CN113754413A - 一种具备高耐酸耐温耐压性能特种瓷砖的制备方法 - Google Patents

一种具备高耐酸耐温耐压性能特种瓷砖的制备方法 Download PDF

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CN113754413A
CN113754413A CN202111139790.8A CN202111139790A CN113754413A CN 113754413 A CN113754413 A CN 113754413A CN 202111139790 A CN202111139790 A CN 202111139790A CN 113754413 A CN113754413 A CN 113754413A
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赖志军
朱陵辉
罗德平
曾情
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Jiangxi Pingxiang Longfa Enterprise Co ltd
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Abstract

本发明公开了一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，将可塑性粘土5‑10wt%、煅烧氧化铝30‑40wt%、石英粉30‑40wt%、贵州土10‑20wt%、白云石3‑5wt%和瓷土5‑10wt%及适量的水加入球磨机内球磨混合制成半干态的基料，再加入基料重量1‑3%的碳化硅‑石墨烯复合粉和0.3‑0.5%的镁锆复合添加剂并喷水球磨混碾制成熟料，将熟料送入螺旋挤压机内，并加入粘接剂，挤压炼泥，挤压成型制得瓷砖坯体，将干坯高温烧制得到耐酸耐温和耐压瓷砖。本发明不仅具有高的耐酸腐蚀性，而且具有高的抗压强度和耐温度，可提高酸产量10%以上，增加使用寿命5年以上，降低生产成本30%以上，从而实现高产低耗。

