- Preparation method of pentafluoro ethoxy cyclotriphosphazene
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The invention relates to the field of organic chemistry, in particular to a preparation method of pentafluoro ethoxy cyclotriphosphazene. The provided preparation method of pentafluoro ethoxy cyclotriphosphazene comprises the steps of 1, a fluorination reaction, wherein hexachloro cyclotriphosphazene reacts with hydrogen fluoride in the presence of a catalyst to prepare hexafluoro cyclotriphosphazene; 2, an etherification reaction, wherein the hexafluoro cyclotriphosphazene reacts with sodium alkoxide to prepare the pentafluoro ethoxy cyclotriphosphazene. The preparation method of the pentafluoro ethoxy cyclotriphosphazene has the advantages of being simple in reaction steps, reasonable in cost and suitable for large-scale industrialization.
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Paragraph 0043; 0062-0083
(2019/08/15)
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- Preparation method of pentafluoroethoxycyclotriphosphazene
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The invention discloses a preparation method of pentafluoroethoxycyclotriphosphazene. The preparation method comprises the following steps: (1) adding reactants including hexafluorocyclotriphosphazeneand ethanol to an organic solvent, and adding a catalyst and an acid binding agent so as to obtain a reaction liquid after completion of a reaction; and (2) filtering the reaction liquid so as to obtain a filtrate, and rectifying the filtrate so as to obtain the target product pentafluoroethoxycyclotriphosphazene, wherein the organic solvent is an arbitrary one of n-hexane, cyclohexane, toluene,xylene, chlorobenzene, acetonitrile, acetone, tetrahydrofuran, dioxane, petroleum ether, ethyl acetate, dichloroethane, dimethyl carbonate and diethyl carbonate, and the catalyst comprises a main catalyst and a cocatalyst; and the main catalyst is alkali metal iodide, the cocatalyst is a phase transfer catalyst, and the acid binding agent is an arbitrary one of sodium carbonate, potassium carbonate, ammonia and triethylamine. The preparation method of pentafluoroethoxycyclotriphosphazene has a low reaction temperature, few by-products and a high conversion rate.
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Paragraph 0033-0037
(2019/03/28)
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- Preparation method of pentafluoroalkoxyl cyclotriphosphazene
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The invention discloses a preparation method of pentafluoroalkoxyl cyclotriphosphazene. The preparation method comprises the following steps: (1) adding hexachlorocyclotriphosphazene, a fluorinating agent and an organic solvent into a reaction container for reaction at a temperature between -30 DEG C and 80 DEG C to obtain a reaction solution containing hexafluorocyclotriphosphazene; (2) washing the reaction solution obtained in the step (1) with water, then carrying out standing for liquid separation to obtain an organic phase containing hexafluorocyclotriphosphazene, and distilling the organic phase to obtain the hexafluorocyclotriphosphazene; (3) adding an organic solvent, an alcohol, an acid binding agent and the hexafluorocyclotriphosphazene obtained in the step (2) into another reaction container to react at a temperature between -30 DEG C and 80 DEG C to obtain a reaction solution containing pentafluoroalkoxyl cyclotriphosphazene; (4) rectifying the reaction solution obtained inthe step (3) to obtain the pentafluoroalkoxyl cyclotriphosphazene. The method provided by the invention has the advantages of less side reactions and high yield of pentafluoroalkoxyl cyclotriphosphazene, has the high yield higher than 62%, and is suitable for industrial large-scale production.
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Paragraph 0016-0031
(2018/03/24)
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- Fluoridation catalyst of phosphonitrile and phosphonitrile derivative and synthetic method of fluoride
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The invention discloses a catalyst for fluoridation of phosphonitrile and a phosphonitrile derivative and a synthetic method of fluoride. The method comprises the following steps: dissolving chlorophosphonitrile or its derivative in an organic solvent, adding a fluorating agent and a catalyst and reacting for 1-48 h to obtain fluorophosphonitrile and a derivative thereof. The catalyst accounts for1-40% of total mass of the raw materials. The catalyst is an ionic liquid, has high melting/boiling point, is stable and green and environmentally-friendly, and has high catalytic efficiency. In addition, yield is greatly raised, and average yield reaches 98% and above.
