CN110845540A - Preparation method and preparation device of hexaphenoxycyclotriphosphazene - Google Patents
Preparation method and preparation device of hexaphenoxycyclotriphosphazene Download PDFInfo
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- CN110845540A CN110845540A CN201911084234.8A CN201911084234A CN110845540A CN 110845540 A CN110845540 A CN 110845540A CN 201911084234 A CN201911084234 A CN 201911084234A CN 110845540 A CN110845540 A CN 110845540A
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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
Abstract
The invention discloses a preparation method of hexaphenoxycyclotriphosphazene, which comprises the following steps: mixing the solutions of hexachlorocyclotriphosphazene and sodium phenolate, reacting the two solutions to obtain a solid-liquid mixture, carrying out solid-liquid separation on the solid-liquid mixture, feeding the obtained separation liquid into a distillation tower with a filter screen arranged therein in a spraying manner, controlling the distillation temperature to quickly vaporize the organic solvent and discharge the organic solvent from the upper part of the distillation tower so that the hexachlorocyclotriphosphazene is in a liquid state and is discharged from the bottom of the distillation tower, and leaving the unreacted sodium phenolate on the filter screen in a solid state; washing the liquid hexaphenoxycyclotriphosphazene with low-carbon alcohol, and then carrying out solid-liquid separation to obtain a solid hexaphenoxycyclotriphosphazene. The method has the advantages of simple process, high synthesis efficiency and no wastewater generation.
Description
Technical Field
The invention relates to a preparation method of a hexaphenoxycyclotriphosphazene flame retardant with high purity and high yield, belonging to the technical field of synthesis of phosphazene compounds.
Background
The hexaphenoxycyclotriphosphazene is an annular phosphazene compound, is light yellow or white-like powder or crystal, is a halogen-free flame retardant, has the outstanding characteristics of high thermal decomposition temperature, excellent flame retardant effect, low smoke generation amount and toxic gas generation amount, good compatibility with high polymer materials and the like, and is widely applied to the industries of engineering plastics, high-end high-voltage cables, copper-clad plates and the like.
There are many research reports about hexaphenoxycyclotriphosphazene at home and abroad, and the current general process adopts hexachlorocyclotriphosphazene to react with sodium phenolate to generate a target product. In the phenoxy substitution process, the steric hindrance effect can cause the lack of the phenoxy substitution degree to further influence the yield of hexaphenoxy cyclotriphosphazene, and the phenoxy substitution degree is generally improved by adopting the measures of increasing the reaction temperature, increasing the concentration of sodium phenolate, prolonging the reaction time and the like. The key of the process is to improve the substitution degree of the phenoxy as much as possible and improve the yield and the purity of the product. The existing production process mainly adopts a kettle type reactor, and the reaction is carried out under the condition of complete mixing.
For example, in US patent US4600791, a chloroalkane (or chloroarene) solution containing hexachlorocyclotriphosphazene and having a high boiling point is added dropwise to an aqueous solution of phenol, potassium hydroxide and quaternary ammonium salt, and after 21 hours of reaction, the mixture is allowed to stand for layering, and then subjected to primary acid washing, alkali washing, water washing, drying and solvent removal to obtain a product. The phase transfer catalysis method has the advantages of low reaction speed, long reaction time, poor product quality, high impurity content of low substituent, high yield of only 70-80 percent, high cost and no contribution to industrial conversion.
For example, in chinese patent CN106336435B, a chlorobenzene solution containing hexachlorocyclotriphosphazene is added dropwise to a chlorobenzene solution of phenol, a phase transfer catalyst, solid beads, and sodium hydroxide, and after reaction for 7 to 13 hours, the product is obtained by cooling, filtering, washing with water, removing a solvent, crystallizing with absolute ethanol, filtering, and drying. The method for promoting solid-liquid two-phase transfer catalysis by grinding reduces the dosage of the catalyst and shortens the reaction time to a certain extent. The disadvantage is that the addition of solid beads affects the service life of the reaction vessel and is not conducive to industrial conversion.
