CN116619847A - 一种长效保温复合岩棉板及其制备方法 - Google Patents

一种长效保温复合岩棉板及其制备方法 Download PDF

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CN116619847A
CN116619847A CN202310396352.2A CN202310396352A CN116619847A CN 116619847 A CN116619847 A CN 116619847A CN 202310396352 A CN202310396352 A CN 202310396352A CN 116619847 A CN116619847 A CN 116619847A
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rock wool
wool board
modified
long
phosphorus
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渠涛
沈长涛
李前防
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Xuzhou Jingxin New Material Co ltd
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Xuzhou Jingxin New Material Co ltd
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Abstract

本发明公开了一种长效保温复合岩棉板及其制备方法，所述复合岩棉板由改性岩棉板、耐碱玻纤网格布、改性防水砂浆和界面剂复合而成；所述改性岩棉板是以正硅酸乙酯作为硅源，再加入三甲基氯硅烷进行改性，得到SiO2气凝胶，将其配制成溶液，通过浸润的方法对岩棉板进行改性；所述改性防水砂浆是以含磷超支化阻燃剂、聚醚多元醇、二苯基甲烷二异氰酸酯为原料制得含磷型超支化阻燃聚氨酯材料，再加入填料砂、水泥，制得改性防水砂浆。本发明不仅极大地提升了岩棉板疏水性及保温性能，还改善了防火阻燃性能，增强了强度和弹性性能，使其使用年限增长，达到长效保温效果。

Description

一种长效保温复合岩棉板及其制备方法
技术领域
本发明涉及岩棉板技术领域，具体为一种长效保温复合岩棉板及其制备方法。
背景技术
岩棉制品以其优异的防火保温特性是国际上公认的“第五常规能源”中的主要节能材料。在建筑上每使用1吨岩棉制品进行保温，一年至少可节省相当于1吨石油的能量，符合低碳、节能、减排趋势，然而岩棉材料具有吸水性，受潮后耐久性不好，不仅影响其使用寿命及结构稳定性，也进一步影响了该材料的防火性能和保温性能，限制了其在建筑保温材料领域的推广和发展。因此，我们提出一种长效保温复合岩棉板及其制备方法。
发明内容
本发明的目的在于提供一种长效保温复合岩棉板及其制备方法，以解决上述背景技术中提出的问题。
为了解决上述技术问题，本发明提供如下技术方案：一种长效保温复合岩棉板的制备方法，包括以下步骤：
(1)制作改性岩棉板：用SiO2气凝胶对岩棉板进行改性处理；
(2)制作改性防水砂浆：由含磷型超支化阻燃性聚氨酯材料、砂和水泥混合均匀组成；
(3)制作复合岩棉板：在改性岩棉板上表面叠加平铺一层耐碱玻纤网格布，依次涂布界面剂、改性防水砂浆，干燥；将改性岩棉板下表面翻转，叠加平铺一层耐碱玻纤网格布，依次涂布界面剂、改性防水砂浆，干燥后，制得一个板材，通过层压机将板材保压成型。层压压力为0～16MPa，热机压力为12级，冷压压力为5级。压力精度为±0.05MPa；层压温度为128～180℃，温度精度为±3℃；层压热压时间为20～30min，层压冷压时间为12～16min。
