CN113004332B - Preparation method of hexafluorocyclotriphosphazene - Google Patents
Preparation method of hexafluorocyclotriphosphazene Download PDFInfo
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- CN113004332B CN113004332B CN201911324114.0A CN201911324114A CN113004332B CN 113004332 B CN113004332 B CN 113004332B CN 201911324114 A CN201911324114 A CN 201911324114A CN 113004332 B CN113004332 B CN 113004332B
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- ethylene glycol
- hexafluorocyclotriphosphazene
- hexachlorocyclotriphosphazene
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- DKQPXAWBVGCNHG-UHFFFAOYSA-N 2,2,4,4,6,6-hexafluoro-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound FP1(F)=NP(F)(F)=NP(F)(F)=N1 DKQPXAWBVGCNHG-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 19
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 7
- 239000012454 non-polar solvent Substances 0.000 claims abstract description 7
- 239000012025 fluorinating agent Substances 0.000 claims abstract description 5
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical group [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 28
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 20
- 235000003270 potassium fluoride Nutrition 0.000 claims description 14
- 239000011698 potassium fluoride Substances 0.000 claims description 14
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 42
- 238000009835 boiling Methods 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 description 17
- 238000010992 reflux Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002798 polar solvent Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical class OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical class CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 description 1
- -1 phosphonitrile compound Chemical class 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
Classifications
-
- 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 Table
- 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
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0201—Oxygen-containing compounds
- B01J31/0204—Ethers
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of hexafluorocyclotriphosphazene, which comprises the following steps: adding hexachlorocyclotriphosphazene and a fluorinating agent into a nonpolar solvent under the condition of a catalyst to carry out fluorination reaction to obtain hexachlorocyclotriphosphazene; the catalyst is a combined catalyst formed by ethylene glycol monomethyl ether and ethylene glycol monobutyl ether, and the mass ratio of the ethylene glycol monomethyl ether to the ethylene glycol monobutyl ether is 1: 0.1-10; the dosage of the combined catalyst is 0.1-20% of the mass of the hexachlorocyclotriphosphazene. The invention has the advantages that: the preparation time is short, the route is simple, the reaction is complete under the proportion and the dosage of a proper combined catalyst, and the adopted combined catalyst has a boiling point far higher than that of the product, so the combined catalyst is easy to separate from the product; the product has high yield and high purity.
Description
Technical Field
The invention relates to a preparation method of hexafluorocyclotriphosphazene.
Background
The phosphonitrile compound has excellent flame retardant property, and the hexafluorocyclotriphosphazene is an intermediate of a plurality of phosphonitrile compounds. The synthesis of the hexachlorocyclotriphosphazene has good application prospect.
Hexachlorocyclotriphosphazene having the formula:
the synthesis of the hexafluorocyclotriphosphazene is mostly carried out in a polar solvent, for example, in CN102757026A, KI is used as a catalyst, and the hexafluorocyclotriphosphazene is synthesized in the polar solvent. It is preferable that hexafluorocyclotriphosphazene is more active in a polar solvent and causes more side reactions when synthesizing other phosphazene derivatives, and thus, it is preferable that hexafluorocyclotriphosphazene is synthesized in a nonpolar solvent.
In CN105732718A, the hexachlorocyclotriphosphazene is synthesized in a nonpolar solvent by using polyethylene glycols as a catalyst, but the reaction time is long and the reaction is incomplete.
