CN108358747A - A kind of preparation method of high-purity linear-chain perfluoroalkyl iodo alkane - Google Patents
A kind of preparation method of high-purity linear-chain perfluoroalkyl iodo alkane Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of high-purity linear-chain perfluoroalkyl iodo alkane, and addition reaction is carried out in the presence of initiator and auxiliary agent using perfluoroalkyl iodides and alkene as reaction substrate.Reaction system is added simultaneously by initiator and alkene, the generation of free radical is made to be cooperateed with addition reaction, reduces the generation of addition branched isomer, reduce the generation of branched isomer, the perfluoroalkyl iodo alkane yield finally obtained is about 97.5%, and purity is about 99%, is conducive to industrialized production.
Description
Technical field
The invention belongs to chemical industry and medicine intermediate preparation fields, and in particular to a kind of high-purity linear-chain perfluoroalkyl iodo
The preparation method of alkane
Background technology
Perfluoroalkyl alkane, general structure are F (CF2)n(CH2)mH or F (CF2)n(CH2)m(CF2)nF is aliphatic carbon
The alkane derivative that a part of hydrogen atom in hydrogen chain is replaced by fluorine atoms.The shorter liquid perfluoroalkyl alkane of carbochain is used as
Fluorine-containing lubricating oil component, for military project, rocket engine etc., it can also be used in the plasma etching industrial of various integrated circuits；
The longer solid state class perfluoroalkyl alkane of chain is used for the key component of various fluorine-containing waxes, has excellent fast light weather resistance.By
In the special nature of fluorine atom, perfluoroalkyl alkane has special biochemical action, is also commonly used for field of medicaments.
Linear perfluoroalkyl alkane iodide is the key intermediate for preparing perfluoroalkyl alkane.Perfluoroalkyl iodo alkane is again
It is to be obtained by addition reaction using perfluoroalkyl iodides and alkene as raw material.The addition reaction is usually radical reaction, instead
Answer formula as follows：
In the reaction, since the double bond both ends of alkene can realize free radical addition, linear perfluoroalkyl iodine can be generated
For the mixture of alkane and branched chain perfluoroalkyl group alkane iodide.And the perfluoroalkyl alkane applied to field of medicaments needs purity very
High straight chain product, if using the mixture of linear perfluoroalkyl alkane iodide and branched chain perfluoroalkyl group alkane iodide as intermediate
Addition reaction is carried out, the selectivity of meeting extreme influence addition compound product perfluoroalkyl alkane causes product purity not high, not meeting makes
Use standard.
Grandson hundred opens et al. discloses a kind of preparation method of fluorine-containing lubricating oil in Chinese patent CN102041134A.With weight
34-72 parts of perfluoroalkyl iodides of part or perfluor alkyl ethide iodine are measured, 5-13 parts of olefin monomers are added 0.8-1.5 parts as major ingredient
Synthetic reaction, reaction time 0.5-4 hour, the perfluoroalkyl iodo alkane being prepared are carried out after initiator at 40-120 DEG C.
Initiator amount is larger in this method and is to be added at one time, it is more difficult to realize the control of reaction temperature, while exacerbate side reaction
Generation, impurity increases.
Nguyen T H et al. are in Journal of the Korean Chemical Society, 2012,56 (5)
It describes and the iodo- propane of 3- perfluoro capryls -2-, yield 93% is prepared as raw material addition using perfluoro octyl iodide and propylene.
L.Conte et al. is in Journal of Fluorine Chemistry, 2007,128 (5):It is introduced in 493-499
Using perfluoroalkyl iodides and alkadienes as reaction substrate, in azodiisobutyronitrile (AIBN) and metabisulfite solution
(Na2S2O5) the lower progress addition reaction of effect, but reaction yield is relatively low.
A.Manseri et al. is described in 78 (1996) 145-150 of Journal of Fluorine Chemistry
The content for the branched isomer that perfluoroalkyl iodides are obtained with hexafluoropropene addition is 5~10%.
In conclusion the content and yield of the linear perfluoroalkyl alkane iodide of prior art preparation need to further increase.
Invention content
In order to solve the problem above-mentioned, the present invention provides a kind of preparation sides of high-purity linear-chain perfluoroalkyl iodo alkane
Method.
