CN110080036A - 一种含微纤化纤维素的纤维复合材料及其制备方法 - Google Patents
一种含微纤化纤维素的纤维复合材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种含微纤化纤维素的纤维复合材料及其制备方法。首先用阴离子助剂对微纤化纤维素进行改性,同时用阳离子助剂对无机填料进行改性,然后将改性后两种水分散液混合,并加入纤维、胶乳和助剂,所得浆料再经抄造、脱水、干燥、硫化后得到含微纤化纤维素的纤维复合材料。本发明方法操作方便、工艺简单、适用性强,有利于规模化生产。本发明提供的含微纤化纤维素的纤维复合材料具有无机填料含量高、昂贵增强纤维用量少、材料拉伸强度好的优点。
Description
技术领域
本发明属于复合材料与纤维材料的交叉领域,具体涉及一种含微纤化纤维素的纤维复合材料及其制备方法。
背景技术
复合材料是由两种或两种以上不同性质的材料经物理或化学的方法在宏观或微观上组合而成的具有新性能的材料。各种材料在性能上可互相取长补短,产生协同效应,使复合材料的综合性能优于原组成材料而满足各种不同的要求。纤维复合密封材料主要用于制造各种密封垫片,广泛应用于各种车辆、机械设备以及各类管道连接处的密封,对车辆、机械的使用性能以及工业生产过程中的环境卫生和操作安全起着关键性的作用。目前常用的纤维复合密封材料主要由纤维、胶乳、无机填料和助剂组成。从降低成本和提高材料的耐热性方面考虑,必须尽量提高材料中的无机填料含量,但填料的大量增加必定会导致密封材料力学性能的损失,所以为了提高材料的力学强度,就需要加入芳纶纤维、碳纤维等对材料进行增强,但通常这些增强纤维的价格昂贵,不利于纤维复合密封材料的成本控制。所以如何提高填料含量的同时又能保证材料的力学强度和其它综合性能,已成为本领域技术人员急需解决的问题之一。
发明内容
针对上述问题,本发明的目的在于提供一种含微纤化纤维素的纤维复合材料及其制备方法,该纤维复合材料的填料含量高、有机纤维用量低,且具有良好的拉伸强度、压缩性、回弹性和密封性能。
为实现上述目的,本发明采用的技术方案是:
一种含微纤化纤维素的纤维复合材料的制备方法,其特征在于,包括如下步骤:
(1)微纤化纤维素的改性:将微纤化纤维素分散在水中,加入阴离子助剂并搅拌均匀;
(2)无机填料的改性:将无机填料分散在水中,加入阳离子助剂并搅拌均匀;
(3)浆料配制:将改性后的微纤化纤维素水分散液与改性后的无机填料水分散液混合并搅拌均匀,再加入纤维、胶乳和助剂,配制成浆料;
(4)材料成型:将配置好的浆料采用抄纸法抄造成湿片层,再经脱水、干燥、硫化后得到含微纤化纤维素的纤维复合材料。
所述的微纤化纤维素为含有羧基、或羧甲基、或羧乙基、或磺酸基、或不含上述任意一种取代基的微纤化纤维素纤维中的至少一种,取代度优选为0-0.5;其纤维直径在5nm至1um之间,优选为20nm-500nm之间;纤维长度在100nm-1mm之间,优选为500nm-500μm之间。
所述的阴离子助剂为阴离子聚丙烯酰胺、木质素磺酸钠、羧甲基纤维素钠、聚甲基丙烯酸钠中的一种,其用量为微纤化纤维素的0-2wt%,优选为0.01-0.5wt%。
所述的无机填料为碳酸钙、高岭土、云母粉、硅灰石、膨润土、碳化硅、氧化锌、滑石粉、硫酸钡、白炭黑、膨胀石墨中的至少一种。