进一步的，改性岩棉板由以下工艺制得：
(1)取正硅酸乙酯加入去离子水中，搅拌均匀后，逐滴加入0.1M的HCl溶液，得到溶胶；接着加入0.5M的氨水，持续搅拌，得到凝胶；把凝胶放入50～60℃水浴锅进行水浴老化24～48h，接着用去离子水水洗和无水乙醇醇洗12～24h，再离心，得到湿凝胶；将湿凝胶放入三甲基氯硅烷和正己烷混合液(体积比为1：5)中浸泡12～24h，接着用正己烷洗涤三次，最后放入60～70℃的烘箱干燥24～48h，得到SiO2气凝胶；
(2)将SiO2气凝胶和乙醇混合制备成溶液(气凝胶占比为5～10％)作为改性剂，通过浸润的方法对岩棉进行改性，3～5min后取出，放置常温下干燥24～48h后，得到改性岩棉板。
进一步的，所述步骤(1)中正硅酸乙酯、异丙醇与水的质量比为1：(1.15～1.2)：(0.35～0.52)。
进一步的，所述步骤(1)中三甲基氯硅烷的用量是正硅酸乙酯体积的0.7～0.9倍。
进一步的，所述步骤(2)中SiO2气凝胶的用量是乙醇体积的0.05～0.1倍。
进一步的，所述步骤(2)中岩棉被裁剪成为300*300mm，厚度为30mm的岩棉试样。
进一步的，改性防水砂浆的制备工艺如下：
(1)向装有电动搅拌、冷凝管和氮气保护的干燥完全的四口烧瓶中，加入聚醚多元醇(加热至120℃真空脱水2h)、含磷超支化阻燃剂和N,N-二甲基乙酰胺(DMAc)，混合均匀，打开冷凝管，通入氮气，升温至70～80℃；再滴加经过DMAc溶解的二苯基甲烷二异氰酸酯(MDI)，2～3h内滴完，在60～80℃反应2～3h，然后在加入1，4-丁二醇，再滴加经过DMAC溶解的MDI，2～3h内滴完；加入苹果酸增稠剂，常温搅拌1～2h，冷却出料，制得含磷型超支化阻燃性聚氨酯材料；
(2)把经过60目筛过的填料砂和水泥混合(砂∶水泥＝2：1)，加入阻燃性聚氨酯材料和间苯二胺固化剂，室温搅拌均匀后，得改性防水砂浆。
进一步的，所述步骤(1)中聚醚多元醇与二苯基甲烷二异氰酸酯质量比为(5.6：1)～(6.3：1)。
进一步的，所述步骤(2)中超支化阻燃性聚氨酯材料含量为填料(砂、水泥)的9～15％。
进一步的，含磷超支化阻燃剂的制备工艺如下：
(1)按比例加入水和乙醇(体积比为2：3)置于烧杯中，室温下搅拌均匀，再加入四丙基氢氧化铵(25％)，二乙胺基甲基三乙氧基硅烷和苯胺甲基三甲氧基硅烷，反应10～12h，抽滤，真空干燥，得含胺基的有机硅；
(2)先在3-羟基苯二甲酸酐中加入二甲基甲酰胺(DMF)，充分溶解；再向四口烧瓶中加入二异丙醇胺，搅拌均匀，滴加充分溶解的3-羟基苯二甲酸酐，常温反应3～4h；然后加入含胺基的有机硅和对甲苯磺酸，开始加热，加热到120～130℃，冷凝回流，保温6～8h，减压蒸馏得超支化聚合物；向装有温度计、搅拌器的四口烧瓶中加入上述得到的超支化聚合物，升温到50～60℃，加入聚磷酸试剂和对甲苯磺酸，混合均匀后升温到70～80℃，保温反应5～6h，水解2～3h，减压蒸馏，制备出含磷型超支化阻燃剂。
进一步的，所述步骤(1)中二乙胺基甲基三乙氧基硅烷与苯胺甲基三甲氧基硅烷质量比为(1：2.5)～(1：3.0)
进一步的，所述步骤(2)中3-羟基苯二甲酸酐与二异丙醇胺的质量比为(1：1)～(1：1.5)。
与现有技术相比，本发明所达到的有益效果是：
(1)本发明通过SiO2气凝胶对岩棉板进行改性，大大提升了岩棉板的使用寿命和保暖性，SiO2气凝胶是一种超级疏水材料，疏水角可以达到150°，属于憎水材料，不仅具有优越的保温隔热性能，而且具有良好的疏水性、隔声性和透光性。改性后的岩棉板导热系数降低，疏水性提高。
