CN110511005B - 一种轴盘式旋转陶瓷支撑体的制备方法 - Google Patents
一种轴盘式旋转陶瓷支撑体的制备方法 Download PDFInfo
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- CN110511005B CN110511005B CN201910747629.5A CN201910747629A CN110511005B CN 110511005 B CN110511005 B CN 110511005B CN 201910747629 A CN201910747629 A CN 201910747629A CN 110511005 B CN110511005 B CN 110511005B
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Abstract
本发明涉及多孔陶瓷材料及膜分离技术领域，具体是一种轴盘式旋转陶瓷支撑体的制备方法。其主要特征在于选用微球陶瓷原料，通过液压机压制成型，低温液相法烧制成型的一种轴盘式旋转陶瓷支撑体。该制备方法具有烧结温度低、生产能耗低、工艺方法简单、设备要求低、生产成本和投资成本低、控制灵活、成型容易、适合工业定制、满足规模化生产的特点。该方法生产的轴盘式旋转陶瓷支撑体具有亲水性好，渗透通量超大，孔隙率高、成品率高，无需开设导流槽，耐酸碱性好、使用寿命长的特点。
Description
技术领域
本发明专利涉及无机多孔材料技术领域，特别涉及无机陶瓷膜分离材料技术领域，具体为一种轴盘式旋转陶瓷支撑体的制备方法。
背景技术
相较于传统聚合物分离膜材料，陶瓷膜具有化学稳定性好、能耐酸碱、耐有机溶剂、机械强度大、可反冲洗、抗微生物能力强、耐高温、孔径分布窄和分离效率高等优点，在食品工业、生物工程、环境工程、化学工业、石油化工和冶金工业等领域得到了广泛的应用。
然而，陶瓷膜也同样存在着膜污染的问题，导致膜渗透通量低，膜清洗频繁，运行费用高等一系列的弊端。为了减缓陶瓷膜污堵的趋势，多通道管式陶瓷膜通常采用错流过滤的模式，利用高速流体在膜表面产生的剪切力，来消除浓差极化或滤饼层带来的膜污堵问题。此种运行模式的确可以减缓膜渗透通量的降低，保证膜的分离效率能平稳运行。但是大的膜面流速需要大流量的水泵来驱动，能耗高，运行成本大。平板式陶瓷膜一般采用浸没式死端过滤模式，利用负压泵产生的抽吸力作为膜过滤的传质动力，并且需要配合鼓风机曝气产生的气泡来冲刷膜表面，以此减缓浓差极化或滤饼层带来的膜污染。此种过滤模式负压泵的能耗相对较低，但是分离膜的过滤效率没有被充分利用，曝气风机的能耗偏高，膜的装填密度大，投资成本高。
一种轴盘式旋转陶瓷膜过滤技术，采用膜片旋转时产生的剪切力来减缓膜表面的浓差极化或滤饼层等污染物，并采用负压抽吸的过滤模式来降低膜过滤的能耗和延长膜污堵的时间。该膜分离技术是兼顾上述两种运行模式的优点，而避开其不足之处，是一种将陶瓷膜过滤潜力彻底挖掘的全新过滤模式，并且具有浓缩倍数高，能耗低，投资成本和运行成本低等优势。专利CN106512751A和CN208694725U都曾公开报道这种多通道式或者多流道式的圆盘形状可旋转的陶瓷膜制备方法。这些专利都很明确地报道这种圆盘式陶瓷膜饼中间开设直线型或者曲线形的导水槽，降低膜的渗透阻力以及有利于膜渗透液的流通。但是这种在膜饼中间开设导流槽的设计大大增加了膜制造工艺的难度、工艺复杂性和制造成本，并且导致膜产品的合格率极低。因为该工艺需要两种模具，尤其是带有导流槽的模具在脱模时的难度很高，并且需要将两块不同厚度的素坯扣合成一个完整的圆饼，扣合处还需要高温结合剂粘合，很容易产生不规格品，或存在泄漏风险。此外制备这种圆盘式陶瓷膜一般都采用的是机械研磨的粉料，这种不规格粉体堆积形成的多孔陶瓷孔隙率低，支撑体的渗透阻力大，产水通量低。
