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CN115648664A - Carbon fiber widening and shaping composite processing method - Google Patents

Carbon fiber widening and shaping composite processing method
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CN115648664A
CN115648664ACN202211311976.1ACN202211311976ACN115648664ACN 115648664 ACN115648664 ACN 115648664ACN 202211311976 ACN202211311976 ACN 202211311976ACN 115648664 ACN115648664 ACN 115648664A
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widening
hot
carbon fiber
shaping
fiber
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CN115648664B (en
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曹伟伟
乔琨
张敏
王永伟
孙永连
林治涛
朱波
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Shandong Guangyuan New Material Technology Co ltd
Shandong University
Tiangong University
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Shandong Guangyuan New Material Technology Co ltd
Tianjin Polytechnic University
Shandong University
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Abstract

The invention relates to a carbon fiber widening and shaping composite processing mode which comprises a carbon fiber widening and widening shaping method and a base film composite processing method. Firstly, carrying out double-roller heating extrusion treatment on continuous long-tow carbon fibers under the action of constant tension to realize widening, carrying out hot-pressing infiltration setting at certain intervals by adopting a transverse hot-melt wire after widening is finished, finally coating a setting thermoplastic sizing agent with certain concentration on the widened fiber tows after hot-melt fiber setting, finishing the setting composite treatment of the widened carbon fibers, and effectively improving the widening setting of the continuous carbon fiber filaments.

Description

Carbon fiber widening and shaping composite processing method
Technical Field
The invention belongs to the field of carbon fiber preparation, and particularly relates to a carbon fiber stretching and shaping composite treatment method.
Background
The information disclosed in this background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
The flowability of the thermoplastic resin and the carbon fiber reinforcement during compounding is poor, so that the problems of poor infiltration effect of a resin matrix at a fiber monofilament interface in an infiltration process, unstable interface bonding effect and the like exist, the performance of the interface performance of the composite material is seriously influenced, and the stability of the macroscopic mechanical property is further influenced. In order to improve the hot-melt composite effect of a thermoplastic resin matrix, researchers perform expanding treatment on carbon fibers, perform expanding treatment on conventional continuous filament bundle carbon fibers in the width direction, and expand the monofilament carbon fibers in the filament bundle in the width direction in the treatment mode so that the monofilament fibers are arranged in parallel. Traditional carbon fiber widening and shaping are compounded, the widening and widening of monofilament fibers are generally completed through heating extrusion of a continuous traditional roller or matching ultrasonic oscillation under the action of axial tension, the widening treatment needs to be completed under the action of constant axial tension, and in order to guarantee the fiber widening and widening effect, specific coating treatment needs to be carried out on the surfaces of continuous fibers before processing so as to guarantee the arrangement stability of fiber widening monofilaments. When the tension is removed after the fiber is widened, the continuous monofilaments inevitably slip and shrink to cause instability of monofilament arrangement, and sometimes even the widening effect is influenced.
Disclosure of Invention
Aiming at the technical problem, the invention provides a sizing and compounding method for widening treatment of carbon fibers, which adopts a comprehensive treatment mode of transverse hot-melt sizing and sizing film-forming sizing after the fiber filament bundle is widened, effectively improves the widening and sizing of continuous carbon fiber filaments and provides a good fiber arrangement aggregate for the subsequent compounding processing of thermoplastic resin matrix composite materials.
In order to achieve the above object, the present invention provides the following technical solutions.
A carbon fiber widening and shaping composite processing method comprises the following steps: firstly, carrying out double-roller heating extrusion treatment on continuous long-tow carbon fibers under the action of constant tension, pasting hot-melt fiber filaments in the direction vertical to the fibers after widening for shaping, carrying out infiltration shaping treatment on the carbon fiber widening tows pasted with the hot-melt fiber filaments, and finally coating shaping sizing agent on the widening fiber tows after shaping the hot-melt fibers to finish the shaping composite treatment of the widening carbon fibers.
The continuous carbon fiber tows used for widening the carbon fibers can be any one of T300, T700, T800, T1000, M40, M55, M60 and the like, and the widened carbon fiber tows can be of any different specifications such as 3K, 6K, 12K, 24K and the like.
The stretching tension of the carbon fiber filament bundle is controlled to be 5-8N, the yarn stretching speed is controlled to be 1-8 m/min, the carbon fiber is heated within the range of 80-150 ℃ under constant tension, and the final yarn stretching width is 3-5 times of the original width of the carbon fiber filament bundle.
