680 A CN201110246680 A CN 201110246680A CN 102351636 A CN102351636 A CN 102351636A
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Abstract
A novel technology for preparing pentafluoroethyl iodide by a one-step method. By the adoption of a multiple-stage tower reactor series connection process flow (N is greater than or equal to 2 upon the process requirements), an iodine pentafluoride solution, a gas mixture of perfluoroalkyl sulfonyl fluoride and fluorine nitrogen and tetrafluoroethene respectively enter into the multiple-stage tower reactor from two ends and countercurrently flow for reaction. The invention has the following advantages: fluorine gas, iodine and tetrafluoroethene are used as raw materials to react so as to synthesize pentafluoroethyl iodide in one step; the newborn iodine pentafluoride in the invention has high activity and can perform a mild reaction at the temperature of 60-65 DEG C; the catalyst perfluoroalkyl sulfonyl fluoride can be used as a catalyst and a surfactant to raise the reaction rate and the yield; two iodine-eroded grooves and a tail gas absorbing tower cooperate and are alternatively used to make the reaction continuously automated; unreacted fluorine gas can be adsorbed by active alumina and then recovered and reused; the technological equipment and parts, which are made from regular steel, undergo a pock-free electroless nickel plating treatment and a fluorine passivation treatment, so as to prevent the damage of corrosive chemicals to the equipment, reduce the investment cost and benefit for industrialization.
Description
Technical field
The invention belongs to single stage method and prepare the novel process of PFEI, be specifically related to a kind of with iodine, fluorine gas, tetrafluoroethylene be raw material, be solvent with the iodine pentafluoride, the gas-liquid counter current reaction under the perfluoroalkyl sulfonyl fluoride atmosphere, in the reaction of high order tower, carried out continuously.
Background technology
PFEI is the important source material of synthesizing perfluoroalkyl iodide, is mainly used in the initial telogen of producing perfluoroalkyl iodides, also can be used for producing fluorine-containing fine chemicals such as fluorine-containing medicines midbody.As the midbody of building-up reactions purposes is widely arranged with PFEI derived product full-fluorine alkyl iodide; Like fluorochemical surfactant, fluorine finishing composition etc.; Use very extensively; Along with the increasing of industrialization, raw-material pulling function is strengthened day by day, therefore the research to the PFEI suitability for industrialized production has important practical sense.
Prepare C in the past
2F
5The I great majority adopt IF
5, tetrafluoroethylene, iodine be synthetic under the katalysis of metal fluoride, the PFEI of production is discharged by the bubble-plate column top with gas form, in the condensing surface in downstream, liquefying is stored in the container.This method flow process is short, and the required reaction times is few, and product purity and yield are high, and the three wastes are few, temperature of reaction, pressure range broad, and processing ease, but the purity of iodine pentafluoride is bigger to the reaction influence.Used raw material iodine and iodine pentafluoride in the reaction, strongly-acid is very big to the corrodibility of reaction medium, and this has relatively high expectations to reaction unit, and the method that generally adopts stainless steel to add coating solves corrosion problems.Control also can effectively reduce the corrosion of reactant to device than low reaction temperatures.The production technique of most of company all adopts this method now.
With the iodine pentafluoride is in the technology of fluorizating agent, the difficult control of the quality of iodine pentafluoride, and this directly has influence on the yield of PFEI.(WO9504020) replaced IF with ICl and HF
5, this method raw material is easy to get, and yield is higher, but the reaction times is long, is unfavorable for suitability for industrialized production.
Can also adopt 1,2-diiodo-Tetrafluoroethane (CF
2ICF
2I) with iodine pentafluoride or hydrofluoric mixture reaction, adding Nb is or oxygen acid catalyzer (H
5IO
6, NaClO
3Or SO
2Cl
2Deng), under certain reaction conditions, just can obtain the PFEI of certain productive rate.But this method has significant disadvantages: 1, and 2-diiodo-Tetrafluoroethane (CF
2ICF
2I), iodine pentafluoride, hydrogen fluoride etc. all are toxic substances, wherein 1,2-diiodo-Tetrafluoroethane toxicity is still indeterminate both at home and abroad, acute suction belongs to hypertoxic type, the operation protection is important.And contain oxygen halate or halate, have unstable, misoperation in the reaction process sets off an explosion easily.