发明内容
本发明的目的是针对陶瓷膜制造工艺复杂，制造成本和投资成本高，运行能耗和运行费用高等问题；以及圆盘式陶瓷膜制造难度大，成品率低以及渗透通量小等问题。提供一种制造工艺简单、制造成本和投资成本低、烧结温度低、成品率高、渗透通量大、控制灵活、成型容易、适合工业定制、满足规模化生产的制造方法。
本发明要解决的一个问题是：现有陶瓷膜生产原料是由陶瓷块状原料依靠破碎、研磨以及分选获得的不规则粉料，再通过高温烧结，形成具有三维孔隙的多孔陶瓷膜；该陶瓷膜孔隙率偏低，用在液体或气体过滤过程中，渗透阻力大，需要的驱动压力高，从而产生的运行成本偏高。提供一种采用二氧化硅微球作为陶瓷膜烧结原料和烧结温度在700～1400℃下制备多孔轴盘式旋转陶瓷支撑体的方法。
本发明要解决的另一个问题是：现有的圆盘式陶瓷膜膜饼中间设有直线型或曲线型导水槽，并且采用双模具工艺压制成型，高温粘合成整体圆饼状陶瓷膜片。制造工艺复杂，脱模难度大，成品率低以及投资成本高等缺点。提供一种模具结构简单，制造工艺简单，一次性压制成型，脱模容易，烧制过程不开裂和翘曲，可制备大尺寸薄壁的轴盘式旋转陶瓷支撑体的方法。
为解决轴盘式旋转陶瓷支撑体在制备过程中存在的技术问题，本发明技术方案如下：
一种轴盘式旋转陶瓷支撑体的制备方法，所使用的原料包括二氧化硅微球、烧结助剂、塑性剂、溶剂和脱模剂，其中：二氧化硅微球是粒径范围在1～200μm、集中度在80％以上；烧结助剂是由硅溶胶、铝溶胶、碳酸镁、磷酸二氢铝和高岭土构成，按照质量百分比为(35wt％～55wt％)：(10wt％～30wt％)：(10wt％～25wt％)：(5wt％～20wt％)：(5wt％～20wt％)混合，各组分质量百分比之和为100％，该烧结助剂是低温液相法烧结轴盘式旋转陶瓷支撑体的技术核心，其作用是在高温下形成液相，将二氧化硅微球粘结在一起；塑性剂是由甲基纤维素、羧甲基纤维素钠、羟丙基甲基纤维素和聚乙烯醇中一种或一种以上构成，其水解后具有一定的粘性，主要作用是常温下将二氧化硅微球和烧结助剂等瘠性料赋予一定的可塑性，能通过压机压制成型；溶剂是由水、乙醇或水和乙醇形成的混合物中的一种或一种以上构成，其作用是水解塑性剂，使其具有一定的粘性，将瘠性的原料和烧结助剂在压机作用下压制成圆饼形状。脱模剂由油酸、桐油、硬脂酸铝和石墨中的一种或一种以上构成，其作用是润滑，方便成型的圆饼与模具凹槽分离，保证完整无缺陷的圆饼素形状的坯成型；
通过上述原料的组合，配合合理的烘干和烧成制度，可获得制造工艺简单，孔隙率高，渗透通量超大的轴盘式旋转陶瓷支撑体，制备方法步骤如下：
(1)原料混合
将粒径范围在1～200μm的二氧化硅微球、烧结助剂、塑性剂、溶剂和脱模剂按照质量百分比为(95wt％～75wt％)：(25wt％～5wt％)：(1wt％～5wt％)(5wt％～20wt％)：(0.5wt％～8wt％)混合，除溶剂和脱模剂外，各组分质量百分比之和为100％；作为优选，将二氧化硅微球、烧结助剂和塑性剂在强力混料机中干混5～30min，在造粒机上缓慢添加溶剂和脱模剂直至黄豆大的颗粒成型为止，将造好颗粒的湿料用真空袋密封好，在20～25℃的温度和50～80％的湿度下陈腐12～24h。
(2)压制成型
根据设计要求加工直径100～500mm的圆饼形状模具，模具中心有直径10～100mm的圆孔，圆饼厚度3～50mm。安装模具及模具套在陶瓷粉末液压成型机的上下缸头处，在模具凹槽面上均匀撒上一层石墨粉，将步骤(1)中准备好的颗粒料加入模具凹槽内，然后通过液压机压制成中心有缺孔的圆饼形状的素坯，并采用吸盘将其转移到陶瓷托板上烘干。
