CN111471359A - 一种广谱高发射颗粒材料的制备方法及应用 - Google Patents
一种广谱高发射颗粒材料的制备方法及应用 Download PDFInfo
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
本发明涉及一种广谱高发射颗粒材料的制备方法及应用,其制备方法包括:1)制备硅前驱体和铝前驱体;2)制备硅铝酸盐水合凝胶;3)硅铝酸盐水合凝胶水热晶化;4)得到无功耗制冷粉体;5)制得无功耗制冷颗粒。本方法制备的广谱高发射颗粒材料在无功耗制冷涂料领域,或者无功耗制冷薄膜领域中的应用。本发明方法制得的颗粒产品本身具备可见‑近红外高反射、中远红外高发射性能,相较于以上提到的辐射制冷材料,无需额外的结构设计就能实现较好的辐射制冷效果的广谱高发射颗粒材料的制备方法;同时该材料具有独特的微孔结构,具备一定的隔热性能;而且原材料容易获得、工艺简单、生产成本较低。
Description
技术领域
本发明涉及被动式无功耗制冷技术领域,特别指一种广谱高发射颗粒材料的制备方法及应用。
背景技术
由科学家对大气广谱透过性的分析可知,大气层对不同波长的电磁波有不同的透射率。透射率较高的波段称为“大气窗口”,例如:0.3~2.5μm、3.2~4.8μm、8~13μm等。其中8~13μm波段是人民最感兴趣的,因为这个波段的透过率是最大的,同时常温下的黑体辐射主要集中在这一波段。地表上的物体热能就是通过辐射换热的方式,将自身热量以电磁波的形式,通过8~13μm的“大气窗口”波段排放到温度接近绝零度的外部太空,达到自身冷却的目的。通常把这种完全以辐射方式将热量释放到宇宙空间的制冷方式成为“辐射制冷”。
人们对辐射制冷的研究几十年前就已经开始,之前的研究大多数都集中在夜间的辐射制冷,实用价值不高。但要实现全天候的辐射制冷,对材料的光谱要求非常苛刻,因为白天有太阳辐射存在,太阳的辐射能有5%在紫外波段(200~400nm);45%在可见光波段(400~780nm);50%在近红外波段(780~2500nm)。当太阳的能量作用在物体表面时,会被物体吸收而产生大量的热量,为了减少因太阳辐射而产生的热量,这就要求材料在紫外-可见-近红外波段的具有非常高的反射率(接近100%)。
目前能实现全天候辐射制冷并且能够大规模、长时间应用的材料在国际上才刚刚起步。
关于辐射制冷材料的制备与研究主要集中在光子晶体结构设计以及超材料结构设计上。如2014年斯坦福大学范善辉教授团队的研究A.P.Raman,M.A.Anoma,L.Zhu,E.Rephaeli,S.Fan,Passive radiative cooling below ambient air temperatureunder direct sunlight.Nature 515,540–544(2014)。团队设计并制备出了多达九层纳米薄膜的光子晶体结构。该光子晶体辐射制冷器件能够反射97%以上的太阳能量,且在8~14μm“大气窗口”内的发射率超过0.7,在850W/m2的太阳直射下的净辐射功率超过了40W/m2,具有很好的辐射制冷效果。但是该光子晶体辐射制冷器的设计结构复杂、制备精度控制要求高、制备成本高昂,无法产业化。