CN108547151A - 一种水性环氧树脂碳纤维上浆剂 - Google Patents
一种水性环氧树脂碳纤维上浆剂 Download PDFInfo
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- CN108547151A CN108547151A CN201810289613.XA CN201810289613A CN108547151A CN 108547151 A CN108547151 A CN 108547151A CN 201810289613 A CN201810289613 A CN 201810289613A CN 108547151 A CN108547151 A CN 108547151A
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- epoxy resins
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明公开了一种水性环氧树脂碳纤维上浆剂,属于碳纤维生产技术领域。本发明按重量份数计,将20~30份水性环氧树脂,20~30份改性海藻酸钠液,20~30份聚乙烯醇液,10~20份氨水,10~20份纳米二氧化硅,10~20份碳酸氢钙溶液,10~20份碱性酚醛树脂,10~20份改性海泡石,10~20份硅烷偶联剂,5~8份多巴胺溶液,1~2份氯化铬置于3号烧杯中,于转速为300~500r/min条件下,搅拌混合40~60min,即得水性环氧树脂碳纤维上浆剂。本发明提供的水性环氧树脂碳纤维上浆剂具有优异的抗剪切强度和耐磨性能。
Description
技术领域
本发明公开了一种水性环氧树脂碳纤维上浆剂,属于碳纤维生产技术领域。
背景技术
碳纤维(CF)是1种含碳质量分数在90%以上的新型无机高分子纤维材料,具有高比强度、高比模量、耐高温、耐腐蚀、导电导热和电磁屏蔽性好等一系列优异性能,广泛应用于航空航天、汽车、体育用品、风力发电等领域。由于碳纤维为脆性材料,在加工过程中容易发生起毛、断丝等现象,导致其力学强度等性能降低,所以为了改善碳纤维的加工性能,在生产工艺中有一道重要的工序就是上浆。随着各个行业对于碳纤维性能要求的提高,上浆剂作为碳纤维助剂在提高碳纤维各个性能方面表现优异,迅速成为碳纤维企业的发展重点。
碳纤维上浆剂作为高性能碳纤维制造的关键环节,主要有以下几个作用:1)提高碳纤维的集束性和耐磨性,保护碳纤维表面。对于碳纤维本身而言,在经过上浆工艺后,碳纤维的集束性和耐磨性得到了提高,减少了碳纤维在后加工过程中容易起毛、断丝的现象;其次在经过上浆干燥后,上浆剂会在碳纤维表面形成一层薄膜,这层薄膜可以避免碳纤维表面吸附空气中的水分和灰尘;2)提高树脂对碳纤维的浸润性。在复合材料的制备过程中,由于碳纤维和树脂是2种不同的材料,所以树脂在碳纤维中的浸润性至关重要,上浆剂作为1种润湿剂,能分别与树脂和纤维进行匹配,涂覆于碳纤维表面之后,能够提高碳纤维表面被树脂的浸润能力;3)提高复合材料的界面性能,复合材料的性能除了碳纤维和树脂本身的性能外,界面性能也是重要的性能之一,良好的上浆剂可以作为纤维和树脂之间的连接体,改善纤维与基体树脂的粘合力及后加工性能。对于目前传统上浆剂还存在的抗剪切性能和耐磨性能不佳的问题,需对其进行进一步研究。
发明内容
本发明主要解决的技术问题是:针对传统上浆剂抗剪切性能和耐磨性能不佳的问题,提供了一种水性环氧树脂碳纤维上浆剂。
为了解决上述技术问题,本发明所采用的技术方案是:
一种水性环氧树脂碳纤维上浆剂,是由以下重量份数的原料组成:
水性环氧树脂 20~30份
改性海藻酸钠液 20~30份
聚乙烯醇液 20~30份
氨水 10~20份
纳米二氧化硅 10~20份
碳酸氢钙溶液 10~20份
碱性酚醛树脂 10~20份
改性海泡石 10~20份
硅烷偶联剂 10~20份
多巴胺溶液 5~8份
氯化铬 1~2份
所述水性环氧树脂碳纤维上浆剂的制备过程为:按原料组成称量各原料,将水性环氧树脂,改性海藻酸钠液,聚乙烯醇液,氨水,纳米二氧化硅,碳酸氢钙溶液,碱性酚醛树脂,改性海泡石,硅烷偶联剂,多巴胺溶液和氯化铬搅拌混合,即得水性环氧树脂碳纤维上浆剂。
