CN106770915A - The method of quick test carbon fiber electrolytic liquid concentration - Google Patents
The method of quick test carbon fiber electrolytic liquid concentration Download PDFInfo
- Publication number
- CN106770915A CN106770915A CN201611150875.5A CN201611150875A CN106770915A CN 106770915 A CN106770915 A CN 106770915A CN 201611150875 A CN201611150875 A CN 201611150875A CN 106770915 A CN106770915 A CN 106770915A
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- China
- Prior art keywords
- electrolyte
- concentration
- carbon fiber
- refraction index
- refractometer
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Classifications
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- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
Abstract
The present invention relates to carbon fiber production technical field, specifically a kind of method of quick test carbon fiber electrolytic liquid concentration comprises the following steps：Using the electrolyte of high concentration, the electrolyte of several various concentrations is diluted to respectively, be utilized respectively titration test concentration of electrolyte；The electrolyte 50ml of various concentrations after diluting is taken respectively, quantitative phenolphthalein reagent is added thereto to, and after being well mixed, the refraction index of the solution is tested using refractometer, using NH4HCO3Concentration of electrolyte and refraction index, set up concentration --- the standard curve of refraction index, and standard curve is set up on refractometer.The present invention improves the safety in utilization and safe operation of chemical reagent in operating process, meanwhile, the method can more quick, accurate, intuitively ensure the accuracy of detection of carbon fiber electrolytic liquid concentration, be conducive to quickly instructing actual production.
Description
Technical field
The present invention relates to carbon fiber production technical field, NH in specifically a kind of carbon fiber production process4HCO3Electrolysis
The fast and accurately detection method of liquid concentration.
Background technology
It is known that the features such as carbon fiber has excellent specific strength, specific modulus and heat resistance, is to prepare advanced composite material
One of main reinforcement material of material, is widely used in the every field of national economy, and especially being played in national defence can not
The effect of replacement, but because carbon fiber surface is smooth, composite wood poor in the adhesive property between chemical inertness, with matrix resin
Material boundary strength is low, the performance of influence material entirety excellent properties, therefore, in order to improve the overall performance of composite, it is necessary to
Carbon fiber surface is modified.
Carbon fiber depends on active group and the body tree of carbon fiber surface with the Nian Jie degree of body resin two-phase interface
Fat active group carries out the chemical bond of chemical reaction generation.In NH4HCO3Carbon fiber surface mainly there occurs the electric discharge of water in solution
The electrochemical oxidation reactions of oxygen evolution reaction and fiber surface electroactive material, the absorption produced in the electric discharge oxygen evolution reaction of water
The oxygen atom of state hydroxide ion and nascent state directly can react generation phase in the presence of anode current with fiber surface
The hydroxyl and carbonyl answered.The purpose of surface treatment of carbon fibers is to improve Chemical bonding.
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of quick test carbon fiber electrolytic liquid concentration
Method, quickly, accurately detects NH4HCO3Concentration of electrolyte, shortens detection cycle, improves NH in carbon fiber production process4HCO3Electricity
Promptness, dynamic and control accuracy that solution liquid concentration is controlled.
The present invention solve above-mentioned technical problem use technical scheme be：A kind of quick test carbon fiber electrolytic liquid concentration
Method, comprises the following steps：Using the electrolyte of high concentration, the electrolyte of several various concentrations is diluted to respectively, be utilized respectively
Titration tests concentration of electrolyte；The electrolyte 50ml of various concentrations after diluting is taken respectively, is added thereto to quantitative phenolphthalein examination
Agent, after being well mixed, the refraction index of the solution is tested using refractometer, using NH4HCO3Concentration of electrolyte and refraction index,
Set up concentration --- the standard curve of refraction index, and standard curve is set up on refractometer.
The beneficial effects of the invention are as follows improve the safety in utilization and safe operation of chemical reagent in operating process, together
When, the method can more quick, accurate, intuitively ensure the accuracy of detection of carbon fiber electrolytic liquid concentration, be conducive to quickly referring to
Lead actual production.
Specific embodiment
With reference to embodiment, the invention will be further described：
Using the electrolyte of high concentration, the electrolyte of several various concentrations is diluted to respectively, be utilized respectively titration test electrolysis
Liquid concentration.