French Atofina company had applied for a patent about novel synthetic PFEI (2794465) in 2000, was about to pentafluoride ethane (C
2F
5H) and I
2The mixed gas of forming, the basic metal of flowing through (alkaline earth salt/carrier) catalyst layer, reaction can obtain C under its catalysis
2F
5I, CF
3Gaseous mixtures such as I.This method selection rate and yield are wayward, and its carrier employing activated carbon, have easy oxidation of support of the catalyst or carbon distribution problem, are unfavorable for suitability for industrialized production.
Summary of the invention
The objective of the invention is to overcome the defective of above patent, adopt fluorine gas, iodine, tetrafluoroethylene direct reaction, but design provides a kind of mild condition operate continuously, also a step prepares the method for PFEI.
Single stage method of the present invention prepares the novel process of PFEI, adopts multistage tower reactor series process flow, and according to arts demand, the tower number can be 1～N level, N>=2; Iodine solution (iodine pentafluoride is done solvent cycle and used), a small amount of perfluoroalkyl sulfonyl fluoride R
fSO
2F (uses R as catalyst recirculation
fRepresent perfluoroalkyl chain, carbonatoms is 1～12) countercurrent flow of entering reaction of high order tower reacts from two ends respectively with fluorine nitrogen mixed gas, tetrafluoroethylene gas.The heat that produces in heat that absorbs when dissolving iodine and the reaction is taken out of through the condensing surface between each tower; Between reaction tower and the condensing surface with U type pipe coupling; U type liquid sealing pipe the inside is full of iodine solution during reaction, thereby has avoided fluorine gas to get into the iodine solution pipeline, reaches the effect that prevents the pipeline short circuit.Iodine solution concentration reduces step by step; Concentration of fluorine and tetrafluoroethylene concentration are reverse to be reduced step by step; And the flow of iodine solution concentration, fluorine nitrogen mixed gas ratio, tetrafluoroethylene can be according to temperature of reaction interlock regulation and control in reaction process, with control reaction temperature between 60～65 ℃.
Iodine pentafluoride in the said groove can flow into through recycle pump and dissolve the iodine groove.
Said perfluoroalkyl sulfonyl fluoride R
fSO
2The amount of F is 0.1～1 ‰, as catalyzer, uses repeatedly through recycle pump with iodine pentafluoride solution.
Said perfluoroalkyl sulfonyl fluoride R
fSO
2The amount of F is 0.1～1 ‰ of iodine pentafluoride solution and a perfluoroalkyl sulfonyl fluoride total amount (the total amount here refers to weight unit), as catalyzer.
Said iodine solution concentration can be through iodine pentafluoride internal circulating load and temperature of reaction interlock regulation and control, and scope is 5～20% of a solution.
Said fluorine nitrogen mixing ratio can be through the temperature of reaction regulation and control that link, and wherein concentration of fluorine is 10～98% of a gas gross.
Ratio＜1/0.6 (mol ratio) of the fluorine gas inlet in said tetrafluoroethylene gas inlet and the fluorine nitrogen mixed gas, promptly fluorine gas be about excessive.
Interlock recited above regulation and control are exactly to how much the regulating and control of added thing, and avoid temperature too high.
Single stage method of the present invention prepares the novel process of PFEI, and concrete steps are following:
(1) before the driving, adding part iodine pentafluoride is subsequent use in E-8 in advance, valve-off V-5, V-15, V-7, V-8, V-14, V-18; All the other valves are all opened; Charge into nitrogen through pipeline P-23 and P-25, valve-off V-6, V-9 again open valve V-7, V-8 finds time; Circulation repeatedly to get rid of air and the aqueous vapor in the total system, is closed all valves then;
(2) Open valve V-1, V-2, V-10, V-11 through recycle pump E-9, make to dissolve in iodine groove and the U type pipe to be filled with iodine pentafluoride, then valve-off V-2, V-11;
(3) Open valve V-5 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-1, closes then; Heating E-1 to 60～65 ℃, and stir, treat that iodine wherein is dissolved in the iodine pentafluoride fully; Open valve V-6 closes after charging into nitrogen, and Open valve V-7 closes after finding time, and the program of finding time that so circulates three times is opened equilibrium valve V-16, makes the total system pressure equilibrium;
(4) the Open valve V-1 iodine pentafluoride solution that is dissolved with iodine gets into E-3 through condensing surface E-10 successively, gets into E-4 through condensing surface E-11, gets into E-8 through condensing surface E-13; Be 25 ℃ water in the condensing surface, the heat that reaction is produced was pulled away before getting into reaction towers at different levels;
