CN111675543A - 一种陶瓷过滤器浆料用复合添加剂体系 - Google Patents

一种陶瓷过滤器浆料用复合添加剂体系 Download PDF

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CN111675543A
CN111675543A CN202010535678.5A CN202010535678A CN111675543A CN 111675543 A CN111675543 A CN 111675543A CN 202010535678 A CN202010535678 A CN 202010535678A CN 111675543 A CN111675543 A CN 111675543A
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slurry
ceramic filter
filter slurry
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张金钊
龚红宇
张玉军
林骁
冯玉润
王姗
孙姗
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Shandong University
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Abstract

本发明涉及一种陶瓷过滤器浆料用复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：分散剂0.18％‑0.22％；粘结剂0.25％‑0.35％。在制备过滤器的浆料中加入该体系可以制备高固含量、低粘度的浆料，增强了浆料的触变性和悬浮稳定性，提高了浆料对有机泡沫的附着能力，增加了浆料的实收率，从而提高了产品的力学性能，降低了生产成本。

Description

一种陶瓷过滤器浆料用复合添加剂体系
技术领域
本发明属于铸造冶金用陶瓷过滤器的制造领域，涉及一种陶瓷过滤器浆料用复合添加剂体系。
背景技术
材料，是现代化工业的基础，材料的属性决定了工业产品的上限。随着现代化工业进程的加快，诸如军工、通信、航空、汽车等重要领域对铸件的力学性能和综合质量的要求也越来越高。影响铸件性能的核心变量便是冶炼浇注过程中金属液的纯净度。泡沫陶瓷过滤器因为其独有的三维立体网络骨架结构在冶金和铸造的应用方面拥有许多传统过滤方式(如过滤网、直孔过滤器等)不具备的优良特性，可以有效的去除金属液中夹渣，甚至是大部分几微米小的悬浮夹杂物，因此，在高精尖制造业方面有较高的发挥余地。
泡沫陶瓷过滤器的制备工艺中，要求浆料具备高固含量、低粘度、良好的触变性和悬浮稳定性等性能，除了浆料配方体系影响之外，添加剂对浆料性能也有重要影响。添加剂对浆料的作用机理主要是影响颗粒间的作用力或电动电位的大小，因此，良好的陶瓷过滤器浆料用的复合添加剂可以使得浆料具备高固含量、低粘度、良好的触变性和悬浮稳定性等性能。
关于陶瓷过滤器方面有诸多专利文件报道，例如：CN107973616A公开了一种陶瓷过滤器及其制备方法，主要采用的添加剂为粘结剂。CN108484181A公开了一种能在低温下实现烧结的、化学稳定性和抗热震性优异的氧化铝短纤增强氧化镁基泡沫陶瓷过滤器及其制备方法，主要采用的添加剂为硅溶胶、流变剂等。然而，现有技术中主要是研究陶瓷过滤器浆料的配方，对于添加剂的对浆料的影响研究较少。
发明内容
针对现有技术的不足，本发明提供一种陶瓷过滤器浆料用复合添加剂体系，可以增加浆料的实收率，提高浆料的附着力，增加产品的力学性能。本发明的分散剂体系可以有效的提高浆料的流变性，提高浆料固含量和实收率并缩短研磨时间，降低生产成本；本发明的复合粘结剂体系可以有效的提高浆料稳定性和产品的挂浆量，增加过滤器的中高温强度，提高产品的力学性能。
术语说明：
CMC：羧甲基纤维素，结构式为(C6H9O4-O-CH2COONa)n。
PVA：聚乙烯醇。
