CN110952673A - 一种阻燃防氡保温墙体材料的制备方法 - Google Patents
一种阻燃防氡保温墙体材料的制备方法 Download PDFInfo
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- CN110952673A CN110952673A CN201911299719.9A CN201911299719A CN110952673A CN 110952673 A CN110952673 A CN 110952673A CN 201911299719 A CN201911299719 A CN 201911299719A CN 110952673 A CN110952673 A CN 110952673A
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- radon
- aerogel
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- cellulose ester
- retardant
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Abstract
本发明公开了一种阻燃防氡保温墙体材料的制备方法，本发明属于建材技术领域。本发明采用有机无机胶凝材料，其导热系数低、耐荷性好、抗弯强度高、不吸水、不腐烂、不虫蛀鼠咬、阻燃性好、耐温范围大，将生态材料及纳米吸附材料引入防氡辐射墙材的制备，得到了低成本高效的功能复合材料与技术，可以降低氡气的析出，具有更加经济实用和便于推广应用的优点因此，既具有优良的阻氡性能，又符合现有墙材的各项指标，具有应用性强、绿色环保、价格低、便于推广等特点。在核试验工程、国防工事以及工业和民用建筑工程中均可得到良好的应用，为解决我国建筑行业节能保温阻燃智能墙体材料瓶颈难题提供了有效途径。
Description
技术领域
本发明属于建材技术领域，尤其是一种阻燃防氡保温墙体材料的制备方法。
背景技术
氡是天然存在的气态惰性放射性核素，它无色、无味、无嗅，还可以进一步衰变产生28Po、2Pb、21Bi等子体，普遍存在于人类生活环境中。氡及其子体对人体的辐射伤害占人体所受到的全部环境辐射中的55%以上，会对人体造成极大的危害，极易引起肺癌，长期暴露于氡环境中，还可能引起骨髓性白血病、胃癌、肾癌、黑色素瘤等后果，是国际卫生组织规定的19种重要致癌物质之一。建筑墙体材料是室内氡放射污染的主要来源之一，目前在我国利用粉煤灰、煤渣等工业废料生产建筑材料是灰渣资源的主要用途，虽可提高废物利用率，减少环境污染，但易造成建筑工程的室内氡辐射污染，如粉煤灰和煤渣对煤中的天然放射性核素有富集作用，尤其对22Ra、32Th的富集程度可达4~5倍，导致粉煤灰、煤渣建筑材料具有明显的核辐射与氡辐射污染，硏究显示，掺粉煤灰新型墙体材料建造的房屋室内氡浓度远超过了“民用建筑工程室内环境污染控制规范”中的限制，因此，我们必须高度重视室内氡污染，并加强治理。在国内外相关技术中，建筑物防氡的研究多采用加强通风设施，其次是采用涂装的方法。氡污染控制方面，主要为国防和核工业中用大掺量重晶石和高分子材料或经过复杂的多层施工方法(如CN95110815，CN01106724，中国成果库94211702等报道)，在室内墙材氡污染控制方面，主要为采用环氧树脂等防氡涂料，虽然防氡辐射效果好，但成本高，资源的精细化利用技术低;也有主要成分是氯偏乳液的防氡涂料，但成本高，环保安全性差，且并不防火，而且必须经过涂装，减少了人们对于建材环境的可选择性。目前市场上鲜有防氡效果良好的墙体材料，或者并不具备防氡效果，而大幅度降低成本，安全环保就更可望而不可即，本领域技术人员亟待开发出一种阻燃防氡保温墙体材料的制备方法，满足更高的性能要求和广泛的市场需求。