(2)本发明在砂浆中添加含磷型超支化阻燃聚氨酯材料使复合岩棉板阻燃性和柔性提高。超支化聚合物本身含有的支链多并且粘度低，这就使得超支化聚合物与材料具有很好的相容性，减少了对材料造成不利影响，同时，超支化聚合物末端含有大量的活性官能团，可以对其末端进行改性，将阻燃元素引入到超支化聚合物大分子中，使其能够成为更多材料的阻燃剂。
(3)含磷型超支化阻聚氨酯在燃烧的过程中，表面会形成一层致密、完整、蓬松的炭层。这种炭层具有隔氧、隔热、阻隔火焰传递的作用。除此之外，加入的这种含磷型阻燃体系突出的优点则是燃烧时释放大量低毒、无害的气体，如N2等，而且不会形成二次危害，它们会扩散然后降低燃烧材料周围空气中氧的浓度，从而起到了降低了材料的燃点的作用。在氮、磷、硅三种阻燃元素的协同作用下，使材料同时具有炭化、发泡、隔氧绝热、抑制材料降解等能力，发挥协同效果，具有高的Si含量，显著提高基材的抗冲性能、拉伸性能等力学性能。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本实施例中，正硅酸乙酯硅含量28％，购自上海卓锐化工有限公司；三甲基氯硅烷购自山东利尔邦新材料有限公司；氨水纯度28％，购自上海阿拉丁生化科技股份有限公司；无水乙醇购自西安三浦化学试剂有限公司；正己烷购自吉林市北化精细化工有限公司；聚醚多元醇质均分子量MW:2000-3000，购自湖北巨胜科技有限公司；N,N-二甲基乙酰胺购自山东金悦源新材料有限公司；二苯基甲烷二异氰酸酯购自上海麦克林生化科技股份有限公司；1，4-丁二醇购自南通润丰石油化工有限公司；苹果酸购自陕西富聚源生物科技有限公司；间苯二胺购自济南世纪通达化工有限公司；四丙基氢氧化铵购自武汉鹏垒生物科技有限公司；二乙胺基甲基三乙氧基硅烷购自湖北科孚乐材料科技有限公司；苯胺甲基三甲氧基硅烷购自上海相辉医药科技有限公司；3-羟基苯二甲酸酐购自山东轩鸿生物医药有限公司；二甲基甲酰胺购自上海迈瑞尔生化科技有限公司；二异丙醇胺购自上海麦克林生化科技股份有限公司；对甲基苯磺酸购自上海易恩化学技术有限公司；聚磷酸中P2O5含量≥85％，购自上海阿拉丁生化科技股份有限公司；耐碱玻纤网格布的厚度为1mm，购自衡连金属丝网制品(大连)有限责任公司；界面剂：EL1230柔韧型，厚度为1.5～3mm，购自北京沃土建材有限公司；岩棉板的厚度在30～200mm之间，岩棉板购自蓝宁岩棉夹芯板厂；改性防水砂浆厚度为6～8mm。
实施例1：一种长效保温复合岩棉板的制备方法，包括以下工艺：
1.改性岩棉板的制备工艺如下：
(1)取13g正硅酸乙酯和15g异丙醇加入5ml去离子水中，搅拌均匀后，逐滴加入0.1M的HCl溶液，调节pH值到3时，停止滴加，得到溶胶；接着加入0.5M氨水，持续搅拌，调整pH值8时，停止加入，得到凝胶；把凝胶放入50℃水浴锅进行水浴老化48h，接着用去离子水水洗和无水乙醇醇洗24h，再离心，得到湿凝胶；将湿凝胶放入三甲基氯硅烷和正己烷混合液(体积比为1：5)中浸泡24h，接着用正己烷洗涤三次，最后放入60℃的烘箱干燥48h，得到SiO2气凝胶；
(2)将10gSiO2气凝胶和200g乙醇混合制备成溶液(气凝胶占比为5％)作为改性剂，通过浸润的方法对300*300mm的岩棉试样进行改性，5min后取出，放置常温下干燥48h后，得到改性岩棉板。
2.含磷超支化阻燃剂的制备工艺如下：
(1)按比例加入40ml水和60ml乙醇(体积比为2：3)置于烧杯中，室温下搅拌均匀，再加入0.5ml四丙基氢氧化铵(25％)，10g二乙胺基甲基三乙氧基硅烷和27g苯胺甲基三甲氧基硅烷，反应12h，抽滤，真空干燥，得含胺基的有机硅；