本发明的技术方案如下:
一种陶瓷过滤器浆料用复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
分散剂0.18％-0.22％；
粘结剂0.25％-0.35％。
根据本发明，优选的，所述的分散剂为聚丙烯酰胺、聚丙烯酸钠、水玻璃等中的一种或两种以上混合。
根据本发明，优选的，所述的粘结剂为磷酸盐、硫酸盐、PVA、纤维素、黄原胶、铝溶胶、淀粉中的一种或两种以上混合。
根据本发明，优选的，所述的复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
分散剂0.2％；
粘结剂0.3％。
根据本发明，优选的，所述的复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
聚丙烯酸钠0.2％；
PVA 0.3％。
根据本发明，优选的，所述的分散剂通过球磨的方式加入到浆料中，所述的粘结剂通过搅拌的方式加入到浆料中。
根据本发明，优选的，所述的陶瓷过滤器浆料，包括如下质量百分比的组分组成：
325目碳化硅36.67wt％，1000目碳化硅18.33wt％，氧化铝28.8wt％，氧化硅9.9wt％，；苏州土5.04wt％，河北土1.26wt％。
根据本发明，优选的，所述的陶瓷过滤器浆料的固含量为81％。
根据本发明，优选的，所述的陶瓷过滤器浆料的pH＝9-12，进一步优选pH＝10。
根据本发明，优选的，按陶瓷过滤器浆料质量百分比计，所述的复合添加剂体系还包括CMC 0.5wt％。
根据本发明，优选的，按陶瓷过滤器浆料质量百分比计，所述的复合添加剂体系还包括硅溶胶1wt％。
根据本发明，由于添加剂作用的浆料会在研磨、搅拌、浸渍和挤压等过程中出现大量气泡，不仅影响浆料的均匀性，也会使浆料在干燥时出现脱落等现象，从而降低附着量及挂浆量，会使最终产品发生破裂、甚至塌落。因此本发明在制备浆料时按照浆料的总质量加入0.5-2％的消泡剂，优选的消泡剂为辛醇。
本发明与现有方法相比具有以下增益效果：
1、本发明复合添加剂体系使用的分散剂和pH值控制范围，可以有效地提高浆料的固含量和流变性能，并缩短研磨时间，降低了生产成本。
2、本发明复合添加剂体系使用的粘结剂有效的提高了产品的挂浆重量和中高温强度，降低了干燥和烧成过程中因粘结剂挥发、坯体强度差而造成的产品开裂和塌陷等问题。
附图说明
图1为试验例2中随着聚丙烯酸钠加入量的增加，浆料流动性的变化曲线。
图2是试验例3中随着PVA水溶液添加量的增加，浆料粘度的变化曲线。
图3为试验例4中CMC在碱性条件下不同的pH值对浆料粘度的影响曲线。
图4为试验例5中浆料粘度、产品孔隙率随着硅溶胶添加量的变化曲线。
图5为试验例5中浆料抗压强度和热震性随着硅溶胶添加量的变化曲线。
图6为试验例5中产品塌陷缺陷图。
具体实施方式
下面结合具体实施例和附图对本发明作进一步说明，但不限于此。
实施例中所用添加剂的添加量均为浆料质量的百分比。
实施例中浆料的配方组成为：325目碳化硅36.67wt％；1000目碳化硅18.33wt％；氧化铝28.8wt％；氧化硅9.9wt％；苏州土5.04wt％；河北土1.26wt％，固含量为81％，2kg球磨罐的料球比均为1:1.8，转速固定为120r/min，研磨24h。实施例中在制备浆料时按照浆料的总量加入0.5-2％的消泡剂(辛醇)。
PVA作为常用的陶瓷粘结剂加入到浆料中可以增加浆料粘度、增加挂浆量、提高干燥强度，防止干燥和烧成过程中的裂纹和塌陷等。PVA是常温时难溶于水的聚合物，因此实施例中首先利用水浴加热制备质量浓度为10％的PVA水溶液。
实施例1
一种陶瓷过滤器浆料用复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
聚丙烯酸钠0.2wt％，PVA水溶液0.3wt％，CMC 0.5wt％和硅溶胶1wt％。
(1)将聚丙烯酸钠0.2wt％加入到球磨中研磨21h；
(2)将PVA水溶液0.3wt％、CMC 0.5wt％和硅溶胶1wt％混合均匀，加入到研磨好的浆料中；
