CN102351636B - 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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Abstract
A 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 technique of PFEI, be specifically related to a kind of gas-liquid counter current reaction of carrying out continuously as raw material, taking iodine pentafluoride as solvent, under perfluoroalkyl sulfonyl fluoride atmosphere, in reaction of high order tower taking iodine, fluorine gas, tetrafluoroethylene.
Background technology
PFEI is the important source material of synthesizing perfluoroalkyl iodide, mainly for the production of the initial telogen of perfluoroalkyl iodides, also can be used for producing the fluorine-containing fine chemicals such as fluorine-containing medicines intermediate.There is purposes widely using PFEI derived product full-fluorine alkyl iodide as the intermediate of building-up reactions, as fluorochemical surfactant, fluorine finishing composition etc., apply very extensive, along with the increasing of industrialization, raw-material pulling function is strengthened day by day, therefore the research of PFEI suitability for industrialized production is had to important realistic meaning.
Prepare in the past C
2f
5i great majority adopt IF
5, tetrafluoroethylene, iodine be synthetic under the katalysis of metal fluoride, the PFEI of production is discharged by bubble-plate column top with gas form, in the condenser in downstream, liquefies and is stored in 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, and temperature of reaction, pressure range are wider, processing ease, but the purity of iodine pentafluoride is larger on reaction impact.In reaction, used raw material iodine and iodine pentafluoride, strongly-acid is very large 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 compared with low reaction temperatures, also can effectively reduce the corrosion of reactant to device.The production technique of most of company all adopts this method now.
In technique taking iodine pentafluoride as fluorizating agent, the more difficult control of the mass ratio of iodine pentafluoride, 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, add Nb to be 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 obvious shortcoming: 1,2-diiodo-Tetrafluoroethane (CF
2iCF
2i), iodine pentafluoride, hydrogen fluoride etc. are all toxic substances, wherein 1,2-diiodo-Tetrafluoroethane toxicity is still not clear both at home and abroad, Acute inhalation belongs to hypertoxic type, operation protection is important.And containing oxygen halate or halate, have unstable, misoperation in reaction process, easily sets off an explosion.
Within 2000, French Atofina company has applied for a patent about novel synthetic PFEI (2794465), by pentafluoride ethane (C
2f
5and I H)
2the mixed gas of composition, the basic metal of flowing through (alkaline earth salt/carrier) catalyst layer reacts under its catalysis, can obtain C
2f
5i, CF
3the gaseous mixtures such as I.This method selection rate and yield are wayward, and its carrier employing activated carbon, have easily oxidation or carbon distribution problem of support of the catalyst, are unfavorable for suitability for industrialized production.
Summary of the invention
The object of the invention is to overcome the defect of above patent, adopt fluorine gas, iodine, tetrafluoroethylene direct reaction, design provide a kind of mild condition, can operate continuously, and a step prepare the method for PFEI.
Single stage method of the present invention is prepared the technique of PFEI, adopts the technical process of Multistage tower-type reactors in series, and according to technique needs, tower number can be 1～N level, N>=2; Iodine solution (iodine pentafluoride does solvent cycle and uses), a small amount of perfluoroalkyl sulfonyl fluoride R
fsO
2f (uses R as catalyst recirculation
frepresent perfluoroalkyl chain, carbonatoms is 1～12) enter respectively the countercurrent flow of reaction of high order tower from two ends and react with fluorine nitrogen mixed gas, tetrafluoroethylene gas.The heat producing in the heat absorbing when molten iodine and reaction is taken out of by the condenser between each tower, between reaction tower and condenser, connect with U-shaped pipe, when reaction, U-shaped liquid sealing pipe the inside is full of iodine solution, thereby has avoided fluorine gas to enter iodine solution pipeline, reaches the effect that prevents 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, to control temperature of reaction between 60～65 DEG C in reaction process.
Iodine pentafluoride in described groove can flow into molten iodine groove by recycle pump.
Described perfluoroalkyl sulfonyl fluoride R
fsO
2the amount of F is 0.1～1 ‰, as catalyzer, passes through recycle pump Reusability together with iodine pentafluoride solution.
Described perfluoroalkyl sulfonyl fluoride R
fsO
2the amount of F is 0.1～1 ‰ of iodine pentafluoride solution and perfluoroalkyl sulfonyl fluoride total amount (total amount herein refers to weight unit), as catalyzer.
Described iodine solution concentration can regulate and control by the interlock of iodine pentafluoride internal circulating load and temperature of reaction, and scope is solution 5～20%.
