CN114113027A - Method for efficiently and visually inspecting carbon fiber sizing effect - Google Patents
Method for efficiently and visually inspecting carbon fiber sizing effect Download PDFInfo
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- CN114113027A CN114113027A CN202111632113.XA CN202111632113A CN114113027A CN 114113027 A CN114113027 A CN 114113027A CN 202111632113 A CN202111632113 A CN 202111632113A CN 114113027 A CN114113027 A CN 114113027A
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6439—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" with indicators, stains, dyes, tags, labels, marks
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Abstract
The invention discloses a method for efficiently and visually inspecting the sizing effect of carbon fibers, which comprises the following steps of S1: selecting and hydrolyzing a fluorescent whitening agent; step S2: mixing of fluorescent whitening agent and sizing agent; step S3: sizing the carbon fiber tows; step S4: and (4) evaluating the irradiation and sizing effect of the carbon fiber tows. The specific operation steps for finishing the evaluation of the sizing effect are as follows: selecting a fluorescent whitening agent, dissolving the fluorescent whitening agent in deionized water at 50-60 ℃, adding the dissolved fluorescent whitening agent into a carbon fiber sizing circulation tank, adding a fluorescent agent for 30 minutes, and irradiating finished fibers by an ultraviolet lamp in a filament collecting working section, so that the dispersing uniformity of the sizing agent can be judged through fluorescent distribution, and the sizing effect can be evaluated. The method has no influence on the mechanical property of the fiber, visually represents the sizing effect by adding the fluorescent whitening agent and irradiating the ultraviolet light by a visual method, has the characteristics of intuition and high efficiency, and fills the blank of the method for representing the sizing effect of the carbon fiber.
Description
Technical Field
The invention relates to the technical field of carbon fiber production, in particular to a method for efficiently and visually inspecting the sizing effect of carbon fibers.
Background
Carbon Fibers (CF) are fibrous polymers that are converted from organic fibers by a solid-phase reaction. The fiber has a series of excellent performances of high specific strength, high specific modulus, high temperature resistance, chemical corrosion resistance, fatigue resistance, thermal shock resistance, radiation resistance, electric conduction, heat transfer, small specific gravity and the like, and belongs to typical high-performance fibers. The preparation process of the carbon fiber is complex and relates to a plurality of disciplines, wherein the sizing process is a necessary procedure in the preparation process of the carbon fiber, and not only influences the physical state of the fiber, but also directly influences the downstream processing manufacturability and product performance of the carbon fiber. In order to visually characterize the sizing effect. Therefore, the method is improved, and the method for efficiently and visually checking the sizing effect of the carbon fibers is provided.
Disclosure of Invention
In order to solve the technical problems, the invention provides the following technical scheme:
the invention relates to a method for efficiently and visually inspecting the sizing effect of carbon fibers, which comprises the following steps of:
step S1: selecting and hydrolyzing a fluorescent whitening agent, selecting a fluorescent whitening agent, and dissolving the fluorescent whitening agent by using deionized water;
step S2: mixing the fluorescent whitening agent and the sizing agent, adding the hydrolyzed fluorescent whitening agent into a carbon fiber sizing circulation tank, adding the sizing agent, and stirring to uniformly mix the fluorescent whitening agent and the sizing agent;
step S3: sizing the carbon fiber tows, wherein the carbon fiber tows pass through a carbon fiber sizing circulation tank filled with a sizing agent, and the sizing agent permeates into the carbon fiber tows and is attached to the surface of a single fiber in the operation process to finish the sizing process;
step S4: and (3) evaluating the irradiation and sizing effect of the carbon fiber tows, irradiating finished carbon fiber tows by using an ultraviolet lamp at a filament collecting working section, judging the dispersion uniformity of a sizing agent through fluorescence distribution, and finishing evaluation on the sizing effect.
As a preferable technical scheme of the present invention, in step S1, the fluorescent whitening agent is selected from fluorescent whitening agents that are all light-colored after hydrolysis, and there is no significant difference in appearance of the carbon fiber tow after sizing of the fluorescent whitening agent.
In a preferred embodiment of the present invention, in step S1, the fluorescent whitening agent is a planar conjugated system with pi electrons in all molecules, and has a structure of-C-or-N-C-N-C, and has no chemical reaction with the main component of the sizing agent.
