CN107266113A - 一种梯度孔道碳化硅陶瓷过滤板及其制备方法 - Google Patents
一种梯度孔道碳化硅陶瓷过滤板及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种梯度孔道碳化硅陶瓷过滤板及其制备方法,属于过滤介质领域。本发明取粗孔、中孔、细孔软质聚氨酯泡沫体剪裁成相同大小的圆片状,依次用氢氧化钠溶液和羧甲基纤维素钠溶液浸泡处理,得粗孔、中孔、细孔预处理软质聚氨酯泡沫体,将碳化硅、高岭土等混合球磨,并筛选出各级粒度复合粉料,分别与去离子水、磷酸二氢铝搅拌均匀得各级粒度陶瓷浆料,分别加入粗孔、中孔、细孔预处理软质聚氨酯泡沫体浸泡,辊压后从上往下按照粗孔、中孔、细孔堆叠整齐得组合泡沫体,干燥后经挂浆、干燥、烧制得梯度孔道碳化硅陶瓷过滤板。本发明的有益效果是:本发明梯度孔道碳化硅陶瓷过滤板强度高,陶粒不易剥落,开口气孔率高、气孔不易堵塞。
Description
技术领域
本发明涉及一种梯度孔道碳化硅陶瓷过滤板及其制备方法,属于过滤介质领域。
背景技术
陶瓷过滤板又称陶瓷滤膜、陶板、滤板等,是由刚玉、碳化硅等经特殊工艺制成的新型过滤介质。陶瓷过滤板也是采用三维网状结构和连通气孔的有机泡沫绵作载体,将其侵入具有触变性的特殊陶瓷浆料中,并采取特殊的辊挤工艺,使陶瓷浆料均匀敷与载体的骨架上,然后经烘干固化再高温焙烧而成。但由于陶瓷过滤板的盲孔多,导致气孔易堵塞,从而使陶瓷过滤板过滤能力大幅下降。中国专利申请号CN200710021711.7公开了一种覆有纳米陶瓷过滤膜的多孔陶瓷过滤板及其制造方法,属固液分离领域,陶瓷基板上覆有纳米陶瓷过滤膜,这种纳米陶瓷过滤膜是将异丙醇铝水解后用10%HNO3溶液进行胶溶,回流老化形成铝溶胶,在铝溶胶中加入纳米氧化铝粉进行混合、分散,形成均匀一致的纳米膜凝胶,再采用浸渍提拉法将纳米膜凝胶均匀涂覆于基板表面,经干燥、烧制而成,所得的多孔陶瓷过滤板有效阻挡了矿浆中的细小颗粒,盲孔少、不易被堵塞,提高了陶瓷过滤板过滤能力,延长了陶瓷过滤板的使用寿命,拓宽了陶瓷过滤机使用的领域。但该陶瓷过滤板强度低,陶粒易剥落,且由于抗热震性差,在使用过程中易出现过滤板断裂现象。综上可知,如何实现一种高性能的陶瓷过滤板是业内亟待解决的技术问题,不仅对陶瓷过滤板的发展具有必要的意义,也对拓宽陶瓷过滤板的使用领域具有必要的意义。
发明内容
本发明所要解决的技术问题:针对陶瓷过滤板强度低,陶粒易剥落,气孔易堵塞的弊端,提供了一种梯度孔道碳化硅陶瓷过滤板及其制备方法。
为解决上述技术问题,本发明采用如下所述的技术方案是:
一种梯度孔道碳化硅陶瓷过滤板,所述过滤板为粗孔、中孔、细孔陶瓷过滤片依次层叠后挂浆、干燥、烧制而成,所述粗孔陶瓷过滤片为粗孔预处理软质聚氨酯泡沫体浸泡25~100μm粒度陶瓷浆料后干燥制得,所述中孔陶瓷过滤片为中孔预处理软质聚氨酯泡沫体浸泡15~25μm粒度陶瓷浆料后干燥制得,所述细孔陶瓷过滤片为细孔预处理软质聚氨酯泡沫体浸泡0.5~15μm粒度陶瓷浆料后干燥制得,所述粗孔、中孔、细孔预处理软质聚氨酯泡沫体孔径依次为500~1000μm、200~500μm、50~200μm。
所述各级粒度陶瓷浆料为各级粒度复合粉料与去离子水、磷酸二氢铝搅拌均匀制得。
所述各级粒度陶瓷浆料由100~120重量份各级粒度复合粉料,50~55重量份去离子水,15~16重量份磷酸二氢铝组成。
所述各级粒度复合粉料为碳化硅、高岭土、钾长石、膨润土、氧化铝、白刚玉、滑石粉、硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的各级粒度复合粉料。
所述各级粒度复合粉料由450~600重量份碳化硅,100~120重量份高岭土,110~130重量份钾长石,50~60重量份膨润土,50~60重量份氧化铝,30~50重量份白刚玉,10~20重量份滑石粉,50~80重量份硅微粉组成。
所述预处理软质聚氨酯泡沫体为软质聚氨酯泡沫体依次用质量分数为10%氢氧化钠溶液和质量分数为2%羧甲基纤维素钠溶液浸泡处理得到。
所述挂浆过程为用0.5~15μm粒度陶瓷浆料对泡沫体淋浆,待泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥12~15min,重复上述淋浆操作2~3次。
