CN105753460A - 一种低收缩高强度大规格陶瓷板及其制备方法 - Google Patents
一种低收缩高强度大规格陶瓷板及其制备方法 Download PDFInfo
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Abstract
本发明提供一种低收缩高强度大规格陶瓷板及其制备方法,所述制备方法包括以下步骤:(1)制备陶瓷原料粉体;(2)将针状硅灰石用硅烷偶联剂进行表面包裹处理并用气相白炭黑进行预分散,得到经预处理的针状硅灰石;(3)将陶瓷原料粉体与经预处理的针状硅灰石充分混合并造粒,其中所述经预处理的针状硅灰石的添加量为所述陶瓷原料粉体的10wt%~30wt%,干压成型,烧成,制得低收缩高强度大规格陶瓷板。本发明充分利用了针状硅灰石增强作用及烧成收缩小的特性,在大规格陶瓷板的制备中引入针状硅灰石,从而提高了大规格陶瓷板的强度,并降低了大规格陶瓷板的烧成收缩率,得到了低收缩高强度大规格陶瓷板。
Description
技术领域
本发明涉及一种陶瓷板制备工艺,特别涉及一种低收缩高强度大规格陶瓷板及其制备方法。
背景技术
由于陶瓷板极大地节约原材料、能源和运输成本,同时节约空间并降低建筑结构承重,特别符合国家的节能环保绿色产业政策。目前大规格陶瓷板工业化生产有干压成型和湿法挤压成型两种。挤压成型工艺要求坯料的含水率大,在干燥过程中坯体容易产生气孔和裂纹,这些都会降低烧成后产品的质量和成品率。相比之下,干压成型工艺更为成熟,产品的质量和收成率更高。
为了进一步提高陶瓷板强度及韧性,可以加入高长径比纤维。例如CN1191853A公开一种大型平板状陶瓷烧结体的制造方法,其在陶瓷原料中添加针状硅灰石和水后,用真空和泥机挤出成圆筒状后压延成型,最后得到具有较高强度的大型平板状陶瓷烧结体。由于采用湿法挤压工艺,针状硅灰石容易沿着挤压的方向形成定向排列,造成成品抗折强度各向异性,垂直挤压方向测成品强度高,平行挤压方向测成品强度低。
干压成型需要制粉,限于设备,采用湿法喷雾造粒工艺制粉对于具有一定长径比的纤维无法喷出,例如CN102173760A公开一种氧化硅陶瓷大薄板的制造方法,在制备原料坯土颗粒时,在原料中添加针状硅灰石,并采用喷雾干燥造粒。但是针状硅灰石对浆料流速影响很大,难喷粉,且长径比大不易过筛除铁,对坯体白度影响较大。因此,对于含有具有一定长径比的纤维的陶瓷,优选的是采用干法制粉工艺,但是采用干法制粉存在纤维难以均匀分散的问题。同时现有陶瓷板配方存在烧成收缩大(10%左右),容易导致尺码不规整等问题。
发明内容
鉴于以上所述,本发明所要解决的技术问题在于提供一种低收缩高强度大规格陶瓷板及其制备方法。使陶瓷板强度高、韧性好、烧成收缩小。
一方面,本发明提供一种低收缩高强度大规格陶瓷板的制备方法,包括以下步骤:
(1)制备陶瓷原料粉体;
(2)将针状硅灰石用硅烷偶联剂进行表面包裹处理并用气相白炭黑进行预分散,得到经预处理的针状硅灰石;
(3)将陶瓷原料粉体与经预处理的针状硅灰石充分混合并造粒,其中所述经预处理的针状硅灰石的添加量为所述陶瓷原料粉体的10wt%~30wt%,干压成型,烧成,制得低收缩高强度大规格陶瓷板。
本发明充分利用了针状硅灰石增强作用及烧成收缩小的特性,在大规格陶瓷板的制备中引入针状硅灰石,从而提高了大规格陶瓷板的强度,并降低了大规格陶瓷板的烧成收缩率,得到了低收缩高强度大规格陶瓷板。同时,采用干压成型工艺,可以提高产品的质量和收成率。而且,将针状硅灰石进行预处理,具体而言,用硅烷偶联剂进行表面改性并用气相白炭黑进行预分散,表面改性解决粉体容易团聚分散性差问题,白碳黑疏松状结构可以进一步提高粉体分散性,从而解决了针状硅灰石分散问题,进一步提高产品质量和收成率。