发明内容
针对上述问题，本发明旨在提供一种阻燃防氡保温墙体材料的制备方法，使用寿命长，制备成本低，防氡保温效果好，而且阻燃。
本发明通过以下技术方案实现：
一种阻燃防氡保温墙体材料的制备方法，包括先制备改性纤维素酯气凝胶浸渍液，然后用改性纤维素酯气凝胶浸渍液浸渍岩棉板，具体为：
步骤一、制备改性纤维素酯气凝胶浸渍液
按重量份数计，将改性纤维素酯气凝胶50~60份、改性剂2~3份、表面活性剂2~4份、去离子水40~50份称取备用，将表面活性剂和去离子水加入到搅拌罐中，以500~800转/分的速度搅拌10~20分钟，使表面活性剂均匀分散在溶剂中；将纤维素酯气凝胶添加到搅拌好的表面活性剂和溶剂混合液中，以300~400转/分的速度搅拌10~20分钟，制备出分散均匀的纤维素酯气凝胶浸渍液；向分散均匀的纤维素酯气凝胶浸渍液中加入改性剂，以900~1000转/分的速度搅拌10~20分钟，制备出改性纤维素酯气凝胶浸渍液；
步骤二、用改性纤维素酯气凝胶浸渍液处理岩棉板：改性纤维素酯气凝胶浸渍液倒入加压浸渍机，将岩棉板全部浸润其中，50~60℃下，压力0.6~0.8MPa加压浸渍10~20min，置入烘箱中，在90~100℃的温度下将浸润改性纤维素酯气凝胶的岩棉板烘干24~48小时至完全干燥，即得到阻燃防氡保温墙体材料。
作为本发明的进一步方案，所述改性纤维素酯气凝胶的制备方法包括以下步骤：(1)将纤维素100~110份溶解于氢氧化锂/硫脲/水溶剂220~240份中，然后加入的十一碳烯酸20~30份和酯化酰氯55~60份、吡啶3~4份，温度50~60℃搅拌反应1~2h得改性纤维素后，加甲醇析出产物，经蒸馏水沉淀、无水乙醇洗涤、抽提、干燥得到纤维素脂肪酸酯；(2)将步骤(1)得到纤维素脂肪酸酯50~60份和聚乙二醇3~5份溶于丙酮70~80份中，将纤维素酯溶液置于冷冻干燥基内在-30℃，压力25Pa的冷冻干燥机中冷冻干燥48h，所述步骤(1)纤维素原料可为微晶纤维素、纤维素棉浆粕中的其中一种，所述步骤(1)酯化酰氯选自对甲苯磺酰氯、肉豆蔻酰氯、椰油酰氯中的其中一种；所述步骤(1)中纤维素长链脂肪酸酯的取代度为0.7~2.5，所述的氢氧化锂/硫脲/水溶剂中的氢氧化锂∶硫脲∶水的重量份数比为8.5∶6.5∶7.8，且该溶剂还添加有质量分数2.5~3.5的氧化锌，所述聚乙二醇为分子量1800~2200的直链聚乙二醇。
作为本发明的进一步方案，所述改性剂为3-氨丙基三羟基硅烷、双-[γ-(三乙氧基硅)丙基]四硫化物的其中一种。
作为本发明的进一步方案，所述表面活性剂为聚乙烯吡咯烷酮、聚乙烯内酰胺、聚乙烯基苄基三甲胺盐中的其中一种。
本发明的有益效果：
本发明从《国语·周语上》:“防民之口，甚于防川。川壅(堵塞)而溃，伤人必多，民亦如之。”得到哲学原理启示。古人千百年前的哲学智慧也需要现今人们的传承和挖掘。川壅(堵塞)而溃，伤人必多，以往的防氡技术或涂料涂装防氡技术采用环氧树脂、聚氨酯、偏氯乳液等高分子材料，通过交联固化形成的漆膜具有良好的密实性，能够短时间阻止墙体材料中的氡向室内扩散，但是随着时间的推移，涂层不可避免的老化和性能下降，墙体材料中的氡依然会像室内扩散，可以说是“川壅(堵塞)而溃，伤人必多，涂料亦如之。”而且无论涂层是否致密，其并不会具备很好的保温效果，本发明公开的阻燃防氡保温墙体材料不仅具备良好的防氡效果，还具备良好的保温性能和阻燃能力，通过气凝胶的在岩棉基体中的分散，提高岩棉板的强度和保温性能，而且进一步提墙材的阻燃能力，而且提高材料的防氡能力。
