CN107649112A - A kind of catalyst produced for fluoro phosphonitrile and its derivatives industry metaplasia - Google Patents
A kind of catalyst produced for fluoro phosphonitrile and its derivatives industry metaplasia Download PDFInfo
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- CN107649112A CN107649112A CN201710874578.3A CN201710874578A CN107649112A CN 107649112 A CN107649112 A CN 107649112A CN 201710874578 A CN201710874578 A CN 201710874578A CN 107649112 A CN107649112 A CN 107649112A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6581—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and nitrogen atoms with or without oxygen or sulfur atoms, as ring hetero atoms
- C07F9/65812—Cyclic phosphazenes [P=N-]n, n>=3
- C07F9/65815—Cyclic phosphazenes [P=N-]n, n>=3 n = 3
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of catalyst produced for fluoro phosphonitrile and its derivatives industry metaplasia, the catalyst is applied to chloro phosphonitrile and its derivative prepares the fluorination reaction of fluoro phosphonitrile and its derivative, and the catalyst is mixture more than one or both of technical grade graphene, graphene oxide, fullerene, Mxene, hydroxyl carbon nano tube, expanded graphite.It is simple using catalyst separation, increase the purity of product, can reuse, reduce the use cost of catalyst.
Description
Technical field
The present invention relates to industrialized production fluoro phosphonitrile and its derivative, and in particular to one kind is used for fluoro phosphonitrile and its spread out
The catalyst of biological industry metaplasia production.
Background technology
Phosphazene compound is the inorganic-organic hybridization compound that a kind of skeleton is alternately arranged by phosphorus and nitrogen, can be divided into ring phosphorus
Nitrile and polyphosphazene.Wherein, chloro phosphonitrile is most representative compound in cyclic phosphazene compound, because chlorine atom is with very strong
Activity, it is easy to substituted by various nucleopilic reagents.Therefore, using chloro phosphonitrile as intermediate, can synthesize has with various
The fluoro phosphine nitrile and its phosphazene derivative of machine functional group.Chlorine atom is compatible poor in lithium battery electrolytes, and fluoro phosphorus
Nitrile and its derivative then have good electrochemistry compatibility.
At present, the synthesis of fluoro phosphonitrile and its derivative mainly with chloro phosphonitrile and villiaumite carry out fluorination reaction yield compared with
Low, in order to accelerate the speed of fluorination reaction and yield, it is necessary to add catalyst into reaction system, its catalyst mainly has tetramethyl
Ammonium chloride, 4 bromide, 18- crown-s 6 and phosphonium bromide and polyethylene glycol etc..
Chinese patent (application number CN201610164612.3), which discloses, can greatly improve fluoro phosphonitrile and its derivative
The polyethylene glycols catalyst of yield, using the catalyst fluoro phosphonitrile and its derivative yield can be made to be promoted to 99%.
Because fluoro phosphonitrile and its derivative then have good electrochemistry compatibility, thus present inventor uses
Polyethylene glycols catalyst optimizes to the industrialized producing technology of existing fluoro phosphonitrile and its derivative, but uses poly-
Glycols catalyst problem present in industrialized production is：Polyethylene glycols catalyst is a kind of phase transfer catalyst,
There is good dissolubility in organic solvent and water so that substantial amounts of polyethylene glycols catalyst in product be present, from product
It is middle that the separation of polyethylene glycols catalyst is relatively difficult, cause product purity to reduce, both influence polyethylene glycols catalyst in work
Application in industry, recycling can not be carried out to polyethylene glycols catalyst, if being carried out again to the product in product pure again
Change, and recycle polyethylene glycols catalyst, not only need to increase R＆D costs, and need to increase separation purifying technique,
Increase process costs.Although the yield of fluoro phosphonitrile and its derivative can be improved using polyethylene glycols catalyst, by
The income that raising of the cost increase far above yield that it brings in above mentioned problem is brought.So as to cause using catalyst in industry
Caused bottleneck in the technique research and development of metaplasia production fluoro phosphonitrile and its derivative raising Business Economic Benefit.
The content of the invention
In order to solve the deficiencies in the prior art, an object of the present invention is to provide one kind and is used for fluoro phosphonitrile and its derivative
The catalyst of thing industrialized production.It is simple using catalyst separation, increase the purity of product, can reuse, reduction is urged
The use cost of agent.