Described fluorine nitrogen mixing ratio can be by the temperature of reaction regulation and control that link, and wherein concentration of fluorine is gas gross 10～98%.
The ratio < 1/0.6 (mol ratio) of the fluorine gas inlet in described tetrafluoroethylene gas inlet and fluorine nitrogen mixed gas, fluorine gas be about excessive.
Interlock recited above regulation and control be exactly to added thing number regulate and control, avoid excess Temperature.
Single stage method of the present invention is prepared the technique of PFEI, and concrete steps are as follows:
(1) before driving, in iodine pentafluoride groove E-8, add part iodine pentafluoride for subsequent use in advance, valve-off V-5, V-15, V-7, V-8, V-14, V-18, all the other valves are all opened, be filled with nitrogen by pipeline P-23 and P-25, then valve-off V-6, V-9, open valve V-7, V-8 and find time, circulation repeatedly, to get rid of air and the aqueous vapor in whole system, is then closed all valves;
(2) Open valve V-1, V-2, V-10, V-11, by recycle pump E-9, makes to be filled with iodine pentafluoride in molten iodine groove and U-shaped pipe then valve-off V-2, V-11;
(3) Open valve V-5 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-1, then closes; Heating E-1 to 60～65 DEG C, and stir, treat that iodine is wherein dissolved in iodine pentafluoride completely; Open valve V-6, closes after being filled with 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 whole system pressure equilibrium;
(4) Open valve V-1, the iodine pentafluoride solution that is dissolved with iodine enters first order reaction tower E-3 through condenser E-10 successively, enters second order reaction tower E-4 through condenser E-11, enters iodine pentafluoride groove E-8 through condenser E-13; In condenser, be the water of 25 DEG C, the heat that reaction is produced was pulled away before entering reaction towers at different levels;
(5) meanwhile, Open valve V-13, V-19 make fluorine nitrogen mixed gas and tetrafluoroethylene gas successively by second order reaction tower E-4, first order reaction tower E-3, with iodine solution countercurrent flow, enter aluminium sesquioxide adsorption tower E-6 and E-7 after having reacted; Iodine solution concentration reduces successively from first order reaction tower E-3, second order reaction tower E-4, PFEI groove E-5, and concentration of fluorine reduces successively from PFEI groove E-5, second order reaction tower E-4, first order reaction tower E-3;
(6), in reaction process, control temperature of reaction between 60 DEG C～65 DEG C; If the excess Temperature in first order reaction tower E-3, can be according to practical situation, Open valve V-12, adds iodine pentafluoride to reduce the concentration of iodine solution by recycle pump E-9, and the concentration range of iodine solution can be 5～20%; If the excess Temperature in PFEI groove E-5, can, according to practical situation, reduce the flow of fluorine gas and tetrafluoroethylene simultaneously, carry out to ensure to react gentleness in reaction towers at different levels.And between reaction towers at different levels and condenser, adopt U-shaped pipe, avoid flow process short circuit;
(7) molten iodine groove E-1 Raw is in reaction, and Open valve V-15 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-2, then closes; Add thermosol iodine groove E-2 to 60～65 DEG C, and stir, treat that iodine is wherein dissolved in iodine pentafluoride completely; Open valve V-9 closes after being filled with nitrogen, and Open valve V-8 closes after finding time, and the program of finding time so circulates three times; Raw material in molten iodine groove E-2 is in stand-by state; After the iodine solution in molten iodine groove E-1 is exhausted, valve-off V-1, V-16, Open valve V-2, V-17 so that reaction carry out continuously;
(8) when reaction Open valve V-3, the complete fluorine gas of nitrogen, unreacted, the C of generation
2f
5i gas E-14 (approximately 25 DEG C) after condenser enters adsorption tower E-6, and all the other materials enter first order reaction tower E-3 through condensing reflux; In E-6 and E-7, fill active A l
2o
3to absorb the complete fluorine gas of a small amount of unreacted, C
2f
5i passes through condenser E-12 (approximately 0 DEG C) again and enters groove by pipeline P-31; Nitrogen is discharged by vacuum breaker V-18, and E-6 and E-7 can be used alternatingly to ensure to prepare the continuity of PFEI;
(9) the iodine liquid of iodine pentafluoride and perfluoroalkyl sulfonyl fluoride flow out to iodine pentafluoride groove E-8 from second order reaction tower E-4, can return in molten iodine groove by valve V-12 and recycle pump E-9.
(10) Open valve V-14, makes C
2f
5the thick product introduction finishing sequence of I; Mode by fractionation is purified, and collects the positive cut of 12.5～13 DEG C.