相比现有技术本发明具有如下优点：
在氡污染控制方面，现有技术大多采用大掺量重晶石或经过复杂的多层施工方法，而环氧树脂等防氡涂料，虽然防氡辐射效果好，但时效短，成本高，资源的精细化利用技术低;也有主要成分是氯偏乳液的防氡涂料，但成本高，环保安全性差，涂层表面极易老化，老化后防氡效果不理想。本发明公开的阻燃防氡墙材具有体积、厚度、比重明显降低，综合经济技术水平达到国内领先水平，将生态材料及纳米吸附材料引入防氡辐射墙材的制备，得到了低成本高效的功能复合材料与技术，与现有的法相比，采用本发明公开的阻燃防氡墙材，可以降低氡气的析出，具有更加经济实用和便于推广应用的优点因此，既具有优良的阻氡性能，又符合现有墙材的各项指标。具有应用性强、价格低、便于推广等特点。在核试验工程、国防工事以及工业和民用建筑工程中均可得到良好的应用。
具体实施方式
下面用具体实施例说明本发明，但并不是对本发明的限制。
实施例1
一种阻燃防氡保温墙体材料的制备方法，包括先制备改性纤维素酯气凝胶浸渍液，然后用改性纤维素酯气凝胶浸渍液浸渍岩棉板，具体为：
步骤一、制备改性纤维素酯气凝胶浸渍液
按重量份数计，将改性纤维素酯气凝胶50份、改性剂2份、表面活性剂2份、去离子水40份称取备用，将表面活性剂和去离子水加入到搅拌罐中，以500转/分的速度搅拌10分钟，使表面活性剂均匀分散在溶剂中；将纤维素酯气凝胶添加到搅拌好的表面活性剂和溶剂混合液中，以300转/分的速度搅拌10分钟，制备出分散均匀的纤维素酯气凝胶浸渍液；向分散均匀的纤维素酯气凝胶浸渍液中加入改性剂，以1000转/分的速度搅拌20分钟，制备出改性纤维素酯气凝胶浸渍液；
步骤二、用改性纤维素酯气凝胶浸渍液处理岩棉板：改性纤维素酯气凝胶浸渍液倒入加压浸渍机，将岩棉板全部浸润其中，50℃下，压力0.6MPa加压浸渍10min，置入烘箱中，在100℃的温度下将浸润改性纤维素酯气凝胶的岩棉板烘干24小时至完全干燥，即得到阻燃防氡保温墙体材料。
作为本发明的进一步方案，所述改性纤维素酯气凝胶的制备方法包括以下步骤：(1)将纤维素110份溶解于氢氧化锂/硫脲/水溶剂220份中，然后加入的十一碳烯酸30份和酯化酰氯60份、吡啶4份，温度50℃搅拌反应1h得改性纤维素后，加甲醇析出产物，经蒸馏水沉淀、无水乙醇洗涤、抽提、干燥得到纤维素脂肪酸酯；(2)将步骤(1)得到纤维素脂肪酸酯60份和聚乙二醇5份溶于丙酮80份中，将纤维素酯溶液置于冷冻干燥基内在-30℃，压力25Pa的冷冻干燥机中冷冻干燥48h，所述步骤(1)纤维素原料可为微晶纤维素，所述步骤(1)酯化酰氯选对甲苯磺酰氯；所述步骤(1)中纤维素长链脂肪酸酯的取代度为2.5，所述的氢氧化锂/硫脲/水溶剂中的氢氧化锂∶硫脲∶水的重量份数比为8.5∶6.5∶7.8，且该溶剂还添加有质量分数3.5的氧化锌，所述聚乙二醇为分子量1800的直链聚乙二醇。
作为本发明的进一步方案，所述改性剂为3-氨丙基三羟基硅烷。
作为本发明的进一步方案，所述表面活性剂为聚乙烯吡咯烷酮。
实施例2
一种阻燃防氡保温墙体材料的制备方法，包括先制备改性纤维素酯气凝胶浸渍液，然后用改性纤维素酯气凝胶浸渍液浸渍岩棉板，具体为：
步骤一、制备改性纤维素酯气凝胶浸渍液