所述烧制过程为将碳化硅陶瓷生坯置于干燥箱中,在110~120℃下干燥6~8h后转入窑炉中,以1℃/min速率升温至600℃,保持温度0.5~1h后,再以1℃/min速率继续升温至1400℃,保温烧制2~3h后自然冷却至室温。
所述的一种梯度孔道碳化硅陶瓷过滤板的制备方法,具体步骤为:
S1.取粗孔、中孔、细孔软质聚氨酯泡沫体剪裁成相同大小的圆片状,依次用质量分数为10%氢氧化钠溶液和质量分数为2%羧甲基纤维素钠溶液浸泡处理,得预处理软质聚氨酯泡沫体;
S2.将碳化硅、高岭土、钾长石、膨润土、氧化铝、白刚玉、滑石粉、硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的复合粉料;
S3.分别将各级粒度的复合粉料与去离子水混合,再加入磷酸二氢铝,搅拌均匀得各级粒度陶瓷浆料;
S4.将粗孔、中孔、细孔预处理软质聚氨酯泡沫体分别浸入25~100μm、15~25μm、0.5~15μm粒度陶瓷浆料中5~10min,取出泡沫体用辊压机压去多余浆料,并从上往下按照粗孔、中孔、细孔堆叠整齐,得组合泡沫体;
S5.将组合泡沫体放入真空干燥箱中,在95~100℃下干燥12~15min后置于铁丝网过滤板上,用0.5~15μm粒度陶瓷浆料对组合泡沫体淋浆,待组合泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥12~15min,重复上述淋浆操作2~3次,得碳化硅陶瓷生坯;
S6.将碳化硅陶瓷生坯干燥后转入窑炉中,以1℃/min速率升温至600℃,保持温度0.5~1h后,再以1℃/min速率继续升温至1400℃,保持温度2~3h,自然冷却至室温,得梯度孔道碳化硅陶瓷过滤板。
本发明与其他方法相比,有益技术效果是:
(1)本发明使用不同孔径的软质聚氨酯泡沫体为骨架,经碱浸泡去除网络间膜,提高表面粗糙度,并用羧甲基纤维素钠溶液改善表面的润湿性,提高泡沫体的挂浆能力,再用配置的碳化硅陶瓷浆料一次浸浆后依次层叠,形成更加合理的孔道梯度,再经多次淋浆固化,制得陶瓷生坯,高温烧结制得梯度孔道碳化硅陶瓷过滤板,本发明通过多次淋浆固化,充分吸附密实陶瓷浆料,强化陶瓷浆料的结合度,改善基体机械强度,减少掉粒现象;
(2)本发明上层网孔大,下层网孔小,有利于孔径调控,产品性能优良,强度高、开口气孔率高,过滤孔不容易堵塞,具有广阔的应用前景。
具体实施方式
先取粗孔、中孔、细孔软质聚氨酯泡沫体剪裁成相同大小的圆片状,并在60~70℃下,浸泡在质量分数为10%氢氧化钠溶液中2~3h,取出软质聚氨酯泡沫体并用去离子水洗涤2~3次后转入质量分数为2%羧甲基纤维素钠溶液中浸泡1~2h,取出得预处理软质聚氨酯泡沫体,再称取450~600g碳化硅,100~120g高岭土,110~130g钾长石,50~60g膨润土,50~60g氧化铝,30~50g白刚玉,10~20g滑石粉,50~80g硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的各级粒度复合粉料,分别取100~120g各级粒度的复合粉料与50~55g去离子水混合,搅拌混合均匀后,再加入15~16g磷酸二氢铝,搅拌均匀得各级粒度陶瓷浆料,将粗孔预处理软质聚氨酯泡沫体浸入25~100μm粒度陶瓷浆料中5~10min,将中孔预处理软质聚氨酯泡沫体浸入15~25μm粒度陶瓷浆料中5~10min,将细孔预处理软质聚氨酯泡沫体浸入0.5~15μm粒度陶瓷浆料中5~10min,取出泡沫体用辊压机压去多余浆料,并从上往下按照粗孔、中孔、细孔堆叠整齐,得组合泡沫体,将组合泡沫体放入真空干燥箱中,在95~100℃下干燥12~15min后置于铁丝网过滤板上,用0.5~15μm粒度陶瓷浆料对组合泡沫体淋浆,待组合泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥12~15min,重复上述淋浆操作2~3次,得碳化硅陶瓷生坯,最后将碳化硅陶瓷生坯置于干燥箱中,在110~120℃下干燥6~8h后转入窑炉中,以1℃/min速率升温至600℃,保持温度0.5~1h后,再以1℃/min速率继续升温至1400℃,保持温度2~3h,自然冷却至室温,得梯度孔道碳化硅陶瓷过滤板,所述粗孔、中孔、细孔预处理软质聚氨酯泡沫体孔径依次为500~1000μm、200~500μm、50~200μm。