For example, Chinese patent CN103588815B is prepared by adding dropwise tetrahydrofuran solution containing hexachlorocyclotriphosphazene into tetrahydrofuran solution of sodium phenolate, reacting for 10-30 h, standing for layering, filtering, concentrating, recrystallizing, purifying, and drying. The homogeneous system has low reaction temperature, long reaction time, difficult recovery of reaction solvent, high product yield of only 85 percent and high cost, and is not beneficial to industrial conversion.
Disclosure of Invention
The invention aims to provide a synthesis method of hexaphenoxycyclotriphosphazene.
In order to realize the aim, the preparation method of hexaphenoxycyclotriphosphazene provided by the invention comprises the following steps:
(1) directly dissolving hexachlorocyclotriphosphazene and sodium phenolate which is excessively used relative to hexachlorocyclotriphosphazene in an organic solvent or respectively dissolving hexachlorocyclotriphosphazene and sodium phenolate which is excessively used relative to hexachlorocyclotriphosphazene in the organic solvent to form a solution, mixing the hexachlorocyclotriphosphazene and the organic solvent solution of sodium phenolate to react the hexachlorocyclotriphosphazene and the sodium phenolate, and obtaining a mixture of the organic solvent solution containing the hexachlorocyclotriphosphazene and sodium chloride after the reaction is finished;
(2) carrying out solid-liquid separation on the mixture obtained in the step (1), and distilling the separated liquid obtained after the solid-liquid separation by using a distillation tower with a built-in filter screen, namely: feeding the separation liquid into an inner cavity of a distillation tower above a filter screen in a spraying manner, controlling the distillation temperature to be in a temperature range from the melting point of hexaphenoxycyclotriphosphazene to the decomposition temperature of less than the hexaphenoxycyclotriphosphazene, quickly vaporizing the organic solvent and discharging the organic solvent from the upper part of the distillation tower, so that the hexaphenoxycyclotriphosphazene is changed into a liquid state and is discharged from the bottom of the distillation tower, and the unreacted sodium phenolate is remained on the filter screen in a solid state;
(3) cooling the liquid hexaphenoxycyclotriphosphazene, and washing with low-carbon alcohol, or directly feeding the liquid hexaphenoxycyclotriphosphazene into the low-carbon alcohol for washing; and (3) carrying out solid-liquid separation after washing is finished, wherein the obtained solid is hexaphenoxycyclotriphosphazene.
The molar ratio of the hexachlorocyclotriphosphazene to the sodium phenolate is 1: 6.5-8.
The reaction conditions of the hexachlorocyclotriphosphazene and the sodium phenolate are as follows: the temperature is 60-80 deg.C, the pressure is 0.5-1 Mpa, and the time is 60-120 min.
The organic solvent is tetrahydrofuran.
The lower alcohol is one or a mixture of more than two of methanol, ethanol and isopropanol.
The distillation temperature is 115-130 ℃.
The preparation method can be realized by a preparation device with the following structure, wherein the preparation device comprises a hexachlorocyclotriphosphazene raw material tank, a sodium phenolate raw material tank, a mixer, a reactor, a pre-filter, a distillation tower, a washing kettle and a post-filter which are sequentially arranged according to a process route; the distillation tower comprises a tower body, a filter screen layer which divides the inner cavity of the tower body into an upper cavity and a lower cavity is arranged in the tower body, the filter screen layer is composed of a plurality of filter screens which are arranged at intervals up and down, the top of the tower body is provided with an air outlet, the bottom of the tower body is provided with a liquid outlet, and a spray head is arranged in the upper cavity of the tower body; the discharge gate of hexachlorocyclotriphosphazene head tank and sodium phenolate head tank and the feed inlet of blender communicate, the discharge gate of blender and the feed inlet of reactor communicate, the discharge gate of reactor and the feed inlet of preceding filter communicate, the filtrating discharge gate and the shower head intercommunication of preceding filter, the leakage fluid dram and the washing cauldron intercommunication of tower body, the discharge gate and the back filter intercommunication of washing cauldron.
An exhaust port at the top of the distillation tower body is communicated with a condenser, and the condenser is communicated with a solvent recovery tank; and a filtrate outlet of the post-filter is communicated with the detergent recovery tank.
The washing kettle is also communicated with a detergent tank.
