CN110658301A - Method for measuring peroxide content in perfluoropolyether - Google Patents
Method for measuring peroxide content in perfluoropolyether Download PDFInfo
- Publication number
- CN110658301A CN110658301A CN201911037397.0A CN201911037397A CN110658301A CN 110658301 A CN110658301 A CN 110658301A CN 201911037397 A CN201911037397 A CN 201911037397A CN 110658301 A CN110658301 A CN 110658301A
- Authority
- CN
- China
- Prior art keywords
- fluorine
- perfluoropolyether
- solution
- peroxide content
- sodium thiosulfate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for measuring peroxide content in perfluoropolyether, and belongs to the technical field of analytical chemistry. The method for measuring the peroxide content in the perfluoropolyether comprises the steps of dissolving the perfluoropolyether of a sample to be measured by using a fluorine-containing solvent in a nitrogen atmosphere, adding a phase transfer catalyst and potassium iodide under an acidic medium condition, adding a sodium thiosulfate solution for titration, and calculating to obtain the peroxide content in the perfluoropolyether of the sample to be measured. The method for measuring the peroxide content in the perfluoropolyether has the advantages of simple process, convenience and quickness in operation, quickness and accuracy in measurement and high accuracy.
Description
Technical Field
The invention relates to a method for measuring peroxide content in perfluoropolyether, and belongs to the technical field of analytical chemistry.
Background
Perfluoropolyether (PFPE) was first studied in the 60 th 20 th century and is a relatively special class of perfluoropolymer compounds, the molecule of which is composed of C, F, O elements in the form of covalent bonds such as C-F bond, C-C bond, C-O bond, etc. Compared with the molecular structure of hydrocarbon polyether, the C-F bond with stronger bond energy in the perfluoropolyether molecule replaces the C-H bond of hydrocarbon, fluorine atoms have strong electronegativity, and most of carbon chains are shielded by the fluorine atoms, so that the perfluoropolyether has the advantages of high density, low surface tension, low volatility, good viscous flow, non-combustibility, good dielectric property, good lubricity and the like, and can be well compatible with plastics, rubber and metal.
The perfluoropolyether material is mainly used as special lubricating oil, industrial fluid, functional chemicals and the like, and the specific application fields are aerospace industry, nuclear industry, electronic and electrical industry, chemical industry, automobile industry and the like. With the progress of science and technology and the popularization of the application field of perfluoropolyether, particularly, the problems of human resources, energy, environmental protection and the like are increasingly paid attention all over the world, so that the perfluoropolyether can meet the application requirements of various industries, and a harmless and environment-friendly product has a tendency of rapidly increasing the demand under general conditions.
The perfluoropolyether is prepared by two methods, one method is obtained by anionic polymerization, the other method is obtained by ultraviolet catalytic oxidation, the product obtained by the latter method often contains a large amount of peroxide, and the peroxide is very active and reacts under the conditions of heat, friction and the like to cause the breakage of molecular chains, so that the performance of the perfluoropolyether is reduced. When the perfluoropolyether containing peroxide is used as a lubricant, the lubricating property of the perfluoropolyether containing peroxide can be greatly reduced due to the breakage of molecular chains, and even the corrosion of equipment is caused; in addition, when the peroxide-containing perfluoropolyether is used as an emulsifier, the polymerization production, particularly the polymerization rate, is seriously affected because the peroxide itself can be used as a polymerization initiator, and the stability is irregular due to the difference of molecular structures, i.e., the decomposition temperature is different, the energy is different, the time is different, and the like. Therefore, it is desirable to detect and control the peroxide content of the perfluoropolyether.
In general, a spectrophotometer method, a colorimetry method, an iodometry method, and a Reinson reagent are methods for measuring the contents of oxides and peroxides in inorganic substances, and the contents of peroxides in organic compounds are difficult to measure.
