CN114053877A - 一种碟式陶瓷膜支撑体的制备方法及其陶瓷膜制品 - Google Patents
一种碟式陶瓷膜支撑体的制备方法及其陶瓷膜制品 Download PDFInfo
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Abstract
本发明公开了一种碟式陶瓷膜支撑体的制备方法,将支撑体生坯分三层结构即上层支撑坯片、中层渗透孔槽坯片、下层支撑坯片分别进行制备,再通过粘结的方式形成整体,经干燥和煅烧而得到碟式陶瓷膜支撑体。此外,还公开了一种碟式陶瓷膜制品的制备方法及其陶瓷膜。本发明解决了复杂形状渗透孔道陶瓷膜成型难的问题,大大降低了碟式陶瓷膜的制备工艺难度,从而可获得高渗透通量、更大尺寸的圆盘型平板陶瓷膜。
Description
技术领域
本发明涉及膜分离技术领域,尤其涉及一种碟式陶瓷膜支撑体的制备方法及其陶瓷膜制品。
背景技术
无机陶瓷膜是以Al2O3、ZrO2、TiO2、SiO2、SiC等陶瓷原料经一系列特殊工艺制作而成的多孔结构分离材料,具有优异的过滤性能,同时还具有耐高温、耐溶剂、耐酸碱腐蚀、高机械强度以及易清洗可再生等优点,在化工、食品、制药等领域有着独特的技术优势。
陶瓷膜根据形状可分为管状、多通道和平板状。其中,平板陶瓷膜采用外压式过滤,即陶瓷膜的外表面为分离层,膜孔道为渗透液通道。由于具有蛋壳效应,在承受相同膜间压的情况下,平板陶瓷膜支撑体的壁厚可以小至1mm,从而大幅降低陶瓷膜的渗透阻力。但是,平板陶瓷膜所采取的膜过滤方式相当于“死端”过滤,即被截留组分直接在膜表面积累,形成浓差极化,在受压情况下形成滤饼层,使得过滤阻力持续增大,加速了膜污染的发生,从而导致渗透通量下降,影响了陶瓷膜的渗透效率和使用寿命。
为减少上述膜污染,当前普遍采用鼓气方式以增加料液的扰动,减少平板陶瓷膜的浓差极化,然而实际效果却不佳,主要是因为气泡对陶瓷膜表面的流体扰动不足。为此,也有通过增设一个旋转的圆板以提高平板陶瓷膜表面的料液扰动,这在一定程度上减少了浓差极化。另外一种解决方法是使平板陶瓷膜旋转,即制备一种碟式陶瓷膜(其中心具有一积水通孔,其内部沿径向方向设有若干孔道),通过陶瓷膜的旋转在膜表面形成剪切力,使过滤膜表面保持比较薄的滤饼层厚度,使得过滤操作保持连续、稳定的过滤状态。目前,国内外对于碟式陶瓷膜普遍是采用常规的干压法或凝胶注模法进行制备。然而,这些方法不适用于制备更为复杂、密集的渗透通道,只能制备出有限数量的直型通道。由于碟式陶瓷膜是处于高速旋转的状态,简单的直型通道加之数量有限不利于获得高的渗透通量。同时,受凝胶铸模湿坯强度的限制,目前现有技术这类陶瓷膜的直径一般是150mm左右,有些可以达到300mm左右,但无法制备出更大尺寸的圆盘型平板陶瓷膜。
发明内容
本发明的目的在于克服现有技术的不足,提供一种碟式陶瓷膜支撑体的制备方法,将支撑体生坯分三层结构即上层支撑坯片、中层渗透孔槽坯片、下层支撑坯片分别进行制备,再通过粘结的方式形成整体,以解决复杂形状渗透孔道陶瓷膜成型难的问题,大大降低碟式陶瓷膜的制备工艺难度。本发明的另一目的在于提供一种碟式陶瓷膜制品的制备方法及其陶瓷膜。
本发明的目的通过以下技术方案予以实现:
