CN114835446B - 一种保温陶粒混凝土材料及其制备方法 - Google Patents
一种保温陶粒混凝土材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种保温陶粒混凝土材料及其制备方法,涉及混凝土技术领域。本发明先将硅酸四苯酯和铝酸三甲酯混合进行一次煅烧,形成二氧化硅气凝胶、氧化铝和碳纳米线,制备得到复合陶粒;再将五氯化磷、复合陶粒、轻砂、水泥、生石灰和水混合,制备得到陶粒混凝土基料;最后,利用聚丙烯基苯甲酸甲酰胺进行二次煅烧,形成以环磷腈为中心的聚丙烯网络,部分聚丙烯网络煅烧形成致密碳层和氮气,致密碳层还原氧化铝形成的铝和氮气反应,形成氮化铝晶粒,制备得到保温陶粒混凝土材料;本发明制备得到的保温陶粒混凝土材料具备良好的保温性能、阻燃性能、抗龟裂性能和韧性。
Description
技术领域
本发明涉及混凝土技术领域,具体为一种保温陶粒混凝土材料及其制备方法。
背景技术
混凝土是由凝胶材料、骨料和水按适当比例配置,再经过一定时间硬化而成的复合材料的统称,是世界上使用量最大的人工土木建筑材料。常见的凝胶材料为水泥,常见的骨料为石子、砂子。混凝土的硬度高、原料来源广泛、成本低廉,广泛使用于房屋、公路、军事工程、核能发电厂等构造物。
随着社会的发展和生活水平的快速提升,人们对建筑物的要求提高,混凝土逐渐朝着轻质保温的方向发展,其中,陶粒混凝土是以陶粒代替石子作为混凝土的骨料而制成的混凝土,因其结构疏松多孔所以质轻且保温,是一种轻骨料混凝土,因此,它也从当前众多混凝土材料中脱颖而出,被广泛应用于建筑领域。
但是现有技术中的陶粒混凝土,在日常使用过程中常常会出现龟裂、老化脱粉等现象,并且其耐火性也不够高,存在较多的安全隐患,较大程度上影响了它的应用。本发明关注到了这一现状,并通过制备一种保温陶粒混凝土材料来解决这些问题。
发明内容
本发明的目的在于提供一种保温陶粒混凝土材料及其制备方法,以解决现有技术中存在的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种保温陶粒混凝土材料,所述保温陶粒混凝土材料是利用聚丙烯基苯甲酸甲酰胺对陶粒混凝土基料进行二次煅烧制备得到。
进一步的,所述陶粒混凝土基料是将五氯化磷、复合陶粒、轻砂、生石灰、水泥和水混合制备得到。
进一步的,所述复合陶粒是将硅酸四苯酯和铝酸三甲酯混合后进行一次煅烧制备得到。
一种保温陶粒混凝土材料的制备方法,所述保温陶粒混凝土材料的制备方法包括以下制备步骤:
(1)将复合陶粒、轻砂、生石灰、水泥和60~80℃去离子水按质量比1:0.3:0.14:0.7:1.1~1:0.5:0.16:0.9:1.3混合,以4500~5000r/min剪切4~6h,随后加入复合陶粒质量0.6~0.8倍的五氯化磷剪切4~6h,在48~52℃下浇筑到模具中固定4~6h后,在80~90℃下烘23~25h,得到陶粒混凝土基料;
(2)在室温和氩气保护条件下,将陶粒混凝土基料放入3~5MPa的密闭容器中,倒入陶粒混凝土基料质量0.4~0.6倍的聚丙烯基苯甲酸甲酰胺,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置1~3h,随后按质量比1:8~1:12加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.01~0.016倍,以30~40kHz超声10~20min,再在2400~2500MHz、700~900W微波条件下微波处理15~25min,加入陶粒混凝土基料质量0.01~0.03倍的硫酸二甲酯,继续微波处理30~50min,脱模,放入0.7~0.9MPa的反应釜中,以9~11℃/min升温至660~680℃,保温2~6h后升温至1200~1400℃,保温4~10h,制备得到陶粒混凝土材料。