Description

一种具备高耐酸耐温耐压性能特种瓷砖的制备方法
技术领域
本发明涉及瓷砖的制备方法，尤其是涉及一种既耐酸、耐高温，又耐压瓷砖的制备方法。
背景技术
在有色金属冶炼、化工行业等各种高温高压反应釜、塔、槽等工况条件非常苛刻设备的内衬砖工程中，对内衬瓷砖的技术要求越来越高，不仅要求瓷砖要有高的耐酸，抗腐蚀性，还要求能耐高压耐高温，具有高的抗急冷急热性，以确保瓷砖在使用期限内中不会出现开裂、变形、生烧、起泡、分层和磕碰等缺陷。
在当前使用的耐酸瓷砖中，耐酸碱度虽然可达到98%以上，但耐温度一般都在200℃以下，耐压强度一般也不会超过50MPa，特别是现有瓷砖抗急冷急热急变性能不高，满足不了高压反应釜、塔、槽等设备内衬的技术要求，而高压反应釜、塔、槽等设备内衬不仅要求耐酸碱性要在99%以上，且耐压强度要达到50 MPa以上、耐温度在300℃以上，抗急冷急热性达到450℃-20℃至少三次不裂。因此如何制造出既耐酸、耐高温，又耐高压的瓷砖是本行业面临的一项重大课题。
发明内容
针对上述现有技术中所存在的问题，本发明提出了一种具备高耐酸耐温耐压性能特种瓷砖的制备方法
本发明要解决的技术问题所采取的技术方案是：一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，它包括以下步骤：
a、先将粘土经1250-1320℃保温2-4小时焙烧制成氧化铝含量为20-26wt%、二氧化硅含量为64-72 wt%的可塑性粘土，
b、将可塑性粘土5-10wt%、煅烧氧化铝30-40wt%、石英粉30-40wt%、贵州土10-20wt%、白云石3-5wt%和瓷土5-10wt%及适量的水加入球磨机内球磨混合制成半干态的基料，
c、在球磨机内加入基料重量1-3%的碳化硅-石墨烯复合粉末并喷水球磨混碾，再在球磨机内加入基料重量0.3-0.5%的镁锆复合添加剂并喷水球磨混碾制成熟料，
d、将熟料送入螺旋挤压机内，并在螺旋挤压机内加入熟料重量3-5%的粘接剂，通过挤压炼泥得到泥料，
e、将泥料陈腐后，再在模具中挤压成型制得瓷砖坯体，将瓷砖坯体自然晾干或加热干燥成干坯，使干坯体中水分小于3%，
f、将干坯置入高温梭式炉中，先按200℃/h升温到400-500℃保温2-5小时后，再按300℃/h升温到1200-1300℃保温5-10小时，随炉冷却得到具备高耐酸耐温耐压性能特种瓷砖。
本发明的主要技术指标：
体积密度（g/cm3）：2.2-2.5， 吸水率（%）：≤2，耐温度℃：≥450，
抗压强度（MPa）：≥100， 气孔率（%）：≤10，耐酸度（%）：≥99.5，
热急冷急热性（450-20℃）：五次不裂、不剥落。
本发明所述贵州土产于遵义市高坪镇鸣庄村，贵州土不仅是一种氧化铝含量高、杂质氧化铁含量少的一种可塑性粘土，其氧化铝含量达35%以上，氧化铁含量小于1%，在高温条件下，且还能使氧化铝与二氧化硅的反应完全转换成为莫来石，消除晶界上铁脆相，从而有利于提高坯体的耐酸度和机械性能。
本发明所述瓷砖中三氧化铝含量可达30-45%，从而可使抗压强度和抗折强度大大提高，可增加塔内载重量，同时还能确保坯体耐酸碱和腐蚀性，耐酸度≥99.5%。
本发明所述碳化硅-石墨烯（C/SiC）复合粉末是一种碳化硅与石墨烯的复合材料，不仅能使瓷砖具有高的高温抗压强度、高热导性，低膨胀率和良好的热震性，而且能使分布在陶瓷基体内的/SiC纳米线表面长出一层或多层的石墨烯膜层，使SiC纳米线表面具有疏水性，从而可显著地提高瓷砖的电学性能，得到性能更优的瓷砖材料。
本发明所述的镁锆复合添加剂是一种能细化陶瓷基体内晶格的物质，能防止莫来石相的产生，降低烧结温度，有利于异相粒子弥散于陶瓷基体中，从而能阻碍晶粒长大，基体晶粒通过晶界移动而长大的途中与镁锆复合添加剂相遇时，将形成许多曲率半径很小的新表面，使基体的自由能升高，减缓晶粒长大的自由过程，实现晶粒细化和致密化，有利于SiC表面形成纳米质点，从而是提高瓷砖的耐温度和机械性能。
所述纳米镁锆复合添加剂是由重量比为1：0.8-1的氧化镁和氧化锆通过高温熔合形成的纲米或微米粉状复合物。
本发明通过长时间的选配，确定原料配方制出泥料，将泥料长时间陈腐后再进行真空挤压成型，并采取长时间自然晾干和烘干以及分段加热保温烧制的办法，解决了现有瓷砖不能同时耐酸、耐温和耐压，不适应高温高压反应釜、塔、槽等工况条件非常苛刻设备的内衬砖工程中对内衬瓷砖的技术要求，本发明不仅具有高的耐酸腐蚀性，而且具有高的抗压强度和耐温度，能适用高的气速要求，在强酸介质中工作具有稳定安全、低阻、低耗、气流分布均匀和高效的特点，可提高酸产量10%以上，增加使用寿命5年以上，降低生产成本30%以上，从而实现高产低耗。
所述粘接剂优选为具有高粘度的胶体、具有粘性、增稠和乳化分散的特点的羧甲基纤维素，也可选用如无机胶水、环氧树脂等粘接剂。
本发明所述耐酸耐温和耐压瓷砖的化学成份（重量百分比例）控制为：氧化铝30-45%、二氧化硅40-50%、氧化铁小于1%、氧化钙小于2%、氧化镁小于2%、氧化钾小于0.1%，氧化钠小于0.1%，本发明所述耐酸耐温和耐压瓷砖中严格控制氧化钾、氧化钠、氧化铁含量，硅铝比控制在1：1.0-1.5，以防止高温烧制时瓷砖出现过烧、起泡，确保瓷砖的耐酸度和抗压强度；本发明在满足硅铝比含量下，通过球磨控制球磨细度在250目筛余5%以下，并采用φ350毫米的真空练泥机可塑发挤压成型，使其比重达到2.2以上，而提高瓷砖的致密度和机械性能。