较佳地,步骤(1)中,陶瓷原料的配方为:水洗泥8~20%、混合泥4~16%、钾砂12~20%、中温砂24~30%、1#钠砂6~12%、2#钠砂16~22%、黑滑石1~2%。
较佳地,步骤(1)中,陶瓷原料粉体的制备方法包括:将各陶瓷原料干燥后预粉碎并过120目筛,筛下原料按配方混合后粉磨加工,控制250目筛余<2%。根据本发明,采用干法造粒工艺一起造粒,可以更好的与针状硅灰石混合均匀。
较佳地,所述针状硅灰石的长径比为10~18。通过采用长径比为10~18的针状硅灰石,既利于针状硅灰石的分散又可以增强陶瓷板的强度。
较佳地,步骤(2)包括:针状硅灰石在表面改性设备中通过喷洒硅烷偶联剂(添加量0.1~0.8%)形成一层改性剂包覆层以减少团聚,再与气相白炭黑(添加量0.1~0.5%)充分混合进行预分散处理。
较佳地,所述硅烷偶联剂为KH550、KH560、KH570中的至少一种。
较佳地,步骤(3)中,所述造粒采用干法造粒。采用干法造粒可以不限于设备,易于制得含针状硅灰石的粉体。
较佳地,步骤(3)中,所述干压成型的压力为86000~96000KN,成型规格为(1150~1300)mm×(2400~2600)mm×(3~6)mm。根据本发明,可以制得大规格的陶瓷坯体。
较佳地,烧成温度为1190~1220℃。
另一方面,本发明提供由上述任意一种方法制备的低收缩高强度大规格陶瓷板,所述陶瓷板的规格为(1100~1260)mm×(2200~2500)mm×(3~6)mm。所述陶瓷板包括瓷质产品和炻瓷砖产品,其中,瓷质产品收缩率为5~8%,抗折强度为55~68Mpa(优选58~68Mpa),吸水率小于0.5%;炻瓷砖产品收缩率为1~5%,抗折强度为40~55MPa,吸水率0.5~10%。
根据本发明,可以提供强度高、韧性好、烧成收缩小的大规格陶瓷板。既可以提高产品烧成规整性,又可以减少耗材,进一步起到节能降耗的作用。
附图说明
图1示出本发明一个实施方式的工艺流程图。
具体实施方式
以下结合附图和下述实施方式进一步说明本发明,应理解,附图及下述实施方式仅用于说明本发明,而非限制本发明。如无特别说明,本发明中述及的含量(添加量)百分比均为质量百分比。
本发明采用干压成型工艺制备低收缩高强度大规格陶瓷板。相较于湿法挤压成型,干压成型工艺更为成熟,产品的质量和收成率更高。本发明在陶瓷板的原料中加入针状硅灰石,以进一步提高陶瓷板强度及韧性,并且可以降低烧成收缩率,提高尺码规整度。另外,在加入针状硅灰石之前,对针状硅灰石进行预处理,以解决针状硅灰石分散问题。图1示出本发明一个实施方式的工艺流程图。以下参照图1说明本发明低收缩高强度大规格陶瓷板的制备方法。
陶瓷原料粉体的制备
陶瓷原料:本发明中,对陶瓷原料没有特别限定,可以采用常用的陶瓷原料。在一个示例中,所用原料及其化学成分如表1所示:
表1所用原料化学成分表(质量%)
SiO2 | Al2O3 | Fe2O3 | TiO2 | CaO | MgO | K2O | Na2O | 烧失 | |
水洗泥 | 61.81 | 25.32 | 0.61 | 0.32 | 0.52 | 0.22 | 0.66 | 0.51 | 9.97 |
混合泥 | 64.89 | 22.08 | 0.68 | 0.32 | 0.55 | 0.28 | 0.54 | 0.52 | 10.34 |
钾砂 | 60.01 | 25.91 | 0.49 | 0.21 | 0.44 | 0.04 | 6.22 | 0.81 | 6.52 |
中温砂 | 72.39 | 16.59 | 0.26 | 0.07 | 1.04 | 0.09 | 2.78 | 3.88 | 2.85 |
