CN110845682B - 一种改性三聚氰胺硬质发泡材料及其制备方法 - Google Patents
一种改性三聚氰胺硬质发泡材料及其制备方法 Download PDFInfo
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Abstract
本发明属于高分子材料技术领域,具体公开了一种改性三聚氰胺硬质发泡材料及其制备方法,由以下重量份数的原料组成:三聚氰胺30~60份,多聚甲醛15~40份,水10~35份,异丁醇5~20份,苯并噁嗪3~10份,聚乙烯醇缩丁醛5~15份,制备得到的三聚氰胺硬质发泡材料具有掉粉率低、闭孔率高、高强度、韧性好、后加工处理与基体粘结强度大的特点。
Description
技术领域
本发明属于高分子材料技术领域,尤其涉及一种改性三聚氰胺硬质发泡材料及其制备方法。
背景技术
三聚氰胺硬质发泡材料是近年来发展起来的外墙外保温领域的一种新型材料,与聚氨酯、聚苯乙烯、酚醛树脂等其它硬质保温材料相比,在不添加其它阻燃剂的情况下即能达到阻燃效果,具有导热系数低、质轻、低烟、环保等特性;但三聚氰胺树脂合成及发泡过程中各种组分、参数控制要求比较严格,组分复杂、条件多变造成产品品质稳定性不是很好,而三聚氰胺所固有的三嗪环结构使得发泡材料易脆、掉粉率高、与基体粘结强度不够,同时也不能满足对使用强度要求较高的场所。
发明内容
本发明的目的是提供一种改性三聚氰胺硬质发泡材料及其制备方法,制备得到的三聚氰胺硬质发泡材料具有掉粉率低、闭孔率高、高强度、韧性好、后加工处理与基体粘结强度大的特点。
为达到上述目的,本发明采用的技术方案是:
一种改性三聚氰胺硬质发泡材料,由以下重量份数的原料组成:三聚氰胺30~60份,多聚甲醛15~40份,水10~35份,异丁醇5~20份,苯并噁嗪3~10份,聚乙烯醇缩丁醛5~15份。
一种改性三聚氰胺硬质发泡材料的制备方法,包括以下步骤:
(1)依次向反应釜中加入水、多聚甲醛、三聚氰胺,升温至85℃~90℃,反应0.5~1.0h,生成多羟基化三聚氰胺;
(2)将苯并噁嗪、聚乙烯醇缩丁醛在异丁醇中溶解后加入到步骤(1)所述的反应釜中,降温至70℃~80℃,反应1.0~2.0h生成预聚体树脂溶液;
(3)将预聚体树脂溶液与固化剂、发泡剂、乳化剂、调节剂等混合均匀后进行微波发泡,熟化后得到改性三聚氰胺硬质发泡材料。
进一步的,所述步骤(1)中的pH值为8.0~9.0,pH调节剂为三乙醇胺。
进一步的,所述步骤(2)中的pH值为6.5~7.5,pH调节剂为1%的盐酸溶液。
进一步的,所述步骤(3)中固化剂为甲酸、乙酸、乙二酸、氨基磺酸、羟基乙酸、乙二胺四乙酸中的至少一种;发泡剂为正戊烷、异己烷、二氯甲烷、三氯三氟甲烷、三氯三氟乙烷中的至少一种;乳化剂为十二烷基苯磺酸钠、十二烷基硫酸钠、脂肪醇聚氧乙烯醚硫酸钠中的至少一种;调节剂为四氟乙基四氟丙基醚、四氟乙基甲基醚、七氟异丙甲醚中的至少一种。
进一步的,所述步骤(3)中固化剂、发泡剂、乳化剂、调节剂的加入量均为预聚体树脂溶液质量的2~15%。
进一步的,所述固化剂的加入量为预聚体树脂溶液的4~10%;所述发泡剂的加入量为预聚体树脂溶液的3~12%;所述乳化剂的加入量为预聚体树脂溶液的5~8%;所述调节剂的加入量为预聚体树脂溶液的2~7%。
进一步的,所述步骤(3)中微波发泡功率为1500~2500W,发泡时间为3~5min;熟化温度为50~90℃,熟化时间为8~24h。
本发明具有的优点是:
1.本发明在改性过程中引入苯并噁嗪,使其先进行开环反应,后参与三维网状缩合反应,苯并噁嗪的氮氧六元噁嗪环结构使得三聚氰胺硬质发泡材料的强度进一步的提高;