按重量份数计，将改性纤维素酯气凝胶60份、改性剂3份、表面活性剂4份、去离子水50份称取备用，将表面活性剂和去离子水加入到搅拌罐中，以800转/分的速度搅拌20分钟，使表面活性剂均匀分散在溶剂中；将纤维素酯气凝胶添加到搅拌好的表面活性剂和溶剂混合液中，以400转/分的速度搅拌20分钟，制备出分散均匀的纤维素酯气凝胶浸渍液；向分散均匀的纤维素酯气凝胶浸渍液中加入改性剂，以1000转/分的速度搅拌20分钟，制备出改性纤维素酯气凝胶浸渍液；
步骤二、用改性纤维素酯气凝胶浸渍液处理岩棉板：改性纤维素酯气凝胶浸渍液倒入加压浸渍机，将岩棉板全部浸润其中，60℃下，压力0.8MPa加压浸渍20min，置入烘箱中，在100℃的温度下将浸润改性纤维素酯气凝胶的岩棉板烘干24小时至完全干燥，即得到阻燃防氡保温墙体材料。
作为本发明的进一步方案，所述改性纤维素酯气凝胶的制备方法包括以下步骤：(1)将纤维素110份溶解于氢氧化锂/硫脲/水溶剂240份中，然后加入的十一碳烯酸30份和酯化酰氯60份、吡啶4份，温度60℃搅拌反应2h得改性纤维素后，加甲醇析出产物，经蒸馏水沉淀、无水乙醇洗涤、抽提、干燥得到纤维素脂肪酸酯；(2)将步骤(1)得到纤维素脂肪酸酯60份和聚乙二醇5份溶于丙酮80份中，将纤维素酯溶液置于冷冻干燥基内在-30℃，压力25Pa的冷冻干燥机中冷冻干燥48h，所述步骤(1)纤维素原料可为微晶纤维素中的其中一种，所述步骤(1)酯化酰氯选自对肉豆蔻酰氯；所述步骤(1)中纤维素长链脂肪酸酯的取代度为2.5，所述的氢氧化锂/硫脲/水溶剂中的氢氧化锂∶硫脲∶水的重量份数比为8.5∶6.5∶7.8，且该溶剂还添加有质量分数3.5的氧化锌，所述聚乙二醇为分子量2200的直链聚乙二醇。
作为本发明的进一步方案，所述改性剂为双-[γ-(三乙氧基硅)丙基]四硫化物。
作为本发明的进一步方案，所述表面活性剂为聚乙烯基苄基三甲胺盐。
对比例1
本对比例1与实施例2相比，在步骤一中省去改性纤维素酯气凝胶，即墙体材料中不含有改性纤维素酯气凝胶，除此外的方法步骤均相同。
对比例2
本对比例2与实施例2相比，在步骤一中省去改性剂，除此外的方法步骤均相同。
对实施例1-2和对比例1~2的阻燃防氡保温墙体材料进行性能测试，测试结果见表1
表1实施例和对比例的阻燃防氡保温墙体材料性能测定结果
注：尺寸允许偏差按GB/T25975规定的方法进行导热系数按GB/T102的方法进行垂直于板面方向的抗拉强度压缩强度按GB/T25975规定的方法进酸度系数按GB/T5480规定的方法进行。短期吸水量质量吸湿奉僧水率按GB/T109规定的方法进行燃烧性能按GB8624-2012规定的方法进行；GB/T8624-2012建筑材料及制品燃烧性能分级GB/T10294-2008绝热材料稳态热阻及有关特性的测定防护热板法GB/T10299-2011绝热材料僧水性试验方法GB/T19686-2005建筑用岩棉、矿渣棉绝热制品GB/T25975-2010建筑外墙外保温用岩棉制品。JG/T420203硬泡聚氨酯板薄抹灰外墙外保温系统材料防氡效率试验使用核工业北京地质研究院公司环境氡测量仪FD216进行测试；（1）降低仪器本底:打开仪器电源开关，在待机状态下按“设置”键检查“氡浓度”测量参数:充气时间10min，测量时间20min，排气时间1min，之后按“确定”返回初始界面；然后用气管将高纯氮气入仪器进气口，打开氮气瓶阀门:仪器选择“空气氡”键，进行连续测量，每次测量结束后LCD(液晶)屏显示氡浓度值，当氡浓度值小于10Bq/m3时，按“退出”键停止测量；（2）测空白氡析出率J0:将氡源平放，用氡聚集罩将氡源罩住，四周密封，24h后打开仪器电源开关在待机状态下检查“氡析出率”参数设置:充气时间3