所述水性环氧树脂的制备过程为:将环氧树脂618与无水乙醇按质量比1:20~1:30搅拌溶解后,升温,滴加环氧树脂618质量0.5~0.6倍的二乙醇胺,恒温搅拌反应,恒温抽真空,调节pH,随后加入无水乙醇质量1~2倍的水,搅拌混合,即得水性环氧树脂。
所述改性海藻酸钠的制备过程为:将海藻酸钠与水按质量比1:50~1:100混合,静置溶胀后,加热搅拌混合,随后加入海藻酸钠质量0.4~0.5倍的高碘酸钠溶液,继续加热搅拌混合,即得改性海藻酸钠液。
所述聚乙烯醇液的制备过程为:将聚乙烯醇与水按质量比1:50~1:100混合,静置溶胀,加热搅拌混合,即得聚乙烯醇液。
所述碱性酚醛树脂的制备过程为:按重量份数计,将30~40份乙二醛溶液,10~20份氢氧化钾溶液,30~40份对苯二酚恒温搅拌反应,降温,加入乙二醛溶液体积0.2~0.3倍的乙烯脲搅拌反应,降温,加入乙二醛溶液体积0.1~0.2倍的硅烷偶联剂KH-570搅拌反应,降温,即得碱性酚醛树脂。
所述改性海泡石的制备过程为:将海泡石用盐酸恒温浸泡后,过滤,洗涤,干燥,焙烧,得改性海泡石。
所述硅烷偶联剂为硅烷偶联剂KH-550,硅烷偶联剂KH-560或硅烷偶联剂KH-570中的任意一种。
本发明的有益效果是:
本发明通过添加改性海藻酸钠液,首先,在制备过程中,海藻酸钠分子链上的羟基易被高碘酸钠氧化成醛基,在混料过程中,体系中的铬离子可促使海藻酸钠液交联,形成三维网络,形成的三维网络对体系起到良好的增稠作用,从而避免体系出现分层,从而提升产品的储存稳定性,其次,在加热固化过程中,改性海藻酸钠液分子中醛基与基体表面的羟基发生羟醛缩合,增强纤维与树脂间的界面结合,从而提升体系的抗剪切强度,再次,在使用过程中,体系中的高碘酸钠可对碳纤维进行氧化,丰富其表面结构的活性基团数量,从而提高碳纤维与树脂之间的结合力,一方面,增强体系的抗剪切强度,另一方面,可使线性的环氧树脂缠绕固定于碳纤维表面,在碳纤维表面中形成相互缠绕的牢固三维网络,从而使线性的大分子聚合物在受到外力作用时运动困难,不易发生不可逆滑移,且牢固三维网络可将外力快速分散到体系的各个角落,从而使机械能转化为热能耗散掉,从而提升产品的耐磨性能。
具体实施方式
将环氧树脂618与无水乙醇按质量比1:20~1:30置于三口烧瓶中,于转速为300~500r/min条件下,搅拌溶解1~2h后,升温至75~85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.5~0.6倍的二乙醇胺,于温度为75~85℃,转速为300~500r/min条件下,恒温搅拌反应2~3h后,再于上述温度条件下恒温抽真空40~60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.1~7.3,随后向三口烧瓶中加入无水乙醇质量1~2倍的水,于转速为300~500r/min条件下,搅拌混合40~60min,即得水性环氧树脂;将海藻酸钠与水按质量比1:50~1:100置于1号烧杯中,用玻璃棒搅拌混合20~30min后,静置溶胀3~4h后,于温度为90~95℃,转速为300~500r/min条件下,加热搅拌混合1~2h,随后向1号烧杯中加入海藻酸钠质量1~2倍质量浓度为150~200mg/L的高碘酸钠溶液,于温度为90~95℃,转速为300~500r/min条件下,恒温搅拌混合40~60min,即得改性海藻酸钠液;将聚乙烯醇与水按质量比1:50~1:100加入1号烧杯中,用玻璃棒搅拌混合20~30min后,静置溶胀3~4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为95~100℃,转速为400~500r/min条件下,加热搅拌溶解40~50min,即得聚乙烯醇液;按重量份数计,将30~40份质量分数为40~50%的乙二醛溶液,10~20份质量分数为20~30%的氢氧化钾溶液,30~40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为76~78℃,转速为300~500r/min条件下,恒温搅拌反应3~4h后,将四口烧瓶中温度降至60~62℃,再向四口烧瓶中加入乙二醛溶液体积0.2~0.3倍的乙烯脲,于温度为60~62℃,转