进一步的,步骤(1)所述复合陶粒的制备方法如下:将复合溶胶放入-4~-2℃冰箱中冷冻47~49h,在10~20Pa、-50~-40℃下干燥47~49h,用无水乙醇洗涤2~4次,放入10~20Pa、19~21℃的烘箱中烘1~3h,再浸渍于复合溶胶质量0.2~0.3倍的质量分数为10%的硝酸镍溶液中10~20h,捞出后放入0.7~0.9MPa的反应釜中,以9~11℃/min升温至690~710℃,保温1~3h后升温至1300~1500℃,保温1~3h,自然冷却至常温,随后用无水乙醇洗涤3~5次,放入30~40℃烘箱烘1~3h,制备得到复合陶粒。
进一步的,所述复合溶胶的制备方法如下:在80~90℃和氩气保护条件下,将铝酸三甲酯和去离子水按质量比1:7~1:9混合,以400~600r/min搅拌1~3h,以40~60滴/min滴加铝酸三甲酯质量0.2~0.3倍的质量分数为11~13%的硝酸溶液,继续搅拌1~3h,加入铝酸三甲酯质量0.01~0.03倍的银,以9~11℃/min升温至500~560℃保温8~10h,再以9~11℃/min降温至24~26℃,加入铝酸三甲酯质量2~4倍的硅酸四苯酯,继续滴加铝酸三甲酯质量8~16倍的乙醇,在60~80℃下继续搅拌2~4h,加入铝酸三甲酯质量0.08~0.16倍氢氧化铵,继续搅拌10~20min,以2~4℃/min升温至65~85℃,继续搅拌10~20min,继续升温至95~105℃,以600~800r/min搅拌60~80min,制备得到复合溶胶。
进一步的,步骤(1)所述轻砂是细度模数为1.6、表观密度为2870kg/m3的天然河砂。
进一步的,步骤(2)所述聚丙烯基苯甲酸甲酰胺的制备方法如下:在室温和氩气保护条件下,将丙烯基苯甲酸和甲酰胺按质量比1:0.6~1:0.8混合,以400~600r/min搅拌20~30min,随后加入丙烯基苯甲酸质量0.06~0.08倍的纳米二氧化钛,以9~10℃/min升温至80~100℃,继续搅拌2~4h,制备得到聚丙烯基苯甲酸甲酰胺。
进一步的,所述聚丙烯基苯甲酸的制备方法如下:室温和氩气保护条件下,将氯代聚丙烯和苯甲酸按质量比1:3~1:5混合,以400~600r/min搅拌10~20min,加入氯代聚丙烯质量0.01~0.03倍的三氯化铝,以2~4℃/min降温至0~4℃,以600~800r/min搅拌7~9h,制备得到聚丙烯基苯甲酸。
进一步的,所述氯代聚丙烯分子量为1000~3000。
与现有技术相比,本发明所达到的有益效果是:
本发明在制备保温陶粒混凝土材料时,先将硅酸四苯酯和铝酸三甲酯混合进行一次煅烧,制备得到复合陶粒;再将五氯化磷、复合陶粒、轻砂、水泥、生石灰和水混合,制备得到陶粒混凝土基料;最后利用聚丙烯基苯甲酸甲酰胺对陶粒混凝土基料进行二次煅烧,制备得到保温陶粒混凝土材料。
首先,硅酸四苯酯和铝酸三甲酯水解、脱去苯酚和甲醇后反应交联,形成二氧化硅气凝胶和氧化铝,增强了复合陶粒的保温性能;甲醇氧化形成甲醛,与苯酚反应交联,形成酚醛网络,酚醛网络碳化后在复合陶粒中形成大量碳纳米线,当产生微裂纹和残余应力时,可以将裂纹钉扎在一起,从而增强了复合陶粒的韧性。
其次,部分五氯化磷水解,形成磷酸和氯化氢,磷酸活化陶粒混凝土基料,在陶粒混凝土基料中形成大量羟基等自由基,聚丙烯基苯甲酸甲酰胺水解,形成甲酰胺和聚丙烯基苯甲酸,甲酰胺分解与氯化氢反应形成氯化铵,氯化铵和部分五氯化磷反应形成六氯环磷腈,增强了保温陶粒混凝土材料的阻燃性能;聚丙烯基苯甲酸上的羧基和陶粒混凝土基料中羟基反应交联,六氯环磷腈和聚丙烯基苯甲酸上的苯环反应交联形成以环磷腈为中心的聚丙烯网络,煅烧时,部分聚丙烯网络中环磷腈为酸源和气源、聚丙烯基苯甲酸为碳源,在陶粒混凝土基料中形成致密碳层和大量氮气,碳层将复合陶粒中的氧化铝还原成铝,部分熔化的铝从复合陶粒中流出与氮气反应形成氮化铝晶粒,将复合陶粒和水泥基料稳固地嵌合在一起,增强了保温陶粒混凝土材料的抗龟裂性能。