所述的阳离子助剂为阳离子聚丙烯酰胺、聚二烯丙基二甲基氯化铵、聚胺、阳离子淀粉、阳离子瓜尔胶、阳离子壳聚糖中的一种,其用量为无机填料的0-1wt%,优选为0.001-0.1wt%。
所述的纤维选自纸浆纤维、芳纶纤维、腈纶纤维、芳砜纶纤维、碳纤维、玻璃纤维、陶瓷纤维中的至少一种。
所述的胶乳选自天然胶乳、丁苯胶乳、丁腈胶乳、氯丁胶乳、丙烯酸胶乳中的至少一种。
所述的助剂包括硫化剂(硫黄和噻唑类)、防老剂(N-苯基-2-萘胺)、颜料(炭黑)、消泡剂(聚二甲基硅氧烷)和絮凝剂(硫酸铝)。
所述的含微纤化纤维素的纤维复合材料的组成具有如下特征:微纤化纤维素0.1-15wt%(优选为1-5wt%)、橡胶5-30wt%、纤维10-40wt%(其中芳纶纤维、碳纤维等昂贵纤维总量优选为0-18wt%)、填料25-75wt%(优选为40-60wt%)、助剂1-5wt%。
本发明与现有技术相比,具有如下优点和有益效果:
1、该方法提供的含微纤化纤维素的纤维复合材料及其制备方法可以使产品在高填料用量下仍保持较高的横向拉伸强度和良好的密封性能。
2、该方法提供的含微纤化纤维素的纤维复合材料及其制备方法可以保证材料强度和力学性能的同时减少芳纶纤维、碳纤维等增强用昂贵纤维的用量,有利于降低制造成本。
3、该方法提供的含微纤化纤维素的纤维复合材料的制备方法操作方便、工艺简单、适用性强的优点,有利于纤维复合材料的工业化生产。
具体实施方式
下面结合具体实施例对本发明作进一步详细描述,但不作为对本发明的限定。
实施例1
(1)将不含任何取代基的微纤化纤维素5g(绝干量,下同)分散在水中,加入0.025g阴离子聚丙烯酰胺并搅拌均匀;
(2)将由30g碳酸钙、30g高岭土和25g滑石粉组成的无机填料分散在水中,加入0.003g阳离子淀粉并搅拌均匀;
(3)将改性后的微纤化纤维素水分散液与改性后的无机填料水分散液混合并搅拌均匀,再加入2g芳纶纤维、1g玻璃纤维、3g丁苯胶乳、2g丁腈胶乳和2g助剂(硫黄∶噻唑类∶N-苯基-2-萘胺∶炭黑∶聚二甲基硅氧烷∶硫酸铝=20∶15∶12∶30∶18∶5),配制成浆料;
(4)将配置好的浆料采用抄纸法抄造成湿片层,再经脱水、干燥、硫化后得到含微纤化纤维素的纤维复合材料。
同时,制备不含微纤化纤维素且未对无机填料进行阳离子助剂改性的纤维复合材料作为对照组A和对照组B。对照组A中,先将无机填料分散在水中,再加入纤维、胶乳和助剂,除芳纶纤维的加入量由2g增加到7g外,其它组分及其加入量不变,按步骤(3)和步骤(4)得到纤维复合材料对照组A。对照组B的制备方法同对照组A,除芳纶纤维加入量仍为2g,玻璃纤维的加入量由1g增加至6g外,其它不变,得到纤维复合材料对照组B。本发明实施例1与对照组A和对照组B所得三种纤维复合材料的性能检测数据如表1所示。
表1实施例1与对照组A和对照组B所得三种纤维复合材料的性能检测数据
实施例2
(1)将取代度为0.2的羧乙基微纤化纤维素10g(绝干量,下同)分散在水中,加入0.01g羧甲基纤维素钠并搅拌均匀;
(2)将由20g云母粉、40g膨润土和10g白炭黑组成的无机填料分散在水中,加入0.8g聚二烯丙基二甲基氯化铵并搅拌均匀;
