CN111471321B - 一种多孔轻质二氧化硅填料的制备方法 - Google Patents
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Abstract
本发明公开了一种多孔轻质二氧化硅填料的制备方法,涉及无机材料技术领域,包括以下制备步骤:(1)制浆清洗;(2)冷冻浓缩;(3)烘干煅烧;(4)破碎分级;(5)高温喷烧;(6)浮选分级。本发明制备的二氧化硅具有轻质、多孔、高强度、比表面积低、吸油值低的特点,尤其是材料的强度远远高于空心玻璃微珠等空心材料;并且制备方法易实现工业化,解决了玻璃微珠加工过程中容易破碎,破碎后失去减重和降低介电常数的问题;同时制备的二氧化硅具有球形形貌,有利于在树脂基体中的大比例填充,从而改善树脂基体的刚度、强度、耐热性、耐磨性、耐腐蚀性及机械加工性等。
Description
技术领域:
本发明涉及无机材料技术领域,具体涉及一种多孔轻质二氧化硅填料的制备方法。
背景技术:
多孔轻质二氧化硅填料具有低密度、良好的稳定性、低介电常数等特点,随着5G产业的兴起,得到了越来越广泛的应用。多孔轻质二氧化硅应用于覆铜板行业,可以代替现有的空心玻璃微珠,降低介电常数和比重,除此之外,还可以提高板材强度。同时,多孔轻质二氧化硅填料还可以应用于多孔保温板材、保温陶瓷涂料、低价开口剂、涂料消光剂、LOW-α二氧化硅等。
轻量化是涉及到电子行业的共同话题,轻量化的诸多优点决定了轻质填料巨大的市场前景,轻质二氧化硅是目前市场上应用最广泛的轻质填料之一。多孔轻质二氧化硅不仅能降低应用体系的比重,同时由于多孔结构,材料中间包含的空气,可大大地提高材料的绝缘性,从而降低体系的介电常数。但是,要实现以上材料的优越性,要求多孔轻质二氧化硅要具有高的强度和良好的加工性能。目前,空心玻璃微珠是广泛应用的轻质材料之一,但是由于其强度有限,往往在加工过程中产生大量的碎片,从而给材料的强度和加工性带来负面影响。白炭黑也是一种高端的轻质材料,但由于比表面积高,粒度小等特点,在体系中的添加量十分有限,并且会降低体系强度。所以,要得到良好的应用,要求轻质二氧化硅要有高的强度和低的比表面积。
目前,多孔轻质二氧化硅填料的规模生产工艺还处于不断开发阶段,仍然存在着大量技术难点,如何高质量、低成本和大批量地制备多孔轻质二氧化硅填料,保证填料的分散性和溶剂相容性是当前的研究热点。
专利CN103342368A提供了一种空心二氧化硅微球的制备方法,利用复合碱液和润湿添加剂,将实心二氧化硅腐蚀制备成空心二氧化硅,此方法能够得到轻质的空心二氧化硅球,但是所得二氧化硅比重难以控制,壳层薄,强度低,废料难以回收,难以实现产业化。
专利CN106430222A提供了一种纳米二氧化硅微球及其制备方法,利用聚合物核体为模板,聚烷氧基硅氧烷为硅源,在水相中反应后再去除聚合物核体,形成轻质二氧化硅球,此方法操作复杂,成本高,难以实现产业化。
发明内容:
本发明所要解决的技术问题在于提供一种多孔轻质二氧化硅填料的制备方法,制得的二氧化硅具有轻质、多孔、高强度、比表面积低、吸油值低的特点,并且制备方法易实现工业化,制备的多孔轻质二氧化硅填料具有球形形貌,有利于在树脂基体中的大比例填充,从而改善树脂基体的加工和应用性能。
本发明所要解决的技术问题采用以下的技术方案来实现:
一种多孔轻质二氧化硅填料的制备方法,包括以下制备步骤:
(1)制浆清洗:将白炭黑制浆,添加硅溶胶,离子清洗至电导率<50μS/cm,去除杂质离子;