(5) meanwhile, Open valve V-13, V-19 make fluorine nitrogen mixed gas and tetrafluoroethylene gas successively through E-4, E-3, with the iodine solution countercurrent flow, have reacted the back and have got into aluminium sesquioxide adsorption tower E-6 and E-7; Iodine solution concentration reduces from E-3, E-4, E-5 successively, and concentration of fluorine reduces from E-5, E-4, E-3 successively;
(6) in reaction process, control reaction temperature is between 60 ℃～65 ℃; If the temperature in the E-3 is too high, can be according to practical situation, Open valve V-12 adds iodine pentafluoride to reduce the concentration of iodine solution through recycle pump E-9, and the concentration range of iodine solution can be 5～20%; If the temperature in the E-5 is too high, can reduce the flow of fluorine gas and tetrafluoroethylene simultaneously according to practical situation, be reflected in the reaction towers at different levels gentleness with assurance and carry out.And adopt U type pipe between reaction towers at different levels and the condensing surface, avoid the flow process short circuit;
(7) raw material is in reaction among the E-1, and Open valve V-15 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-2, close then; Heating E-2 to 60～65 ℃, and stir, treat that iodine wherein is dissolved in the iodine pentafluoride fully; Open valve V-9 closes after charging into nitrogen, and Open valve V-8 closes after finding time, and the program of finding time so circulates three times; Raw material among the E-2 is in stand-by state; After waiting to dissolve iodine solution among the iodine groove E-1 and being exhausted, valve-off V-1, V-16, Open valve V-2, V-17 so that reaction carry out continuously;
Open valve V-3 when (8) reacting, the fluorine gas that nitrogen, unreacted finish, the C of generation
2F
5I gas E-14 (about 25 ℃) behind condensing surface gets into adsorption tower E-6, and all the other materials get into E-3 through condensing reflux; Fill active A l among E-6 and the E-7
2O
3To absorb the intact fluorine gas of a small amount of unreacted, C
2F
5I passes through condensing surface E-12 (about 0 ℃) again and gets into groove through pipeline P-31; Nitrogen is discharged through vacuum breaker V-18, and E-6 and E-7 can be used alternatingly to guarantee the continuity of preparation PFEI;
(9) the iodine liquid of iodine pentafluoride and perfluoroalkyl sulfonyl fluoride flow out to the iodine pentafluoride groove E-8 from E-4, can return again through valve V-12 and recycle pump E-9 and dissolve in the iodine groove.
(10) Open valve V-14 makes C
2F
5The thick product of I gets into finishing sequence; Purify through fractionated mode, collect 12.5～13 ℃ positive cut.
The advantage that single stage method of the present invention prepares the PFEI novel process is: reaction is a raw material one-step synthesis PFEI from fluorine gas, iodine, tetrafluoroethylene, has both saved the energy, has saved the investment to midbody iodine pentafluoride production plant to a greater extent.Producing PFEI in the previous patent reacts under 95 ℃ high temperature usually; Because the boiling point of this temperature and iodine pentafluoride is very approaching, in case temperature control is accidentally, the iodine pentafluoride gasification; Very easily take a large amount of iodine pentafluoride steams out of, not only caused waste but also increased the difficulty of cut.The a small amount of perfluoroalkyl sulfonyl fluoride that adds in this law not only can be as catalyst, and itself is as tensio-active agent, and the effect that reduces solution surface tension and dispersion moistening is arranged, and makes gas-liquid mass transfer reach best effect, helps improving speed of reaction and productive rate.Among the present invention, newborn iodine pentafluoride activity is higher, can under 60～65 ℃ of conditions, react PFEI with the tetrafluoroethylene gentleness.Two molten iodine grooves and two tail gas absorbers cooperations are used alternatingly and help reacting continuous and automatic.Because fluorine gas is excessive, do not have remaining tetrafluoroethylene monomer in the tail gas, the intact fluorine gas of unreacted can be through active aluminium sesquioxide absorption, and the three wastes are beneficial to improvement.This processing unit and parts adopt common iron, and no pit chemical nickel plating is handled and carried out the fluorine gas Passivation Treatment again, not only can effectively prevent the damage of eroding chemical to equipment, and reduce cost of investment, is beneficial to industrialization.
Description of drawings
Fig. 1 prepares the process route chart of PFEI for single stage method.