The electrolyte 50ml of various concentrations after diluting is taken respectively, is added thereto to quantitative phenolphthalein reagent, after being well mixed,
The refraction index of the solution is tested using refractometer, using NH4HCO3Concentration of electrolyte and refraction index set up concentration --- refractive power
The standard curve of index, and standard curve is set up on refractometer.
This method is diluted using the electrolyte of concentration about 15g/L, and tests various concentrations with titration and refractometry
The actual concentrations and refraction index of electrolyte, details such as table 1：
The actual concentrations and refraction index of the various concentrations electrolyte of table 1
| Theoretical Mass percentage, % | Quantity of sampling quantity, ml | Constant volume, ml | Titration tests actual mass percentage, % | Refraction index |
| 15 | —— | —— | 12.8 | 1.34740 |
| 9 | 60 | 100 | 8.04 | 1.34117 |
| 6 | 40 | 100 | 5.34 | 1.33843 |
| 1.5 | 10 | 100 | 1.62 | 1.33424 |
| Pure water（Concentration 0） | —— | —— | 0 | 1.33259 |
Using the concentration and refraction index of electrolyte, concentration is set up --- the standard curve y=0.0011x+ of refraction index
1.3324。
Refractometry tests NH4HCO3The operating procedure of concentration of electrolyte：
1. the NH that 10ml pipettes measure 10ml is measured with graduated cylinder4HCO3Electrolyte, and a certain amount of phenolphthalein reagent is added to middle,
It is well mixed；
2. the power switch of refractometer is opened, test temperature as 25 DEG C is set；Meanwhile, select NH4HCO3The mark of concentration of electrolyte
Directrix curve；
3. 2-3 drops distilled water being taken to prism surface with glue head dropper and covering prism, cover prism lid, refractometer is carried out clearly
Zero；
4. with absorbent cotton by prism wiped clean after, take 2-3 drop mixed liquors and be added on refractometer prism, treat that temperature reaches 25 DEG C
Afterwards, test concentrations value is directly read.
Titration tests NH4HCO3The operating procedure of concentration of electrolyte：
1st, prepare and demarcate dilute H of 0.5mol/L2SO4Standard liquid.
1. it is configured to dilute H of 0.5mol/L2SO4Standard liquid：Take the 15ml concentrated sulfuric acids add 1000ml distilled water in, cooling,
Shake up；
2. the high temperature furnace of 0.95g is weighed with electronic balance（270-300℃）The Na of calcination2CO3, it is dissolved in 50ml distilled water, and
It is added thereto to 10 drop bromocresol greens-methyl red indicator；
3. with the dilute H for preparing2SO4Solution titrates the solution and is extremely changed into kermesinus from green, and boils 2min, continues to drip after cooling
It is in kermesinus to determine to solution, while doing blank test；
4. dilute H of preparation is calculated2SO4The actual concentrations of solution are：
In formula：
M—— Na2CO3Molal weight, (MNa2CO3=53g/mol)；
V1——H2SO4The volume of solution；
V2--- blank assay H2SO4The volume of solution.
2nd, prepare and demarcate the NaOH standard liquids of 0.5mol/L.
1. the NaOH standard liquids of 0.5mol/L are prepared：110gNaOH is weighed, is dissolved in water of the 100ml without carbon dioxide,
It is closed to put limpid to solution, 27ml supernatant liquors are measured with plastic tube, 1000ml is diluted to pure water, and shake up；
2. Potassium Hydrogen Phthalate 3.6g, plus 80ml distillation water dissolves are weighed, then Jia 2 and drip phenolphthalein indicator（10g/L）, with preparation
Good NaOH standard liquids are titrated to solution pinkiness, and keep 30s.Do blank test simultaneously；
3. the actual concentrations of NaOH standard liquids are calculated：
In formula：
The actual mass of m --- Potassium Hydrogen Phthalate；
The molal weight of M=Potassium Hydrogen Phthalates, 204.22g/mol；
V1--- the volume of NaOH solution；
V2--- the volume of blank assay NaOH solution.
3rd, NH is titrated4HCO3Electrolyte.