2017年美国科罗拉多大学杨荣贵教授团队的研究Y.Zhai,Y.Ma,S.N.David,D.Zhao,R.Lou,G.Tan,R.Yang,X.Yin,Scalable-manufacturedrandomized glass-polymer hybrid metamaterial for daytime radiativecooling.Science 355,1062–1066(2017)。团队设计并制备了基于二氧化硅玻璃微珠和TPX高分子基材的超材料。该超材料虽然结构简单、制备成本有所降低,但其对于反射层的反射率要求太高,对于大规模应用来说,成本还是偏高。
发明内容
本发明的目的是针对背景技术中存在的缺点和问题加以改进和创新,提供一种本身具备可见-近红外高反射、中远红外高发射性能的广谱高发射颗粒材料的制备方法。同时该颗粒材料内部具有独特的介孔结构,具备一定的隔热性能。
本发明的另一目的是提供上述方法制备的颗粒材料的应用。
本发明的制备方法包括以下步骤:
1)制备硅前驱体和铝前驱体,即将硅源和铝源分别制成溶液。
2)制备硅铝酸盐水合凝胶,将去离子水、氢氧化钠和上述硅前驱体、铝前驱体按照Na2O:Al2O3:SiO2:H2O=1~6:1~2:1~20:5~200的比例混合均匀,调节体系的pH至2~10,形成硅铝酸盐水合凝胶。
3)硅铝酸盐水合凝胶水热晶化,上述硅铝酸水合凝胶在室温下胶化0.1~2.0小时后加入导向剂,快速升温至60~200℃,恒温静态晶化0.5~20小时。
4)后处理,将上述晶化产物过滤分离,用水和乙醇进行洗涤,洗涤至pH为7~11后放入真空干燥箱内,在50~300℃内干燥1~48小时,得到无功耗制冷粉体。
5)制得无功耗制冷颗粒:取8~30份无功耗制冷粉体、1~7份钛酸钾晶须、1~10份竹纤维、1~5份硅烷偶联剂通过高速混合机混合均匀;80~150度烘干1~5小时;烘干后的混合物与50~100份的氟碳树脂熔融共混,于110~270度挤出造粒,粉碎成0.1~100μm颗粒。
优选的,所述的硅源为水玻璃、硅酸钠、硅溶胶、白炭黑、正硅酸乙酯、正硅酸甲酯中的一种或者多种。
优选的,所述的铝源为偏铝酸钠、拟薄水铝石、三水铝石、异丙醇铝、硝酸铝、金属铝粉中的一种或者多种。
优选的,所述的导向剂为CTAB、CTAC、三乙烯四胺、四甲基乙二胺中的一种或者多种。
本发明方法制备的广谱高发射颗粒材料在无功耗制冷涂料领域中的应用,涂料可涂覆于各种纤维布料、金属板材、陶瓷材料、塑料板材、玻璃、混凝土、防水卷材等表面。
优选的,涂料配方按照重量份计,包括:高分子成膜物质40~60份、分散剂0.5~3份、成膜助剂2~7份、增稠剂0.1~5份、流平剂0.1~4份、消泡剂0.4~7份、pH调节剂0.1~10份、无功耗制冷颗粒13~20份。
优选的,应用中所用高分子成膜物质是丙烯酸乳液、氟碳乳液、苯丙乳液、有机硅树脂、环氧树脂、聚氨酯中的一种或者多种。
优选的,所述分散剂为HY-304、BYK-2015、DM分散剂、PEG600、EBS分散剂。
优选的,所述成膜助剂由乙二醇、丙二醇、醇脂十二的混合物组成,其组成为1~5:2~3:1~5中的任意比例。
优选的,所述增稠剂为PU增稠剂、聚丙烯酰胺增稠剂中的一种。
本发明方法制备的广谱高发射颗粒材料在无功耗制冷薄膜领域中的应用,该无功耗制冷薄膜依次包括反射层、粘结层和功能层,其中功能层是由广谱高发射颗粒材料作为功能填料均匀分散在高分子基材中。