速为300~500r/min条件下,恒温搅拌反应40~60min后,将四口烧瓶中温度降至50~52℃,接着向四口烧瓶中加入乙二醛溶液体积0.1~0.2倍的硅烷偶联剂KH-570,于温度为50~52℃,转速为300~500r/min条件下,恒温搅拌反应40~50min,将四口烧瓶中温度降至40~42℃,于温度为40~42℃,转速为300~500r/min条件下,继续恒温搅拌反应20~30min,即得碱性酚醛树脂;按质量比为1:10~1:12将海泡石和质量分数为10~20%盐酸混合倒入2号烧杯中,并将2号烧杯移入数显测速恒温磁力搅拌器,于温度为45~50℃,转速为300~500r/min条件下,恒温浸泡2~4h,再经过滤,得滤饼,并用去离子水洗涤滤饼3~5次,再将洗涤后的滤饼转入烘箱中,于温度为105~110℃条件下干燥至恒重,得干燥滤饼,再将所得干燥滤饼转入管式炉,于温度为220~240℃条件下,保温焙烧1~3h后,随炉冷却至室温,出料,得改性海泡石;按重量份数计,将20~30份水性环氧树脂,20~30份改性海藻酸钠液,20~30份聚乙烯醇液,10~20份氨水,10~20份纳米二氧化硅,10~20份碳酸氢钙溶液,10~20份碱性酚醛树脂,10~20份改性海泡石,10~20份硅烷偶联剂,5~8份质量浓度为2.5mg/mL多巴胺溶液,1~2份氯化铬置于3号烧杯中,于转速为300~500r/min条件下,搅拌混合40~60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550,硅烷偶联剂KH-560或硅烷偶联剂KH-570中的任意一种。
将环氧树脂618与无水乙醇按质量比1:30置于三口烧瓶中,于转速为500r/min条件下,搅拌溶解2h后,升温至85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.6倍的二乙醇胺,于温度为85℃,转速为500r/min条件下,恒温搅拌反应3h后,再于上述温度条件下恒温抽真空60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.3,随后向三口烧瓶中加入无水乙醇质量2倍的水,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂;将海藻酸钠与水按质量比1:100置于1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h后,于温度为95℃,转速为500r/min条件下,加热搅拌混合2h,随后向1号烧杯中加入海藻酸钠质量2倍质量浓度为200mg/L的高碘酸钠溶液,于温度为95℃,转速为500r/min条件下,恒温搅拌混合60min,即得改性海藻酸钠液;将聚乙烯醇与水按质量比1:100加入1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为100℃,转速为500r/min条件下,加热搅拌溶解50min,即得聚乙烯醇液;按重量份数计,将40份质量分数为50%的乙二醛溶液,20份质量分数为30%的氢氧化钾溶液,40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为78℃,转速为500r/min条件下,恒温搅拌反应4h后,将四口烧瓶中温度降至62℃,再向四口烧瓶中加入乙二醛溶液体积0.3倍的乙烯脲,于温度为62℃,转速为500r/min条件下,恒温搅拌反应60min后,将四口烧瓶中温度降至52℃,接着向四口烧瓶中加入乙二醛溶液体积0.2倍的硅烷偶联剂KH-570,于温度为52℃,转速为500r/min条件下,恒温搅拌反应50min,将四口烧瓶中温度降至42℃,于温度为42℃,转速为500r/min条件下,继续恒温搅拌反应30min,即得碱性酚醛树脂;按质量比为1:12将海泡石和质量分数为20%盐酸混合倒入2号烧杯中,并将2号烧杯移入数显测速恒温磁力搅拌器,于温度为50℃,转速为500r/min条件下,恒温浸泡4h,再经过滤,得滤饼,并用去离子水洗涤滤饼5次,再将洗涤后的滤饼转入烘箱中,于温度为110℃条件下干燥至恒重,得干燥滤饼,再将所得干燥滤饼转入管式炉,于温度为240℃条件下,保温焙烧3h后,随炉冷却至室温,出料,得改性海泡石;按重量份数计,将30份水性环氧树脂,30份改性海藻酸钠液,30份聚乙烯醇液,20份氨水,20份纳米二氧化硅,20份碳酸氢钙溶液,20份碱性酚醛树脂,20份改性海泡石,20份硅烷偶联剂,8份质量浓度为2.5mg/mL多巴胺溶液,2份氯化铬置于3号烧杯中,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550。