In order to overcome the drawbacks of the above reactions, the applicant has made constant tests. It is found that the above defects can be greatly improved by using a combination of a main catalyst and a cocatalyst, wherein the main catalyst is preferably one or more of ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether and tetraethylene glycol dimethyl ether, and the cocatalyst is preferably any one of methanol, ethanol, propanol, n-butanol and phenol. However, the disadvantage of low boiling point of the cocatalyst, which results in poor separation from the product during work-up of the product, is present, which leads to a product yield which is still not optimal.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a preparation method of hexafluorocyclotriphosphazene, which has the advantages of short preparation time, less side reaction, easy product separation and high yield.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of hexafluorocyclotriphosphazene comprises the following steps: adding hexachlorocyclotriphosphazene and a fluorinating agent into a nonpolar solvent under the condition of a catalyst to carry out fluorination reaction to obtain hexachlorocyclotriphosphazene; the catalyst is a combined catalyst formed by ethylene glycol monomethyl ether and ethylene glycol monobutyl ether, and the mass ratio of the ethylene glycol monomethyl ether to the ethylene glycol monobutyl ether is 1: 0.1-10; the dosage of the combined catalyst is 0.1 to 20 percent of the mass of the hexachlorocyclotriphosphazene.
Further, in the preparation method of hexafluorocyclotriphosphazene, the mass ratio of ethylene glycol monomethyl ether to ethylene glycol monobutyl ether is preferably 1: 0.5-5.
Further, in the preparation method of the hexafluorocyclotriphosphazene, the amount of the combined catalyst is 5-10% of the mass of the hexachlorocyclotriphosphazene.
Further, in the preparation method of hexafluorocyclotriphosphazene, the adopted nonpolar solvent is any one or a combination of n-hexane, cyclohexane, toluene, chlorobenzene, xylene and the like.
Further, in the above preparation method of hexafluorocyclotriphosphazene, the fluorinating agent is potassium fluoride or sodium fluoride.
Further, in the preparation method of hexafluorocyclotriphosphazene, the mass ratio of potassium fluoride or sodium fluoride to hexachlorocyclotriphosphazene is 1:1 to 1.2.
Further, in the preparation method of the hexafluorocyclotriphosphazene, the fluorination reaction is carried out at-30-60 ℃ for 1-2 hours.
Further, in the preparation method of the hexafluorocyclotriphosphazene, the fluorination reaction temperature is preferably-20 ℃ to 30 ℃.
The invention has the advantages that: the preparation time is short, the process route is simple, the reaction is complete under the proportion and the dosage of a proper combined catalyst, and the adopted combined catalyst has a boiling point far higher than that of the product, so the combined catalyst is easy to separate from the product; the product has high yield and high purity.
Detailed Description
The present invention is further described below by way of specific examples, but the present invention should not be construed as being limited thereto.
Example 1: adding 600g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to 0 ℃, adding 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, stirring uniformly, dropwise adding 10g of ethylene glycol monomethyl ether and 10g of ethylene glycol monobutyl ether, self-heating to 50 ℃ for reaction, cooling to 20 ℃, and preserving heat for reaction for 1 hour. The reaction solution has no hexachlorocyclotriphosphazene residue and the reaction is complete. Rectification is carried out to obtain 128g of hexafluorocyclotriphosphazene with a molar yield of 90.1%.
Example 2: adding 400g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to-10 ℃, adding 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, stirring uniformly, dropwise adding 16g of ethylene glycol monomethyl ether and 24g of ethylene glycol monobutyl ether, self-heating to 52 ℃ for reaction, cooling to 25 ℃, and preserving heat for reaction for 2 hours. The reaction solution has no hexachlorocyclotriphosphazene residue and the reaction is complete. Rectification was carried out to obtain 125g of hexafluorocyclotriphosphazene in a molar yield of 88.0%.
Example 3: adding 500g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to 20 ℃, adding 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, stirring uniformly, dropwise adding 20g of ethylene glycol monomethyl ether and 2g of ethylene glycol monobutyl ether, and reacting for 2 hours by self-heating to 30 ℃. 50% of hexachlorocyclotriphosphazene remains in the reaction solution, and the reaction is incomplete. Finally rectifying to obtain 70g of hexafluorocyclotriphosphazene with the molar yield of 49.3%. In this example, the catalyst ratio was 1:0.1, and the reaction was allowed to proceed, but the reaction was not completed, which was not preferable.