(3)微波定型和烘干
将陶瓷托板连同压制成形后的素坯一起转移到连续式隧道微波陶瓷干燥器的链板上，微波功率300～850W，传送带速度0.5～5m/min，快速定型1～3遍，再转移至热风电阻干燥箱中，在100～300℃下干燥1～12h。
(4)高温烧结
将烘干的素坯转移到高温电阻窑炉、燃气梭式窑炉或隧道窑炉中，空气气氛下高温烧结。作为优选，烧成制度如下：从室温升温到150℃，升温速率为20～50℃/h，保温1～3h，进行脱水工序；从120℃升温到400℃，升温速率为10～50℃/h，保温2～4h，进行脱胶工序；从400℃升温到750℃，升温速率为30～50℃/h，单纯升温工序；从750℃升温到1400℃，升温速率为10～30℃/h，保温3～5h，进行氧化烧成工序；然后自然降温至室温，即可获得轴盘式旋转陶瓷支撑体。
作为优选，一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：所述的原料名称以及质量百分比由粒径范围在2～10μm的二氧化硅微球、烧结助剂、塑性剂、溶剂和脱模剂按照质量百分比为(90wt％～80wt％)：(10wt％～20wt％)：(2wt％～3wt％)(10wt％～15wt％)：(2wt％～5wt％)混合，除溶剂和脱模剂外，各组分质量百分比之和为100％。
作为优选，一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：所述的烧结助剂原料成分及质量百分比由硅溶胶、铝溶胶、碳酸镁、磷酸二氢铝和高岭土，按照质量百分比为(40wt％～50wt％)：(15wt％～25wt％)：(15wt％～20wt％)：(8wt％～12wt％)：(7wt％～15wt％)混合，各组分质量百分比之和为100％。
作为优选，一种轴盘式旋转陶瓷支撑体的制备方法，所述的成型模具是直径200～300mm的圆饼形状，中心有直径20～50mm的圆孔空缺，圆饼厚度5～20mm。
作为优选，一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：所述的微波快速定型以及烘干控制制度：微波功率300～850W，传送带速度0.5～5m/min，快速定型1～3遍，再转移至热风电阻干燥箱中，在100～300℃下干燥1～12h。
作为优选，一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：所述的高温烧结控制制度：从室温升温到150℃，升温速率为20～50℃/h，保温1～3h，进行脱水工序；从150℃升温到400℃，升温速率为10～50℃/h，保温2～4h，进行脱胶工序；从400℃升温到750℃，升温速率为30～50℃/h，单纯升温工序；从750℃升温到1400℃，升温速率为10～30℃/h，保温3～5h，进行氧化烧成工序；然后自然降温至室温。
作为优选，一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：所述的骨料二氧化硅微球、莫来石微球、氧化铝微球、整形后的瓷粉中的一种或一种以上的复合陶瓷。
本发明一种轴盘式旋转陶瓷支撑体的制备方法的技术方案有如下的有益效果：
1.本发明所述的轴盘式旋转陶瓷支撑体主要成分是二氧化硅微球和硅酸盐类烧结助剂，这些材料本身在水溶液中能形成丰富的硅醇键，能与水分子发生氢键作用，所以亲水性好，因此该材料制备的轴盘式旋转陶瓷支撑体具有很好的亲水性和抗污染性。