(2)冷冻浓缩:经离子清洗后将浆料放入冷冻设备中,冷冻至完全冻住,提高温度使浆料完全融化,去除上层清液后再次放入冷冻设备中,重复前述冷冻和解冻操作1-10次,浓缩抽滤;
(3)烘干煅烧:滤饼烘干后煅烧;
(4)破碎分级:煅烧产物破碎、研磨、过气流磨、分级,粒度在10-150um;
(5)高温闪烧:将粉体用氧气气体载气通入闪烧炉,在高温区域通过气流循环闪烧,得到半成品;
(6)浮选分级:分选出所需粒径,即得成品。
所述白炭黑选用沉淀白炭黑或气相白炭黑。
所述白炭黑的质量浓度为2-20%。
所述硅溶胶的用量为白炭黑质量的0-20%,优选5-15%。所述冷冻温度为-30~-5℃,冷冻时间为6-24h,
所述烘干温度为80~170℃,烘干时间为20-50h。
所述煅烧温度为800~1500℃,煅烧时间为8-72h,升温速率为1-10℃/min;
所述闪烧炉的温度为1600~2000℃,闪烧时间为2-30min。
本发明的设计思路:
通过反复冷冻解冻,使白炭黑收缩沉淀,通过白炭黑小颗粒自组装反向制作大颗粒多孔二氧化硅。反复冷冻解冻对浆料的影响:浆料随着温度的降低,水逐渐沿着温度梯度凝固,凝固产生的冰晶柱将胶体粒子挤压、排开、包埋至冰晶柱之间,解冻后,包埋于冰柱之间的离子形成团聚体,沉降,同时纳米粒子也会包裹在大粒子的表面,将孔道封闭。
本发明的有益效果是:
(1)本发明制得的二氧化硅内部多孔,内部孔壁一方面作为加强筋起到增强材料强度的作用,另一方面内部孔洞多为闭孔在加工过程中能够保持结构的整体完整性(保持低介电常数及减重的作用),同时表面孔洞闭合,因此具有轻质、多孔、高强度、比表面积低、吸油值低的特点,尤其是材料的强度远远高于空心玻璃微珠等空心材料。
(2)本发明的制备方法易实现工业化,解决了玻璃微珠加工过程中容易破碎,破碎后失去减重和降低介电常数的问题。
(3)本发明制备的多孔轻质二氧化硅填料具有球形形貌,有利于在树脂基体中的大比例填充,从而改善树脂基体的刚度、强度、耐热性、耐磨性、耐腐蚀性及机械加工性等。
附图说明:
图1为实施例1所得产品的SEM图。
图2为对比例1所得产品的SEM图。
具体实施方式:
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例和图示,进一步阐述本发明。
实施例1
将沉淀白炭黑制成质量浓度10%的浆料,搅拌下加入占白炭黑质量6%的硅溶胶,离子清洗至电导率为45μS/cm。离子清洗后放入冰柜,温度控制在-14℃,冷冻时间12h,完全冻住,提高温度至浆料完全融化,去除上层清液,再次放入冰柜,按以上调节冷冻,而后再解冻,去除上层清液,如此重复3次,浓缩抽滤。抽滤后将料饼在150℃下烘干24h,将烘干料置于马弗炉在1000℃煅烧10h,升温速率5℃/min。煅烧产物破碎、研磨、过气流磨、分级,处理成中位粒度为15um的粉体。将粉体用氧气气体载气通入闪烧炉,闪烧炉温度1700℃,在高温区域通过气流循环闪烧25min,浮选分级,成品。
实施例2
将沉淀白炭黑制成质量浓度10%的浆料,搅拌下加入占白炭黑质量分数10%的硅溶胶,离子清洗至电导率为40μS/cm。离子清洗后放入冰柜,温度控制在-14℃,冷冻时间15h,完全冻住,提高温度至浆料完全融化,去除上层清液,再次放入冰柜,按以上调节冷冻,而后再解冻,去除上层清液,如此重复3次,浓缩抽滤。抽滤后将料饼在150℃下烘干30h。将烘干料置于马弗炉在1000℃煅烧10h,升温速率5℃/min。煅烧产物破碎、研磨、过气流磨、分级,处理成中位粒度为15um的粉体。将粉体用氧气气体载气通入闪烧炉,闪烧炉温度1700℃,在高温区域通过气流循环闪烧25min,浮选分级,成品。
