CN108358747B - Preparation method of high-purity linear perfluoroalkyl iodoalkane - Google Patents
Preparation method of high-purity linear perfluoroalkyl iodoalkane Download PDFInfo
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- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/26—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton
- C07C17/272—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton by addition reactions
- C07C17/275—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton by addition reactions of hydrocarbons and halogenated hydrocarbons
Abstract
The invention discloses a preparation method of high-purity linear perfluoroalkyl iodoalkane, which takes perfluoroalkyl iodide and alkene as reaction substrates to carry out addition reaction in the presence of an initiator and an auxiliary agent. By adding the initiator and the olefin into the reaction system simultaneously, the generation of free radicals and the addition reaction are coordinated, the generation of addition branched chain isomers is reduced, the generation of branched chain isomers is reduced, the yield of the finally obtained perfluoroalkyl iodoalkane is about 97.5 percent, the purity is about 99 percent, and the method is favorable for industrial production.
Description
Technical Field
The invention belongs to the field of chemical industry and preparation of medical intermediates, and particularly relates to a preparation method of high-purity linear perfluoroalkyl iodoalkane
Background
Perfluoroalkyl alkane with the structural general formula of F (CF)2)n(CH2)mH, or F (CF)2)n(CH2)m(CF2)nF is a part of hydrogen atoms in an aliphatic hydrocarbon chainAlkane compounds substituted with fluorine atoms. The liquid perfluoroalkyl alkane with shorter carbon chain is used as the component of the fluorine-containing lubricating oil, is used for military industry, rocket engines and the like, and can also be used in the plasma etching process of various integrated circuits; the solid perfluoroalkyl alkane with longer chain is used as the main component of various fluorine-containing waxes and has excellent light resistance and weather resistance. Perfluoroalkyl alkanes have special biochemical effects due to the special nature of the fluorine atom and are also frequently used in the medical field.
Linear perfluoroalkyl iodoalkanes are key intermediates for the preparation of perfluoroalkyl alkanes. The perfluoroalkyl iodoalkane is obtained by taking perfluoroalkyl iodide and olefin as raw materials through addition reaction. The addition reaction is generally a free radical reaction, and the reaction formula is as follows:
in this reaction, since free radical addition can be achieved at both ends of the double bond of the olefin, a mixture of linear perfluoroalkyl iodoalkane and branched perfluoroalkyl iodoalkane is produced. The perfluoroalkyl alkane applied to the medical field needs a linear chain product with high purity, and if the mixture of the linear chain perfluoroalkyl alkyl iodide alkane and the branched chain perfluoroalkyl alkyl iodide alkane is used as an intermediate for addition reaction, the selectivity of the addition product perfluoroalkyl alkane can be greatly influenced, so that the product purity is not high, and the product does not meet the use standard.
Sun Bai Kao et al, in Chinese patent CN102041134A, disclose a method for preparing fluorine-containing lubricating oil. 34-72 parts of perfluoroalkyl iodide or perfluoroalkyl ethyl iodide and 5-13 parts of olefin monomer are taken as main materials, 0.8-1.5 parts of initiator is added, and then synthetic reaction is carried out at 40-120 ℃, the reaction time is 0.5-4 hours, and the perfluoroalkyl iodoalkane is prepared. In the method, the initiator is used in a large amount and is added at one time, so that the control of the reaction temperature is difficult to realize, and the generation of side reactions and the increase of impurities are aggravated.
Nguyen T H et al, Journal of the Korean Chemical Society,2012,56(5), describe the preparation of 3-perfluorooctyl-2-iodo-propane by the addition of perfluorooctyl iodide with propylene as starting materials in 93% yield.
L.Conte et al in Journal of Fluorine Chemistry,2007,128(5):493 499 describe the reaction of perfluoroalkyl iodides with diolefins on Azobisisobutyronitrile (AIBN) and aqueous sodium metabisulfite (Na) solution2S2O5) The addition reaction is carried out under the action of the catalyst, but the reaction yield is lower.
Manseri et al, Journal of Fluorine Chemistry 78(1996)145-150, describe that the content of branched chain isomers obtained by the addition of perfluoroalkyl iodides and hexafluoropropylene is 5-10%.
In summary, the content and yield of linear perfluoroalkyl iodoalkane prepared by the prior art need to be further improved.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing a high-purity linear perfluoroalkyl iodoalkane.