US4908323A describes a peroxide measurement method based on an aqueous solution of a titanium (IV) compound and an organic solvent, using an organic solvent to make Ti4+The ions form titanyl cations of peroxide with a specific color with the peroxide for the determination. However, the organic solvent in the invention is selected from aliphatic alcohols containing 1-5 carbon atoms or their combination, such as methanol, ethanol, n-propanol, isopropanol, etc., which can not dissolve perfluoropolyether. The iodometry method specified by the national standard is used for measuring the content of the organic peroxide, wherein the used reagents are dichloromethane or trichloromethane, and the reagents can not well dissolve the perfluoropolyether. Heterogeneous reaction has higher requirement on the uniformity of solution, the more uniform the solution is, the more favorable the reaction is, and the more accurate the test result is. Therefore, none of the above solvents can be used for the determination of peroxide content in perfluoropolyethers.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art, and provides a method for measuring the content of peroxide in perfluoropolyether, which has the advantages of simple process, convenience and rapidness in operation, quickness and accuracy in measurement and high accuracy.
The method for measuring the peroxide content in the perfluoropolyether comprises the steps of dissolving the perfluoropolyether of a sample to be measured by using a fluorine-containing solvent in a nitrogen atmosphere, adding a phase transfer catalyst and potassium iodide under an acidic medium condition, adding a sodium thiosulfate solution for titration, and calculating to obtain the peroxide content in the perfluoropolyether of the sample to be measured.
Preferably, the fluorine-containing solvent is one or more of perfluoro-4-methyl-2-pentene, trifluorotrichloroethane, pentafluorobutane, perfluoropentane or perfluorooctane.
Preferably, the acidic medium is glacial acetic acid or acetic anhydride.
Preferably, the phase transfer catalyst is a compound such as fluorine-containing carboxylate, fluorine-containing sulfonate, fluorine-containing sulfate ester salt, fluorine-containing phosphate ester salt, fluorine-containing quaternary ammonium salt, fluorine-containing quaternary phosphonium salt, fluorine-containing quaternary ammonium carboxylate, fluorine-containing quaternary ammonium sulfonate, fluorine-containing quaternary ammonium sulfate salt, fluorine-containing alcohol, fluorine-containing ether, or the like.
The method for measuring the peroxide content in the perfluoropolyether specifically comprises the following steps:
(1) introducing nitrogen into the used reagent for treatment before use, wherein the reagent is prevented from contacting air in the whole operation process;
(2) completely dissolving a sample to be tested in a fluorine-containing solvent;
(3) adding an acidic medium into the solution obtained in the step (2), slightly shaking, and introducing nitrogen into a reaction container;
(4) adding a phase transfer catalyst into the solution obtained in the step (3), and slightly shaking;
(5) adding a potassium iodide solution into the mixed solution obtained in the step (4), and shaking gently;
(6) placing the solution obtained in the step (5) in a dark place, and stirring and reacting for a certain time at a certain temperature;
(7) adding distilled water into the solution obtained in the step (6), titrating the solution to be light yellow by using a sodium thiosulfate solution, adding a starch indicator, continuously titrating the solution to be colorless, and recording the volume of the used sodium thiosulfate solution;
(8) testing the volume of the blank solution consuming the sodium thiosulfate solution under the same conditions;
(9) the peroxide content in the perfluoropolyether is calculated according to the following formula:
wherein PO is peroxide content in perfluoropolyether (Perperfluoropolyether) in g active oxygen/100 g oil, C is sodium thiosulfate concentration in mol/L, and V1Consumption of the volume of sodium thiosulfate solution for the sample in mL, V2The volume of sodium thiosulfate solution consumed for the blank test is in mL, and m is the mass of the sample to be tested and is in g.
In the step (1), the purity of nitrogen is more than or equal to 99.99 percent, and the solvent treatment time within 500mL is more than or equal to 30 min.
In the step (1), the reagent is a fluorine-containing solvent, an acidic medium and distilled water.
In the step (2), the concentration of the sample to be tested in the fluorine-containing solvent is 0.005-1 g/mL, preferably 0.01-0.1 g/mL.
In the step (3), the purity of the nitrogen is more than or equal to 99.99 percent, and the nitrogen is introduced into the reaction vessel for not less than 1 min.
The volume ratio of the fluorine-containing solvent to the acidic medium is 1: 0.5-3.
