CN101943687A - Method for detecting carboxylic group content of surface of carbon fiber - Google Patents
Method for detecting carboxylic group content of surface of carbon fiber Download PDFInfo
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- CN101943687A CN101943687A CN 201010284059 CN201010284059A CN101943687A CN 101943687 A CN101943687 A CN 101943687A CN 201010284059 CN201010284059 CN 201010284059 CN 201010284059 A CN201010284059 A CN 201010284059A CN 101943687 A CN101943687 A CN 101943687A
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Abstract
The invention relates to a method for detecting the carboxylic group content of the surface of a carbon fiber, which comprises the following steps of: 1, determining the reaction time of the carbon fiber in sodium bicarbonate with fixed concentration; 2, determining a blank; and 3, detecting the carboxylic group content of the surface of the carbon fiber. The method has the advantages of solving the technical problems of error proneness, expensive apparatus and complex data analysis in the conventional methods for measuring the carboxylic group content of the surface of the carbon fiber, and accurately determining the content of a trace functional group, along with simple operation.
Description
Technical field
The invention belongs to the detection technique field, be specifically related to a kind of method that detects the carbon fiber surface functional group content, be used to detect carbon fiber surface hydroxy-acid group content.
Background technology
Carbon fiber is a kind of novel charcoal material that rises the sixties in last century, it has a series of excellent properties such as high specific strength, high ratio modulus, high conductivity and thermal conductivity, low thermal coefficient of expansion, low-density, high temperature resistant, endurance, creep resistant, self-lubricating, be a kind of desirable functional material and structured material, be widely used in fields such as space flight, civil aviation, style and transportation, and have broad application prospects.
Not surface treated carbon fiber surface is comparatively smooth, surface energy is low, lack chemically active functional group, thereby causes it to be on duty mutually with the adhesive property between the matrix two-phase interfaces such as resin, can not give full play of the potential mechanical property of compound substance.In order to improve the composite performance of carbon fiber, people have adopted many SURFACE TREATMENT OF CARBON FIBER methods, but the variation of carbon fiber surface functional group as carboxylic acid, phenolic hydroxyl group and lactone etc., has increased complicacy for its composite material interface chemical action research.Therefore the foundation to the assay method of carbon fiber surface functional group is very important.In the past chemical titrations that adopt more, this method equipment is simple, can determine the content of carbon fiber surface functional group preferably, but for the lower carbon fiber of surface functional group content, error appears in titration end-point bad grasp easily.In addition, the x-ray photoelectron power spectrum also can be used to measure the content of carbon fiber surface functional group, and the instrument of this method is comparatively expensive, and the data analysis more complicated.
Summary of the invention
For error, instrument costliness, data analysis complicated technology problem appear in method easily that solve existing measurement carbon fiber surface hydroxy-acid group content, the invention provides a kind of method of fast detecting carbon fiber surface hydroxy-acid group content, but this method adopts the hydroxy-acid group content of chemical reaction type headspace analysis technology accurate detection carbon fiber surface.
