CN103361768A - Surface modification method of polyacrylonitrile-based carbon fiber - Google Patents
Surface modification method of polyacrylonitrile-based carbon fiber Download PDFInfo
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Abstract
The invention relates to a surface modification method of polyacrylonitrile-based carbon fiber. The surface modification method comprises the following steps of: performing plasma treatment on the polyacrylonitrile-based carbon fiber in an inert gas atmosphere; and further performing atomization treatment on the carbon fiber after plasma treatment through a grafting solution. The method disclosed by the invention has the advantages that as for the carbon fiber after the treatment according to the invention, the surface energy is increased, the wettability is improved, the treatment uniformity is good, the mechanical properties are less damaged, and the interlaminar shear strength value of a carbon fiber composite material is improved. The method disclosed by the invention has the advantages of simplicity and convenience in operation and control, simple process steps and online continuous treatment.
Description
Technical field
The present invention relates to the preparation method of polyacrylonitrile-based carbon fibre, specifically, relate to a kind of polyacrylonitrile-based carbon fibre surface modifying method.
Background technology
Carbon fiber is that phosphorus content is at the inorganic polymer fiber more than 90%, utilize the carbonization and making under inert gas medium and high temperature state of various organic fibers, it has the soft machinability that the intrinsic intrinsic property of carbon graphite material has both again textile fabric, is fortifying fibre of new generation.Carbon fiber not only has a series of excellent properties such as high specific strength and specific modulus, high conductivity, low thermal coefficient of expansion, high temperature resistant, anticorrosive, creep resistant, is widely used in the various fields such as the leading-edge fields such as Aero-Space, national defense and military and communications and transportation, civil construction, senior sports goods, medical supplies.
Polyacrylonitrile carbon fiber is the main method of producing carbon fiber, and the manufacturing of polyacrylonitrile carbon fiber comprises the multiple working procedures such as polymerization, spinning, pre-oxidation, carbonization, surface treatment and starching, thereby the production of carbon fiber is the integrated of multidisciplinary, many technology.
Surface treatment procedure is important in the production of a carbon fiber link.Because carbon fiber surface is inertia, specific area is little, surface energy is low, and the wettability between the resin and interfacial bond property are poor, thereby have influence on the performance of whole composite.In order to improve the cohesiveness of carbon fiber and resin matrix, improve the shearing strength between layers of composite, must process its surface.Purpose is polar group such as the functional groups such as carboxyl, carbonyl that increase carbon fiber surface, increases surface area, improves the wettability with resin matrix.In recent years, adopted several different methods that carbon fiber is carried out surface modification, having comprised: the methods such as gaseous oxidation, liquid phase oxidation, electrochemistry anodic oxidation, coupling agent treatment, chemical graft, low temperature plasma.
Chinese patent CN1032042A discloses a kind of vapour phase oxidation process of carbon fiber surface modification, be that the ozone of 0.5～15mg/L imports continuously the surface treatment of carbon fibers stove carbon fiber is carried out surface treatment with concentration namely, the interlaminar shear strength of carbon fibre composite increases after treatment, but this method is larger to the damage of tensile strength of fiber, in addition along with the difference of fiber, the difference for the treatment of temperature, the gaseous oxidation result also is not quite similar.
US Patent No. P3723607 discloses the processing method of ozone oxidation carbon fiber surface, this method be with air or oxygen after cyclone separator, filter, drier etc. carry out strict dry decontamination dedusting, electrion environment by ozone generator produces ozone, so that carbon fiber is processed in ozone environment.Effect can but complex process.
US Patent No. P3J13094 discloses a kind of liquid phase oxidation of carbon fiber surface modification, but the technique of its description is comparatively complicated, and the processing time is long, can not be complementary with carbon fiber production line, and is usually multiplex in laboratory research.
The people such as Liu Hongpeng are at article " novel charcoal material " 2005,20 (1), report in 39～43, take NH4HCO3 as electrolyte carbon fiber being carried out continuous surface processes, found that, after electrochemical surface is processed, carbon fiber surface becomes lyophily by lyophobicity, be conducive to improve the interlaminar shear strength of carbon fiber enhancement resin base composite material (CFRP), though electrochemistry anodic oxidation has industrial utility value, the carbon fiber after electrolytic anodization is processed must be first through hot water washing step flush away electrolyte, drying operation more then could starching.This method relates to the problems such as wastewater treatment and energy consumption, and more numerous and diverse on the technique.