The potassium iodide solution is a saturated solution and is ready for use. The volume ratio of the potassium iodide solution to the fluorine-containing solvent is 0.05-0.5: 1, and the molar ratio of the potassium iodide solution to the phase transfer catalyst is 10: 0.01-1.
In the step (6), the reaction temperature is 30-60 ℃, preferably 30-40 ℃, and the reaction time is 15-60 min, preferably 20-30 min.
The volume ratio of the distilled water added in the step (7) to the fluorine-containing solvent and the acidic medium respectively added in the steps (2) and (3) is 1-10: 1: 0.5-3, and preferably 3-1: 1: 1-2; the concentration of the sodium thiosulfate solution is 0.001-0.5 mol/L.
The reagents used in the invention are analytically pure reagents, and the distilled water is tertiary water.
In the test reaction process, the open contact of a container with air is avoided before titration by using a sodium thiosulfate solution; during titration with sodium thiosulfate, attention should be paid to control the titration speed, that is, the titration speed cannot be too fast to influence the judgment of the titration end point, and the titration speed cannot be too slow to increase the test result.
The judgment basis of the accuracy of the test result of the invention is that the relative standard deviation is less than or equal to 5 percent.
In the invention, a sample to be detected is firstly dissolved in a fluorine-containing solvent, the concentration of the sample to be detected is controlled, the acidity of the solution is adjusted by an acidic medium, and then a phase transfer catalyst and a potassium iodide solution are added to ensure that peroxide in the sample to be detected completely reacts. The amount of iodide ions oxidized by peroxide was analyzed titrated with sodium thiosulfate, a reducing agent, using starch as an indicator. And calculating the content of the peroxide in the perfluoropolyether according to the using amount of the sodium thiosulfate and the stoichiometric ratio of each substance in the reaction process.
The method selects the fluorine-containing solvent to dissolve the perfluoropolyether, thereby improving the uniformity of the solution; for heterogeneous reaction, besides a proper solvent is selected to improve the solubility of a sample, a proper auxiliary agent such as a phase transfer catalyst is added to solve the problems of slow reaction rate and incomplete reaction caused by contact resistance of reactants in different phases, so that the method adds the phase transfer catalyst to improve the reaction completeness of perfluoropolyether and ions in a water phase and accelerate the reaction, and simultaneously strictly controls the oxygen content in the reaction process to improve the accuracy of a test result.
Compared with the prior art, the invention has the following beneficial effects:
(1) the use of the fluorine-containing solvent and the phase transfer catalyst improves the accuracy of the test result;
(2) the reagent and the reaction system used in the invention are treated by nitrogen, thus improving the accuracy of the test result;
(3) the method is suitable for measuring the content of the peroxide in the perfluoropolyether, the test method is simple to operate, and the content of the peroxide in the perfluoropolyether can be quickly, accurately and precisely measured;
(4) the method has the advantages of excellent effect, high precision and relative standard deviation of the measurement result of less than or equal to 5 percent for the determination of the sample with the peroxide content of less than 0.001g/100 g.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
Example 1
A method for determining the peroxide content of perfluoropolyethers, the peroxide content being estimated to be > 0.1g/100g of oil, comprising the following steps:
(1) introducing nitrogen into pentafluorobutane, glacial acetic acid and distilled water which are respectively about 500mL before use for treatment for 1 h;
(2) accurately weighing about 0.1g of a sample to be tested (three parts of perfluoropolyether A, perfluoropolyether B and perfluoropolyether C) into a 125mL conical flask, adding 20mL of pentafluorobutane, plugging a bottle stopper, and shaking up until the sample is completely dissolved;
(3) adding 20mL of glacial acetic acid into the solution in the step (2), slightly shaking, introducing nitrogen into the conical flask for about 1min, and plugging the bottle stopper;
(4) 200mg of C3F7OC2F4OCF2Adding COONa into the solution in the step (3), and shaking gently;
(5) adding 4mL of saturated potassium iodide solution into the mixed solution in the step (4), slightly shaking, and plugging a bottle stopper;