The reactor is a tubular reactor, and the mixer is a static mixer.
The invention has the advantages that: the method has the advantages of simple process and high synthesis efficiency, the yield of the hexaphenoxycyclotriphosphazene reaches over 88 percent, the purity reaches over 99 percent, and no wastewater is generated. The preparation device provided by the invention is used for preparing hexaphenoxycyclotriphosphazene, so that the reaction time can be greatly shortened, the continuous production can be realized, and the solvent can be conveniently recovered.
Drawings
FIG. 1 is a schematic view of the structural principle of a manufacturing apparatus.
Detailed Description
The method can be realized by a preparation device with the following structure, as shown in figure 1, the preparation device comprises a hexachlorocyclotriphosphazene raw material tank 1, a sodium phenolate raw material tank 2, a mixer 3, a reactor 4, a pre-filter 5, a distillation tower 6, a washing kettle 7 and a post-filter 8 which are sequentially arranged according to a process route. The hexachlorocyclotriphosphazene raw material tank 1 is used for storing hexachlorocyclotriphosphazene solution, and the sodium phenolate raw material tank 2 is used for storing sodium phenolate solution; the washing kettle 7 is similar to the existing reaction kettle and comprises a kettle body, wherein a stirring device is arranged in the kettle body, namely, the washing kettle 7 can adopt the existing reaction kettle with the stirring device; the reactor 4 may be an existing tubular reactor, and the mixer 3 may be an existing static mixer. The pre-filter 5 and the post-filter 8 may be any filter capable of separating solid from liquid, such as a filter press or a centrifugal solid-liquid separator. The distillation tower 6 comprises a tower body, a heating device (omitted in the figure) is arranged on the outer wall of the tower body, a filter screen layer which divides the inner cavity of the tower body into an upper cavity 14 and a lower cavity 15 is arranged in the tower body, the filter screen layer is composed of a plurality of filter screens 13 which are arranged at intervals up and down, an exhaust port 16 is arranged at the top of the tower body, a liquid discharge port 17 is arranged at the bottom of the tower body, and a spray head 18 is; discharge gates of hexachlorocyclotriphosphazene raw material tank 1 and sodium phenolate raw material tank 2 are respectively communicated with two feed inlets of mixer 3, the discharge gate of mixer 3 is communicated with the feed inlet of reactor 4, the discharge gate of reactor 4 is communicated with the feed inlet of front filter 5, the filtrate discharge gate of front filter 5 is communicated with spray header 18, liquid discharge port 17 of the tower body is communicated with washing kettle 7, and the discharge gate of washing kettle 7 is communicated with rear filter 8. In order to facilitate the recovery of the gas discharged from the top of the distillation tower, a gas outlet 16 at the top of the tower body of the distillation tower 6 is communicated with a condenser 9, and the condenser 9 is communicated with a solvent recovery tank 10. To facilitate the recovery of the detergent, the filtrate outlet of the post-filter 8 is in communication with a detergent recovery tank 11. In order to facilitate the addition of detergent to the washing vessel 7, the washing vessel 7 is also connected to a detergent tank 12.
The following detailed description of the method for preparing hexaphenoxycyclotriphosphazene provided by the present invention is provided in conjunction with the preparation apparatus shown in FIG. 1 and described in the above paragraph, so as to make the skilled in the art more clearly understand the essence of the present invention, without limiting the scope of the present invention to the specific description of the examples.
Example 1
The preparation method of hexaphenoxycyclotriphosphazene comprises the following steps:
(1) adding a tetrahydrofuran solution of hexachlorocyclotriphosphazene with the concentration of 1 mol/L into a hexachlorocyclotriphosphazene raw material tank 1, and adding a tetrahydrofuran solution of sodium phenolate with the concentration of 1 mol/L into a sodium phenolate raw material tank 2; then simultaneously conveying the tetrahydrofuran solution of hexachlorocyclotriphosphazene and the tetrahydrofuran solution of sodium phenolate into a mixer 3 according to the volume flow ratio of 1:6.5 for mixing to form a mixed solution, wherein the mixing temperature is controlled at 10 ℃; and the mixed solution flows out of the mixer 3 and enters a reactor 4 (a tubular reactor), the flow rate of the mixed solution in the reactor 4 is controlled, the hexachlorocyclotriphosphazene and the sodium phenolate react for 60 min under the reaction conditions that the temperature is 60 ℃ and the pressure is 0.5 Mpa, and the mixture of tetrahydrofuran solution of the hexaphenoxycyclotriphosphazene and sodium chloride is obtained after the reaction.
