CN107056312A - 一种硅质可塑料及其制备方法 - Google Patents
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Abstract
本发明涉及一种硅质可塑料及其制备方法。其技术方案是:在水浴条件下,将脲醛树脂、聚丙烯酰胺、羧甲基纤维素、聚乙二醇200和水搅拌,得结合剂。将石英岩、硅微粉、碳化硅和白云石混磨至粒度≤80μm,在20~30MPa条件下压制成型,在空气气氛和1300~1450℃条件下热处理,将所述热处理后的物料破碎,筛分,分别得到粒度为3~4mm的A物料、粒度为1~2mm的B物料、粒度为0.088~0.5mm的C物料和粒度≤80μm的D物料;再将所述粒度不同的四种物料和氮化硅微粉混合,制得混合均质料。向所述混合均质料中加入所述结合剂,混合均匀,制得硅质可塑料。本发明具有成本低廉和工艺简单的特点;所制备的硅质可塑料的硬化时间长、体积密度大和强度高。
Description
技术领域
本发明属于可塑料技术领域。具体涉及一种硅质可塑料及其制备方法。
背景技术
可塑料是将粒状和粉状物料按一定比例配制,并引入结合剂而制备的一类不定形耐火材料,其主要特性为长时间内保持较高的可塑性。可塑料根据硬化方式可分为气硬性和热硬性两类,根据骨料材质不同可分为硅质、镁质、黏土质和高铝质等。
“一种坚甲可塑料及其制备方法”(CN201010158430.8)专利技术,公开了一种干熄焦炉用坚甲可塑料,主要以SiC、莫来石和含硅质微粉(小于2200目)为原料,以磷酸铝和磷酸为结合剂,经混炼、挤料、切坯后包装,该技术的主要缺点在于磷酸盐或磷酸的硬化速度快,不能长期保存,降低了可塑料的可塑性。
“一种长保存期磷酸结合高铝质可塑料及制备方法”(CN201310004596.8)专利技术,该技术主要通过引入缓蚀剂改善磷酸结合剂的硬化速度,延长可塑料的硬化时间,但其主要缺点在于可塑料的强度等性能较差。
发明内容
本发明旨在克服现有技术缺陷,目的在于提供一种成本低廉和工艺简单的硅质可塑料的制备方法;用该方法制备的硅质可塑料的硬化时间长、体积密度大和强度高。
为实现上述目的,本发明采用的技术方案的步骤是:
步骤一、按脲醛树脂∶聚丙烯酰胺∶羧甲基纤维素∶聚乙二醇200∶水的质量比为(0.3~0.35)∶(0.01~0.02)∶(0.01~0.03)∶(0.02~0.04)∶1,在35~40℃水浴条件下,将脲醛树脂、聚丙烯酰胺、羧甲基纤维素、聚乙二醇200和水置入容器中,搅拌5~8分钟,即得结合剂。
步骤二、按石英岩︰硅微粉︰碳化硅︰白云石的质量比为1︰(0.1~0.15)︰(0.02~0.05)︰(0.01~0.04)配料,在球磨机中混磨至粒度≤80μm,即得混合料。
步骤三、将所述混合料在20~30MPa条件下压制成型,再将成型的坯体置于马弗炉中,在空气气氛和1300~1450℃条件下热处理30~60分钟,随炉冷却,得到热处理后的物料。
步骤四、将所述热处理后的物料破碎,研磨,筛分,分别得到粒度为3~4mm的A物料、粒度为1~2mm的B物料、粒度为0.088~0.5mm的C物料和粒度≤80μm的D物料。
步骤五、将16~21wt%的所述A物料、20~25wt%的所述B物料、20~25wt%的所述C物料、32~37wt%的所述D物料和1~4wt%的氮化硅微粉加入搅拌机中,混合5~10分钟,制得混合均质料。
步骤六、按所述混合均质料︰所述结合剂的质量比为1︰(0.05~0.08),向所述混合均质料中加入所述结合剂,混合均匀,制得硅质可塑料。
所述脲醛树脂、聚丙烯酰胺、羧甲基纤维素和聚乙二醇200均为化学纯。
所述石英岩的主要化学成分是:SiO2含量为93~94wt%,CaO含量为0.5~1wt%,Fe2O3含量≤0.2wt%。
所述硅微粉的SiO2含量≥96wt%。