Summary of the invention
The object of the invention is to, a kind of method of polyacrylonitrile-based carbon fibre surface modification is provided, can't meet the demands simultaneously with interlaminar shear strength and the tensile strength of fiber that solves the rear carbon fibre composite of existing method processing, and the numerous and diverse technical problem of technique.
Technical scheme of the present invention is as follows:
A kind of method of polyacrylonitrile-based carbon fibre surface modification comprises the steps: in atmosphere of inert gases polyacrylonitrile-based carbon fibre to be carried out Cement Composite Treated by Plasma; Carbon fiber after plasma is processed is again by the grafting liquid processing that atomizes.
Carbon fiber after atomizing is processed is through starching, oven dry and receive silk, makes the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51.
Described polyacrylonitrile-based carbon fibre list synnema is 1000～3000, and the tow number of share of stock is 50～100 strands, and wire travelling speed is 3～5m/min.
Before described polyacrylonitrile-based carbon fibre carries out Cement Composite Treated by Plasma, carry out the high temperature cabonization below 1500 ℃.
Described inert gas is selected from least a in argon gas, helium, the nitrogen.
What described Cement Composite Treated by Plasma adopted is the dielectric barrier discharge plasma generating means, evenly distributes by form plasma in the dielectric barrier discharge plasma generating means, and its discharge power is 1000W～6000W.
Described grafting liquid is selected from least a in maleic anhydride, methyl acrylate, methyl methacrylate, acrylamide, methacrylic acid, the acrylic acid.
The solvent of described grafting liquid is deionized water, and the mass percent concentration of this grafting liquid is 1%～10%.
Utilize measuring pump to extract out from the solution storage tank grafting liquid, the measuring pump outlet conduit mixes with the purification of compressed air pipeline, in a kind of atomization processing device, via atomizer, vertically sprays to from top to bottom operating carbon fiber.
At 0.05～0.3L/min, the pressure of purification of compressed air is at 0.4～0.6MPa for amount for the pump of described grafting liquid.
The invention provides a kind of method of polyacrylonitrile-based carbon fibre surface modification, the advantage of this method is: through the carbon fiber of the present invention's processing, its surface energy increases, wettability is improved, and the good uniformity of processing, the mechanical property damage is little, and the interlaminar shear strength value of carbon fibre composite is improved.The present invention operates and controls easy, and operation is simple, but the on-line continuous processing belongs to an environment-friendly production technology.
Description of drawings
Fig. 1 is the schematic diagram of dielectric barrier discharge device embodiment of the present invention;
Fig. 2 is the schematic diagram of the embodiment of the method for polyacrylonitrile-based carbon fibre surface modification of the present invention.
The specific embodiment
Further describe concrete technical scheme of the present invention below in conjunction with drawings and Examples, so that those skilled in the art understands the present invention, and do not consist of its Copyright law.
The method of polyacrylonitrile-based carbon fibre surface modification of the present invention comprises the steps: in atmosphere of inert gases polyacrylonitrile-based carbon fibre to be carried out Cement Composite Treated by Plasma; Carbon fiber after plasma is processed is again by the grafting liquid processing that atomizes.In the material surface modifying field, grafting liquid is the common technology term of specialty, the various solution that exemplify, and general character is all to have hydrophilic radical, in case be grafted on fiber surface, this improves fiber surface polarity.Whole processing procedure of the present invention as shown in Figure 2, what wherein Cement Composite Treated by Plasma adopted is dielectric barrier discharge device shown in Figure 1.As shown in Figure 1, described dielectric barrier discharge plasma generating means is all kinds of plasma generators with block media, and it utilizes the high voltage of certain frequency to start, and medium covers on the electrode.Plasma atmosphere is produced by the dielectric barrier discharge plasma generator, and plasma evenly distributes in dielectric barrier discharge plasma generator cavity, and its discharge power is 1000W～6000W, inert atmosphere be argon gas, helium, nitrogen one or more.Measuring pump among Fig. 2 is extracted grafting liquid out from the grafting liquid storage tank, pump when flow increases, suitably improves compressed-air actuated pressure for measuring the very flow of grafting liquid, to guarantee atomizing effect.Pump is larger for amount, and the emitted dose of nozzle is larger.Described atomizing processing mode is: utilize measuring pump to extract out from the solution storage tank grafting liquid, the measuring pump outlet conduit mixes with the purification of compressed air pipeline, in a kind of atomization processing device, via atomizer, vertically spray to from top to bottom operating carbon fiber.In the described atomizing processing mode, at 0.05～0.3L/min, the pressure of purification of compressed air is at 0.4～0.6MPa for amount for the pump of grafting liquid.