(2)先将12g的3-羟基苯二甲酸酐中加入10g二甲基甲酰胺(DMF)，充分溶解；再向四口烧瓶中加入9.7g二异丙醇胺，搅拌均匀，滴加充分溶解的3-羟基苯二甲酸酐，常温反应3h；然后加入1.5g含胺基的有机硅和0.2g对甲苯磺酸，开始加热，加热到125℃，冷凝回流，保温6h，减压蒸馏得超支化聚合物；向装有温度计、搅拌器的四口烧瓶中加入上述得到的超支化聚合物，升温到50℃，分三次加入0.5g聚磷酸试剂和0.2g对甲苯磺酸，混合均匀后升温到80℃，保温反应5h，水解3h，减压蒸馏，制备出含磷型超支化阻燃剂。
3.改性防水砂浆的制备工艺如下：
(1)向装有电动搅拌、冷凝管和氮气保护的干燥完全的四口烧瓶中加入24g聚醚多元醇(加热至120℃真空脱水2h)，加入4g含磷超支化阻燃剂和10gN,N-二甲基乙酰胺(DMAc)，混合均匀，打开冷凝管，通入氮气，升温至70℃；再滴加经过10gDMAc溶解的4g二苯基甲烷二异氰酸酯(MDI)，2h内加完，在60℃反应3h，然后在加入3g的1，4-丁二醇，再滴加35g经过DMAC溶解的MDI，2h内加完；加入0.2g苹果酸增稠剂，常温搅拌1h，冷却出料，制得含磷型超支化阻燃性聚氨酯材料；
(2)把40g经过60目筛过的砂和20g水泥混合(砂∶水泥＝2∶1)，加入12g阻燃性聚氨酯材料和10g间苯二甲胺固化剂，室温搅拌均匀后，得改性防水砂浆。
4.制作复合岩棉板：在改性岩棉板上表面叠加平铺一层耐碱玻纤网格布，依次涂布界面剂、改性防水砂浆，干燥；将改性岩棉板下表面翻转，叠加平铺一层耐碱玻纤网格布，依次涂布界面剂、改性防水砂浆，干燥后，制得一个板材，通过层压机将板材保压成型。层压压力为0～16MPa，热机压力为12级，冷压压力为5级。压力精度为±0.05MPa；层压温度为128～180℃，温度精度为±3℃；层压热压时间为20～30min，层压冷压时间为12～16min。
实施例2：一种长效保温复合岩棉板的制备方法，包括以下工艺：
1.改性岩棉板的具体步骤如下：
(1)取17.3g正硅酸乙酯和20g异丙醇加入6ml去离子水中，搅拌均匀后，逐滴加入0.1M的HCl溶液，调节pH值到3时，停止滴加，得到溶胶；接着加入0.5M氨水，持续搅拌，调整pH值8时，停止加入，得到凝胶；把凝胶放入55℃水浴锅进行水浴老化48h，接着用去离子水水洗和无水乙醇醇洗24h，再离心，得到湿凝胶；将湿凝胶放入三甲基氯硅烷和正己烷混合液(体积比为1：5)中浸泡24h，接着用正己烷洗涤三次，最后放入60℃的烘箱干燥48h，得到SiO2气凝胶；
(2)将15gSiO2气凝胶和200g乙醇混合制备成溶液(气凝胶占比为7.5％)作为改性剂，通过浸润的方法对300*300mm的岩棉试样进行改性，5min后取出，放置常温下干燥48h后，得到改性岩棉板。
2.含磷超支化阻燃剂的制备工艺如下：
(1)按比例加入40ml水和60ml乙醇(体积比为2：3)置于烧杯中，室温下搅拌均匀，再加入0.5ml四丙基氢氧化铵(25％)，12g二乙胺基甲基三乙氧基硅烷和32.4g苯胺甲基三甲氧基硅烷，反应12h，抽滤，真空干燥，得含胺基的有机硅。
(2)先将15g的3-羟基苯二甲酸酐中加入10g二甲基甲酰胺(DMF)，充分溶解；再向四口烧瓶中加入12.2g二异丙醇胺，搅拌均匀，滴加充分溶解的3-羟基苯二甲酸酐，常温反应3h；然后加入1.6g含胺基的有机硅和0.3g对甲苯磺酸，开始加热，加热到125℃，冷凝回流，保温6h，减压蒸馏得超支化聚合物；向装有温度计、搅拌器的四口烧瓶中加入上述得到的超支化聚合物，升温到55℃，分三次加入0.6g聚磷酸试剂和0.3g对甲苯磺酸，混合均匀后升温到80℃，保温反应5h，水解3h，减压蒸馏，制备出含磷型超支化阻燃剂。
3.改性防水砂浆的制备工艺如下：