A process for preparing high-purity linear perfluoroalkyl iodoalkane includes such steps as addition reaction between perfluoroalkyl iodide and olefin as substrate in the presence of trigger and assistant while gradually adding them to perfluoroalkyl iodide solution containing assistant, controlling the generation of free radicals and synchronizing with addition reaction, and preventing the generation of large amount of free radicals, resulting in high purity of target product.
The general formula of the perfluoroalkyl iodide is RfI，RfIs C4～C8A linear perfluoroalkyl group of (a); the olefin being C4～C12Linear terminal olefin of (2) or (C)4～C8Linear terminal diolefins of (a).
When the olefin is linear chain terminal olefin, the general formula of the main component of the high-purity linear chain perfluoroalkyl iodoalkane is RfCH2CH(I)(CH2)n-3CH3Wherein n is 4-12;
when the olefin is linear chain terminal olefin, the general formula of the main component of the high-purity linear chain perfluoroalkyl iodoalkane is RfCH2CH(I)(CH2)m-4CH(I)CH2RfWherein m is 4-8.
The feeding molar ratio of the perfluoroalkyl iodide to the linear chain terminal olefin is 1: 1.05-2.00; the feeding molar ratio of perfluoroalkyl iodide to straight chain terminal diene is 1: 0.50-0.52;
uniformly mixing the initiator and olefin, and then gradually adding the mixture into perfluoroalkyl iodide solution containing an auxiliary agent;
or dissolving the initiator by using a certain amount of water to prepare an aqueous solution containing the initiator, and then simultaneously and gradually adding the aqueous solution containing the initiator and the olefin into the perfluoroalkyl iodide solution containing the auxiliary agent within the same time (the term "simultaneously and gradually adding within the same time" means that the ratio of the adding speed of the aqueous solution and the olefin is basically consistent with the ratio of the fed amount). The molar ratio of the water to the perfluoroalkyl iodide is 1: 4-1: 8.
In the method, the adding time is controlled to be 0.5-3 hours, and the reaction is carried out for 0.5-3 hours after the adding is finished. The feeding mode is preferably dropwise.
The initiator is one of benzoyl peroxide, azobisisobutyronitrile, azobisisoheptonitrile and dimethyl azobisisobutyrate, and the molar ratio of perfluoroalkyl iodide to the initiator is 1: 0.005-1: 0.05.
The auxiliary agent is one or a combination of sodium thiosulfate, sodium sulfite, sodium bisulfite, sodium sulfide and sodium hydrosulfide; the molar ratio of the auxiliary agent is 0.5-2.5 times of the perfluoroalkyl iodide, and the preferred molar amount of the auxiliary agent is 1.0-1.5 times of the perfluoroalkyl iodide. The addition of the auxiliary agent can effectively control the kaladana effect of iodine free radicals.
The addition reaction temperature is 60-110 ℃, the preferable addition reaction temperature is 80-100 ℃, the preferable addition time is 1-2 h, and the heat preservation reaction is carried out for 1-2 h after the addition. Preferably, the addition speed of the aqueous solution containing the initiator and the olefin is constant.
Compared with the prior art, the invention has the following advantages:
by adding the initiator and the olefin into the reaction system at the same time, the generation of free radicals and the addition reaction are coordinated, and the generation of addition branched chain isomers is reduced; the Carassian effect of iodine free radicals is effectively controlled by adding the auxiliary agent. According to the application of the scheme, the content of the branched chain isomer is about 1.0%, the yield of the obtained perfluoroalkyl iodoalkane is about 97.5%, the purity is about 99%, and the method is beneficial to industrial production.
Detailed Description
Example 1
In a 1000mL four-necked flask equipped with a mechanical stirrer, a thermometer and a condenser, 346g (1mol) of perfluorobutyl iodide and 240.2g (1.0mol) of sodium sulfide nonahydrate were added, and the mixture was stirred and heated to 80 ℃; adding 3.4g (with the water content of 28 percent and the mole of 0.01) of benzoyl peroxide and 117.8g (with the mole of 1.05) of n-octene into another 500mL three-neck flask with a bottom dropping device, a mechanical stirring device and a condensing tube at room temperature in advance, uniformly stirring, dropping a mixture of benzoyl peroxide and n-octene into a 1000mL four-neck flask with the temperature of 80 ℃, controlling the dropping time to be 3.0 hours, controlling the dropping reaction temperature to be 80 ℃, continuing the heat preservation reaction at 80 ℃ for 1.0 hour, cooling to room temperature after the reaction is finished, filtering to remove insoluble substances, and distilling under reduced pressure to obtain 1,1,1,2,2,3,3,4, 4-nonafluoro-6-dodecane iodine 448.9g with the content of 99.0 percent and the yield of 97.0 percent; wherein the content of the isomer 1,1,1,2,2,3,3,4, 4-nonafluoro-5-iodomethylundecane is 1.0%.