Comparative example 1
The wire travelling speed of 50 strands of 1K carbon fibers of control is 3m/min, after high temperature cabonization is processed, without any surface modification treatment, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 1
The wire travelling speed of 50 strands of 1K carbon fibers of control is 3m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 1500W, and then the carbon fiber after plasma is processed carries out the atomizing of maleic anhydride solution again to be processed, maleic anhydride solution quality percent concentration 2%, pump is for amount 0.05L/min, the pressure 0.4Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 2
The wire travelling speed of 50 strands of 1K carbon fibers of control is 3.5m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 3000W, and then the carbon fiber after plasma is processed carries out the atomizing of maleic anhydride solution again to be processed, maleic anhydride solution quality percent concentration 2.5%, pump is for amount 0.1L/min, the pressure 0.5Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 3
The wire travelling speed of 50 strands of 1K carbon fibers of control is 3.5m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 3000W, and then the carbon fiber after plasma is processed carries out the atomizing of methyl acrylate and acrylamide mixed solution again to be processed, this mixed solution mass percent concentration 2.5%, methyl acrylate: acrylamide=1: 1 (mol ratio), pump is for amount 0.1L/min, the pressure 0.5Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 4
The wire travelling speed of 50 strands of 1K carbon fibers of control is 3.5m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 3000W, and then the carbon fiber after plasma is processed carries out the atomizing of methyl methacrylate and acrylamide mixed solution again to be processed, this mixed solution mass percent concentration 3%, methyl methacrylate: acrylamide=1: 1 (mol ratio), pump is for amount 0.1L/min, the pressure 0.5Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 5
The wire travelling speed of 50 strands of 1K carbon fibers of control is 3.5m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 3000W, and then the carbon fiber after plasma is processed carries out the atomizing of methacrylic acid solution again to be processed, methacrylic acid solution mass percent concentration 3%, pump is for amount 0.1L/min, the pressure 0.5Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 6
The wire travelling speed of 50 strands of 3K carbon fibers of control is 3.5m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 4000W, and then the carbon fiber after plasma is processed carries out the atomizing of acrylic acid solution again to be processed, acrylic acid solution mass percent concentration 2.5%, pump is for amount 0.1L/min, the pressure 0.5Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 7
The wire travelling speed of 100 strands of 3K carbon fibers of control is 4.5m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 5000W, and then the carbon fiber after plasma is processed carries out the atomizing of acrylic acid solution again to be processed, acrylic acid solution mass percent concentration 3.5%, pump is for amount 0.2L/min, the pressure 0.5Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
Embodiment 8
The wire travelling speed of 100 strands of 3K carbon fibers of control is 5m/min, utilizes the dielectric barrier discharge plasma generating means, and at atmospheric pressure, the carbon fiber to the high temperature cabonization outlet of still under the argon gas carries out Cement Composite Treated by Plasma.Dielectric barrier discharge plasma generating means discharge power is 6000W, and then the carbon fiber after plasma is processed carries out the atomizing of acrylic acid solution again to be processed, acrylic acid solution mass percent concentration 3.5%, pump is for amount 0.3L/min, the pressure 0.6Mpa of purification of compressed air.After the polyacrylonitrile-based carbon fibre surface modification is finished, directly send into starching, oven dry and receive wire process, make the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51, measure its interlaminar shear strength value.