(1)向装有电动搅拌、冷凝管和氮气保护的干燥完全的四口烧瓶中加入30g聚醚多元醇(加热至120℃真空脱水2h)，加入5g含磷超支化阻燃剂和10gN,N-二甲基乙酰胺(DMAc)，混合均匀，打开冷凝管，通入氮气，升温至70℃；再滴加经过10gDMAc溶解的5g二苯基甲烷二异氰酸酯(MDI)，2h内加完，在70℃反应3h，然后在加入3g的1，4-丁二醇，再滴加35g经过DMAC溶解的MDI，2h内加完；加入0.2g苹果酸增稠剂，常温搅拌1h，冷却出料，制得含磷型超支化阻燃性聚氨酯材料；
(2)把40g经过60目筛过的砂和20g水泥混合(砂∶水泥＝2∶1)，加入15g阻燃性聚氨酯材料和11g间苯二甲胺固化剂，室温搅拌均匀后，得改性防水砂浆。
其他工艺与实施例1相同。
实施例3：一种长效保温复合岩棉板的制备方法，包括以下工艺：
1.所述改性岩棉板的具体步骤如下：
(1)取17.3g正硅酸乙酯和20g异丙醇加入6ml去离子水中，搅拌均匀后，逐滴加入0.1M的HCl溶液，调节pH值到3时，停止滴加，得到溶胶；接着加入0.5M氨水，持续搅拌，调整pH值8时，停止加入，得到凝胶；把凝胶放入60℃水浴锅进行水浴老化48h，接着用去离子水水洗和无水乙醇醇洗24h，再离心，得到湿凝胶；将湿凝胶放入三甲基氯硅烷和正己烷混合液(体积比为1：5)中浸泡24h，接着用正己烷洗涤三次，最后放入60℃的烘箱干燥48h，得到SiO2气凝胶；
(2)将20gSiO2气凝胶和200g乙醇混合制备成溶液(气凝胶占比为10％)作为改性剂，通过浸润的方法对300*300mm的岩棉试样进行改性5min后取出，放置常温下干燥48h后，得到改性岩棉板。
2.所述含磷超支化阻燃剂的制备工艺如下：
(1)按比例加入40ml水和60ml乙醇(体积比为2：3)置于烧杯中，室温下搅拌均匀，再加入0.5ml四丙基氢氧化铵(25％)，15g二乙胺基甲基三乙氧基硅烷和40.5g苯胺甲基三甲氧基硅烷，反应12h，抽滤，真空干燥，得含胺基的有机硅。
(2)先将18g的3-羟基苯二甲酸酐中加入15g二甲基甲酰胺(DMF)，充分溶解；再向四口烧瓶中加入14.8g二异丙醇胺，搅拌均匀，滴加充分溶解的3-羟基苯二甲酸酐，常温反应3h；然后加入1.8g含胺基的有机硅和0.4g对甲苯磺酸，开始加热，加热到125℃，冷凝回流，保温6h，减压蒸馏得超支化聚合物；向装有温度计、搅拌器的四口烧瓶中加入上述得到的超支化聚合物，升温到60℃，分三次加入0.7g聚磷酸试剂和0.4g对甲苯磺酸，混合均匀后升温到80℃，保温反应5h，水解3h，减压蒸馏，制备出含磷型超支化阻燃剂。
3.改性防水砂浆的制备工艺如下：
(1)向装有电动搅拌、冷凝管和氮气保护的干燥完全的四口烧瓶中加入30g聚醚多元醇，在加热至120℃真空脱水2h后，加入5g含磷超支化阻燃剂和10gN,N-二甲基乙酰胺(DMAc)，混合均匀，打开冷凝管，通入氮气，升温至70℃；再滴加经过10gDMAc溶解的5g二苯基甲烷二异氰酸酯(MDI)，2h内加完，在80℃反应3h，然后在加入3g的1，4-丁二醇，再滴加35g经过DMAC溶解的MDI，2h内加完；加入0.02g苹果酸增稠剂，常温搅拌1h，冷却出料，制得含磷型超支化阻燃性聚氨酯材料；
(2)把40g经过60目筛过的砂和20g水泥混合(砂∶水泥＝2∶1)，加入20g阻燃性聚氨酯材料和12g间苯二甲胺固化剂，室温搅拌均匀后，得改性防水砂浆。
其他工艺与实施例1相同。
对比例1：一种长效保温复合岩棉板的制备方法，
与实施例2相比，对比例1选用同规格常规岩棉板，不进行SiO2气凝胶改性；其他步骤与实例2相同，得一种长效保温复合岩棉板。
对比例2：一种长效保温复合岩棉板的制备方法，
与实施例2相比，对比例2选用同规格普通砂浆，不添加含磷型超支化阻燃性聚氨酯材料；其他步骤与实例2相同，得一种长效保温复合岩棉板。