具体实施方式
下面将结合本发明实施例,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。
为了更清楚的说明本发明提供的方法通过以下实施例进行详细说明,在将以下实施例中制备得到的保温陶粒混凝土材料的各指标测试方法如下:
保温性能:取相同质量的实施例和对比例制备得到的保温陶粒混凝土材料按照GB/T10295标准法来测定导热系数来测定保温性能。
阻燃性能:取相同质量的实施例和对比例制备得到的保温陶粒混凝土材料按照GB/T29051标准法测试氧指数来测定阻燃性。
抗龟裂性能:取相同长度和宽度的实施例和对比例制备得到的保温陶粒混凝土材料按照GB/T50081标准法测定劈裂抗拉强度来测定抗龟裂性能。
韧性:取相同长度和宽度的实施例和对比例制备得到的超细晶钛基高塑性陶瓷材料按照ASTMC1421测试断裂韧性。
实施例1
一种保温陶粒混凝土材料的制备方法,所述保温陶粒混凝土材料的制备方法包括以下制备步骤:
(1)在80℃和氩气保护条件下,将铝酸三甲酯和去离子水按质量比1:7混合,以400r/min搅拌1h,以40滴/min滴加铝酸三甲酯质量0.2倍的质量分数为11%的硝酸溶液,继续搅拌1h,加入铝酸三甲酯质量0.01倍的银,以9℃/min升温至500℃保温8h,再以9℃/min降温至24℃,加入铝酸三甲酯质量2倍的硅酸四苯酯,继续滴加铝酸三甲酯质量8倍的乙醇,在60℃下继续搅拌2h,加入铝酸三甲酯质量0.08倍氢氧化铵,继续搅拌10min,以2℃/min升温至65℃,继续搅拌10min,继续升温至95℃,以600r/min搅拌60min,制备得到复合溶胶;将复合溶胶放入-4℃冰箱中冷冻47h,在10Pa、-50℃下干燥47h,用无水乙醇洗涤2次,放入10Pa、19℃的烘箱中烘1h,再浸渍于复合溶胶质量0.2倍的质量分数为10%的硝酸镍溶液中10h,捞出后放入0.7MPa的反应釜中,以9℃/min升温至690℃,保温1h后升温至1300℃,保温1h,自然冷却至常温,随后用无水乙醇洗涤3次,放入30℃烘箱烘1h,制备得到复合陶粒;
(2)将复合陶粒、轻砂、生石灰、水泥和60℃去离子水按质量比1:0.3:0.14:0.7:1.1混合,以4500r/min剪切4h,随后加入复合陶粒质量0.6倍的五氯化磷剪切4h,在48℃下浇筑到模具中固定4h后,在80℃下烘23h,得到陶粒混凝土基料;
(3)室温和氩气保护条件下,将分子量为1000的氯代聚丙烯和苯甲酸按质量比1:3混合,以400r/min搅拌10min,加入氯代聚丙烯质量0.01倍的三氯化铝,以2℃/min降温至0℃,以600r/min搅拌7h,制备得到聚丙烯基苯甲酸;在室温和氩气保护条件下,将丙烯基苯甲酸和甲酰胺按质量比1:0.6混合,以400r/min搅拌20min,随后加入丙烯基苯甲酸质量0.06倍的纳米二氧化钛,以9℃/min升温至80℃,继续搅拌2h,制备得到聚丙烯基苯甲酸甲酰胺;在室温和氩气保护条件下,将陶粒混凝土基料放入3MPa的密闭容器中,倒入陶粒混凝土基料质量0.4倍的聚丙烯基苯甲酸甲酰胺,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置1h,随后按质量比1:8加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.01倍,以30kHz超声10min,再在2400MHz、700W微波条件下微波处理15min,加入陶粒混凝土基料质量0.01倍的硫酸二甲酯,继续微波处理30min,脱模,放入0.7MPa的反应釜中,以9℃/min升温至660℃,保温2h后升温至1200℃,保温4h,制备得到陶粒混凝土材料。
