CN101235590A - Ultrasonic chemistry surface modifying method for PBO fiber - Google Patents
Ultrasonic chemistry surface modifying method for PBO fiber Download PDFInfo
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- CN101235590A CN101235590A CNA2008101008768A CN200810100876A CN101235590A CN 101235590 A CN101235590 A CN 101235590A CN A2008101008768 A CNA2008101008768 A CN A2008101008768A CN 200810100876 A CN200810100876 A CN 200810100876A CN 101235590 A CN101235590 A CN 101235590A
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Abstract
The invention relates to the technical field of macromolecule fiber surface modification and in particular provides a method for modifying the ultrasonic chemical surface of PBO fiber. The method of the invention is characterized in that the method comprises: dipping the PBO fiber into chemical solution which is well arranged and evenly dispersed, vibrating for 1-10min with ultrasonic wave under the condition that the ultrasonic power is 30-100W, the ultrasonic frequency is 20-60 kHz, and the water bath temperature is 20-60DEG C, taking out the PBO fiber after modification, using deionized water or distilled water to wash repeatedly, taking out the PBO fiber which is modified after washing, and drying in 50-150DEG C, wherein chemical solution is at least one of mixed solution of polyphosphoric acid and anhydrous alcohol, polyphosphoric acid, methanesulfonic acid, nitric acid, formic acid and silane coupling agent. The investment cost for equipment which is used in the invention is low, the operation is convenient, the technical process is short, the modifying process is stable, the modified effect of the PBO fiber surface is increased, the fiber property loss is small, and the quality is reliable.
Description
Technical field
The invention belongs to macromolecular fibre process for modifying surface field, a kind of PBO (being polyparaphenylene's benzo-dioxazole) particularly is provided the ultrasonic chemistry surface modifying method of fiber.
Background technology
Polyparaphenylene's benzo-dioxazole (PBO) fiber is the very-high performance macromolecular fibre that people such as early 1980s Wolfe develop, general diameter is about 12 μ m, have the specific strength higher than aramid fiber, specific modulus and a series of excellent properties such as high temperature resistant, its density is about 1.57g/cm
3, tensile strength reaches 5.8GPa, and stretch modulus reaches 280GPa, and heat resisting temperature reaches 650 ℃.As enhancing body of advanced composite material of new generation etc., pbo fiber is at national economy, Aero-Space and the defence and military every field [Jin Junhong that is with a wide range of applications, Luo Kaiqing, Jiang Jianming, Deng. ionic group is to the influence of the surface property and the interfacial bond property thereof of pbo fiber. the composite journal, 2006,23 (6): 69-74].But, the pbo fiber smooth surface, polarity is little and active low, be difficult for and metal, combination such as inorganic particle or resin matrix, cause and be that matrix prepares that metallic cover pbo fiber or inorganic particle coat pbo fiber with the pbo fiber and be that wild phase is when preparing the fiber reinforcing texture composite with the pbo fiber, the interfacial combined function that usually occurs between fiber and the other materials is poor, interface shear strength is low, problems such as the transmission poor-performing of power, thereby influence the performance of composite material combination property, restricted pbo fiber further applying in advanced field of compound material.Therefore, modification being carried out on the pbo fiber surface, to improve the cementitiousness of pbo fiber and other materials, is bottleneck problem of being badly in need of solution during pbo fiber is used.
It is more at present the method for modification to be carried out on the pbo fiber surface, mainly comprises chemical method, plasma processing method, surperficial high-energy radiation method, modification by copolymerization method and coupling agent treatment method etc.These methods are all at the surface property that has improved pbo fiber in varying degrees, but exist the fiber surface degree of treatment and be difficult to control, surface modification is inhomogeneous, and modification time is long, and is problems such as cost with the mechanical property or the hot property of losing pbo fiber mostly.Therefore, the new pbo fiber surface modifying method of exploitation has crucial meaning.