实施例3
将气相白炭黑制成质量浓度5%的浆料,搅拌下加入占白炭黑质量分数8%的硅溶胶,离子清洗至电导率为43μS/cm。离子清洗后放入冰柜,温度控制在-14℃,冷冻时间12h,完全冻住,提高温度至浆料完全融化,去除上层清液,再次放入冰柜,按以上调节冷冻,而后再解冻,去除上层清液,如此重复8次,浓缩抽滤。抽滤后将料饼在150℃下烘干多长时间20h。将烘干料置于马弗炉在900℃煅烧15h,升温速率2℃/min。煅烧产物破碎、研磨、过气流磨、分级,处理成中位粒度为20um的粉体。将粉体用氧气气体载气通入闪烧炉,闪烧炉温度1650℃,在高温区域通过气流循环闪烧25min,浮选分级,成品。
对比例1
将沉淀白炭黑制成质量浓度10%的浆料,离子清洗至电导率40μS/cm,而后抽滤,离子清洗后放入冰柜,温度控制在-14℃,冷冻时间12h,完全冻住,提高温度至浆料完全融化,去除上层清液,再次放入冰柜,按以上调节冷冻,而后再解冻,去除上层清液,如此重复3次,浓缩抽滤。抽滤后将料饼在150℃下进行烘干。将烘干料置于马弗炉在1000℃煅烧10h,升温速率5℃/min。煅烧产物破碎、研磨、过气流磨、分级,处理成中位粒度为15um的粉体。将粉体用氧气气体载气通入闪烧炉,闪烧炉温度1700℃,在高温区域通过气流循环闪烧25min,浮选分级,成品。
对比例2
将沉淀白炭黑制成质量浓度10%的浆料,离子清洗至电导率45μS/cm,悬浮液,无法抽滤,后续步骤无法继续。
由图1可以看出,所得产品为球型,表面比较光滑,基本实现表面闭合。
表1实施例和对比例的产品指标
“-”表示不适用。
由表1可知,本发明的方法适用于沉淀白炭黑和气相白炭黑,得到的产品的比表面积小,比重低,强度高。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种多孔轻质二氧化硅填料的制备方法,其特征在于:包括以下制备步骤:
(1) 制浆清洗:将白炭黑制浆,添加硅溶胶,离子清洗至电导率<50μS/cm,去除杂质离子;
(2) 冷冻浓缩:经离子清洗后将浆料放入冷冻设备中,冷冻至完全冻住,提高温度使浆料完全融化,去除上层清液后再次放入冷冻设备中,重复前述冷冻和解冻操作1-10次,浓缩抽滤;
(3) 烘干煅烧:滤饼烘干后煅烧;
(4) 破碎分级:煅烧产物破碎、研磨、过气流磨、分级,粒度在10-150um;
(5) 高温闪烧:将粉体用氧气气体载气通入闪烧炉,在高温区域通过气流循环闪烧,得到半成品;
(6) 浮选分级:分选出所需粒径,即得成品;
所述白炭黑的质量浓度为2-20%;
所述硅溶胶的用量为白炭黑质量的5-15%。
2.根据权利要求1所述的多孔轻质二氧化硅填料的制备方法,其特征在于:所述白炭黑选用沉淀白炭黑或气相白炭黑。
3.根据权利要求1所述的多孔轻质二氧化硅填料的制备方法,其特征在于:所述冷冻温度为-30~-5℃,冷冻时间为6-24h。
4.根据权利要求1所述的多孔轻质二氧化硅填料的制备方法,其特征在于:所述烘干温度为80~170℃,烘干时间为20-50h。
5.根据权利要求1所述的多孔轻质二氧化硅填料的制备方法,其特征在于:所述煅烧温度为800~1500℃,煅烧时间为8-72h,升温速率为1-10℃/min。
6.根据权利要求1所述的多孔轻质二氧化硅填料的制备方法,其特征在于:所述闪烧炉的温度为1600~2000℃,闪烧时间为2-30min。
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