(3)用氨水将浆料的PH值调节为10，并进行充分搅拌；
(4)将30ppi的聚氨酯泡沫裁切成70x70x22mm的形状，将浆料涂挂在泡沫上，干燥后1400℃烧成。
实施例2
一种陶瓷过滤器浆料用复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
聚丙烯酰胺0.2wt％，磷酸二氢铝0.35wt％，CMC 0.5wt％和硅溶胶1wt％。
(1)将聚丙烯酰胺0.2wt％加入到球磨中研磨21h；
(2)将磷酸二氢铝0.35wt％、CMC 0.5wt％和硅溶胶1wt％混合均匀，加入到研磨好的浆料中；
(3)用氨水将浆料的PH值调节为10，并进行充分搅拌；
(4)将30ppi的聚氨酯泡沫裁切成70x70x22mm的形状，将浆料涂挂在泡沫上，干燥后1400℃烧成。
实施例3
一种陶瓷过滤器浆料用复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
聚丙烯酸钠0.18wt％，PVA水溶液0.3wt％，CMC 0.5wt％和硅溶胶1wt％。
(1)将聚丙烯酸钠0.18wt％加入到球磨中研磨21h；
(2)将PVA水溶液0.3wt％、CMC 0.5wt％和硅溶胶1wt％混合均匀，加入到研磨好的浆料中；
(3)用氨水将浆料的PH值调节为12，并进行充分搅拌；
(4)将30ppi的聚氨酯泡沫裁切成70x70x22mm的形状，将浆料涂挂在泡沫上，干燥后1400℃烧成。
试验例1
以无添加剂为对比，测试实施例1-3的相关性能测试，如表1所示。
表1
Figure BDA0002536899720000041
Figure BDA0002536899720000051
由表1可知，加入本发明的添加剂后出浆率、体积密度和抗压强度相比未加入添加剂的浆料，明显提高。
试验例2
研究聚丙烯酸钠(PAA-Na)的加入量对浆料流动性的影响，结果如图1所示。
PAA-Na对浆料流动性的影响机理是：PAA-Na在水中会发生水解反应，电离形成RCOO-+Na+，RCOO-会依附在颗粒表面，增加颗粒间的静电斥力，从而提升浆料的流动性。
从图1可知，随着PAA-Na加入量的提高，浆料的流动性先降低然后再升高，最佳流动性的添加量为0.2wt％。这是因为PAA-Na用量小时，RCOO-基团在粒子表面的位完全吸附，颗粒表面未被负离子基团有效覆盖或吸附层厚度太薄，颗粒间静电斥力小；随着PAA-Na用量增加，当吸附达到一定程度，系统电位最大，颗粒间静电斥力最大，系统粘度最低，流动性最好，此时浆料的得料率可达到89％；随着PAA-Na含量继续增多，分散剂在粒子间的搭桥效应可能会导致颗粒的絮凝，影响其粘度和流动性。
试验例3
研究PVA的加入量对浆料粘度、增加挂浆量的影响，结果如图2、表2所示。
图2是随着PVA水溶液添加量的增加，浆料粘度的变化曲线。由图2可以看出，当PVA水溶液加入浆料时，浆料粘度发生明显的上升，同时随着PVA水溶液加入量的增加，浆料粘度呈上逐渐升趋势，这是因为PVA水溶液有着较高的粘度，同时对体系料浆有较好的结合力，可以明显提升浆料的粘度。但是浆料粘度的增加与PVA水溶液的添加量不是成正比关系，随着PVA水溶液加入量的增加，浆料粘度的上升趋势逐渐减缓，当加入量达到0.5％时，浆料粘度反而出现大幅下降，这说明PVA存在一个最佳用量。这是因为随着PVA水溶液的增加，浆料中的水分相应增加，会导致浆料的固含量出现下降，因此会出现随着PVA水溶液加入量的增加，浆料粘度的上升趋势逐渐减缓的现象，当加入量超过0.5％时，PVA的粘结作用不足以抵消因固含量的降低而导致的粘度下降。
表2为PVA水溶液添加量的增加，浆料挂浆重量和增重率数据。
表2
Figure BDA0002536899720000061
表2中也可以看出，当PVA水溶液的加入量在0.3％时，产品挂浆增重率最高。因此，当PVA做粘结剂时，其水溶液加入量选择0.3％。
试验例4
研究CMC在碱性条件下不同的pH值对浆料粘度的影响，结果如图3所示。