(6) putting the solution in the step (5) in a dark place, and reacting for 30min at 35 ℃;
(7) adding 50mL of distilled water into the solution obtained in the step (6), titrating the solution to be light yellow by using 0.02mol/L sodium thiosulfate solution, adding 1mL of starch indicator with the concentration of 10g/L, continuously titrating the solution to be colorless, and recording the volume of the used sodium thiosulfate solution;
(8) testing the blank solution under the same conditions, and recording the volume of the consumed sodium thiosulfate solution;
(9) the peroxide content in the perfluoropolyether was calculated. The results are shown in table 1:
TABLE 1 peroxide content in perfluoropolyethers
Comparative example 1
The operation process changes pentafluorobutane into trichloromethane, and other operation steps are the same as example 1. The test results are shown in table 2:
TABLE 2 peroxide content in perfluoropolyethers
Comparative example 2
The operation procedure was the same as example 1 except that pentafluorobutane was changed to ethanol. The test results are shown in table 3:
TABLE 3 peroxide content in perfluoropolyethers
Example 2
A method for determining the peroxide content of perfluoropolyethers, the peroxide content being estimated to be > 0.1g/100g of oil, comprising the following steps:
(1) introducing nitrogen into trifluorotrichloroethane, glacial acetic acid and distilled water which are about 500mL respectively for treatment for 1h before use;
(2) accurately weighing about 0.1g of a sample to be tested (three parts of perfluoropolyether D, perfluoropolyether E and perfluoropolyether F) into a 125mL conical flask, adding 15mL of trifluorotrichloroethane, plugging a bottle stopper, and shaking up until the sample is completely dissolved;
(3) adding 20mL of glacial acetic acid into the solution in the step (2), slightly shaking, introducing nitrogen into the conical flask for about 1min, and plugging the bottle stopper;
(4) adding 50mg of ammonium hexafluoropropylene oxide trimer chloride into the solution in the step (3), and slightly shaking;
(5) adding 2mL of saturated potassium iodide solution into the mixed solution in the step (4), slightly shaking, and plugging a bottle stopper;
(6) putting the solution in the step (5) in a dark place, and reacting for 15min at 60 ℃;
(7) adding 50mL of distilled water into the solution obtained in the step (6), titrating the solution to be light yellow by using a sodium thiosulfate solution with the concentration of about 0.02mol/L, adding 1mL of starch indicator with the concentration of 10g/L, continuously titrating the solution to be colorless, and recording the volume of the used sodium thiosulfate solution;
(8) testing the blank solution under the same conditions, and recording the volume of the consumed sodium thiosulfate solution;
(9) the peroxide content in the perfluoropolyether was calculated. The results are shown in Table 4:
TABLE 4 peroxide content in perfluoropolyethers
Comparative example 3
3mg of hexafluoropropylene oxide trimer ammonium chloride was added in this procedure, and the other procedures were the same as in example 2. The test results are shown in table 5:
TABLE 5 peroxide content in perfluoropolyethers
Comparative example 4
The operation process is carried out without adding hexafluoropropylene oxide trimer ammonium chloride, and the other operation steps are the same as example 2. The test results are shown in table 6:
TABLE 6 peroxide content in perfluoropolyethers
Example 3
A method for determining the peroxide content of perfluoropolyethers, the peroxide content being estimated to be < 0.005g/100g of oil, by the following steps:
(1) introducing nitrogen into about 300mL of trifluorotrichloroethane, glacial acetic acid and distilled water for treatment for 30min before use;
(2) accurately weighing about 0.5G of a sample to be tested (three parts of perfluoropolyether G, perfluoropolyether H and perfluoropolyether I) into a 125mL conical flask, adding 10mL of trifluorotrichloroethane, plugging a bottle stopper, and shaking up until the sample is completely dissolved;
(3) adding 10mL of glacial acetic acid into the solution in the step (2), introducing nitrogen into the conical flask for about 1min, and plugging a bottle stopper;
(4) mixing 10mg of C7F15(CH2)3N+(CH3)3Br-Adding the mixture into the solution in the step (3) and shaking gently.
(5) And (3) adding 1mL of saturated potassium iodide solution into the mixed solution in the step (4), and plugging a bottle stopper.
(6) And (3) putting the solution in the step (5) in the dark, and reacting for 60min at 30 ℃.