As everyone knows, ultrasonic wave energy produces cavitation, and generation speed is about 110ms
-1Microjet, make fluid be in higher-order of oscillation state [L H Thomopson simultaneously, L K Doraiswamy.Sonochemistry:science and engineering.Industrial and Engineering Chemistry Research, 1999,38 (4): 1215-1249].Discover, ultrasonic technology is introduced in the surface modification of material, can improve the surface modification quality of material, shorten modification time, reduce consuming simultaneously, reduce environmental pollution.Therefore, ultrasonic technology is introduced, combined, will help to solve the deficiency that exists in the present pbo fiber surface modification with existing P BO fiber surface modification technology.The research that relevant ultrasonic technology is used in the pbo fiber surface modification has not yet to see open report.
Summary of the invention
The object of the present invention is to provide a kind of ultrasonic chemistry surface modifying method of pbo fiber, the cavitation of utilizing ultrasonic wave to have, with under laboratory condition and commercial production conditions, all be easy to realize, and operate the simplest, the chemical method that production cost is minimum combines, pbo fiber is carried out surface modification, so that the modification degree that exists when solving traditional chemical method modification pbo fiber surface is restive, modification evenness is poor, the fibre property damage is serious and modification time is longer, problems such as production cost height, overcome existing P BO fiber surface because of smooth and active low and metal, the defective of the interfacial combined function difference of inorganic particle or resin etc., the interface performance that pbo fiber is combined with other materials is improved.
The ultrasonic chemistry surface modifying technology of pbo fiber of the present invention is as follows:
1, pbo fiber is dipped in polyphosphoric acids absolute ethyl alcohol mixed solution or polyphosphoric acids or pyrovinic acid or nitric acid or formic acid or the silane coupler chemical solution, under the condition of 20～60 ℃ of ultrasonic power 30～100W, ultrasonic frequency 20～60kHz, bath temperatures, sonic oscillation 1～10min;
2, the pbo fiber after the above-mentioned modification of taking-up cleans repeatedly with deionized water or distilled water;
3, the modification pbo fiber after the above-mentioned cleaning is taken out, in 50～150 ℃ of oven dry.
The concentration of polyphosphoric acids of the present invention is 80～99.9wt%, the concentration of absolute ethyl alcohol is 93～99.99wt%, and the concentration of pyrovinic acid is 70～100wt%, and the concentration of nitric acid is 45～90wt%, the concentration of formic acid is 85～99wt%, and the concentration of silane coupler is 90～99wt%.
Require for polyphosphoric acids absolute ethyl alcohol mixed solution: the volume ratio of polyphosphoric acids and absolute ethyl alcohol is 0.5～1.5: 1, the polyphosphoric acids absolute ethyl alcohol mixed solution that configures is put into ultrasonic equipment, under the condition of ultrasonic power 30～100W, ultrasonic frequency 20～60kHz, carry out ultrasonic dispersion 5～120min, prepare homodisperse chemical solution.
The invention has the advantages that pbo fiber surface modification device therefor investment cost is low, easy and simple to handle, technological process is short, modifying process is stable, and has improved the pbo fiber surface modification effect, and the fibre property loss is little, reliable in quality, go back energy savings simultaneously, shorten modification time in a large number, reduce chemicals usage and product cost, reduce environmental pollution, be applicable to suitability for industrialized production.
The specific embodiment
Embodiment 1:
With 80wt% polyphosphoric acids and 99.7wt% absolute ethyl alcohol is that the polyphosphoric acids absolute ethyl alcohol mixed solution that configures at 1: 1 is put into ultrasonic equipment by volume, under the condition of ultrasonic power 30W, ultrasonic frequency 45kHz, carry out ultrasonic dispersion 5min, prepare homodisperse mixed solution.
Pbo fiber is dipped in the above-mentioned scattered polyphosphoric acids absolute ethyl alcohol mixed solution, under the condition of 50 ℃ of ultrasonic power 60W, ultrasonic frequency 50kHz, bath temperatures, continues sonic oscillation 3min;
Take out the pbo fiber after the above-mentioned modification, clean repeatedly with deionized water.
Modification pbo fiber after the above-mentioned cleaning is taken out,, promptly obtain the pbo fiber after the surface modification in 60 ℃ of oven dry.