实施例2
一种保温陶粒混凝土材料的制备方法,所述保温陶粒混凝土材料的制备方法包括以下制备步骤:
(1)在85℃和氩气保护条件下,将铝酸三甲酯和去离子水按质量比1:8混合,以500r/min搅拌2h,以50滴/min滴加铝酸三甲酯质量0.25倍的质量分数为12%的硝酸溶液,继续搅拌2h,加入铝酸三甲酯质量0.02倍的银,以10℃/min升温至530℃保温9h,再以10℃/min降温至25℃,加入铝酸三甲酯质量3倍的硅酸四苯酯,继续滴加铝酸三甲酯质量12倍的乙醇,在70℃下继续搅拌3h,加入铝酸三甲酯质量0.12倍氢氧化铵,继续搅拌15min,以3℃/min升温至75℃,继续搅拌15min,继续升温至100℃,以700r/min搅拌70min,制备得到复合溶胶;将复合溶胶放入-3℃冰箱中冷冻48h,在15Pa、-45℃下干燥48h,用无水乙醇洗涤3次,放入15Pa、20℃的烘箱中烘2h,再浸渍于复合溶胶质量0.25倍的质量分数为10%的硝酸镍溶液中15h,捞出后放入0.8MPa的反应釜中,以10℃/min升温至700℃,保温2h后升温至1400℃,保温2h,自然冷却至常温,随后用无水乙醇洗涤4次,放入35℃烘箱烘2h,制备得到复合陶粒;
(2)将复合陶粒、轻砂、生石灰、水泥和70℃去离子水按质量比1:0.4:0.15:0.8:1.2混合,以4750r/min剪切5h,随后加入复合陶粒质量0.7倍的五氯化磷剪切5h,在50℃下浇筑到模具中固定5h后,在85℃下烘24h,得到陶粒混凝土基料;
(3)室温和氩气保护条件下,将分子量为2000的氯代聚丙烯和苯甲酸按质量比1:4混合,以500r/min搅拌15min,加入氯代聚丙烯质量0.02倍的三氯化铝,以3℃/min降温至2℃,以700r/min搅拌8h,制备得到聚丙烯基苯甲酸;在室温和氩气保护条件下,将丙烯基苯甲酸和甲酰胺按质量比1:0.7混合,以500r/min搅拌25min,随后加入丙烯基苯甲酸质量0.07倍的纳米二氧化钛,以9.5℃/min升温至90℃,继续搅拌3h,制备得到聚丙烯基苯甲酸甲酰胺;在室温和氩气保护条件下,将陶粒混凝土基料放入4MPa的密闭容器中,倒入陶粒混凝土基料质量0.5倍的聚丙烯基苯甲酸甲酰胺,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置2h,随后按质量比1:10加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.013倍,以35kHz超声15min,再在2450MHz、800W微波条件下微波处理20min,加入陶粒混凝土基料质量0.02倍的硫酸二甲酯,继续微波处理40min,脱模,放入0.8MPa的反应釜中,以10℃/min升温至670℃,保温4h后升温至1300℃,保温7h,制备得到陶粒混凝土材料。
实施例3
一种保温陶粒混凝土材料的制备方法,所述保温陶粒混凝土材料的制备方法包括以下制备步骤:
(1)在90℃和氩气保护条件下,将铝酸三甲酯和去离子水按质量比1:9混合,以600r/min搅拌3h,以60滴/min滴加铝酸三甲酯质量0.3倍的质量分数为13%的硝酸溶液,继续搅拌3h,加入铝酸三甲酯质量0.03倍的银,以11℃/min升温至560℃保温10h,再以11℃/min降温至26℃,加入铝酸三甲酯质量4倍的硅酸四苯酯,继续滴加铝酸三甲酯质量16倍的乙醇,在80℃下继续搅拌4h,加入铝酸三甲酯质量0.16倍氢氧化铵,继续搅拌20min,以4℃/min升温至85℃,继续搅拌20min,继续升温至105℃,以800r/min搅拌80min,制备得到复合溶胶;将复合溶胶放入-2℃冰箱中冷冻49h,在20Pa、-40℃下干燥49h,用无水乙醇洗涤4次,放入20Pa、21℃的烘箱中烘3h,再浸渍于复合溶胶质量0.3倍的质量分数为10%的硝酸镍溶液中20h,捞出后放入0.9MPa的反应釜中,以11℃/min升温至710℃,保温3h后升温至1500℃,保温3h,自然冷却至常温,随后用无水乙醇洗涤5次,放入40℃烘箱烘3h,制备得到复合陶粒;
(2)将复合陶粒、轻砂、生石灰、水泥和80℃去离子水按质量比1:0.5:0.16:0.9:1.3混合,以5000r/min剪切6h,随后加入复合陶粒质量0.8倍的五氯化磷剪切6h,在52℃下浇筑到模具中固定6h后,在90℃下烘25h,得到陶粒混凝土基料;
(3)室温和氩气保护条件下,将分子量为3000的氯代聚丙烯和苯甲酸按质量比1:5混合,以600r/min搅拌20min,加入氯代聚丙烯质量0.03倍的三氯化铝,以4℃/min降温至4℃,以800r/min搅拌9h,制备得到聚丙烯基苯甲酸;在室温和氩气保护条件下,将丙烯基苯甲酸和甲酰胺按质量比1:0.8混合,以600r/min搅拌30min,随后加入丙烯基苯甲酸质量0.08倍的纳米二氧化钛,以10℃/min升温至100℃,继续搅拌4h,制备得到聚丙烯基苯甲酸甲酰胺;在室温和氩气保护条件下,将陶粒混凝土基料放入5MPa的密闭容器中,倒入陶粒混凝土基料质量0.6倍的聚丙烯基苯甲酸甲酰胺,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置3h,随后按质量比1:12加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.016倍,以40kHz超声20min,再在2500MHz、900W微波条件下微波处理25min,加入陶粒混凝土基料质量0.03倍的硫酸二甲酯,继续微波处理50min,脱模,放入0.9MPa的反应釜中,以11℃/min升温至680℃,保温6h后升温至1400℃,保温10h,制备得到陶粒混凝土材料。
对比例1
对比例1与实施例2的区别仅在于步骤(1)的不同,将步骤(1)修改为:在85℃和氩气保护条件下,将铝酸三甲酯和去离子水按质量比1:8混合,以500r/min搅拌2h,以50滴/min滴加铝酸三甲酯质量0.25倍的质量分数为12%的硝酸溶液,继续搅拌2h,加入铝酸三甲酯质量0.02倍的银,以10℃/min升温至530℃保温9h,再以10℃/min降温至25℃,继续滴加铝酸三甲酯质量12倍的乙醇,在70℃下继续搅拌3h,加入铝酸三甲酯质量0.12倍氢氧化铵,继续搅拌15min,以3℃/min升温至75℃,继续搅拌15min,继续升温至100℃,以700r/min搅拌70min,制备得到复合溶胶;将复合溶胶放入-3℃冰箱中冷冻48h,在15Pa、-45℃下干燥48h,用无水乙醇洗涤3次,放入15Pa、20℃的烘箱中烘2h,再浸渍于复合溶胶质量0.25倍的质量分数为10%的硝酸镍溶液中15h,捞出后放入0.8MPa的反应釜中,以10℃/min升温至700℃,保温2h后升温至1400℃,保温2h,自然冷却至常温,随后用无水乙醇洗涤4次,放入35℃烘箱烘2h,制备得到复合陶粒。其余制备步骤同实施例2。
对比例2
