CN114184737A - Method for measuring content of hexafluorocyclotriphosphazene - Google Patents
Method for measuring content of hexafluorocyclotriphosphazene Download PDFInfo
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- CN114184737A CN114184737A CN202111494701.1A CN202111494701A CN114184737A CN 114184737 A CN114184737 A CN 114184737A CN 202111494701 A CN202111494701 A CN 202111494701A CN 114184737 A CN114184737 A CN 114184737A
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- hexafluorocyclotriphosphazene
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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 62
- 238000000034 method Methods 0.000 title claims abstract description 26
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000000243 solution Substances 0.000 claims abstract description 67
- 238000004448 titration Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012490 blank solution Substances 0.000 claims abstract description 9
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 13
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical group C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000523 sample Substances 0.000 claims description 10
- PRZSXZWFJHEZBJ-UHFFFAOYSA-N thymol blue Chemical compound C1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=CC(O)=C(C(C)C)C=2)C)=C1C PRZSXZWFJHEZBJ-UHFFFAOYSA-N 0.000 claims description 9
- 230000002378 acidificating effect Effects 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- ZPLCXHWYPWVJDL-UHFFFAOYSA-N 4-[(4-hydroxyphenyl)methyl]-1,3-oxazolidin-2-one Chemical compound C1=CC(O)=CC=C1CC1NC(=O)OC1 ZPLCXHWYPWVJDL-UHFFFAOYSA-N 0.000 claims description 5
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000002798 polar solvent Substances 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 6
- 230000035772 mutation Effects 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 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 2
- VNIBTHCKBVEHRM-UHFFFAOYSA-N FP(N=P(F)(F)F)(NP)(F)F Chemical compound FP(N=P(F)(F)F)(NP)(F)F VNIBTHCKBVEHRM-UHFFFAOYSA-N 0.000 description 2
- 239000012025 fluorinating agent Substances 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- JKUAHMKHSDOYKZ-UHFFFAOYSA-N FC(C(F)(F)F)(OP1N=PN=P[N]1)F Chemical compound FC(C(F)(F)F)(OP1N=PN=P[N]1)F JKUAHMKHSDOYKZ-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- DGTVXEHQMSJRPE-UHFFFAOYSA-M difluorophosphinate Chemical compound [O-]P(F)(F)=O DGTVXEHQMSJRPE-UHFFFAOYSA-M 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- -1 phosphazene compound Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring the content of a hexafluorocyclotriphosphazene product, which comprises the steps of dissolving a sample by using a solvent, adding an excessive sodium methoxide solution, adding a proper amount of water, titrating by using an inorganic acid, determining a titration end point by using the mutation of an indicator, preparing a blank solution by the same method, and calculating the content of the hexafluorocyclotriphosphazene product. The method can effectively determine the content of the hexafluorocyclotriphosphazene product. The method has the advantages of simple operation, high accuracy, short detection time and low detection cost, and greatly simplifies the determination steps of the hexafluorocyclotriphosphazene product.
Description
Technical Field
The invention belongs to the field of analysis and test, and particularly relates to a method for testing the content of hexafluorocyclotriphosphazene.
Background
The phosphazene compound has excellent flame retardant property. The hexachlorocyclotriphosphazene is an intermediate of a plurality of phosphazene compounds, so the synthesis of the hexachlorocyclotriphosphazene has good application prospect; some derivatives of the flame retardant are high-end flame retardants, and are widely applied to high-efficiency flame retardance of lithium batteries, such as pentafluoroethoxy cyclotriphosphazene and pentafluorophosphazenyl difluorophosphate. At present, the hexafluorocyclotriphosphazene is mainly prepared by fluorinating hexachlorocyclotriphosphazene and a fluorinating agent, the hexachlorocyclotriphosphazene is dissolved in an organic solvent, the fluorinating agent and a catalyst are added, and the target product hexafluorocyclotriphosphazene is obtained after the fluorination reaction and the rectification (CN113004322A and patent application No. CN 112175010A).
The common methods for detecting the hexafluorocyclotriphosphazene are liquid chromatography (patent application No. CN 112175010A) and gas chromatography (document No.: gas chromatography-nitrogen and phosphorus detector is used for detecting melamine in milk and milk powder), and the method has the disadvantages of expensive instrument, long instrument stabilization time and long whole detection period, and is not beneficial to the rapid detection of the hexafluorocyclotriphosphazene. The method is innovative in that excessive sodium methoxide is added into a hexafluorocyclotriphosphazene organic solvent, the hexafluorocyclotriphosphazene and the sodium methoxide react according to the molar ratio of 1:3, the excessive sodium methoxide is changed into sodium hydroxide and methanol by adopting water, inorganic acid is adopted for titration, and the content of the hexafluorocyclotriphosphazene is determined by indicator color change measurement. The method is simple to operate, greatly simplifies the measuring steps of the content of the hexafluorocyclotriphosphazene product, shortens the analysis time and reduces the analysis cost; meanwhile, the titration end point jump is obvious, the human error is reduced, and the result repeatability and accuracy are improved.