CMC((C6H9O4-O-CH2COONa)n)溶于水后粘度低、流动性好，符合牛顿流体特性，在浆料中既能起到分散剂的作用，保持浆料的悬浮稳定性，也能起到粘结剂的作用，且粘结性能很强。同时，CMC在不同的酸碱环境下发生不同的电离反应：当在酸性浆料中时，CMC表现为增稠剂的作用，这是因为CMC的羧酸基基团会与水发生反应失去表面活性，会导致粘度急剧上升；而在碱性浆料中时，CMC表现为分散剂的效果，这是因为CMC通过提高颗粒表面的静电位能和空间位阻层两种作用来提升浆料的分散性和悬浮稳定性。因此研究PVA水溶液添加量为0.3wt％时，CMC在碱性条件下不同的pH值对浆料粘度的影响。
图3为不同pH值状态下，CMC的加入量对浆料粘度的影响，这里可以从两个维度进行讨论：单纯看pH值对浆料的影响，随着pH值的增大，浆料碱性增强，浆料的粘度出现下降，随着CMC的添加量增加，浆料粘度的影响增强，这继续证明了CMC在碱性溶液中的分散效果；单独分析相同pH值下CMC对浆料粘度的影响表现为，当pH＝10时浆料粘度随着CMC的添加量增加而缓慢上升，当添加量达到0.7％时，浆料粘度急剧增加，其粘结作用超过其分散作用，使得浆料无法正常使用；当pH＝11时，浆料粘度在CMC添加量为0.3％时出现最高粘度，之后随着添加量的提高，浆料粘度逐步下降，当添加至0.7％时粘度再次上升；当pH＝12时，CMC添加量为0.1％时出现最高粘度，随着添加量的继续增加，浆料粘度逐步下降，当添加至0.7％时粘度再次上升。两个维度的表现说明CMC在做粘结剂和分散剂时，在不同的pH值下存在一个最优添加量。当pH＝10、CMC加入量为0.5％时，浆料的粘度和分散性能最优，可以制得高粘度、高悬浮稳定性能的浆料。
综合上述分析，当pH＝10时颗粒之间的分散效果更好，可制备流动性和稳定性俱佳的浆料。同时在此pH值下，PVA水溶液添加量为0.3％，CMC添加量为0.5％时，出现满足使用要求的最佳粘度，可提升产品的挂浆性能。
试验例5
研究硅溶胶对浆料力学性能和高温性能的影响，结果如图4、5所示。
硅溶胶在泡沫陶瓷浆料中主要起浆料的常温分散作用和中高温的粘结剂作用。因为在烧成过程中，随着有机粘结剂在500℃下基本彻底挥发，此时失去粘结效果的坯体强度降低，容易造成开裂、塌陷等现象。硅溶胶中的氧化硅是结合力很强的网状结构，活性强，可以弥补有机粘结剂在高温烧结方面的不足。但是如果添加过量会引入过多玻璃相而降低过滤器的力学性能和高温性能，因此需要探索硅溶胶的最佳添加量。本发明在pH＝10的浆料中，加入0.3％的PVA水溶液和0.5％的CMC，通过实验硅溶胶不同加入量与产品的孔隙率、热震性和抗压强度的关系，来确定硅溶胶的添加量。产品的烧结温度为1400℃，保温2h。
图4为浆料粘度、产品孔隙率随着硅溶胶添加量的变化曲线。图5为抗压强度和热震性随着硅溶胶添加量的变化曲线。
从图4和图5中可以看出硅溶胶在浆料中的分散作用和粘结作用是存在最佳添加量的。因为硅溶胶的分散机理是由于其本身带负电荷的胶体，吸附在颗粒表面上时，会使颗粒间的双电层作用增强，颗粒间的排斥力增大，增强浆料的分散效果和稳定性。另一方面，硅溶胶也具有高温粘结作用，当硅溶胶的添加量为0.5wt％时，硅溶胶在常温浆料中的分散作用大于粘结作用，浆料粘度下降，挂浆量不足导致陶瓷烧结后有塌陷，强度很低，如图6所示。随着硅溶胶的添加量增加，当硅溶胶的添加量为1wt％时，可以发现浆料的粘度明显增加，虽然孔隙率下降至84％，但仍符合产品要求，同时抗压强度和热震性分别达到最优的1.75MPa，13次；随着硅溶胶添加量的继续增加，当硅溶胶的添加量为1.5％时，虽然浆料粘度和挂浆效果继续提升，但是产品的热震性和抗压强度出现明显下滑，这是因为硅溶胶的添加量出现过量，多余的SiO2会在烧结过程中出现方石英相，方石英在冷却时会发生3％的体积变化，产品产生微裂纹而大大降低过滤器的强度和高温性能。
综合上述，在pH＝10的浆料中添加0.3％的PVA水溶液、0.5％的CMC和1％的硅溶胶可以保障浆料粘度和稳定性的同时，提升产品的力学性能和高温性能。