实例1
先取粗孔、中孔、细孔软质聚氨酯泡沫体剪裁成相同大小的圆片状,并在60℃下,浸泡在质量分数为10%氢氧化钠溶液中2h,取出软质聚氨酯泡沫体并用去离子水洗涤2次后转入质量分数为2%羧甲基纤维素钠溶液中浸泡1h,取出得预处理软质聚氨酯泡沫体,再称取450g碳化硅,100g高岭土,110g钾长石,50g膨润土,50g氧化铝,30g白刚玉,10g滑石粉,50g硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的各级粒度复合粉料,分别取100g各级粒度的复合粉料与50g去离子水混合,搅拌混合均匀后,再加入15g磷酸二氢铝,搅拌均匀得各级粒度陶瓷浆料,将粗孔预处理软质聚氨酯泡沫体浸入25~100μm粒度陶瓷浆料中5min,将中孔预处理软质聚氨酯泡沫体浸入15~25μm粒度陶瓷浆料中5min,将细孔预处理软质聚氨酯泡沫体浸入0.5~15μm粒度陶瓷浆料中5min,取出泡沫体用辊压机压去多余浆料,并从上往下按照粗孔、中孔、细孔堆叠整齐,得组合泡沫体,将组合泡沫体放入真空干燥箱中,在95℃下干燥12min后置于铁丝网过滤板上,用0.5~15μm粒度陶瓷浆料对组合泡沫体淋浆,待组合泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥12min,重复上述淋浆操作2次,得碳化硅陶瓷生坯,最后将碳化硅陶瓷生坯置于干燥箱中,在110℃下干燥6h后转入窑炉中,以1℃/min速率升温至600℃,保持温度0.5h后,再以1℃/min速率继续升温至1400℃,保持温度2h,自然冷却至室温,得梯度孔道碳化硅陶瓷过滤板,所述粗孔、中孔、细孔预处理软质聚氨酯泡沫体孔径依次为1000μm、500μm、200μm。
实例2
先取粗孔、中孔、细孔软质聚氨酯泡沫体剪裁成相同大小的圆片状,并在65℃下,浸泡在质量分数为10%氢氧化钠溶液中3h,取出软质聚氨酯泡沫体并用去离子水洗涤3次后转入质量分数为2%羧甲基纤维素钠溶液中浸泡2h,取出得预处理软质聚氨酯泡沫体,再称取520g碳化硅,110g高岭土,120g钾长石,55g膨润土,55g氧化铝,40g白刚玉,15g滑石粉,65g硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的各级粒度复合粉料,分别取110g各级粒度的复合粉料与53g去离子水混合,搅拌混合均匀后,再加入16g磷酸二氢铝,搅拌均匀得各级粒度陶瓷浆料,将粗孔预处理软质聚氨酯泡沫体浸入25~100μm粒度陶瓷浆料中8min,将中孔预处理软质聚氨酯泡沫体浸入15~25μm粒度陶瓷浆料中8min,将细孔预处理软质聚氨酯泡沫体浸入0.5~15μm粒度陶瓷浆料中8min,取出泡沫体用辊压机压去多余浆料,并从上往下按照粗孔、中孔、细孔堆叠整齐,得组合泡沫体,将组合泡沫体放入真空干燥箱中,在98℃下干燥13min后置于铁丝网过滤板上,用0.5~15μm粒度陶瓷浆料对组合泡沫体淋浆,待组合泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥13min,重复上述淋浆操作3次,得碳化硅陶瓷生坯,最后将碳化硅陶瓷生坯置于干燥箱中,在115℃下干燥7h后转入窑炉中,以1℃/min速率升温至600℃,保持温度0.8h后,再以1℃/min速率继续升温至1400℃,保持温度3h,自然冷却至室温,得梯度孔道碳化硅陶瓷过滤板,所述粗孔、中孔、细孔预处理软质聚氨酯泡沫体孔径依次为1000μm、500μm、200μm。
实例3