(2) The mixture of tetrahydrofuran solution of hexaphenoxycyclotriphosphazene and sodium chloride flows into a front filter 5 after flowing out from a reactor 4, separation liquid, namely filtrate is obtained after solid-liquid separation of the front filter 5, the filtrate is sent to a spray head 18 in a distillation tower 6, the filtrate enters an upper cavity 14 of the distillation tower 6 in a spraying mode, the distillation temperature is controlled to be 120 ℃, the tetrahydrofuran is rapidly vaporized, the hexaphenoxycyclotriphosphazene separated in the rapid vaporization process of the tetrahydrofuran is changed into liquid, the separated sodium phenolate which is not reacted is changed into solid, the liquid hexaphenoxycyclotriphosphazene passes through a filter screen to reach the bottom of the distillation tower 6, namely to enter a lower cavity 15 of the distillation tower 6, the solid sodium phenolate is remained on the filter screen 13 under the blockage of the filter screen 13, and the gaseous tetrahydrofuran enters a condenser 9 from an exhaust port 16 at the top of the distillation tower 6, condensed to become liquid and flow into the solvent recovery tank 10.
(3) The liquid hexaphenoxy cyclotriphosphazene at the bottom of the distillation tower 6 flows into the washing kettle 7 through a liquid outlet 17, the washing kettle 7 is used for washing with absolute ethyl alcohol under stirring, the liquid hexaphenoxy cyclotriphosphazene is cooled and crystallized into a solid state in the washing process, and a solid-liquid mixture is obtained after the washing is finished; the solid-liquid mixture flows into a post-filter 8 through a discharge hole of a washing kettle 7, after solid-liquid separation is carried out by the post-filter 8, the obtained solid is hexaphenoxycyclotriphosphazene, the obtained liquid is recovered absolute ethyl alcohol, and the recovered absolute ethyl alcohol flows into a detergent recovery tank 11 through a filtrate outlet of the filter 8. In this example, the yield of hexaphenoxycyclotriphosphazene was 88.0%, and the purity of hexaphenoxycyclotriphosphazene was 99.0%.
Example 2
The preparation method of hexaphenoxycyclotriphosphazene comprises the following steps:
(1) adding a tetrahydrofuran solution of hexachlorocyclotriphosphazene with the concentration of 1 mol/L into a hexachlorocyclotriphosphazene raw material tank 1, and adding a tetrahydrofuran solution of sodium phenolate with the concentration of 1 mol/L into a sodium phenolate raw material tank 2; then simultaneously conveying the tetrahydrofuran solution of hexachlorocyclotriphosphazene and the tetrahydrofuran solution of sodium phenolate into a mixer 3 according to the volume flow ratio of 1:7 for mixing to form a mixed solution, wherein the mixing temperature is controlled at 20 ℃; and the mixed solution flows out of the mixer 3 and enters a reactor 4 (a tubular reactor), the flow rate of the mixed solution in the reactor 4 is controlled, the hexachlorocyclotriphosphazene and the sodium phenolate react for 90 min under the reaction conditions that the temperature is 70 ℃ and the pressure is 0.7Mpa, and the mixture of tetrahydrofuran solution of the hexaphenoxycyclotriphosphazene and sodium chloride is obtained after the reaction.