A kind of preparation method of high-purity linear-chain perfluoroalkyl iodo alkane is reaction bottom with perfluoroalkyl iodides and alkene
Object, carries out addition reaction in the presence of initiator and auxiliary agent, and initiator is added step-wise to the perfluor containing auxiliary agent simultaneously with alkene
In alkyl iodine solution, the generation for controlling free radical is synchronous with addition reaction, prevents a large amount of free radicals from generating and addition reaction is made to produce
Raw a large amount of isomers and impurity, it is final to obtain high-purity target product.
The perfluoroalkyl iodides general formula is RfI, RfFor C4~C8Linear perfluoroalkyl；Alkene is C4~C12Straight chain end
Terminal olefine or C4~C8Straight chain terminal alkadienes.
When the alkene is straight chain terminal alkene, the principal component of the high-purity linear-chain perfluoroalkyl iodo alkane
General formula be RfCH2CH(I)(CH2)n-3CH3, wherein n is 4~12；
When the alkene is straight chain terminal alkene, the principal component of the high-purity linear-chain perfluoroalkyl iodo alkane
General formula be RfCH2CH(I)(CH2)m-4CH(I)CH2Rf, wherein m is 4~8.
The perfluoroalkyl iodides are 1 with straight chain terminal alkene molar ratio:1.05~2.00；Perfluoroalkyl iodides and straight chain
End alkadienes molar ratio is 1:0.50~0.52；
By the initiator and olefin it is uniform after be added step-wise to again in the perfluoroalkyl iodine solution containing auxiliary agent；
Alternatively, with the initiator described in a certain amount of water dissolution, it is made into the aqueous solution comprising initiator, then will include to cause
The aqueous solution of agent is added step-wise in the perfluoroalkyl iodine solution containing auxiliary agent in same time (" identical simultaneously with alkene
It is gradually added simultaneously in time " refer to that the ratio between the ratio between addition speed of aqueous solution and alkene and inventory are consistent substantially).
The dosage of the water and the molar ratio of perfluoroalkyl iodides are 1:4~1:8.
In above-mentioned method, 0.5~3 hour time is added in control, 0.5~3h of insulation reaction after being added.Described
Feeding manner is preferably added dropwise.
The initiator is benzoyl peroxide, azodiisobutyronitrile, azobisisoheptonitrile, azo-bis-iso-dimethyl
In one kind, perfluoroalkyl iodides and initiator molar ratio are 1:0.005~1:0.05.
The auxiliary agent is sodium thiosulfate, sodium sulfite, sodium hydrogensulfite, vulcanized sodium, one kind of NaHS or combination；
Auxiliary agent molar ratio is 0.5~2.5 times of perfluoroalkyl iodides, and preferred auxiliary agent mole is 1.0~1.5 times of perfluoroalkyl iodides.
The addition of auxiliary agent, the OK a karaoke club that can effectively control iodine free radical apply effect.
The addition reaction temperature is 60~110 DEG C, and preferred addition reaction temperature is 80~100 DEG C, preferably, institute
It states and the time is added as 1~2h, 1~2h of insulation reaction after adding.Preferably, the aqueous solution and alkene comprising initiator
Addition speed be at the uniform velocity be added.
Compared with the existing technology, the present invention has the advantage that：
Reaction system is added simultaneously by initiator and alkene, the generation of free radical is made to be cooperateed with addition reaction, reduces and adds
At the generation of branched isomer；By the addition of auxiliary agent, the OK a karaoke club for effectively controlling iodine free radical applies effect.The present invention program's answers
With the perfluoroalkyl iodo alkane yield of branched isomer content about 1.0%, acquisition is about 97.5%, and purity is about 99%, is had
Conducive to industrialized production.