(7) Adding 30mL of distilled water into the solution obtained in the step (6), titrating the solution to be light yellow by using a sodium thiosulfate solution with 0.002mol/L, adding 1mL of starch indicator with the concentration of 10g/L, continuously titrating the solution to be colorless, and recording the volume of the used sodium thiosulfate solution.
(8) The blank solution was tested under the same conditions and the volume of sodium thiosulfate solution consumed was recorded.
(9) The peroxide content in the perfluoropolyether was calculated. The results are shown in Table 7:
TABLE 7 peroxide content in perfluoropolyethers
Comparative example 5
The reagents used in the process were not purged with nitrogen, and the flask was not purged with nitrogen, and the other steps were the same as those in example 3.
The test results are shown in table 8:
TABLE 8 peroxide content in perfluoropolyethers
As can be seen from the results obtained in the above examples and comparative examples, the method for determining the peroxide content in the perfluoropolyether of the present invention has a relatively high accuracy, and is also excellent for testing perfluoropolyethers having a peroxide content of less than 0.001g active oxygen per 100g oil.
Claims (10)
1. A method for measuring the peroxide content in perfluoropolyether is characterized by comprising the following steps: dissolving perfluoropolyether of a sample to be tested in a fluorine-containing solvent under the nitrogen atmosphere, adding a phase transfer catalyst and potassium iodide under the acidic medium condition, adding a sodium thiosulfate solution for titration, and calculating to obtain the content of peroxide in the perfluoropolyether of the sample to be tested.
2. The method according to claim 1, wherein the peroxide content in the perfluoropolyether is determined by: the fluorine-containing solvent is one or more of perfluoro-4-methyl-2-pentene, trichlorotrifluoroethane, pentafluorobutane, perfluoropentane or perfluorooctane.
3. The method according to claim 1, wherein the peroxide content in the perfluoropolyether is determined by: the acidic medium is glacial acetic acid or acetic anhydride.
4. The method according to claim 1, wherein the peroxide content in the perfluoropolyether is determined by: the phase transfer catalyst is fluorine-containing carboxylate, fluorine-containing sulfonate, fluorine-containing sulfate, fluorine-containing phosphate, fluorine-containing quaternary ammonium salt, fluorine-containing quaternary phosphonium salt, fluorine-containing quaternary ammonium carboxylate, fluorine-containing quaternary ammonium sulfonate, fluorine-containing quaternary ammonium sulfate, fluorine-containing alcohol or fluorine-containing ether compound.
5. The method according to claim 1, wherein the peroxide content in the perfluoropolyether is determined by: the method comprises the following steps:
(1) introducing nitrogen into the used reagent for treatment before use;
(2) dissolving a sample to be tested in a fluorine-containing solvent;
(3) adding an acidic medium into the solution obtained in the step (2), shaking, and introducing nitrogen into a reaction vessel;
(4) adding a phase transfer catalyst into the solution obtained in the step (3), and shaking;
(5) adding a potassium iodide solution into the mixed solution obtained in the step (4), and shaking;
(6) placing the solution obtained in the step (5) in a dark place, and stirring and reacting for a certain time at a certain temperature;
(7) adding distilled water into the solution obtained in the step (6), titrating the solution to be light yellow by using a sodium thiosulfate solution, adding a starch indicator, continuously titrating the solution to be colorless, and recording the volume of the used sodium thiosulfate solution;
(8) testing the volume of the blank solution consuming the sodium thiosulfate solution under the same conditions;
(9) the peroxide content in the perfluoropolyether is calculated according to the following formula:
wherein PO is peroxide content in perfluoropolyether (Perperfluoropolyether) in g active oxygen/100 g oil, C is sodium thiosulfate concentration in mol/L, and V1Consumption of the volume of sodium thiosulfate solution for the sample in mL, V2The volume of sodium thiosulfate solution consumed for the blank test is in mL, and m is the mass of the sample to be tested and is in g.
6. The method according to claim 5, wherein: in the step (1), the purity of nitrogen is more than or equal to 99.99 percent, and the solvent treatment time within 500mL is more than or equal to 30 min.