In a preferred embodiment of the present invention, the temperature for dissolving the fluorescent whitening agent and the deionized water in step S1 is 50-60 ℃.
In a preferred embodiment of the present invention, in step S2, the sizing agent is a water-soluble sizing agent whose main component is epoxy resin, and the sizing agent does not chemically react with molecules of the fluorescent whitening agent, and does not affect various properties of the final fiber.
As a preferred technical solution of the present invention, in the step S3, the carbon fiber tows are sized by a direct dipping method, and the carbon fiber tows are in a tensioned state all the time during the sizing process.
In a preferred embodiment of the present invention, the sizing of the carbon fiber tow in step S3 is determined by the length of the dipping distance and the running speed of the carbon fiber tow in the carbon fiber sizing circulation tank.
As a preferable technical scheme, the carbon fiber tows obtained in the step S4 are irradiated by the ultraviolet lamp under dark conditions, and the radiation intensity value of the ultraviolet lamp is 70 mu m/cm2To 90 μm/cm2。
The invention has the beneficial effects that:
according to the method for efficiently and visually inspecting the carbon fiber sizing effect, the sizing effect is visually represented by adding the fluorescent whitening agent and irradiating a visual method by ultraviolet rays, technical innovation in the field is achieved, and the blank of the sizing effect representation method is filled. The most remarkable characteristics are as follows: the addition of the optical brightener does not have any influence on the appearance of the fibers and on the mechanical properties and interlaminar shear strength.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a fluorescence effect diagram of example 3 of a method for efficiently and visually inspecting the sizing effect of carbon fibers according to the present invention;
FIG. 2 is a fluorescence effect diagram of embodiment 4 of the method for efficiently and visually inspecting the sizing effect of the carbon fiber.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1:
as shown in figure 1-the invention relates to a method for efficiently and visually checking the sizing effect of carbon fibers, which comprises the following steps:
step S1: selecting and hydrolyzing a fluorescent whitening agent, selecting a fluorescent whitening agent, and dissolving the fluorescent whitening agent by using deionized water;
step S2: mixing the fluorescent whitening agent and the sizing agent, adding the hydrolyzed fluorescent whitening agent into a carbon fiber sizing circulation tank, adding the sizing agent, and stirring to uniformly mix the fluorescent whitening agent and the sizing agent;
step S3: sizing the carbon fiber tows, wherein the carbon fiber tows pass through a carbon fiber sizing circulation tank filled with a sizing agent, and the sizing agent permeates into the carbon fiber tows and is attached to the surface of a single fiber in the operation process to finish the sizing process;
step S4: and (3) evaluating the irradiation and sizing effect of the carbon fiber tows, irradiating finished carbon fiber tows by using an ultraviolet lamp at a filament collecting working section, judging the dispersion uniformity of a sizing agent through fluorescence distribution, and finishing evaluation on the sizing effect.
Example 2:
based on example 1, in step S1, the fluorescent whitening agent is selected from fluorescent whitening agents which are all light-colored after hydrolysis, and the sizing of the fluorescent whitening agent has no obvious difference under natural light of appearance of the carbon fiber tow, and the fluorescent whitening agent which is light-colored after hydrolysis
In step S1, the fluorescent whitening agent is a planar conjugated system with pi electrons in its molecule, and has a structure of-C-or-N-C, and does not chemically react with the main component of the sizing agent.
Wherein the temperature for dissolving the fluorescent whitening agent and the deionized water in the step S1 is 50-60 ℃.
In step S2, the sizing agent is a water-soluble sizing agent whose main component is epoxy resin, and the sizing agent and the molecules of the fluorescent whitening agent do not have chemical reaction and do not have any influence on various properties of the final fiber.
The carbon fiber tows are sized in the step S3 by a direct dipping method, the carbon fiber tows are always in a tensioning state in the sizing process, sizing agents used in the carbon fiber preparation process are all water-soluble, and the time required for completely infiltrating the carbon fibers is long under the condition that the carbon fiber tows are tensioned, so that the dipping distance and the running speed of the carbon fiber tows in the carbon fiber sizing circulation tank are controlled.