The advantage that single stage method of the present invention is prepared PFEI technique is: reaction is raw material one-step synthesis PFEI from fluorine gas, iodine, tetrafluoroethylene, has both saved the energy, has saved to a greater extent the investment to intermediate iodine pentafluoride production plant.In previous patent, produce PFEI reacts conventionally under the high temperature of 95 DEG C, because the boiling point of this temperature and iodine pentafluoride is very approaching, once temperature control is careless, 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 adding in this law not only can be served as catalyst, and itself is as tensio-active agent, has the effect that reduces solution surface tension and dispersion moistening, makes gas-liquid mass transfer reach best effect, is conducive to improve speed of reaction and productive rate.In the present invention, newborn iodine pentafluoride activity is higher, can under 60～65 DEG C of conditions, react PFEI with tetrafluoroethylene gentleness.Two molten iodine grooves and two tail gas absorbers cooperations are used alternatingly and are conducive to react continuous and automatic.In tail gas, because fluorine gas is excessive, without remaining tetrafluoroethylene monomer, the complete fluorine gas of unreacted can adsorb by active aluminium sesquioxide, and the three wastes are beneficial to improvement.This processing unit and parts, adopt common iron, processes and carry out fluorine gas Passivation Treatment again without pit chemical nickel plating, not only can effectively prevent the damage of eroding chemical to equipment, and reduce cost of investment, is beneficial to industrialization.
Brief description of the drawings
Fig. 1 is the process route chart that single stage method is prepared PFEI.
Wherein: the molten iodine groove of E-1, E-2 E-3 first order reaction tower E-4 second order reaction tower
E-5 PFEI groove E-6, E-7 adsorption tower E-8 iodine pentafluoride groove
E-9 recycle pump E-10～E-14 condenser V-1～V-19 valve
P-29～P-31U type pipe.
Embodiment
Shown in Fig. 1, single stage method of the present invention is prepared the technique of PFEI, adopts the technical process of Multistage tower-type reactors in series, and according to technique needs, tower number can be 1～N level, N >=2; Iodine solution (iodine pentafluoride makees solvent), perfluoroalkyl sulfonyl fluoride and fluorine nitrogen mixed gas, tetrafluoroethylene gas enter respectively the countercurrent flow of reaction of high order tower and react from two ends.The heat producing in the heat absorbing when molten iodine and reaction is taken out of by the condenser between each tower, between reaction tower and condenser, connect with U-shaped pipe, when reaction, U-shaped liquid sealing pipe the inside is full of iodine solution, thereby has avoided fluorine gas to enter iodine solution pipeline, reaches the effect that prevents 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, to control temperature of reaction between 60～65 DEG C in reaction process.
Iodine pentafluoride in described groove can flow into molten iodine groove by recycle pump.
Described perfluoroalkyl sulfonyl fluoride R
fsO
2the amount of F is 0.1～1 ‰, as catalyzer, passes through recycle pump Reusability together with iodine pentafluoride solution.
Described iodine solution concentration can regulate and control by the interlock of iodine pentafluoride internal circulating load and temperature of reaction, and scope is solution 5～20%.
Described fluorine nitrogen mixing ratio can be by the temperature of reaction regulation and control that link, and wherein concentration of fluorine is gas gross 10～98%.
The ratio < 1/0.6 (mol ratio) of described tetrafluoroethylene gas inlet and fluorine gas inlet, fluorine gas be about excessive.