To achieve these goals, the technical scheme is that：
A kind of catalyst produced for fluoro phosphonitrile and its derivatives industry metaplasia, the catalyst are applied to chloro phosphonitrile
And its derivative prepares the fluorination reaction of fluoro phosphonitrile and its derivative, the catalyst is technical grade graphene, graphite oxide
Mixture more than one or both of alkene, fullerene, Mxene, hydroxyl carbon nano tube, expanded graphite.
The either catalyst such as tetramethyl ammonium chloride, 4 bromide, 18- crown-s 6 and phosphonium bromide, or polyethylene glycol
Class catalyst, is a kind of phase transfer catalyst, and its Catalysis Principles is：The fluorization agents such as potassium fluoride, sodium fluoride are inorganic matters, difficult
To be dissolved in organic solvent, and what fluorization agent was fluorinated to chloro phosphonitrile and its derivative is on P positions by fluorine ion
Chlorine carry out nucleophilic displacement of fluorine, phase transfer catalyst can be dissolved in organic solvent, while it also has hydrophilic radical, can be by fluorine
Fluorine ion in agent is transferred in organic solvent, so as to accelerate the bombardment to P positions of fluorine ion, so as to play catalytic action,
Thus phase transfer catalyst wants the optimal catalytic effect that reaches, ensures that it in the solubility of organic solvent is the most important condition.
And according to solid catalyst, because it can not be dissolved in organic solvent, thus it is the same without image of Buddha phase transfer catalyst, leads to
Cross phase transfer catalyst fluorine ion is transferred to realize catalytic performance in organic solvent, so solid catalyst pair can not be used
The fluorination reaction of chloro phosphonitrile and its derivative carries out catalytic applications.
Technical grade graphene that the present invention uses, graphene oxide, fullerene, Mxene, hydroxyl carbon nano tube, expansion
Contain aerobic or hydroxyl in graphite, the affinity interaction of catalyst and solvent can be strengthened, add contact of the catalyst with raw material
Probability, and contain substantial amounts of conjugated structure in these catalyst, and contain nitrogen phosphorus double bond in phosphonitrile, can with catalyst
Material form π-pi-conjugated structure so that catalyst can raw material form stronger molecular separating force, and have in itself in catalyst
Electric conductivity, fluorine ion can directly be bombarded P positions so as to which nucleophilic displacement of fluorine occur by catalyst.
Because the present invention is using graphene, graphene oxide, fullerene, Mxene, hydroxyl carbon nano tube, expanded graphite
As catalyst, catalyst only may separate out by filtering insoluble in organic solvent, thus after reacting completely, so as to improve
The purity of product.
The second object of the present invention is to provide a kind of synthetic method of fluoro phosphonitrile and its derivative, and chloro phosphonitrile is dissolved
In organic solvent, add fluorization agent and above-mentioned catalyst is reacted, after filtering distillation, produce fluoro phosphonitrile and its derivative
Thing.
The third object of the present invention is to provide a kind of above-mentioned synthetic method and is preparing fluoro phosphonitrile and its derivative species battery
Application in electrolyte.
The fourth object of the present invention is to provide above-mentioned synthetic method in fluoro phosphonitrile and its derivative species battery is prepared
Using.
Beneficial effects of the present invention are：
1. the separation for the catalyst that the present invention uses is simple, it is possible to increase the purity of product is greatly improved, using the present invention
Catalyst the purity of product can be improved to 99%.
2. reaction condition of the present invention is gentle, operability is good, is mass produced suitable for industrialization.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
The formula of chloro phosphonitrile and its derivative described herein is
Wherein, R1~R6Can be with identical, can also be different, it is selected from as chlorine element, alkyl, chloro alkyl, chloro alcoxyl
Base, askarel, alkoxy, alkyl silicon, chloroalkene base, xenyl phenyl, chlorophenyl, alkyl phosphate, alkoxyl silicone,
Boron alkoxide or amide groups, R1~R6In at least one be chlorine element, work as R1~R6It is chloro phosphonitrile when being chlorine element.
As background technology is introduced, exist contains in the product for preparing fluoro phosphonitrile and its derivative in the prior art
Be difficult to the deficiency of catalyst separated, in order to solve technical problem as above, present applicant proposes one kind be used for fluoro phosphonitrile and
The catalyst of its derivatives industry metaplasia production.