The hot-melt fiber filament is transversely pasted and applied along the axial length at a certain interval after the carbon fiber filament bundle is widened, the hot-melt fiber filament can be selected from polyethylene, polypropylene, polystyrene, polyphenylene sulfide, polyamide, polyimide, polyether ketone, polyether ether ketone, ethylene terephthalate, butylene terephthalate and the like, and is not limited to the types, and the type of the hot-melt fiber is matched with or similar to that of the final thermoplastic resin.
The hot melt fiber filament can be replaced by a strip-shaped hot melt adhesive film with a certain width, the type of the hot melt adhesive film is the same as that of the hot melt fiber filament, the hot melt fiber filament can be arranged by 1-10 fibers in parallel, the hot melt strip-shaped adhesive film with the thickness ranging from 0.05mm to 2mm can also be adopted, and the width of the strip-shaped hot melt adhesive film can be flexibly adjusted within the range of 2-5 mm.
The spacing distance of the hot-melt filament or the hot-melt strip-shaped adhesive film along the fiber axial direction is controlled to be 10-30cm for flexible adjustment, and the hot-melt filament or the hot-melt strip-shaped adhesive film can be subjected to hot-melt treatment by adopting various modes such as filament single-side arrangement, upper and lower surface alternative arrangement or multi-bundle spread fiber plain-weave alternative arrangement.
The hot melting treatment temperature of the hot melting fiber or the strip-shaped hot melting adhesive film is based on the infiltration composite temperature of a hot melting resin type, the hot melting temperature is controlled to be flexibly adjusted within the range of 120-300 ℃, and the hot melting setting time is flexibly adjusted within the range of 0.5-5 seconds. The hot melting pressure is controlled within the range of 0.5-3MPa. And ensuring synchronous application of stretching tension in the infiltration process.
After the spread fiber is subjected to transverse interval infiltration and shaping treatment of the hot-melt fiber, shaping sizing agent coating with certain concentration is carried out on the surface of one side or the surfaces of both sides, and finally, a shaping composite film coating is formed on the surface of the spread fiber through heating and drying.
The coating mode can be a spraying or dipping coating mode, one-side coating or double-side continuous coating mode treatment can be adopted, wherein the spraying pressure of spraying coating is controlled within the range of 0.5-2MPa, and the spraying thickness on the surface of the carbon fiber widening yarn is finally within the range of 0.02-0.1 mm.
The dipping coating can be carried out in a dipping sizing tank at a constant temperature of 40-60 ℃ by adopting an emulsion sizing agent with a certain concentration, the dipping coating effect can be improved by matching with ultrasonic equipment, and the adopted sizing agent for spraying or dipping coating can adopt a thermoplastic sizing emulsion with solid content of 5-20%.
The emulsion of sizing agent can be selected from polyethylene, polypropylene, polystyrene, polyphenylene sulfide, polyamide, polyimide, polyether ketone, polyether ether ketone, ethylene terephthalate, butylene terephthalate, etc. and is not limited to the above types of emulsion systems.
After sizing, shaping and coating, drying treatment is carried out at the temperature of 100-150 ℃, and the drying time is controlled within the range of 10-30min and flexibly adjusted according to the drying effect.
Compared with the prior art, the invention has the following effects:
(1) The comprehensive treatment mode of transverse hot melt setting and sizing film forming setting is adopted, so that the spreading setting of the continuous carbon fiber filaments is effectively improved, and the fiber filaments are well arranged.
(2) The thermoplastic sizing agent matched with or similar to the hot melt wire or the hot melt adhesive film is adopted and mutually matched, so that the fiber widening and shaping are facilitated, and the heating infiltration effect is effectively improved.
(3) The widening tension is synchronously applied in the infiltration process, so that the widening contraction of the carbon fiber filaments in the infiltration process is avoided.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a schematic structural diagram of single-side arrangement of hot-melt filaments in the carbon fiber widening and shaping composite treatment method of the invention.
Fig. 2 is a schematic structural view of the upper and lower surfaces of the banded hot-melt adhesive film alternately arranged in the carbon fiber widening and shaping composite processing method of the invention.