1#钠砂 | 71.73 | 17.07 | 0.26 | 0.05 | 0.61 | 0.08 | 0.93 | 8.29 | 0.94 |
2#钠砂 | 70.18 | 17.34 | 0.2 | 0.07 | 0.97 | 0.03 | 0.37 | 9.36 | 1.35 |
黑滑石 | 58.38 | 1.13 | 0.21 | / | 2.42 | 27.88 | 0.05 | / | 9.77 |
优选地,陶瓷原料配方如下:
水洗泥8~20%、混合泥4~16%、钾砂12~20%、中温砂24~30%、1#钠砂6~12%、2#钠砂16~22%、黑滑石1~2%。
将所用陶瓷原料进行干燥。优选地,干燥至水分<4%。干燥后,采用预粉碎设备对单个陶瓷原料进行预粉碎并过120目筛。筛上料继续粉磨;筛下原料按配方进行预混配料,然后一起进行粉磨加工(研磨制粉),控制250目筛余<2%。将粉料混合,得到陶瓷原料粉体。
针状硅灰石
本发明中,针状硅灰石的长径比优选为10~18。如果长径比大于18,会难以分散;如果长径比小于10,会影响增强效果。针状硅灰石的直径可为10微米~60微米。
针状硅灰石的预处理
本发明中,对针状硅灰石进行如下预处理:用硅烷偶联剂进行表面包裹处理并用气相白炭黑进行预分散。硅烷偶联剂可对针状硅灰石进行表面改性,以增强其与陶瓷原料的相容性。气相白炭黑可对针状硅灰石进行预分散。由此,可以明显改善针状硅灰石的分散性,从而使针状硅灰石可以均匀地分散在陶瓷原料中。作为硅烷偶联剂,包括但不限于KH550、KH560、KH570,优选为KH550。在一个示例中,预处理的具体方法为:针状硅灰石在表面改性设备中通过喷洒硅烷偶联剂(添加量0.1~0.8%)形成一层改性剂包覆层,再与气相白炭黑(添加量0.1~0.5%)充分混合进行预分散处理。这里的添加量百分比都是针对针状硅灰石而言。
将经预处理的针状硅灰石与上述陶瓷原料粉体充分混合,形成混合粉。混合方法例如可为球磨混合。针状硅灰石的添加量优选为10%~30%。如果其添加量大于30%,会烧成温度偏低,烧结范围小,不利于烧成;如果其添加量小于10%,收缩比较大,增大尺码小,达不到效果。更优选地,针状硅灰石的添加量为15%~20%。
然后,将混合粉造粒。由于采用湿法喷雾造粒工艺制粉对于具有一定长径比的纤维无法喷出,因此本发明优选为干法造粒。而且,由于针状硅灰石经预处理后具有良好的分散性,因此适于干法造粒。在一个示例中,造粒的具体方法为:干法悬浮态造粒工艺:陶瓷墙地砖的原料包括粘土类原料、石英类以及长石类原料。陶瓷原料经过配比使用新型盘式磨机干法粉磨至粒径D50=11.3μm的微粉。根据粉体表面物理化学原理,此时微粉颗粒本身受表面张力、分子间作用力作用会自发产生团聚现象,再加上原料中含有大约25%的粘土类原料使得微粉自身的团聚能力进一步增强,当微粉进入悬浮造粒设备的混合直筒内,在风力作用下均匀分散并与有一定黏性的雾化液滴充分接触、粘结,微粉以雾滴或者大颗粒微粉为颗粒核心,晶核附近的微粉物料会一层层地包在核心之上从而成为较大的固体颗粒,同时由于雾化液滴具有一定黏性它可以把更多的微粉颗粒粘结在一起,进一步团聚成形。初次成形的颗粒粒度较小、强度较低,随即进入特制旋风筒内,进入旋风筒内的物料沿着筒壁摩擦滚动受摩擦、物料彼此撞击作用力作用,从而使颗粒进一步团聚、球形度更加完美,粉体的强度也相应提高,有助于保持粉料球形状态。造粒形成的颗粒的粒径可为0.1~1mm。
然后将上述颗粒干压成型。在干压成型之前,还可以将颗粒进一步干燥、筛分、陈腐(例如24小时)等,以更适于干压成型。干压成型的压力可为86000KN~96000KN。成型规格可为(1150~1300)mm×(2400~2600)mm×(3~6)mm。