min，测量时间13mim，排气时间4min，之后按“确定”返回初始界面;按“氡析出率”键，仪器提示输入密封时间，依次按下“0”、“0”、“3”、“0”数字键，然后按“确认”键，仪器自动开始测量，测量结束后读取氡析出率J0；（3）记录数值后，关闭仪器，打开氡聚集罩，实验室条件下放置24h；（4）降低仪器本底:重复本章节步骤（1）；（5）测防氡材料试件氡析出率:将氡源平放，将实施例和对比例防氡材料覆盖在氡源上，并用氡聚集罩扣严，四周密封，然后按照本章节步骤（2）进行操作，测量结束后读取氡析出率值五按公式(2)计算防氡效率η=（J0-J1）/J0×100%式中η-防氧效率，未使用防氡材料的空白析出率，J0/(m2·s)—一使用防氡材料后的析出率J1/(m2·s)。
Claims (4)
1.一种阻燃防氡保温墙体材料的制备方法，其特征在于，包括含以下步骤：先制备改性纤维素酯气凝胶浸渍液，然后用改性纤维素酯气凝胶浸渍液浸渍岩棉板，具体为：
步骤一、制备改性纤维素酯气凝胶浸渍液
（按重量份数计，将改性纤维素酯气凝胶50~60份、改性剂2~3份、表面活性剂2~4份、去离子水40~50份称取备用，将表面活性剂和去离子水加入到搅拌罐中，以500~800转/分的速度搅拌10~20分钟，使表面活性剂均匀分散在溶剂中；将纤维素酯气凝胶添加到搅拌好的表面活性剂和溶剂混合液中，以300~400转/分的速度搅拌10~20分钟，制备出分散均匀的纤维素酯气凝胶浸渍液；向分散均匀的纤维素酯气凝胶浸渍液中加入改性剂，以900~1000转/分的速度搅拌10~20分钟，制备出改性纤维素酯气凝胶浸渍液；
步骤二、用改性纤维素酯气凝胶浸渍液处理岩棉板：改性纤维素酯气凝胶浸渍液倒入加压浸渍机，将岩棉板全部浸润其中，50~60℃下，压力0.6~0.8MPa加压浸渍10~20min，置入烘箱中，在90~100℃的温度下将浸润改性纤维素酯气凝胶的岩棉板烘干24~48小时至完全干燥，即得到阻燃防氡保温墙体材料。
2.根据权利要求1所述的一种阻燃防氡保温墙体材料的制备方法，其特征在于，改性纤维素酯气凝胶的制备方法包括以下步骤：(1)将纤维素100~110份溶解于氢氧化锂/硫脲/水溶剂220~240份中，然后加入的十一碳烯酸20~30份和酯化酰氯55~60份、吡啶3~4份，温度50~60℃搅拌反应1~2h得改性纤维素后，加甲醇析出产物，经蒸馏水沉淀、无水乙醇洗涤、抽提、干燥得到纤维素脂肪酸酯；(2)将步骤(1)得到纤维素脂肪酸酯50~60份和聚乙二醇3~5份溶于丙酮70~80份中，将纤维素酯溶液置于冷冻干燥基内在-30℃，压力25Pa的冷冻干燥机中冷冻干燥48h，所述步骤(1)纤维素原料可为微晶纤维素、纤维素棉浆粕中的其中一种，所述步骤(1)酯化酰氯选自对甲苯磺酰氯、肉豆蔻酰氯、椰油酰氯中的其中一种；所述步骤(1)中纤维素长链脂肪酸酯的取代度为0.7~2.5，所述的氢氧化锂/硫脲/水溶剂中的氢氧化锂∶硫脲∶水的重量份数比为8.5∶6.5∶7.8，且该溶剂还添加有质量分数2.5~3.5的氧化锌，所述聚乙二醇为分子量1800~2200的直链聚乙二醇。
3.根据权利要求1所述的一种阻燃防氡保温墙体材料的制备方法，其特征在于，所述改性剂为3-氨丙基三羟基硅烷、双-[γ-(三乙氧基硅)丙基]四硫化物的其中一种。
4.根据权利要求1所述的一种阻燃防氡保温墙体材料的制备方法，其特征在于，所述表面活性剂为聚乙烯吡咯烷酮、聚乙烯内酰胺、聚乙烯基苄基三甲胺盐中的其中一种。
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