2.本发明所述的轴盘式旋转陶瓷支撑体的骨料采用的是比较规整的微球，这些微球颗粒堆积形成发达的三维孔隙结构，因此该支撑体不需要在圆饼中间做导流槽，也能实现高渗透通量的效果。
3.本发明所述的轴盘式旋转陶瓷支撑体是在空气气氛中，1400℃以下强氧化焰烧结，因此该方法具有烧结温度低、生产能耗低、工艺方法简单、设备要求低和生产成本和投资成本低的优点。
4.本发明所述的轴盘式旋转陶瓷支撑体是通过液压机一次压制成圆饼形状，圆饼中间无需留导水槽，也无需将半张圆饼通过高温结合剂粘结成整张圆饼，所以制造工艺简单，成品率高，且可压制大尺寸薄壁的产品。
5.本发明所述的轴盘式旋转陶瓷支撑体制备的旋片式陶瓷膜应用领域广，可用于化工、生物发酵、造纸、食品饮料、矿物加工等行业特种分离，也可以用于自来水净化、污水提标改造、废水处理及回收有用物质、中水回用等环节，还可应用在汽车尾气净化、煤化工粗煤气过滤、高温烟气处理等气体净化。
附图说明
图1轴盘式旋转陶瓷支撑体的断面示意图。
图2轴盘式旋转陶瓷支撑体的俯视图。
具体实施方式：
下面结合实例进一步说明本发明，但并不是本发明内容范围的任何限制。
实施例1
将中粒径5μm的二氧化硅微球、羟丙基甲基纤维素和烧结助剂(45wt％硅溶胶、20wt％铝溶胶、15wt％碳酸镁、10wt％磷酸二氢铝和10wt％高岭土)按质量百分比例为85：2：13共混，其中二氧化硅微球、羟丙基甲基纤维素、碳酸镁、磷酸二氢铝和高岭土先在强力混料机中混15min，然后再按比例添加液态的硅溶胶和铝溶胶；将混好的原料转移到造粒机上，然后缓慢添加占二氧化硅微球、羟丙基甲基纤维素和烧结助剂总重量分别为10wt％和4.5wt％的水和桐油，直至黄豆大的颗粒成型为止，将造好颗粒的湿料用真空袋密封好，20～25℃的温度和50～80％的湿度下陈腐24h；将陈腐好的湿料颗粒添加到已经撒了一层石墨粉的模具凹槽中，模具尺寸是内径50mm，外径200mm，厚度6mm的缺心环饼，在400吨液压机下压制成旋片陶瓷素坯，并采用吸盘将其转移到陶瓷托板上，然后陶瓷托板和压制好的素坯一起转移到连续式隧道微波陶瓷干燥器的链板上，微波功率600W，传送带速度1.5m/min，快速定型2遍，再转移至热风电阻干燥箱中，在110℃下干燥4h；将烘干的素坯转移到天燃气梭式窑炉中，空气气氛下高温烧结，烧成制度如下：从室温升温到150℃，升温速率为30℃/h，保温3h，进行脱水工序；从150℃升温到400℃，升温速率为20℃/h，保温3h，进行脱胶工序；从400℃升温到750℃，升温速率为50℃/h，单纯升温工序；从750℃升温到1320℃，升温速率为15℃/h，保温3h，进行氧化烧成工序；然后自然降温至室温，即可获得轴盘式旋转陶瓷支撑体，并进行各种性能测试。
实施例2
只是将二氧化硅微球的中粒径换成18μm，其他操作步骤、添加量和控制参数与实施例1相同。
实施例3
只是将二氧化硅微球的中粒径换成45μm，其他操作步骤、添加量和控制参数与实施例1相同。
实施例4
只是将二氧化硅微球的中粒径换成62μm，其他操作步骤、添加量和控制参数与实施例1相同。
实施例5
只是将二氧化硅微球换成中粒径5μm氧化铝微球，其他操作步骤、添加量和控制参数与实施例1相同。
实施例6
只是将二氧化硅微球换成中粒径53μm莫来石微球，其他操作步骤、添加量和控制参数与实施例1相同。
实施例7
只是将二氧化硅微球换成中粒径53μm整形后的瓷粉微球，其他操作步骤、添加量和控制参数与实施例1相同。
本发明制备的多孔碳化硅陶瓷支撑体性能评价方法如表1：
表2以上实施例中多孔碳化硅陶瓷支撑体性能测试：
以上所述，仅为本发明专利较佳实施例而已，不能依次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着的等效变化及修饰，皆应属于本发明涵盖的范围内。