Specific implementation mode
Embodiment 1
In the 1000mL four-hole bottles equipped with mechanical agitation, thermometer and condenser pipe, 346g (1mol) perfluoro butyl is added
Iodine, nine water vulcanized sodium of 240.2g (1.0mol), agitating and heating are warming up to 80 DEG C；At another with bottom of bottle Dropping feeder, machine
Tool stirs in the 500mL there-necked flasks with condenser pipe, adds good 3.4g (moisture 28%, 0.01mol) peroxidating in advance at room temperature
Benzoyl and 117.8g (1.05mol) positive octene, stir evenly, and 80 DEG C of 1000mL four-hole bottles are had reached to temperature, peroxide is added dropwise
Change benzoyl and positive octene mixture, control time for adding 3.0 hours controls 80 DEG C of drip reacting temperature, is added dropwise, continues
80 DEG C of insulation reactions 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, and vacuum distillation obtains 1,1,1,2,
2,3,3,4,4- nine fluoro- 6- iodine dodecane 448.9g, content 99.0%, yield 97.0%；Wherein isomers 1,1,1,2,2,3,
Nine fluoro- 5- iodomethyls hendecane contents 1.0% of 3,4,4-.
Embodiment 2-7
Reaction method is same as Example 1, and main material is 346g (1mol) perfluoro butyl iodine, other change in reaction conditions
Afterwards, it as a result sees below：
Embodiment 8
Equipped with mechanical agitation, thermometer, condenser pipe 1000mL four-hole bottles in, be added 446g (1mol) perfluoro hexyl
Iodine, nine water vulcanized sodium of 240.2g (1.0mol), agitating and heating are warming up to 90 DEG C；Another is with bottom of bottle Dropping feeder, machinery
It stirs, in the 500mL there-necked flasks of condenser pipe, adds good 3.4g (moisture 28%, 0.01mol) benzoyl peroxide first in advance at room temperature
Acyl and 117.8g (1.05mol) positive octene, stir evenly, and 90 DEG C of 1000mL four-hole bottles are had reached to temperature, benzoyl peroxide is added dropwise
Formyl and positive octene mixture, control time for adding 2.0 hours, control 90 DEG C of drip reacting temperature, are added dropwise, and continue 90 DEG C
Insulation reaction 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, and vacuum distillation obtains 1,1,1,2,2,3,
3,4,4,5,5,6,6- ten three fluoro- 8- iodine tetradecane 548.0g, content 99.1%, yield 97.3%；Wherein isomers 1,1,1,
13 fluoro- 7- iodomethyls tridecane contents 0.9% of 2,2,3,3,4,4,5,5,6,6-.
Embodiment 9-14
Reaction method is same as Example 8, and main material is 446g (1mol) perfluoro-hexyl iodide, other change in reaction conditions
Afterwards, it as a result sees below：
Embodiment 15
In the 1000mL four-hole bottles equipped with mechanical agitation, thermometer and condenser pipe, 546g (1mol) perfluoro capryl is added
Iodine, nine water vulcanized sodium of 240.2g (1.0mol), agitating and heating are warming up to 95 DEG C；Another is with bottom of bottle Dropping feeder, machinery
In the 500mL there-necked flasks of stirring and condenser pipe, add good 3.4g (moisture 28%, 0.01mol) benzoyl peroxide in advance at room temperature
Formyl and 117.8g (1.05mol) positive octene, stir evenly, and 95 DEG C of 1000mL four-hole bottles are had reached to temperature, peroxidating is added dropwise
Benzoyl and positive octene mixture, control time for adding 2.0 hours, control 95 DEG C of drip reacting temperature, are added dropwise, and continue 95
DEG C insulation reaction 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, and vacuum distillation obtains 1,1,1,2,2,
3,3,4,4,5,5,6,6,7,7,8,8- ten seven fluoro- 10- cetyl iodides 646.9g, content 99.2%, yield 97.5%；It is wherein different
17 fluoro- 9 methyl pentadecane contents 0.8% of structure body 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-.
Embodiment 16-21
Reaction method is identical as embodiment 15, and main material is 546g (1mol) perfluoro octyl iodide, other change in reaction conditions
Afterwards, it as a result sees below：
Embodiment 22
Equipped with mechanical agitation, thermometer, condenser pipe 1000mL four-hole bottles in, be added 346g (1mol) perfluoro butyl
Iodine, nine water vulcanized sodium of 240.2g (1.0mol), agitating and heating are warming up to 80 DEG C；Another is with bottom of bottle Dropping feeder, machinery
It stirs, in the 500mL there-necked flasks of condenser pipe, adds good 3.4g (moisture 28%, 0.01mol) benzoyl peroxide first in advance at room temperature
Acyl and 41.1g (0.5mol) 1,5- hexadienes, stir evenly, and 80 DEG C of 1000mL four-hole bottles are had reached to temperature, peroxidating is added dropwise
Benzoyl and 1,5- hexadiene mixtures, control time for adding 3 hours control 80 DEG C of drip reacting temperature, are added dropwise, continue
80 DEG C of insulation reactions 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, and vacuum distillation obtains 1,1,1,2,
2,3,3,4,4,9,9,10,10,11,11,12,12,12- ten octafluoro -6,9- diiodo- tetradecane 381.5g, content 98.5% are received
Rate 97.1%；Wherein content of isomer 1.5%.