Disclosure of Invention
The invention aims to solve the problems of long detection period and the like in the prior art, the content of the hexafluorocyclotriphosphazene is determined by adopting a back titration method, the cost is low compared with the analysis cost of an instrument, no complex pretreatment is needed, the content of the hexafluorocyclotriphosphazene can be rapidly determined, and a simple and rapid analysis method is provided for the content determination of the hexafluorocyclotriphosphazene.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the method for measuring the content of the hexafluoro-cyclotriphosphazene is characterized by comprising the following specific steps of:
1) weighing a hexafluorocyclotriphosphazene product, placing the hexafluorocyclotriphosphazene product in a conical flask containing 50mL of solvent, adding an excessive sodium methoxide solution, adding 50mL of water and 3-5 drops of indicator, titrating by using an inorganic acid standard titration solution, and titrating until the indicator is mutated to be the end point.
2) In step 1, a blank test was also performed except for no sample.
3) The content of the hexafluorocyclotriphosphazene reaction liquid is calculated by the following formula.
W is the content of the product (or reaction liquid) of the hexafluorocyclotriphosphazene, and is calculated by the mass fraction of the hexafluorocyclotriphosphazene;
c is the concentration of the acidic standard titration solution, and the unit mol/L;
v is the volume of the acidic standard titration solution consumed by the sample solution, and the unit is ml;
V0the volume of the acidic standard titration solution in ml is consumed for the blank solution;
m is the molar mass of the hexafluorocyclotriphosphazene;
m is the mass of the sample in g.
The solvent is selected from polar solvents for dissolving hexafluorocyclotriphosphazene, including acetonitrile or organic alcohols such as methanol, ethanol, propanol, butanol, etc., but not limited thereto.
The inorganic acid standard titration solution is inorganic acid standard titration solution and the like, but is not limited to the inorganic acid standard titration solution;
the standard titrating solution of the electrodeless acid is selected from sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid and perchloric acid;
the indicator is selected from an ethanol solution containing phenolphthalein, methyl red, thymol blue, bromothymol blue or thymol blue;
preferably, the indicator is phenolphthalein, methyl red, thymol blue, bromothymol blue or thymol blue ethanol solution with the mass fraction of 1%;
the sodium methoxide solution is selected from a solvent for dissolving sodium methoxide, such as methanol, ethanol, propanol, and the like, but is not limited thereto, and the concentration of the sodium methoxide solution is 0.05mol/L to 0.2 mol/L.
The mass ratio of the hexafluorocyclotriphosphazene to the sodium methoxide in the step 1) is 1: 3-1: 8.
The invention has the beneficial effects that:
1. the invention provides a new idea for measuring the content of the hexafluorocyclotriphosphazene product, the method is simple to operate, the result is accurate and reliable, and a new method is provided for the quality control of the hexafluorocyclotriphosphazene product by a manufacturer and the quality identification of the hexafluorocyclotriphosphazene product by a third-party detection mechanism.
2. According to the properties of a hexafluoro-cyclotriphosphazene product, acetonitrile or alcohol is adopted as a solvent to be beneficial to the reaction of a sodium methoxide solution and the sodium methoxide solution, and after water is added, the sodium methoxide is changed into methanol and sodium hydroxide; inorganic acid standard titration solution is used as a titrant and a proper indicator, and the solution is uniform and transparent in the whole titration process and has an obvious jump endpoint; the accuracy and the repeatability of the content of the hexafluoro-cyclotriphosphazene product are ensured.
3. The method adopts the inorganic acidic standard solution to measure the content of the hexafluorocyclotriphosphazene product, reduces the inspection cost compared with the instrument analysis, shortens the analysis event, and is simpler, more convenient and faster.
Detailed Description
The present invention will be further illustrated by the following examples, which are intended to be merely illustrative and not limitative.