A kind of exemplary embodiment of the application, there is provided a kind of to produce for fluoro phosphonitrile and its derivatives industry metaplasia
Catalyst, the catalyst is applied to chloro phosphonitrile and its derivative prepares the fluorination reaction of fluoro phosphonitrile and its derivative, institute
Catalyst is stated as one in technical grade graphene, graphene oxide, fullerene, Mxene, hydroxyl carbon nano tube, expanded graphite
Kind or two or more mixtures.
The either catalyst such as tetramethyl ammonium chloride, 4 bromide, 18- crown-s 6 and phosphonium bromide, or polyethylene glycol
Class catalyst, is a kind of phase transfer catalyst, and its Catalysis Principles is：The fluorization agents such as potassium fluoride, sodium fluoride are inorganic matters, difficult
To be dissolved in organic solvent, and what fluorization agent was fluorinated to chloro phosphonitrile and its derivative is on P positions by fluorine ion
Chlorine carry out nucleophilic displacement of fluorine, phase transfer catalyst can be dissolved in organic solvent, while it also has hydrophilic radical, can be by fluorine
Fluorine ion in agent is transferred in organic solvent, so as to accelerate the bombardment to P positions of fluorine ion, so as to play catalytic action,
Thus phase transfer catalyst wants the optimal catalytic effect that reaches, ensures that it in the solubility of organic solvent is the most important condition.
And according to solid catalyst, because it can not be dissolved in organic solvent, thus it is the same without image of Buddha phase transfer catalyst, leads to
Cross phase transfer catalyst fluorine ion is transferred to realize catalytic performance in organic solvent, so solid catalyst pair can not be used
The fluorination reaction of chloro phosphonitrile and its derivative carries out catalytic applications.
Because the present invention is using industry level graphene, graphene oxide, fullerene, Mxene, hydroxyl carbon nano tube, expansion
Graphite only may separate out catalyst as catalyst, insoluble in organic solvent, thus after reacting completely by filtering, so as to
Improve the purity of product.
Another exemplary embodiment of the application, there is provided a kind of synthetic method of fluoro phosphonitrile and its derivative, will
Chloro phosphonitrile or fluoro phosphazene derivative are dissolved in organic solvent, add fluorization agent and above-mentioned catalyst is reacted, filter
After distillation, fluoro phosphonitrile and its derivative are produced.
In order to ensure that reaction is complete, the application is preferable, and the reaction time is 1~20h.
Preferably, the reaction temperature is 30~120 DEG C.
In order to ensure the catalytic effect of catalyst, the application is preferable, the addition of the catalyst for chloro phosphonitrile and
The 1~20% of fluorization agent gross mass, or the 1~20% of fluoro phosphazene derivative and fluorization agent gross mass.
Preferably, the ratio between the chloro phosphonitrile or the amount of material of fluoro phosphazene derivative and fluorization agent are 1:1~1.5.
Improve the conversion ratio of chloro phosphonitrile.
Preferably, the fluorization agent is one kind or its two kinds mixture in sodium fluoride and potassium fluoride.
Preferably, the organic solvent be tetrahydrofuran, n-hexane, toluene, chlorobenzene, petroleum ether, pyridine, N, N- diformazans
Mixture more than one or both of base formamide (DMF), acetonitrile or benzonitrile.
Embodiment there is provided a kind of above-mentioned synthetic method to prepare fluoro phosphonitrile or derivatives thereof for the third of the application
Application in class battery electrolyte.
Embodiment there is provided a kind of above-mentioned synthetic method to prepare fluoro phosphonitrile or derivatives thereof for the 4th kind of the application
Application in class battery.
In order that the technical scheme of the application can clearly be understood by obtaining those skilled in the art, below with reference to tool
The embodiment of body describes the technical scheme of the application in detail.
Embodiment 1：
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution, Xiang Rong in 200mL tetrahydrofurans
It is anti-as catalyst, and under 30 DEG C of temperature conditionss as fluorization agent, addition 2g technical grade graphenes that 27g sodium fluorides are added in liquid
10h is answered, the phosphonitrile of phosphazene derivative hexafluoro ring three, yield 99%, purity 98% are obtained after filtered, vacuum distillation.