本发明提供的一种碟式陶瓷膜支撑体的制备方法,包括以下步骤:
(1)支撑体薄型坯片的制备
首先制备厚度为1.0~2.5mm的圆形坯片;
(2)支撑体生坯组件的制备
使用冲压机在所述圆形坯片的中央冲压出第一中心通孔,得到上层支撑坯片、下层支撑坯片;在所述圆形坯片的中央冲压出第二中心通孔、坯面冲压出均布的、呈镂空的渗透孔槽,得到中层渗透孔槽坯片;所述渗透孔槽的一端与第二中心通孔连通、另一端封闭;
(3)支撑体生坯组件的粘结、烧成
按照所述上层支撑坯片、中层渗透孔槽坯片、下层支撑坯片的顺序叠放,使用粘结剂溶液粘结在一起并通过压力整形而形成三层结构的整体,干燥后得到支撑体生坯,经煅烧后即得到碟式陶瓷膜支撑体。
上述方案中,本发明所述渗透孔槽以弧形呈径向设置,而排列形成螺旋状。
进一步地,本发明所述步骤(3)的粘结剂溶液为水、或浓度为0.05~3wt%的聚乙烯醇或羟丙基甲基纤维素的水溶液。
本发明的另一目的通过以下技术方案予以实现:
本发明提供的一种碟式陶瓷膜制品的制备方法,在上述碟式陶瓷膜支撑体的制备方法得到的支撑体表面涂覆分离膜层浆料形成分离膜层,而得到碟式陶瓷膜制品。
进一步地,本发明所述碟式陶瓷膜支撑体、分离膜层的原料组成及制备如下:
所述碟式陶瓷膜支撑体的薄型坯片采用干压法制备时的原料组成为:平均粒径为5~50μm的陶瓷粉体、以及用量分别为该陶瓷粉体1~8wt%、2~6wt%、1~10wt%的造孔剂、粘结剂、水;所述各组成在混料机中混合成均匀的混合料,然后将所述混合料均匀加入模具中,通过压片机压力成型而得到坯片;
所述碟式陶瓷膜支撑体的薄型坯片采用辊轧法制备时的原料组成为:平均粒径为5~50μm的陶瓷粉体、以及用量分别为该陶瓷粉体1~8wt%、2~6wt%、10~38wt%、3~6wt%的造孔剂、粘结剂、水、润滑剂;首先将陶瓷粉体、造孔剂和粘结剂在混料机中混合成均匀的混合料,然后将所述混合料与水、润滑剂在捏泥机中捏合成泥、陈腐后,使用辊轧机辊轧而得到坯片;
所述碟式陶瓷膜支撑体的薄型坯片采用流延法制备时的原料组成为:平均粒径为5~50μm的陶瓷粉体、以及用量分别为该陶瓷粉体2~6wt%、0.5~1.2wt%、1~4wt%、100~250wt%的粘结剂、分散剂、稳定剂、水;所述各组成在球磨机内球磨混合2~8h,经除泡后,在流延机上流延而得到坯片;
所述分离膜层浆料由平均粒径为0.5~1μm的陶瓷粉体、用量分别为该陶瓷粉体0.5~1.2wt%、1~4wt%、700~920wt%的分散剂、稳定剂、水组成,经搅拌混合形成悬浮液浆料。
上述方案中,本发明所述陶瓷粉体为Al2O3、ZrO2、TiO2、SiO2、SiC中的一种或其组合;所述造孔剂为淀粉;所述粘结剂为羧甲基纤维素、甲基纤维素、聚乙烯醇、羟丙基甲基纤维素中的一种或其组合;所述润滑剂为甘油、油酸、聚乙烯醇;所述分散剂为聚丙烯酸、Dolapix系列分散剂、聚乙烯吡咯烷酮中的一种或其组合,或聚乙烯亚胺,或聚乙烯亚胺与聚乙烯吡咯烷酮的组合;所述稳定剂为聚丙烯酸或聚乙烯亚胺、聚丙烯吡咯烷酮、聚乙烯醇中的一种或其组合(聚丙烯酸不能与聚乙烯亚胺互配使用)。
进一步地,本发明所述碟式陶瓷膜支撑体的生坯在1500~1650℃温度下煅烧,保温时间为2~4h,得到碟式陶瓷膜支撑体。