The sizing of the carbon fiber tows in the step S3 is determined by the dipping distance and the running speed of the carbon fiber tows in the carbon fiber sizing circulation tank, and the sizing agent permeates into the carbon fiber tows and adheres to the surface of single fibers in the running process to complete the sizing process.
Wherein the carbon fiber tows obtained in the step S4 are irradiated by the ultraviolet lamp under dark conditions, and the radiation intensity value of the ultraviolet lamp is 70 mu m/cm2To 90 μm/cm2Under the dark condition, the ultraviolet lamp light is convenient to irradiate on the carbon fiber tows to enable fluorescent particles in the fluorescent whitening agent to emit light, whether sizing of the sizing agent is uniform or not is convenient to observe, and when the radiation intensity value of the ultraviolet lamp is lower than 70 mu m/cm2Or more than 90 mu m/cm2And in the process, the fluorescent particles in the fluorescent whitening agent do not obviously emit light, and the sizing effect is reduced.
Example 3:
on the basis of example 2, a method for testing the sizing effect of the carbon fiber is established:
and (3) completely dissolving 300g of ER fluorescent whitening agent in 500ml of deionized water at 60 ℃, adding the mixture into a carbon fiber sizing circulation tank, adding fluorescent whitening agent with the concentration of 0.05 per mill, and irradiating a finished carbon fiber tow by using an ultraviolet lamp at a filament collecting working section after adding the fluorescent whitening agent for 30 minutes.
Example 4:
on the basis of example 3, a comparative method for testing the sizing effect of the carbon fibers is established:
100g of ER fluorescent whitening agent and 400g of BC fluorescent whitening agent are respectively taken, and are completely dissolved by 1200ml of deionized water at the temperature of 60 ℃, then the mixture is added into a carbon fiber sizing circulating tank, the concentration of the fluorescent whitening agent is 0.08 per mill, and after fluorescent agent is added for 30 minutes, the finished carbon fiber tows are irradiated by an ultraviolet lamp at a reeling section.
The results of comparing the mechanical properties before and after the two groups of examples are shown in Table 1:
mechanical properties | strength/MPa | modulus/GPa | Interlaminar shear strength/MPa |
Before implementation | 4689 | 243 | 70.2 |
Example 3 | 4703 | 241 | 71.8 |
Example 4 | 4677 | 244 | 69.9 |
Finally, it should be noted that the above embodiments are implemented:
1. a centrifugal machine is needed to be used for mixing and stirring in the mixing of the fluorescent whitening agent and the sizing agent, so that the stirring is more uniform, and the problem that the detection effect is not obvious due to the uneven mixing of the fluorescent whitening agent and the sizing agent is avoided;
2. the temperature change should be monitored in real time during the heating process of the deionized water solution, so as to prevent the detection result from being influenced by overhigh or overlow temperature.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for efficiently and visually inspecting the sizing effect of carbon fibers is characterized by comprising the following steps:
step S1: selecting and hydrolyzing a fluorescent whitening agent, selecting a fluorescent whitening agent, and dissolving the fluorescent whitening agent by using deionized water;
step S2: mixing the fluorescent whitening agent and the sizing agent, adding the hydrolyzed fluorescent whitening agent into a carbon fiber sizing circulation tank, adding the sizing agent, and stirring to uniformly mix the fluorescent whitening agent and the sizing agent;
step S3: sizing the carbon fiber tows, wherein the carbon fiber tows pass through a carbon fiber sizing circulation tank filled with a sizing agent, and the sizing agent permeates into the carbon fiber tows and is attached to the surface of a single fiber in the operation process to finish the sizing process;
step S4: and (3) evaluating the irradiation and sizing effect of the carbon fiber tows, irradiating finished carbon fiber tows by using an ultraviolet lamp at a filament collecting working section, judging the dispersion uniformity of a sizing agent through fluorescence distribution, and finishing evaluation on the sizing effect.
2. The method for efficiently and intuitively inspecting the sizing effect of the carbon fibers according to claim 1, wherein the fluorescent whitening agent in the step S1 is a fluorescent whitening agent which is light in color after hydrolysis, and the sizing of the fluorescent whitening agent has no obvious difference in the appearance of the carbon fiber tows under natural light.