本发明所述基料在球磨时还可加入基料重量1-3%的陶瓷分散剂（如聚乙烯醇、聚丙烯酰胺），所述陶瓷分散剂可牢固地吸附在颗粒的裂缝上并能深入到裂缝深处，在颗粒粉碎过程中形成的新界面，能迅速被分散剂包裹，阻碍了新生界面的重新结合从而加速粉碎过程，明显地缩短粉碎时间，节约能耗，提高研磨效率。
具体实施方式
实施例一，一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，它包括以下步骤：
a、先将粘土经1250-1320℃保温2-4小时焙烧制成氧化铝含量为20-26wt%、二氧化硅含量为64-72 wt%的可塑性粘土，
b、将可塑性粘土5wt%、煅烧氧化铝30wt%、石英粉35wt%、经过高温烧制的贵州土15wt%、白云石5wt%和经过高温烧制的瓷土10wt%及适量的水加入球磨机内球磨混合制成半干态的基料，
c、在球磨机内加入上述基料重量2%的碳化硅-石墨烯复合粉末并喷水球磨混碾，再在球磨机内加入上述基料重量0.5%的镁锆复合添加剂并喷水球磨混碾制成熟料，
d、将熟料送入螺旋挤压机内，并在螺旋挤压机内加入熟料重量5%的羧甲基纤维素粘接剂，通过挤压炼泥得到泥料，
e、将泥料陈腐24小时后，再在模具中挤压成型制得瓷砖坯体，将瓷砖坯体自然晾干或加热干燥成干坯，使干坯体中水分小于3%，
f、将干坯置入高温梭式炉中，先按200℃/h升温到450℃保温3小时后，再按300℃/h升温到1200-1300℃保温7小时，随炉冷却得到具备高耐酸耐温耐压性能特种瓷砖。
所述瓷土的主要化学成份为SiO2 46.51%，Al2O3 39.54%，H2O 13.95%。
所述碳化硅-石墨烯复合粉末采用两步烧结法制成，具体是将碳化硅、氧化铝和单质镁（重量比85：8：7）的混合粉在120MPa压成块体，将块体在0.5-1MPa二氧化碳氛中升温到2100℃保温30-40min后，再降温至1800℃保温4-8小时冷却破碎后得到粒度在300目以上的碳化硅-石墨烯复合粉末。
本发明的主要技术指标：
体积密度（g/cm3）：2.38， 吸水率（%）：1.52，耐温度℃：461，
抗压强度（MPa）：103， 气孔率（%）：7.8，耐酸度（%）：99.9，
热急冷急热性（450-20℃）：五次不裂、不剥落。
实施例二，一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，它包括以下步骤：
a、先将粘土经1250-1320℃保温2-4小时焙烧制成氧化铝含量为20-26wt%、二氧化硅含量为64-72 wt%的可塑性粘土，
b、将可塑性粘土8wt%、煅烧氧化铝32wt%、石英粉38wt%、经过高温烧制的贵州土12wt%、白云石4wt%和经过高温烧制的瓷土6wt%及适量的水加入球磨机内球磨混合制成半干态的基料，
c、在球磨机内加入上述基料重量2.5%的碳化硅-石墨烯复合粉末并喷水球磨混碾，再在球磨机内加入上述基料重量0.35%的镁锆复合添加剂并喷水球磨混碾制成熟料，
d、将熟料送入螺旋挤压机内，并在螺旋挤压机内加入熟料重量4%的羧甲基纤维素粘接剂，通过挤压炼泥得到泥料，
e、将泥料陈腐24小时后，再在模具中挤压成型制得瓷砖坯体，将瓷砖坯体自然晾干或加热干燥成干坯，使干坯体中水分小于3%，
f、将干坯置入高温梭式炉中，先按200℃/h升温到450℃保温3小时后，再按300℃/h升温到1200-1300℃保温7小时，随炉冷却得到具备高耐酸耐温耐压性能特种瓷砖。
本发明的主要技术指标：
体积密度（g/cm3）：2.27， 吸水率（%）：1.72，耐温度℃：476，
抗压强度（MPa）：108， 气孔率（%）：5.9，耐酸度（%）：99.9，
热急冷急热性（450-20℃）：五次不裂、不剥落。
实施例三，一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，它包括以下步骤：
a、先将粘土经1250-1320℃保温2-4小时焙烧制成氧化铝含量为20-26wt%、二氧化硅含量为64-72 wt%的可塑性粘土，
b、将可塑性粘土10wt%、煅烧氧化铝35wt%、石英粉35wt%、贵州土10wt%、白云石3wt%和瓷土7wt%及适量的水加入球磨机内球磨混合制成半干态的基料，
c、在球磨机内加入上述基料重量3%的碳化硅-石墨烯复合粉末并喷水球磨混碾，再在球磨机内分别加入上述基料重量0.4%的镁锆复合添加剂和基料重量1-3%的聚乙烯醇分散剂并喷水球磨混碾制成熟料，
d、将熟料送入螺旋挤压机内，并在螺旋挤压机内加入熟料重量3%的无机胶水粘接剂，通过挤压炼泥得到泥料，
e、将泥料陈腐24小时后，再在模具中挤压成型制得瓷砖坯体，将瓷砖坯体自然晾干或加热干燥成干坯，使干坯体中水分小于3%，
f、将干坯置入高温梭式炉中，先按200℃/h升温到450℃保温4小时后，再按300℃/h升温到1200-1300℃保温8小时，随炉冷却得到具备高耐酸耐温耐压性能特种瓷砖。
本发明的主要技术指标：
体积密度（g/cm3）：2.41， 吸水率（%）：1.46，耐温度℃：485，
抗压强度（MPa）：112， 气孔率（%）：6.6，耐酸度（%）：99.9，
热急冷急热性（450-20℃）：五次不裂、不剥落。