对比例3：一种长效保温复合岩棉板的制备方法，
与实施例2相比，对比例3在改性防水砂浆制备工艺中，不添加含磷超支化阻燃剂，制作同等质量的常规聚氨酯材料，删除含磷超支化阻燃剂的制备工艺，其余步骤与实施例2中的相同，得到一种长效保温复合岩棉板。
实验
取实施例1-3中含磷型超支化阻燃性聚氨酯材料、对比例1含磷型超支化阻燃性聚氨酯材料、对比例3中常规聚氨酯材料，分别制得试样，对其性能进行检测并记录检测结果：
根据GB/T 2408-2021《塑料燃烧性能的测定(水平法和垂直法)》测定燃烧性能，实验步骤：将制备好的聚氨酯材料涂敷在聚四氟乙烯板上成膜，在真空干燥箱中60℃下干燥一夜，干燥后裁剪为3cm×3cm的正方形试样，安装试样，点燃本生灯，将本生灯火焰对准试样下端面中心，点燃试样并进行测定，观察试样垂直燃烧后现象，记录数据。
生成炭层 UL94-V等级
实施例1 多而厚，且致密 V-2
实施例2 多而厚，且致密 V-2
实施例3 多而厚，且致密 V-2
对比例1 多而厚 不够等级
对比例3 有，但不成片 不够等级
取实施例1-3、对比例1-3中得到的复合岩棉板，制得试样，分别对其性能进行检测并记录检测结果：
根据GB/T 10299-2011《绝热材料憎水性试验方法》测定吸湿性，实验步骤：复合岩棉板试样的尺寸为300*300mm，厚度为30mm，在40℃，相对湿度90％的条件下，将试样放入憎水试验，试验时间为96个小时，分别对实验前后试样的质量进行测定。
根据GB/T 10294-2008《绝热材料稳态热阻及有关特性的测定(防护热板法)》测定导热系数，实验步骤：试件尺寸为300*300mm，厚度为30mm，称试件重量，计算试件密度；开启电源，按图安装试件，夹持力设定在(9～18)kg范书内，测量试件厚度；设定热板温度、冷板温度。功率设定为自动功能，开始自动记录数据，待冷板、热板温度稳定后，初步估算功率。
根据GB/T 30804-2014《建筑用绝热制品垂直于表面抗拉强度的测定》测定抗拉强度，实验步骤：试样尺寸为300*300mm，厚度为30mm，将试样分别养护3天和28天，粘结在两刚性板或刚性块上，然后安装在试验机上，以恒定的速度进行拉伸试验直至破坏。
记录最大拉伸载荷，计算试样的抗拉强度。
根据上表中的数据，可以清楚得到以下结论：
1、与对比例1相比，实验例1-3中得到的复合岩棉板经过SiO2气凝胶改性后是完全疏水的，大大提高了复合岩棉板的疏水性能；
2、与实施例1-3相比，对比例1和对比例3所得的产物燃烧性能下降，可知本发明中含磷型超支化阻燃性聚氨酯材料能够提升复合岩棉板的防火阻燃性，降低导热系数从而达到保温的效果。
3、与对比例2相比，实施例1-3的抗拉强度升高，可知改性防水砂浆可以增加复合岩棉板的强度和弹性性能，延长使用年限。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程方法物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程方法物品或者设备所固有的要素。
最后应说明的是：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (9)

1.一种长效保温复合岩棉板的制备方法，其特征在于：包括以下步骤：
(1)制作改性岩棉板：用SiO2气凝胶对岩棉板进行改性处理；
(2)制作改性防水砂浆：由含磷型超支化阻燃性聚氨酯材料、砂和水泥混合均匀组成；
(3)制作复合岩棉板：在改性岩棉板上表面叠加平铺一层耐碱玻纤网格布，依次涂布界面剂、改性防水砂浆，干燥；将改性岩棉板下表面翻转，叠加平铺一层耐碱玻纤网格布，依次涂布界面剂、改性防水砂浆，干燥后，制得一个板材，通过层压机将板材保压成型。
