CN110885237A - 一种低温烧结氧化铝陶瓷支撑体的制备方法 - Google Patents
一种低温烧结氧化铝陶瓷支撑体的制备方法 Download PDFInfo
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Abstract
本发明涉及多孔陶瓷材料技术领域,具体是一种低温烧结氧化铝陶瓷支撑体的制备方法。其主要特征在于创新性设计出一种能在1200~1300℃范围内烧成氧化铝陶瓷的烧结助剂,该烧结助剂的添加使得氧化铝多孔陶瓷材料的烧成温度明显降低,有效节约烧结能耗和时间,为用在环保领域的氧化铝陶瓷膜的制造提供一种低温烧结的支撑体。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。该方法生产的氧化铝陶瓷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,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陶瓷多孔材料技术领域,特别涉及无机陶瓷分离膜材料技术领域,具体为一种低温烧结氧化铝陶瓷支撑体的制备方法。
背景技术
分离膜材料是膜分离技术的核心,现有分离膜材料主要分为有机聚合物膜和无机陶瓷膜,相比于有机聚合物膜材料,无机陶瓷膜材料具有机械强度高、耐酸碱、耐高温、耐有机溶剂、耐生物腐蚀、耐氧化剂氧化、孔径分布窄、孔隙率高、孔集中度好、亲水性好、抗污染能力强、使用寿命长和应用范围广等优点。特别适用于海水淡化、废水处理与资源化、中水回用和饮用水净化等领域,是目前最具发展前景的分离材料。
然而,陶瓷膜除了具有上述诸多优点外,也存在着显著的缺点,那就是陶瓷膜制备工艺复杂,制造成本高。其造成陶瓷膜成本高的主要原因是工艺流程长、需要二次烧结或多次烧结、烧结温度高、升温和保温时间长、降温时间更长等,从而导致陶瓷膜生产周期长和膜产品产率低。专利(申请号:201610329412.9)曾公开的一种氧化铝陶瓷烧结方法,其烧结温度高达1700℃;专利(申请号:201710280509.X)曾公开一种用于污水处理的氧化铝陶瓷膜的制备方法,其烧结温度高达1400℃,并且还需要在无氧和惰性气氛保护环境下;专利(申请号:201711351472.1)也同样报道一种氧化铝陶瓷膜烧结温度需要达到1400℃。根据如上各种氧化铝陶瓷膜的制备方法的报道,烧结氧化铝陶瓷膜所需要的温度高达1400℃以上,高温需要的燃料或电能都很大,升温需要的时间长,能量消耗很大,从而导致陶瓷膜制造成本大幅提高,使得陶瓷膜优良的分离性能失去高的信价比。因此,降低氧化铝陶瓷膜的烧结温度是氧化铝陶瓷行业所关心和必需解决的问题。
发明内容
本发明的目的是针对当前氧化铝陶瓷膜烧结温度高,制造成本和投资成本高等问题。提供一种低温烧结氧化铝陶瓷支撑体的制备方法,其技术优势就是一种能在低温环境(1200~1250℃)和空气气氛下烧制具有高孔隙率和高机械强度的氧化铝多孔陶瓷膜材料;其技术核心就是适合氧化铝粉体在低温环境和空气气氛下结合在一起的烧结助剂。该烧结助剂配方的热膨胀系数低,并且热膨胀系数与氧化铝粉体匹配,在低温下形成液相熔融剂使氧化铝颗粒接触点黏连在一起,未接触的地方形成孔隙,从而制备多孔的氧化铝陶瓷膜。该方法制造工艺简单、制造成本和投资成本低、烧结温度低、成品率高、渗透通量大、适合工业定制、满足规模化生产的制造方法。
为解决氧化铝陶瓷支撑体在制备过程中存在的高温烧结的问题,本发明技术方案如下:
一种低温烧结氧化铝陶瓷支撑体的制备方法,所使用的原料包括α-Al2O3粉、烧结助剂、塑化剂、造孔剂、增塑剂、润滑剂和溶剂,其中:骨料采用α-Al2O3粉粒径范围是0.5~50μm;烧结助剂是由高岭土、氧化镁、碳酸钙、硅微粉、高硼硅玻璃粉和水玻璃构成,按照质量百分比为(30wt%~40wt%):(15wt%~25wt%):(5wt%~15wt%):(15wt%~25wt%):(5wt%~15wt%):(1wt%~10wt%)混合,各组分质量百分比之和为100%,该烧结助剂是低温烧结氧化铝陶瓷支撑体的技术核心,其作用是在1200~1250℃形成熔融液相,粘结氧化铝粉颗粒之间相互接触的部位,与氧化铝粉形成连续固熔体;塑化剂是由易溶于水的高分子聚合物如甲基纤维素、羧甲基纤维素钠、羟乙基纤维素、羟丙基甲基纤维素和聚乙烯醇中的一种或一种以上构成,其水溶液有一定的粘性,主要作用是将氧化铝粉和烧结助剂等这些瘠性料的颗粒黏连在一起,在常温下能通过挤出机的挤压力和模具相互作用形成具有一定的形状的泥坯;造孔剂是由淀粉、石墨、竹粉和纤维素中的一种或一种以上构成,其作用是在高温下被氧化生成二氧化碳气体,从而使得氧化铝粉颗粒之间具有一定的孔隙,提高氧化铝支撑体的孔隙率;增塑剂是由甘油、聚乙二醇、聚乙烯醇和聚丙烯酸中的一种或一种以上构成,其作用是防止挤出成型后的泥坯在陈腐过程中散失水分,而继续保持可塑的形状,不开裂和不翘曲;润滑剂是由油酸、桐油、硬脂酸铝和石墨中的一种或一种以上构成,其作用增强颗粒之间的流动性,减少颗粒在挤出过程中与模具之间的磨损;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,其作用是溶解塑化剂,使其具有一定的粘性,将瘠性的原料和烧结助剂在挤出机中挤压成型;