Examples 2 to 7
The reaction method is the same as that of example 1, the main raw material is 346g (1mol) of perfluorobutyl iodide, and after other reaction conditions are changed, the result is shown as follows:
example 8
446g (1mol) of perfluorohexyl iodide and 240.2g (1.0mol) of sodium sulfide nonahydrate are added into a 1000mL four-mouth bottle provided with a mechanical stirrer, a thermometer and a condenser tube, and the mixture is stirred and heated to 90 ℃; adding 3.4g (with the water content of 28 percent and the water content of 0.01mol) of benzoyl peroxide and 117.8g (with the water content of 1.05mol) of n-octene into a 500mL three-neck flask with a bottom dropping device, mechanically stirring and condensing tubes at room temperature, uniformly stirring, dropping a mixture of benzoyl peroxide and n-octene into a 1000mL four-neck flask with the temperature of 90 ℃, controlling the dropping time to be 2.0 hours, controlling the dropping reaction temperature to be 90 ℃, continuing to perform the heat preservation reaction at 90 ℃ for 1.0 hour, cooling to room temperature after the reaction is finished, filtering to remove insoluble substances, and distilling under reduced pressure to obtain 548.0g of 1,1,1,2,2,3,3,4,4,5,5,6, 6-tridecafluoro-8-iodotetradecane, the content of 99.1 percent and the yield of 97.3 percent; wherein the content of the isomer 1,1,1,2,2,3,3,4,4,5,5,6, 6-tridecafluoro-7-iodomethyltridecane is 0.9 percent.
Examples 9 to 14
The reaction method is the same as that of example 8, the main raw material is 446g (1mol) of perfluorohexyl iodide, and after other reaction conditions are changed, the result is shown as follows:
example 15
In a 1000mL four-necked flask equipped with a mechanical stirrer, a thermometer and a condenser, 546g (1mol) of perfluorooctyl iodide and 240.2g (1.0mol) of sodium sulfide nonahydrate are added, stirred and heated to 95 ℃; adding 3.4g (with the water content of 28 percent and the water content of 0.01mol) of benzoyl peroxide and 117.8g (with the water content of 1.05mol) of n-octene into a 500mL three-necked bottle with a bottle bottom dropping device, a mechanical stirring device and a condensing tube in advance at room temperature, uniformly stirring, dropping a mixture of benzoyl peroxide and n-octene into a 1000mL four-necked bottle with the temperature of 95 ℃, controlling the dropping time to be 2.0 hours, controlling the dropping reaction temperature to be 95 ℃, continuing to perform the heat preservation reaction at 95 ℃ for 1.0 hour, cooling to room temperature after the reaction is finished, filtering to remove insoluble substances, and distilling under reduced pressure to obtain 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8, 8-heptadecafluoro-10-iodohexadecane 646.9g with the content of 99.2 percent and the yield of 97.5 percent; wherein the content of the isomer 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8, 8-heptadecafluoro-9-methyl pentadecane is 0.8 percent.
Examples 16 to 21
The reaction method is the same as that of example 15, the main raw material is 546g (1mol) of perfluorooctyl iodide, and the results are shown below after other reaction conditions are changed:
example 22
In a 1000mL four-necked flask equipped with a mechanical stirrer, a thermometer and a condenser, 346g (1mol) of perfluorobutyl iodide and 240.2g (1.0mol) of sodium sulfide nonahydrate were added, and the mixture was stirred and heated to 80 ℃; adding 3.4g (with the water content of 28 percent and the water content of 0.01mol) of benzoyl peroxide and 41.1g (with the water content of 0.5mol) of 1, 5-hexadiene into a 500mL three-neck flask with a bottle bottom dropping device, mechanically stirring and a condensing tube in advance at room temperature, uniformly stirring, dropping a mixture of the benzoyl peroxide and the 1, 5-hexadiene into a 1000mL four-neck flask with the temperature reaching 80 ℃, controlling the dropping time to be 3 hours, controlling the dropping reaction temperature to be 80 ℃, continuing the 80 ℃ heat preservation reaction for 1.0 hour, finishing the reaction, cooling to room temperature, filtering to remove insoluble substances, and distilling under reduced pressure to obtain 381.5g of 1,1,1,2,2,3,3,4,4,9,9,10,10,11,11,12,12, 12-octadecane-6, 9-diiodotetradecane, the content of 98.5 percent and the yield of 97.1 percent; the isomer content was 1.5%.
