CN115932158A - Method for testing content of residual chlorine element on surface of powder toughening material - Google Patents
Method for testing content of residual chlorine element on surface of powder toughening material Download PDFInfo
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- CN115932158A CN115932158A CN202211590806.1A CN202211590806A CN115932158A CN 115932158 A CN115932158 A CN 115932158A CN 202211590806 A CN202211590806 A CN 202211590806A CN 115932158 A CN115932158 A CN 115932158A
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- 239000000463 material Substances 0.000 title claims abstract description 41
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 239000000460 chlorine Substances 0.000 title claims abstract description 30
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 27
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000012360 testing method Methods 0.000 title claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 38
- 239000001301 oxygen Substances 0.000 claims abstract description 38
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000003918 potentiometric titration Methods 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 23
- 238000004448 titration Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000523 sample Substances 0.000 claims description 11
- 239000012496 blank sample Substances 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000012085 test solution Substances 0.000 claims description 5
- 239000004952 Polyamide Substances 0.000 claims description 4
- 238000002485 combustion reaction Methods 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- 239000004417 polycarbonate Substances 0.000 claims description 4
- 229920000515 polycarbonate Polymers 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- -1 chlorine ions Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920001643 poly(ether ketone) Polymers 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims 2
- 238000011156 evaluation Methods 0.000 abstract description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 6
- 239000004917 carbon fiber Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 239000004695 Polyether sulfone Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 229920006393 polyether sulfone Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000012815 thermoplastic material Substances 0.000 description 2
- NHPBNQZEXDUUIO-UHFFFAOYSA-N [Ag+].[Ag+].[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound [Ag+].[Ag+].[O-][N+]([O-])=O.[O-][N+]([O-])=O NHPBNQZEXDUUIO-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/70—Wind energy
- Y02E10/72—Wind turbines with rotation axis in wind direction
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for testing the content of residual chlorine on the surface of a powder toughening material. The method comprises the steps of placing a powder toughening material to be tested in an oxygen bomb crucible, introducing water into a calorimeter, completely combusting the powder toughening material in a high-pressure oxygen environment, converting chloride remaining on the surface of the material into freely moving chloride ions, and carrying out potentiometric titration through a silver nitrate solution to obtain the content of chlorine remaining on the surface of the powder toughening material. The method is simple and convenient, has high repeatability, can accurately measure the content of the residual chlorine on the surface of the powder toughening material, and is convenient for subsequent evaluation of the quality of the powder toughening material.
Description
Technical Field
The invention belongs to the field of powder materials, and relates to a method for testing the content of residual chlorine on the surface of a powder toughening material.
Background
Carbon fiber reinforced composite materials are widely used in the manufacturing industry where tensile and compressive stresses are to be applied, such as structural members of airplanes, blades of windmills, and turbines, because of their excellent strength and impact resistance. The powder toughening material prepared by using a thermoplastic material comprising polyether sulfone, polyurethane, polyamide, polyimide, polycarbonate and the like as a main material is a micron-sized powder material, has a white powdery appearance, is commonly used for coordinating with carbon fibers and a resin matrix, and aims to improve the performances of the prepreg in the aspects of high-temperature and high-humidity environment tolerance, compressive strength, carbon fiber interlayer toughness and the like.
In recent years, as materials such as thermoplastic materials and elastomers containing polyether sulfone, polyurethane, polyamide, polyimide, polycarbonate and other main components are studied, the materials are applied in consideration of material characteristics, environmental resistance, stress resistance, and effects of compounding applications. In the process of preparing the toughening agent by using the materials, the chlorine-containing organic compound participates in the synthesis preparation process of the materials, but the chlorine-containing organic compound is a non-material constituent and can be classified as impurities or interfering substances except for effective components of products, so the content of chlorine in the powder toughening material is required to be detected and controlled below a certain limit value. At present, no report of a systematic, clear and mature standard test method for the chlorine content in the powder toughening material exists, and the rapid development of the carbon fiber industry and the composite materials such as prepreg and the like is limited.
The content of chloride ions in water can be measured by potentiometric titration, and the standard document is silver nitrate titration method for measuring chloride in water (GB 11896-89). A potentiometric titration method for measuring chloride uses a chlorine electrode as an indicating electrode, a glass electrode or a double-liquid reference electrode as a reference, a silver nitrate standard solution is used for titration, a millivoltmeter is used for measuring the potential change between the two electrodes, and in the process of constantly adding a small amount of silver nitrate, the reading of an instrument when the potential change is maximum is the titration end point.
Disclosure of Invention
The invention aims to provide a method for testing the content of residual chlorine on the surface of a powder toughening material.