Example 1
0.2483g of hexafluorocyclotriphosphazene (M248.93 g/moL) sample is weighed and placed in a 250mL conical flask containing 50mL of acetonitrile, 50mL of 0.1moL/L sodium methoxide solution (dissolved in ethanol to obtain 0.1moL/L sodium methoxide solution) is added, 3 drops to 10 drops of 1% phenolphthalein indicator (1 g is weighed and dissolved in 100mL of ethanol) and 20mL of water are added, and then 0.1021moL/L hydrochloric acid standard titration solution (prepared and calibrated according to GB/T601) is used for titration until the solution turns from red to colorless, and the titration volume is 21.05 mL. A blank test was carried out using 50mL of a 0.1mol/L sodium methoxide solution, and the titration volume of the blank solution was 50.23 mL. The hexafluorocyclotriphosphazene content was found to be 99.47%. The content of the hexafluorocyclotriphosphazene is 99.56 percent as measured by a high performance liquid chromatography.
The content of the hexafluorotricyclotriphosphazene is calculated by the following formula:
example 2
0.2475g of hexafluorocyclotriphosphazene (M248.93 g/moL) sample is weighed and placed in a 250mL conical flask containing 50mL of ethanol, 50mL of 0.1moL/L sodium methoxide solution (dissolved by adding ethanol to prepare 0.1moL/L sodium methoxide solution) is added, 3 drops to 10 drops of 1% thymol blue indicator (1 g is weighed and dissolved in 100mL of ethanol) and 20mL of water are added, and then 0.1005moL/L perchloric acid standard titration solution (prepared and calibrated according to GB/T601) is used for titration until the solution turns yellow from blue and the titration volume is 21.55 mL. A blank test was carried out using 50mL of 0.1mol/L sodium methoxide solution, and the titration volume of the blank solution was 51.03 mL. The hexafluorocyclotriphosphazene content was found to be 99.33%.
The content of the hexafluorotricyclotriphosphazene is calculated by the following formula:
example 3
0.2456g of hexafluorocyclotriphosphazene (M248.93 g/moL) sample was weighed out, placed in a 250mL Erlenmeyer flask containing 50mL of methanol, 50mL of 0.1moL/L sodium methoxide solution (dissolved in 100mL of ethanol) was added, 3 to 10 drops of 1% methyl red indicator (1 g of methyl red was weighed out and dissolved in 100mL of ethanol) and 20mL of water were added, and then titrated with 0.05105moL/L sulfuric acid standard titration solution (GB/T601) until the solution became red and the titration volume was 21.19 mL. A blank test was carried out using 50mL of 0.1mol/L sodium methoxide solution, and the titration volume of the blank solution was 50.04 mL. The hexafluorocyclotriphosphazene content was found to be 99.52%.
The content of the hexafluorotricyclotriphosphazene is calculated by the following formula:
example 4
0.4476g of hexafluorocyclotriphosphazene (M248.93 g/moL) sample was weighed out, placed in a 250mL Erlenmeyer flask containing 50mL of propanol, 50mL of 0.2moL/L sodium methoxide solution was added (dissolved in propanol to make a 0.2moL/L sodium methoxide solution), 3 drops of 1% phenolphthalein indicator and 20mL of water were added, and then titrated with 0.4956moL/L hydrochloric acid standard titration solution (GB/T601) until the solution turned from red to colorless, and the titration volume was 14.21 mL. A blank test is carried out by using 50mL of 0.2mol/L sodium methoxide solution, and the titration volume of the blank solution is 25.30 mL. The hexafluorocyclotriphosphazene content was found to be 99.52%.
The content of the hexafluorotricyclotriphosphazene is calculated by the following formula:
example 5
0.2546g of hexafluorocyclotriphosphazene (M248.93 g/moL) sample is weighed and placed in a 250mL Erlenmeyer flask containing 50mL of butanol, 50mL of 0.1moL/L sodium methoxide solution (dissolved in butanol to prepare 0.1moL/L sodium methoxide solution) is added, 3 drops to 10 drops of 1% thymol blue indicator (1 g of thymol blue is weighed and dissolved in 100mL of ethanol) and 20mL of water are added, and then the solution is titrated by 0.05060moL/L of phosphoric acid standard titration solution (refer to GB/T601) until the color of the solution changes from blue to yellow, and the titration volume is 21.06 mL. A blank test was carried out using 50mL of a 0.1mol/L sodium methoxide solution, and the titration volume of the blank solution was 51.23 mL. The hexafluorocyclotriphosphazene content was found to be 99.51%.