The results of this example show that under the reaction conditions of the present invention, better conversion and selectivity can be obtained for the more highly selective linear terminal diolefins.
Example 23
446g (1mol) of perfluorohexyl iodide and 84g (1.5mol) of sodium hydrosulfide are added into a 1000mL four-mouth bottle provided with a mechanical stirrer, a thermometer and a condenser tube, and the mixture is stirred and heated to 85 ℃; in another 500mL three-necked flask with a bottom dropping device, mechanical stirring and a condensing tube, 3.3g (0.02mol) of azobisisobutyronitrile and 49.0g (0.51mol) of 1, 6-heptadiene are added in advance at room temperature, the mixture of azobisisobutyronitrile and 1, 6-heptadiene is uniformly stirred, a 1000mL four-necked flask with the temperature of 85 ℃ is dropped, the dropping time is controlled for 3.0 hours, the dropping reaction temperature is controlled to be 85 ℃, the dropping is finished, the heat preservation reaction at 85 ℃ is continued for 1.0 hour, the reaction is finished, the temperature is reduced to room temperature, insoluble substances are removed by filtration, and the reduced pressure distillation is carried out to obtain 487.0g of 1,1,1,2,2,3,3,4,4,5,5,6,6,14,14,15,15,16, 17,17,18,18,19, 19-twenty-hexafluoro-8, 12-diiodononadecane, the content is 98.6 percent, and the yield is 97.2 percent; the isomer content was 1.4%.
Example 24
In a 1000mL four-necked flask equipped with a mechanical stirrer, a thermometer and a condenser, 346g (1mol) of perfluorobutyl iodide and 248.2g (1.0mol) of sodium thiosulfate pentahydrate were added, and the mixture was stirred and heated to 85 ℃; in another 500mL three-mouth bottle with a bottle bottom dropping device, a mechanical stirring and condensing tube, 2.5g (0.01mol) of azodiisoheptanonitrile and 57.3g (0.52mol) of 1, 7-octadiene are added in advance at room temperature, the mixture of azodiisoheptanonitrile and 1, 7-octadiene is uniformly stirred, a 1000mL four-mouth bottle with the temperature reaching 85 ℃ is dropped, the dropping time is controlled for 2 hours, the dropping reaction temperature is controlled to be 85 ℃, the dropping is finished, the heat preservation reaction at 85 ℃ is continued for 1.0 hour, the reaction is finished, the temperature is reduced to room temperature, insoluble substances are removed by filtration, and reduced pressure distillation is carried out, so that 1,1,1,2,2,3,3,4,4,13,13,14,14,15,15,16,16, 16-octadecafluoro-6, 11-diiodohexadecane 397.0g with the content of 98.5 percent and the yield of 97.5 percent is obtained; the isomer content was 1.5%.
Example 25
In a 1000mL pressure kettle equipped with a mechanical stirrer, a thermometer and a feeding pipe, 346g (1mol) of perfluorobutyl iodide and 240.2g (1.0mol) of sodium sulfide nonahydrate are added, stirred and heated to 90 ℃; in another 250mL three-mouth bottle with a mechanical stirring and condensing tube, 3.4g (with 28% of water content, 0.01mol) of benzoyl peroxide and 100mL of water are added in advance at room temperature and stirred uniformly; 61.7g (1.1mol) of n-butene were metered into a further pressure vessel. Injecting a mixture of benzoyl peroxide and water into a 1000mL pressure kettle with the temperature of 90 ℃ by using a plunger pump, simultaneously injecting n-butene into the 1000mL pressure kettle with the temperature of 90 ℃ by using the plunger pump, controlling the feeding time of the two plunger pumps to be 3 hours, controlling the reaction temperature to be 90 ℃ when in feeding, continuing to perform heat preservation reaction at 90 ℃ for 1.0 hour after finishing dripping, cooling to room temperature after finishing the reaction, filtering to remove insoluble substances, and performing reduced pressure distillation to obtain 395.5g of 1,1,1,2,2,3,3,4, 4-nonafluoro-6-iodooctane, wherein the content is 99.1 percent, and the yield is 97.5 percent; wherein the isomer 1,1,1,2,2,3,3,4, 4-nonafluoro-5-iodomethylheptane content is 0.9%.
