CN107285743B - 一种废弃氧化镁制备多孔陶瓷的方法 - Google Patents

一种废弃氧化镁制备多孔陶瓷的方法 Download PDF

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CN107285743B
CN107285743B CN201610191835.9A CN201610191835A CN107285743B CN 107285743 B CN107285743 B CN 107285743B CN 201610191835 A CN201610191835 A CN 201610191835A CN 107285743 B CN107285743 B CN 107285743B
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殷玫婕
黄雪松
胡义纯
倪建春
吴昊
张明
周浩梁
黄晓明
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Baoshan Iron and Steel Co Ltd
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Abstract

本发明公开了一种废弃氧化镁制备多孔陶瓷的方法,包括有机浸渍,有机浸渍制备过程包括如下步骤:(1)将废弃氧化镁70‑85份,Al2O3 10‑20份,MgF25‑10份溶于2‑6%的羧甲基纤维素溶液中,砂磨0.5‑2h,过筛,得到固含量为50‑60%的陶瓷粉体浆料;(2)将孔径分布为2‑25孔/厘米的聚氨酯泡沫浸泡在步骤(1)得到的浆料中,每隔20‑40min挂浆,重复,直到挂浆后,有机泡沫质量不再增加,干燥后升高到1300‑1550℃,烧结2‑4h,随炉冷却后得到氧化镁多孔陶瓷。本发明采用取向硅钢用氧化镁废弃物,其镁元素基本得到回用,制备工艺简单且成本低,回收效率达100%,经济环保。