通过上述原料的组合,配合合理的烘干和烧成制度,可获得成型工艺简单,烧结温度低,机械强度高、孔隙率大的氧化铝陶瓷支撑体,制备方法步骤如下:
(1)混料和陈腐
将粒径范围是1~50μm的氧化铝粉、烧结助剂、塑化剂、造孔剂、增塑剂、润滑剂和溶剂,按照质量百分比为(95wt%~75wt%):(25wt%~5wt%):(1wt%~10wt%):(1wt%~10wt%):(0.5wt%~5wt%):(1wt%~10wt%):(10wt%~30wt%)混合;除溶剂外,各组分质量百分比之和为100%;在强力混料机运行过程中按照如下顺序和操作添加各种原料:氧化铝粉、塑化剂、已经按比例混合好的烧结助剂、造孔剂、溶解了增塑剂的溶剂和润滑剂,每添加一种原料,都需要混合1~10min,混料过程中温度不超过34℃,否则塑化剂会失去粘性,不能起到塑化作用;然后在捏合机中捏合10~60min,捏合过程中温度也同样也不超过34℃;在带冷却水的粗练泥机上练泥1~3遍后,真空度不小于-0.095MPa下练泥一遍;在温是度20~25℃和湿度是50~80%下陈腐12~72h;
(2)成型和干燥
根据设计要求挤出成型,加工单通道管式、多通道平板式和多通道管式的氧化铝支撑体;挤出机的真空度在-0.095MPa以上,挤出速度是0.1~5m/min,挤出压力是1~10MPa挤出成型;切割成所需长度后转运到连续微波中快速定型,每个箱体的功率在300~850W范围内调节,传送带速度是0.5~5m/min;然后再转运到鼓风干燥箱中,在50~120℃下烘干1~24h;
(3)脱胶和烧结
将烘干的素坯转运到高温电阻炉、燃气梭式或抽屉式窑炉和燃气隧道窑炉中的一种,空气气氛下脱胶和烧成;烧成制度控制如下:从室温~200℃,升温速率为20~50℃/h,脱出吸附水;从200~550℃,升温速率为10~30℃/h,保温1~5h,进行脱胶工序;从550~600℃,升温速率为5~10℃/h,规避相变开裂;从600℃~烧成温度,升温速率为10~30℃/h,升温形成熔融体;烧成温度范围是1100~1300℃下保温3~5h,熔融液相完全生成,整个窑炉达到热均衡;然后自然降温至室温,即可得到低温烧结氧化铝陶瓷支撑体。
作为优选,一种低温烧结氧化铝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是1~50μm的氧化铝粉、烧结助剂、塑化剂、造孔剂、增塑剂、润滑剂和溶剂,按照质量百分比为(95wt%~75wt%):(25wt%~5wt%):(1wt%~10wt%):(1wt%~10wt%):(0.5wt%~5wt%):(1wt%~10wt%):(10wt%~30wt%)混合,除溶剂外,各组分质量百分比之和为100%。
作为优选,一种低温烧结氧化铝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由高岭土、氧化镁、碳酸钙、硅微粉、高硼硅玻璃粉和水玻璃构成,按照质量百分比为(35wt%~38wt%):(20wt%~22wt%):(8wt%~10wt%):(20wt%~23wt%):(10wt%~12wt%):(5wt%~7wt%)混合,各组分质量百分比之和为100%。
作为优选,一种低温烧结氧化铝陶瓷支撑体的制备方法,所述的多通道平板式和多通道管式的通道形状是正方形、长方形、圆形、椭圆形和菱形中的一种或一种以上的组合。
作为优选,一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:所述的挤出参数是挤出机的真空度在-0.095MPa以上,挤出速度是0.1~5m/min,挤出压力是1~10MPa。
作为优选,一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:所述的快速定型和烘干参数是连续微波每个箱体的功率在300~850W范围内调节,传送带速度是0.5~5m/min;鼓风干燥箱是在50~120℃下烘干1~24h。
作为优选,一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:所述的烧成制度控制如下:从室温~200℃,升温速率为20~50℃/h;从200~550℃,升温速率为10~30℃/h,保温1~5h,;从550~600℃,升温速率为5~10℃/h;从600℃~1250℃,升温速率为10~30℃/h;在1100~1300℃下保温3~5h;然后自然降温至室温。