Example 26
446g (1mol) of perfluorohexyl iodide and 84g (1.5mol) of sodium hydrosulfide are added into a 1000mL pressure kettle provided with a mechanical stirrer, a thermometer and a feeding pipe, and the mixture is stirred and heated to 90 ℃; in another 250mL three-necked flask with a mechanical stirring and condensing tube, 2.5g (0.01mol) of azodiisoheptanonitrile and 100mL of water are added in advance at room temperature and stirred uniformly; 61.7g (1.1mol) of n-butene were metered into a further pressure vessel. Injecting a mixture of azodiisoheptanonitrile and water into a 1000mL pressure kettle with the temperature of 90 ℃ by using a plunger pump, simultaneously injecting n-butene into the 1000mL pressure kettle with the temperature of 90 ℃ by using the plunger pump, controlling the feeding time of the two plunger pumps to be 3.0 hours, controlling the reaction temperature to be 90 ℃ during feeding, finishing dripping, continuing to perform heat preservation reaction at 90 ℃ for 1.0 hour, cooling to room temperature after finishing the reaction, filtering to remove insoluble substances, and performing reduced pressure distillation to obtain 494.0g of 1,1,1,2,2,3,3,4,4,5,5,6, 6-tridecafluoro-8-iododecane, wherein the content is 99.2 percent, and the yield is 97.6 percent; wherein the content of the isomer 1,1,1,2,2,3,3,4,4,5,5,6, 6-tridecafluoro-7-iodomethylnonane is 0.8 percent.
Example 27
In a 1000mL pressure kettle equipped with a mechanical stirrer, a thermometer and a feeding pipe, 546g (1mol) of perfluorooctyl iodide and 248.2g (1.0mol) of sodium thiosulfate pentahydrate are added, stirred and heated to 100 ℃; in another 250mL three-necked flask with a mechanical stirring and condensing tube, 2.5g (0.01mol) of azodiisoheptanonitrile and 100mL of water are added in advance at room temperature and stirred uniformly; measuring 84.2g (1.2mol) of n-pentene in another pressure vessel, injecting a mixture of azobisisoheptonitrile and water into a 1000mL pressure kettle with the temperature of 100 ℃ by using a plunger pump, simultaneously injecting the n-pentene into the 1000mL pressure kettle with the temperature of 100 ℃ by using a plunger pump, controlling the feeding time of the two plunger pumps to be 2.0 hours, controlling the reaction temperature to be 100 ℃ during feeding, finishing the dropwise adding, continuing the 100 ℃ heat preservation reaction for 1.0 hour, cooling to room temperature, filtering to remove insoluble substances, and carrying out reduced pressure distillation to obtain 603.7g of 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8, 8-heptadecafluoro-10-iodotridecane, wherein the content is 99.4%, and the yield is 97.4%; wherein the isomer 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8, 8-heptadecafluoro-9-iodomethyldodecane is 0.6 percent.
Example 28
In a 1000mL pressure kettle equipped with a mechanical stirrer, a thermometer and a feeding pipe, 346g (1mol) of perfluorobutyl iodide and 240.2g (1.0mol) of sodium sulfide nonahydrate are added, stirred and heated to 90 ℃; in another 250mL three-mouth bottle with a mechanical stirring and condensing tube, 3.4g (with 28% of water content, 0.01mol) of benzoyl peroxide and 100mL of water are added in advance at room temperature and stirred uniformly; in a further pressure vessel 28.1g (0.52mol) of 1.3-butadiene were metered in. Injecting a mixture of benzoyl peroxide and water into a 1000mL pressure kettle with the temperature of 90 ℃ by using a plunger pump, simultaneously injecting 1.3-butadiene into the 1000mL pressure kettle with the temperature of 90 ℃ by using the plunger pump, controlling the feeding time of the two plunger pumps to be 2 hours, controlling the reaction temperature to be 90 ℃ during feeding, finishing dripping, continuing to perform heat preservation reaction at 90 ℃ for 1.0 hour, cooling to room temperature after finishing the reaction, filtering to remove insoluble substances, and performing reduced pressure distillation to obtain 366.2g of 1,1,1,2,2,3,3,4,4,9,9,10,10,11,11,12,12, 12-octadecafluoro-6, 7-diiodododecane with the content of 98.8 percent and the yield of 97.0 percent; the isomer content was 1.2%.