将环氧树脂618与无水乙醇按质量比1:30置于三口烧瓶中,于转速为500r/min条件下,搅拌溶解2h后,升温至85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.6倍的二乙醇胺,于温度为85℃,转速为500r/min条件下,恒温搅拌反应3h后,再于上述温度条件下恒温抽真空60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.3,随后向三口烧瓶中加入无水乙醇质量2倍的水,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂;将聚乙烯醇与水按质量比1:100加入1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为100℃,转速为500r/min条件下,加热搅拌溶解50min,即得聚乙烯醇液;按重量份数计,将40份质量分数为50%的乙二醛溶液,20份质量分数为30%的氢氧化钾溶液,40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为78℃,转速为500r/min条件下,恒温搅拌反应4h后,将四口烧瓶中温度降至62℃,再向四口烧瓶中加入乙二醛溶液体积0.3倍的乙烯脲,于温度为62℃,转速为500r/min条件下,恒温搅拌反应60min后,将四口烧瓶中温度降至52℃,接着向四口烧瓶中加入乙二醛溶液体积0.2倍的硅烷偶联剂KH-570,于温度为52℃,转速为500r/min条件下,恒温搅拌反应50min,将四口烧瓶中温度降至42℃,于温度为42℃,转速为500r/min条件下,继续恒温搅拌反应30min,即得碱性酚醛树脂;按质量比为1:12将海泡石和质量分数为20%盐酸混合倒入2号烧杯中,并将2号烧杯移入数显测速恒温磁力搅拌器,于温度为50℃,转速为500r/min条件下,恒温浸泡4h,再经过滤,得滤饼,并用去离子水洗涤滤饼5次,再将洗涤后的滤饼转入烘箱中,于温度为110℃条件下干燥至恒重,得干燥滤饼,再将所得干燥滤饼转入管式炉,于温度为240℃条件下,保温焙烧3h后,随炉冷却至室温,出料,得改性海泡石;按重量份数计,将30份水性环氧树脂,30份聚乙烯醇液,20份氨水,20份纳米二氧化硅,20份碳酸氢钙溶液,20份碱性酚醛树脂,20份改性海泡石,20份硅烷偶联剂,8份质量浓度为2.5mg/mL多巴胺溶液,2份氯化铬置于3号烧杯中,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550。
将环氧树脂618与无水乙醇按质量比1:30置于三口烧瓶中,于转速为500r/min条件下,搅拌溶解2h后,升温至85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.6倍的二乙醇胺,于温度为85℃,转速为500r/min条件下,恒温搅拌反应3h后,再于上述温度条件下恒温抽真空60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.3,随后向三口烧瓶中加入无水乙醇质量2倍的水,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂;将海藻酸钠与水按质量比1:100置于1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h后,于温度为95℃,转速为500r/min条件下,加热搅拌混合2h,随后向1号烧杯中加入海藻酸钠质量2倍质量浓度为200mg/L的高碘酸钠溶液,于温度为95℃,转速为500r/min条件下,恒温搅拌混合60min,即