Single stage method of the present invention is prepared the technique of PFEI, and concrete steps are as follows:
(1) before driving, in iodine pentafluoride groove E-8, add part iodine pentafluoride for subsequent use in advance, valve-off V-5, V-15, V-7, V-8, V-14, V-18, all the other valves are all opened, be filled with nitrogen by pipeline P-23 and P-25, then valve-off V-6, V-9, open valve V-7, V-8 and find time, circulation repeatedly, to get rid of air and the aqueous vapor in whole system, is then closed all valves;
(2) Open valve V-1, V-2, V-10, V-11, by recycle pump E-9, makes to be filled with iodine pentafluoride in molten iodine groove and U-shaped pipe then valve-off V-2, V-11;
(3) Open valve V-5 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-1, then closes; Add thermosol iodine groove E-1 to 60～65 DEG C, and stir, treat that iodine is wherein dissolved in iodine pentafluoride completely; Open valve V-6, closes after being filled with 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 whole system pressure equilibrium;
(4) Open valve V-1, the iodine pentafluoride solution that is dissolved with iodine enters first order reaction tower E-3 through condenser E-10 successively, enters second order reaction tower E-4 through condenser E-11, enters iodine pentafluoride groove E-8 through condenser E-13; In condenser, be the water of 25 DEG C, the heat that reaction is produced was pulled away before entering reaction towers at different levels;
(5) meanwhile, Open valve V-13, V-19 make fluorine nitrogen mixed gas and tetrafluoroethylene gas successively by second order reaction tower E-4, first order reaction tower E-3, with iodine solution countercurrent flow, enter aluminium sesquioxide adsorption tower E-6 and E-7 after having reacted; Iodine solution concentration reduces successively from first order reaction tower E-3, second order reaction tower E-4, PFEI groove E-5, and concentration of fluorine reduces successively from PFEI groove E-5, second order reaction tower E-4, first order reaction tower E-3;
(6), in reaction process, control temperature of reaction between 60 DEG C～65 DEG C; If the excess Temperature in first order reaction tower E-3, can be according to practical situation, Open valve V-12, adds iodine pentafluoride to reduce the concentration of iodine solution by recycle pump E-9, and the concentration range of iodine solution can be 5～20%; If the excess Temperature in E-5, can, according to practical situation, reduce the flow of fluorine gas and tetrafluoroethylene simultaneously, carry out to ensure to react gentleness in reaction towers at different levels.And between reaction towers at different levels and condenser, adopt U-shaped pipe, avoid flow process short circuit;
(7) molten iodine groove E-1 Raw is in reaction, and Open valve V-15 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-2, then closes; Add thermosol iodine groove E-2 to 60～65 DEG C, and stir, treat that iodine is wherein dissolved in iodine pentafluoride completely; Open valve V-9 closes after being filled with nitrogen, and Open valve V-8 closes after finding time, and the program of finding time so circulates three times; Raw material in molten iodine groove E-2 is in stand-by state; After the iodine solution in molten iodine groove E-1 is exhausted, valve-off V-1, V-16, Open valve V-2, V-17 so that reaction carry out continuously;
(8) when reaction Open valve V-3, the complete fluorine gas of nitrogen, unreacted, the C of generation
2f
5i gas E-14 (approximately 25 DEG C) after condenser enters adsorption tower E-6, and all the other materials enter first order reaction tower E-3 through condensing reflux; In E-6 and E-7, fill active A l
2o
3to absorb the complete fluorine gas of a small amount of unreacted, C
2f
5i passes through condenser E-12 (approximately 0 DEG C) again and enters groove by pipeline P-31; Nitrogen is discharged by vacuum breaker V-18, and E-6 and E-7 can be used alternatingly to ensure to prepare the continuity of PFEI;
(9) the iodine liquid of iodine pentafluoride and perfluoroalkyl sulfonyl fluoride flow out to iodine pentafluoride groove E-8 from second order reaction tower E-4, can return in molten iodine groove by valve V-12 and recycle pump E-9;
(10) Open valve V-14, makes C
2f
5the thick product introduction finishing sequence of I; Mode by fractionation is purified, and collects the positive cut of 12.5～13 DEG C.
Be not limited to above-described embodiment, have multiple embodiment according to the difference of the addition of reactant in method steps.
Claims (7)
1. single stage method is prepared the technique of PFEI, it is characterized in that: adopt the technical process of Multistage tower-type reactors in series, iodine pentafluoride solution, perfluoroalkyl sulfonyl fluoride and fluorine nitrogen mixed gas, the tetrafluoroethylene of iodine enter respectively the countercurrent flow of reaction of high order tower and react from two ends; Concrete steps are as follows:
(1) before driving, in iodine pentafluoride groove E-8, add part iodine pentafluoride for subsequent use in advance, valve-off V-5, V-15, V-7, V-8, V-14, V-18, all the other valves are all opened, be filled with nitrogen by pipeline P-23 and P-25, then valve-off V-6, V-9, open valve V-7, V-8 and find time, circulation repeatedly, to get rid of air and the aqueous vapor in whole system, is then closed all valves;