1. the NH of about 10g is weighed with electronic balance4HCO3Electrolyte is added thereto to 50ml in 250ml conical flasks
Dilute H2SO4Standard liquid, shakes conical flask, sample is reacted completely；
2. conical flask is placed on electric furnace, carrying out heating to it boils, and evicts carbon dioxide from；
3. 3-4 drops methyl red-methylene blue indicator is added after cooling down；
4. it is terminal to titrate the solution gray with the NaOH standard liquids prepared；
5. calculate：
In formula：C1--- dilute H2SO4The concentration of standard liquid；
V1--- dilute H2SO4The volume of standard liquid；
C2--- the concentration of NaOH standard liquids；
V2--- the volume of NaOH standard liquids；
V --- measure NH4HCO3The volume of electrolyte.
Embodiment 1,8% concentration of electrolyte is about with refractometry test concentrations.
Embodiment 2,3% concentration of electrolyte is about with refractometry test concentrations.
Comparative example 1,8% concentration of electrolyte is about using titration test concentrations.
Comparative example 2,3% concentration of electrolyte is about using titration test concentrations.
Test concentrations is relatively shown in Table 2 between embodiment 1, embodiment 2, comparative example 1 and comparative example 2：
The comparing of the electrolyte test concentrations of table 2
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | Sample 8 | |
| Embodiment 1 | 8.4% | 8.8 % | 7.8 % | 8.7 % | 8.7 % | 9.0 % | 7.9 % | 8.3 % |
| Comparative example 1 | 8.5 % | 8.5% | 7.7% | 8.6% | 8.3 % | 8.2 % | 7.8% | 8.2 % |
| Embodiment 2 | 3.7 % | 3.4% | 3.7 % | 3.7 % | 3.1 % | 3.8% | 3.6% | 3.6 % |
| Comparative example 2 | 3.8% | 3.2 % | 3.8 % | 3.8 % | 3.1 % | 3.0 % | 3.4% | 3.8 % |
Claims (1)
1. a kind of method of quick test carbon fiber electrolytic liquid concentration, comprises the following steps：Using the electrolyte of high concentration, difference
The electrolyte of several various concentrations is diluted to, titration test concentration of electrolyte is utilized respectively；Various concentrations after dilution are taken respectively
Electrolyte 50ml, be added thereto to quantitative phenolphthalein reagent, be well mixed after, the refractive power for testing the solution using refractometer refers to
Number, using NH4HCO3Concentration of electrolyte and refraction index, set up concentration --- the standard curve of refraction index, and on refractometer
Set up standard curve.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109115589A (en) * | 2018-09-05 | 2019-01-01 | 广西玉柴机器股份有限公司 | It is a kind of to measure the effective working concentration method of anti-icing fluid with saccharometer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06288924A (en) * | 1993-03-30 | 1994-10-18 | Idemitsu Petrochem Co Ltd | Measuring method for electrolyte |
| CN101871887A (en) * | 2010-06-28 | 2010-10-27 | 中国科学院西安光学精密机械研究所 | Method for on-line detection of coagulation bath concentration in production of polyacrylonitrile strands for carbon fibers |
| CN103160852A (en) * | 2013-04-04 | 2013-06-19 | 安徽首文碳纤维有限公司 | Method for detecting concentration of electrolyte on carbon fiber production line |
-
2016
- 2016-12-14 CN CN201611150875.5A patent/CN106770915A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06288924A (en) * | 1993-03-30 | 1994-10-18 | Idemitsu Petrochem Co Ltd | Measuring method for electrolyte |
| CN101871887A (en) * | 2010-06-28 | 2010-10-27 | 中国科学院西安光学精密机械研究所 | Method for on-line detection of coagulation bath concentration in production of polyacrylonitrile strands for carbon fibers |
| CN103160852A (en) * | 2013-04-04 | 2013-06-19 | 安徽首文碳纤维有限公司 | Method for detecting concentration of electrolyte on carbon fiber production line |
Non-Patent Citations (1)
| Title |
|---|
| 张黎明: "折光法在碳纤维上浆溶液浓度分析中的应用", 《石油化工技术与经济》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109115589A (en) * | 2018-09-05 | 2019-01-01 | 广西玉柴机器股份有限公司 | It is a kind of to measure the effective working concentration method of anti-icing fluid with saccharometer |
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