进一步地,本发明采用喷涂-浸涂法将所述分离膜层浆料涂覆在碟式陶瓷膜支撑体的表面,首先将分离膜层浆料置于喷枪料筒内,通过控制喷涂时间来控制喷涂厚度,干燥后将碟式陶瓷膜支撑体以径向方向置于盛有分离膜层浆料的料斗内,分离膜层浆料的液面超过碟式陶瓷膜支撑体的半径,使得碟式陶瓷膜支撑体的一半浸没到分离膜层浆料中,通过旋转使碟式陶瓷膜支撑体的所有外表面与分离膜层浆料接触而形成湿膜,经过干燥、煅烧,得到平均孔径为0.1~0.5μm、厚度为15~40μm的分离膜层。
上述方案中,本发明所述湿膜干燥后在1300~1450℃温度下煅烧,保温2~4h。
利用上述碟式陶瓷膜制品的制备方法制得的陶瓷膜。
本发明具有以下有益效果:
(1)解决了复杂渗透孔道的制备难题。
由于膜分离过程在与渗透通道处相对应的分离膜层处具有最小的渗透距离,所以,膜渗透孔道尽可能的要大。但是,膜渗透孔道过大导致上下层的膜层失去支撑,因此,要求膜渗透孔道要尽可能窄且密集分布。而且,碟片陶瓷膜是处于高速旋转状态,因此,螺旋形等特殊复杂形状更有利于获得高的渗透通量。而复杂形状以及密集度高的渗透孔道增加了常规干压法或者注浆法的工艺难度。本发明支撑体以三层组件结构的方式进行制备,采用冲压法很容易获得具有复杂形状和密集度的渗透孔道,再经过粘结方式形成整体,大大降低了碟式陶瓷膜的制备工艺难度。
(2)解决了碟式陶瓷膜烧结变形的问题。
常规干压法或者注浆法均会存在因受力不均或者坯体厚度不均等因素而导致碟式陶瓷膜密度不均的问题,这影响了碟式陶瓷膜在烧结过程中的烧结速率和烧结程度,进而产生比较大的烧结应力,导致碟式陶瓷膜发生变形。而碟式陶瓷膜对形变的容忍度很低,因为碟式陶瓷膜在使用过程中要处于较高的转速状态,即使较小的形变也会导致碟式陶瓷膜发生摇摆,进而断裂。本发明支撑体以三层组件结构的方式进行制备,有助于采用干压、辊压或者流延的方式先形成均匀厚度的坯片,然后再冲压形成一定的形状,经粘结后得到碟式陶瓷膜支撑体。本发明制备过程能够控制碟式陶瓷膜支撑体生坯的密度处于均匀对称的状态,从而能够有效控制烧结变形。
(3)解决了复杂形状陶瓷膜的成型问题。
本发明采用将碟式陶瓷膜支撑体拆分为三层进行制备,然后粘结在一起,形成复杂形状生坯,最终烧结成为结合良好的一体,解决了复杂形状陶瓷膜的成型问题。并且,可以制备出直径达450mm的大尺寸圆盘型平板陶瓷膜。
附图说明
下面将结合实施例和附图对本发明对作进一步的详细描述:
图1是本发明实施例上层支撑坯片、下层支撑坯片的结构示意图;
图2是本发明实施例中层渗透孔槽坯片的结构示意图;
图3是本发明实施例上层支撑坯片、中层渗透孔槽坯片、下层支撑坯片的装配示意图。
图中:第一中心通孔1-1,坯面1-2,第二中心通孔2-1,渗透孔槽2-2
具体实施方式
图1~图3所示为本发明一种碟式陶瓷膜制品的制备方法的实施例,在碟式陶瓷膜支撑体的表面涂覆分离膜层浆料形成分离膜层而制得。
其中,碟式陶瓷膜支撑体的制备方法,其步骤如下:
(1)采用辊轧法制备支撑体薄型坯片
将50kg平均粒径为40μm的氧化铝粉、4kg淀粉、2.5kg羟丙基甲基纤维素在混料机中混合成均匀的混合料,然后加入9kg水、1kg甘油、0.5kg聚乙烯醇在捏泥机中捏合成泥、陈腐1周后,使用辊轧机辊轧后、置于恒温恒湿干燥箱中(温度80℃,湿度90%)干燥2h,得到厚度为2mm、直径为450mm的圆形坯片;