Wherein: E-1, E-2 dissolve iodine groove E-3 first order reaction tower E-4 second order reaction tower
E-5 fluorine iodoethane groove E-6, E-7 adsorption tower E-8 iodine pentafluoride groove
E-9 recycle pump E-10～E-14 condensing surface V-1～V-19 valve
P-29～P-31U type pipe.
Embodiment
According to shown in Figure 1, single stage method of the present invention prepares the novel process of PFEI, adopts multistage tower reactor series process flow, and according to arts demand, the tower number can be 1～N level, N >=2; Iodine solution (iodine pentafluoride is made solvent), perfluoroalkyl sulfonyl fluoride and fluorine nitrogen mixed gas, tetrafluoroethylene gas get into the countercurrent flow of reaction of high order tower respectively and react from two ends.The heat that produces in heat that absorbs when dissolving iodine and the reaction is taken out of through the condensing surface between each tower; Between reaction tower and the condensing surface with U type pipe coupling; U type liquid sealing pipe the inside is full of iodine solution during reaction, thereby has avoided fluorine gas to get into the iodine solution pipeline, reaches the effect that prevents the pipeline short circuit.Iodine solution concentration reduces step by step; Concentration of fluorine and tetrafluoroethylene concentration are reverse to be reduced step by step; And the flow of iodine solution concentration, fluorine nitrogen mixed gas ratio, tetrafluoroethylene can be according to temperature of reaction interlock regulation and control in reaction process, with control reaction temperature between 60～65 ℃.
Iodine pentafluoride in the said groove can flow into through recycle pump and dissolve the iodine groove.
Said perfluoroalkyl sulfonyl fluoride R
fSO
2The amount of F is 0.1～1 ‰, as catalyzer, uses repeatedly through recycle pump with iodine pentafluoride solution.
Said iodine solution concentration can be through iodine pentafluoride internal circulating load and temperature of reaction interlock regulation and control, and scope is 5～20% of a solution.
Said fluorine nitrogen mixing ratio can be through the temperature of reaction regulation and control that link, and wherein concentration of fluorine is 10～98% of a gas gross.
Ratio＜1/0.6 (mol ratio) of said tetrafluoroethylene gas inlet and fluorine gas inlet, promptly fluorine gas be about excessive.
Single stage method of the present invention prepares the novel process of PFEI, and concrete steps are following:
(1) before the driving, adding part iodine pentafluoride is subsequent use in E-8 in advance, valve-off V-5, V-15, V-7, V-8, V-14, V-18; All the other valves are all opened; Charge into nitrogen through pipeline P-23 and P-25, valve-off V-6, V-9 again open valve V-7, V-8 finds time; Circulation repeatedly to get rid of air and the aqueous vapor in the total system, is closed all valves then;
(2) Open valve V-1, V-2, V-10, V-11 through recycle pump E-9, make to dissolve in iodine groove and the U type pipe to be filled with iodine pentafluoride, then valve-off V-2, V-11;
(3) Open valve V-5 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-1, closes then; Heating E-1 to 60～65 ℃, and stir, treat that iodine wherein is dissolved in the iodine pentafluoride fully; Open valve V-6 closes after charging into nitrogen, and Open valve V-7 closes after finding time, and the program of finding time that so circulates three times is opened equilibrium valve V-16, makes the total system pressure equilibrium;
(4) Open valve V-1, the iodine pentafluoride solution that is dissolved with iodine gets into E-3 through condensing surface E-10 successively, gets into E-4 through condensing surface E-11, gets into E-8 through condensing surface E-13; Be 25 ℃ water in the condensing surface, the heat that reaction is produced was pulled away before getting into reaction towers at different levels;
(5) meanwhile, Open valve V-13, V-19 make fluorine nitrogen mixed gas and tetrafluoroethylene gas successively through E-4, E-3, with the iodine solution countercurrent flow, have reacted the back and have got into aluminium sesquioxide adsorption tower E-6 and E-7; Iodine solution concentration reduces from E-3, E-4, E-5 successively, and concentration of fluorine reduces from E-5, E-4, E-3 successively;