7. The method according to claim 5, wherein: in the step (2), the concentration of the sample to be tested in the fluorine-containing solvent is 0.005-1 g/mL.
8. The method according to claim 5, wherein: the volume ratio of the fluorine-containing solvent to the acidic medium is 1: 0.5-3; the volume ratio of the potassium iodide solution to the fluorine-containing solvent is 0.05-0.5: 1, and the molar ratio of the potassium iodide solution to the phase transfer catalyst is 10: 0.01-1.
9. The method according to claim 5, wherein: the reaction temperature is 30-60 ℃, and the reaction time is 15-60 min.
10. The method according to claim 5, wherein: the volume ratio of the distilled water added in the step (7) to the fluorine-containing solvent and the acidic medium respectively added in the steps (2) and (3) is 1-10: 1: 0.5-3; the concentration of the sodium thiosulfate solution is 0.001-0.5 mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911037397.0A CN110658301A (en) | 2019-10-29 | 2019-10-29 | Method for measuring peroxide content in perfluoropolyether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911037397.0A CN110658301A (en) | 2019-10-29 | 2019-10-29 | Method for measuring peroxide content in perfluoropolyether |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110658301A true CN110658301A (en) | 2020-01-07 |
Family
ID=69042076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911037397.0A Pending CN110658301A (en) | 2019-10-29 | 2019-10-29 | Method for measuring peroxide content in perfluoropolyether |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110658301A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413457A (en) * | 2020-04-21 | 2020-07-14 | 山东东岳高分子材料有限公司 | Method for measuring peroxide content in perfluoropolyether by potentiometric titration |
| CN111551668A (en) * | 2020-05-08 | 2020-08-18 | 山东东岳高分子材料有限公司 | Method for measuring acid value content in perfluoropolyether |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635064A (en) * | 2003-12-30 | 2005-07-06 | 中国科学院兰州化学物理研究所 | Process for preparing ZrO#-[2]/perfluoropolyether composite lubrication thin film |
| CN101156107A (en) * | 2005-02-03 | 2008-04-02 | 北卡罗来纳大学查珀尔希尔分校 | Low surface energy polymeric material for use in liquid crystal displays |
| US20110207880A1 (en) * | 2008-08-15 | 2011-08-25 | Nova-Duet Technologies, Pty. Ltd. | Peroxidic fluoropolyether and its use in emulsion polymerization of fluorin-containing monomer |
| CN102426169A (en) * | 2011-11-09 | 2012-04-25 | 天津市天骄辐射固化材料有限公司 | Method for detecting content of peroxide in polyether polyol |
| US20130213270A1 (en) * | 2010-11-02 | 2013-08-22 | Zhonghao Chenguang Research Institute Of Chemical Industry Co., Ltd. | Preparation method and use for fluorine-containing microemulsion |
| CN106317398A (en) * | 2015-07-01 | 2017-01-11 | 中昊晨光化工研究院有限公司 | Method for decomposition of peroxide in perfluoropolyether |
| CN109928891A (en) * | 2017-12-18 | 2019-06-25 | 乳源东阳光氟有限公司 | A kind of perfluoropolyether and its preparation method and application of polyamide connection |
-
2019
- 2019-10-29 CN CN201911037397.0A patent/CN110658301A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635064A (en) * | 2003-12-30 | 2005-07-06 | 中国科学院兰州化学物理研究所 | Process for preparing ZrO#-[2]/perfluoropolyether composite lubrication thin film |
| CN101156107A (en) * | 2005-02-03 | 2008-04-02 | 北卡罗来纳大学查珀尔希尔分校 | Low surface energy polymeric material for use in liquid crystal displays |
| US20110207880A1 (en) * | 2008-08-15 | 2011-08-25 | Nova-Duet Technologies, Pty. Ltd. | Peroxidic fluoropolyether and its use in emulsion polymerization of fluorin-containing monomer |