FIG. 3 is a schematic structural view of a multi-bundle spread fiber plain alternate arrangement of a hot-melt filament or a banded hot-melt adhesive film in a carbon fiber spreading and shaping composite treatment method of the present invention
Wherein, 1-carbon fiber filament, 2-hot melt filament and 3-hot melt adhesive film.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
As shown in fig. 1 to 3, under the action of a constant tension, T700 high-strength carbon fiber with 6K tow is used as carbon fiber stretched tow to carry out double-roll heating extrusion treatment, the stretching tension is 6N, the stretching rate is 3 m/min, and the heating temperature of the carbon fiber is 120 ℃. And after widening, pasting polyethylene fiber filaments in a direction vertical to the fibers for shaping, wherein the pasting filaments are arranged in parallel by adopting 5 fibers, the pasting mode is that the filaments are arranged on a single surface, and the pasting distance is 10cm. And (3) carrying out infiltration and shaping treatment on the carbon fiber spread tows coated with the polyethylene fiber filaments, wherein the hot melting temperature is set to be 190 ℃, the hot melting time is set to be 3 seconds, and the hot melting pressure is set to be 2MPa. And synchronously applying stretching tension in the infiltration process, wherein the final yarn stretching width is 3 times of the original width of the carbon fiber filament bundle.
After the spread fiber is subjected to transverse interval infiltration and shaping treatment of the hot-melt fiber, polyethylene emulsion with the solid content of 10% is sprayed on the surface of one side of the spread fiber, the spraying pressure of the spraying is set to be 1MPa, and the spraying thickness is 0.05mm. And after the sizing and coating of the thermoplastic sizing agent are finished, drying the thermoplastic sizing agent at 120 ℃, wherein the drying time is 20min.
Example 2
Under the action of constant tension, M55 high-modulus carbon fiber with a tow of 12K is used as a carbon fiber widening tow to carry out double-roller heating extrusion treatment, the widening tension is 5N, the widening rate is 4M/min, and the heating temperature of the carbon fiber is 130 ℃. And (3) after widening, adhering polyphenylene sulfide fiber filaments in a direction vertical to the fibers, wherein the adhering filaments are arranged in parallel by adopting 6 fibers, the upper surface and the lower surface of each filament are alternately arranged, and the adhering distance is 15cm. And carrying out infiltration and shaping treatment on the carbon fiber spread tows coated with the polyphenylene sulfide fiber filaments, wherein the hot melting temperature is set to be 260 ℃, the hot melting time is set to be 4 seconds, and the hot melting pressure is set to be 2.5MPa. And synchronously applying stretching tension in the infiltration process, wherein the final yarn stretching width is 4 times of the original width of the carbon fiber filament bundle.
After transverse interval infiltration and shaping treatment of the hot-melt fiber, the spread fiber is matched with ultrasonic equipment to be dipped and coated in a constant temperature dipping and sizing tank at 60 ℃, and a sizing agent is polyphenylene sulfide emulsion with solid content of 15%. And after the shaping and coating of the thermoplastic sizing agent are finished, drying at 150 ℃ for 15min.
Example 3
Under the action of constant tension, T1000 high-strength carbon fiber with 24K of tow is used as carbon fiber widening tow to be subjected to double-roller heating extrusion treatment, the widening tension is 7N, the widening rate is 5 m/min, and the heating temperature of the carbon fiber is 130 ℃. After widening, a polyamide hot melt adhesive film with a certain width is pasted in the direction vertical to the fibers, the thickness is 0.5mm, the width is 3mm, the pasting mode is that a plurality of bundles of widening fibers are arranged in a plain mode in an alternating mode, and the pasting interval is 25cm. And (3) carrying out infiltration and shaping treatment on the carbon fiber spread tows pasted with the polyamide hot melt adhesive film, wherein the hot melting temperature is set to be 150 ℃, the hot melting time is set to be 5 seconds, and the hot melting pressure is set to be 2.5MPa. And synchronously applying stretching tension in the infiltration process, wherein the final yarn stretching width is 3 times of the original width of the carbon fiber filament bundle.
After the spread fiber is subjected to transverse interval infiltration and shaping treatment of the hot melt fiber, polyamide emulsion with the solid content of 15% is sprayed on the surface of one side of the spread fiber, the spraying pressure of the spraying is set to be 1.5MPa, and the spraying thickness is 0.06mm. And after the shaping and coating of the thermoplastic sizing agent are finished, drying at 100 ℃ for 30min.