The technical scheme for realizing the purpose of the invention is as follows:
the method for testing the content of the residual chlorine element on the surface of the powder toughening material comprises the following steps:
(1) Will qualityIs m Sample (A) The powder toughening material sample is placed in an oxygen bomb crucible, distilled water is introduced into a calorimeter to be used as absorption liquid during oxygen bomb combustion, the oxygen bomb is connected with an oxygen cylinder and then filled with oxygen, and then the oxygen bomb is connected with an ignition device to ignite and combust;
(2) After the chlorine bomb is fully combusted, the oxygen bomb is cooled to the room temperature and slowly rolls, and the contact frequency and the contact area of the sucked distilled water and the oxygen bomb are increased, so that the generated chlorine ions are fully absorbed into the distilled water;
(3) Taking out the liquid in the oxygen bomb, transferring the liquid into a container, cleaning the inside of the oxygen bomb with methanol, mixing the cleaned methanol with the liquid, adding methanol to a constant volume, uniformly stirring to obtain a solution to be detected, and recording the volume V of the solution to be detected General assembly ；
(4) Repeating the steps (1) to (3) by taking an empty oxygen bomb crucible as a blank control group to serve as a blank sample;
(5) Respectively move to obtain a volume V Measuring The solution to be tested and the blank sample are taken as test solutions, concentrated nitric acid is dripped until the PH of the test solution is 3-5, a silver nitrate potentiometric titration method is adopted, automatic titration is carried out by using a silver nitrate solution, and an end point is recorded, wherein the titration consumption volume of the solution to be tested is V 1 The titration consumption volume of the blank sample is V 0 ；
(6) According to formula C (Cl-) ＝(V 1 -V 0 )×C Silver nitrate ×35.45×1000/V Measuring And calculating to obtain the concentration C of chloride ions in the solution to be detected (Cl-) ；
(7) According to the formula m (Cl) ＝C (Cl-) ×V General assembly Calculating the mass m of chlorine (Cl-) ；
(8) According to the formula
The calculated content of the chlorine element in the powder toughening material is obtained>
The powder toughening material is a micron-sized powder material which takes polycarbonate, polyether ketone, polyurethane or polyamide as main components. The performances of the prepreg such as high temperature and high humidity environment tolerance, compression strength resistance, carbon fiber interlayer toughness and the like can be effectively improved through the coordination effect between the powder toughening material and the carbon fiber and resin matrix.
Preferably, in the step (1), oxygen is filled to a pressure of 2.5 to 3.5MPa.
Preferably, in the step (5), the titration solution is 0.01mol/L silver nitrate solution.
The method comprises the steps of completely burning the powder toughening material containing trace chloride in a high-pressure oxygen environment, converting the chloride remaining on the surface of the material into freely moving chloride ions, and carrying out potentiometric titration on the chloride ions by using a silver nitrate solution, so as to measure the content of the chlorine element remaining on the surface of the powder toughening material. The method is simple and convenient, has high repeatability, can accurately measure the content of the residual chlorine on the surface of the powder toughening material, and is convenient for subsequent evaluation of the quality of the powder toughening material.
Detailed Description
The present invention will be described in more detail with reference to specific examples.
In the following examples, the instruments used were a SJLRY-8000 microcomputer high-precision full-automatic calorimeter (Sanjie instrument, jimura) and a model ZDCL-2 chloride ion automatic potentiometric titrator (Shanghai Leimao).
Example 1
1. Pretreatment and combustion process
(1) Thoroughly cleaning a heat measuring cylinder and a crucible by using a small amount of distilled water, accurately weighing 2.02g of a powder toughening material sample, and placing the sample in the crucible after a bopp film is coated without pouring;
(2) Confirming that the calorimeter is connected with distilled water;
(3) Correctly installing an oxygen bomb, checking whether all components of the calorimeter are normal or not, connecting the oxygen bomb with an oxygen bottle, and filling oxygen until the pressure is 3.0Mpa;
(4) Immersing the oxygen bomb in a water bath and checking for no leakage; the water content of the oxygen bomb is wiped dry, and the oxygen bomb is connected to the ignition device for ignition.
2. Chlorine-containing test solution treatment process
(1) After full combustion, cooling the oxygen bomb to room temperature, and slowly rolling for 3-5mins;
(2) And slowly releasing the pressure of the oxygen bomb to atmospheric environment pressure, taking off an oxygen bomb cover, transferring the liquid into a 100ml beaker, cleaning the inside of the oxygen bomb by using a methanol reagent, adding the methanol reagent after cleaning to reach a constant volume of 80ml, and uniformly stirring to obtain the liquid to be detected.
3. Blank control procedure
(1) Repeating the steps 1 and 2, not placing the sample in the crucible, and repeating the experiment process by using the bopp film with the same specification to perform a blank experiment to obtain a blank sample.