对比例2与实施例2的区别仅在于步骤(1)的不同,将步骤(1)修改为:在25℃下,将硅酸四苯酯和乙醇按质量比1:4混合,以500r/min搅拌25min,随后以50滴/min滴加硅酸四苯酯质量0.25倍的质量分数为12%的硝酸溶液,在85℃下继续搅拌3h,自然冷却至室温,制备得到复合溶胶;将复合溶胶放入-3℃冰箱中冷冻48h,在15Pa、-45℃下干燥48h,用无水乙醇洗涤3次,放入15Pa、20℃的烘箱中烘2h,再浸渍于复合溶胶质量0.25倍的质量分数为10%的硝酸镍溶液中15h,捞出后放入0.8MPa的反应釜中,以10℃/min升温至700℃,保温2h后升温至1400℃,保温2h,自然冷却至常温,随后用无水乙醇洗涤4次,放入35℃烘箱烘2h,制备得到复合陶粒。其余制备步骤同实施例2。
对比例3
一种保温陶粒混凝土材料的制备方法,所述保温陶粒混凝土材料的制备方法包括以下制备步骤:
(1)将页岩陶粒、轻砂、生石灰、水泥和70℃去离子水按质量比1:0.4:0.15:0.8:1.2混合,以4750r/min剪切5h,随后加入页岩陶粒质量0.7倍的五氯化磷剪切5h,在50℃下浇筑到模具中固定5h后,在85℃下烘24h,得到陶粒混凝土基料;
(2)室温和氩气保护条件下,将分子量为2000的氯代聚丙烯和苯甲酸按质量比1:4混合,以500r/min搅拌15min,加入氯代聚丙烯质量0.02倍的三氯化铝,以3℃/min降温至2℃,以700r/min搅拌8h,制备得到聚丙烯基苯甲酸;在室温和氩气保护条件下,将丙烯基苯甲酸和甲酰胺按质量比1:0.7混合,以500r/min搅拌25min,随后加入丙烯基苯甲酸质量0.07倍的纳米二氧化钛,以9.5℃/min升温至90℃,继续搅拌3h,制备得到聚丙烯基苯甲酸甲酰胺;在室温和氩气保护条件下,将陶粒混凝土基料放入4MPa的密闭容器中,倒入陶粒混凝土基料质量0.5倍的聚丙烯基苯甲酸甲酰胺,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置2h,随后按质量比1:10加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.013倍,以35kHz超声15min,再在2450MHz、800W微波条件下微波处理20min,加入陶粒混凝土基料质量0.02倍的硫酸二甲酯,继续微波处理40min,脱模,放入0.8MPa的反应釜中,以10℃/min升温至670℃,保温4h后升温至1300℃,保温7h,制备得到陶粒混凝土材料。
对比例4
对比例4与实施例2的区别仅在于步骤(2)的不同,将步骤(2)修改为:将复合陶粒、轻砂、生石灰、水泥和70℃去离子水按质量比1:0.4:0.15:0.8:1.2混合,以4750r/min剪切5h,在50℃下浇筑到模具中固定5h后,在85℃下烘24h,得到陶粒混凝土基料。其余制备步骤同实施例2。
对比例5
对比例5与实施例2的区别仅在于步骤(3)的不同,将步骤(3)修改为:在室温和氩气保护条件下,将陶粒混凝土基料放入4MPa的密闭容器中,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置2h,随后按质量比1:10加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.013倍,以35kHz超声15min,再在2450MHz、800W微波条件下微波处理20min,加入陶粒混凝土基料质量0.02倍的硫酸二甲酯,继续微波处理40min,脱模,放入0.8MPa的反应釜中,以10℃/min升温至670℃,保温4h后升温至1300℃,保温7h,制备得到陶粒混凝土材料。其余制备步骤同实施例2。
对比例6