Description

一种废弃氧化镁制备多孔陶瓷的方法
技术领域
本发明涉及多孔陶瓷制备领域,具体涉及一种用废弃氧化镁制备多孔陶瓷的方法。
背景技术
镁合金具有高的比强度、比刚度和比弹性模量,以及阻尼抗震性好等优点,因此在交通运输、航空航天、电子通讯等领域应用广泛。然而,无论采用电解法还是采用还原法生产的纯镁中都含有多种夹杂物,这些夹杂物对材料的力学、耐腐蚀等性能有极大危害,需要进一步净化处理才能达到使用要求,因而阻碍了镁金属材料应用范围的拓展。同目前已系列化的Al2O3、ZrO、SiC、Si3N4等泡沫陶瓷相比,采用MgO泡沫陶瓷净化镁液具有除杂效率高、成本低、操作简便等优点,是一种很好的物理净化镁液的方法。它是利用机械过滤的方法,借助陶瓷网络自发吸附镁液中液态熔剂夹杂物和固态颗粒夹杂物,而其本身在镁液中保持化学性质稳定,不污染镁液,特别适合于镁液净化。
国内研制的几种泡沫陶瓷都含有30%以上的SiO2,由于它与镁液之间有很高的反应活性,所以这种粘结性泡沫陶瓷不能用于镁液过滤;MgO泡沫陶瓷是利用在高温下保温,使较纯的MgO微细粉末烧结熔合在一起。中国专利CN200710128439.2,CN87102516,CN200710139287.6等以MgO为主体的泡沫陶瓷烧结温度普遍在1450℃-1800℃之间,常用温度1650℃,烧结温度较高,烧结困难,耗能大。
发明内容
因此,本发明要解决的技术问题是提供一种用废弃氧化镁制备多孔陶瓷的方法,该多孔陶瓷适用于粗镁过滤净化。
本发明的技术方案是,一种废弃氧化镁制备多孔陶瓷的方法,包括有机浸渍,所述有机浸渍制备过程包括如下步骤:
(1)将废弃氧化镁70-85份,Al2O3 10-20份,MgF25-10份溶于2-6%的羧甲基纤维素溶液中,砂磨0.5-2h,过筛,得到固含量为50-60%的陶瓷粉体浆料;
(2)将孔径分布为2-25孔/厘米的聚氨酯泡沫浸泡在步骤(1)得到的浆料中,每隔20-40min挂浆,重复,直到挂浆后,有机泡沫质量不再增加,干燥后,以0.5-3℃/min的升温速度升高到1300-1550℃,烧结2-4h,随炉冷却后即可得到氧化镁多孔陶瓷。
步骤(1)中,可以先把氧化镁和氧化铝溶于水,再将MgF2是溶于CMC,两种溶液混合;或者MgF2先溶于CMC溶液,再与氧化镁和氧化铝混合,加入少量水溶解氧化镁和氧化铝,也与MgF2的CMC溶液混合,最后再统一砂磨、过筛。以上提到的都是重量份。
挂浆的间隔时间、重复次数跟挂浆量,以及均匀性有关。
孔径大小跟后期所制备的陶瓷泡沫的强度有紧密联系,大了容易坍塌,强度下降,小了容易发生堵塞。因此上述聚氨酯泡沫的孔径分布为2-25孔/厘米。
氧化镁为泡沫陶瓷主要成分,Al2O3为增强氧化镁陶瓷强度、降低烧结温度的作用。MgF2+CMC,提高陶瓷前驱体浆料的分散性,降低烧结温度作用。
根据本发明的废弃氧化镁制备多孔陶瓷的方法,优选的是,步骤(1)所述砂磨转速为1000-1600r/min。
根据本发明的废弃氧化镁制备多孔陶瓷的方法,优选的是,步骤(1)所述过筛为过200-400目筛。
根据本发明的废弃氧化镁制备多孔陶瓷的方法,优选的是,步骤(2)所述温度为1300-1400℃。
根据本发明的废弃氧化镁制备多孔陶瓷的方法,优选的是,步骤(1)所述氧化镁选自取向硅钢生产过程中废弃的氧化镁。
进一步地,所述废弃的氧化镁中氧化镁含量占90%。氧化镁废弃物中除了含有Mg、O外,还含有Si、Al、Fe等杂质,其中氧化镁含量占90%以上。
根据本发明的用于粗镁过滤净化的废弃氧化镁制备多孔陶瓷的方法,优选的是,步骤(2)所述重复次数为三次以上。
本发明利用取向硅钢生产过程中废弃的氧化镁作为原料,在掺杂少量的Al2O3的情况下,利用加入CMC表面活性剂增加浆料的分散性,加入MgF2作为助溶剂,降低氧化镁陶瓷的烧结问题,在较低的升温速率下,实现氧化镁多孔陶瓷的制备,得到的氧化镁多孔陶瓷尤其适用于粗镁过滤净化。一方面,取向硅钢用氧化镁废弃物回收效率达到100%,减少了固体废弃物的零排放、实现绿色环保,又达到废弃物回收再利用的目的;另一方面,以氧化镁废弃物为原料,除了主成分氧化镁以外,含有的其他Si、Al、Fe等杂质也起到一定作用,制得具有良好性能的氧化镁多孔陶瓷,解决了现有氧化镁多孔陶瓷的强度、空隙、氧化铝含量高等问题。
本技术方案和已有技术相比,其技术进步是显著的。本发明提供的氧化镁多孔陶瓷不仅制备工艺简单,成本低,而且实现了硅钢用氧化镁废弃物的回收利用,大大提高了其经济效益和社会效益。该方法操作简单,适用于工业化生产。
附图说明
图1是实施例1氧化镁多孔陶瓷烧结前后的XRD图。
具体实施方式
实施例1
(1)将MgO废弃物:70份,Al2O3:20份,MgF2 10份,溶于4%的羧甲基纤维素溶液中,在1300r/min下进行砂磨1h,过325目筛,干燥得到固含量为约50%的陶瓷粉体浆料。
(2)将孔径分布为2-25孔/厘米的聚氨酯泡沫浸泡在(1)得到浆料中,每隔30min挂浆,重复三次,直到挂浆后,有机泡沫质量不再增加,干燥后,以1℃/min的升温速度升高到在1450℃下,烧结2h,随炉冷却后即可得到氧化镁多孔陶瓷。
该氧化镁多孔陶瓷材料的抗压强度为2.1MPa。
实施例2
(1)将MgO废弃物:85份,Al2O3:10份,MgF2 5份溶于4%的羧甲基纤维素溶液中,在1300r/min下进行砂磨1h,过325目筛,得到固含量为约60%的陶瓷粉体浆料。
(2)将孔径分布为2-25孔/厘米的聚氨酯泡沫浸泡在(1)得到浆料中,每隔30min挂浆,重复三次,直到挂浆后,有机泡沫质量不再增加,干燥后,以1℃/min的升温速度升高到在1550℃下,烧结4h,随炉冷却后即可得到氧化镁多孔陶瓷。
该氧化镁多孔陶瓷材料的抗压强度为2.7MPa。
实施例3
(1)将组合材料MgO废弃物:80份,Al2O3:15份,MgF2 5份溶于5%的羧甲基纤维素溶液中,在1300r/min下进行砂磨1h,过325目筛,得到固含量为约50-60%的陶瓷粉体浆料。
(2)将孔径分布为2-25孔/厘米的聚氨酯泡沫浸泡在(1)得到浆料中,每隔30min挂浆,重复三次,直到挂浆后,有机泡沫质量不再增加,干燥后,以1℃/min的升温速度升高到在1450℃下,烧结2-4h,随炉冷却后即可得到氧化镁多孔陶瓷。
该氧化镁多孔陶瓷材料的抗压强度为2.4MPa。
实施例4
(1)将组合材料MgO废弃物:75份,Al2O3:15份,MgF2 10份溶于4%的羧甲基纤维素溶液中,在1300r/min下进行砂磨1h,过325目筛,得到固含量为约55%的陶瓷粉体浆料。
(2)将孔径分布为2-25孔/厘米的聚氨酯泡沫浸泡在(1)得到浆料中,每隔30min挂浆,重复三次,直到挂浆后,有机泡沫质量不再增加,干燥后,以1℃/min的升温速度升高到在1300℃下,烧结4h,随炉冷却后即可得到氧化镁多孔陶瓷。
该氧化镁多孔陶瓷材料的抗压强度为2.0MPa。
实施例5
(1)将组合材料MgO废弃物:78份,Al2O3:16份,MgF2 6份溶于6%的羧甲基纤维素溶液中,在1500r/min下进行砂磨2h,过400目筛,得到固含量为约60%的陶瓷粉体浆料。
(2)将孔径分布为2-25孔/厘米的聚氨酯泡沫浸泡在(1)得到浆料中,每隔30min挂浆,重复三次,直到挂浆后,有机泡沫质量不再增加,干燥后,以2℃/min的升温速度升高到在1350℃下,烧结4h,随炉冷却后即可得到氧化镁多孔陶瓷。
该氧化镁多孔陶瓷材料的抗压强度为2.5MPa。
本技术方案可以将硅钢生产过程中产生的大量含氧化镁的废弃物回收再利用,制备适用于粗镁过滤净化的氧化镁多孔陶瓷。通过本发明所述的技术方案,取向硅钢用氧化镁废弃物中的镁元素基本得到回用,制备工艺简单且成本低,回收效率达100%,避免了其造成的环境污染,可广泛应用硅钢产线的氧化镁废弃物资源化利用,既可以减少废弃物排放处置费用又能够取得一定经济效益。