(2)支撑体生坯组件的制备
使用冲压机在上述圆形坯片的中央冲压出第一中心通孔1-1,得到如图1所示的具有坯面1-2的上层支撑坯片、下层支撑坯片;在上述圆形坯片的中央冲压出第二中心通孔2-1、坯面冲压出均布的、呈镂空的渗透孔槽2-2,得到如图2所示的中层渗透孔槽坯片;渗透孔槽2-2的一端与第二中心通孔2-1连通、另一端封闭,以弧形呈径向设置而排列形成螺旋状;
(3)支撑体生坯组件的粘结、烧成
使用浓度为0.05wt%的PVA水溶液作为粘结剂溶液,均匀喷涂于支撑体生坯组件的表面后,按照上层支撑坯片、中层渗透孔槽坯片、下层支撑坯片的顺序叠放(见图3),经粘结剂溶液粘结在一起、并使用1MPa的压力整形而形成三层结构的整体,置于恒温恒湿干燥箱中(温度80℃,湿度90%)干燥12h得到支撑体生坯,经1650℃煅烧、保温4h,得到平均孔径为1~4μm的碟式陶瓷膜支撑体。
分离膜层浆料的制备如下:取0.05g Dolapix CE-64溶解于90g水中,加入10g平均粒径为0.5~1μm的氧化铝粉体分散后,再加入0.35g聚乙烯醇1750(聚乙烯醇需事先配制成溶液),在剧烈搅拌条件下混合在一起,获得稳定的悬浮液浆料。
分离膜层的制备如下:
采用喷涂-浸涂法将上述分离膜层浆料涂覆在碟式陶瓷膜支撑体的表面,首先将分离膜层浆料置于喷枪料筒内,向碟式陶瓷膜支撑体的表面喷涂1min得到的膜层经室温干燥后,将碟式陶瓷膜支撑体以径向方向置于盛有分离膜层浆料的料斗内。分离膜层浆料的液面超过碟式陶瓷膜支撑体的半径,使得碟式陶瓷膜支撑体的一半浸没到分离膜层浆料中,通过旋转使碟式陶瓷膜支撑体的所有外表面与分离膜层浆料接触而形成湿膜,浸涂30s,室温干燥后,经1450℃煅烧,保温3h,得到平均孔径为0.1~0.5μm、厚度为20μm的分离膜层,即制得碟式陶瓷膜制品。
Claims (10)
1.一种碟式陶瓷膜支撑体的制备方法,其特征在于包括以下步骤:
(1)支撑体薄型坯片的制备
首先制备厚度为1.0~2.5mm的圆形坯片;
(2)支撑体生坯组件的制备
使用冲压机在所述圆形坯片的中央冲压出第一中心通孔(1-1),得到上层支撑坯片、下层支撑坯片;在所述圆形坯片的中央冲压出第二中心通孔(2-1)、坯面冲压出均布的、呈镂空的渗透孔槽(2-2),得到中层渗透孔槽坯片;所述渗透孔槽(2-2)的一端与第二中心通孔(2-1)连通、另一端封闭;
(3)支撑体生坯组件的粘结、烧成
按照所述上层支撑坯片、中层渗透孔槽坯片、下层支撑坯片的顺序叠放,使用粘结剂溶液粘结在一起并通过压力整形而形成三层结构的整体,干燥后得到支撑体生坯,经煅烧后即得到碟式陶瓷膜支撑体。
2.根据权利要求1所述的碟式陶瓷膜支撑体的制备方法,其特征在于:所述渗透孔槽(2-2)以弧形呈径向设置,而排列形成螺旋状。
3.根据权利要求1所述的碟式陶瓷膜支撑体的制备方法,其特征在于:所述步骤(3)的粘结剂溶液为水、或浓度为0.05~3wt%的聚乙烯醇或羟丙基甲基纤维素的水溶液。
4.一种碟式陶瓷膜制品的制备方法,其特征在于:在权利要求1-3之一所述制备方法得到的碟式陶瓷膜支撑体表面涂覆分离膜层浆料形成分离膜层,而得到碟式陶瓷膜制品。
