CN113858720B - 碳纤维复合板材及其制备方法 - Google Patents

碳纤维复合板材及其制备方法 Download PDF

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CN113858720B
CN113858720B CN202111159799.5A CN202111159799A CN113858720B CN 113858720 B CN113858720 B CN 113858720B CN 202111159799 A CN202111159799 A CN 202111159799A CN 113858720 B CN113858720 B CN 113858720B
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CN113858720A (zh
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陈同亮
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Shenzhen Leimu New Material Technology Co ltd
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Abstract

本发明公开了碳纤维复合板材及其制备方法，涉及板材领域，包括基层、缓冲层、增强碳纤维层，基层的上下两面均设置有缓冲层，缓冲层的外侧设置有增强碳纤维层；在三口烧瓶中加入聚乙二醇、催化剂和NaOH颗粒，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，得到中间体A；解决了碳纤维不易被树脂浸润及发生化学反应，因粘结性能差导致产品使用寿命短和抗冲击性差的问题；多羟基结构聚合甲苯二异氰酸酯，使得改性聚氨酯的大分子链数目增多、链段增长，大分子链和交联的网络结构形成类似于半互穿聚合物网络结构，物理交联结构增加，防止裂纹的产生和扩大，增强材料的抗冲击性能，从而达到了提升材料抗冲击性的目的。

Description

碳纤维复合板材及其制备方法
技术领域
本发明涉及板材领域，具体涉及碳纤维复合板材及其制备方法。
背景技术
碳纤维是一种含碳量达到95%以上的具有高比强度、高比模量、耐高温、抗化学腐蚀、低电阻、高热导、低热膨胀等特殊物理和化学性能的新型材料，在有机溶剂、酸、碱中不溶不胀，耐蚀性出类拔萃，碳纤维还具有纤维的柔软性和可编织性等优点，密度不足钢的1/4，但抗拉强度却是钢的7-9倍，通常来说，用碳纤维增强树脂、金属、陶瓷、水泥等基体制备复合材料，可以显著提升材料强度，碳纤维增强复合材料也被广泛的应用于军事、风电、石油开采、汽车制造等众多领域；
碳纤维的类石墨结构决定了其表面呈化学惰性，不易被树脂浸润及发生化学反应，因粘结性能差导致产品使用寿命短，且碳纤维复合板材的抗冲击性能差。
发明内容
为了克服上述的技术问题，本发明的目的在于提供了碳纤维复合板材及其制备方法：
（1）将木质素和腈纶溶于二甲基亚砜中装入纺丝罐中进行纺丝，进入干燥热辊进行干燥，得到共混原丝，将共混原丝碳纤维化处理，得到碳纤维，将碳纤维置于浓硝酸中超声处理，将碳纤维纺织成型，用丙酮稀释环氧树脂，加入熔融的间苯二胺，用刷子正交涂刷到纺织成型的碳纤维的正反两面并铺展逐次叠层，置于平板模具之间固化、卸压脱模得到该增强碳纤维层，通过制备得到该增强碳纤维层解决了碳纤维不易被树脂浸润及发生化学反应，因粘结性能差导致产品使用寿命短的问题；
（2）在三口烧瓶中加入聚乙二醇、催化剂和NaOH颗粒，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，得到中间体A，向中间体A中加入蒸馏水，加入浓硫酸，得到中间体B，在塑料杯内依次加入定量的1,4-丁二醇、中间体B、甲苯二异氰酸酯，搅拌均匀后倒入聚四氟乙烯模具中并铺平，将模具放入真空干燥箱中，得到该缓冲层，通过制备得到缓冲层解决了碳纤维复合板材的抗冲击性能差的问题。