2.根据权利要求1所述的一种长效保温复合岩棉板的制备方法，其特征在于：步骤(1)中改性岩棉板制备工艺如下：
(1)取正硅酸乙酯和异丙醇加入去离子水中，搅拌均匀后，逐滴加入HCl溶液，得到溶胶；接着加入氨水，持续搅拌，得到凝胶；把凝胶放入50～60℃水浴锅进行水浴老化24～48h，接着用去离子水水洗和无水乙醇醇洗12～24h，再离心，得到湿凝胶；将湿凝胶放入三甲基氯硅烷和正己烷混合液中浸泡12～24h，接着用正己烷洗涤三次，最后放入60～70℃的烘箱干燥24～48h，得到SiO2气凝胶；
(2)将SiO2气凝胶和乙醇混合制备成溶液作为改性剂，通过浸润的方法对岩棉进行改性，3～5min后取出，放置常温下干燥24～48h后，得到改性岩棉板。
3.根据权利要求1所述的一种长效保温复合岩棉板的制备方法，其特征在于：步骤(3)中改性防水砂浆制备工艺如下：
(1)将聚醚多元醇、含磷超支化阻燃剂和N,N-二甲基乙酰胺，混合均匀，在氮气氛围下，升温至70～80℃；再滴加经过N,N-二甲基乙酰胺溶解的二苯基甲烷二异氰酸酯，2～3h内加完，在60～80℃反应2～3h，然后再加入1，4-丁二醇，滴加经过N,N-二甲基乙酰溶解的二苯基甲烷二异氰酸酯，2～3h内加完，冷却出料，制得含磷型超支化阻燃性聚氨酯材料；
(2)将填料砂和水泥混合，加入含磷型超支化阻燃性聚氨酯材料，搅拌均匀后，得改性防水砂浆。
4.根据权利要求3所述的一种长效保温复合岩棉板的制备方法，其特征在于：所述步骤(1)含磷超支化阻燃剂的制备工艺如下：
(1)将水和无水乙醇混合均匀，加入四丙基氢氧化铵，二乙胺基甲基三乙氧基硅烷和苯胺甲基三甲氧基硅烷，反应10～12h，抽滤，真空干燥，得到含胺基的有机硅；
(2)向二异丙醇胺中滴加3-羟基苯二甲酸酐的二甲基甲酰胺溶液，常温反应2～3h；然后加入含胺基的有机硅和对甲苯磺酸，加热到120～130℃，保温6～8h，减压蒸馏，得超支化聚合物；
(3)加入超支化聚合物，升温到50～60℃，再加入聚磷酸试剂和对甲苯磺酸，混合均匀后升温到70～80℃，保温反应3～5h，水解2～3h，减压蒸馏，制备出含磷型超支化阻燃剂。
5.根据权利要求3所述的一种长效保温复合岩棉板的制备方法，其特征在于：所述步骤(1)中正硅酸乙酯、异丙醇与水的质量比为1：(1.15～1.2)：(0.35～0.52)。
6.根据权利要求2所述的一种长效保温复合岩棉板的制备方法，其特征在于：所述步骤(1)中聚醚多元醇与二苯基甲烷二异氰酸酯质量比为(5.6：1)～(6.3：1)。
7.根据权利要求2所述的一种长效保温复合岩棉板的制备方法，其特征在于：所述步骤(2)改性防水砂浆包括以下质量组分：12～20份阻燃性聚氨酯材料、40份砂、20份水泥。
8.根据权利要求3所述的一种长效保温复合岩棉板的制备方法，其特征在于：所述步骤(2)中3-羟基苯二甲酸酐与二异丙醇胺的质量比为(1：1)～(1：1.5)。
9.根据权利要求1-8任一项所述制备方法制得的一种长效保温复合岩棉板及其制备方法。
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CN117465104A (zh) * 2023-12-28 2024-01-30 优佰特(山东)新材料技术有限公司 一种介孔绝热材料聚氨酯拉挤复合型材

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CN117465104B (zh) * 2023-12-28 2024-03-12 优佰特(山东)新材料技术有限公司 一种介孔绝热材料聚氨酯拉挤复合型材

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