对比例6与实施例2的区别仅在于步骤(3)的不同,将步骤(3)修改为:室温和氩气保护条件下,将分子量为2000的氯代聚丙烯和苯甲酸按质量比1:4混合,以500r/min搅拌15min,加入氯代聚丙烯质量0.02倍的三氯化铝,以3℃/min降温至2℃,以700r/min搅拌8h,制备得到聚丙烯基苯甲酸;在室温和氩气保护条件下,将丙烯基苯甲酸和甲酰胺按质量比1:0.7混合,以500r/min搅拌25min,随后加入丙烯基苯甲酸质量0.07倍的纳米二氧化钛,以9.5℃/min升温至90℃,继续搅拌3h,制备得到聚丙烯基苯甲酸甲酰胺;在室温和氩气保护条件下,将陶粒混凝土基料放入4MPa的密闭容器中,倒入陶粒混凝土基料质量0.5倍的聚丙烯基苯甲酸甲酰胺,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置2h,随后按质量比1:10加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.013倍,以35kHz超声15min,再在2450MHz、800W微波条件下微波处理20min,加入陶粒混凝土基料质量0.02倍的硫酸二甲酯,继续微波处理40min,脱模,制备得到陶粒混凝土材料。其余制备步骤同实施例2。
效果例
下表1给出了采用本发明实施例1至3与对比例1至6制备得到的保温陶粒混凝土材料的保温性能、阻燃性能、抗龟裂性能和韧性的分析结果。
表1
从表1中可发现实施例1、2、3制备得到的保温陶粒混凝土材料的保温性能、阻燃性能、抗龟裂性能和韧性较强;从实施例1、2、3和对比例1的实验数据比较可发现,使用硅酸四苯酯制备复合陶粒,可以在复合陶粒中形成碳纳米线和二氧化硅气凝胶,制备得到的保温陶粒混凝土材料的保温性和韧性较强;从实施例1、2、3和对比例2的实验数据可发现,使用铝酸三甲酯制备复合陶粒,可以在复合陶粒中形成碳纳米线,后续制备保温陶粒混凝土材料时,可以形成氮化铝晶粒,制备得到的保温陶粒混凝土材料的韧性和抗龟裂性能较强;从实施例1、2、3和对比例3的实验数据可发现,使用硅酸四苯酯和铝酸三甲酯制备的复合陶粒制备保温陶粒混凝土材料,可以形成碳纳米线和氮化铝晶粒,制备得到韧性和抗龟裂性能较强;从实施例1、2、3和对比例4的实验数据可发现,使用五氯化磷制备保温陶粒混凝土材料,可以形成以环磷腈为中心的聚丙烯网络和氮化铝晶粒,制备得到的保温陶粒混凝土材料的阻燃性能和抗龟裂性能较强;从实施例1、2、3和对比例5的实验数据可发现,使用聚丙烯基苯甲酸甲酰胺制备保温陶粒混凝土材料,可以形成以环磷腈为中心的聚丙烯网络和氮化铝晶粒,制备得到的保温陶粒混凝土材料的阻燃性能和抗龟裂性能较强;从实施例1、2、3和对比例6实验数据可发现,利用二次煅烧制备保温陶粒混凝土材料,可以形成氮化铝晶粒,制备得到的保温陶粒混凝土材料的抗龟裂性能较强。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何标记视为限制所涉及的权利要求。
Claims (4)
1.一种保温陶粒混凝土材料的制备方法,其特征在于,所述保温陶粒混凝土材料的制备方法包括以下制备步骤:
(1)将复合陶粒、轻砂、生石灰、水泥和60~80℃去离子水按质量比1:0.3:0.14:0.7:1.1~1:0.5:0.16:0.9:1.3混合,以4500~5000r/min剪切4~6h,随后加入复合陶粒质量0.6~0.8倍的五氯化磷剪切4~6h,在48~52℃下浇筑到模具中固定4~6h后,在80~90℃下烘23~25h,得到陶粒混凝土基料;
(2)室温和氩气保护条件下,将氯化聚丙烯和苯甲酸按质量比1:3~1:5混合,以400~600r/min搅拌10~20min,加入氯化聚丙烯质量0.01~0.03倍的三氯化铝,以2~4℃/min降温至0~4℃,以600~800r/min搅拌7~9h,制备得到聚丙烯基苯甲酸;在室温和氩气保护条件下,将聚丙烯基苯甲酸和甲酰胺按质量比1:0.6~1:0.8混合,以400~600r/min搅拌20~30min,随后加入聚丙烯基苯甲酸质量0.06~0.08倍的纳米二氧化钛,以9~10℃/min升