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Paragraph 0037-0038; 0041-0042; 0045-0046; 0049-0050; 0053
(2018/03/24)
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- A Fluorination Method for Phosphonitrilic Chloride Trimer and Its Derivatives
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The present invention relates to a fluorination method for phosphonitrilic chloride trimer and its derivatives including using phosphonitrilic chloride or partially substituted phosphonitrilic chloride trimer as raw material to fluorinate with fluoridating agent in an ionic liquid to replace the chlorine in chloro-cyclotiphosphazene molecule. The present invention uses non-volatile and pollution free ionic liquids as solvent, and just controls a distillation temperature to get a hexafluorocyclotriphosphazene or derivatives thereof with high-purity. It overcomes the shortcoming of the average solvent system that the solvent forms azeotrope with products. The post-process is simple. The production rate is high, and the ionic liquid can be recycled. The present invention produces products with high purity.
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Paragraph 0018
(2018/05/17)
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- A synthetic method of alkoxy(pentafluoro) or phenoxyl(pentafluoro) cyclotriphosphazene
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A synthetic method of alkoxy(pentafluoro) or phenoxyl(pentafluoro) cyclotriphosphazene is disclosed. The method includes (1) a step of subjecting hexachlorocyclotriphosphazene that is adopted as a raw material to a fluorination reaction in an organic solvent under a heating reflux state to obtain hexafluorocyclotriphosphazene by using an inorganic fluoride salt, and directly preparing the hexafluorocyclotriphosphazene through distillation and rectification; and (2) subjecting the hexafluorocyclotriphosphazene and an ethanol or a catalytic amount of a sodium alkoxide solution to a reaction under stirring at room temperature for 1-3 h, and performing vacuum distillation to obtain the alkoxy(pentafluoro) cyclotriphosphazene or phenoxyl(pentafluoro) cyclotriphosphazene. Product purity is 99% (GC). The method has characteristics of mild reaction conditions, low energy consumption, and simple process steps. A product of the step (1) can be directly used for the next reaction without the need of purification.
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Paragraph 0018; 0020
(2017/08/28)
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- Five tertrafluoroethylene or phenoxy link method for preparing three Phosphazenium
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The invention relates to a preparation method of pentafluoroalkoxy or phenoxy cyclotriphosphazene. The preparation method comprises the steps of taking hexachlorocyclotriphosphazene as raw material, using the nucleophilic reagent alkoxide (or phenoxide) t
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Paragraph 0017; 0019
(2016/10/07)
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- Preparation method of phosphonitrile fluoride trimer, and preparation method of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene
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The invention belongs to the technical field of preparation methods of phosphonitrile derivatives, and concretely relates to a preparation method of phosphonitrile fluoride trimer, and a preparation method of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene. The preparation method of phosphonitrile fluoride trimer is characterized in that tris(phosphorusnitridedifluoride) is obtained through a reaction of pyridine hydrofluoride and phosphonitrilic chloride trimer at a low temperature. The preparation method of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene is characterized in that the product 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene is obtained through a reaction of the obtained phosphonitrile fluoride trimer and ethylate. The preparation method of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene has the advantages of mild conditions in a perfluorination step, easiness in realization, and high yield of the 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene, and is a feasible preparation method for industrially producing ethoxypentafluorocyclotriphosphazene.
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Paragraph 0032; 0033; 0034; 0035; 0036; 0037; 0038-0043
(2017/05/23)
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- Method for producing amino-substituted phosphazene compound, method for producing electrolyte solution for non-aqueous secondary batteries, and method for manufacturing non-aqueous secondary battery
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A method for producing an amino-substituted phosphazene compound is provided, wherein a fluorinated phosphazene compound and an amine compound are reacted with each other in the presence of a Lewis acid catalyst, so that a compound is synthesized by substituting the fluorinated phosphazene compound with the amine compound.
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Paragraph 0261; 0262; 0263; 0264
(2016/10/10)
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