CN105565785B - 陶瓷膜支撑体的制备方法 - Google Patents

陶瓷膜支撑体的制备方法 Download PDF

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CN105565785B
CN105565785B CN201510997212.6A CN201510997212A CN105565785B CN 105565785 B CN105565785 B CN 105565785B CN 201510997212 A CN201510997212 A CN 201510997212A CN 105565785 B CN105565785 B CN 105565785B
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product
preparation
film support
ceramic film
polyhedron
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CN105565785A (zh
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孟凡朋
樊震坤
张超
张健
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Shandong silicon membrane Mstar Technology Ltd
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SHANDONG SILICON NEW MATERIAL CO Ltd
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Priority to CN201510997212.6A priority Critical patent/CN105565785B/zh
Publication of CN105565785A publication Critical patent/CN105565785A/zh
Priority to US15/542,649 priority patent/US10427980B2/en
Priority to PCT/CN2016/091004 priority patent/WO2017107477A1/zh
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Abstract

本发明属于支撑体制备技术领域，具体涉及一种陶瓷膜支撑体的制备方法。以烧结法碳分分解工艺生产的氢氧化铝为原料进行预烧，得到低温氧化铝产物A；产物A中加入矿化剂进行煅烧，煅烧后研磨得到α氧化铝产物B；产物B与Al2O3·nH2O混合，同时加入矿化剂进行煅烧，煅烧后得到α氧化铝产物C；将煅烧保温后的α氧化铝产物C研磨打散分级得到多面体氧化铝粉；多面体氧化铝粉、粘结剂、水、保湿剂和分散剂混合烧结得到多孔氧化铝支撑体。本发明科学合理、方便实施，制得的支撑体易烧结、氧化铝纯度高、耐腐蚀性能好、孔隙率和通量提升。