所述碳化硅的SiC含量≥99wt%。
所述白云石的主要化学成分是:CaCO3含量为50~52wt%,MgCO3含量为45~47wt%。
所述氮化硅微粉的Si3N4含量≥98wt%;氮化硅微粉的粒度为60~80μm。
由于采取上述技术方案,本发明与现有技术相比具有如下积极效果:
1、本发明所用原料来源丰富,成本低廉,在制备过程中无需特殊的处理技术与设备,工艺简单;
2、本发明通过“有机-无机”复合结合剂的包覆作用提升硅质可塑料的致密度,延长可硅质塑料的硬化时间,提高硅质可塑料的强度。
本发明制备的硅质可塑料经测定:硬化时间为9~12个月;120℃×6h热处理后体积密度为2.60~2.65g/cm3;120℃×6h热处理后冷态耐压强度为22~25MPa。
因此,本发明具有成本低廉和工艺简单的特点;所制备的硅质可塑料的硬化时间长、体积密度大和强度高。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述,并非对其保护范围的限制。
为避免重复,先将本具体实施方式所涉及的物料统一描述如下,实施例中不再赘述:
所述脲醛树脂、聚丙烯酰胺、羧甲基纤维素和聚乙二醇200均为化学纯。
所述石英岩的主要化学成分是:SiO2含量为93~94wt%,CaO含量为0.5~1wt%,Fe2O3含量≤0.2wt%。
所述硅微粉的SiO2含量≥96wt%。
所述碳化硅的SiC含量≥99wt%。
所述白云石的主要化学成分是:CaCO3含量为50~52wt%,MgCO3含量为45~47wt%。
所述氮化硅微粉的Si3N4含量≥98wt%;氮化硅微粉的粒度为60~80μm。
实施例1
一种硅质可塑料及其制备方法。本实施例所述制备方法的具体步骤是:
步骤一、按脲醛树脂∶聚丙烯酰胺∶羧甲基纤维素∶聚乙二醇200∶水的质量比为(0.3~0.32)∶(0.01~0.02)∶(0.01~0.02)∶(0.02~0.03)∶1,在35~40℃水浴条件下,将脲醛树脂、聚丙烯酰胺、羧甲基纤维素、聚乙二醇200和水置入容器中,搅拌5~8分钟,即得结合剂。
步骤二、按石英岩︰硅微粉︰碳化硅︰白云石的质量比为1︰(0.1~0.12)︰(0.02~0.04)︰(0.01~0.03)配料,在球磨机中混磨至粒度≤80μm,即得混合料。
步骤三、将所述混合料在20~30MPa条件下压制成型,再将成型的坯体置于马弗炉中,在空气气氛和1300~1400℃条件下热处理30~60分钟,随炉冷却,得到热处理后的物料。
步骤四、将所述热处理后的物料破碎,研磨,筛分,分别得到粒度为3~4mm的A物料、粒度为1~2mm的B物料、粒度为0.088~0.5mm的C物料和粒度≤80μm的D物料。
步骤五、将19~21wt%的所述A物料、23~25wt%的所述B物料、20~22wt%的所述C物料、32~34wt%的所述D物料和1~3wt%的氮化硅微粉加入搅拌机中,混合5~10分钟,制得混合均质料。
步骤六、按所述混合均质料︰所述结合剂的质量比为1︰(0.05~0.07),向所述混合均质料中加入所述结合剂,混合均匀,制得硅质可塑料。
本实施例制备的硅质可塑料经测定:硬化时间为9~11个月;120℃×6h热处理后体积密度为2.60~2.62g/cm3;120℃×6h热处理后冷态耐压强度为22~24MPa。
实施例2
一种硅质可塑料及其制备方法。本实施例所述制备方法的具体步骤是:
步骤一、按脲醛树脂∶聚丙烯酰胺∶羧甲基纤维素∶聚乙二醇200∶水的质量比为(0.31~0.33)∶(0.01~0.02)∶(0.01~0.02)∶(0.02~0.03)∶1,在35~40℃水浴条件下,将脲醛树脂、聚丙烯酰胺、羧甲基纤维素、聚乙二醇200和水置入容器中,搅拌5~8分钟,即得结合剂。
步骤二、按石英岩︰硅微粉︰碳化硅︰白云石的质量比为1︰(0.11~0.13)︰(0.02~0.04)︰(0.01~0.03)配料,在球磨机中混磨至粒度≤80μm,即得混合料。
