CN106554521A - 一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料及其制备方法 - Google Patents

一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料及其制备方法 Download PDF

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CN106554521A
CN106554521A CN201610913338.5A CN201610913338A CN106554521A CN 106554521 A CN106554521 A CN 106554521A CN 201610913338 A CN201610913338 A CN 201610913338A CN 106554521 A CN106554521 A CN 106554521A
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吴传兴
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Maanshan Jiechuang Plastic Science & Technology Co Ltd
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Abstract

本发明公开了一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料及其制备工艺，其特征在于，以丁二烯（聚合级）、环烷油、环烷酸镍、三异丁基铝、三氟化硼乙醚络合物、辛醛、聚己内酯二元醇、石墨、抗氧剂TNP、紫外线吸收剂UV‑9、甲苯二异氰酸酯、二甲硫基甲苯二胺、多壁碳纳米管、二甲基甲酰胺、十二烷基苯磺酸钠、四氯化硅、双环戊二烯树脂、尼龙、双酚A型环氧树脂等为原料。本发明通过预聚体法制备了耐水解聚氨酯弹性体，石墨与聚氨酯基体发生了插层聚合且在基体中的分散性良好；制备了表面含有胺基官能团的多壁碳纳米管，改善了与尼龙之间的相容性，提高了在尼龙基体中的分散性；得到一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料。