Description

陶瓷膜支撑体的制备方法
技术领域
本发明属于支撑体制备技术领域，具体涉及一种陶瓷膜支撑体的制备方法。
背景技术
无机陶瓷膜因具有优良的耐高温、化学稳定性好、过滤精度高、抗化学侵蚀性及机械强度高等优点，被广泛应用于石油化工、食品、医药等行业。陶瓷支撑体是整个陶瓷膜制备和使用的基础，其性能的好坏对后期膜层的质量及整体应用性能起着至关重要的作用。
α-Al2O3以其优越的化学稳定性和良好的力学性能等特点，成为制备多孔陶瓷膜支撑体最常用的原料。对于市场上常用的99多孔氧化铝陶瓷支撑体而言，根据颗粒堆积理论要获得平均孔径在5～10μm的膜支撑体，为了保证支撑体具有高渗透性，氧化铝颗粒粒径应在20～30μm之间。目前国外商品化陶瓷膜支撑体的制备主要是采用平均粒径为30μ左右椭球形粉体，其中美国专利U.S.Pat.No.4,250,058公开了一种在热油中分散含氨前躯体的酸性铝溶胶方法制备具有良好机械强度的球形氧化铝颗粒，此外U.S.Pat.No.4,514,511也描述了一种类似的制备球形氧化铝粉体工艺。上述的方案虽能制备出机械强度高、近球形的氧化铝粉体，但是存在着成本和操作复杂等问题，另外后期制备支撑体时需要1750℃以上的烧结温度，目前国内烧结设备尚不能此高温烧结。国内因氧化铝粉体制备技术不足，多采用棒状或棒状的刚玉、氧化铝粉制作陶瓷膜支撑体。球形粉体专利如CN1278458A公开了一种采用喷雾造粒工艺制备球形氧化铝粉体的制备工艺，丁祥金等用此球形氧化铝粉D50＝22.4微米进行系列实验，在满足商业要求大于3M的抗爆强度下，产品空隙率仅为29％；专利CN101337808A公开了一种以氧化铝为原料加入矿化剂然后高温煅烧，再进行球磨、水洗、分级等工艺制备近球形氧化铝粉。上述专利虽然制备出球形氧化铝粉体，但在制备支撑体时存在着粉体过圆不利烧结和制备大孔隙率、球形氧化铝粉颗粒(＜20μm)、操作复杂、过程难控制、成本高等问题，直接导致陶瓷膜支撑体性能不稳定、使用寿命短、复杂的制作工艺和制作成本，限制了其在工业应用。
发明内容
本发明的目的是提供一种陶瓷膜支撑体的制备方法，科学合理、简单易行，制备的支撑体易烧结、孔隙率和通量较高、强度高、氧化铝纯度高、耐腐蚀性能好。
本发明所述的陶瓷膜支撑体的制备方法，步骤如下：
(1)以烧结法碳分分解工艺生产的氢氧化铝为原料进行预烧，得到低温氧化铝产物A；
(2)产物A中加入矿化剂进行煅烧，煅烧后研磨至粒度5-15微米，得到α氧化铝产物B；
(3)产物B与Al2O3·nH2O，n＝1-3混合，同时加入矿化剂进行煅烧，煅烧后得到α氧化铝产物C；
(4)将煅烧保温后的α氧化铝产物C研磨打散分级得到多面体氧化铝粉；
(5)取D50＝20-25微米和D50＝3-5微米的多面体氧化铝粉作为骨料，加入量分别为多面体氧化铝粉总质量的75-85％和15-25％；然后与粘结剂、水、保湿剂和分散剂混合搅拌均匀形成泥料；将泥料在密封下陈腐，然后在挤出机中挤出生坯，将生坯烘干水分，保温，烧结成多孔氧化铝支撑体。
步骤(1)中所述的预烧温度为300-500℃，预烧时间为1-10h。
步骤(2)中所述的矿化剂为氯化铝、硝酸铝、硼酸、硼酸钠、氟化铝、氟化铵、氟化钙、氟化镁、碳酸镁、氯化镁、氯化钠、氯化铵、氟化铈、氧化铈或氧化镧中的一种或多种，矿化剂的加入量为产物A的0.1-2wt％。
步骤(2)中所述的煅烧温度为1400-1700℃，煅烧时间为8-20h。
步骤(3)中所述的产物B与Al2O3·nH2O的质量比为1-10：1，Al2O3·nH2O为拟薄水铝石、勃姆石或氢氧化铝中的一种或多种。
步骤(3)中所述的矿化剂为氯化铝、硝酸铝、硼酸、硼酸钠、氟化铝、氟化铵、氟化钙、氟化镁、碳酸镁、氯化镁、氯化钠、氯化铵、氟化铈、氧化铈或氧化镧中的一种或多种，矿化剂的加入量为产物B与Al2O3·nH2O总质量的0.1-2wt％。
步骤(3)中所述的煅烧温度为1300-1400℃，煅烧时间为3-10h。
步骤(4)中所述的多面体氧化铝粉的一次粒径D50＝1-30微米。
步骤(5)中所述粘结剂为甲基纤维素或羟丙基甲基纤维素，粘结剂加入量为多面体氧化铝粉总质量的4-10％；水的质量为多面体氧化铝粉总质量的20-40％；保湿剂为甘油，保湿剂加入量为多面体氧化铝粉总质量的1.5-3.5％；分散剂为聚乙二醇类或PVA类分散剂，分散剂加入量为多面体氧化铝粉总质量的2-5％。
步骤(5)中所述的陈腐时间为24-36小时，保温温度为1650-1680℃，保温时间为3-6小时。
本发明可先制备出多面体氧化铝粉体，该粉体具有多面体型、大晶体、高比重、粒径可调控。在此骨料下按一定配比即可制得支撑体平均孔径为1-10微米可调控，孔隙率为33-40％。
本发明采用烧结法氢氧化铝为原料，通过三段烧结工艺生产出支撑体用氧化铝粉，该粉体具有大晶体(一次粒径D50＞20微米)、椭圆多面体结构、纯度高，可作为陶瓷膜支撑体的原料。本发明的多面体氧化铝外表圆润，使得颗粒相互之间接触面加大，仅采用多面体氧化铝本身即可烧结得到高强度的多孔氧化铝陶瓷膜支撑体，克服了球形氧化铝太圆难烧结、孔隙率不高、一次粒径D50<20微米等问题，使得支撑体易烧结、氧化铝纯度高、耐腐蚀性能好，孔隙率和通量提升。
本发明所述的陶瓷膜支撑体的制备方法，具体步骤如下：
(1)以烧结法碳分分解工艺生产的氢氧化铝为原料，经300-500℃进行预烧1-10h，得到低温氧化铝产物A；
(2)产物A中加入矿化剂，利用梭式窑或隧道窑在1400-1700℃温度下进行煅烧8-20h，煅烧后研磨至粒度5-15微米，得到α氧化铝产物B；
