CN106751474B - 利用改性介孔sba-15制备自修复环氧树脂复合材料的方法 - Google Patents
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Abstract
本发明公开了一种利用改性介孔材料SBA‑15制备自修复复合材料的方法。用不同硅烷偶联剂对盐酸酸化的介孔SBA‑15进行表面改性;随后取双环戊二烯和苯乙烯单体混合物(DS液)加入到改性介孔材料SBA‑15中,饱和吸附2小时,过滤除去多余的DS液;将饱和吸附DS液的改性介孔材料加入到环氧树脂E51、固化剂二乙烯三胺和Grubbs催化剂的混合液中,手工混合后超声振动,待抽真空至无气泡,固化后得到具有多次自修复功能的环氧树脂复合材料。本发明对延长聚合物基复合材料的使用寿命,改善了复合材料的使用性能和安全性,使其在军工航天、电子电器以及建筑建材等领域有着极其重要的应用价值。
Description
技术领域
本发明所属技术领域为聚合物基复合材料自修复领域,利用饱和吸附修复剂的改性介孔材料制备环氧树脂/ SBA-15自修复材料。
背景技术
介孔材料SBA-15是一种具有高度有序二维六方结构孔道的多孔材料,在介孔材料表面具有大量的硅羟基,但是这种硅羟基几乎不具有活性,与树脂基体相容性差,使介孔材料在各方面的应用上受到很大的限制。为了解决这一问题,同时保持其自身的优越性能的基础上,需要对介孔材料进行表面活化改性,扩大介孔SBA-15在吸附、分离、催化和载体等方面的应用。
由于活化后的介孔SBA-15表面具有大量的活性位点,可以使其进行各种有目的的化学改性,此优点为制备具有特定性能的复合介孔材料提供了可能。改性介孔材料表面所覆有硅烷偶联剂中非水解官能团与有机材料的化学性质是决定复合材料最佳性能的重要条件。而适合的硅烷偶联剂可以使介孔材料SBA-15吸附修复剂双环戊二烯(DCPD)的能力增强、与环氧树脂基材的相容性提高,同时增加复合材料的拉伸强度。当基体产生微裂纹时,改性介孔材料吸附的修复剂通过虹吸作用与断裂面的Grubbs催化剂接触,进而引发开环位移聚合反应(ROMP),生成聚合物而修复微裂纹。由于改性介孔SBA-15独特的结构,使其在基体中可进行多次释放,从而实现多次自修复,进一步增加了复合材料的使用期限。
发明内容
为了有效解决基体材料内部或表面产生局部损伤及微裂纹、使用介孔材料在基体中的分散性不理想及自修复系统很难进行多次有效自修复的问题,本发明提供一种利用饱和吸附愈合剂的改性介孔材料SBA-15在聚合物基体中的缓释功能,得到能够有效进行多次自修复的方法。
具体步骤为:
(1)将5~10质量份浓度为2 mol/L的盐酸加入到1质量份的介孔SBA-15进行酸化后,再加入1~5质量份的硅烷偶联剂进行表面改性,得到改性介孔材料SBA-15备用。
(2)将1~10质量份的双环戊二烯(DCPD)和苯乙烯按体积比9:1混合,得单体混合物即DS液。
(3)将1质量份步骤(1)所得改性介孔材料SBA-15加入到步骤(2)中所得DS液中,饱和吸附2小时,过滤除去多余的DS液。
(4)将100质量份环氧树脂E51、10质量份固化剂二乙烯三胺(DETA)和0.01~1质量份Grubbs催化剂混合得混合液。
(5)将10~100质量份步骤(3)所得饱和吸附DS液的改性介孔材料加入到步骤(4)所得混合液中,手工混合后超声振动,使之混合均匀后,待抽真空至无气泡,倒入模具中,固化后得到具有多次自修复功能的环氧树脂复合材料。
所述硅烷偶联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷中的一种或多种。
所述原材料均为工业级。
本发明具有以下特点:
1.原料来源广泛,易处理。
2.操作简单,误差相对较小。
3.介孔材料有更好的分散性,所得修复率较高,可多次自修复。
具体实施方式
以下所述原材料均为工业级。
实施例1:
(1)将3.0 g介孔SBA-15与11 mL浓度为 2.0 mol/L的盐酸混合均匀,室温酸化;取1.0 g酸化后的介孔SBA-15与2.5 mL的硅烷偶联剂乙烯基三乙氧基硅烷(KH151)混合均匀,氮气氛围下80 ℃反应11小时,得到改性介孔材料KH151-S。
(2)取1.68 g的双环戊二烯(DCPD)和苯乙烯得单体混合物即DS液,双环戊二烯(DCPD)和苯乙烯体积比为9:1。
(3)将0.30 g步骤(1)所得改性介孔材料KH550-S加入到步骤(2)所得DS液中,饱和吸附2 小时,过滤除去多余的DS液。
(4)将6.0 g环氧树脂E51、0.6 g固化剂二乙烯三胺(DETA)和0.0067 g Grubbs催化剂混合得混合液。