Technical solution of the present invention:
A kind of method that detects carbon fiber surface hydroxy-acid group content, its special character is: may further comprise the steps:
1] carbon fiber determining in the fixed concentration reaction of sodium bicarbonate time:
1.1] take by weighing the carbon fiber that many parts of quality equate, be respectively put in the head space bottle of a plurality of same sizes, add the sodium bicarbonate of equal volume same concentrations respectively, sealing head space bottle;
1.2] above-mentioned a plurality of head space bottles are put into constant temperature water bath vibrate, described constant temperature water bath temperature is 50～80 ℃, every 2 minutes, extracting in the 1 microlitre head space bottle gas of gas-bearing formation portion with micro syringe is injected in the gas chromatograph and measures, content until the carbon dioxide of measuring is constant, and the mean oscillatory time of this moment is the reaction time of carbon fiber under this concentration sodium bicarbonate;
2] mensuration of blank sample:
Get a head space bottle, the sodium bicarbonate of equal volume same concentrations in adding and the step 1, sealing head space bottle, the head space bottle is put into constant temperature water bath to vibrate, described constant temperature water bath temperature is 50～80 ℃, duration of oscillation and step 1] in the determined time identical, extract in the 1 microlitre head space bottle gas of gas-bearing formation portion with micro syringe and be injected in the gas chromatograph and measure, obtain Carbon Dioxide in Air and sodium bicarbonate self and decompose the content that generates carbon dioxide;
3] detection of carbon fiber surface hydroxy-acid group content:
3.1] take by weighing the carbon fiber with step 1 equal in quality, put into the head space bottle, add the sodium bicarbonate that has the equal volume same concentrations with step 1, sealing head space bottle;
3.2] the head space bottle is put into constant temperature water bath vibrate, described constant temperature water bath temperature is 50～80 ℃, duration of oscillation and step 1] in the determined time identical, extract in the 1 microlitre head space bottle gas of gas-bearing formation portion with micro syringe and be injected in the gas chromatograph and measure, record the content of result for all carbon dioxide in the head space bottle;
3.3] with step 3.2] and in resulting carbon dioxide content deduction Carbon Dioxide in Air and sodium bicarbonate self decompose the content that generates carbon dioxide, can calculate the content of the carbon dioxide that the carbon fiber surface hydroxy-acid group produced, thereby calculate the content of carbon fiber unit mass surface hydroxy-acid group.
The advantage that the present invention had:
The present invention adopts chemical reaction type headspace analysis technology for detection carbon fiber surface hydroxy-acid group content, the composition (nonvolatile) that original gas chromatography can not be measured is converted into volatile composition, thereby realizes with the indirect determination of gas chromatography to this involatile constituent.Compare with detection method in the past, this method is simple to operate, can accurately measure the content of micro-functional group.
Embodiment
The present invention adopts the content of chemical reaction type headspace analysis technology for detection carbon fiber surface hydroxy-acid group, comprise that a certain amount of carbon fiber adds the determining of finite concentration reaction of sodium bicarbonate time, the mensuration of blank sample, the job steps such as detection of carbon fiber surface hydroxy-acid group content, its concrete steps are:
Step 1, a certain amount of carbon fiber add determining of finite concentration reaction of sodium bicarbonate time:
Take by weighing 5 parts on the carbon fiber of homogenous quantities, put in the head space bottle of five 20ml, add the finite concentration sodium bicarbonate of 10ml respectively, sealing head space bottle is put into constant temperature water bath with the head space bottle, in 50～80 ℃, vibrates 6～14 minutes.Beginning in 6 minutes every 2 minutes, is injected into the gas of gas-bearing formation portion in the 1 microlitre head space bottle in the gas chromatograph with micro syringe and measures, and is constant until the content of carbon dioxide, thereby determines average reaction time.
The mensuration of step 2, blank sample:
Get a head space bottle, add the finite concentration sodium bicarbonate of 10ml, sealing head space bottle is put into constant temperature water bath with the head space bottle, in 50-80 ℃, the vibration certain hour is identical in this time and the step 1.With micro syringe the gas of gas-bearing formation portion in the 1 microlitre head space bottle is injected in the gas chromatograph and measures, be used for deducting air and sodium bicarbonate self decomposes the influence that generates carbon dioxide.
The detection of step 3, carbon fiber surface hydroxy-acid group content:
Take by weighing the carbon fiber with the step 1 equal in quality, put into the head space bottle, add the sodium bicarbonate of 10ml, identical in the concentration of sodium bicarbonate and the step 1, sealing head space bottle is put into constant temperature water bath with the head space bottle, under 50～80 ℃ of temperature, vibrate, identical in duration of oscillation and the step 1.After vibration finishes, with micro syringe the gas of gas-bearing formation portion in the 1 microlitre head space bottle is injected in the gas chromatograph and measures.The result deducts Carbon Dioxide in Air and sodium bicarbonate self decomposes the content that generates carbon dioxide according to recording, and calculates the content of carbon fiber unit mass surface hydroxy-acid group.