(3)产物B与Al2O3·nH2O(n＝1-3)混合，同时加入矿化剂，利用梭式窑或隧道窑在1300-1400℃温度下进行煅烧3-10h，煅烧后得到α氧化铝产物C；
(4)将煅烧保温后的α氧化铝产物C研磨打散分级得到多面体氧化铝粉；
(5)取D50＝20-25微米和D50＝3-5微米的多面体氧化铝粉作为骨料，加入量分别为氧化铝粉总质量的75-85％和15-25％；然后与粘结剂、水、保湿剂、分散剂混合搅拌均匀形成泥料；将泥料在密封下陈腐24-36小时，然后在挤出机中通过模具挤出成圆管状或者板状生坯；将生坯烘干水分，经过升温在1650-1680℃条件下保温3-6小时，烧结成多孔氧化铝支撑体。
本发明与现有技术相比，具有如下有益效果：
1、本发明可以制备出D50＝1-30μm的陶瓷支撑体用系列多面体氧化铝粉，尤其是可以制备出粉体一次粒径D50>20μm的粉体，有利于制备出5-10μm的大孔径、孔隙率为35-40％的氧化铝陶瓷支撑体。
2、本发明的多面体氧化铝不是规则圆形，使得颗粒相互之间接触面加大，仅采用多面体氧化铝本身即可烧结得到高强度的多孔氧化铝陶瓷膜支撑体。粉体D50＝20μm、D50＝3μm多面体氧化铝，在1650℃即可获得孔隙率为37％，外径30mm四通道支撑体三点抗折强度为4300N，避免了为保证制品烧结强度而采用提高温度或者外加烧结助剂、粉体包覆等繁杂工艺环节，简化了工艺流程和降低成本。
附图说明
图1是实施例1的多面体氧化铝粉体电镜照片。
图2是实施例1的多孔陶瓷支撑体的电镜照片。
具体实施方式
以下结合实施例对本发明做进一步描述。
实施例1
选取烧结法氢氧化铝为原料，350℃预烧2小时得到低温氧化铝A，A添加氟化铵矿化剂，添加量为0.5wt％，利用梭式窑煅烧，煅烧温度1550℃，保温15小时，煅烧后物料用球磨机研磨120分钟，得到粒度为10微米的煅烧氧化铝微粉B，B与勃姆石按5:1混合，同时添加硼酸矿化剂，添加量为0.3wt％，利用梭式窑煅烧，煅烧温度1350℃，保温5小时，经球磨机研磨120分钟后分级，得20微米和3微米多面体氧化铝。
取D50＝20微米、D50＝3微米多面体氧化铝，二者质量分别为多面体氧化铝总质量的85％、15％。加入多面体氧化铝总质量的2％的聚乙二醇600，作为分散剂，置于容器中球磨分散1小时，再加入多面体氧化铝质量5％的甲基纤维素，与氧化铝混合均匀，加入多面体氧化铝质量25％的水以及多面体氧化铝质量1％的甘油，搅拌成泥料后真空挤出成为单通道、四通道的氧化铝支撑体生坯，烘干生坯水分，将其烧结到1650℃，保温4小时，得到多面体氧化铝陶瓷膜支撑体。检测其孔隙率为39％，孔径为2微米。外径30mm四通道支撑体三点抗折强度为4500N，经40％浓硫酸100℃浸泡24小时，20％氢氧化钠溶液100℃浸泡24小时，强度损失率均低于1％，质量损失率低于0.01％。
实施例2
选取烧结法氢氧化铝为原料，500℃预烧1小时得到低温氧化铝A，A添加氟化铝与氯化铝复合矿化剂，添加总量为0.6wt％，利用梭式窑煅烧，煅烧温度1500℃，保温10小时，煅烧后物料用球磨机研磨90分钟，得到粒度为15微米的煅烧氧化铝微粉B，B与氢氧化铝按6:1混合，同时添加硼酸矿化剂，添加量为0.3wt％，利用梭式窑煅烧，煅烧温度1400℃，保温10小时，经球磨机研磨120分钟后分级，得25微米和5微米多面体氧化铝。
取D50＝25微米、D50＝5微米多面体氧化铝，二者质量分别为多面体氧化铝总质量的75％、25％。加入多面体氧化铝总质量的4％的聚乙二醇600，作为分散剂，置于容器中球磨分散1小时，再加入多面体氧化铝质量8％的甲基纤维素，与氧化铝混合均匀，加入多面体氧化铝质量30％的水以及多面体氧化铝质量1％的甘油，搅拌成泥料后真空挤出成为单通道、四通道的氧化铝支撑体生坯，烘干生坯水分，将其烧结到1680℃，保温6小时，得到多面体氧化铝陶瓷膜支撑体。检测其孔隙率为34％，孔径为8微米。外径30mm四通道支撑体三点抗折强度为4200N，经40％浓硫酸100℃浸泡24小时，20％氢氧化钠溶液100℃浸泡24小时，强度损失率均低于1.5％，质量损失率低于0.01％。
实施例3
选取烧结法氢氧化铝为原料，400℃预烧8小时得到低温氧化铝A，A添加氟化铝、氟化镁、硝酸铝复合矿化剂，添加总量为1wt％，利用梭式窑煅烧，煅烧温度1450℃，保温15小时，煅烧后物料用球磨机研磨120分钟，得到粒度为12微米的煅烧氧化铝微粉B，B与氢氧化铝按3:1混合，同时添加硼酸矿化剂，添加量为0.5wt％，利用梭式窑煅烧，煅烧温度1600℃，保温8小时，经球磨机研磨120分钟后分级，得22微米和5微米多面体氧化铝。
取D50＝22微米、D50＝5微米多面体氧化铝，二者质量分别为多面体氧化铝总质量的80％、20％。加入多面体氧化铝总质量的5％的聚乙二醇600，作为分散剂，置于容器中球磨分散1小时，再加入多面体氧化铝质量6％的羟丙基甲基纤维素，与氧化铝混合均匀，加入多面体氧化铝质量28％的水以及多面体氧化铝质量2％的甘油，搅拌成泥料后真空挤出成为单通道、四通道的氧化铝支撑体生坯，烘干生坯水分，将其烧结到1680℃，保温5小时，得到多面体氧化铝陶瓷膜支撑体。检测其孔隙率为37％，孔径为2微米。外径30mm四通道支撑体三点抗折强度为4400N，经40％浓硫酸100℃浸泡24小时，20％氢氧化钠溶液100℃浸泡24小时，强度损失率均低于1.2％，质量损失率低于0.01％。
以上所述，仅为本发明较佳实施例而已，故不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。