(6) in reaction process, control reaction temperature is between 60 ℃～65 ℃; If the temperature in the E-3 is too high, can be according to practical situation, Open valve V-12 adds iodine pentafluoride to reduce the concentration of iodine solution through recycle pump E-9, and the concentration range of iodine solution can be 5～20%; If the temperature in the E-5 is too high, can reduce the flow of fluorine gas and tetrafluoroethylene simultaneously according to practical situation, be reflected in the reaction towers at different levels gentleness with assurance and carry out.And adopt U type pipe between reaction towers at different levels and the condensing surface, avoid the flow process short circuit;
(7) raw material is in reaction among the E-1, and Open valve V-15 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-2, close then; Heating E-2 to 60～65 ℃, and stir, treat that iodine wherein is dissolved in the iodine pentafluoride fully; Open valve V-9 closes after charging into nitrogen, and Open valve V-8 closes after finding time, and the program of finding time so circulates three times; Raw material among the E-2 is in stand-by state; After waiting to dissolve iodine solution among the iodine groove E-1 and being exhausted, valve-off V-1, V-16, Open valve V-2, V-17 so that reaction carry out continuously;
Open valve V-3 when (8) reacting, the fluorine gas that nitrogen, unreacted finish, the C of generation
2F
5I gas E-14 (about 25 ℃) behind condensing surface gets into adsorption tower E-6, and all the other materials get into E-3 through condensing reflux; Fill active A l among E-6 and the E-7
2O
3To absorb the intact fluorine gas of a small amount of unreacted, C
2F
5I passes through condensing surface E-12 (about 0 ℃) again and gets into groove through pipeline P-31; Nitrogen is discharged through vacuum breaker V-18, and E-6 and E-7 can be used alternatingly to guarantee the continuity of preparation PFEI;
(9) the iodine liquid of iodine pentafluoride and perfluoroalkyl sulfonyl fluoride flow out to the iodine pentafluoride groove E-8 from E-4, can return again through valve V-12 and recycle pump E-9 and dissolve in the iodine groove;
(10) Open valve V-14 makes C
2F
5The thick product of I gets into finishing sequence; Purify through fractionated mode, collect 12.5～13 ℃ positive cut.
Be not limited to the foregoing description, a plurality of embodiment arranged according to the difference of the addition of reactant in the method steps.
Claims (8)
1. single stage method prepares the novel process of PFEI; It is characterized in that: adopt multistage tower reactor series process flow, the iodine pentafluoride solution of iodine, perfluoroalkyl sulfonyl fluoride and fluorine nitrogen mixed gas, tetrafluoroethylene get into the countercurrent flow of reaction of high order tower respectively and react from two ends.
2. single stage method according to claim 1 prepares the novel process of PFEI, it is characterized in that: said perfluoroalkyl sulfonyl fluoride R
fSO
2The amount of F is 0.1～1 ‰ of iodine pentafluoride solution and a perfluoroalkyl sulfonyl fluoride total amount, as catalyzer.
3. single stage method according to claim 1 prepares the novel process of PFEI, it is characterized in that: said iodine solution concentration can be through iodine pentafluoride internal circulating load and temperature of reaction interlock regulation and control, and scope is 5～20% of a solution.
4. single stage method according to claim 1 prepares the novel process of PFEI, it is characterized in that: said fluorine nitrogen mixing ratio can be through the temperature of reaction regulation and control that link, and wherein concentration of fluorine is 10～98% of a fluorine nitrogen mixed gas total amount.
5. single stage method according to claim 1 prepares the novel process of PFEI, it is characterized in that: ratio＜1/0.6 (mol ratio) of the fluorine gas inlet in said tetrafluoroethylene gas inlet and the fluorine nitrogen mixed gas, promptly fluorine gas be about excessive.
6. single stage method according to claim 1 prepares the novel process of PFEI; It is characterized in that: the flow of iodine solution concentration, fluorine nitrogen mixed gas ratio, tetrafluoroethylene can be according to temperature of reaction interlock regulation and control in reaction process, with control reaction temperature between 60～65 ℃.