优选的,功能层的厚度为1~5000μm中的任意一种厚度,功能层的成膜工艺为吹膜成型、流延成型、浇筑成型中的任意一种。
优选的,所用高分子基材是丙烯酸聚酯、氟碳树脂、聚乙烯、三元乙丙橡胶、聚苯乙烯、聚氯乙烯、TPO、聚丙烯、涤纶聚酯、PBT、TPX中的一种或者多种的组合。
优选的,所述反射层为基于高分子聚合物薄膜的镀银或者镀铝,所述金属镀银、镀铝的厚度在10~1000nm之间的任意一厚度,所述高分子聚合物为PET、PE、PMMA、PC、PP,所述镀银或者镀铝是化学方法或是物理方法。
优选的,所述粘结层可以是PU粘合剂、UV粘合剂、乙烯-醋酸乙烯共聚物热熔胶。
本发明的优点及有益效果:
1、本发明材料同时具备可见光-近红外波段高反射(反射率大于95%)、中远红外波段高发射(发射率大于0.9)的特性,能够将太阳能量反射回去的同时将自身内部的热量以红外辐射的方式通过“大气窗口”辐射到外太空,不需要额外的结构设计就能实现较好的辐射制冷效果。
2、本发明材料具备优异的光谱性能的同时还具有独特的介孔结构,具有一定的隔热性能,在建筑节能以及中央空调节能领域具有很大的应用前景。
3、本发明涉及的颗粒材料制备方法原材料容易获得、工艺简单、生产成本较低、能够根据需求有效调控颗粒颗粒尺寸。
附图说明
图1为实例1可见光-近红外反射光谱。
图2为实例1中远红外发射光谱。
图3为实例1电镜照片。
图4为实例1孔径分布曲线。
图5为实例2可见光-近红外反射光谱。
图6为实例2中远红外发射光谱。
图7为实例2电镜照片。
图8为实例2孔径分布曲线。
图9为实例3可见光-近红外反射曲线。
图10为实例3中远红外发射曲线。
图11为实例3电镜照片。
图12为实例3孔径分布曲线。
具体实施方式
为便于理解本发明,下面给出了本发明的几个实施例。但是,本发明可以以许多不同的形式来实现,并不限于本文所描述的实施例。相反地,提供这些实施例的目的是使对本发明的公开内容更加透彻全面。
除非另有定义,本文中所使用的所有的技术和科学术语与本发明的技术领域的技术人员通常理解的含义相同。说明书中所使用的术语只是为了描述具体的实施目的,不是旨在于限制本发明。
实施例1:
1、制备硅前驱体,即将硅源配制成溶液,具体方法如下:称取50g的硅钠比为2.5的工业用硅酸钠(Na2O·5SiO2),用去离子水稀释到比重为1.2,再通过高温蒸汽加热0.5小时,使用上部的清液作为硅前驱体,清液的浓度约为0.1mol/L。
2、制备铝前驱体,将铝源分别配制成溶液,具体方法如下:将78g固体氢氧化钠加水溶解,配制成含Na2O 1.5mol/L的氢氧化钠溶液,加热至沸腾,按Na2O/Al2O3=2.0的比例,在不断搅拌下慢慢加入Al(OH)3,待Al(OH)3全部溶解后,停止加热,并加水稀释,冷却到50℃左右,得到铝前驱体,其化学反应式如下:
12Al(OH)3+12NaOH→12NaAl(OH)4
3、初始凝胶形成:将去离子水、上述氢氧化钠溶液、上述硅前驱体溶液、上述铝前驱体溶液按照Na2O:Al2O3:SiO2:H2O=3:1:2:185的比例混合均匀,先将铝前驱体溶液、氢氧化钠溶液和去离子水放入反应釜中,在搅拌状态下降反应釜内溶液预热到30℃,再将硅前驱体溶液快速倒入,继续搅拌30min,调节体系的pH至7~10,形成硅铝酸盐水合凝胶。