5.根据权利要求4所述的碟式陶瓷膜制品的制备方法,其特征在于所述碟式陶瓷膜支撑体、分离膜层的原料组成及制备如下:
所述碟式陶瓷膜支撑体的薄型坯片采用干压法制备时的原料组成为:平均粒径为5~50μm的陶瓷粉体、以及用量分别为该陶瓷粉体1~8wt%、2~6wt%、1~10wt%的造孔剂、粘结剂、水;所述各组成在混料机中混合成均匀的混合料,然后将所述混合料均匀加入模具中,通过压片机压力成型而得到坯片;
所述碟式陶瓷膜支撑体的薄型坯片采用辊轧法制备时的原料组成为:平均粒径为5~50μm的陶瓷粉体、以及用量分别为该陶瓷粉体1~8wt%、2~6wt%、10~38wt%、3~6wt%的造孔剂、粘结剂、水、润滑剂;首先将陶瓷粉体、造孔剂和粘结剂在混料机中混合成均匀的混合料,然后将所述混合料与水、润滑剂在捏泥机中捏合成泥、陈腐后,使用辊轧机辊轧而得到坯片;
所述碟式陶瓷膜支撑体的薄型坯片采用流延法制备时的原料组成为:平均粒径为5~50μm的陶瓷粉体、以及用量分别为该陶瓷粉体2~6wt%、0.5~1.2wt%、1~4wt%、100~250wt%的粘结剂、分散剂、稳定剂、水;所述各组成在球磨机内球磨混合2~8h,经除泡后,在流延机上流延而得到坯片;
所述分离膜层浆料由平均粒径为0.5~1μm的陶瓷粉体、用量分别为该陶瓷粉体0.5~1.2wt%、1~4wt%、700~920wt%的分散剂、稳定剂、水组成,经搅拌混合形成悬浮液浆料。
6.根据权利要求5所述的碟式陶瓷膜制品的制备方法,其特征在于:
所述陶瓷粉体为Al2O3、ZrO2、TiO2、SiO2、SiC中的一种或其组合;
所述造孔剂为淀粉;
所述粘结剂为羧甲基纤维素、甲基纤维素、聚乙烯醇、羟丙基甲基纤维素中的一种或其组合;
所述润滑剂为甘油、油酸、聚乙烯醇;
所述分散剂为聚丙烯酸、Dolapix系列分散剂、聚乙烯吡咯烷酮中的一种或其组合,或聚乙烯亚胺,或聚乙烯亚胺与聚乙烯吡咯烷酮的组合;
所述稳定剂为聚丙烯酸或聚乙烯亚胺、聚丙烯吡咯烷酮、聚乙烯醇中的一种或其组合。
7.根据权利要求5所述的碟式陶瓷膜制品的制备方法,其特征在于:所述碟式陶瓷膜支撑体的生坯在1500~1650℃温度下煅烧,保温时间为2~4h,得到碟式陶瓷膜支撑体。
8.根据权利要求4或5或6或7所述的碟式陶瓷膜制品的制备方法,其特征在于:采用喷涂-浸涂法将所述分离膜层浆料涂覆在碟式陶瓷膜支撑体的表面,首先将分离膜层浆料置于喷枪料筒内,通过控制喷涂时间来控制喷涂厚度,干燥后将碟式陶瓷膜支撑体以径向方向置于盛有分离膜层浆料的料斗内,分离膜层浆料的液面超过碟式陶瓷膜支撑体的半径,使得碟式陶瓷膜支撑体的一半浸没到分离膜层浆料中,通过旋转使碟式陶瓷膜支撑体的所有外表面与分离膜层浆料接触而形成湿膜,经过干燥、煅烧,得到平均孔径为0.1~0.5μm、厚度为15~40μm的分离膜层。
9.根据权利要求8所述的碟式陶瓷膜制品的制备方法,其特征在于:所述湿膜干燥后在1300~1450℃温度下煅烧,保温2~4h。
10.利用权利要求4-9之一所述碟式陶瓷膜制品的制备方法制得的陶瓷膜。
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