Example 4
Under the action of constant tension, M60 high-modulus carbon fiber with 24K tow is adopted as carbon fiber widening tow to carry out double-roller heating extrusion treatment, the widening tension is 7N, the widening rate is 2M/min, and the heating temperature of the carbon fiber is 140 ℃. After widening, a polypropylene hot melt adhesive film with a certain width is pasted in the direction vertical to the fibers, the thickness is 0.4mm, the width is 4mm, the pasting mode is that a plurality of bundles of widening fibers are arranged in a plain mode in an alternating mode, and the pasting interval is 20cm. And (3) carrying out infiltration and shaping treatment on the carbon fiber spread tows pasted with the polypropylene hot melt adhesive film, wherein the hot melting temperature is set to be 160 ℃, the hot melting time is set to be 4 seconds, and the hot melting pressure is set to be 2MPa. And synchronously applying stretching tension in the infiltration process, wherein the final yarn stretching width is 3 times of the original width of the carbon fiber filament bundle.
After transverse interval infiltration and shaping treatment of the hot-melt fiber, the spread fiber is matched with ultrasonic equipment to be dipped and coated in a constant-temperature dipping and sizing tank at 50 ℃, and a sizing agent is 15% of polypropylene emulsion with solid content. And after the shaping and coating of the thermoplastic sizing agent are finished, drying at 150 ℃ for 20min.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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 (10)

Translated fromChinese
1.一种碳纤维展宽定型复合处理方法,其特征在于,包括如下步骤:首先在恒定张力的作用下将连续长丝束碳纤维进行对辊加热挤压处理,展宽结束后在垂直纤维方向贴敷热熔纤维长丝进行定型处理,将贴敷热熔纤维长丝的碳纤维展宽丝束进行熔渗定型处理,最终将热熔纤维定型后的展宽纤维丝束涂覆定型上浆剂,完成展宽碳纤维的定型复合处理。1. A carbon fiber widening and shaping composite processing method, is characterized in that, comprises the following steps: first under the effect of constant tension, continuous long filament bundle carbon fiber is carried out to roller heating and extruding treatment, after widening ends, apply heat in the vertical fiber direction The fused fiber filaments are subjected to shaping treatment, and the carbon fiber widened tow pasted with hot-melt fiber filaments is subjected to infiltration and shaping treatment, and finally the widened fiber tow after the hot-melt fiber is shaped is coated with a shaping sizing agent to complete the shaping of the widened carbon fiber Composite processing.2.根据权利要求1所述碳纤维展宽定型复合处理方法,其特征在于,所述的连续长丝束碳纤维选自T300、T700、T800、T1000、M40、M55、M60其中的任意一种,其规格选自3K、6K、12K、24K中的一种。2. The composite treatment method of carbon fiber widening and shaping according to claim 1, wherein the continuous filament bundle carbon fiber is selected from any one of T300, T700, T800, T1000, M40, M55, and M60, and its specification One selected from 3K, 6K, 12K, 24K.3.根据权利要求1所述碳纤维展宽定型复合处理方法,其特征在于,对辊加热挤压处理的条件为:展宽张力控制在5-8N,展纱速率在1-8m/分钟,在恒定张力下将连续长丝束碳纤维在80-150℃范围内加热。3. The carbon fiber widening and shaping composite treatment method according to claim 1, characterized in that, the conditions for the heated extrusion treatment of the rollers are: the widening tension is controlled at 5-8N, the spreading speed is at 1-8m/min, at a constant tension The continuous filament bundle carbon fiber is heated in the range of 80-150°C.4.根据权利要求1所述碳纤维展宽定型复合处理方法,其特征在于,热熔纤维长丝选自聚乙烯、聚丙烯、聚苯乙烯、聚苯硫醚、聚酰胺、聚酰亚胺、聚醚酮、聚醚醚酮、对苯二甲酸乙二醇酯、对苯二甲酸丁二醇酯中的一种或多种。4. according to claim 1, said carbon fiber widening and shaping composite processing method, it is characterized in that, hot-melt fiber filament is selected from polyethylene, polypropylene, polystyrene, polyphenylene sulfide, polyamide, polyimide, poly One or more of ether ketone, polyether ether ketone, ethylene terephthalate, and butylene terephthalate.5.