CN107056312B - 一种硅质可塑料及其制备方法 - Google Patents

一种硅质可塑料及其制备方法 Download PDF

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CN107056312B
CN107056312B CN201710414271.5A CN201710414271A CN107056312B CN 107056312 B CN107056312 B CN 107056312B CN 201710414271 A CN201710414271 A CN 201710414271A CN 107056312 B CN107056312 B CN 107056312B
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CN107056312A (zh
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张寒
赵惠忠
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Gucheng Huayi Silicon Industry Co.,Ltd.
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Wuhan University of Science and Engineering WUSE
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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

一种硅质可塑料及其制备方法
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 (7)

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；
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。
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％。
3.根据权利要求1所述的硅质可塑料的制备方法，其特征在于所述硅微粉的SiO2含量≥96wt％。
4.根据权利要求1所述的硅质可塑料的制备方法，其特征在于所述碳化硅的SiC含量≥99wt％。
5.根据权利要求1所述的硅质可塑料的制备方法，其特征在于所述白云石的主要化学成分是：CaCO3含量为50～52wt％，MgCO3含量为45～47wt％。
6.根据权利要求1所述的硅质可塑料的制备方法，其特征在于所述氮化硅微粉的Si3N4含量≥98wt％；氮化硅微粉的粒度为60～80μm。
7.一种硅质可塑料，其特征在于所述硅质可塑料是根据权利要求1～6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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