The embodiment the result shows that, under the reaction conditions of the present invention, for selectivity require higher straight chain terminal
Alkadienes can also obtain preferable conversion ratio and selectivity.
Embodiment 23
Equipped with mechanical agitation, thermometer, condenser pipe 1000mL four-hole bottles in, be added 446g (1mol) perfluoro hexyl
Iodine, 84g (1.5mol) NaHS, agitating and heating are warming up to 85 DEG C；Another with bottom of bottle Dropping feeder, mechanical agitation,
In the 500mL there-necked flasks of condenser pipe, add good 3.3g (0.02mol) azodiisobutyronitriles and 49.0g (0.51mol) in advance at room temperature
1,6- heptadiene, stirs evenly, and 85 DEG C of 1000mL four-hole bottles is had reached to temperature, azodiisobutyronitrile and 1,6- heptan two is added dropwise
Alkene mixture, control time for adding 3.0 hours, controls 85 DEG C of drip reacting temperature, is added dropwise, and continues 85 DEG C of insulation reactions
1.0 hours, reaction finished, and was cooled to room temperature, was filtered to remove insoluble matter, and vacuum distillation obtains 1,1,1,2,2,3,3,4,4,5,
5,6,6,14,14,15,15,16,16,17,17,18,18,19,19,19- bis- ten hexafluoro -8,12- diiodo- nonadecane 487.0g,
Content 98.6%, yield 97.2%；Wherein content of isomer 1.4%.
Embodiment 24
Equipped with mechanical agitation, thermometer, condenser pipe 1000mL four-hole bottles in, be added 346g (1mol) perfluoro butyl
Iodine, five water sodium thiosulfate of 248.2g (1.0mol), agitating and heating are warming up to 85 DEG C；Another with bottom of bottle Dropping feeder,
Mechanical agitation, condenser pipe 500mL there-necked flasks in, at room temperature in advance plus good 2.5g (0.01mol) azobisisoheptonitrile and 57.3g
(0.52mol) 1,7- octadienes, stir evenly, to temperature have reached 85 DEG C 1000mL four-hole bottles be added dropwise azobisisoheptonitrile and
1,7- octadiene mixture, control time for adding 2 hours, controls 85 DEG C of drip reacting temperature, is added dropwise, and continues 85 DEG C of heat preservations
Reaction 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, and vacuum distillation obtains 1,1,1,2,2,3,3,4,
4,13,13,14,14,15,15,16,16,16- ten octafluoro -6,11-, bis- cetyl iodide 397.0g, content 98.5%, yield
97.5%；Wherein content of isomer 1.5%.
Embodiment 25
Equipped with mechanical agitation, thermometer, feed pipe 1000mL autoclave pressures in, be added 346g (1mol) perfluoro butyl
Iodine, nine water vulcanized sodium of 240.2g (1.0mol), agitating and heating are warming up to 90 DEG C；Another is with mechanical agitation, condenser pipe
In 250mL there-necked flasks, add good 3.4g (moisture 28%, 0.01mol) benzoyl peroxides and 100mL water in advance at room temperature,
It stirs evenly；61.7g (1.1mol) n-butene is measured in another pressure vessel.With a plunger pump 90 are had reached to temperature
DEG C 1000mL autoclave pressures note into benzoyl peroxide and aqueous mixtures, while having reached 90 DEG C to temperature with a plunger pump
1000mL autoclave pressures are noted into n-butene, and two plunger pump feed times of control are all 3 hours, reaction temperature 90 when control is fed
DEG C, it is added dropwise, 90 DEG C of continuation insulation reaction 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, and decompression is steamed
It evaporates, obtains 1,1,1,2,2,3,3,4,4- nine fluoro- 6- iodo-octanes 395.5g, content 99.1%, yield 97.5%；Wherein isomers
Nine fluoro- 5- iodomethyls heptane contents 0.9% of 1,1,1,2,2,3,3,4,4-.