得改性海藻酸钠液;将聚乙烯醇与水按质量比1:100加入1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为100℃,转速为500r/min条件下,加热搅拌溶解50min,即得聚乙烯醇液;按重量份数计,将40份质量分数为50%的乙二醛溶液,20份质量分数为30%的氢氧化钾溶液,40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为78℃,转速为500r/min条件下,恒温搅拌反应4h后,将四口烧瓶中温度降至62℃,再向四口烧瓶中加入乙二醛溶液体积0.3倍的乙烯脲,于温度为62℃,转速为500r/min条件下,恒温搅拌反应60min后,将四口烧瓶中温度降至52℃,接着向四口烧瓶中加入乙二醛溶液体积0.2倍的硅烷偶联剂KH-570,于温度为52℃,转速为500r/min条件下,恒温搅拌反应50min,将四口烧瓶中温度降至42℃,于温度为42℃,转速为500r/min条件下,继续恒温搅拌反应30min,即得碱性酚醛树脂;按质量比为1:12将海泡石和质量分数为20%盐酸混合倒入2号烧杯中,并将2号烧杯移入数显测速恒温磁力搅拌器,于温度为50℃,转速为500r/min条件下,恒温浸泡4h,再经过滤,得滤饼,并用去离子水洗涤滤饼5次,再将洗涤后的滤饼转入烘箱中,于温度为110℃条件下干燥至恒重,得干燥滤饼,再将所得干燥滤饼转入管式炉,于温度为240℃条件下,保温焙烧3h后,随炉冷却至室温,出料,得改性海泡石;按重量份数计,将30份水性环氧树脂,30份改性海藻酸钠液,30份聚乙烯醇液,20份纳米二氧化硅,20份碳酸氢钙溶液,20份碱性酚醛树脂,20份改性海泡石,20份硅烷偶联剂,8份质量浓度为2.5mg/mL多巴胺溶液,2份氯化铬置于3号烧杯中,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550。
将环氧树脂618与无水乙醇按质量比1:30置于三口烧瓶中,于转速为500r/min条件下,搅拌溶解2h后,升温至85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.6倍的二乙醇胺,于温度为85℃,转速为500r/min条件下,恒温搅拌反应3h后,再于上述温度条件下恒温抽真空60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.3,随后向三口烧瓶中加入无水乙醇质量2倍的水,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂;将海藻酸钠与水按质量比1:100置于1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h后,于温度为95℃,转速为500r/min条件下,加热搅拌混合2h,随后向1号烧杯中加入海藻酸钠质量2倍质量浓度为200mg/L的高碘酸钠溶液,于温度为95℃,转速为500r/min条件下,恒温搅拌混合60min,即得改性海藻酸钠液;将聚乙烯醇与水按质量比1:100加入1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为100℃,转速为500r/min条件下,加热搅拌溶解50min,即得聚乙烯醇液;按重量份数计,将40份质量分数为50%的乙二醛溶液,20份质量分数为30%的氢氧化钾溶液,40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为78℃,转速为500r/min条件下,恒温搅拌反应4h后,将四口烧瓶中温度降至62℃,再向四口烧瓶中加入乙二醛溶液体积0.3倍的乙烯脲,于温度为62℃,转速为500r/min条件下,恒温搅拌反应60min后,将四口烧瓶中温度降至52℃,接着向四口烧瓶中加入乙二醛溶液体积0.2倍的硅烷偶联剂KH-570,于温度为52℃,转速为500r/min条件下,恒温搅拌反应50min,将四口烧瓶中温度降至42℃,于温度为42℃,转速为500r/min条件下,继续恒温搅拌反应30min,即得碱性酚醛树脂;按质量比为1:12将海泡石和质量分数为20%盐酸混合倒入