Claims (10)

1.一种陶瓷膜支撑体的制备方法，其特征在于步骤如下：
(1)以烧结法碳分分解工艺生产的氢氧化铝为原料进行预烧，得到低温氧化铝产物A；
(2)产物A中加入矿化剂进行煅烧，煅烧后研磨至粒度5-15微米，得到α氧化铝产物B；
(3)产物B与Al2O3·nH2O，n＝1-3混合，同时加入矿化剂进行煅烧，煅烧后得到α氧化铝产物C；
(4)将煅烧保温后的α氧化铝产物C研磨打散分级得到多面体氧化铝粉；
(5)取D50＝20-25微米和D50＝3-5微米的多面体氧化铝粉作为骨料，加入量分别为多面体氧化铝粉总质量的75-85％和15-25％；然后与粘结剂、水、保湿剂和分散剂混合搅拌均匀形成泥料；将泥料在密封下陈腐，然后在挤出机中挤出生坯，将生坯烘干水分，保温，烧结成多孔氧化铝支撑体。
2.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(1)中所述的预烧温度为300-500℃，预烧时间为1-10h。
3.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(2)中所述的矿化剂为氯化铝、硝酸铝、硼酸、硼酸钠、氟化铝、氟化铵、氟化钙、氟化镁、碳酸镁、氯化镁、氯化钠、氯化铵、氟化铈、氧化铈或氧化镧中的一种或多种，矿化剂的加入量为产物A的0.1-2wt％。
4.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(2)中所述的煅烧温度为1400-1700℃，煅烧时间为8-20h。
5.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(3)中所述的产物B与Al2O3·nH2O的质量比为1-10：1，Al2O3·nH2O为拟薄水铝石、勃姆石或氢氧化铝中的一种或多种。
6.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(3)中所述的矿化剂为氯化铝、硝酸铝、硼酸、硼酸钠、氟化铝、氟化铵、氟化钙、氟化镁、碳酸镁、氯化镁、氯化钠、氯化铵、氟化铈、氧化铈或氧化镧中的一种或多种，矿化剂的加入量为产物B与Al2O3·nH2O总质量的0.1-2wt％。
7.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(3)中所述的煅烧温度为1300-1400℃，煅烧时间为3-10h。
8.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(4)中所述的多面体氧化铝粉的一次粒径D50＝1-30微米。
9.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(5)中所述粘结剂为甲基纤维素或羟丙基甲基纤维素，粘结剂加入量为多面体氧化铝粉总质量的4-10％；水的质量为多面体氧化铝粉总质量的20-40％；保湿剂为甘油，保湿剂加入量为多面体氧化铝粉总质量的1.5-3.5％；分散剂为聚乙二醇类或PVA类分散剂，分散剂加入量为多面体氧化铝粉总质量的2-5％。
10.根据权利要求1所述的陶瓷膜支撑体的制备方法，其特征在于步骤(5)中所述的陈腐时间为24-36小时，保温温度为1650-1680℃，保温时间为3-6小时。
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