The strand specification of carbon fiber is larger, and the expression tow is more, so pump increases for amount, the mass percent concentration of grafting liquid improves, and discharge power needs to increase night, guarantees the surface treatment effect of tow with this, in like manner, when wire travelling speed increases, also need to improve discharge power.
Comparative example and embodiment, the performance test results of acquisition is as shown in table 1:
Table 1
The method of polyacrylonitrile-based carbon fibre surface modification of the present invention operates and controls easy, and operation is simple, but on-line continuous is processed.The modification of plasma only limits to the material list surface layer, does not affect the matrix proper property.The ozone treatment carbon fiber, larger to the strength damage of carbon fiber, treatment effect of the present invention is so that the combination property of final carbon fibre composite is better than the processing method of ozone oxidation carbon fiber surface.Simultaneously, treatment effect of the present invention can reach the effect of electrochemistry anodic oxidation, and advantage just is that technique is simple, does not relate to wastewater treatment and high energy consumption problem.
Above-described embodiment only is explanation technological thought of the present invention and characteristics; its purpose is to make those skilled in the art can understand content of the present invention and implements according to this; can not limit according to this protection scope of the present invention; the equalization of namely being done with disclosed spirit changes or derives, and must be encompassed in protection scope of the present invention.
Claims (10)
1. the method for a polyacrylonitrile-based carbon fibre surface modification comprises the steps:
In atmosphere of inert gases, polyacrylonitrile-based carbon fibre is carried out Cement Composite Treated by Plasma;
Carbon fiber after plasma is processed is again by the grafting liquid processing that atomizes.
2. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 1 is characterized in that, the carbon fiber after atomizing is processed is through starching, oven dry and receive silk, makes the finished product carbon fiber, and with the compound carbon fibre composite of making of resin matrix epoxy E-51.
3. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 1 is characterized in that, described polyacrylonitrile-based carbon fibre list synnema is 1000～3000, and the tow number of share of stock is 50～100 strands, and wire travelling speed is 3～5m/min.
4. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 1 is characterized in that, before described polyacrylonitrile-based carbon fibre carries out Cement Composite Treated by Plasma, carries out the high temperature cabonization below 1500 ℃.
5. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 1 is characterized in that, described inert gas is selected from least a in argon gas, helium, the nitrogen.
6. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 1, it is characterized in that, what described Cement Composite Treated by Plasma adopted is the dielectric barrier discharge plasma generating means, evenly distribute by form plasma in the dielectric barrier discharge plasma generating means, its discharge power is 1000W～6000W.
7. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 1, it is characterized in that, described grafting liquid is selected from least a in maleic anhydride, acrylic acid, methyl acrylate, acrylamide, methacrylic acid, methyl methacrylate, the hydroxy acrylic acid.
8. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 7 is characterized in that, the solvent of described grafting liquid is deionized water, and the mass percent concentration of this grafting liquid is 1%～10%.
9. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 8, it is characterized in that, utilize measuring pump from the solution storage tank, to extract out grafting liquid, the measuring pump outlet conduit mixes with the purification of compressed air pipeline, in a kind of atomization processing device, via atomizer, vertically spray to from top to bottom operating carbon fiber.
10. the method for polyacrylonitrile-based carbon fibre surface modification as claimed in claim 9 is characterized in that, at 0.05～0.3L/min, the pressure of purification of compressed air is at 0.4～0.6MPa for amount for the pump of described grafting liquid.