The content of the hexafluorotricyclotriphosphazene is calculated by the following formula:
example 6
0.2435g of hexafluorocyclotriphosphazene (M248.93 g/moL) sample is weighed and placed in a 250mL Erlenmeyer flask containing 50mL of methanol, 30mL of 0.1moL/L sodium methoxide solution (dissolved in methanol to prepare a solution containing 0.1moL/L sodium methoxide) is added, 3 drops to 10 drops of 1% bromothymol blue indicator (1 g of bromothymol blue is weighed and dissolved in 100mL of ethanol) and 20mL of water are added, and then the solution is titrated by 0.1011moL/L nitric acid standard titration solution (refer to GB/T601) until the solution turns from red to colorless, and the titration volume is 2.19 mL. A blank test was carried out using 30mL of 0.1mol/L sodium methoxide solution, and the titration volume of the blank solution was 31.02 mL. The hexafluorocyclotriphosphazene content was found to be 99.32%.
The content of the hexafluorotricyclotriphosphazene is calculated by the following formula:
example 7 (repeatability test)
Respectively weighing about 0.25g of hexafluorotriphosphazene, placing the hexafluorotriphosphazene into 6 250mL beakers containing 50mL of acetonitrile, adding 50mL of 0.1mol/L sodium methoxide solution (dissolving the sodium methoxide solution by adding ethanol to prepare 0.1 mol/L), adding 3 to 10 drops of 1% phenolphthalein indicator (weighing 1g of sodium methoxide solution and dissolving the sodium methoxide solution in 100mL of ethanol) and 20mL of water, titrating the solution by 0.1021mol/L hydrochloric acid standard titration solution (prepared and calibrated according to GB/T601) until the solution turns from red to colorless, and carrying out blank test in the same way.
TABLE 1 repeatability test
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | RSD/％ | Extremely poor/% |
| Method of the invention/% | 99.64 | 99.32 | 99.10 | 99.65 | 99.56 | 99.21 | 0.24 | 0.54 |
Although the present invention has been described with reference to the specific embodiments, it is not intended to limit the scope of the present invention, and various modifications and variations can be made by those skilled in the art without inventive changes based on the technical solution of the present invention.
Claims (9)
1. The method for measuring the content of the hexafluorocyclotriphosphazene is characterized by comprising the following specific steps of:
1) weighing hexafluoro-cyclotriphosphazene, placing the hexafluoro-cyclotriphosphazene in a conical flask containing a solvent, adding a sodium methoxide solution, adding water and 3-5 drops of an indicator, and titrating with an inorganic acid standard titration solution until the indicator is mutated to be an end point;
2) performing blank tests in the step 1) except for no sample;
3) calculating the content of the hexafluorocyclotriphosphazene reaction liquid according to the following calculation formula:
w is the content of the hexafluorocyclotriphosphazene (or the reaction liquid), and is calculated by the mass fraction of the hexafluorocyclotriphosphazene;
c is the concentration of the acidic standard titration solution, and the unit mol/L;
v is the volume of the acidic standard titration solution consumed by the sample solution, and the unit is ml;
V0the volume of the acidic standard titration solution in ml is consumed for the blank solution;
m is the molar mass of the hexafluorocyclotriphosphazene;
m is the mass of the sample in g.
2. The method for measuring the content of hexafluorocyclotriphosphazene according to claim 1, wherein the solvent in the step 1) is selected from polar solvents which dissolve hexafluorocyclotriphosphazene.
3. The method for measuring the content of hexafluorocyclotriphosphazene according to claim 2, wherein the polar solvent comprises acetonitrile or an organic alcohol, preferably an organic alcohol comprising methanol, ethanol, propanol, butanol.
4. The method for measuring the hexafluorocyclotriphosphazene content according to claim 1, wherein the concentration of the acidic standard titration solution is 0.05 to 0.5 mol/L; the inorganic acid standard titration solution is selected from sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid and perchloric acid.
5. The method according to claim 1, wherein the indicator is selected from the group consisting of phenolphthalein, methyl red, thymol blue, bromothymol blue, and thymol blue ethanol solution.
6. The method for measuring the content of hexafluorocyclotriphosphazene according to claim 1, wherein the solvent of the sodium methoxide solution is methanol, ethanol or propanol in which sodium methoxide is dissolved.
7. The method for measuring the content of hexafluorocyclotriphosphazene according to claim 1, wherein the concentration of the sodium methoxide solution is 0.05 to 0.2 mol/L.
8. The method for measuring the content of hexafluorocyclotriphosphazene according to claim 1, wherein the ratio of the amount of the hexafluorocyclotriphosphazene to the amount of sodium methoxide in step 1) is 1:3 to 1: 8.
9. The method for measuring the content of hexafluorocyclotriphosphazene according to claim 3, wherein the organic alcohol comprises methanol, ethanol, propanol, butanol.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001089487A (en) * | 1999-09-22 | 2001-04-03 | Mitsui Chemicals Inc | Method for producing phosphazenium salt |
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