(2) Open valve V-1, V-2, V-10, V-11, by recycle pump E-9, makes to be filled with iodine pentafluoride in molten iodine groove and U-shaped pipe then valve-off V-2, V-11;
(3) Open valve V-5 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-1, then closes; Heating E-1 to 60～65 DEG C, and stir, treat that iodine is wherein dissolved in iodine pentafluoride completely; Open valve V-6, closes after being filled with 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 whole system pressure equilibrium;
(4) Open valve V-1, the iodine pentafluoride solution that is dissolved with iodine enters first order reaction tower E-3 through condenser E-10 successively, enters second order reaction tower E-4 through condenser E-11, enters iodine pentafluoride groove E-8 through condenser E-13; In condenser, be the water of 25 DEG C, the heat that reaction is produced was pulled away before entering reaction towers at different levels;
(5) meanwhile, Open valve V-13, V-19 make fluorine nitrogen mixed gas and tetrafluoroethylene gas successively by second order reaction tower E-4, first order reaction tower E-3, with iodine solution countercurrent flow, enter aluminium sesquioxide adsorption tower E-6 and E-7 after having reacted; Iodine solution concentration reduces successively from first order reaction tower E-3, second order reaction tower E-4, PFEI groove E-5, and concentration of fluorine reduces successively from PFEI groove E-5, second order reaction tower E-4, first order reaction tower E-3;
(6), in reaction process, control temperature of reaction between 60 DEG C～65 DEG C; If the excess Temperature in first order reaction tower E-3, can be according to practical situation, Open valve V-12, adds iodine pentafluoride to reduce the concentration of iodine solution by recycle pump E-9, and the concentration range of iodine solution can be 5～20%; If the excess Temperature in PFEI groove E-5, can, according to practical situation, reduce the flow of fluorine gas and tetrafluoroethylene simultaneously, carry out to ensure to react gentleness in reaction towers at different levels.And between reaction towers at different levels and condenser, adopt U-shaped pipe, avoid flow process short circuit;
(7) molten iodine groove E-1 Raw is in reaction, and Open valve V-15 adds iodine, perfluoroalkyl sulfonyl fluoride in molten iodine groove E-2, then closes; Add thermosol iodine groove E-2 to 60～65 DEG C, and stir, treat that iodine is wherein dissolved in iodine pentafluoride completely; Open valve V-9 closes after being filled with nitrogen, and Open valve V-8 closes after finding time, and the program of finding time so circulates three times; Raw material in molten iodine groove E-2 is in stand-by state; After the iodine solution in molten iodine groove E-1 is exhausted, valve-off V-1, V-16, Open valve V-2, V-17 so that reaction carry out continuously;
(8) when reaction Open valve V-3, the complete fluorine gas of nitrogen, unreacted, the C of generation
2f
5i gas E-14 after condenser enters adsorption tower E-6, and all the other materials enter first order reaction tower E-3 through condensing reflux; In E-6 and E-7, fill active A l
2o
3to absorb the complete fluorine gas of a small amount of unreacted, C
2f
5i enters groove through condenser E-12 by pipeline P-31 again; Nitrogen is discharged by vacuum breaker V-18, and E-6 and E-7 can be used alternatingly to ensure to prepare the continuity of PFEI;
(9) the iodine liquid of iodine pentafluoride and perfluoroalkyl sulfonyl fluoride flow out to iodine pentafluoride groove E-8 from second order reaction tower E-4, can return in molten iodine groove by valve V-12 and recycle pump E-9;
(10) Open valve V-14, makes C
2f
5the thick product introduction finishing sequence of I; Mode by fractionation is purified, and collects the positive cut of 12.5～13 DEG C.
2. single stage method according to claim 1 is prepared the technique of PFEI, it is characterized in that: the amount of described perfluoroalkyl sulfonyl fluoride is 0.1～1 ‰ of iodine pentafluoride solution and perfluoroalkyl sulfonyl fluoride total amount, as catalyzer.
3. single stage method according to claim 1 is prepared the technique of PFEI, it is characterized in that: described iodine solution concentration can regulate and control by the interlock of iodine pentafluoride internal circulating load and temperature of reaction, and scope is solution 5～20%.
4. single stage method according to claim 1 is prepared the technique of PFEI, it is characterized in that: described fluorine nitrogen mixing ratio can be by the temperature of reaction regulation and control that link, and wherein concentration of fluorine is 10～98% of fluorine nitrogen mixed gas total amount.
5. single stage method according to claim 1 is prepared the technique of PFEI, it is characterized in that: ratio < 1/0.6 mol ratio of the fluorine gas inlet in described tetrafluoroethylene gas inlet and fluorine nitrogen mixed gas.
6. single stage method according to claim 1 is prepared the technique of PFEI, it is characterized in that: in reaction process, the flow of iodine solution concentration, fluorine nitrogen mixed gas ratio, tetrafluoroethylene can be according to temperature of reaction interlock regulation and control, to control temperature of reaction between 60～65 DEG C.
7. single stage method according to claim 1 is prepared the technique of PFEI, it is characterized in that: reaction is raw material one-step synthesis PFEI from fluorine gas, iodine, tetrafluoroethylene.
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