(2) The mixture of tetrahydrofuran solution of hexaphenoxycyclotriphosphazene and sodium chloride flows into a front filter 5 after flowing out from a reactor 4, separation liquid, namely filtrate is obtained after solid-liquid separation of the front filter 5, the filtrate is sent to a spray head 18 in a distillation tower 6, the filtrate enters an upper cavity 14 of the distillation tower 6 in a spraying mode, the distillation temperature is controlled to be 125 ℃, the tetrahydrofuran is rapidly vaporized, the hexaphenoxycyclotriphosphazene separated in the rapid vaporization process of the tetrahydrofuran is changed into liquid, the separated sodium phenolate which is not reacted is changed into solid, the liquid hexaphenoxycyclotriphosphazene passes through a filter screen to reach the bottom of the distillation tower 6, namely to enter a lower cavity 15 of the distillation tower 6, the solid sodium phenolate is remained on the filter screen 13 under the blockage of the filter screen 13, and the gaseous tetrahydrofuran enters a condenser 9 from an exhaust port 16 at the top of the distillation tower 6, condensed to become liquid and flows into a solvent recovery tank 10;
(3) the liquid hexaphenoxy cyclotriphosphazene at the bottom of the distillation tower 6 flows into the washing kettle 7 through a liquid outlet 17, the washing kettle 7 is used for washing with anhydrous methanol under stirring, the liquid hexaphenoxy cyclotriphosphazene is cooled and crystallized into a solid state in the washing process, and a solid-liquid mixture is obtained after the washing is finished; the solid-liquid mixture flows into a post-filter 8 through a discharge hole of a washing kettle 7, after solid-liquid separation is carried out by the post-filter 8, the obtained solid is hexaphenoxycyclotriphosphazene, the obtained liquid is recovered anhydrous methanol, and the recovered anhydrous methanol flows into a detergent recovery tank 11 through a filtrate outlet of the filter 8. In this example, the yield of hexaphenoxycyclotriphosphazene was 89.5%, and the purity of hexaphenoxycyclotriphosphazene was 99.1%.
Example 3
The preparation method of hexaphenoxycyclotriphosphazene comprises the following steps:
(1) adding a tetrahydrofuran solution of hexachlorocyclotriphosphazene with the concentration of 1 mol/L into a hexachlorocyclotriphosphazene raw material tank 1, and adding a tetrahydrofuran solution of sodium phenolate with the concentration of 1 mol/L into a sodium phenolate raw material tank 2; then simultaneously conveying the tetrahydrofuran solution of hexachlorocyclotriphosphazene and the tetrahydrofuran solution of sodium phenolate into a mixer 3 according to the volume flow ratio of 1:8 for mixing to form a mixed solution, wherein the mixing temperature is controlled at 30 ℃; and the mixed solution flows out of the mixer 3 and enters a reactor 4 (a tubular reactor), the flow rate of the mixed solution in the reactor 4 is controlled, the hexachlorocyclotriphosphazene and the sodium phenolate react for 120 min under the reaction conditions that the temperature is 80 ℃ and the pressure is 1Mpa, and the mixture of tetrahydrofuran solution of the hexaphenoxycyclotriphosphazene and sodium chloride is obtained after the reaction.
(2) The mixture of tetrahydrofuran solution of hexaphenoxycyclotriphosphazene and sodium chloride flows into a front filter 5 after flowing out from a reactor 4, separation liquid, namely filtrate is obtained after solid-liquid separation of the front filter 5, the filtrate is sent to a spray head 18 in a distillation tower 6, the filtrate enters an upper cavity 14 of the distillation tower 6 in a spraying mode, the distillation temperature is controlled at 130 ℃, the tetrahydrofuran is rapidly vaporized, the hexaphenoxycyclotriphosphazene separated in the rapid vaporization process of the tetrahydrofuran is changed into liquid, the separated sodium phenolate which is not reacted is changed into solid, the liquid hexaphenoxycyclotriphosphazene passes through a filter screen to reach the bottom of the distillation tower 6, namely to enter a lower cavity 15 of the distillation tower 6, the solid sodium phenolate is remained on the filter screen 13 under the blockage of the filter screen 13, and the gaseous tetrahydrofuran enters a condenser 9 from an exhaust port 16 at the top of the distillation tower 6, condensed to become liquid and flows into a solvent recovery tank 10;
(3) the liquid hexaphenoxy cyclotriphosphazene at the bottom of the distillation tower 6 flows into the washing kettle 7 through a liquid outlet 17, the washing kettle 7 is used for washing with anhydrous isopropanol under stirring, the liquid hexaphenoxy cyclotriphosphazene is cooled and crystallized into a solid state in the washing process, and a solid-liquid mixture is obtained after the washing is finished; the solid-liquid mixture flows into the post-filter 8 through a discharge hole of the washing kettle 7, after solid-liquid separation is carried out by the post-filter 8, the obtained solid is hexaphenoxycyclotriphosphazene, the obtained liquid is recovered anhydrous isopropanol, and the recovered anhydrous isopropanol flows into the detergent recovery tank 11 through a filtrate outlet of the filter 8. In this example, the yield of hexaphenoxycyclotriphosphazene was 90%, and the purity of hexaphenoxycyclotriphosphazene was 99.0%.
