CN107936469A - 一种建筑外墙用的酚醛树脂泡沫保温板及其制备方法 - Google Patents
一种建筑外墙用的酚醛树脂泡沫保温板及其制备方法 Download PDFInfo
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 2
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Abstract
一种建筑外墙用的酚醛树脂泡沫保温板，其特征在于，首先制备酚醛树脂；其次将空心玻璃微珠清洗去油、表面粗化和偶联处理得到表面偶联处理玻璃微珠；然后采用水热法将二氧化钛和氧化镧沉积在空心玻璃微珠的表面，得到修饰空心玻璃微珠；最后，以丙烯酸‑苯乙烯共聚乳液和修饰空心玻璃微珠为增韧剂，混合，注模，发泡，固化，得到一种建筑外墙用的酚醛树脂泡沫保温板。本发明的酚醛树脂泡沫保温板，相比于现有酚醛泡沫板，其韧性和强度大幅提升，而且可很好地解决现有增韧途径中出现的难燃性能降低、烟密度和烟气毒性增加的问题。
Description
技术领域
本发明属于建筑领域，具体涉及一种建筑外墙用的酚醛树脂泡沫保温板及其制备方法。
背景技术
目前，建筑用能约占整个社会用能的30%以上。建筑节能是有效降低全社会能源消耗的重点领域，而高效的有机保温材料对建筑外墙进行保温是建筑节能的重要技术。现阶段建筑节能大量采用燃烧等级低的材料，燃烧时产生大量有毒气体，导致了火灾事故频发和埋下重大安全隐患。由于酚醛树脂中存在着大量的苯环结构，在高温下形成炭化的“石墨”骨架，在250-400℃温度下，酚醛泡沫进一步缩合并放出水和甲醛；在400-600℃温度下，逐步氧化放出CO、CO2；在600-750℃温度下，逐步炭化形成的炭起隔热作用，阻止泡沫体进一步燃烧。在燃烧时不会释放有毒气体和烟雾，由于酚醛泡沫的这些特性，大量运用于建筑节能工程中，起到了既可有效防火、又可高效节能的效果，其用量每年以15%以上速度增加。但是，由于酚醛固有的苯环结构，酚醛泡沫体的刚性大，脆性高，易粉化和断裂，限制了酚醛泡沫的使用。
发明内容
本发明的目的在于提供一种不易粉化的建筑外墙用的酚醛树脂泡沫保温板及其制备方法。
为了实现上述的目的，本发明采用了如下的技术方案：
一种建筑外墙用的酚醛树脂泡沫保温板，其特征在于，首先制备酚醛树脂；其次将空心玻璃微珠清洗去油、表面粗化和偶联处理得到表面偶联处理玻璃微珠；然后采用水热法将二氧化钛和氧化镧沉积在空心玻璃微珠的表面，得到修饰空心玻璃微珠；最后，以丙烯酸-苯乙烯共聚乳液和修饰空心玻璃微珠为增韧剂，混合，注模，发泡，固化，得到一种建筑外墙用的酚醛树脂泡沫保温板。
所述的建筑外墙用的酚醛树脂泡沫保温板，其特征在于，其由如下具体步骤制备而成：
（1）将苯酚置于45-50℃的恒温水浴中融化；将氢氧化钠、尿素和熔化的苯酚以1：3-4：10-12的质量比加入反应釜内，混合搅拌15-20min；加入1.5-1.8倍重量份的37%的甲醛溶液，升高温度至至65-75℃，恒温磁力搅拌5-6h；冷却，降温至40℃以下，出料得到酚醛树脂；
（2）将玻璃微珠置于10-12倍重量份的80-90℃的水中磁力搅拌20-30min清洗去油，水洗2-3次，真空抽滤；将清洗后的玻璃微珠置于8-10倍重量份的4-5%的氢氟酸溶液中磁力搅拌表面粗化5-8min，水洗2-3次，真空抽滤，干燥，得到表面粗化玻璃微珠；将硅烷偶联剂kh-570加入到25-30倍重量份的无水乙醇与去离子水以1：1的质量比配置的混合液中，磁力搅拌50-60min，加入表面粗化玻璃微珠，60-65℃恒温磁力搅拌4-5h，真空抽滤，干燥，得到表面偶联处理玻璃微珠；
（3）将硫酸钛和硝酸镧加入到1/2的去离子水中，升高温度至60-70℃，混合搅拌至完全溶解，加入尿素，继续磁力搅拌50-60min；加入表面偶联处理玻璃微珠，超声震荡30-40min，加入剩余的去离子水，转移至反应釜中，密封后将其放置在均相反应器中，以2-3℃/min的速率升温至140-150℃后，恒温反应3-4h；待反应结束后，过滤，用丙酮、无水乙醇和去离子水分别洗涤2-3次，70-80℃真空干燥，得到修饰空心玻璃微珠；