2号烧杯中,并将2号烧杯移入数显测速恒温磁力搅拌器,于温度为50℃,转速为500r/min条件下,恒温浸泡4h,再经过滤,得滤饼,并用去离子水洗涤滤饼5次,再将洗涤后的滤饼转入烘箱中,于温度为110℃条件下干燥至恒重,得干燥滤饼,再将所得干燥滤饼转入管式炉,于温度为240℃条件下,保温焙烧3h后,随炉冷却至室温,出料,得改性海泡石;按重量份数计,将30份水性环氧树脂,30份改性海藻酸钠液,30份聚乙烯醇液,20份氨水,20份纳米二氧化硅,20份碱性酚醛树脂,20份改性海泡石,20份硅烷偶联剂,8份质量浓度为2.5mg/mL多巴胺溶液,2份氯化铬置于3号烧杯中,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550。
将环氧树脂618与无水乙醇按质量比1:30置于三口烧瓶中,于转速为500r/min条件下,搅拌溶解2h后,升温至85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.6倍的二乙醇胺,于温度为85℃,转速为500r/min条件下,恒温搅拌反应3h后,再于上述温度条件下恒温抽真空60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.3,随后向三口烧瓶中加入无水乙醇质量2倍的水,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂;将海藻酸钠与水按质量比1:100置于1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h后,于温度为95℃,转速为500r/min条件下,加热搅拌混合2h,随后向1号烧杯中加入海藻酸钠质量2倍质量浓度为200mg/L的高碘酸钠溶液,于温度为95℃,转速为500r/min条件下,恒温搅拌混合60min,即得改性海藻酸钠液;将聚乙烯醇与水按质量比1:100加入1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为100℃,转速为500r/min条件下,加热搅拌溶解50min,即得聚乙烯醇液;按重量份数计,将40份质量分数为50%的乙二醛溶液,20份质量分数为30%的氢氧化钾溶液,40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为78℃,转速为500r/min条件下,恒温搅拌反应4h后,将四口烧瓶中温度降至62℃,再向四口烧瓶中加入乙二醛溶液体积0.3倍的乙烯脲,于温度为62℃,转速为500r/min条件下,恒温搅拌反应60min后,将四口烧瓶中温度降至52℃,接着向四口烧瓶中加入乙二醛溶液体积0.2倍的硅烷偶联剂KH-570,于温度为52℃,转速为500r/min条件下,恒温搅拌反应50min,将四口烧瓶中温度降至42℃,于温度为42℃,转速为500r/min条件下,继续恒温搅拌反应30min,即得碱性酚醛树脂;按重量份数计,将30份水性环氧树脂,30份改性海藻酸钠液,30份聚乙烯醇液,20份氨水,20份纳米二氧化硅,20份碳酸氢钙溶液,20份碱性酚醛树脂,20份硅烷偶联剂,8份质量浓度为2.5mg/mL多巴胺溶液,2份氯化铬置于3号烧杯中,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550。
将环氧树脂618与无水乙醇按质量比1:30置于三口烧瓶中,于转速为500r/min条件下,搅拌溶解2h后,升温至85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.6倍的二乙醇胺,于温度为85℃,转速为500r/min条件下,恒温搅拌反应3h后,再于上述温度条件下恒温抽真空60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.3,随后向三口烧瓶中加入无水乙醇质量2倍的水,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂;将海藻酸钠与水按质量比1:100置于1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