本发明一种低温烧结氧化铝陶瓷支撑体的制备方法的技术方案有如下的有益效果:
1.本发明所述的低温烧结氧化铝陶瓷支撑体是在空气气氛中,比较低的温度1250℃以下氧化焰烧结,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。
2.本发明所述的低温烧结氧化铝陶瓷支撑体是采用高温熔融液相烧结法,技术核心是烧结助剂的配方,该配方原料筛选和比例优化后的结果与氧化铝热膨胀系数匹配,不会在烧制过程中出现开裂、翘曲和表面缺陷的问题。
3.本发明所述的低温烧结氧化铝陶瓷支撑体的方法,烧成的产品具有机械强度高、孔隙率大、耐酸碱、耐高温、耐氧化剂、耐热震等性能。
附图说明
图1方孔道平板氧化铝陶瓷支撑体的断面示意图。
图2单通道管式氧化铝陶瓷支撑体的断面示意图。
图3多通道管式氧化铝陶瓷支撑体的断面示意图。
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85%α-Al2O3粉、15%烧结助剂(35%高岭土、20%氧化镁、10%碳酸钙、20%硅微粉、10%高硼硅玻璃粉和5%水玻璃)、5.5%羟丙基甲基纤维素(粘度10万)6%的石墨粉(5000目)、6%油酸和22%水(包含2‰聚丙烯酸溶解在水),在强力混料机中混合40min;然后在捏合机中捏合30min;在粗练泥机上练泥1~3遍后,真空度不小于-0.095MPa下练泥一遍;在温度20~25℃和湿度50~80%下陈腐24h;然后再次在真空度不小于-0.095MPa下练泥一遍;在在真空度不小于-0.095MPa的挤出机上挤出多孔道的管式氧化铝支撑体,支撑体外径30mm,19孔道,孔道直径4mm;连续式微波快速定型,微波功率600w,传送带速度1.5m/min,微波两个遍;在110℃的电阻热风烘干箱中烘12h;在天然气抽屉式窑炉中高温烧结,高温窑炉控制程序是从室温~200℃,升温速率为30℃/h;从200~550℃,升温速率为20℃/h,保温3h;从550~600℃,升温速率为8℃/h;从600℃~1250℃,升温速率为20℃/h;在1250℃下保温3h;自然降温至室温,即可得到多通道管式氧化铝支撑体。并进行各种性能测试。
实施例2
只是将烧成温度换成1100℃,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
只是将烧成温度换成1150℃,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
只是将烧成温度换成1200℃,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
只是将烧成温度换成1300℃,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:
实施例2和实施例3烧成的氧化铝支撑体几乎没有强度,氧化铝粉之间没有烧结在一起,说明该温度下的烧成不合适。
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 (5)
1.一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:原料包括α-Al2O3粉、烧结助剂、塑化剂、造孔剂、增塑剂、润滑剂和溶剂;其中α-Al2O3粉粒径范围是0.5~50μm;
烧结助剂是由高岭土、氧化镁、碳酸钙、硅微粉、高硼硅玻璃粉和水玻璃构成,按照质量百分比为(30wt%~40wt%):(15wt%~25wt%):(5wt%~15wt%):(15wt%~25wt%):(5wt%~15wt%):(1wt%~10wt%)混合,各组分质量百分比之和为100%;
塑化剂是由易溶于水的高分子聚合物如甲基纤维素、羧甲基纤维素钠、羟乙基纤维素、羟丙基甲基纤维素和聚乙烯醇中的一种或一种以上构成;
造孔剂是由淀粉、石墨、竹粉和纤维素中的一种或一种以上构成;
增塑剂是由甘油、聚乙二醇、聚乙烯醇和聚丙烯酸中的一种或一种以上构成;
润滑剂是由油酸、桐油、硬脂酸铝和石墨中的一种或一种以上构成;
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;
具体制备步骤如下:
(1)混料和陈腐
将粒径范围是1~50μm的氧化铝粉、烧结助剂、塑化剂、造孔剂、增塑剂、润滑剂和溶剂,按照质量百分比为(95wt%~75wt%):(25wt%~5wt%):(1wt%~10wt%):(1wt%~10wt%):(0.5wt%~5wt%):(1wt%~10wt%):(10wt%~30wt%)混合;除溶剂外,各组分质量百分比之和为100%;然后进行混合、捏合和陈腐处理;
(2)成型和干燥