步骤三、将所述混合料在20~30MPa条件下压制成型,再将成型的坯体置于马弗炉中,在空气气氛和1300~1400℃条件下热处理30~60分钟,随炉冷却,得到热处理后的物料。
步骤四、将所述热处理后的物料破碎,研磨,筛分,分别得到粒度为3~4mm的A物料、粒度为1~2mm的B物料、粒度为0.088~0.5mm的C物料和粒度≤80μm的D物料。
步骤五、将18~20wt%的所述A物料、22~24wt%的所述B物料、21~23wt%的所述C物料、33~35wt%的所述D物料和1~3wt%的氮化硅微粉加入搅拌机中,混合5~10分钟,制得混合均质料。
步骤六、按所述混合均质料︰所述结合剂的质量比为1︰(0.05~0.07),向所述混合均质料中加入所述结合剂,混合均匀,制得硅质可塑料。
本实施例制备的硅质可塑料经测定:硬化时间为9~11个月;120℃×6h热处理后体积密度为2.61~2.63g/cm3;120℃×6h热处理后冷态耐压强度为22~24MPa。
实施例3
一种硅质可塑料及其制备方法。本实施例所述制备方法的具体步骤是:
步骤一、按脲醛树脂∶聚丙烯酰胺∶羧甲基纤维素∶聚乙二醇200∶水的质量比为(0.32~0.34)∶(0.01~0.02)∶(0.02~0.03)∶(0.03~0.04)∶1,在35~40℃水浴条件下,将脲醛树脂、聚丙烯酰胺、羧甲基纤维素、聚乙二醇200和水置入容器中,搅拌5~8分钟,即得结合剂。
步骤二、按石英岩︰硅微粉︰碳化硅︰白云石的质量比为1︰(0.12~0.14)︰(0.03~0.05)︰(0.02~0.04)配料,在球磨机中混磨至粒度≤80μm,即得混合料。
步骤三、将所述混合料在20~30MPa条件下压制成型,再将成型的坯体置于马弗炉中,在空气气氛和1350~1450℃条件下热处理30~60分钟,随炉冷却,得到热处理后的物料。
步骤四、将所述热处理后的物料破碎,研磨,筛分,分别得到粒度为3~4mm的A物料、粒度为1~2mm的B物料、粒度为0.088~0.5mm的C物料和粒度≤80μm的D物料。
步骤五、将17~19wt%的所述A物料、21~23wt%的所述B物料、22~24wt%的所述C物料、34~36wt%的所述D物料和2~4wt%的氮化硅微粉加入搅拌机中,混合5~10分钟,制得混合均质料。
步骤六、按所述混合均质料︰所述结合剂的质量比为1︰(0.06~0.08),向所述混合均质料中加入所述结合剂,混合均匀,制得硅质可塑料。
本实施例制备的硅质可塑料经测定:硬化时间为10~12个月;120℃×6h热处理后体积密度为2.62~2.64g/cm3;120℃×6h热处理后冷态耐压强度为23~25MPa。
实施例4
一种硅质可塑料及其制备方法。本实施例所述制备方法的具体步骤是:
步骤一、按脲醛树脂∶聚丙烯酰胺∶羧甲基纤维素∶聚乙二醇200∶水的质量比为(0.33~0.35)∶(0.01~0.02)∶(0.02~0.03)∶(0.03~0.04)∶1,在35~40℃水浴条件下,将脲醛树脂、聚丙烯酰胺、羧甲基纤维素、聚乙二醇200和水置入容器中,搅拌5~8分钟,即得结合剂。
步骤二、按石英岩︰硅微粉︰碳化硅︰白云石的质量比为1︰(0.13~0.15)︰(0.03~0.05)︰(0.02~0.04)配料,在球磨机中混磨至粒度≤80μm,即得混合料。
步骤三、将所述混合料在20~30MPa条件下压制成型,再将成型的坯体置于马弗炉中,在空气气氛和1350~1450℃条件下热处理30~60分钟,随炉冷却,得到热处理后的物料。
步骤四、将所述热处理后的物料破碎,研磨,筛分,分别得到粒度为3~4mm的A物料、粒度为1~2mm的B物料、粒度为0.088~0.5mm的C物料和粒度≤80μm的D物料。