h后,于温度为95℃,转速为500r/min条件下,加热搅拌混合2h,随后向1号烧杯中加入海藻酸钠质量2倍质量浓度为200mg/L的高碘酸钠溶液,于温度为95℃,转速为500r/min条件下,恒温搅拌混合60min,即得改性海藻酸钠液;将聚乙烯醇与水按质量比1:100加入1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为100℃,转速为500r/min条件下,加热搅拌溶解50min,即得聚乙烯醇液;按重量份数计,将40份质量分数为50%的乙二醛溶液,20份质量分数为30%的氢氧化钾溶液,40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为78℃,转速为500r/min条件下,恒温搅拌反应4h后,将四口烧瓶中温度降至62℃,再向四口烧瓶中加入乙二醛溶液体积0.3倍的乙烯脲,于温度为62℃,转速为500r/min条件下,恒温搅拌反应60min后,将四口烧瓶中温度降至52℃,接着向四口烧瓶中加入乙二醛溶液体积0.2倍的硅烷偶联剂KH-570,于温度为52℃,转速为500r/min条件下,恒温搅拌反应50min,将四口烧瓶中温度降至42℃,于温度为42℃,转速为500r/min条件下,继续恒温搅拌反应30min,即得碱性酚醛树脂;按质量比为1:12将海泡石和质量分数为20%盐酸混合倒入2号烧杯中,并将2号烧杯移入数显测速恒温磁力搅拌器,于温度为50℃,转速为500r/min条件下,恒温浸泡4h,再经过滤,得滤饼,并用去离子水洗涤滤饼5次,再将洗涤后的滤饼转入烘箱中,于温度为110℃条件下干燥至恒重,得干燥滤饼,再将所得干燥滤饼转入管式炉,于温度为240℃条件下,保温焙烧3h后,随炉冷却至室温,出料,得改性海泡石;按重量份数计,将30份水性环氧树脂,30份改性海藻酸钠液,30份聚乙烯醇液,20份氨水,20份纳米二氧化硅,20份碳酸氢钙溶液,20份碱性酚醛树脂,20份改性海泡石,20份硅烷偶联剂,2份氯化铬置于3号烧杯中,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550。
将环氧树脂618与无水乙醇按质量比1:30置于三口烧瓶中,于转速为500r/min条件下,搅拌溶解2h后,升温至85℃条件下,并用胶头滴管向三口烧瓶中滴加环氧树脂618质量0.6倍的二乙醇胺,于温度为85℃,转速为500r/min条件下,恒温搅拌反应3h后,再于上述温度条件下恒温抽真空60min,随后向三口烧瓶中滴加冰醋酸调节pH至7.3,随后向三口烧瓶中加入无水乙醇质量2倍的水,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂;将海藻酸钠与水按质量比1:100置于1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h后,于温度为95℃,转速为500r/min条件下,加热搅拌混合2h,随后向1号烧杯中加入海藻酸钠质量2倍质量浓度为200mg/L的高碘酸钠溶液,于温度为95℃,转速为500r/min条件下,恒温搅拌混合60min,即得改性海藻酸钠液;将聚乙烯醇与水按质量比1:100加入1号烧杯中,用玻璃棒搅拌混合30min后,静置溶胀4h,再将1号烧杯移入数显测速恒温磁力搅拌器,于温度为100℃,转速为500r/min条件下,加热搅拌溶解50min,即得聚乙烯醇液;按重量份数计,将40份质量分数为50%的乙二醛溶液,20份质量分数为30%的氢氧化钾溶液,40份对苯二酚置于四口烧瓶中,并将四口烧瓶置于数显测速恒温磁力搅拌器中,于温度为78℃,转速为500r/min条件下,恒温搅拌反应4h后,将四口烧瓶中温度降至62℃,再向四口烧瓶中加入乙二醛溶液体积0.3倍的乙烯脲,于温度为62℃,转速为500r/min条件下,恒温搅拌反应60min后,将四口烧瓶中温度降至52℃,接着向四口烧瓶中加入乙二醛溶液体积0.2倍的硅烷偶联剂KH-570,于温度为52℃,转速为500r/min条件下,恒温搅拌反应50min,将四口烧瓶中温度降至42℃,于温度为42℃,转速为500r/min条件下,继续恒温搅拌反应30min,