先取粗孔、中孔、细孔软质聚氨酯泡沫体剪裁成相同大小的圆片状,并在70℃下,浸泡在质量分数为10%氢氧化钠溶液中3h,取出软质聚氨酯泡沫体并用去离子水洗涤3次后转入质量分数为2%羧甲基纤维素钠溶液中浸泡2h,取出得预处理软质聚氨酯泡沫体,再称取600g碳化硅,120g高岭土,130g钾长石,60g膨润土,60g氧化铝,50g白刚玉,20g滑石粉,80g硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的复合粉料,分别取120g各级粒度的复合粉料与55g去离子水混合,搅拌混合均匀后,再加入16g磷酸二氢铝,搅拌均匀得各级粒度陶瓷浆料,将粗孔预处理软质聚氨酯泡沫体浸入25~100μm粒度陶瓷浆料中10min,将中孔预处理软质聚氨酯泡沫体浸入15~25μm粒度陶瓷浆料中10min,将细孔预处理软质聚氨酯泡沫体浸入0.5~15μm粒度陶瓷浆料中10min,取出泡沫体用辊压机压去多余浆料,并从上往下按照粗孔、中孔、细孔堆叠整齐,得组合泡沫体,将组合泡沫体放入真空干燥箱中,在100℃下干燥15min后置于铁丝网过滤板上,用0.5~15μm粒度陶瓷浆料对组合泡沫体淋浆,待组合泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥15min,重复上述淋浆操作3次,得碳化硅陶瓷生坯,最后将碳化硅陶瓷生坯置于干燥箱中,在120℃下干燥8h后转入窑炉中,以1℃/min速率升温至600℃,保持温度1h后,再以1℃/min速率继续升温至1400℃,保持温度3h,自然冷却至室温,得梯度孔道碳化硅陶瓷过滤板,所述粗孔、中孔、细孔预处理软质聚氨酯泡沫体孔径依次为1000μm、500μm、200μm。
对照例:宜兴某公司生产的陶瓷过滤板。
将上述实施例所得梯度孔道碳化硅陶瓷过滤板与对照例的陶瓷过滤板进行检测,具体检测如下:
1、常温抗压强度:按照GB/T4740标准进行测定;
2、常温抗折强度:按照GB/T4741标准,采用电子万能试验机进行测定;
3、开口气孔率:按照GB/T1966标准进行测定;
4、抗热震性:按照《耐火制品抗热震性试验方法》(YB4018)进行测定,先将加热炉预热至750℃保温15min后,再分别将上述实施例所得梯度孔道碳化硅陶瓷过滤板与对照例的陶瓷过滤板迅速移入到炉膛内,并保持30min,然后打开炉门,将陶瓷过滤板迅速移出炉膛,让其暴露在空气中自然冷却,这一过程重复6次后,观察陶瓷过滤板是否出现开裂、陶粒剥落、断裂现象。
结果如表一所示。
表一:
由上表可知,本发明梯度孔道碳化硅陶瓷过滤板具有较高的强度,开口气孔率高,值得推广与使用。
Claims (9)
1.一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述过滤板为粗孔、中孔、细孔陶瓷过滤片依次层叠后挂浆、干燥、烧制而成,所述粗孔陶瓷过滤片为粗孔预处理软质聚氨酯泡沫体浸泡25~100μm粒度陶瓷浆料后干燥制得,所述中孔陶瓷过滤片为中孔预处理软质聚氨酯泡沫体浸泡15~25μm粒度陶瓷浆料后干燥制得,所述细孔陶瓷过滤片为细孔预处理软质聚氨酯泡沫体浸泡0.5~15μm粒度陶瓷浆料后干燥制得,所述粗孔、中孔、细孔预处理软质聚氨酯泡沫体孔径依次为500~1000μm、200~500μm、50~200μm。
2.如权利要求1所述的一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述各级粒度陶瓷浆料为各级粒度复合粉料与去离子水、磷酸二氢铝搅拌均匀制得。
3.如权利要求2所述的一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述各级粒度陶瓷浆料由100~120重量份各级粒度复合粉料,50~55重量份去离子水,15~16重量份磷酸二氢铝组成。
4.如权利要求2或3所述的一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述各级粒度复合粉料为碳化硅、高岭土、钾长石、膨润土、氧化铝、白刚玉、滑石粉、硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的各级粒度复合粉料。
5.如权利要求2~4任意一项所述的一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述各级粒度复合粉料由450~600重量份碳化硅,100~120重量份高岭土,110~130重量份钾长石,50~60重量份膨润土,50~60重量份氧化铝,30~50重量份白刚玉,10~20重量份滑石粉,50~80重量份硅微粉组成。