In the above embodiment, the content of hexaphenoxycyclotriphosphazene is determined by high performance liquid chromatography, and the conditions of the liquid chromatography are as follows: a C18 column (250 mm. times.4.6 mm. times.5 μm); mobile phase: v (acetonitrile)/V (water) = 85/15; flow rate: 1.0 ml/min; column temperature: room temperature; detection wavelength: 210 nm. The liquid chromatograph used was an Agilent model 1200 high performance liquid chromatograph from Agilent, inc.
Claims (6)
1. A preparation method of hexaphenoxycyclotriphosphazene is characterized by comprising the following steps:
(1) directly dissolving hexachlorocyclotriphosphazene and sodium phenolate which is excessively used relative to hexachlorocyclotriphosphazene in an organic solvent or respectively dissolving hexachlorocyclotriphosphazene and sodium phenolate which is excessively used relative to hexachlorocyclotriphosphazene in the organic solvent to form a solution, mixing the hexachlorocyclotriphosphazene and the organic solvent solution of sodium phenolate to react the hexachlorocyclotriphosphazene and the sodium phenolate, and obtaining a mixture of the organic solvent solution containing the hexachlorocyclotriphosphazene and sodium chloride after the reaction is finished;
(2) carrying out solid-liquid separation on the mixture obtained in the step (1), and distilling the separated liquid obtained after the solid-liquid separation by using a distillation tower with a built-in filter screen, namely: feeding the separation liquid into an inner cavity of a distillation tower above a filter screen in a spraying manner, controlling the distillation temperature to be in a temperature range from the melting point of hexaphenoxycyclotriphosphazene to the decomposition temperature of less than the hexaphenoxycyclotriphosphazene, quickly vaporizing the organic solvent and discharging the organic solvent from the upper part of the distillation tower, so that the hexaphenoxycyclotriphosphazene is changed into a liquid state and is discharged from the bottom of the distillation tower, and the unreacted sodium phenolate is remained on the filter screen in a solid state;
(3) cooling the liquid hexaphenoxycyclotriphosphazene, and washing with low-carbon alcohol, or directly feeding the liquid hexaphenoxycyclotriphosphazene into the low-carbon alcohol for washing; and (3) carrying out solid-liquid separation after washing is finished, wherein the obtained solid is hexaphenoxycyclotriphosphazene.
2. The method of preparing hexaphenoxycyclotriphosphazene as claimed in claim 1, wherein: the molar ratio of the hexachlorocyclotriphosphazene to the sodium phenolate is 1: 6.5-8.
3. The method of preparing hexaphenoxycyclotriphosphazene as claimed in claim 1, wherein: the reaction conditions of the hexachlorocyclotriphosphazene and the sodium phenolate are as follows: the temperature is 60-80 deg.C, the pressure is 0.5-1 Mpa, and the time is 60-120 min.
4. The method of preparing hexaphenoxycyclotriphosphazene as claimed in claim 1, wherein: the organic solvent is tetrahydrofuran.
5. The method of preparing hexaphenoxycyclotriphosphazene as claimed in claim 1, wherein: the lower alcohol is one or a mixture of more than two of methanol, ethanol and isopropanol.
6. The method of preparing hexaphenoxycyclotriphosphazene as claimed in claim 1, wherein: the distillation temperature is 115-130 ℃.
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| CN115044104A (en) * | 2022-07-15 | 2022-09-13 | 什邡市太丰新型阻燃剂有限责任公司 | Preparation method of phosphazene-coated aluminum hypophosphite |
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