Description

一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料及其制 备方法
技术领域
本发明涉及高分子材料加工技术，具体涉及一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料，及其制备工艺。
背景技术
聚丁二烯橡胶具有高拉伸强度、高撕裂强度、高耐磨性等众多优异的性能特征。尼龙具有良好的综合性能，包括力学性能、耐热性、耐磨损性、耐化学药品性和自润滑性，且摩擦系数低，有一定的阻燃性，易于加工。
赵永兵在其硕士论文《充油顺丁橡胶工艺技术的研究与发展》中，配制丁二烯与溶剂油（加氢汽油；填充油：环烷油）的混合物，放入恒温水浴，加热至聚合温度70℃，用针管将配制好的催化剂（环烷酸镍和三异丁基铝混合，陈化；三氟化硼乙醚络合物和辛醛先按一定比例配好，并稀释至500-1000倍）加入其中，搅拌使其充分混匀，待釜内温度稳定后搅拌2h充油完成，再将充油顺丁橡胶胶液经水蒸气凝聚后，用开炼机干燥。但用于高压油管存在耐腐蚀性不足。
本发明以聚己内酯二元醇、甲苯二异氰酸酯和二甲硫基甲苯二胺为原材料，以石墨为填料，通过预聚体法制备了耐水解聚氨酯弹性体，石墨与聚氨酯基体发生了插层聚合且在基体中的分散性良好；制备了分散均匀、表面含有胺基官能团的多壁碳纳米管，改善了与尼龙之间的相容性，提高了在尼龙基体中的分散性；
通过调节催化剂配比合成高门尼粘度基础胶；在预聚体固化剂中掺入环氧树脂，制备了环氧树脂改性的聚氨酯弹性体，弹性体中存在噁唑烷酮结构，提高了弹性体的热分解温度和耐热性能；得到一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料。
发明内容
本发明主要解决的技术问题是提供一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料及其制备工艺，依照该工艺制作的汽车吸塑材料具有耐磨、耐油、耐撕裂、回弹力好、耐化学腐蚀等优良性能。
本发明所要解决的技术问题采用以下的技术方案来实现：
丁二烯（聚合级）20-28，环烷油10-19，环烷酸镍3-5，三异丁基铝4-7，三氟化硼乙醚络合物3-6，辛醛2-4，聚己内酯二元醇2-3，石墨1-3，抗氧剂TNP 0.5-1.5，紫外线吸收剂UV-90.1-0.2，甲苯二异氰酸酯1-2，二甲硫基甲苯二胺1-3，2,4,6-三(二甲氨基甲基)苯酚2-4，扩链剂BDO 1-2，双酚A型环氧树脂E-51 4-8，多壁碳纳米管1-3，二甲基甲酰胺1-2，乙二胺1-2，十二烷基苯磺酸钠2-4，四氯化硅1-3，双环戊二烯树脂3-5，尼龙5-9，SOCl2、四氢呋喃、乙醇、环己烷适量。
一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料的制备方法，其特征在于，按以下步骤进行：
a. 将聚己内酯二元醇和石墨混合搅拌1-2h，升温到100-140℃真空脱水1-2h，降温至40-50℃后，快速搅拌下加入抗氧剂TNP、紫外线吸收剂UV-9、甲苯二异氰酸酯，在70-90℃下反应1-3h，真空脱泡1-2h，再加热至80-90℃，加入二甲硫基甲苯二胺，迅速搅拌均匀，待用；
b. 将a中所得物料预热至70-80℃，在快速搅拌下加入2,4,6-三(二甲氨基甲基)苯酚、扩链剂BDO及双酚A型环氧树脂E-51，迅速搅拌5-10min，浇注到预热至140 -160℃并涂有脱模剂的平板模具中，待凝胶后，合上模具，在5-10 MPa 下加压硫化1-2 h后脱模，并在110 -130℃的烘箱中后硫化2-4h，即制得环氧树脂改性聚氨酯弹性体；
c. 向多壁碳纳米管中以20:1-2加入SOCl2和二甲基甲酰胺，于60-90℃的水浴中恒温加热搅拌2-4h，与乙二胺混合，在恒温130-170℃油浴下搅拌1-2h，用四氢呋喃和乙醇洗涤3-5次，过滤，将滤饼在70-90℃下真空干燥2-5h后，待用；
d. 将十二烷基苯磺酸钠、环烷酸镍、三异丁基铝混合，于50-90℃恒温加热磁力搅拌，反应2-3h后，加入三氟化硼乙醚络合物、辛醛、四氯化硅进行偶联1-2h，用乙醇洗涤3-5次，过滤，将产物先于通风橱中风干，再置于50-80℃的真空干燥箱中，干燥至恒重；
e. 将丁二烯与环烷油混合，加入双环戊二烯树脂的环己烷溶液，放入恒温水浴，加热至聚合温度70-90℃，用针管将d中所得催化剂加入其中，搅拌使其充分混匀，温度稳定为60-80℃搅拌2-4h充油完成，再将充油顺丁橡胶胶液经水蒸气凝聚后，在110-140℃滚筒上滚干；
f. 将b、c、e中所得物料及其他剩余成分混合均匀，加入双螺杆挤出机内，
于230-260℃、50-120r/min 熔融共混，挤出造粒，即得到一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料。
本发明的反应机理及有益效果如下：
（1）以聚己内酯二元醇、甲苯二异氰酸酯和二甲硫基甲苯二胺为原材料，以石墨为填料，通过预聚体法制备了耐水解聚氨酯弹性体，石墨与聚氨酯基体发生了插层聚合且在基体中的分散性良好，复合材料具有优异的耐磨、耐油、耐撕裂、回弹力好、耐化学腐蚀等特性，从而延长了油管的使用寿命。
（2）在预聚体固化剂中掺入环氧树脂，制备了环氧树脂改性的聚氨酯弹性体，弹性体中存在噁唑烷酮结构，提高了弹性体的热分解温度和耐热性能。
（3）对多壁碳纳米管进行胺化处理，在其表面接枝了胺基官能团，制备了分散均匀、表面含有胺基官能团的多壁碳纳米管，改善了与尼龙之间的相容性，提高了在尼龙基体中的分散性。
（4）以十二烷基苯磺酸钠、环烷酸镍、三异丁基铝、三氟化硼乙醚络合物、辛醛、四氯化硅制备新型催化剂，调节催化剂配比合成高门尼粘度基础胶；使高门尼基础胶生产简便易行、控制灵活，门尼粘度高，充油性好，性能稳定。
（5）尼龙具有良好的综合性能，包括力学性能、耐热性、耐磨损性、耐化学药品性和自润滑性，且摩擦系数低，有一定的阻燃性，易于加工；聚丁二烯橡胶具有高拉伸强度、高撕裂强度、高耐磨性等众多优异的性能特征。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例
一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料，由下述重量份(g)的原料制得：
丁二烯（聚合级）28，环烷油19，环烷酸镍5，三异丁基铝7，三氟化硼乙
醚络合物3，辛醛2，聚己内酯二元醇3，石墨1，抗氧剂TNP 0.5，紫外线吸收剂UV-9 0.1，甲苯二异氰酸酯2，二甲硫基甲苯二胺3，2,4,6-三(二甲氨基甲基)苯酚4，扩链剂BDO 1，双酚A型环氧树脂E-51 8，多壁碳纳米管3，二甲基甲酰胺1，乙二胺1，十二烷基苯磺酸钠4，四氯化硅1，双环戊二烯树脂3，尼龙9，SOCl2、四氢呋喃、乙醇、环己烷适量。
一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料的制备方法，其特征在于，按以下步骤进行：
a. 将聚己内酯二元醇和石墨混合搅拌1h，升温到130-140℃真空脱水1h，降温至40-50℃后，快速搅拌下加入抗氧剂TNP、紫外线吸收剂UV-9、甲苯二异氰酸酯，在70-80℃下反应1h，真空脱泡1h，再加热至80-90℃，加入二甲硫基甲苯二胺，迅速搅拌均匀，待用；
b. 将a中所得物料预热至70-80℃，在快速搅拌下加入2,4,6-三(二甲氨基甲基)苯酚、扩链剂BDO及双酚A型环氧树脂E-51，迅速搅拌10min，浇注到预热至150 -160℃并涂有脱模剂的平板模具中，待凝胶后，合上模具，在10 MPa 下加压硫化2h后脱模，并在120 -130℃的烘箱中后硫化2h，即制得环氧树脂改性聚氨酯弹性体；
c. 向多壁碳纳米管中以20:1加入SOCl2和二甲基甲酰胺，于60-70℃的水浴中恒温加热搅拌2h，与乙二胺混合，在恒温160-170℃油浴下搅拌1h，用四氢呋喃和乙醇洗涤3次，过滤，将滤饼在80-90℃下真空干燥2h后，待用；
d. 将十二烷基苯磺酸钠、环烷酸镍、三异丁基铝混合，于70-80℃恒温加热磁力搅拌，反应2h后，加入三氟化硼乙醚络合物、辛醛、四氯化硅进行偶联1h，用乙醇洗涤5次，过滤，将产物先于通风橱中风干，再置于70-80℃的真空干燥箱中，干燥至恒重；
e. 将丁二烯与环烷油混合，加入双环戊二烯树脂的环己烷溶液，放入恒温水浴，加热至聚合温度70-80℃，用针管将d中配制好的催化剂加入其中，搅拌使其充分混匀，温度稳定为60-70℃搅拌4h充油完成，再将充油顺丁橡胶胶液经水蒸气凝聚后，在110-120℃滚筒上滚干；
f. 将b、c、e中所得物料及其他剩余成分混合均匀，加入双螺杆挤出机内，
于250-260℃、90-120r/min 熔融共混，挤出造粒，即得到一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料。
上述实施例制备的一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料的性能检测结果如下所示：
拉伸强度9MPa，断裂生长率183%；
热老化试验(160℃，200h)：拉伸强度变化率11.3%，断裂伸长率变化率11.8%；
耐矿物油实验(80℃，200h)：拉伸强度变化率10.9%，断裂伸长率变化率12.6%。