即得碱性酚醛树脂;按质量比为1:12将海泡石和质量分数为20%盐酸混合倒入2号烧杯中,并将2号烧杯移入数显测速恒温磁力搅拌器,于温度为50℃,转速为500r/min条件下,恒温浸泡4h,再经过滤,得滤饼,并用去离子水洗涤滤饼5次,再将洗涤后的滤饼转入烘箱中,于温度为110℃条件下干燥至恒重,得干燥滤饼,再将所得干燥滤饼转入管式炉,于温度为240℃条件下,保温焙烧3h后,随炉冷却至室温,出料,得改性海泡石;按重量份数计,将30份水性环氧树脂,30份改性海藻酸钠液,30份聚乙烯醇液,20份氨水,20份纳米二氧化硅,20份碳酸氢钙溶液,20份碱性酚醛树脂,20份改性海泡石,20份硅烷偶联剂,8份质量浓度为2.5mg/mL多巴胺溶液置于3号烧杯中,于转速为500r/min条件下,搅拌混合60min,即得水性环氧树脂碳纤维上浆剂。所述硅烷偶联剂为硅烷偶联剂KH-550。
对比例:武汉某新材料科技有限公司生产的上浆剂。
将实例1至7所得上浆剂和对比例产品进行性能检测,具体检测方法如下:
剪切强度按照JC/T773进行测定,摩擦系数依据《碳纤维与石墨纤维》摩擦系数测定方法测定。具体检测结果如表1所示:
表1:性能检测表
检测内容 | 实例1 | 实例2 | 实例3 | 实例4 | 实例5 | 实例6 | 实例7 | 对比例 |
剪切强度/MPa | 92.6 | 89 | 88.4 | 88.8 | 89.3 | 88.5 | 89.1 | 85.5 |
摩擦系数 | 0.249 | 0.226 | 0.231 | 0.224 | 0.228 | 0.234 | 0.225 | 0.205 |
由表1检测结果可知,本发明所得水性环氧树脂碳纤维上浆剂具有优异的抗剪切强度和耐磨性能。
Claims (7)
1.一种水性环氧树脂碳纤维上浆剂,其特征在于:是由以下重量份数的原料组成:
水性环氧树脂 20~30份
改性海藻酸钠液 20~30份
聚乙烯醇液 20~30份
氨水 10~20份
纳米二氧化硅 10~20份
碳酸氢钙溶液 10~20份
碱性酚醛树脂 10~20份
改性海泡石 10~20份
硅烷偶联剂 10~20份
多巴胺溶液 5~8份
氯化铬 1~2份
所述水性环氧树脂碳纤维上浆剂的制备过程为:按原料组成称量各原料,将水性环氧树脂,改性海藻酸钠液,聚乙烯醇液,氨水,纳米二氧化硅,碳酸氢钙溶液,碱性酚醛树脂,改性海泡石,硅烷偶联剂,多巴胺溶液和氯化铬搅拌混合,即得水性环氧树脂碳纤维上浆剂。
2.根据权利要求1所述一种水性环氧树脂碳纤维上浆剂,其特征在于:所述水性环氧树脂的制备过程为:将环氧树脂618与无水乙醇按质量比1:20~1:30搅拌溶解后,升温,滴加环氧树脂618质量0.5~0.6倍的二乙醇胺,恒温搅拌反应,恒温抽真空,调节pH,随后加入无水乙醇质量1~2倍的水,搅拌混合,即得水性环氧树脂。
3.根据权利要求1所述一种水性环氧树脂碳纤维上浆剂,其特征在于:所述改性海藻酸钠的制备过程为:将海藻酸钠与水按质量比1:50~1:100混合,静置溶胀后,加热搅拌混合,随后加入海藻酸钠质量0.4~0.5倍的高碘酸钠溶液,继续加热搅拌混合,即得改性海藻酸钠液。
4.根据权利要求1所述一种水性环氧树脂碳纤维上浆剂,其特征在于:所述聚乙烯醇液的制备过程为:将聚乙烯醇与水按质量比1:50~1:100混合,静置溶胀,加热搅拌混合,即得聚乙烯醇液。
5.根据权利要求1所述一种水性环氧树脂碳纤维上浆剂,其特征在于:所述碱性酚醛树脂的制备过程为:按重量份数计,将30~40份乙二醛溶液,10~20份氢氧化钾溶液,30~40份对苯二酚恒温搅拌反应,降温,加入乙二醛溶液体积0.2~0.3倍的乙烯脲搅拌反应,降温,加入乙二醛溶液体积0.1~0.2倍的硅烷偶联剂KH-570搅拌反应,降温,即得碱性酚醛树脂。
6.根据权利要求1所述一种水性环氧树脂碳纤维上浆剂,其特征在于:所述改性海泡石的制备过程为:将海泡石用盐酸恒温浸泡后,过滤,洗涤,干燥,焙烧,得改性海泡石。
7.根据权利要求1所述一种水性环氧树脂碳纤维上浆剂,其特征在于:所述硅烷偶联剂为硅烷偶联剂KH-550,硅烷偶联剂KH-560或硅烷偶联剂KH-570中的任意一种。
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