Claims (4)
1.一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：所使用的原料包括二氧化硅微球、烧结助剂、塑性剂、溶剂和脱模剂，其中：二氧化硅微球是粒径范围1～200μm、集中度在80％以上；烧结助剂是由硅溶胶、铝溶胶、碳酸镁、磷酸二氢铝和高岭土构成，按照质量百分比为(35wt％～55wt％)：(10wt％～30wt％)：(10wt％～25wt％)：(5wt％～20wt％)：(5wt％～20wt％)混合，各组分质量百分比之和为100％；塑性剂是由甲基纤维素、羧甲基纤维素钠、羟丙基甲基纤维素和聚乙烯醇中一种以上构成；溶剂是由水、乙醇或水和乙醇形成的混合物构成；脱模剂由油酸、桐油、硬脂酸铝和石墨中的一种以上构成；具体制备步骤如下：
(1)原料混合
将粒径范围在1～200μm的二氧化硅微球、烧结助剂、塑性剂、溶剂和脱模剂按照质量百分比为85wt％：13wt％：2wt％：10wt％：4.5wt％混合，除溶剂和脱模剂外，各组分质量百分比之和为100％；然后造粒；
(2)压制成型
加工直径100～500mm的圆饼形状的模具，模具中心有直径10～100mm的圆孔，圆饼厚度3～50mm；安装模具及模具套在陶瓷粉末液压成型机的上下缸头处，在模具凹槽面上均匀撒上一层石墨粉，将步骤(1)中准备好的颗粒料加入模具凹槽内，然后通过液压机压制成中心有缺孔的圆饼形状的素坯，并采用吸盘将其转移到陶瓷托板上烘干；
(3)微波定型和烘干
将陶瓷托板连同压制成形后的素坯一起转移到连续式隧道微波陶瓷干燥器的链板上，微波功率300～850W，传送带速度0.5～5m/min，快速定型1～3遍，再转移至热风电阻干燥箱中，在100～300℃下干燥1～12h；
(4)高温烧结
将烘干的素坯转移到高温电阻窑炉、燃气梭式窑炉或隧道窑炉中，空气气氛下高温烧结，即可制得轴盘式旋转陶瓷支撑体；所述的高温烧结控制制度：从室温升温到150℃，升温速率为20～50℃/h，保温1～3h，进行脱水工序；从150℃升温到400℃，升温速率为10～50℃/h，保温2～4h，进行脱胶工序；从400℃升温到750℃，升温速率为30～50℃/h，单纯升温工序；从750℃升温到1400℃，升温速率为10～30℃/h，保温3～5h，进行氧化烧成工序；然后自然降温至室温。
2.根据权利要求1所述的一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：所述的烧结助剂原料成分及质量百分比由硅溶胶、铝溶胶、碳酸镁、磷酸二氢铝和高岭土，按照质量百分比为(40wt％～50wt％)：(15wt％～25wt％)：(15wt％～20wt％)：(8wt％～12wt％)：(7wt％～15wt％)混合，各组分质量百分比之和为100％。
3.根据权利要求1所述的一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于所述的成型模具是直径200～300mm的圆饼形状，中心有直径20～50mm的圆孔空缺，圆饼厚度5～20mm。
4.根据权利要求1所述的一种轴盘式旋转陶瓷支撑体的制备方法，其特征在于：原料混合过程中，二氧化硅微球、烧结助剂和塑性剂在强力混料机中干混5～30min，在造粒机中缓慢添加溶剂和脱模剂直至黄豆大的颗粒成型为止，将造好颗粒的湿料用真空袋密封好，在20～25℃的温度和50～80％的湿度下陈腐12～24h。
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