| US20130213270A1 (en) * | 2010-11-02 | 2013-08-22 | Zhonghao Chenguang Research Institute Of Chemical Industry Co., Ltd. | Preparation method and use for fluorine-containing microemulsion |
| CN102426169A (en) * | 2011-11-09 | 2012-04-25 | 天津市天骄辐射固化材料有限公司 | Method for detecting content of peroxide in polyether polyol |
| CN106317398A (en) * | 2015-07-01 | 2017-01-11 | 中昊晨光化工研究院有限公司 | Method for decomposition of peroxide in perfluoropolyether |
| CN109928891A (en) * | 2017-12-18 | 2019-06-25 | 乳源东阳光氟有限公司 | A kind of perfluoropolyether and its preparation method and application of polyamide connection |
Non-Patent Citations (7)
| Title |
|---|
| GB/T 5538-1995 油脂过氧化值测定: "《中华人民共和国国家标准 GB/T 5538-1995》", 17 August 1995 * |
| 张鸣等: "光氧化法制备全氟聚醚酸工艺研究", 《化工生产与技术》 * |
| 李倩等: "高速纺丝油剂用丁醇聚醚主链的稳定性", 《纺织学报》 * |
| 王金清等: "单晶硅表面全氟聚醚润滑膜的制备及摩擦特性研究", 《摩擦学学报》 * |
| 申圣强: "聚醚中过氧化物含量测定方法的研究", 《精细石油化工进展》 * |
| 苏州大学有机化学教研室: "《有机化学演示实验》", 30 September 1992, 高等教育出版社 * |
| 许世红等: "钼/全氟聚醚复合薄膜的制备及摩擦学性能研究", 《摩擦学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413457A (en) * | 2020-04-21 | 2020-07-14 | 山东东岳高分子材料有限公司 | Method for measuring peroxide content in perfluoropolyether by potentiometric titration |
| CN111551668A (en) * | 2020-05-08 | 2020-08-18 | 山东东岳高分子材料有限公司 | Method for measuring acid value content in perfluoropolyether |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Moss et al. | Potentiometric Titration of Weak Aċids in Anhydrous Ethylenediamine | |
| Penneman et al. | Quantitative determination of hydrazine | |
| Fritz et al. | Titration of acids in nonaqueous solvents | |
| CN110658301A (en) | Method for measuring peroxide content in perfluoropolyether | |
| CN105067756A (en) | Potentiometric titration determining method of boric acid in water-based adhesive | |
| EP3423188B1 (en) | Method for removing perfluorinated alkanoic acids | |
| CN112782306A (en) | Method for detecting purity of fluorosulfonic acid | |
| Katayama et al. | Colloid titration of heparin using Cat-Floc (polydiallyldimethyl ammonium chloride) as standard polycation | |
| CN111551668A (en) | Method for measuring acid value content in perfluoropolyether | |
| Johnson et al. | Determination of carboxylic acid anhydrides by reaction with morpholine | |
| CN111413457A (en) | Method for measuring peroxide content in perfluoropolyether by potentiometric titration | |
| CN102901765B (en) | Potentiometric titration method for measuring content of Hg<2+> in solution | |
| CN113984757B (en) | Method for measuring total acid value of jet fuel | |
| Smith et al. | Titrimetric determination of water in organic liquids using acetyl chloride and pyridine | |
| Critchfield et al. | Determination of Alpha, Beta-Unsaturated Compounds by Reaction with Sodium Sulfite | |
| CN1865993A (en) | Combined detection method for high-purity SO3 gas and impurity SO2 gas therein | |
| CN109633076A (en) | The measuring method of Theil indices in the preprocess method and tin stripper of tin stripper | |
| CN112649556A (en) | Method for rapidly measuring concentration of hydrogen peroxide | |
| CN101173891B (en) | Method for measuring ethane nitrile content | |
| Radić et al. | Kinetic-potentiometric determination of aluminium in acidic solution using a fluoride ion-selective electrode | |
| CN113109502A (en) | Method for analyzing peroxide residue in polymer | |
| CN114414558B (en) | Method for measuring acid value content of water-based fluorocarbon resin | |
| CN114894925B (en) | Method for measuring oxalic acid content in dimethyl oxalate | |
| CN118243853A (en) | Method for measuring unsaturation degree of polyether | |
| CN117571920A (en) | Detection method of hydrochloric acid and adipic acid in dichloropropanol and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200107 |