(3)将改性后的微纤化纤维素水分散液与改性后的无机填料水分散液混合并搅拌均匀,再加入2g碳纤维、2g纸浆纤维、1g陶瓷纤维、3g丁腈胶乳、4g氯丁胶乳、3g丙烯酸胶乳和5g助剂(硫黄∶噻唑类∶N-苯基-2-萘胺∶炭黑∶聚二甲基硅氧烷∶硫酸铝=30∶15∶10∶28∶15∶2),配制成浆料;
(4)将配置好的浆料采用抄纸法抄造成湿片层,再经脱水、干燥、硫化后得到含微纤化纤维素的纤维复合材料。
同时,制备不含微纤化纤维素且未对无机填料进行阳离子助剂改性的纤维复合材料作为对照组C和对照组D。对照组C中,先将无机填料分散在水中,再加入纤维、胶乳和助剂,除碳纤维的加入量由2g增加到7g外,其它组分及其加入量不变,按步骤(3)和步骤(4)得到纤维复合材料对照组C。对照组D的制备方法同对照组C,除碳纤维加入量仍为2g,纸浆纤维的加入量由2g增加至7g外,其它不变,得到纤维复合材料对照组D。本发明实施例2与对照组C和对照组D所得三种纤维复合材料的性能检测数据如表2所示。
表2实施例2与对照组C和对照组D所得三种纤维复合材料的性能检测数据
实施例3
(1)将取代度为0.05的2,2,6,6-四甲基哌啶氮氧化物(TEMPO)氧化的微纤化纤维素3g(绝干量,下同)分散在水中,加入0.045g聚甲基丙烯酸钠并搅拌均匀;
(2)将由20g硅灰石、50g碳化硅和17g硫酸钡组成的无机填料分散在水中,加入0.18g阳离子聚丙烯酰胺并搅拌均匀;
(3)将改性后的微纤化纤维素水分散液与改性后的无机填料水分散液混合并搅拌均匀,再加入0.5g腈纶纤维、0.5g芳砜纶纤维、3g丁苯胶乳、1g丁腈胶乳、2g氯丁胶乳和3g助剂(硫黄∶噻唑类∶N-苯基-2-萘胺∶炭黑∶聚二甲基硅氧烷∶硫酸铝=25∶15∶15∶25∶15∶5),配制成浆料;
(4)将配置好的浆料采用抄纸法抄造成湿片层,再经脱水、干燥、硫化后得到含微纤化纤维素的纤维复合材料。
同时,制备不含微纤化纤维素且未对无机填料进行阳离子助剂改性的纤维复合材料作为对照组E和对照组F。对照组E中,先将无机填料分散在水中,再加入纤维、胶乳和助剂,除腈纶纤维的加入量由0.5g增加到3.5g外,其它组分及其加入量不变,按步骤(3)和步骤(4)得到纤维复合材料对照组E。对照组F的制备方法同对照组E,除腈纶纤维加入量仍为0.5g,芳砜纶纤维的加入量由0.5g增加至3.5g外,其它不变,得到纤维复合材料对照组F。本发明实施例3与对照组E和对照组F所得三种纤维复合材料的性能检测数据如表3所示。
表3实施例3与对照组E和对照组F所得三种纤维复合材料的性能检测数据
实施例4
(1)将取代度为0.4的磺酸基微纤化纤维素12g(绝干量,下同)分散在水中,加入0.0024g木质素磺酸钠并搅拌均匀;
(2)将由30g高岭土、15g氧化锌和15g膨胀石墨组成的无机填料分散在水中,加入0.03g阳离子瓜尔胶并搅拌均匀;
(3)将改性后的微纤化纤维素水分散液与改性后的无机填料水分散液混合并搅拌均匀,再加入4g芳纶纤维、1g玻璃纤维、2g陶瓷纤维、3g天然胶乳、3g氯丁胶乳、8g丁苯胶乳和7g助剂(硫黄∶噻唑类∶N-苯基-2-萘胺∶炭黑∶聚二甲基硅氧烷∶硫酸铝=35∶15∶12∶20∶15∶3),配制成浆料;
(4)将配置好的浆料采用抄纸法抄造成湿片层,再经脱水、干燥、硫化后得到含微纤化纤维素的纤维复合材料。