然后,将成型后的生坯进行烧成,制得陶瓷板。在一个示例中,烧成温度为1190~1220℃。烧成时间可为50~65分钟。烧成后还可以再施釉印花装饰进行釉烧。或者也可以在生坯上施釉印花装饰后一次烧成。另外,在烧成之前,还可先将生坯干燥。例如可在180~210℃干燥25~35分钟。
本发明中,烧成后的成品为大规格陶瓷板,其规格可为(1100~1260)mm×(2200~2500)mm×(3~6)mm。烧成后还可切割磨边以获得最终产品。本发明充分利用了针状硅灰石烧成收缩小的特性,瓷质产品的烧成收缩率为5~8%。同时,由于针状硅灰石的增强作用,本发明的陶瓷板的抗折强度高达58~68MPa。且吸水率小于0.5%。本发明的陶瓷板可为瓷质砖产品或炻瓷砖产品。瓷质砖产品收缩率为5~8%,抗折强度为55~68MPa,吸水率小于0.5%;炻瓷砖产品收缩率为1~5%,抗折强度为40~55MPa,吸水率0.5~10%。
下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。
下述实施例中的测试方法如下:
针状硅灰石长径比的测定:偏光显微镜;
烧成收缩率的测定:烧前在砖面中心部位画两条相互垂直的直线,利用游标卡尺过直线交叉点取10mm长的线段,烧后再测该线段的长度,就可计算出收缩率;
抗折强度的测定:SKZ数显式抗折仪;
吸水率的测定:TXY数显式陶瓷吸水率测定仪,采用真空法可对建筑卫生陶瓷的吸水率、显气孔率、体积密度进行测定(真空度:≥0.095MPa可调;抽真空时间:0~99分钟59秒连续可调;浸泡时间:0~99小时59分连续可调;容积:电源:~220V)。
实施例1
陶瓷原料配方:水洗泥15%、混合泥10%、钾砂16%、中温砂28%、1#钠砂10%、2#钠砂20%、黑滑石1%;各原料的化学成分如上述表1所示;
针状硅灰石:长径比为15,直径为30微米,购自江西奥特精细粉体有限公司,型号AT-针状粉。
具体步骤如下:
1)将所用陶瓷原料进行干燥(控制水分<4%);再采用预粉碎设备对单个陶瓷原料进行预粉碎并过120目筛;筛上料继续粉磨;筛下原料按配方进行预混配料,然后一起进行粉磨加工,控制250目筛余<2%,获得粉体。
2)将针状硅灰石用硅烷偶联剂进行表面包裹处理并用0.4%气相白炭黑进行预分散,具体步骤为:针状硅灰石在表面改性设备中通过喷洒硅烷偶联剂(添加量0.5%)形成一层改性剂包覆层以减少团聚,再与气相白炭黑(添加量0.4%)充分混合进行预分散处理。
3)将步骤1)所得的粉体与步骤2)所得的经预处理的针状硅灰石充分混合,经预处理的针状硅灰石的添加量为13%。然后造粒,造粒方法为干法悬浮态造粒工艺。
4)粒子陈腐24小时后送压机成型,压制压力为90000KN,成型后的坯体的规格为1275mm*2550mm*5.9mm。
5)将坯体于1210℃烧成55分钟,得到陶瓷板。成品规格为1180mm*2359mm*5.5mm,成品收缩率为7.5%,抗折强度为60Mpa,吸水率为0.27%。
实施例2
与实施例1相比,不同之处仅在于经预处理的针状硅灰石的添加量为22%。最终得到的陶瓷板成品规格为1204mm*2407mm*5.4mm,成品收缩率为5.6%,抗折强度为65MPa,吸水率为0.34%。
实施例3
与实施例1相比,不同之处仅在于经预处理的针状硅灰石的添加量为28%。最终得到的陶瓷板成品规格为1210mm*2420mm*5.6mm,成品收缩率为5.1%,抗折强度为66MPa,吸水率为0.45%。
实施例4
与实施例1相比,不同之处仅在于经预处理的针状硅灰石的添加量为11%。最终得到的陶瓷板成品(炻瓷砖产品)规格为1223mm*2445mm*5.5mm,成品收缩率为4.1%,抗折强度为42MPa,吸水率为9%。