温至80~100℃,继续搅拌2~4h,制备得到聚丙烯基苯甲酸甲酰胺;在室温和氩气保护条件下,将陶粒混凝土基料放入3~5MPa的密闭容器中,倒入陶粒混凝土基料质量0.4~0.6倍的聚丙烯基苯甲酸甲酰胺,以60滴/min滴加质量分数为30%的氢氧化钠溶液,调节pH至9,静置1~3h,随后按质量比1:8~1:12加入氧化锌和吡啶,氧化锌的质量是陶粒混凝土基料的质量的0.01~0.016倍,以30~40kHz超声10~20min,再在2400~2500MHz、700~900W微波条件下微波处理15~25min,加入陶粒混凝土基料质量0.01~0.03倍的硫酸二甲酯,继续微波处理30~50min,脱模,放入0.7~0.9MPa的反应釜中,以9~11℃/min升温至660~680℃,保温2~6h后升温至1200~1400℃,保温4~10h,制备得到陶粒混凝土材料。
2.根据权利要求1所述的一种保温陶粒混凝土材料的制备方法,其特征在于,步骤(1)所述复合陶粒的制备方法如下:在80~90℃和氩气保护条件下,将铝酸三甲酯和去离子水按质量比1:7~1:9混合,以400~600r/min搅拌1~3h,以40~60滴/min滴加铝酸三甲酯质量0.2~0.3倍的质量分数为11~13%的硝酸溶液,继续搅拌1~3h,加入铝酸三甲酯质量0.01~0.03倍的银,以9~11℃/min升温至500~560℃保温8~10h,再以9~11℃/min降温至24~26℃,加入铝酸三甲酯质量2~4倍的硅酸四苯酯,继续滴加铝酸三甲酯质量8~16倍的乙醇,在60~80℃下继续搅拌2~4h,加入铝酸三甲酯质量0.08~0.16倍氢氧化铵,继续搅拌10~20min,以2~4℃/min升温至65~85℃,继续搅拌10~20min,继续升温至95~105℃,以600~800r/min搅拌60~80min,制备得到复合溶胶;将复合溶胶放入-4~-2℃冰箱中冷冻47~49h,在10~20Pa、-50~-40℃下干燥47~49h,用无水乙醇洗涤2~4次,放入10~20Pa、19~21℃的烘箱中烘1~3h,再浸渍于复合溶胶质量0.2~0.3倍的质量分数为10%的硝酸镍溶液中10~20h,捞出后放入0.7~0.9MPa的反应釜中,以9~11℃/min升温至690~710℃,保温1~3h后升温至1300~1500℃,保温1~3h,自然冷却至常温,随后用无水乙醇洗涤3~5次,放入30~40℃烘箱烘1~3h,制备得到复合陶粒。
3.根据权利要求1所述的一种保温陶粒混凝土材料的制备方法,其特征在于,步骤(1)所述轻砂是细度模数为1.6、表观密度为2870kg/m3的天然河砂。
4.根据权利要求1所述的一种保温陶粒混凝土材料的制备方法,其特征在于,步骤(2)所述氯化聚丙烯分子量为1000~3000。
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CN110451864A (zh) * | 2019-09-18 | 2019-11-15 | 湖北昌耀新材料股份有限公司 | 磷石膏免烧陶粒轻集料及其制备方法 |
CN112919924B (zh) * | 2021-04-12 | 2022-12-16 | 毕节市通发电力电杆有限公司 | 一种高强度的轻质混凝土及制备方法 |
CN113501698A (zh) * | 2021-08-18 | 2021-10-15 | 广州中创建筑科技有限公司 | 一种轻骨料混凝土 |
CN114455887B (zh) * | 2022-03-25 | 2023-01-17 | 中咨数据有限公司 | 一种高强沥青混凝土及其制备方法 |
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