4、硅铝酸盐水合凝胶水热晶化:称取7.29g CTAB溶解于100mL的去离子水中,不断搅拌形成透明液体,得到CTAB溶液。将上步制得的硅铝酸水合凝胶在室温下胶化2小时后加入CTAB,调节体系pH至6~10,快速升温至150℃,并在150℃条件下恒温静态晶化15小时。
5、后处理得广谱高发射粉体:晶化反应结束后,将上产物过滤分离,用水和乙醇分别洗涤至pH=8后放入真空干燥箱内,在220℃内干燥24小时得广谱高发射粉体。
6、制得无功耗制冷颗粒:30份无功耗制冷粉体、7份钛酸钾晶须、6份竹纤维、5份硅烷偶联剂通过高速混合机混合均匀;100度烘干1小时;烘干后的混合物与100份的氟碳树脂熔融共混,于270度挤出造粒,粉碎成8μm颗粒。
本实施例制备的广谱高发射颗粒的可见光-近红外反射率为0.98,“大气窗口”(8~14μm)波段发射率为0.93,平均粒径为150nm,平均孔径为17nm。
本实例产品送检情况见图1-4。
实施例2:
1、制备硅前驱体,即将硅源配制成溶液,具体方法如下:将80g固体氢氧化钠加水溶解,配制成含Na2O 1.5mol/L的氢氧化钠溶液,称取41.6g正硅酸乙酯,逐滴加入到氢氧化钠溶液中,加入200mL的无水乙醇,搅拌1h,得到硅前驱体溶液。
2、制备铝前驱体,将铝源分别配制成溶液,具体方法如下:将80g固体氢氧化钠加水溶解,配制成含Na2O 1.5mol/L的氢氧化钠溶液,加热至沸腾,按Na2O/Al2O3=2.0的比例,在不断搅拌下慢慢加入Al(OH)3,待Al(OH)3全部溶解后,停止加热,并加水稀释,冷却到50℃左右,得到铝前驱体,其化学反应式如下:
12Al(OH)3+12NaOH→12NaAl(OH)4
3、初始凝胶形成:将去离子水、上述氢氧化钠溶液、上述硅前驱体溶液、上述铝前驱体溶液按照Na2O:Al2O3:SiO2:H2O=2:1.2:9:135的比例混合均匀,先将铝前驱体溶液、氢氧化钠溶液和去离子水放入反应釜中,在搅拌状态下降反应釜内溶液预热到30℃,再将硅前驱体溶液快速倒入,继续搅拌30min,调节体系的pH至6~9,形成硅铝酸盐水合凝胶。
4、硅铝酸盐水合凝胶水热晶化:称取20.8g四甲基乙二胺溶解于100mL的去离子水中,不断搅拌形成透明液体,得到四甲基乙二胺溶液。将上步制得的硅铝酸水合凝胶在室温下胶化1小时后加入四甲基乙二胺溶液,调节体系pH至6~10,快速升温至185℃,并在185℃条件下恒温静态晶化8小时。
5、后处理得广谱高发射粉体:晶化反应结束后,将上产物过滤分离,用水和乙醇分别洗涤至pH=8后放入真空干燥箱内,在220℃内干燥24小时得广谱高发射粉体。
6、制得无功耗制冷颗粒:20份无功耗制冷粉体、4份钛酸钾晶须、4份竹纤维、3份硅烷偶联剂通过高速混合机混合均匀;120度烘干2小时;烘干后的混合物与80份的氟碳树脂熔融共混,于250度挤出造粒,粉碎成30μm颗粒。
本实施例制备的广谱高发射颗粒的可见光-近红外反射率为0.97,“大气窗口”(8~14μm)波段发射率为0.90,平均粒径为100nm,平均孔径为10nm。
本实例产品送检情况见图5-8。
本发明制备的广谱高发射颗粒材料应用在无功耗制冷薄膜中,本颗粒作为功能填料,可选树脂为丙烯酸聚酯、氟碳树脂、聚乙烯、聚苯乙烯、聚氯乙烯、聚丙烯、涤纶聚酯、PBT、TPX。
实施例3:
1、制备硅前驱体,即将硅源配制成溶液,具体方法如下:将80g固体氢氧化钠加水溶解,配制成含Na2O 1.5mol/L的氢氧化钠溶液,称取30.4g正硅酸甲酯,逐滴加入到氢氧化钠溶液中,加入200mL的无水乙醇,搅拌1h,得到硅前驱体溶液。
2、制备铝前驱体,将铝源分别配制成溶液,具体方法如下:将80g固体氢氧化钠加水溶解,配制成含Na2O 1.5mol/L的氢氧化钠溶液,加热至沸腾,按Na2O/Al2O3=2.0的比例,在不断搅拌下慢慢加入Al(OH)3,待Al(OH)3全部溶解后,停止加热,并加水稀释,冷却到50℃左右,得到铝前驱体,其化学反应式如下:
12Al(OH)3+12NaOH→12NaAl(OH)4
3、初始凝胶形成:将去离子水、上述氢氧化钠溶液、上述硅前驱体溶液、上述铝前驱体溶液按照Na2O:Al2O3:SiO2:H2O=4.68:1:10:180的比例混合均匀,先将铝前驱体溶液、氢氧化钠溶液和去离子水放入反应釜中,在搅拌状态下降反应釜内溶液预热到30℃,再将硅前驱体溶液快速倒入,继续搅拌30min,调节体系的pH至9~10,形成硅铝酸盐水合凝胶。
4、硅铝酸盐水合凝胶水热晶化:称取20.8g四甲基乙二胺溶解于100mL的去离子水中,不断搅拌形成透明液体,得到四甲基乙二胺溶液。将上步制得的硅铝酸水合凝胶在室温下胶化1小时后加入四甲基乙二胺溶液,调节体系pH至6~10,快速升温至185℃,并在185℃条件下恒温静态晶化8小时。
5、后处理得广谱高发射粉体:晶化反应结束后,将上产物过滤分离,用水和乙醇分别洗涤至pH=8后放入真空干燥箱内,在220℃内干燥24小时得广谱高发射粉体。
6、制得无功耗制冷颗粒:15份无功耗制冷粉体、6份钛酸钾晶须、8份竹纤维、3份硅烷偶联剂通过高速混合机混合均匀;90度烘干3.5小时;烘干后的混合物与95份的氟碳树脂熔融共混,于190度挤出造粒,粉碎成2μm颗粒。
本实施例制备的广谱高发射颗粒的可见光-近红外反射率为0.95,“大气窗口”(8~14μm)波段发射率为0.90,平均粒径为200nm,平均孔径为5nm。
本实例产品送检情况见图9-12。
实施例4:
本发明制备的广谱高发射颗粒材料应用于无功耗制冷涂料中,本颗粒产品作为功能填料,涂料配方按照重量份计,包括:苯丙乳液60份、分散剂3份、成膜助剂7份、增稠剂5份、流平剂3份、消泡剂5份、pH调节剂3份、无功耗制冷颗粒20份。其中:分散剂为BYK-2015,成膜助剂由重量比为2:3:3的乙二醇、丙二醇、醇脂十二混合物,增稠剂为PU增稠剂。
上述涂料可涂覆于各种纤维布料、金属板材、陶瓷材料、塑料、玻璃、混凝土、防水卷材等表面。
实施例5:
本发明方法制备的广谱高发射颗粒材料应用于无功耗制冷薄膜领域中,具体应用时本发明广谱高发射颗粒作为功能填料,无功耗制冷薄膜反射层为采用物理镀膜法制备的PET/Al薄膜,粘结层为PU粘合剂,功能层所用的高分子基材为聚乙烯。
具体制备方法如下:将聚乙烯与广谱高发射颗粒通过高速混合机搅拌充分混合,然后将混合物料放于烘箱中,100度下烘6小时,然后将烘干的物料利用双螺杆挤出机加工成粒料,然后用单螺杆挤出机挤出流延成膜,收卷待用。采用连续磁控溅射的方法在PET薄膜表面镀一层500nm厚的Al膜,镀膜完成后收卷待用,最后将反射层和功能层通过乙烯-醋酸乙烯共聚物热熔胶粘结层热压复合得到无功耗制冷薄膜。