（4）将丙烯酸-苯乙烯共聚乳液加入到分散罐中，启动搅拌机开始搅拌，调节搅拌机转速150-200r/min，依次加入修饰空心玻璃微珠、聚磷酸铵和道康宁乳液349，继续搅拌40-50min，密封备用；
（5）将酚醛树脂、吐温-80、正戊烷和步骤（4）的产物加入到分散罐中，启动搅拌机，调节搅拌机转速为1800-2000r/min，搅拌15-20min，加入六次甲基四胺，调节搅拌机转速为2500-3000r/min，搅拌15-20s，将搅拌好的物料倒入模具中，振捣20-30s，将模具放入75-80℃的烘箱中进行发泡成型，待发泡成型完成后，将模具取出、拆模，得到一种建筑外墙用的酚醛树脂泡沫保温板。
所述的建筑外墙用的酚醛树脂泡沫保温板的制备方法，其特征在于，步骤（3）中硫酸钛、硝酸镧、尿素、表面偶联处理玻璃微珠和去离子水的质量比为1：0.2-0.25：0.5-0.6：8-10：100-120。
所述的建筑外墙用的酚醛树脂泡沫保温板的制备方法，其特征在于，步骤（4）中丙烯酸-苯乙烯共聚乳液、修饰空心玻璃微珠、聚磷酸铵和道康宁乳液349的质量比为1：0.18-0.2：0.06-0.07：0.05-0.06。
所述的建筑外墙用的酚醛树脂泡沫保温板的制备方法，其特征在于，步骤（5）中酚醛树脂、吐温-80、正戊烷、步骤（4）的产物和六次甲基四胺的质量比为1：0.04-0.05：0.06-0.07：0.3-0.4：0.15-0.18。
通过上述的技术方案，本发明的有益效果是：
本发明将空心玻璃微珠清洗去油、表面粗化和偶联处理得到表面偶联处理玻璃微珠；然后采用水热法将二氧化钛和氧化镧沉积在空心玻璃微珠的表面，得到修饰空心玻璃微珠；本发明以丙烯酸-苯乙烯共聚乳液和修饰空心玻璃微珠为酚醛树脂的增韧剂，一方面空心微珠作为一种大热惯量中空结构材料，具有较低热传导系数，减少了对红外热辐射能的传递和吸收，增加了酚醛树脂泡沫体的强度；另一方面，沉积空心玻璃微珠表面的二氧化钛和氧化镧能吸收空气中的红外辐射，并将此辐射能量反射出去，从而隔断热能进入基层，增加了酚醛树脂泡沫保温板隔热保温效果；同时，丙烯酸-苯乙烯共聚乳液与酚醛树脂共混改性，改性后的酚醛树脂继承了酚醛树脂高温下形成炭化骨架的防火性能，通过引入的软段——丙烯酸-苯乙烯共聚物，降低了酚醛树脂泡沫体的刚性，改善了酚醛树脂的易脆的问题；本发明的酚醛树脂泡沫保温板，相比于现有酚醛泡沫板，其韧性和强度大幅提升，而且可很好地解决现有增韧途径中出现的难燃性能降低、烟密度和烟气毒性增加的问题。
具体实施方式
本实施例的建筑外墙用的酚醛树脂泡沫保温板，其由如下具体步骤制备而成：
（1）将苯酚置于50℃的恒温水浴中融化；将氢氧化钠、尿素和熔化的苯酚以1：4：12的质量比加入反应釜内，混合搅拌20min；加入1.8倍重量份的37%的甲醛溶液，升高温度至至75℃，恒温磁力搅拌6h；冷却，降温至40℃以下，出料得到酚醛树脂；
（2）将玻璃微珠置于12倍重量份的85℃的水中磁力搅拌30min清洗去油，水洗3次，真空抽滤；将清洗后的玻璃微珠置于10倍重量份的5%的氢氟酸溶液中磁力搅拌表面粗化8min，水洗3次，真空抽滤，干燥，得到表面粗化玻璃微珠；将硅烷偶联剂kh-570加入到30倍重量份的无水乙醇与去离子水以1：1的质量比配置的混合液中，磁力搅拌60min，加入表面粗化玻璃微珠，65℃恒温磁力搅拌5h，真空抽滤，干燥，得到表面偶联处理玻璃微珠；
（3）将硫酸钛和硝酸镧加入到1/2的去离子水中，升高温度至70℃，混合搅拌至完全溶解，加入尿素，继续磁力搅拌60min；加入表面偶联处理玻璃微珠，超声震荡40min，加入剩余的去离子水，转移至反应釜中，密封后将其放置在均相反应器中，以3℃/min的速率升温至150℃后，恒温反应4h；待反应结束后，过滤，用丙酮、无水乙醇和去离子水分别洗涤3次，80℃真空干燥，得到修饰空心玻璃微珠；
（4）将丙烯酸-苯乙烯共聚乳液加入到分散罐中，启动搅拌机开始搅拌，调节搅拌机转速200r/min，依次加入修饰空心玻璃微珠、聚磷酸铵和道康宁乳液349，继续搅拌50min，密封备用；
（5）将酚醛树脂、吐温-80、正戊烷和步骤（4）的产物加入到分散罐中，启动搅拌机，调节搅拌机转速为2000r/min，搅拌20min，加入六次甲基四胺，调节搅拌机转速为3000r/min，搅拌20s，将搅拌好的物料倒入模具中，振捣20-30s，将模具放入80℃的烘箱中进行发泡成型，待发泡成型完成后，将模具取出、拆模，得到一种建筑外墙用的酚醛树脂泡沫保温板。