4. Titration and data processing procedure
(1) Recording the total volume of the water sample to be measured as V General assembly =80ml, and remove V Side survey Transfer of =20ml into a test vial; dropwise adding concentrated nitric acid until the PH of the water sample to be detected is 3-5;
(2) Inputting test conditions by using a potentiometer of an automatic potentiometric titrator for chloride ions, and then cleaning/filling the burette by using a titration solution C Silver nitrate Silver nitrate solution of =0.01 mol/L;
(3) Placing a sample to be measured and a blank sample solution on a potentiometer table, and inputting measurement conditions;
(4) Automatically titrating the sample with silver nitrate solution, and automatically recording the end point, wherein the titration consumption volume of the solution to be measured is V 1 =0.16ml, titration consumption volume of blank sample V 0 ＝0.10ml；
(6) According to formula C (Cl-) ＝(V 1 -V 0 )×C Silver nitrate ×35.45×1000/V Measuring Wherein 35.45 is the molar mass of chloride ions (g/mol), C (Cl-) The unit of (a) is mg/L, and the concentration C of the chloride ions in the solution to be detected is obtained by calculation (Cl-) ＝1.06mg/L；
(7) According to the formula m (Cl) ＝C (Cl-) ×V General assembly Calculating the mass m of chlorine (Cl-) ＝0.085mg；
(8) According to the formula
The content of the chlorine element in the powder toughening material is obtained by calculation
/>
Claims (4)
1. The method for testing the content of the residual chlorine element on the surface of the powder toughening material is characterized by comprising the following steps of:
(1) With mass m Sample (A) The powder toughening material sample is placed in an oxygen bomb crucible, distilled water is introduced into a calorimeter to be used as absorption liquid during oxygen bomb combustion, the oxygen bomb is connected with an oxygen cylinder and then filled with oxygen, and then the oxygen bomb is connected with an ignition device to ignite and combust;
(2) After the chlorine bomb is fully combusted, the oxygen bomb is cooled to the room temperature and slowly rolls, and the contact frequency and the contact area of the sucked distilled water and the oxygen bomb are increased, so that the generated chlorine ions are fully absorbed into the distilled water;
(3) Taking out the liquid in the oxygen bomb, transferring the liquid into a container, cleaning the inside of the oxygen bomb with methanol, mixing the cleaned methanol with the liquid, adding methanol to a constant volume, uniformly stirring to obtain a solution to be detected, and recording the volume V of the solution to be detected General assembly ；
(4) Repeating the steps (1) to (3) by taking an empty oxygen bomb crucible as a blank control group to serve as a blank sample;
(5) Respectively take a volume V Measuring The solution to be tested and the blank sample are taken as test solutions, concentrated nitric acid is dripped until the PH of the test solution is 3-5, a silver nitrate potentiometric titration method is adopted, automatic titration is carried out by using a silver nitrate solution, and an end point is recorded, wherein the titration consumption volume of the solution to be tested is V 1 The titration consumption volume of the blank sample is V 0 ；
(6) According to formula C (Cl-) ＝(V 1 -V 0 )×C Silver nitrate ×35.45×1000/V Measuring And calculating to obtain the concentration C of chloride ions in the solution to be detected (Cl-) ；
(7) According to the formula m (Cl) ＝C (Cl-) ×V General assembly Calculating the mass m of chlorine (Cl-) ；
(8) According to the formula
The calculated content of the chlorine element in the powder toughening material is obtained>
2. The testing method according to claim 1, wherein in the step (1), the powder toughening material is a micron-sized powder material which mainly comprises polycarbonate, polyether ketone, polyurethane or polyamide.
3. The test method as set forth in claim 1, wherein in the step (1), oxygen is filled to a pressure of 2.5 to 3.5Mpa.
4. The test method according to claim 1, wherein in the step (5), the titration solution is 0.01mol/L silver nitrate solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211590806.1A CN115932158A (en) | 2022-12-12 | 2022-12-12 | Method for testing content of residual chlorine element on surface of powder toughening material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211590806.1A CN115932158A (en) | 2022-12-12 | 2022-12-12 | Method for testing content of residual chlorine element on surface of powder toughening material |
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| CN202211590806.1A Pending CN115932158A (en) | 2022-12-12 | 2022-12-12 | Method for testing content of residual chlorine element on surface of powder toughening material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017084189A1 (en) * | 2015-11-17 | 2017-05-26 | 西北大学 | Micro rotating bomb calorimeter |
| CN113484444A (en) * | 2021-07-30 | 2021-10-08 | 中冶南方都市环保工程技术股份有限公司 | Method for testing content of chlorine element in combustible solid waste |
| CN114965537A (en) * | 2022-06-02 | 2022-08-30 | 聊城鲁西聚碳酸酯有限公司 | Method for measuring total chlorine and inorganic chlorine content in polycarbonate resin |
-
2022
- 2022-12-12 CN CN202211590806.1A patent/CN115932158A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017084189A1 (en) * | 2015-11-17 | 2017-05-26 | 西北大学 | Micro rotating bomb calorimeter |
| CN113484444A (en) * | 2021-07-30 | 2021-10-08 | 中冶南方都市环保工程技术股份有限公司 | Method for testing content of chlorine element in combustible solid waste |
| CN114965537A (en) * | 2022-06-02 | 2022-08-30 | 聊城鲁西聚碳酸酯有限公司 | Method for measuring total chlorine and inorganic chlorine content in polycarbonate resin |
Non-Patent Citations (1)
| Title |
|---|
| 金谷等: "《分析化学实验》", 31 January 2020, 中国科学技术大学出版社, pages: 182 - 183 * |
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