Embodiment 2:
Pbo fiber is dipped in the 98wt% pyrovinic acid solution, under the condition of 60 ℃ of ultrasonic power 70W, ultrasonic frequency 60kHz, bath temperatures, sonic oscillation 1min;
Take out the pbo fiber after the above-mentioned modification, clean repeatedly with distilled water.
Modification pbo fiber after the above-mentioned cleaning is taken out,, promptly obtain the pbo fiber after the surface modification in 70 ℃ of oven dry.
Embodiment 3:
Pbo fiber is dipped in the 80wt% poly phosphoric acid solution, under the condition of 40 ℃ of ultrasonic power 100W, ultrasonic frequency 20kHz, bath temperatures, sonic oscillation 1min;
Take out the pbo fiber after the above-mentioned modification, clean repeatedly with deionized water.
Modification pbo fiber after the above-mentioned cleaning is taken out,, promptly obtain the pbo fiber after the surface modification in 80 ℃ of oven dry.
Claims (3)
1. the ultrasonic chemistry surface modifying method of a pbo fiber is characterized in that:
(1) pbo fiber is dipped in polyphosphoric acids absolute ethyl alcohol mixed solution or polyphosphoric acids or pyrovinic acid or nitric acid or formic acid or the silane coupler chemical solution, under the condition of 20～60 ℃ of ultrasonic power 30～100W, ultrasonic frequency 20～60kHz, bath temperatures, sonic oscillation 1～10min;
(2) pbo fiber after the taking-up modification cleans repeatedly with deionized water or distilled water;
(3) the modification pbo fiber after the above-mentioned cleaning is taken out, in 50～150 ℃ of oven dry.
2. the ultrasonic chemistry surface modifying method of pbo fiber as claimed in claim 1, it is characterized in that for the requirement of polyphosphoric acids absolute ethyl alcohol mixed solution: the volume ratio of polyphosphoric acids and absolute ethyl alcohol is 0.5～1.5: 1; The concentration of polyphosphoric acids is 80～99.9wt%, and the concentration of absolute ethyl alcohol is 93～99.99wt%; The polyphosphoric acids absolute ethyl alcohol mixed solution that configures is put into ultrasonic equipment, under the condition of ultrasonic power 30～100W, ultrasonic frequency 20～60kHz, carry out ultrasonic dispersion 5～120min, prepare homodisperse chemical solution.
3. the ultrasonic chemistry surface modifying method of pbo fiber as claimed in claim 1, the concentration that it is characterized in that pyrovinic acid is 70～100wt%, the concentration of nitric acid is 45～90wt%, and the concentration of formic acid is 85～99wt%, and the concentration of silane coupler is 90～99wt%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101008768A CN101235590B (en) | 2008-02-25 | 2008-02-25 | Ultrasonic chemistry surface modifying method for PBO fiber |
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| CN2008101008768A CN101235590B (en) | 2008-02-25 | 2008-02-25 | Ultrasonic chemistry surface modifying method for PBO fiber |
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| CN101235590A true CN101235590A (en) | 2008-08-06 |
| CN101235590B CN101235590B (en) | 2011-08-24 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101770947B (en) * | 2008-12-30 | 2011-10-05 | 中芯国际集成电路制造(上海)有限公司 | Poly(p-phenylene benzobisoxazole) fiber surface-processing method |
| CN102675825A (en) * | 2011-12-03 | 2012-09-19 | 西北工业大学 | High-performance wave-transmitting composite material based on PBO (poly-p-phenylene benzobisthiazole) fiber and preparation method thereof |
| CN102808325A (en) * | 2012-07-10 | 2012-12-05 | 西北工业大学 | Surface modifying method of PBO (polybenzoxazole) fiber |
| CN102863634A (en) * | 2012-10-12 | 2013-01-09 | 西北工业大学 | Process for preparing poly-p-phenylenebenzobisthiazole (PBO) fiber/benzoxazine composite material |