Claims (10)

1.一种陶瓷过滤器浆料用复合添加剂体系，其特征在于，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
分散剂0.18％-0.22％；
粘结剂0.25％-0.35％。
2.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，所述的分散剂为聚丙烯酰胺、聚丙烯酸钠、水玻璃等中的一种或两种以上混合。
3.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，所述的粘结剂为磷酸盐、硫酸盐、PVA、纤维素、黄原胶、铝溶胶、淀粉中的一种或两种以上混合。
4.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，所述的复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
分散剂0.2％；
粘结剂0.3％。
5.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，所述的复合添加剂体系，按陶瓷过滤器浆料质量百分比计，包括如下组分组成：
聚丙烯酸钠0.2％；
PVA 0.3％。
6.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，所述的分散剂通过球磨的方式加入到浆料中，所述的粘结剂通过搅拌的方式加入到浆料中。
7.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，所述的陶瓷过滤器浆料，包括如下质量百分比的组分组成：
325目碳化硅36.67wt％，1000目碳化硅18.33wt％，氧化铝28.8wt％，氧化硅9.9wt％，；苏州土5.04wt％，河北土1.26wt％。
8.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，所述的陶瓷过滤器浆料的pH＝9-12，优选pH＝10。
9.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，按陶瓷过滤器浆料质量百分比计，所述的复合添加剂体系还包括CMC 0.5wt％。
10.根据权利要求1所述的陶瓷过滤器浆料用复合添加剂体系，其特征在于，按陶瓷过滤器浆料质量百分比计，所述的复合添加剂体系还包括硅溶胶1wt％。
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CN113582699A (zh) * 2021-07-22 2021-11-02 武汉工程大学 一种低粘度、高固含量的陶瓷浆料及其制备方法

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黄晶: "高固相碳化硅陶瓷浆料的性能研究及泡沫陶瓷的研制", 《中国学术期刊（光盘版）工程科技I辑》 *

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CN113582699A (zh) * 2021-07-22 2021-11-02 武汉工程大学 一种低粘度、高固含量的陶瓷浆料及其制备方法
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