本发明所述的实施例仅仅是对本发明的优选实施方式进行的描述,并非对本发明构思和范围进行限定,在不脱离本发明设计思想的前提下,本领域中工程技术人员对本发明的技术方案作出的各种变型和改进,均应落入本发明的保护范围,本发明请求保护的技术内容,已经全部记载在权利要求书中。
Claims (10)
1.一种广谱高发射颗粒材料的制备方法,其特征在于包括以下步骤:
1)制备硅前驱体和铝前驱体,即将硅源和铝源分别制成溶液;
2)制备硅铝酸盐水合凝胶,将去离子水、氢氧化钠和上述硅前驱体、铝前驱体按照Na2O:Al2O3:SiO2:H2O=1~6:1~2:1~20:5~200的比例混合均匀,调节体系的pH至2~10,形成硅铝酸盐水合凝胶;
3)硅铝酸盐水合凝胶水热晶化,上述硅铝酸水合凝胶在室温下胶化0.1~2.0小时后加入导向剂,快速升温至60~200℃,恒温静态晶化0.5~20小时;
4)后处理,将上述晶化产物过滤分离,用水和乙醇进行洗涤,洗涤至pH为7~11后放入真空干燥箱内,在50~300℃内干燥1~48小时,得到无功耗制冷粉体;
5)制得无功耗制冷颗粒:取8~30份无功耗制冷粉体、1~7份钛酸钾晶须、1~10份竹纤维、1~5份硅烷偶联剂通过高速混合机混合均匀;80~150度烘干1~5小时;烘干后的混合物与50~100份的氟碳树脂熔融共混,于110~270度挤出造粒,粉碎成0.1~100μm颗粒。
2.根据权利要求1所述的广谱高发射颗粒材料的制备方法,其特征在于所述的硅源为水玻璃、硅酸钠、硅溶胶、白炭黑、正硅酸乙酯、正硅酸甲酯中的一种或者多种。
3.根据权利要求1所述的广谱高发射颗粒材料的制备方法,其特征在于所述的铝源为偏铝酸钠、拟薄水铝石、三水铝石、异丙醇铝、硝酸铝、金属铝粉中的一种或者多种。
4.根据权利要求1所述的广谱高发射颗粒材料的制备方法,其特征在于所述的导向剂为CTAB、CTAC、三乙烯四胺、四甲基乙二胺中的一种或者多种。
5.权利要求1-4所述的任一方法制备的广谱高发射颗粒材料在无功耗制冷涂料领域的应用,或者无功耗制冷薄膜领域中的应用。
6.根据权利要求5所述的广谱高发射颗粒材料在无功耗制冷涂料领域的应用,其特征在于:涂料配方按照重量份计,包括:高分子成膜物质40~60份、分散剂0.5~3份、成膜助剂2~7份、增稠剂0.1~5份、流平剂0.1~4份、消泡剂0.4~7份、pH调节剂0.1~10份、无功耗制冷颗粒13~20份。
7.根据权利要求6所述的广谱高发射颗粒材料在无功耗制冷涂料领域的应用,其特征在于:应用中所用高分子成膜物质是丙烯酸乳液、氟碳乳液、苯丙乳液、有机硅树脂、环氧树脂、聚氨酯中的一种或者多种。
8.根据权利要求5所述的广谱高发射颗粒材料在无功耗制冷薄膜领域中的应用,其特征在于:无功耗制冷薄膜依次包括反射层、粘结层和功能层,其中功能层是由广谱高发射颗粒材料作为功能填料均匀分散在高分子基材中。
9.根据权利要求8所述的广谱高发射颗粒材料在无功耗制冷薄膜领域中的应用,其特征在于:功能层的厚度为1~5000μm中的任意一种厚度,功能层的成膜工艺为吹膜成型、流延成型、浇筑成型中的任意一种。
10.根据权利要求8所述的广谱高发射颗粒材料在无功耗制冷薄膜领域中的应用,其特征在于:所用高分子基材是丙烯酸聚酯、氟碳树脂、聚乙烯、三元乙丙橡胶、聚苯乙烯、聚氯乙烯、TPO、聚丙烯、涤纶聚酯、PBT、TPX中的一种或者多种的组合。
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