2.本发明在改性过程中加入聚乙烯醇缩丁醛,聚乙烯醇缩丁醛优良的柔韧性及较好的粘结强度使得三聚氰胺硬质发泡材料韧性好、与基体粘结强度大,同时能够抑制掉粉现象;
3.本发明使用异丁醇预先溶解苯并噁嗪及聚乙烯醇缩丁醛,避免了苯并噁嗪与聚乙烯醇缩丁醛在水性环境中溶解度低的问题,同时异丁醇的沸点为107℃,与水较为接近,而又高于发泡剂的沸点,不会打破发泡过程各发泡助剂之间的平衡关系;
4.本发明在三维网状缩合反应阶段,温度降低,有利于控制反应速率,使得聚合物分子量分布均匀,降低树脂交联固化速度快进而凝结的风险;
5.本发明在发泡过程中引入氟醚类调节剂,能有效调节发泡材料的孔洞,使得闭孔率提高,材料质感强,吸水率低。
具体实施方式
下面结合实施例对本发明做进一步的说明,但实施例不是本发明保护范围的限制,实施例中参与反应的原料重量和份数的换算为:每10g重量为一份。
实施例1
向反应釜中加入300g水、330g多聚甲醛与550g三聚氰胺,升温至85℃,用三乙醇胺调节体系pH值为8.0,搅拌反应45min;将60g苯并噁嗪与80g聚乙烯醇缩丁醛溶解在150g异丁醇后一起加入到反应釜中,降温至75℃,用1%盐酸调节反应pH值为7.0,搅拌反应1.5h后得到三聚氰胺预聚体树脂液。
取500g三聚氰胺预聚体树脂液,加入乙酸22g、正戊烷30g、十二烷基苯磺酸钠26g、四氟乙基甲基醚15g,搅拌均匀后,在微波炉中发泡5min,发泡功率为2000W,然后移至烘箱在60℃条件下熟化20h,得到改性三聚氰胺硬质发泡材料。
实施例2
向反应釜中加入400g水、370g多聚甲醛与650g三聚氰胺,升温至90℃,用三乙醇胺调节体系pH值为8.5,搅拌反应60min;将40g苯并噁嗪与60g聚乙烯醇缩丁醛溶解在120g异丁醇后一起加入到反应釜中,降温至70℃,用1%盐酸调节反应pH值为6.5,搅拌反应1.2h后得到三聚氰胺预聚体树脂液。
取500g三聚氰胺预聚体树脂液,加入甲酸26g、异己烷20g、十二烷基硫酸钠22g、四氟乙基四氟丙基醚16g,搅拌均匀后,在微波炉中发泡3min,发泡功率为1600W,然后移至烘箱在50℃条件下熟化24h,得到改性三聚氰胺硬质发泡材料。
实施例3
向反应釜中加入350g水、300g多聚甲醛与610g三聚氰胺,升温至82℃,用三乙醇胺调节体系pH值为9.0,搅拌反应35min。将90g苯并噁嗪与40g聚乙烯醇缩丁醛溶解在110g异丁醇后一起加入到反应釜中,降温至80℃,用1%盐酸调节反应pH值为7.5,搅拌反应1.8h后得到三聚氰胺预聚体树脂液。
取500g三聚氰胺预聚体树脂液,加入乙二酸22g、二氯甲烷25g、脂肪醇聚氧乙烯醚硫酸钠24g、七氟异丙甲醚18g,搅拌均匀后,在微波炉中发泡4min,发泡功率为1800W,然后移至烘箱在70℃条件下熟化16h,得到改性三聚氰胺硬质发泡材料。
实施例4
向反应釜中加入450g水、460g多聚甲醛与590g三聚氰胺,升温至87℃,用三乙醇胺调节体系pH值为8.0,搅拌反应55min;将65g苯并噁嗪与70g聚乙烯醇缩丁醛溶解在140g异丁醇后一起加入到反应釜中,降温至75℃,用1%盐酸调节反应pH值为7.0,搅拌反应2.0h后得到三聚氰胺预聚体树脂液。
取500g三聚氰胺预聚体树脂液,加入氨基磺酸22g、三氯三氟甲烷34g、十二烷基苯磺酸钠20g、四氟乙基甲基醚19g,搅拌均匀后,在微波炉中发泡5min,发泡功率为2200W,然后移至烘箱在80℃条件下熟化12h,得到改性三聚氰胺硬质发泡材料。
对比例1
该实施例为对比例,在反应釜中不加入苯并噁嗪、聚乙烯醇。
向反应釜中加入280g水、310g多聚甲醛与460g三聚氰胺,升温至84℃,用三乙醇胺调节体系pH值为8.5,搅拌反应50min;然后降温至70℃,用1%盐酸调节反应pH值为6.5,搅拌反应1.5h后得到三聚氰胺预聚体树脂液。