Embodiment 2
The phosphonitrile dissolution of crystals of 27.5g ethyoxyl pentachloro-s ring three is formed into ethyoxyl pentachloro- ring three in 200mL tetrahydrofurans
Phosphonitrile solution, 27g sodium fluorides are added into solution and are used as fluorization agent, addition 2g technical grade graphenes are as catalyst, and 30
React 15h under DEG C temperature conditionss, it is filtered, be evaporated under reduced pressure after obtain the phosphonitrile of five fluorine ring of phosphazene derivative ethyoxyl three, yield
99%, purity 97%.
Embodiment 3
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution in 200mL DMF, into solution
Add 27g sodium fluorides and react 5h under 60 DEG C of temperature conditionss as catalyst as fluorization agent, addition 2g graphene oxides,
The phosphonitrile of phosphazene derivative hexafluoro ring three, yield 99%, purity 98% are obtained after filtered, vacuum distillation.
Embodiment 4
The phosphonitrile dissolution of crystals of 27.5g ethyoxyl pentachloro-s ring three is formed into the phosphonitrile of ethyoxyl pentachloro- ring three in 200mL DMF
Solution, 27g sodium fluorides are added into solution and are used as fluorization agent, addition 2g graphene oxides are as catalyst, and in 60 DEG C of temperature
Under the conditions of react 5h, it is filtered, be evaporated under reduced pressure after obtain the phosphonitrile of five fluorine ring of phosphazene derivative ethyoxyl three, yield 99%, purity
For 98%.
Embodiment 5
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution in 200mL petroleum ethers, to solution
Middle addition 27g sodium fluorides react 3h under 100 DEG C of temperature conditionss as catalyst, passed through as fluorization agent, addition 2g fullerenes
Filtering, obtain the phosphonitrile of phosphazene derivative hexafluoro ring three, yield 99%, purity 97% after being evaporated under reduced pressure.
Embodiment 6
The phosphonitrile dissolution of crystals of 27.5g ethyoxyl pentachloro-s ring three is formed into the phosphorus of ethyoxyl pentachloro- ring three in 200mL petroleum ethers
Nitrile solution, 27g sodium fluorides are added into solution and are used as fluorization agent, addition 2g fullerenes are as catalyst, and in 100 DEG C of temperature strips
5h is reacted under part, obtains the phosphonitrile of five fluorine ring of phosphazene derivative ethyoxyl three, yield 99% after filtered, vacuum distillation, purity is
97%.
Embodiment 7
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution in 200mL n-hexanes, to solution
For middle addition 27g sodium fluorides as fluorization agent, 2g Mxene are as catalyst for addition, and react 2h under 120 DEG C of temperature conditionss, pass through
Filtering, obtain the phosphonitrile of phosphazene derivative hexafluoro ring three, yield 99%, purity 98% after being evaporated under reduced pressure.
Embodiment 8
The phosphonitrile dissolution of crystals of 27.5g ethyoxyl pentachloro-s ring three is formed into the phosphorus of ethyoxyl pentachloro- ring three in 200mL n-hexanes
Nitrile solution, 27g sodium fluorides being added into solution as fluorization agent, 2g Mxene are as catalyst for addition, and in 120 DEG C of temperature strips
2h is reacted under part, obtains the phosphonitrile of five fluorine ring of phosphazene derivative ethyoxyl three, yield 99% after filtered, vacuum distillation, purity is
98%.
Embodiment 9
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution in 200mL toluene, into solution
27g sodium fluorides are added as fluorization agent, add 2g hydroxyl carbon nano tubes as catalyst, and reacted under 80 DEG C of temperature conditionss
4h, the phosphonitrile of phosphazene derivative hexafluoro ring three, yield 99%, purity 98% are obtained after filtered, vacuum distillation.
Embodiment 10
The phosphonitrile dissolution of crystals of 27.5g ethyoxyl pentachloro-s ring three is formed into the phosphonitrile of ethyoxyl pentachloro- ring three in 200mL toluene
Solution, 27g sodium fluorides are added into solution and are used as fluorization agent, addition 2g hydroxyl carbon nano tubes are as catalyst, and at 80 DEG C
React 4h under temperature conditionss, it is filtered, be evaporated under reduced pressure after obtain the phosphonitrile of five fluorine ring of phosphazene derivative ethyoxyl three, yield 99%,
Purity is 98%.