Claims (2)

1.一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料，其特征在于，由下述重量份的原料制得：
丁二烯（聚合级）20-28，环烷油10-19，环烷酸镍3-5，三异丁基铝4-7，三
氟化硼乙醚络合物3-6，辛醛2-4，聚己内酯二元醇2-3，石墨1-3，抗氧剂TNP 0.5-1.5，紫外线吸收剂UV-9 0.1-0.2，甲苯二异氰酸酯1-2，二甲硫基甲苯二胺1-3，2,4,6-三(二甲氨基甲基)苯酚2-4，扩链剂BDO 1-2，双酚A型环氧树脂E-51 4-8，多壁碳纳米管1-3，二甲基甲酰胺1-2，乙二胺1-2，十二烷基苯磺酸钠2-4，四氯化硅1-3，双环戊二烯树脂3-5，尼龙5-9，SOCl2、四氢呋喃、乙醇、环己烷适量。
2.根据权利要求1所述的一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料的制备方法，其特征在于，按以下步骤进行：
a. 将聚己内酯二元醇和石墨混合搅拌1-2h，升温到100-140℃真空脱水1-2h，降温至40-50℃后，快速搅拌下加入抗氧剂TNP、紫外线吸收剂UV-9、甲苯二异氰酸酯，在70-90℃下反应1-3h，真空脱泡1-2h，再加热至80-90℃，加入二甲硫基甲苯二胺，迅速搅拌均匀，待用；
b. 将a中所得物料预热至70-80℃，在快速搅拌下加入2,4,6-三(二甲氨基甲基)苯酚、扩链剂BDO及双酚A型环氧树脂E-51，迅速搅拌5-10min，浇注到预热至140 -160℃并涂有脱模剂的平板模具中，待凝胶后，合上模具，在5-10 MPa 下加压硫化1-2 h后脱模，并在110 -130℃的烘箱中后硫化2-4h，即制得环氧树脂改性聚氨酯弹性体；
c. 向多壁碳纳米管中以20:1-2加入SOCl2和二甲基甲酰胺，于60-90℃的水浴中恒温加热搅拌2-4h，与乙二胺混合，在恒温130-170℃油浴下搅拌1-2h，用四氢呋喃和乙醇洗涤3-5次，过滤，将滤饼在70-90℃下真空干燥2-5h后，待用；
d. 将十二烷基苯磺酸钠、环烷酸镍、三异丁基铝混合，于50-90℃恒温加热磁力搅拌，反应2-3h后，加入三氟化硼乙醚络合物、辛醛、四氯化硅进行偶联1-2h，用乙醇洗涤3-5次，过滤，将产物先于通风橱中风干，再置于50-80℃的真空干燥箱中，干燥至恒重；
e. 将丁二烯与环烷油混合，加入双环戊二烯树脂的环己烷溶液，放入恒温水浴，加热至聚合温度70-90℃，用针管将d中所得催化剂加入其中，搅拌使其充分混匀，温度稳定为60-80℃搅拌2-4h充油完成，再将充油顺丁橡胶胶液经水蒸气凝聚后，在110-140℃滚筒上滚干；
f. 将b、c、e中所得物料及其他剩余成分混合均匀，加入双螺杆挤出机内，
于230-260℃、50-120r/min 熔融共混，挤出造粒，即得到一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料。
CN201610913338.5A 2016-10-20 2016-10-20 一种环氧树脂改性的用于高压油管的耐油耐腐蚀材料及其制备方法 Withdrawn CN106554521A (zh)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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