本发明的目的可以通过以下技术方案实现：
碳纤维复合板材及其制备方法，包括基层、缓冲层、增强碳纤维层，所述基层的上下两面均设置有缓冲层，所述缓冲层的外侧设置有增强碳纤维层；
所述增强碳纤维层由以下步骤制备得到：
S1：将木质素和腈纶溶于二甲基亚砜中，在60-70℃水浴中搅拌24-26h，在60-70℃烘箱中静置10-12h，装入纺丝罐中进行纺丝，纺丝液在氮气压力下通过喷丝板进入60-70℃的纯水凝固浴中，进入70-80℃的水浴中洗涤、牵伸，进入110-120℃的干燥热辊进行干燥，得到共混原丝；
S2：将共混原丝从200-210℃以1-2℃/min的升温速率到250-260℃，并停留0.5-1h，在氮气气氛下以10-15℃/min的速率从室温加热到700-720℃，停留20-30min，继续升温到1400-1450℃，停留10-20min，得到碳纤维；
S3：将碳纤维置于60-70℃的浓硝酸中超声处理2-3h，用去离子水将碳纤维清洗至中性，再于80-85℃真空下烘干至恒重，将碳纤维纺织成型，用丙酮稀释环氧树脂浓度为36-38%，加入熔融的间苯二胺并搅拌混合均匀，用刷子正交涂刷到纺织成型的碳纤维的正反两面并铺展逐次叠层，铺4-6层，置于平板模具之间固化、卸压脱模得到该增强碳纤维层。
作为本发明进一步的方案：所述基层为芳纶纤维层。
作为本发明进一步的方案：步骤S1中所述木质素、腈纶的用量比为20g：110g。
作为本发明进一步的方案：步骤S3中所述浓硝酸的质量分数为65%，所述环氧树脂与碳纤维的质量比为4:6，所述间苯二胺的质量为环氧树脂质量的14%。
作为本发明进一步的方案：所述缓冲层的制备步骤如下：
S51：在三口烧瓶中加入聚乙二醇、催化剂和总量一半的NaOH颗粒，搅拌均匀后预热到40-50℃，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，调节温度至55-60℃，将另一半的NaOH颗粒加入到三口烧瓶中，在55-60℃下搅拌1.5-3h，冷却至室温，抽滤，用硫酸调至中性，减压蒸馏，得到中间体A；
S52：向中间体A中加入蒸馏水，加入浓硫酸，室温下水解3-4h，用碳酸钠调至中性，在温度为90-95℃、真空度为0.085-0.090MPa下减压蒸馏、抽滤，得到中间体B；
S53：在塑料杯内依次加入定量的1,4-丁二醇、中间体B、甲苯二异氰酸酯，搅拌均匀后倒入聚四氟乙烯模具中并铺平，将模具放入真空干燥箱中，用油泵抽真空进行脱泡处理30-60min后，60-70℃固化10-20h，得到该缓冲层。
作为本发明进一步的方案：步骤S51中所述催化剂为四正丁基溴化铵，所述聚乙二醇、甲基环氧氯丙烷、NaOH颗粒与催化剂的摩尔比为1:2.5:3:0.03。
作为本发明进一步的方案：步骤S52中所述浓硫酸的质量分数为98%，所述中间体A、蒸馏水与浓硫酸的用量比为23.1g：50mL：3g。
作为本发明进一步的方案：步骤S53中所述1,4-丁二醇、中间体B与甲苯二异氰酸酯的摩尔比为9:2:18。
碳纤维复合板材的制备方法，该碳纤维复合板材的制备方法具体步骤如下：
S91：按照碳纤维复合板材的尺寸规格裁剪基层、缓冲层与增强碳纤维层原材料；
S92：将裁剪好的原材料按照顺序铺设在一起，每层之间均匀涂刷纳米粘结剂，放入模具内，并将模具放入热压成型机热压成型；
S93：根据所需产品的形状和外观，采用全自动数控机床精加工成成品。
本发明的有益效果：
（1）本发明将木质素和腈纶溶于二甲基亚砜中装入纺丝罐中进行纺丝，进入干燥热辊进行干燥，得到共混原丝，将共混原丝碳纤维化处理，得到碳纤维，将碳纤维置于浓硝酸中超声处理，将碳纤维纺织成型，用丙酮稀释环氧树脂，加入熔融的间苯二胺，用刷子正交涂刷到纺织成型的碳纤维的正反两面并铺展逐次叠层，置于平板模具之间固化、卸压脱模得到该增强碳纤维层，木质素是制备碳纤维的理想原料，木质素为复杂的三维网状聚合物，采用腈纶、聚丙烯腈的聚合物与木质素共混改性，再通过湿法纺丝工艺制得连续纤维，避免木质素以“黑液”的形式排入江河或者被浓缩烧掉的现状，节约宝贵的材料，且保护生态环境，以木质素为原料得到碳纤维后对其表面作改性处理，超声波的“空化效应”对碳纤维表面冲击产生了空化刻蚀作用，在硝酸的协同作用下的碳纤维表面不仅产生了较深的沟壑，而且表面新增了大量大小不一的块状、球状或线状等凸起和斑痕，碳纤维的表面变得粗糙，使增强碳纤维层与缓冲层材料的粘结性得到改善，从而达到了增强复合材料的界面结合强度的目的；