Claims (5)

1.一种废弃氧化镁制备多孔陶瓷的方法,包括有机浸渍,其特征在于,所述有机浸渍制备过程包括如下步骤:
(1) 将废弃氧化镁70-85份,Al2O3 10-20份,MgF25-10份溶于2-6%的羧甲基纤维素溶液中,砂磨0.5-2h,过筛,得到固含量为50-60%的陶瓷粉体浆料;所述废弃氧化镁选自取向硅钢生产过程中废弃的氧化镁;
(2)将孔径分布为2-25孔/厘米的聚氨酯泡沫浸泡在步骤(1)得到的浆料中,每隔20-40min挂浆,重复,重复次数为三次以上,直到挂浆后,有机泡沫质量不再增加,干燥后,以0.5-3℃/min的升温速度升高到1300-1550℃,烧结2-4h,随炉冷却后即可得到氧化镁多孔陶瓷。
2.根据权利要求1所述的废弃氧化镁制备多孔陶瓷的方法,其特征在于:步骤(1)所述砂磨转速为1000-1600r/min。
3.根据权利要求1所述的废弃氧化镁制备多孔陶瓷的方法,其特征在于:步骤(1)所述过筛为过200-400目筛。
4.根据权利要求1所述的废弃氧化镁制备多孔陶瓷的方法,其特征在于:步骤(2)所述烧结温度为1300-1400℃。
5.根据权利要求1所述的废弃氧化镁制备多孔陶瓷的方法,其特征在于:所述废弃的氧化镁中氧化镁含量占90%。
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