根据权利要求1所述碳纤维展宽定型复合处理方法,其特征在于,所述的热熔纤维长丝用带状热熔胶膜予以替代,热熔胶膜选自聚乙烯、聚丙烯、聚苯乙烯、聚苯硫醚、聚酰胺、聚酰亚胺、聚醚酮、聚醚醚酮、对苯二甲酸乙二醇酯、对苯二甲酸丁二醇酯中的一种或多种。5. according to claim 1, said carbon fiber widening sizing composite processing method, it is characterized in that, described hot-melt fiber filament is replaced with strip-shaped hot-melt adhesive film, and hot-melt adhesive film is selected from polyethylene, polypropylene, polypropylene One or more of styrene, polyphenylene sulfide, polyamide, polyimide, polyether ketone, polyether ether ketone, ethylene terephthalate, butylene terephthalate.6.根据权利要求4或5所述碳纤维展宽定型复合处理方法,其特征在于,热熔纤维长丝采用1-10根纤维并行排布;或带状热熔胶膜厚度范围为0.05-2mm,带状热熔胶膜的宽度控制在2-5mm范围内;6. According to claim 4 or 5, the carbon fiber widening and shaping composite treatment method is characterized in that, the hot-melt fiber filaments are arranged in parallel by 1-10 fibers; or the thickness range of the strip-shaped hot-melt adhesive film is 0.05-2mm, The width of the strip-shaped hot melt adhesive film is controlled within the range of 2-5mm;所述的热熔纤维长丝或带状热熔胶膜沿纤维轴向的间隔距离控制在10-30cm,热熔长丝或带状热熔胶膜采用长丝单面排布、上下表面交替排布或多束展宽纤维平纹交替排布进行热熔处理。The distance between the hot-melt fiber filaments or the strip-shaped hot-melt adhesive film along the fiber axis is controlled at 10-30cm, and the hot-melt filaments or strip-shaped hot-melt adhesive film are arranged on one side of the filaments, and the upper and lower surfaces alternate Arrangement or alternate arrangement of multi-bundle widened fiber plain weave for hot-melt treatment.7.根据权利要求6所述碳纤维展宽定型复合处理方法,其特征在于,热熔温度为120-300℃,热熔定型时间为0.5-5秒,热熔压力为0.5-3MPa。7. The composite treatment method of carbon fiber widening and shaping according to claim 6, characterized in that the hot melting temperature is 120-300°C, the hot melting setting time is 0.5-5 seconds, and the hot melting pressure is 0.5-3 MPa.8.根据权利要求1所述碳纤维展宽定型复合处理方法,其特征在于,在单侧表面或双侧表面进行定型上浆剂涂覆,通过加热烘干形成定型复合膜涂层;8. The carbon fiber widening and shaping composite treatment method according to claim 1, wherein the shaping and sizing agent coating is carried out on the surface of one side or both sides, and the shaping composite film coating is formed by heating and drying;所述的涂覆方式为喷涂或浸渍;The coating method is spraying or dipping;优选的,所述喷涂的喷射压力为0.5-2MPa,喷涂厚度为0.02-0.1㎜;Preferably, the injection pressure of the spraying is 0.5-2MPa, and the spraying thickness is 0.02-0.1mm;优选的,所述浸渍为在40-60℃的恒定温度浸渍上浆槽中进行;更优选的,配合超声装备提高浸渍涂覆效果。Preferably, the impregnation is carried out in a dipping and sizing tank at a constant temperature of 40-60° C.; more preferably, ultrasonic equipment is used to improve the dip coating effect.9.根据权利要求1所述碳纤维展宽定型复合处理方法,其特征在于,所述定型上浆剂为热塑性上浆乳液,其固含量为5-20%;所采用的热塑性上浆乳液选自聚乙烯、聚丙烯、聚苯乙烯、聚苯硫醚、聚酰胺、聚酰亚胺、聚醚酮、聚醚醚酮、对苯二甲酸乙二醇酯、对苯二甲酸丁二醇酯中的一种或多种。9. The carbon fiber widening and shaping composite treatment method according to claim 1, characterized in that, the shaping sizing agent is a thermoplastic sizing emulsion with a solid content of 5-20%; the adopted thermoplastic sizing emulsion is selected from polyethylene, poly One of acrylic, polystyrene, polyphenylene sulfide, polyamide, polyimide, polyether ketone, polyether ether ketone, ethylene terephthalate, butylene terephthalate or Various.10.根据权利要求9所述碳纤维展宽定型复合处理方法,其特征在于,涂覆定型上浆剂后在100-150℃下进行烘干处理,烘干时间为10-30min。10 . The composite treatment method for carbon fiber widening and shaping according to claim 9 , characterized in that, drying treatment is carried out at 100-150° C. for 10-30 minutes after coating the shaping sizing agent. 11 .
CN202211311976.1A2022-10-252022-10-25 A carbon fiber widening and shaping composite processing methodActiveCN115648664B (en)

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CN118854669A (en)*2024-07-222024-10-29中复神鹰碳纤维股份有限公司 Carbon fiber and preparation method thereof

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