Example 29
A1000 mL autoclave equipped with a mechanical stirrer, a thermometer, and a condenser was charged with 446g (1mol) of perfluorohexyl iodide, 112g (1mol) of n-octene, and 2.5g (0.015mol) of azobisisobutyronitrile. Stirring, heating, initiating a reaction at 80 ℃, controlling the reaction temperature to 80 ℃ for 1h, cooling to room temperature after the reaction is finished, filtering to remove insoluble substances, and carrying out reduced pressure distillation to obtain 540g of perfluorohexyloctane, wherein the content of perfluorohexyloctane is 94.5%, and the yield is 91.4%; the isomer content therein was 3.8%.
Example 30
A1000 mL autoclave equipped with mechanical stirring, thermometer, and condenser was charged with 446g (1mol) of perfluorohexyl iodide, 112g (1mol) of n-octene, and 2.4g (0.01mol) of benzoyl peroxide. Stirring, heating, initiating reaction at 90 ℃, controlling the reaction temperature to 90 ℃ for 1h, cooling to room temperature after the reaction is finished, filtering to remove insoluble substances, and carrying out reduced pressure distillation to obtain 542g of perfluorohexyloctane, wherein the content of the perfluorohexyloctane is 94.3%, and the yield of the perfluorohexyloctane is 91.6%; the isomer content therein was 3.5%.
Claims (11)
1. A preparation method of high-purity linear perfluoroalkyl iodoalkane takes perfluoroalkyl iodide and alkene as reaction substrates, and carries out addition reaction in the presence of an initiator and an auxiliary agent, and is characterized in that the initiator and the alkene are gradually added into a perfluoroalkyl iodide solution mixed with the auxiliary agent simultaneously, the generation of free radicals and the addition reaction are controlled to be synchronous, and the high-purity linear perfluoroalkyl iodoalkane is finally obtained;
the auxiliary agent is one or more of sodium thiosulfate, sodium sulfite, sodium bisulfite, sodium sulfide, sodium hydrosulfide and respective hydrates.
2. The method of claim 1, wherein the perfluoroalkyl iodide has the general formula RfI，RfIs C4～C8A linear perfluoroalkyl group of (a); the olefin is C4～C12Linear terminal olefin of (2) or (C)4～C8Linear terminal diolefins of (a).
3. The method for preparing a high purity linear perfluoroalkyl iodoalkane according to claim 2, wherein the molar ratio of perfluoroalkyl iodide to linear terminal olefin is 1:1.05 to 2.00; the molar ratio of the perfluoroalkyl iodide to the straight chain terminal diolefin is 1: 0.50-0.52.
4. The method for preparing high-purity linear perfluoroalkyl iodo alkane according to claim 1, wherein the initiator and the olefin are uniformly mixed and then gradually added into the perfluoroalkyl iodide solution containing the auxiliary agent, the adding time is controlled to be 0.5-3 hours, and the reaction is carried out for 0.5-3 hours after the adding.
5. The preparation method of high-purity linear perfluoroalkyl iodoalkane according to claim 1, wherein the initiator is dissolved by water to prepare an aqueous solution containing the initiator, the aqueous solution containing the initiator and olefin are simultaneously and gradually added into the perfluoroalkyl iodine solution containing the auxiliary agent within the same time, the adding time is controlled to be 0.5-3 hours, and the reaction is carried out for 0.5-3 hours after the addition;
the molar ratio of the water to the perfluoroalkyl iodide is 1: 4-1: 8.
6. The method of claim 1, wherein the initiator is one of benzoyl peroxide, azobisisobutyronitrile, azobisisoheptonitrile, and dimethyl azobisisobutyrate.
7. The method for preparing a high-purity linear perfluoroalkyl iodoalkane according to claim 1 or 6, wherein the molar ratio of perfluoroalkyl iodide to initiator is 1: 0.005-0.05.
8. The method of claim 1, wherein the molar amount of the auxiliary is 0.5 to 2.5 times that of the perfluoroalkyl iodide.
9. The method of claim 8, wherein the molar amount of the auxiliary is 1.0 to 1.5 times that of the perfluoroalkyl iodide.
10. The method for preparing a high-purity linear perfluoroalkyl iodoalkane according to claim 4 or 5, wherein the temperature of the addition reaction is 60 to 110 ℃;
the adding time is 1-2 h, and the reaction is carried out for 1-2 h after the adding is finished.
11. The method for preparing a high purity linear perfluoroalkyl iodoalkane according to claim 10, wherein the addition reaction temperature is 80-100 ℃.
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