(5)将步骤(3)所得饱和吸附DS液的改性介孔材料加入到步骤(4)所得混合液中,手工混合后超声振动,使之混合均匀后,待抽真空至无气泡,倒入模具中,固化后得到一次修复率为68.7 %左右的环氧树脂复合材料,其二次、三次修复率可分别达到65.1 %和58.4%。
实施例2:
(1)将3.0 g介孔SBA-15与11 ml 2.0 mol/L的盐酸混合均匀,室温酸化;取1.0 g酸化后的介孔SBA-15与2.5 mL的硅烷偶联剂γ―(2,3-环氧丙氧) 丙基三甲氧基硅烷(KH560)混合均匀,氮气氛围下80 ℃反应11小时,得到改性介孔材料KH560-S。
(2)取1.59 g的双环戊二烯(DCPD)和苯乙烯混合得单体混合物即DS液,双环戊二烯(DCPD)和苯乙烯体积比为9:1。
(3)将0.30 g改性介孔材料KH560-S加入到步骤(2)所得DS液中,饱和吸附2小时,过滤除去多余的DS液。
(4)将6.0 g环氧树脂E51、0.6 g固化剂DETA和0.0064 g Grubbs催化剂混合得混合液。
(5)将步骤(3)所得饱和吸附DS液的改性介孔材料加入到步骤(4)所得混合液中,手工混合后超声振动,使之混合均匀后,待抽真空至无气泡,倒入模具中,固化后得到具有多次自修复功能的环氧树脂复合材料,其一次、二次和三次修复率最高可达到70.0 %、62.5%、55.7 %。
实施例3:
(1)将3.0 g介孔SBA-15与11 mL浓度为2.0 mol/L的盐酸混合均匀,室温酸化;取1.0 g酸化后的介孔SBA-15与2.5 mL的硅烷偶联剂γ-(甲基丙烯酰氧)丙基三甲氧基硅烷(KH570)混合均匀,氮气氛围下80 ℃反应11小时,得到改性介孔材料KH570-S。
(2)取1.73 g的双环戊二烯(DCPD)和苯乙烯得单体混合物即DS液,双环戊二烯(DCPD)和苯乙烯体积比为9:1。
(3)将0.30 g步骤(1)所得改性介孔材料KH570-S加入到步骤(2)所得DS液中,饱和吸附2 小时,过滤除去多余的DS液。
(4)将6.0 g环氧树脂E51、0.6 g固化剂DETA和0.0069 g Grubbs催化剂混合得混合液。
(5)将步骤(3)所得饱和吸附DS液的改性介孔材料加入到步骤(4)所得混合液中,手工混合后超声振动,使之混合均匀后,待抽真空至无气泡,倒入模具中,固化后得到具有多次自修复功能的环氧树脂复合材料,其一次、二次和三次修复率最高可达到71.9 %、65.1%、58.2 %。
Claims (1)
1.一种利用改性介孔材料SBA-15制备自修复环氧树脂复合材料的方法,其特征在于具体步骤为:
(1)将5~10质量份浓度为2 mol/L的盐酸加入到1质量份的介孔SBA-15进行酸化后,再加入1~5质量份的硅烷偶联剂进行表面改性,得到改性介孔材料SBA-15备用;
(2)将1~10质量份的双环戊二烯和苯乙烯按体积比9:1混合,得单体混合物即DS液;
(3)将1质量份步骤(1)所得改性介孔材料SBA-15加入到步骤(2)中所得DS液中,饱和吸附2小时,过滤除去多余的DS液;
(4)将100质量份环氧树脂E51、10质量份固化剂二乙烯三胺和0.01~1质量份Grubbs催化剂混合得混合液;
(5)将10~100质量份步骤(3)所得饱和吸附DS液的改性介孔材料加入到步骤(4)所得混合液中,手工混合后超声振动,使之混合均匀后,待抽真空至无气泡,倒入模具中,固化后得到具有多次自修复功能的环氧树脂复合材料;
所述硅烷偶联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷中的一种或多种;
所述原材料均为工业级。
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Application publication date: 20170531 Assignee: Guangxi Aigui Intelligent Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044282 Denomination of invention: Method for preparing self-healing epoxy resin composite materials using modified mesoporous SBA-15 Granted publication date: 20181106 License type: Common License Record date: 20231025 |