3. The method for efficiently and intuitively inspecting the sizing effect of the carbon fiber according to claim 1, wherein the fluorescent whitening agent in the step S1 is a planar conjugated system with pi-electrons in the molecules, and the structure of the system is as follows, -C-or-N-C, and the system has no chemical reaction with the main component of the sizing agent.
4. The method for high-efficiency visual inspection of carbon fiber sizing effect according to claim 1, wherein the temperature for dissolving the fluorescent whitening agent and the deionized water in the step S1 is 50-60 ℃.
5. The method for high-efficiency visual inspection of the sizing effect of carbon fibers according to claim 1, wherein the sizing agent in step S2 is a water-soluble sizing agent with epoxy resin as a main component, and the sizing agent has no chemical reaction with molecules of a fluorescent whitening agent and has no influence on various properties of the final fibers.
6. The method for efficiently and visually inspecting the sizing effect of the carbon fiber according to claim 1, wherein the sizing of the carbon fiber tows in the step S3 is performed by a direct dipping method, and the carbon fiber tows are in a tensioned state all the time during the sizing.
7. The method for efficiently and visually inspecting the sizing effect of the carbon fiber according to claim 1, wherein the sizing of the carbon fiber tows in the step S3 is determined by the dipping distance and the running speed of the carbon fiber tows in the carbon fiber sizing circulation tank.
8. The efficient visual inspection carbon fiber sizing effect of claim 1The method is characterized in that the carbon fiber tows obtained in the step S4 are irradiated by an ultraviolet lamp under dark conditions, and the radiation intensity value of the ultraviolet lamp is 70 mu m/cm2To 90 μm/cm2。
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Citations (6)
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---|---|---|---|---|
US4738866A (en) * | 1987-03-20 | 1988-04-19 | Burlington Industries, Inc. | Apparatus and method for determining whether an adequate amount of sizing has been applied to yarn ends |
CN1143943A (en) * | 1994-03-14 | 1997-02-26 | Ppg工业公司 | Glass fibre sizing and sized glass fibers and polyolefin reinforcing articles |
US6020064A (en) * | 1997-05-13 | 2000-02-01 | Owens Corning Fiberglas Technology, Inc. | Nonaqueous sizing for glass and carbon fibers |
JP2016169469A (en) * | 2016-05-25 | 2016-09-23 | 倉敷紡績株式会社 | Method for producing fiber for fiber-reinforced resin |
CN108333205A (en) * | 2018-02-23 | 2018-07-27 | 江苏恒神股份有限公司 | A kind of test method of carbon fiber starching uniformity |
CN112725962A (en) * | 2020-12-24 | 2021-04-30 | 武汉鑫碳科技有限公司 | Process, equipment and application for sizing and twisting spread carbon fiber tows |
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- 2021-12-29 CN CN202111632113.XA patent/CN114113027A/en active Pending
Patent Citations (7)
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US4738866A (en) * | 1987-03-20 | 1988-04-19 | Burlington Industries, Inc. | Apparatus and method for determining whether an adequate amount of sizing has been applied to yarn ends |
CN1143943A (en) * | 1994-03-14 | 1997-02-26 | Ppg工业公司 | Glass fibre sizing and sized glass fibers and polyolefin reinforcing articles |
US5646207A (en) * | 1994-03-14 | 1997-07-08 | Ppg Industries, Inc. | Aqueous sizing compositions for glass fibers providing improved whiteness in glass fiber reinforced plastics |
US6020064A (en) * | 1997-05-13 | 2000-02-01 | Owens Corning Fiberglas Technology, Inc. | Nonaqueous sizing for glass and carbon fibers |
JP2016169469A (en) * | 2016-05-25 | 2016-09-23 | 倉敷紡績株式会社 | Method for producing fiber for fiber-reinforced resin |
CN108333205A (en) * | 2018-02-23 | 2018-07-27 | 江苏恒神股份有限公司 | A kind of test method of carbon fiber starching uniformity |
CN112725962A (en) * | 2020-12-24 | 2021-04-30 | 武汉鑫碳科技有限公司 | Process, equipment and application for sizing and twisting spread carbon fiber tows |
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