Embodiment 26
Equipped with mechanical agitation, thermometer, feed pipe 1000mL autoclave pressures in, be added 446g (1mol) perfluoro hexyl
Iodine, 84g (1.5mol) NaHS, agitating and heating are warming up to 90 DEG C；Another 250mL with mechanical agitation, condenser pipe
In there-necked flask, adds good 2.5g (0.01mol) azobisisoheptonitrile and 100mL water in advance at room temperature, stir evenly；Another pressure
61.7g (1.1mol) n-butene is measured in force container.With a plunger pump to temperature have reached 90 DEG C 1000mL autoclave pressures note
Into azobisisoheptonitrile and aqueous mixtures, while the 1000mL autoclave pressures for having reached to temperature with a plunger pump 90 DEG C are noted into just
Butylene, two plunger pump feed times of control are all 3.0 hours, and 90 DEG C of reaction temperature when control is fed is added dropwise, and continues 90
DEG C insulation reaction 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, and vacuum distillation obtains 1,1,1,2,2,
3,3,4,4,5,5,6,6- ten three fluoro- 8- iodine decane 494.0g, content 99.2%, yield 97.6%；Wherein isomers 1,1,1,
13 fluoro- 7- iodomethyls nonane contents 0.8% of 2,2,3,3,4,4,5,5,6,6-.
Embodiment 27
Equipped with mechanical agitation, thermometer, feed pipe 1000mL autoclave pressures in, be added 546g (1mol) perfluoro capryl
Iodine, five water sodium thiosulfate of 248.2g (1.0mol), agitating and heating are warming up to 100 DEG C；Another is with mechanical agitation, condensation
In the 250mL there-necked flasks of pipe, adds good 2.5g (0.01mol) azobisisoheptonitrile and 100mL water in advance at room temperature, stir evenly；
84.2g (1.2mol) n-pentene is measured in another pressure vessel, and 100 DEG C are had reached to temperature with a plunger pump
1000mL autoclave pressures are noted into azobisisoheptonitrile and aqueous mixtures, while having reached 100 DEG C to temperature with a plunger pump
1000mL autoclave pressures are noted into n-pentene, and two plunger pump feed times of control are all 2.0 hours, reaction temperature when control is fed
It 100 DEG C, is added dropwise, 100 DEG C of continuation insulation reaction 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble matter, subtracts
Pressure distillation obtains 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8- ten seven fluoro- 10- iodine tridecane 603.7g, content
99.4%, yield 97.4%；Wherein 17 fluoro- 9- iodomethyls of isomers 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-
Dodecane content 0.6%.
Embodiment 28
Equipped with mechanical agitation, thermometer, feed pipe 1000mL autoclave pressures in, be added 346g (1mol) perfluoro butyl
Iodine, nine water vulcanized sodium of 240.2g (1.0mol), agitating and heating are warming up to 90 DEG C；Another is with mechanical agitation, condenser pipe
In 250mL there-necked flasks, add good 3.4g (moisture 28%, 0.01mol) benzoyl peroxides and 100mL water in advance at room temperature,
It stirs evenly；28.1g (0.52mol) 1.3- butadiene is measured in another pressure vessel.With a plunger pump to temperature
Reach 90 DEG C of 1000mL autoclave pressures to note into benzoyl peroxide and aqueous mixtures, while being had reached to temperature with a plunger pump
90 DEG C of 1000mL autoclave pressures are noted into 1.3- butadiene, and two plunger pump feed times of control are all 2 hours, and control is anti-when feeding
90 DEG C of temperature is answered, is added dropwise, 90 DEG C of continuation insulation reaction 1.0 hours, reaction finishes, and is cooled to room temperature, is filtered to remove insoluble
Object, vacuum distillation, obtains 1,1,1,2,2,3,3,4,4,9,9,10,10,11,11,12,12,12- ten octafluoro -6,7- diiodo- ten
Dioxane 366.2g, content 98.8%, yield 97.0%；Wherein content of isomer 1.2%.