Claims (4)

1.一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，其特征是：它包括以下步骤：
a、先将粘土经1250-1320℃保温2-4小时焙烧制成氧化铝含量为20-26wt%、二氧化硅含量为64-72 wt%的可塑性粘土，
b、将可塑性粘土5-10wt%、煅烧氧化铝30-40wt%、石英粉30-40wt%、贵州土10-20wt%、白云石3-5wt%和瓷土5-10wt%及适量的水加入球磨机内球磨混合制成半干态的基料，
c、在球磨机内加入基料重量1-3%的碳化硅-石墨烯复合粉末并喷水球磨混碾，再在球磨机内加入基料重量0.3-0.5%的镁锆复合添加剂并喷水球磨混碾制成熟料，
d、将熟料送入螺旋挤压机内，并在螺旋挤压机内加入熟料重量3-5%的粘接剂，通过挤压炼泥得到泥料，
e、将泥料陈腐后，再在模具中挤压成型制得瓷砖坯体，将瓷砖坯体自然晾干或加热干燥成干坯，使干坯体中水分小于3%，
f、将干坯置入高温梭式炉中，先按200℃/h升温到400-500℃保温2-5小时后，再按300℃/h升温到1200-1300℃保温5-10小时，随炉冷却得到高耐酸耐温耐压性能特种瓷砖。
2.根据权利要求1所述的一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，其特征在于：所述步骤c中加入基料重量1-3%的分散剂并喷水球磨混碾制成熟料。
3.根据权利要求1所述的一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，其特征在于：所述贵州土产于遵义市高坪镇鸣庄村，贵州土氧化铝含量达35%以上，氧化铁含量小于1%。
4.根据权利要求1所述的一种具备高耐酸耐温耐压性能特种瓷砖的制备方法，其特征在于：所述高耐酸耐温耐压性能特种瓷砖的化学成份比例为：氧化铝30-45%、二氧化硅40-50%、氧化铁小于1%、氧化钙小于2%、氧化镁小于2%、氧化钾小于0.1%，氧化钠小于0.1%。
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