Example 4: adding 800g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to 20 ℃, adding 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, stirring uniformly, dropwise adding 3.6g of ethylene glycol monomethyl ether and 36.4g of ethylene glycol monobutyl ether, and reacting for 2 hours after the temperature is automatically raised to 40 ℃. 30% of hexachlorocyclotriphosphazene remains in the reaction solution, and the reaction is incomplete. Rectification was carried out to obtain 95g of hexafluorocyclotriphosphazene in a molar yield of 66.9%. In this example, the catalyst ratio was 1:10, and the reaction was allowed to proceed, but the reaction was not completed, which was not preferable.
Example 5: adding 600g of dimethylbenzene into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to-10 ℃, adding 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, uniformly stirring, dropwise adding 6.6g of ethylene glycol monomethyl ether and 13.3g of ethylene glycol monobutyl ether, reacting, self-heating to 56 ℃, and cooling to 20 ℃ for reacting for 1 hour. The reaction solution has no hexachlorocyclotriphosphazene residue and the reaction is complete. Rectification was carried out to give 132g of hexafluorocyclotriphosphazene in a molar yield of 93.0%.
Example 6: adding 600g of cyclohexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to 20 ℃, adding 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, stirring uniformly, adding 1.33g of ethylene glycol monomethyl ether and 0.67g of ethylene glycol monobutyl ether, and reacting for 2 hours after the temperature is automatically increased to 40 ℃. 60% of hexachlorocyclotriphosphazene remains in the reaction solution, and the reaction is incomplete. Rectification was carried out to obtain 50g of hexafluorocyclotriphosphazene in a molar yield of 35.2%. Too little catalyst is used and the reaction is incomplete.
Example 7: adding 600g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to-10 ℃, adding 200g of hexachlorocyclotriphosphazene and 240g of potassium fluoride, stirring uniformly, dropwise adding 10g of ethylene glycol monomethyl ether and 5g of ethylene glycol monobutyl ether, self-heating to 50 ℃ for reaction, cooling to-20 ℃, and preserving heat for reaction for 2 hours. The reaction solution has no hexachlorocyclotriphosphazene residue and the reaction is complete. Rectification was carried out to obtain 126g of hexafluorocyclotriphosphazene in a molar yield of 88.7%.
Example 8: adding 600g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to 20 ℃, adding 200g of hexachlorocyclotriphosphazene and 220g of potassium fluoride, stirring uniformly, dropwise adding 15g of ethylene glycol monomethyl ether and 5g of ethylene glycol monobutyl ether, heating to 30 ℃ for reaction, cooling to 20 ℃, and keeping the temperature for reaction for 2 hours. 50% of hexachlorocyclotriphosphazene remains in the reaction solution, and the reaction is incomplete. Rectification was carried out to obtain 68g of hexafluorocyclotriphosphazene in a molar yield of 47.9%.
Example 9: adding 600g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to 20 ℃, adding 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, stirring uniformly, dropwise adding 2g of ethylene glycol monomethyl ether and 2g of ethylene glycol monobutyl ether, reacting by raising the temperature to 30 ℃, cooling to 20 ℃, and preserving the temperature for reacting for 2 hours. 60% of hexachlorocyclotriphosphazene remains in the reaction solution, and the reaction is incomplete. Rectification was carried out to obtain 80g of hexafluorocyclotriphosphazene in a molar yield of 56.3%.
Example 10: adding 600g of n-hexane into a 2000mL three-neck flask provided with an electric stirrer, a reflux condenser tube and a thermometer, cooling to 20 ℃, adding 200g of hexachlorocyclotriphosphazene and 220g of potassium fluoride, stirring uniformly, dropwise adding 5g of ethylene glycol monomethyl ether and 30g of ethylene glycol monobutyl ether, reacting by self-heating to 30 ℃, cooling to 20 ℃, and preserving heat for reacting for 2 hours. 55% of hexachlorocyclotriphosphazene remains in the reaction solution, and the reaction is incomplete. 60g of hexafluorocyclotriphosphazene is obtained by rectification, and the molar yield is 42.2%.