在三口烧瓶中加入聚乙二醇、催化剂和NaOH颗粒，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，得到中间体A，向中间体A中加入蒸馏水，加入浓硫酸，得到中间体B，在塑料杯内依次加入定量的1,4-丁二醇、中间体B、甲苯二异氰酸酯，搅拌均匀后倒入聚四氟乙烯模具中并铺平，将模具放入真空干燥箱中，得到该缓冲层，通过制备得到缓冲层，通过聚乙二醇和甲基环氧氯丙烷反应引入环氧基团，再开环形成多羟基结构，聚合生成的聚氨酯在空间上呈现三维形态，不用加入小分子交联剂便可自身固化，避免了小分子交联剂易于迁徙的缺点，多羟基结构聚合甲苯二异氰酸酯，使得改性聚氨酯的大分子链数目增多、链段增长，大分子链和交联的网络结构形成类似于半互穿聚合物网络结构，物理交联结构增加，防止裂纹的产生和扩大，增强材料的抗冲击性能，从而达到了提升材料抗冲击性的目的。
附图说明
下面结合附图对本发明作进一步的说明；
图1是本发明中碳纤维复合板材的整体结构示意图；
图2是本发明中碳纤维复合板材的正视图；
图3是本发明中步骤S51的化学反应式；
图4是本发明中步骤S52的化学反应式；
图5是本发明中步骤S53的化学反应式；
图6是本发明中步骤S53的化学反应式中R基团结构式；
图中：1、基层；2、缓冲层；3、增强碳纤维层。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
根据图1-2所示，碳纤维复合板材，包括基层1、缓冲层2、增强碳纤维层3，基层1的上下两面均设置有缓冲层2，缓冲层2的外侧设置有增强碳纤维层3；
实施例1：
本实施例为碳纤维复合板材，基层1的上下两面均设置有缓冲层2，缓冲层2的外侧设置有增强碳纤维层3；
其中增强碳纤维层3由以下步骤制备得到：
S1：将木质素和腈纶溶于二甲基亚砜中，在60℃水浴中搅拌24h，在60℃烘箱中静置10h，装入纺丝罐中进行纺丝，纺丝液在氮气压力下通过喷丝板进入60℃的纯水凝固浴中，进入70℃的水浴中洗涤、牵伸，进入110℃的干燥热辊进行干燥，得到共混原丝；
S2：将共混原丝从200℃以1℃/min的升温速率到250℃，并停留0.5h，在氮气气氛下以10℃/min的速率从室温加热到700℃，停留20min，继续升温到1400℃，停留10min，得到碳纤维；
S3：将碳纤维置于60℃的浓硝酸中超声处理2h，用去离子水将碳纤维清洗至中性，再于80℃真空下烘干至恒重，将碳纤维纺织成型，用丙酮稀释环氧树脂浓度为36%，加入熔融的间苯二胺并搅拌混合均匀，用刷子正交涂刷到纺织成型的碳纤维的正反两面并铺展逐次叠层，铺4层，置于平板模具之间固化、卸压脱模得到该增强碳纤维层3；
其中缓冲层2的制备步骤如下：
S51：在三口烧瓶中加入聚乙二醇、催化剂和总量一半的NaOH颗粒，搅拌均匀后预热到40℃，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，调节温度至55℃，将另一半的NaOH颗粒加入到三口烧瓶中，在55℃下搅拌1.5h，冷却至室温，抽滤，用硫酸调至中性，减压蒸馏，得到中间体A；
S52：向中间体A中加入蒸馏水，加入浓硫酸，室温下水解3-4h，用碳酸钠调至中性，在温度为90℃、真空度为0.085MPa下减压蒸馏、抽滤，得到中间体B；
S53：在塑料杯内依次加入定量的1,4-丁二醇、中间体B、甲苯二异氰酸酯，搅拌均匀后倒入聚四氟乙烯模具中并铺平，将模具放入真空干燥箱中，用油泵抽真空进行脱泡处理30min后，60℃固化10h，得到该缓冲层2。
实施例2：
本实施例与实施例1的区别在于：
其中增强碳纤维层3由以下步骤制备得到：