6.如权利要求1所述的一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述预处理软质聚氨酯泡沫体为软质聚氨酯泡沫体依次用质量分数为10%氢氧化钠溶液和质量分数为2%羧甲基纤维素钠溶液浸泡处理得到。
7.如权利要求1所述的一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述挂浆过程为用0.5~15μm粒度陶瓷浆料对泡沫体淋浆,待泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥12~15min,重复上述淋浆操作2~3次。
8.如权利要求1所述的一种梯度孔道碳化硅陶瓷过滤板,其特征在于,所述烧制过程为将碳化硅陶瓷生坯置于干燥箱中,在110~120℃下干燥6~8h后转入窑炉中,以1℃/min速率升温至600℃,保持温度0.5~1h后,再以1℃/min速率继续升温至1400℃,保温烧制2~3h后自然冷却至室温。
9.如权利要求1~8任意一项所述的一种梯度孔道碳化硅陶瓷过滤板的制备方法,其特征在于,具体步骤为:
S1.取粗孔、中孔、细孔软质聚氨酯泡沫体剪裁成相同大小的圆片状,依次用质量分数为10%氢氧化钠溶液和质量分数为2%羧甲基纤维素钠溶液浸泡处理,得预处理软质聚氨酯泡沫体;
S2.将碳化硅、高岭土、钾长石、膨润土、氧化铝、白刚玉、滑石粉、硅微粉,装入球磨机中球磨,并筛选出粒度为25~100μm,15~25μm,0.5~15μm的各级粒度复合粉料;
S3.分别将各级粒度的复合粉料与去离子水混合,再加入磷酸二氢铝,搅拌均匀得各级粒度陶瓷浆料;
S4.将粗孔预处理软质聚氨酯泡沫体浸入25~100μm粒度陶瓷浆料中5~10min,将中孔预处理软质聚氨酯泡沫体浸入15~25μm粒度陶瓷浆料中5~10min,将细孔预处理软质聚氨酯泡沫体浸入0.5~15μm粒度陶瓷浆料中5~10min,取出泡沫体用辊压机压去多余浆料,并从上往下按照粗孔、中孔、细孔堆叠整齐,得组合泡沫体;
S5.将组合泡沫体放入真空干燥箱中,在95~100℃下干燥12~15min后置于铁丝网过滤板上,用0.5~15μm粒度陶瓷浆料对组合泡沫体淋浆,待组合泡沫体上浆料不再流出,用辊压机将多余的浆料挤出,再转入干燥箱中干燥12~15min,重复上述淋浆操作2~3次,得碳化硅陶瓷生坯;
S6.将碳化硅陶瓷生坯干燥后转入窑炉中,以1℃/min速率升温至600℃,保持温度0.5~1h后,再以1℃/min速率继续升温至1400℃,保持温度2~3h,自然冷却至室温,得梯度孔道碳化硅陶瓷过滤板。
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CN108373323A (zh) * | 2018-02-24 | 2018-08-07 | 福建贝迪陶瓷科技有限公司 | 一种泡沫陶瓷生态滤材及其制备方法 |
CN108585929A (zh) * | 2018-05-10 | 2018-09-28 | 巢湖市南特精密制造有限公司 | 一种切削液多级过滤器的加工工艺 |
CN110935237A (zh) * | 2019-11-18 | 2020-03-31 | 武汉科技大学 | 高温烟气过滤用多级孔碳化硅多孔陶瓷及其制备方法 |
CN110935237B (zh) * | 2019-11-18 | 2021-09-03 | 武汉科技大学 | 高温烟气过滤用多级孔碳化硅多孔陶瓷及其制备方法 |
CN113135770A (zh) * | 2021-04-22 | 2021-07-20 | 熊伟 | 一种直通梯度孔结构的陶瓷吸音材料及其制备方法 |
CN113548672A (zh) * | 2021-07-22 | 2021-10-26 | 南通斐腾新材料科技有限公司 | 一种有机泡沫化学生长法制备泡沫结构沸石分子筛的方法 |
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