本实施例的步骤（3）中硫酸钛、硝酸镧、尿素、表面偶联处理玻璃微珠和去离子水的质量比为1：0.25：0.6：10：120。
本实施例的步骤（4）中丙烯酸-苯乙烯共聚乳液、修饰空心玻璃微珠、聚磷酸铵和道康宁乳液349的质量比为1：0.2：0.07：0.06。
本实施例的步骤（5）中酚醛树脂、吐温-80、正戊烷、步骤（4）的产物和六次甲基四胺的质量比为1：0.05：0.07：0.4：0.18。
Claims (5)
1.一种建筑外墙用的酚醛树脂泡沫保温板，其特征在于，首先制备酚醛树脂；其次将空心玻璃微珠清洗去油、表面粗化和偶联处理得到表面偶联处理玻璃微珠；然后采用水热法将二氧化钛和氧化镧沉积在空心玻璃微珠的表面，得到修饰空心玻璃微珠；最后，以丙烯酸-苯乙烯共聚乳液和修饰空心玻璃微珠为增韧剂，混合，注模，发泡，固化，得到一种建筑外墙用的酚醛树脂泡沫保温板。
2.根据权利要求书1所述的建筑外墙用的酚醛树脂泡沫保温板，其特征在于，其由如下具体步骤制备而成：
（1）将苯酚置于45-50℃的恒温水浴中融化；将氢氧化钠、尿素和熔化的苯酚以1：3-4：10-12的质量比加入反应釜内，混合搅拌15-20min；加入1.5-1.8倍重量份的37%的甲醛溶液，升高温度至至65-75℃，恒温磁力搅拌5-6h；冷却，降温至40℃以下，出料得到酚醛树脂；
（2）将玻璃微珠置于10-12倍重量份的80-90℃的水中磁力搅拌20-30min清洗去油，水洗2-3次，真空抽滤；将清洗后的玻璃微珠置于8-10倍重量份的4-5%的氢氟酸溶液中磁力搅拌表面粗化5-8min，水洗2-3次，真空抽滤，干燥，得到表面粗化玻璃微珠；将硅烷偶联剂kh-570加入到25-30倍重量份的无水乙醇与去离子水以1：1的质量比配置的混合液中，磁力搅拌50-60min，加入表面粗化玻璃微珠，60-65℃恒温磁力搅拌4-5h，真空抽滤，干燥，得到表面偶联处理玻璃微珠；
（3）将硫酸钛和硝酸镧加入到1/2的去离子水中，升高温度至60-70℃，混合搅拌至完全溶解，加入尿素，继续磁力搅拌50-60min；加入表面偶联处理玻璃微珠，超声震荡30-40min，加入剩余的去离子水，转移至反应釜中，密封后将其放置在均相反应器中，以2-3℃/min的速率升温至140-150℃后，恒温反应3-4h；待反应结束后，过滤，用丙酮、无水乙醇和去离子水分别洗涤2-3次，70-80℃真空干燥，得到修饰空心玻璃微珠；
（4）将丙烯酸-苯乙烯共聚乳液加入到分散罐中，启动搅拌机开始搅拌，调节搅拌机转速150-200r/min，依次加入修饰空心玻璃微珠、聚磷酸铵和道康宁乳液349，继续搅拌40-50min，密封备用；
（5）将酚醛树脂、吐温-80、正戊烷和步骤（4）的产物加入到分散罐中，启动搅拌机，调节搅拌机转速为1800-2000r/min，搅拌15-20min，加入六次甲基四胺，调节搅拌机转速为2500-3000r/min，搅拌15-20s，将搅拌好的物料倒入模具中，振捣20-30s，将模具放入75-80℃的烘箱中进行发泡成型，待发泡成型完成后，将模具取出、拆模，得到一种建筑外墙用的酚醛树脂泡沫保温板。
3.根据权利要求书2所述的建筑外墙用的酚醛树脂泡沫保温板的制备方法，其特征在于，步骤（3）中硫酸钛、硝酸镧、尿素、表面偶联处理玻璃微珠和去离子水的质量比为1：0.2-0.25：0.5-0.6：8-10：100-120。
4.根据权利要求书2所述的建筑外墙用的酚醛树脂泡沫保温板的制备方法，其特征在于，步骤（4）中丙烯酸-苯乙烯共聚乳液、修饰空心玻璃微珠、聚磷酸铵和道康宁乳液349的质量比为1：0.18-0.2：0.06-0.07：0.05-0.06。
5.根据权利要求书2所述的建筑外墙用的酚醛树脂泡沫保温板的制备方法，其特征在于，步骤（5）中酚醛树脂、吐温-80、正戊烷、步骤（4）的产物和六次甲基四胺的质量比为1：0.04-0.05：0.06-0.07：0.3-0.4：0.15-0.18。
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