S1：将木质素和腈纶溶于二甲基亚砜中，在60℃水浴中搅拌24h，在60℃烘箱中静置10h，装入纺丝罐中进行纺丝，纺丝液在氮气压力下通过喷丝板进入60℃的纯水凝固浴中，进入70℃的水浴中洗涤、牵伸，进入110℃的干燥热辊进行干燥，得到共混原丝；
S2：将共混原丝从200℃以1℃/min的升温速率到250℃，并停留0.5h，在氮气气氛下以10℃/min的速率从室温加热到700℃，停留20min，继续升温到1400℃，停留10min，得到碳纤维；
S3：将碳纤维置于60℃的浓硝酸中超声处理2h，用去离子水将碳纤维清洗至中性，再于80℃真空下烘干至恒重，将碳纤维纺织成型，用丙酮稀释环氧树脂浓度为36%，加入熔融的间苯二胺并搅拌混合均匀，用刷子正交涂刷到纺织成型的碳纤维的正反两面并铺展逐次叠层，铺4层，置于平板模具之间固化、卸压脱模得到该增强碳纤维层3；
其中缓冲层2的制备步骤如下：
S51：在三口烧瓶中加入聚乙二醇、催化剂和总量一半的NaOH颗粒，搅拌均匀后预热到50℃，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，调节温度至60℃，将另一半的NaOH颗粒加入到三口烧瓶中，在60℃下搅拌3h，冷却至室温，抽滤，用硫酸调至中性，减压蒸馏，得到中间体A；
S52：向中间体A中加入蒸馏水，加入浓硫酸，室温下水解4h，用碳酸钠调至中性，在温度为95℃、真空度为0.090MPa下减压蒸馏、抽滤，得到中间体B；
S53：在塑料杯内依次加入定量的1,4-丁二醇、中间体B、甲苯二异氰酸酯，搅拌均匀后倒入聚四氟乙烯模具中并铺平，将模具放入真空干燥箱中，用油泵抽真空进行脱泡处理60min后，70℃固化20h，得到该缓冲层2。
实施例3：
本实施例与实施例1的区别在于：
其中增强碳纤维层3由以下步骤制备得到：
S1：将木质素和腈纶溶于二甲基亚砜中，在70℃水浴中搅拌26h，在70℃烘箱中静置12h，装入纺丝罐中进行纺丝，纺丝液在氮气压力下通过喷丝板进入70℃的纯水凝固浴中，进入80℃的水浴中洗涤、牵伸，进入120℃的干燥热辊进行干燥，得到共混原丝；
S2：将共混原丝从210℃以2℃/min的升温速率到260℃，并停留1h，在氮气气氛下以15℃/min的速率从室温加热到720℃，停留30min，继续升温到1450℃，停留20min，得到碳纤维；
S3：将碳纤维置于70℃的浓硝酸中超声处理3h，用去离子水将碳纤维清洗至中性，再于85℃真空下烘干至恒重，将碳纤维纺织成型，用丙酮稀释环氧树脂浓度为38%，加入熔融的间苯二胺并搅拌混合均匀，用刷子正交涂刷到纺织成型的碳纤维的正反两面并铺展逐次叠层，铺6层，置于平板模具之间固化、卸压脱模得到该增强碳纤维层3；
其中缓冲层2的制备步骤如下：
S51：在三口烧瓶中加入聚乙二醇、催化剂和总量一半的NaOH颗粒，搅拌均匀后预热到50℃，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，调节温度至60℃，将另一半的NaOH颗粒加入到三口烧瓶中，在60℃下搅拌3h，冷却至室温，抽滤，用硫酸调至中性，减压蒸馏，得到中间体A；
S52：向中间体A中加入蒸馏水，加入浓硫酸，室温下水解4h，用碳酸钠调至中性，在温度为95℃、真空度为0.090MPa下减压蒸馏、抽滤，得到中间体B；
S53：在塑料杯内依次加入定量的1,4-丁二醇、中间体B、甲苯二异氰酸酯，搅拌均匀后倒入聚四氟乙烯模具中并铺平，将模具放入真空干燥箱中，用油泵抽真空进行脱泡处理60min后，70℃固化20h，得到该缓冲层2。
对比例1：
本对比例与实施例1相比未设置缓冲层2。
对比例2：
本对比例与实施例1相比增强碳纤维层未经过步骤S3处理。
将实施例1-3以及对比例1-2的碳纤维复合板材进行测试，采用CMT微机控制电子万能试验机，将热压成型后的样品用哑铃型裁刀裁剪成哑铃样条，测试拉伸强度、弯曲强度等性能；
检测结果如下表所示：