Embodiment 29
Equipped with mechanical agitation, thermometer, condenser pipe 1000mL autoclave pressures in, be added 446g (1mol) perfluoro hexyl
Iodine, 112g (1mol) positive octene, 2.5g (0.015mol) azodiisobutyronitrile.Stirring is opened, is heated up, 80 DEG C of initiation reactions, so
80 DEG C of reaction 1h of controlling reaction temperature, reaction finish, are cooled to room temperature, are filtered to remove insoluble matter, be evaporated under reduced pressure, obtain perfluor afterwards
Hexyl octane 540g, content 94.5%, yield 91.4%；Wherein content of isomer 3.8%.
Embodiment 30
Equipped with mechanical agitation, thermometer, condenser pipe 1000mL autoclave pressures in, be added 446g (1mol) perfluoro hexyl
Iodine, 112g (1mol) positive octene, 2.4g (0.01mol) benzoyl peroxide.Stirring is opened, is heated up, 90 DEG C of initiation reactions, then
90 DEG C of controlling reaction temperature reaction 1h, reaction finish, are cooled to room temperature, are filtered to remove insoluble matter, be evaporated under reduced pressure, obtain perfluor oneself
Base octane 542g, content 94.3%, yield 91.6%；Wherein content of isomer 3.5%.
Claims (10)
1. a kind of preparation method of high-purity linear-chain perfluoroalkyl iodo alkane, using perfluoroalkyl iodides and alkene as reaction substrate,
Addition reaction is carried out in the presence of initiator and auxiliary agent, which is characterized in that the initiator is added step-wise to simultaneously with alkene
It is mixed in the perfluoroalkyl iodine solution of auxiliary agent, the generation for controlling free radical is synchronous with addition reaction, high-purity described in final acquisition
Spend linear perfluoroalkyl alkane iodide.
2. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 1, which is characterized in that described
Perfluoroalkyl iodides general formula be RfI, RfFor C4~C8Linear perfluoroalkyl；The alkene is C4~C12Straight chain terminal alkene
Hydrocarbon or C4~C8Straight chain terminal alkadienes.
3. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 2, which is characterized in that perfluor
Alkyl iodide is 1 with straight chain terminal olefin molar ratio:1.05~2.00；Perfluoroalkyl iodides are 1 with straight chain terminal alkadienes molar ratio:
0.50~0.52.
4. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 1, which is characterized in that by institute
State initiator and olefin it is uniform after be added step-wise to again in the perfluoroalkyl iodine solution containing auxiliary agent, control is added the time and is
0.5~3 hour, 0.5~3h of insulation reaction after adding.
5. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 1, which is characterized in that use water
The dissolving initiator, is made into the aqueous solution comprising initiator, then by the aqueous solution comprising initiator with alkene when identical
Interior to be added step-wise in the perfluoroalkyl iodine solution containing auxiliary agent simultaneously, 0.5~3 hour time is added in control, after adding
0.5~3h of insulation reaction；
The dosage of the water and the molar ratio of perfluoroalkyl iodides are 1:4~1:8.
6. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 1, which is characterized in that described
Initiator is one kind in benzoyl peroxide, azodiisobutyronitrile, azobisisoheptonitrile, azo-bis-iso-dimethyl.
7. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 1 or 6, which is characterized in that
Perfluoroalkyl iodides are 1 with initiator molar ratio:0.005~0.05.
8. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 1, which is characterized in that described
Auxiliary agent be sodium thiosulfate, sodium sulfite, sodium hydrogensulfite, vulcanized sodium, NaHS and respective hydrate one kind or more
Kind.
9. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 1, which is characterized in that described
The mole of auxiliary agent be 0.5~2.5 times of perfluoroalkyl iodides, the mole of preferred auxiliary agent be perfluoroalkyl iodides 1.0~
1.5 again.
10. the preparation method of high-purity linear-chain perfluoroalkyl iodo alkane according to claim 4 or 5, which is characterized in that
The addition reaction temperature is 60~110 DEG C, and preferred addition reaction temperature is 80~100 DEG C；
The addition time is 1~2h, 1~2h of insulation reaction after adding.
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