Embodiment: taking by weighing this laboratory is the carbon fiber 0.5g of starching through surface treatment, puts it in the head space bottle of 20ml, and adding 10ml concentration in the head space bottle is 5.00 * 10
-3The sodium bicarbonate solution of mol/L, sealing head space bottle is put into constant temperature water bath with the head space bottle, in 60 ℃, vibrates 10 minutes.Then the gas of gas-bearing formation portion in the 1 microlitre head space bottle is injected in the gas chromatograph and measures with micro syringe.Determine the content 5.82 * 10 of carbon dioxide by the head space gas in the mensuration equilibrium system
-6Mol/g.Do blank test, decompose the influence that generates carbon dioxide with sodium bicarbonate self in the deduction air.From the result who obtains, calculate the content 4.98 * 10 of this carbon fiber surface hydroxy-acid group
-6Mol/g.
Claims (1)
1. method that detects carbon fiber surface hydroxy-acid group content is characterized in that: may further comprise the steps:
1] carbon fiber determining in the fixed concentration reaction of sodium bicarbonate time:
1.1] take by weighing the carbon fiber that many parts of quality equate, be respectively put in the head space bottle of a plurality of same sizes, add the sodium bicarbonate of equal volume same concentrations respectively, sealing head space bottle;
1.2] above-mentioned a plurality of head space bottles are put into constant temperature water bath vibrate, described constant temperature water bath temperature is 50～80 ℃, every 2 minutes, extracting in the 1 microlitre head space bottle gas of gas-bearing formation portion with micro syringe is injected in the gas chromatograph and measures, content until the carbon dioxide of measuring is constant, and the mean oscillatory time of this moment is the reaction time of carbon fiber under this concentration sodium bicarbonate;
2] mensuration of blank sample:
Get a head space bottle, the sodium bicarbonate of equal volume same concentrations in adding and the step 1, sealing head space bottle, the head space bottle is put into constant temperature water bath to vibrate, described constant temperature water bath temperature is 50～80 ℃, duration of oscillation and step 1] in the determined time identical, extract in the 1 microlitre head space bottle gas of gas-bearing formation portion with micro syringe and be injected in the gas chromatograph and measure, obtain Carbon Dioxide in Air and sodium bicarbonate self and decompose the content that generates carbon dioxide;
3] detection of carbon fiber surface hydroxy-acid group content:
3.1] take by weighing the carbon fiber with step 1 equal in quality, put into the head space bottle, add the sodium bicarbonate that has the equal volume same concentrations with step 1, sealing head space bottle;
3.2] the head space bottle is put into constant temperature water bath vibrate, described constant temperature water bath temperature is 50～80 ℃, duration of oscillation and step 1] in the determined time identical, extract in the 1 microlitre head space bottle gas of gas-bearing formation portion with micro syringe and be injected in the gas chromatograph and measure, record the content of result for all carbon dioxide in the head space bottle;
3.3] with step 3.2] and in resulting carbon dioxide content deduction Carbon Dioxide in Air and sodium bicarbonate self decompose the content that generates carbon dioxide, can calculate the content of the carbon dioxide that the carbon fiber surface hydroxy-acid group produced, thereby calculate the content of carbon fiber unit mass surface hydroxy-acid group.
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| CN 201010284059 CN101943687A (en) | 2010-09-16 | 2010-09-16 | Method for detecting carboxylic group content of surface of carbon fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109540945A (en) * | 2018-08-30 | 2019-03-29 | 北京化工大学 | The method of quantitatively characterizing carbon fiber physical structure |
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2010
- 2010-09-16 CN CN 201010284059 patent/CN101943687A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《中国造纸》 20050930 侯庆喜 等 应用顶空气相色谱测定纸浆纤维的羧基含量 1 第24卷, 第9期 * |
| 《化学进展》 20080531 柴欣生 等 静态顶空气相色谱技术 全文 1 第20卷, 第5期 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109540945A (en) * | 2018-08-30 | 2019-03-29 | 北京化工大学 | The method of quantitatively characterizing carbon fiber physical structure |
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Application publication date: 20110112 |