同时,制备不含微纤化纤维素且未对无机填料进行阳离子助剂改性的纤维复合材料作为对照组G和对照组H。对照组G中,先将无机填料分散在水中,再加入纤维、胶乳和助剂,除芳纶纤维的加入量由4g增加到16g外,其它组分及其加入量不变,按步骤(3)和步骤(4)得到纤维复合材料对照组G。对照组H的制备方法同对照组G,除芳纶纤维加入量仍为4g,陶瓷纤维的加入量由2g增加至14g外,其它不变,得到纤维复合材料对照组H。本发明实施例4与对照组G和对照组H所得三种纤维复合材料的性能检测数据如表1所示。
表4实施例4与对照组G和对照组H所得三种纤维复合材料的性能检测数据
以上实施例仅为本发明的示例性实施例,不用于限制本发明,本发明的保护范围由权利要求书限定。本领域技术人员可以在本发明的实质和保护范围内,对本发明做出各种修改或等同替换,这种修改或等同替换也应视为落在本发明的保护范围内。
Claims (7)
1.一种含微纤化纤维素的纤维复合材料的制备方法,其特征在于,包括如下步骤:
(1)微纤化纤维素的改性:将微纤化纤维素分散在水中,加入阴离子助剂并搅拌均匀;
(2)无机填料的改性:将无机填料分散在水中,加入阳离子助剂并搅拌均匀;
(3)浆料配制:将改性后的微纤化纤维素水分散液与改性后的无机填料水分散液混合并搅拌均匀,再加入纤维、胶乳和助剂,配制成浆料;
(4)材料成型:将配置好的浆料采用抄纸法抄造成湿片层,再经脱水、干燥、硫化后得到含微纤化纤维素的纤维复合材料。
2.根据权利要求1所述的含微纤化纤维素的纤维复合材料的制备方法,其特征在于,所述步骤(1)中微纤化纤维素为含有羧基、或羧甲基、或羧乙基、或磺酸基、或不含上述任意一种取代基的微纤化纤维素纤维中的至少一种,其纤维直径在5nm至1um之间,长度在100nm-1mm之间。
3.根据权利要求1所述的含微纤化纤维素的纤维复合材料的制备方法,其特征在于,所述步骤(1)中阴离子助剂为阴离子聚丙烯酰胺、木质素磺酸钠、羧甲基纤维素钠、聚甲基丙烯酸钠中的一种,其用量为微纤化纤维素的0-2wt%。
4.根据权利要求1所述的含微纤化纤维素的纤维复合材料的制备方法,其特征在于,所述步骤(2)中无机填料为碳酸钙、高岭土、云母粉、硅灰石、膨润土、碳化硅、氧化锌、滑石粉、硫酸钡、白炭黑、膨胀石墨中的至少一种。
5.根据权利要求1所述的含微纤化纤维素的纤维复合材料的制备方法,其特征在于,所述步骤(2)中阳离子助剂为阳离子聚丙烯酰胺、聚二烯丙基二甲基氯化铵、聚胺阳离子淀粉、阳离子瓜尔胶、阳离子壳聚糖中的一种,其用量为无机填料的0-1wt%。
6.根据权利要求1所述的含微纤化纤维素的纤维复合材料的制备方法,其特征在于,所述步骤(3)中纤维选自纸浆纤维、芳纶纤维、腈纶纤维、芳砜纶纤维、碳纤维、玻璃纤维、陶瓷纤维中的至少一种,胶乳选自天然胶乳、丁苯胶乳、丁腈胶乳、氯丁胶乳、丙烯酸胶乳中的至少一种,助剂包括硫化剂(硫黄和噻唑类)、防老剂(N-苯基-2-萘胺)、颜料(炭黑)、消泡剂(聚二甲基硅氧烷)和絮凝剂(硫酸铝)。
7.一种含微纤化纤维素的纤维复合材料,其特征在于,所述含微纤化纤维素的纤维复合材料由权利要求1-7任意一种所述含微纤化纤维素的纤维复合材料制备方法制备而得;所述含微纤化纤维素的纤维复合材料其特征在于,其各组分含量如下:微纤化纤维素0.1-15wt%、橡胶5-30wt%、纤维10-40wt%、填料25-75wt%、助剂1-5wt%。
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