根据设计要求,加工挤出成型的模具;挤出机的真空度是-0.095MPa以上,挤出速度是0.1~5m/min,挤出压力是1~10MPa,通过模具挤出成各种形状和用途的泥坯;切割成所需长度后转运到连续微波中快速定型,每个箱体的功率在300~850W范围内调节,传送带速度是0.5~5m/min;然后再转运到鼓风干燥箱中,在50~120℃下烘干1~24h;
(3)脱胶和烧结
将烘干的素坯转运到高温电阻炉、燃气梭式或抽屉式窑炉和燃气隧道窑炉中的一种,在空气气氛下脱胶和烧成,即可获得低温烧结的氧化铝陶瓷支撑体。
2.根据权利要求1所述的一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:烧结助剂原料成分及质量百分比由高岭土、氧化镁、碳酸钙、硅微粉、高硼硅玻璃粉和水玻璃构成,按照质量百分比为(35wt%~38wt%):(20wt%~22wt%):(8wt%~10wt%):(20wt%~23wt%):(10wt%~12wt%):(5wt%~7wt%)混合,各组分质量百分比之和为100%。
3.根据权利要求1所述的一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:挤出成型模具是单通道管式、多通道平板式和多通道管式中的一种。
4.根据权利要求1所述的一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:混料和陈腐过程中混合、捏合和陈腐,在强力混料机运行过程中按照如下顺序和操作添加各种原料:氧化铝粉、塑化剂、已经按比例混合好的烧结助剂、造孔剂、溶解了增塑剂的溶剂和润滑剂;每添加一种原料,都需要混合1~10min;混料过程中温度不超过34℃;然后在捏合机中捏合10~60min,捏合过程中温度也不超过34℃;在粗练泥机上练泥1~3遍后,真空度不小于-0.095MPa下练泥一遍;在温度是20~25℃和湿度是50~80%下陈腐12~72h。
5.根据权利要求1所述的一种低温烧结氧化铝陶瓷支撑体的制备方法,其特征在于:烧成制度如下:从室温~200℃,升温速率为20~50℃/h;从200~550℃,升温速率为10~30℃/h,保温1~5h;从550~600℃,升温速率为5~10℃/h;从600℃~烧成温度,升温速率为10~30℃/h;烧成温度范围是1100~1300℃下保温3~5h;然后自然降温至室温。
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Cited By (2)
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CN111377746A (zh) * | 2020-03-24 | 2020-07-07 | 洛阳中超新材料股份有限公司 | 低成本环保型蜂窝陶瓷成型用复合助剂及应用方法 |
CN113307599A (zh) * | 2021-06-01 | 2021-08-27 | 九江汇泰科技有限公司 | 一种新型多孔陶瓷组拼方法 |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006212551A (ja) * | 2005-02-04 | 2006-08-17 | Hitachi Zosen Corp | フィルター材及びその製造方法 |
JP2007268463A (ja) * | 2006-03-31 | 2007-10-18 | Hitachi Zosen Corp | フィルター材の製造方法 |
CN101412620A (zh) * | 2008-11-14 | 2009-04-22 | 西安交通大学 | 溶胶作为助剂制备多孔氧化铝陶瓷支撑体的方法 |
JP2009172604A (ja) * | 2009-03-26 | 2009-08-06 | Kyocera Corp | セラミックスフィルタおよびその製造方法 |
CN102408250A (zh) * | 2011-07-25 | 2012-04-11 | 三达膜科技(厦门)有限公司 | 一种陶瓷膜支撑体及其制备方法 |
US20140150389A1 (en) * | 2012-11-30 | 2014-06-05 | Adriane Marie Divens-Dutcher | Cordierite aluminum magnesium titanate compositions and ceramic articles comprising same |
KR101538380B1 (ko) * | 2015-05-14 | 2015-07-22 | 주식회사 신한세라믹 | 주사기용 세라믹필터 및 그 제조방법 |