步骤五、将16~18wt%的所述A物料、20~22wt%的所述B物料、23~25wt%的所述C物料、35~37wt%的所述D物料和2~4wt%的氮化硅微粉加入搅拌机中,混合5~10分钟,制得混合均质料。
步骤六、按所述混合均质料︰所述结合剂的质量比为1︰(0.06~0.08),向所述混合均质料中加入所述结合剂,混合均匀,制得硅质可塑料。
本实施例制备的硅质可塑料经测定:硬化时间为10~12个月;120℃×6h热处理后体积密度为2.63~2.65g/cm3;120℃×6h热处理后冷态耐压强度为23~25MPa。
本具体实施方式与现有技术相比具有如下积极效果:
1、本具体实施方式所用原料来源丰富,成本低廉,在制备过程中无需特殊的处理技术与设备,工艺简单;
2、本具体实施方式通过“有机-无机”复合结合剂的包覆作用提升硅质可塑料的致密度,延长可硅质塑料的硬化时间,提高硅质可塑料的强度。
本具体实施方式制备的硅质可塑料经测定:硬化时间为9~12个月;120℃×6h热处理后体积密度为2.60~2.65g/cm3;120℃×6h热处理后冷态耐压强度为22~25MPa。
因此,本具体实施方式具有成本低廉和工艺简单的特点;所制备的硅质可塑料的硬化时间长、体积密度大和强度高。
Claims (8)
1.一种硅质可塑料的制备方法,其特征在于所述制备方法的步骤是:
步骤一、按脲醛树脂∶聚丙烯酰胺∶羧甲基纤维素∶聚乙二醇200∶水的质量比为(0.3~0.35)∶(0.01~0.02)∶(0.01~0.03)∶(0.02~0.04)∶1,在35~40℃水浴条件下,将脲醛树脂、聚丙烯酰胺、羧甲基纤维素、聚乙二醇200和水置入容器中,搅拌5~8分钟,即得结合剂;
步骤二、按石英岩︰硅微粉︰碳化硅︰白云石的质量比为1︰(0.1~0.15)︰(0.02~0.05)︰(0.01~0.04)配料,在球磨机中混磨至粒度≤80μm,即得混合料;
步骤三、将所述混合料在20~30MPa条件下压制成型,再将成型的坯体置于马弗炉中,在空气气氛和1300~1450℃条件下热处理30~60分钟,随炉冷却,得到热处理后的物料;
步骤四、将所述热处理后的物料破碎,研磨,筛分,分别得到粒度为3~4mm的A物料、粒度为1~2mm的B物料、粒度为0.088~0.5mm的C物料和粒度≤80μm的D物料;
步骤五、将16~21wt%的所述A物料、20~25wt%的所述B物料、20~25wt%的所述C物料、32~37wt%的所述D物料和1~4wt%的氮化硅微粉加入搅拌机中,混合5~10分钟,制得混合均质料;
步骤六、按所述混合均质料︰所述结合剂的质量比为1︰(0.05~0.08),向所述混合均质料中加入所述结合剂,混合均匀,制得硅质可塑料。
2.根据权利要求1所述的硅质可塑料的制备方法,其特征在于所述脲醛树脂、聚丙烯酰胺、羧甲基纤维素和聚乙二醇200均为化学纯。
3.根据权利要求1所述的硅质可塑料的制备方法,其特征在于所述石英岩的主要化学成分是:SiO2含量为93~94wt%,CaO含量为0.5~1wt%,Fe2O3含量≤0.2wt%。
4.根据权利要求1所述的硅质可塑料的制备方法,其特征在于所述硅微粉的SiO2含量≥96wt%。
5.根据权利要求1所述的硅质可塑料的制备方法,其特征在于所述碳化硅的SiC含量≥99wt%。
6.根据权利要求1所述的硅质可塑料的制备方法,其特征在于所述白云石的主要化学成分是:CaCO3含量为50~52wt%,MgCO3含量为45~47wt%。
7.根据权利要求1所述的硅质可塑料的制备方法,其特征在于所述氮化硅微粉的Si3N4含量≥98wt%;氮化硅微粉的粒度为60~80μm。
8.一种硅质可塑料,其特征在于所述硅质可塑料是根据权利要求1~7项中任一项所述的硅质可塑料的制备方法所制备的硅质可塑料。
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