实施例5
与实施例1相比,不同之处仅在于经预处理的针状硅灰石的添加量为27%。最终得到的陶瓷板成品(炻瓷砖产品)规格为1250mm*2499mm*5.5mm,成品收缩率为2%,抗折强度为47MPa,吸水率为6%。
对比例1
与实施例1相比,不添加针状硅灰石,仅用上述陶瓷原料制备陶瓷板。最终得到的陶瓷板成品规格为1141mm*2282mm*5.4mm,成品收缩率为10.5%,抗折强度为48MPa,吸水率为0.23%。
对比例2
与实施例1相比,添加针状硅灰石,但不对针状硅灰石进行预处理,其余步骤同实施例1。结果发现,针状硅灰石分散很不均匀,团聚体温度很高,造成局部烧结度不一致,成品容易在薄弱的地方断裂,理化性能差。最终得到的陶瓷板成品规格为1173mm*2346mm*5.5mm,成品收缩率为8%,抗折强度为48MPa,吸水率为0.6%。
Claims (11)
1.一种低收缩高强度大规格陶瓷板的制备方法,其特征在于,包括以下步骤:
(1)制备陶瓷原料粉体;
(2)将针状硅灰石用硅烷偶联剂进行表面包裹处理并用气相白炭黑进行预分散,得到经预处理的针状硅灰石;
(3)将陶瓷原料粉体与经预处理的针状硅灰石充分混合并造粒,其中所述经预处理的针状硅灰石的添加量为所述陶瓷原料粉体的10wt%~30wt%,干压成型,烧成,制得低收缩高强度大规格陶瓷板。
2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,陶瓷原料的配方为:水洗泥8~20%、混合泥4~16%、钾砂12~20%、中温砂24~30%、1#钠砂6~12%、2#钠砂16~22%、黑滑石1~2%。
3.根据权利要求1或2所述的制备方法,其特征在于,步骤(1)中,陶瓷原料粉体的制备方法包括:将各陶瓷原料干燥后预粉碎并过120目筛,筛下原料按配方混合后粉磨加工,控制250目筛余<2%。
4.根据权利要求1至3中任一项所述的制备方法,其特征在于,所述针状硅灰石的长径比为10~18。
5.根据权利要求1至4中任一项所述的制备方法,其特征在于,步骤(2)包括:针状硅灰石在表面改性设备中通过喷洒硅烷偶联剂形成一层改性剂包覆层,再与气相白炭黑充分混合进行预分散处理,其中硅烷偶联剂的添加量为针状硅灰石的0.1~0.8wt%,气相白炭黑的添加量为针状硅灰石的0.1~0.5wt%。
6.根据权利要求1至5中任一项所述的制备方法,其特征在于,所述硅烷偶联剂为KH550、KH560、KH570中的至少一种。
7.根据权利要求1至6中任一项所述的制备方法,其特征在于,步骤(3)中,所述造粒采用干法造粒。
8.根据权利要求1至7中任一项所述的制备方法,其特征在于,步骤(3)中,所述干压成型的压力为86000~96000KN,成型规格为(1150~1300)mm×(2400~2600)mm×(3~6)mm。
9.根据权利要求1至8中任一项所述的制备方法,其特征在于,步骤(3)中,烧成温度为1190~1220℃。
10.一种由权利要求1至8中任一项所述的制备方法制备的低收缩高强度大规格陶瓷板,其特征在于,所述陶瓷板的规格为(1100~1260)mm×(2200~2500)mm×(3~6)mm。
11.根据权利要求10所述的低收缩高强度大规格陶瓷板,其特征在于,所述陶瓷板包括瓷质产品和炻瓷砖产品,其中,瓷质产品收缩率为5~8%,抗折强度为55~68MPa,吸水率小于0.5%;炻瓷砖产品收缩率为1~5%,抗折强度为40~55MPa,吸水率0.5~10%。
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