取500g三聚氰胺预聚体树脂液,加入羟基乙酸22g、三氯三氟乙烷26g、十二烷基硫酸钠36g、四氟乙基四氟丙基醚12g,搅拌均匀后,在微波炉中发泡3min,发泡功率为2500W,然后移至烘箱在85℃条件下熟化10h,得到改性三聚氰胺硬质发泡材料。
对比例2
该实施例为对比例,在发泡过程中不加入氟醚类调节剂。
向反应釜中加入340g水、370g多聚甲醛与600g三聚氰胺,升温至86℃,用三乙醇胺调节体系pH值为9.0,搅拌反应40min。将40g苯并噁嗪与60g聚乙烯醇缩丁醛溶解在120g异丁醇后一起加入到反应釜中,降温至80℃,用1%盐酸调节反应pH值为7.5,搅拌反应1.2h后得到三聚氰胺预聚体树脂液。
取500g三聚氰胺预聚体树脂液,加入乙二胺四乙酸22g、正戊烷40g、脂肪醇聚氧乙烯醚硫酸钠28g,搅拌均匀后,在微波炉中发泡4min,发泡功率为2100W,然后移至烘箱在75℃条件下熟化12h,得到改性三聚氰胺硬质发泡材料。
取实施例1~实施例4以及两个对比例所制得的三聚氰胺硬质发泡材料进行性能测试,测试结果如下所示:
通过表中数据可以看出,本发明所制得的改性三聚氰胺硬质发泡材料具有较高的力学强度、良好的韧性、闭孔率高、掉粉率低,同时在后续加工处理中与基材的粘结强度大,同时,三聚氰胺本征阻燃、导热系数低,非常适合作为外墙外保温材料。
Claims (7)
1.一种改性三聚氰胺硬质发泡材料,其特征在于,包括以下重量份数的原料:三聚氰胺30~60份,多聚甲醛15~40份,水10~35份,异丁醇5~20份,苯并噁嗪3~10份,聚乙烯醇缩丁醛5~15份;所述的改性三聚氰胺硬质发泡材料的制备方法包括以下步骤:
(1)依次向反应釜中加入水、多聚甲醛、三聚氰胺,升温至85℃~90℃,反应0.5~1.0h,生成多羟基化三聚氰胺;
(2)将苯并噁嗪、聚乙烯醇缩丁醛在异丁醇中溶解后加入到步骤(1)所述的反应釜中,降温至70℃~80℃,反应1.0~2.0h生成预聚体树脂溶液;
(3)将预聚体树脂溶液与固化剂、发泡剂、乳化剂、调节剂混合均匀后进行微波发泡,熟化后得到改性三聚氰胺硬质发泡材料,所述调节剂为四氟乙基四氟丙基醚、四氟乙基甲基醚、七氟异丙甲醚中的至少一种。
2.如权利要求1所述的改性三聚氰胺硬质发泡材料,其特征在于:所述步骤(1)中的pH值为8.0~9.0,pH调节剂为三乙醇胺。
3.如权利要求1所述的改性三聚氰胺硬质发泡材料,其特征在于:所述步骤(2)中的pH值为6.5~7.5,pH调节剂为1%的盐酸溶液。
4.如权利要求1所述的改性三聚氰胺硬质发泡材料,其特征在于:所述步骤(3)中固化剂为甲酸、乙酸、乙二酸、氨基磺酸、羟基乙酸、乙二胺四乙酸中的至少一种;发泡剂为正戊烷、异己烷、二氯甲烷、三氯三氟甲烷、三氯三氟乙烷中的至少一种;乳化剂为十二烷基苯磺酸钠、十二烷基硫酸钠、脂肪醇聚氧乙烯醚硫酸钠中的至少一种。
5.如权利要求1所述的改性三聚氰胺硬质发泡材料,其特征在于:所述步骤(3)中固化剂、发泡剂、乳化剂、调节剂的加入量均为预聚体树脂溶液质量的2~15%。
6.如权利要求5所述的改性三聚氰胺硬质发泡材料,其特征在于:所述固化剂的加入量为预聚体树脂溶液的4~10%;所述发泡剂的加入量为预聚体树脂溶液的3~12%;所述乳化剂的加入量为预聚体树脂溶液的5~8%;所述调节剂的加入量为预聚体树脂溶液的2~7%。
7.如权利要求1所述的改性三聚氰胺硬质发泡材料,其特征在于:所述步骤(3)中微波发泡功率为1500~2500W,发泡时间为3~5min;熟化温度为50~90℃,熟化时间为8~24h。
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