7. single stage method according to claim 1 prepares the novel process of PFEI, it is characterized in that: concrete steps are following:
(1) before the driving, adding part iodine pentafluoride is subsequent use in E-8 in advance, valve-off V-5, V-15, V-7, V-8, V-14, V-18; All the other valves are all opened; Charge into nitrogen through pipeline P-23 and P-25, valve-off V-6, V-9 again open valve V-7, V-8 finds time; Circulation repeatedly to get rid of air and the aqueous vapor in the total system, is closed all valves then;
(2) Open valve V-1, V-2, V-10, V-11 through recycle pump E-9, make to dissolve in iodine groove and the U type pipe to be filled with iodine pentafluoride, then valve-off V-2, V-11;
(3) Open valve V-5 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-1, closes then; Heating E-1 to 60～65 ℃, and stir, treat that iodine wherein is dissolved in the iodine pentafluoride fully; Open valve V-6 closes after charging into nitrogen, and Open valve V-7 closes after finding time, and the program of finding time that so circulates three times is opened equilibrium valve V-16, makes the total system pressure equilibrium;
(4) Open valve V-1, the iodine pentafluoride solution that is dissolved with iodine gets into E-3 through condensing surface E-10 successively, gets into E-4 through condensing surface E-11, gets into E-8 through condensing surface E-13; Be 25 ℃ water in the condensing surface, the heat that reaction is produced was pulled away before getting into reaction towers at different levels;
(5) meanwhile, Open valve V-13, V-19 make fluorine nitrogen mixed gas and tetrafluoroethylene gas successively through E-4, E-3, with the iodine solution countercurrent flow, have reacted the back and have got into aluminium sesquioxide adsorption tower E-6 and E-7; Iodine solution concentration reduces from E-3, E-4, E-5 successively, and concentration of fluorine reduces from E-5, E-4, E-3 successively;
(6) in reaction process, control reaction temperature is between 60 ℃～65 ℃; If the temperature in the E-3 is too high, can be according to practical situation, Open valve V-12 adds iodine pentafluoride to reduce the concentration of iodine solution through recycle pump E-9, and the concentration range of iodine solution can be 5～20%; If the temperature in the E-5 is too high, can reduce the flow of fluorine gas and tetrafluoroethylene simultaneously according to practical situation, be reflected in the reaction towers at different levels gentleness with assurance and carry out.And adopt U type pipe between reaction towers at different levels and the condensing surface, avoid the flow process short circuit;
(7) raw material is in reaction among the E-1, and Open valve V-15 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-2, close then; Heating E-2 to 60～65 ℃, and stir, treat that iodine wherein is dissolved in the iodine pentafluoride fully; Open valve V-9 closes after charging into nitrogen, and Open valve V-8 closes after finding time, and the program of finding time so circulates three times; Raw material among the E-2 is in stand-by state; After waiting to dissolve iodine solution among the iodine groove E-1 and being exhausted, valve-off V-1, V-16, Open valve V-2, V-17 so that reaction carry out continuously;
Open valve V-3 when (8) reacting, the fluorine gas that nitrogen, unreacted finish, the C of generation
2F
5I gas E-14 (about 25 ℃) behind condensing surface gets into adsorption tower E-6, and all the other materials get into E-3 through condensing reflux; Fill active A l among E-6 and the E-7
2O
3To absorb the intact fluorine gas of a small amount of unreacted, C
2F
5I passes through condensing surface E-12 (about 0 ℃) again and gets into groove through pipeline P-31; Nitrogen is discharged through vacuum breaker V-18, and E-6 and E-7 can be used alternatingly to guarantee the continuity of preparation PFEI;
(9) the iodine liquid of iodine pentafluoride and perfluoroalkyl sulfonyl fluoride flow out to the iodine pentafluoride groove E-8 from E-4, can return again through valve V-12 and recycle pump E-9 and dissolve in the iodine groove;
(10) Open valve V-14 makes C
2F
5The thick product of I gets into finishing sequence; Purify through fractionated mode, collect 12.5～13 ℃ positive cut.
8. single stage method according to claim 1 prepares the novel process of PFEI, it is characterized in that: reaction is a raw material one-step synthesis PFEI from fluorine gas, iodine, tetrafluoroethylene.
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| CN105152988A (en) * | 2015-08-13 | 2015-12-16 | 湖北中科博策新材料研究院 | Novel process for preparing N-fluorobenzenesulfonimide with one-step method |
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| CN115947375A (en) * | 2023-01-04 | 2023-04-11 | 湖北卓熙氟化股份有限公司 | Preparation method of manganese trifluoride |
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| CN108195016A (en) * | 2013-09-12 | 2018-06-22 | 格雷迪安特公司 | Humidifier apparatus, condenser device and bubble column condenser |
| CN108195016B (en) * | 2013-09-12 | 2022-08-05 | 格雷迪安特公司 | Humidifier device, condenser device and bubble column condenser |
| CN105152988A (en) * | 2015-08-13 | 2015-12-16 | 湖北中科博策新材料研究院 | Novel process for preparing N-fluorobenzenesulfonimide with one-step method |
| CN115947375A (en) * | 2023-01-04 | 2023-04-11 | 湖北卓熙氟化股份有限公司 | Preparation method of manganese trifluoride |
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