Embodiment 11
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution in 200mL acetonitriles, into solution
27g sodium fluorides are added to react 20h as fluorization agent, addition 2g expanded graphites under 30 DEG C of temperature conditionss as catalyst, pass through
Filtering, obtain the phosphonitrile of phosphazene derivative hexafluoro ring three, yield 99%, purity 97% after being evaporated under reduced pressure.
Embodiment 12
The phosphonitrile dissolution of crystals of 27.5g ethyoxyl pentachloro-s ring three is formed into the phosphonitrile of ethyoxyl pentachloro- ring three in 200mL acetonitriles
Solution, 27g sodium fluorides are added into solution and are used as fluorization agent, addition 2g expanded graphites are as catalyst, and in 30 DEG C of temperature strips
20h is reacted under part, obtains the phosphonitrile of five fluorine ring of phosphazene derivative ethyoxyl three, yield 99% after filtered, vacuum distillation, purity is
97%.
Embodiment 13
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution, Xiang Rong in 200mL tetrahydrofurans
27g sodium fluorides are added in liquid and are used as catalyst as fluorization agent, addition 2g poly glycol monomethyl ethers 800, and in 30 DEG C of temperature strips
1h is reacted under part, the phosphonitrile of phosphazene derivative hexafluoro ring three, yield 99%, purity 85% are obtained after filtered, vacuum distillation.
Embodiment 14
34.7g hexachlorocyclotriph,sphazenes dissolution of crystals is formed into hexachlorocyclotriph,sphazene solution, Xiang Rong in 200mL tetrahydrofurans
27g sodium fluorides are added in liquid as fluorization agent, the obtained precipitation after embodiment 1 is filtered is as catalyst, and in 30 DEG C of temperature
10h is reacted under the conditions of degree, obtains the phosphonitrile of phosphazene derivative hexafluoro ring three, yield 98% after filtered, vacuum distillation, purity is
97%.
The preferred embodiment of the application is the foregoing is only, is not limited to the application, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of catalyst produced for fluoro phosphonitrile and its derivatives industry metaplasia, it is characterized in that, the catalyst is applied to
Chloro phosphonitrile and its derivative prepare the fluorination reaction of fluoro phosphonitrile and its derivative, the catalyst be technical grade graphene,
Mixture more than one or both of graphene oxide, fullerene, Mxene, hydroxyl carbon nano tube, expanded graphite.
2. the synthetic method of a kind of fluoro phosphonitrile and its derivative, it is characterized in that, chloro phosphonitrile or fluoro phosphazene derivative is molten
In organic solvent, the catalyst described in addition fluorization agent and claim 1 is reacted solution, after filtering distillation, produces fluoro
Phosphonitrile and its derivative.
3. synthetic method as claimed in claim 2, it is characterized in that, the reaction time is 1~20h.
4. synthetic method as claimed in claim 2, it is characterized in that, the reaction temperature is 30~120 DEG C.
5. synthetic method as claimed in claim 2, it is characterized in that, the addition of the catalyst is chloro phosphonitrile and fluorization agent
The 1~20% of gross mass, or the 1~20% of fluoro phosphazene derivative and fluorization agent gross mass.
6. synthetic method as claimed in claim 2, it is characterized in that, the chloro phosphonitrile or fluoro phosphazene derivative and fluorization agent
The ratio between the amount of material be 1:1~1.5.
7. synthetic method as claimed in claim 2, it is characterized in that, the fluorization agent be one kind in sodium fluoride and potassium fluoride or
Its two kinds mixture.
8. synthetic method as claimed in claim 2, it is characterized in that, the organic solvent be tetrahydrofuran, n-hexane, toluene,
Mixture more than one or both of chlorobenzene, petroleum ether, pyridine, N,N-dimethylformamide, acetonitrile or benzonitrile.
9. a kind of any described synthetic method of claim 2~8 is preparing fluoro phosphonitrile or derivatives thereof class battery electrolyte
In application.
A kind of 10. any described synthetic method of claim 2~8 answering in fluoro phosphonitrile or derivatives thereof class battery is prepared
With.
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| 杨永清 等: "石墨及其改性产物研究进展", 《材料导报A：综述篇》 * |
| 白烨 等: "羟基化碳纳米管对亚甲基蓝的吸附作用", 《广州化工》 * |
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| CN107649112B (en) | 2019-08-02 |
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