由上表可知，在相同测试条件下，实验例的拉伸强度达到了6.8-7.0MPa，而未设置缓冲层2的对比例1的拉伸强度为6.5MPa，增强碳纤维层未经过步骤S3处理的对比例2的拉伸强度为5.1MPa，实验例的弯曲强度达到了7.2-7.4MPa，而未设置缓冲层2的对比例1的弯曲强度为6.3MPa，增强碳纤维层未经过步骤S3处理的对比例2的弯曲强度为5.2MPa，实验例的冲击强度达到了38-41KJ/m2，而未设置缓冲层2的对比例1的冲击强度为20KJ/m2，增强碳纤维层未经过步骤S3处理的对比例2的冲击强度为34KJ/m2，实验例的各项数据明显优于对比例，说明制备得到的增强碳纤维层3和缓冲层2可以明显提升碳纤维复合板材的力学性能。
在本说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (3)

1.碳纤维复合板材，包括基层（1）、缓冲层（2）、增强碳纤维层（3），其特征在于，所述基层（1）的上下两面均设置有缓冲层（2），所述缓冲层（2）的外侧设置有增强碳纤维层（3）；
所述增强碳纤维层（3）由以下步骤制备得到：
S1：将木质素和腈纶溶于二甲基亚砜中，在60-70℃水浴中搅拌24-26h，在60-70℃烘箱中静置10-12h，装入纺丝罐中进行纺丝，纺丝液在氮气压力下通过喷丝板进入60-70℃的纯水凝固浴中，进入70-80℃的水浴中洗涤、牵伸，进入110-120℃的干燥热辊进行干燥，得到共混原丝；步骤S1中所述木质素、腈纶的用量比为20g：110g；
S2：将共混原丝从200-210℃以1-2℃/min的升温速率到250-260℃，并停留0.5-1h，在氮气气氛下以10-15℃/min的速率从室温加热到700-720℃，停留20-30min，继续升温到1400-1450℃，停留10-20min，得到碳纤维；
S3：将碳纤维置于60-70℃的浓硝酸中超声处理2-3h，用去离子水将碳纤维清洗至中性，再于80-85℃真空下烘干至恒重，将碳纤维纺织成型，用丙酮稀释环氧树脂浓度为36-38%，加入熔融的间苯二胺并搅拌混合均匀，用刷子正交涂刷到纺织成型的碳纤维的正反两面并铺展逐次叠层，铺4-6层，置于平板模具之间固化、卸压脱模得到该增强碳纤维层（3）；步骤S3中所述浓硝酸的质量分数为65%，所述环氧树脂与碳纤维的质量比为4:6，所述间苯二胺的质量为环氧树脂质量的14%；
所述缓冲层（2）的制备步骤如下：
S51：在三口烧瓶中加入聚乙二醇、催化剂和总量一半的NaOH颗粒，搅拌均匀后预热到40-50℃，用滴液漏斗将甲基环氧氯丙烷滴加至三口烧瓶中，调节温度至55-60℃，将另一半的NaOH颗粒加入到三口烧瓶中，在55-60℃下搅拌1.5-3h，冷却至室温，抽滤，用硫酸调至中性，减压蒸馏，得到中间体A；步骤S51中所述催化剂为四正丁基溴化铵，所述聚乙二醇、甲基环氧氯丙烷、NaOH颗粒与催化剂的摩尔比为1:2.5:3:0.03；
S52：向中间体A中加入蒸馏水，加入浓硫酸，室温下水解3-4h，用碳酸钠调至中性，在温度为90-95℃、真空度为0.085-0.090MPa下减压蒸馏、抽滤，得到中间体B；步骤S52中所述浓硫酸的质量分数为98%，所述中间体A、蒸馏水与浓硫酸的用量比为23.1g：50mL：3g；
S53：在塑料杯内依次加入定量的1,4-丁二醇、中间体B、甲苯二异氰酸酯，搅拌均匀后倒入聚四氟乙烯模具中并铺平，将模具放入真空干燥箱中，用油泵抽真空进行脱泡处理30-60min后，60-70℃固化10-20h，得到该缓冲层（2）；步骤S53中所述1,4-丁二醇、中间体B与甲苯二异氰酸酯的摩尔比为9:2:18。
2.根据权利要求1所述的碳纤维复合板材，其特征在于，所述基层（1）为芳纶纤维层。
3.如权利要求1所述的碳纤维复合板材的制备方法，其特征在于，该碳纤维复合板材的制备方法具体步骤如下：
S91：按照碳纤维复合板材的尺寸规格裁剪基层（1）、缓冲层（2）与增强碳纤维层（3）原材料；
S92：将裁剪好的原材料按照顺序铺设在一起，每层之间均匀涂刷纳米粘结剂，放入模具内，并将模具放入热压成型机热压成型；
S93：根据所需产品的形状和外观，采用全自动数控机床精加工成成品。
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