CN106242624A (zh) * | 2016-08-02 | 2016-12-21 | 山东华瓷环保设备科技有限公司 | 一种氧化铝多通道陶瓷膜支撑体的制备方法 |
CN106268334A (zh) * | 2015-05-21 | 2017-01-04 | 佛山市中国科学院上海硅酸盐研究所陶瓷研发中心 | 一种陶瓷分离膜元件及其制备方法 |
CN107619281A (zh) * | 2017-08-03 | 2018-01-23 | 浙江理工大学 | 一种低温烧结耐酸碱多孔碳化硅陶瓷支撑体的制备方法 |
CN107698258A (zh) * | 2017-08-03 | 2018-02-16 | 浙江理工大学 | 一种陶瓷膜涂覆方法 |
CN108117379A (zh) * | 2017-12-01 | 2018-06-05 | 中海油天津化工研究设计院有限公司 | 一种高孔隙率多孔陶瓷膜支撑体及其制备方法 |
-
2019
- 2019-12-08 CN CN201911246104.XA patent/CN110885237B/zh active Active
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006212551A (ja) * | 2005-02-04 | 2006-08-17 | Hitachi Zosen Corp | フィルター材及びその製造方法 |
JP2007268463A (ja) * | 2006-03-31 | 2007-10-18 | Hitachi Zosen Corp | フィルター材の製造方法 |
CN101412620A (zh) * | 2008-11-14 | 2009-04-22 | 西安交通大学 | 溶胶作为助剂制备多孔氧化铝陶瓷支撑体的方法 |
JP2009172604A (ja) * | 2009-03-26 | 2009-08-06 | Kyocera Corp | セラミックスフィルタおよびその製造方法 |
CN102408250A (zh) * | 2011-07-25 | 2012-04-11 | 三达膜科技(厦门)有限公司 | 一种陶瓷膜支撑体及其制备方法 |
US20140150389A1 (en) * | 2012-11-30 | 2014-06-05 | Adriane Marie Divens-Dutcher | Cordierite aluminum magnesium titanate compositions and ceramic articles comprising same |
KR101538380B1 (ko) * | 2015-05-14 | 2015-07-22 | 주식회사 신한세라믹 | 주사기용 세라믹필터 및 그 제조방법 |
CN106268334A (zh) * | 2015-05-21 | 2017-01-04 | 佛山市中国科学院上海硅酸盐研究所陶瓷研发中心 | 一种陶瓷分离膜元件及其制备方法 |
CN106242624A (zh) * | 2016-08-02 | 2016-12-21 | 山东华瓷环保设备科技有限公司 | 一种氧化铝多通道陶瓷膜支撑体的制备方法 |
CN107619281A (zh) * | 2017-08-03 | 2018-01-23 | 浙江理工大学 | 一种低温烧结耐酸碱多孔碳化硅陶瓷支撑体的制备方法 |
CN107698258A (zh) * | 2017-08-03 | 2018-02-16 | 浙江理工大学 | 一种陶瓷膜涂覆方法 |
CN108117379A (zh) * | 2017-12-01 | 2018-06-05 | 中海油天津化工研究设计院有限公司 | 一种高孔隙率多孔陶瓷膜支撑体及其制备方法 |
Non-Patent Citations (1)
Title |
---|
张芳: "多孔氧化铝陶瓷支撑体及其微滤膜的制备与表征", 《中国优秀博硕士学位论文全文数据库 (硕士) 工程科技Ⅱ辑》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111377746A (zh) * | 2020-03-24 | 2020-07-07 | 洛阳中超新材料股份有限公司 | 低成本环保型蜂窝陶瓷成型用复合助剂及应用方法 |
CN111377746B (zh) * | 2020-03-24 | 2020-12-04 | 洛阳中超新材料股份有限公司 | 低成本环保型蜂窝陶瓷成型用复合助剂及应用方法 |
CN113307599A (zh) * | 2021-06-01 | 2021-08-27 | 九江汇泰科技有限公司 | 一种新型多孔陶瓷组拼方法 |
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