Experiments prove that when the mass ratio of the ethylene glycol monomethyl ether to the ethylene glycol monobutyl ether of the combined catalyst is 1: 0.1-10, and the dosage of the combined catalyst is 0.1-20% of the mass of the hexachlorocyclotriphosphazene, the reaction can be carried out, but the reaction can not be carried out completely, and the yield is not necessarily high. However, when the mass ratio of the ethylene glycol monomethyl ether to the ethylene glycol monobutyl ether of the combined catalyst is 1: 0.5-5 and the dosage is 5% -10%, the reaction is complete, and the yield is high. If the ratio of the combined catalyst and the amount of the combined catalyst are not within the above ranges, the reaction is not complete and the yield is low.
The preparation method of the hexafluorocyclotriphosphazene has the advantages of short preparation time, simple route, complete reaction under the proportion and the dosage of a proper combined catalyst, and easy separation from a product because the boiling point of the combined catalyst is far higher than that of the product; the product has high yield and high purity.
Claims (6)
1. A preparation method of hexafluorocyclotriphosphazene comprises the following steps: adding hexachlorocyclotriphosphazene and a fluorinating agent into a nonpolar solvent under the condition of a catalyst to carry out fluorination reaction to obtain hexachlorocyclotriphosphazene; the catalyst is a combined catalyst formed by ethylene glycol monomethyl ether and ethylene glycol monobutyl ether; the mass ratio of the ethylene glycol monomethyl ether to the ethylene glycol monobutyl ether is 1: 0.5-5; the dosage of the combined catalyst is 5-10% of the mass of the hexachlorocyclotriphosphazene.
2. The method for preparing hexafluorocyclotriphosphazene according to claim 1, wherein: the adopted nonpolar solvent is any one or a combination of a plurality of n-hexane, cyclohexane, toluene, chlorobenzene and xylene.
3. The method for producing hexafluorocyclotriphosphazene according to claim 1 or 2, wherein: the fluorinating agent is potassium fluoride or sodium fluoride.
4. The method for preparing hexafluorocyclotriphosphazene according to claim 3, wherein: the mass ratio of potassium fluoride or sodium fluoride to hexachlorocyclotriphosphazene is 1:1 to 1.2.
5. The method for producing hexafluorocyclotriphosphazene according to claim 1 or 2, wherein: the fluorination reaction is carried out for 1-2 hours at-30-60 ℃.
6. The method for preparing hexafluorocyclotriphosphazene according to claim 5, wherein: the fluorination reaction temperature is-20 ℃ to 30 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732718A (en) * | 2016-03-22 | 2016-07-06 | 山东大学 | Synthesis method of fluorocyclotriphosphazene |
| CN107857780A (en) * | 2016-09-22 | 2018-03-30 | 微宏动力系统（湖州）有限公司 | A kind of synthetic method of fluoro phosphonitrile compound, fluoro phosphonitrile compound and battery electrolytic solution |
| CN109503664A (en) * | 2017-09-15 | 2019-03-22 | 张家港市国泰华荣化工新材料有限公司 | The preparation method of three phosphonitrile of hexafluoro ring |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732718A (en) * | 2016-03-22 | 2016-07-06 | 山东大学 | Synthesis method of fluorocyclotriphosphazene |
| CN107857780A (en) * | 2016-09-22 | 2018-03-30 | 微宏动力系统（湖州）有限公司 | A kind of synthetic method of fluoro phosphonitrile compound, fluoro phosphonitrile compound and battery electrolytic solution |
| CN109503664A (en) * | 2017-09-15 | 2019-03-22 | 张家港市国泰华荣化工新材料有限公司 | The preparation method of three phosphonitrile of hexafluoro ring |
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