| CN103321037A (en) * | 2013-06-07 | 2013-09-25 | 南通和泰通讯器材有限公司 | Aramid fiber surface treatment process |
| WO2014011278A2 (en) | 2012-04-11 | 2014-01-16 | Battelle Memorial Institute | Pbo fibers with improved mechanical properties when exposed to high temperatures and high relative humidity |
| CN107620204A (en) * | 2017-11-09 | 2018-01-23 | 成都新晨新材科技有限公司 | A kind of pbo fiber of ultraviolet resistance and preparation method thereof |
| CN108790316A (en) * | 2018-04-16 | 2018-11-13 | 杭州协业超纤有限公司 | A kind of Compound Fabric and preparation method thereof of Tan Xier fibers and cotton gauze |
| CN110272587A (en) * | 2019-06-17 | 2019-09-24 | 中国人民解放军陆军特种作战学院 | A kind of cold-resistant High-temperature-resflamet flamet retardant composite material and preparation method thereof |
| CN115354521A (en) * | 2022-08-16 | 2022-11-18 | 西安工程大学 | Processing method of PBO fiber wet-process non-woven material |
-
2008
- 2008-02-25 CN CN2008101008768A patent/CN101235590B/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101770947B (en) * | 2008-12-30 | 2011-10-05 | 中芯国际集成电路制造(上海)有限公司 | Poly(p-phenylene benzobisoxazole) fiber surface-processing method |
| CN102675825A (en) * | 2011-12-03 | 2012-09-19 | 西北工业大学 | High-performance wave-transmitting composite material based on PBO (poly-p-phenylene benzobisthiazole) fiber and preparation method thereof |
| US9279214B2 (en) | 2012-04-11 | 2016-03-08 | Battelle Memorial Institute | PBO fibers with improved mechanical properties when exposed to high temperatures and high relative humidity |
| WO2014011278A2 (en) | 2012-04-11 | 2014-01-16 | Battelle Memorial Institute | Pbo fibers with improved mechanical properties when exposed to high temperatures and high relative humidity |
| WO2014011278A3 (en) * | 2012-04-11 | 2014-06-26 | Battelle Memorial Institute | Pbo fibers with improved mechanical properties when exposed to high temperatures and high relative humidity |
| CN102808325A (en) * | 2012-07-10 | 2012-12-05 | 西北工业大学 | Surface modifying method of PBO (polybenzoxazole) fiber |
| CN102808325B (en) * | 2012-07-10 | 2014-06-11 | 西北工业大学 | Surface modifying method of PBO (polybenzoxazole) fiber |
| CN102863634A (en) * | 2012-10-12 | 2013-01-09 | 西北工业大学 | Process for preparing poly-p-phenylenebenzobisthiazole (PBO) fiber/benzoxazine composite material |
| CN102863634B (en) * | 2012-10-12 | 2014-08-20 | 西北工业大学 | Process for preparing poly-p-phenylenebenzobisthiazole (PBO) fiber/benzoxazine composite material |
| CN103321037A (en) * | 2013-06-07 | 2013-09-25 | 南通和泰通讯器材有限公司 | Aramid fiber surface treatment process |
| CN107620204A (en) * | 2017-11-09 | 2018-01-23 | 成都新晨新材科技有限公司 | A kind of pbo fiber of ultraviolet resistance and preparation method thereof |
| CN108790316A (en) * | 2018-04-16 | 2018-11-13 | 杭州协业超纤有限公司 | A kind of Compound Fabric and preparation method thereof of Tan Xier fibers and cotton gauze |
| CN108790316B (en) * | 2018-04-16 | 2020-11-13 | 杭州协业超纤有限公司 | Composite cloth of tamsular fiber and all-cotton gauze and preparation method thereof |
| CN110272587A (en) * | 2019-06-17 | 2019-09-24 | 中国人民解放军陆军特种作战学院 | A kind of cold-resistant High-temperature-resflamet flamet retardant composite material and preparation method thereof |
| CN110272587B (en) * | 2019-06-17 | 2021-11-09 | 中国人民解放军陆军特种作战学院 | Cold-resistant high-temperature-resistant flame-retardant composite material and preparation method thereof |
| CN115354521A (en) * | 2022-08-16 | 2022-11-18 | 西安工程大学 | Processing method of PBO fiber wet-process non-woven material |
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| CN101235590B (en) | 2011-08-24 |
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