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| CN103696228A (en) * | 2013-12-19 | 2014-04-02 | 余姚市汇航特种塑料科技有限公司 | Surfaced treatment method for carbon fiber |
| CN105332098A (en) * | 2015-11-25 | 2016-02-17 | 安徽佳力奇航天碳纤维有限公司 | Carbon fiber activation process |
| CN106061089A (en) * | 2016-06-21 | 2016-10-26 | 南京林业大学 | Method for strengthening bonding performance of crop straws employing formaldehyde dielectric barrier discharge plasma |
| CN106654163A (en) * | 2016-12-29 | 2017-05-10 | 中国电子科技集团公司第十八研究所 | Preparation method of cathode of seawater dissolved oxygen battery |
| CN106811966A (en) * | 2017-01-24 | 2017-06-09 | 哈尔滨工业大学 | A kind of method of acrylic amide aqueous solution grafting modified carbon fiber surface size agent |
| CN106835695A (en) * | 2017-01-24 | 2017-06-13 | 哈尔滨工业大学 | A kind of method of acrylic amide organic solution grafting modified carbon fiber surface size agent |
| CN107002347A (en) * | 2014-12-09 | 2017-08-01 | 国立大学法人东京大学 | Surface processed carbon fiber, surface processed carbon fiber beam and their manufacture method |
| CN110761067A (en) * | 2019-10-30 | 2020-02-07 | 中国人民解放军空军工程大学 | Carbon fiber surface continuous treatment method and device based on normal-pressure DBD discharge |
| CN113338027A (en) * | 2021-05-12 | 2021-09-03 | 北京化工大学 | Surface treatment method of carbon fiber |
| CN114427168A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Continuous treatment method for improving surface performance of carbon fiber |
| CN114892393A (en) * | 2022-06-29 | 2022-08-12 | 北京化工大学 | Carbon fiber device based on MXene phase modification |
| CN114892400A (en) * | 2021-11-01 | 2022-08-12 | 中国电力科学研究院有限公司 | Material surface treatment device and method |
| CN114960175A (en) * | 2022-05-16 | 2022-08-30 | 中国人民解放军空军工程大学 | Multi-fiber-bundle high-efficiency plasma surface modification device and method |
| CN114960176A (en) * | 2022-05-25 | 2022-08-30 | 中国人民解放军空军工程大学 | High-degree plasma surface modification device and method for large fiber tows |
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| CN107002347A (en) * | 2014-12-09 | 2017-08-01 | 国立大学法人东京大学 | Surface processed carbon fiber, surface processed carbon fiber beam and their manufacture method |
| CN105332098A (en) * | 2015-11-25 | 2016-02-17 | 安徽佳力奇航天碳纤维有限公司 | Carbon fiber activation process |
| CN106061089A (en) * | 2016-06-21 | 2016-10-26 | 南京林业大学 | Method for strengthening bonding performance of crop straws employing formaldehyde dielectric barrier discharge plasma |
| CN106654163A (en) * | 2016-12-29 | 2017-05-10 | 中国电子科技集团公司第十八研究所 | Preparation method of cathode of seawater dissolved oxygen battery |
| CN106811966A (en) * | 2017-01-24 | 2017-06-09 | 哈尔滨工业大学 | A kind of method of acrylic amide aqueous solution grafting modified carbon fiber surface size agent |
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| CN114427168A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Continuous treatment method for improving surface performance of carbon fiber |
| CN113338027A (en) * | 2021-05-12 | 2021-09-03 | 北京化工大学 | Surface treatment method of carbon fiber |
| CN114892400A (en) * | 2021-11-01 | 2022-08-12 | 中国电力科学研究院有限公司 | Material surface treatment device and method |
| CN114892400B (en) * | 2021-11-01 | 2023-12-26 | 中国电力科学研究院有限公司 | Material surface treatment device and method |
| CN114960175A (en) * | 2022-05-16 | 2022-08-30 | 中国人民解放军空军工程大学 | Multi-fiber-bundle high-efficiency plasma surface modification device and method |
| CN114960175B (en) * | 2022-05-16 | 2023-05-12 | 中国人民解放军空军工程大学 | Multi-fiber-bundle high-efficiency plasma surface modification device and method |
| CN114960176A (en) * | 2022-05-25 | 2022-08-30 | 中国人民解放军空军工程大学 | High-degree plasma surface modification device and method for large fiber tows |
| CN114960176B (en) * | 2022-05-25 | 2023-05-16 | 中国人民解放军空军工程大学 | High-degree plasma surface modification device and method for large fiber tows |
| CN114892393A (en) * | 2022-06-29 | 2022-08-12 | 北京化工大学 | Carbon fiber device based on MXene phase modification |
| CN114892393B (en) * | 2022-06-29 | 2023-01-20 | 北京化工大学 | Carbon fiber device based on MXene phase modification |
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