CN108002807A - 一种比表面积大的多孔陶瓷及其制备方法 - Google Patents
一种比表面积大的多孔陶瓷及其制备方法 Download PDFInfo
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- CN108002807A CN108002807A CN201711141861.1A CN201711141861A CN108002807A CN 108002807 A CN108002807 A CN 108002807A CN 201711141861 A CN201711141861 A CN 201711141861A CN 108002807 A CN108002807 A CN 108002807A
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Abstract
本发明公开了一种比表面积大的多孔陶瓷及其制备方法,包括以下重量法的原料:酚醛树脂3‑8份、氧化铝2.4‑5份、硼砂8‑18份、方解石10‑16份、钠闪石16‑25份、陶土75‑83份、锌镁合金粉0.6‑1.3份、石墨2‑4份、晶须0.8‑1.4份、氧化铬1‑2份、苯酚6‑10份、纳米二氧化硅4‑6份、表面活性剂2‑5份和芋头3‑10份。本发明原料来源广泛,制备工艺简单,通过芋头果胶、多孔的稳定体系等物质相互作用,得到的陶瓷具有高的孔隙率,从而增大了陶瓷的比表面积,满足了人们的使用需求。
Description
技术领域
本发明涉及陶瓷领域,具体是一种比表面积大的多孔陶瓷。
背景技术
陶瓷是用陶土和瓷土这两种不同性质的粘土为原料,经过配料、成型、干燥、焙烧等工艺流程制成的器物。瓷业是我国的传统工业,陶瓷产品是我国轻工行业的支柱产业和出口拳头产品。陶瓷产品不仅仅有日用陶瓷,工业陶瓷的种类也很多,多孔陶瓷就是工业陶瓷的其中一种。
多孔陶瓷材料是以刚玉砂、碳化硅、堇青石等优质原料为主料、经过成型和特殊高温烧结工艺制备的,多孔陶瓷多用于各种介质的精密过滤与分离、高压气体排气消音、气体分布及电解隔膜等。但是现有的多孔陶瓷的孔隙率还达不到人们的预期,人们在用多孔陶瓷当作滤芯时,滤芯的更换周期较短,人们更换滤芯的次数频繁,这就为人们的使用带来了不便。
发明内容
本发明的目的在于提供一种比表面积大的多孔陶瓷,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:
一种比表面积大的多孔陶瓷,包括以下重量法的原料:酚醛树脂3-8份、氧化铝2.4-5份、硼砂8-18份、方解石10-16份、钠闪石16-25份、陶土75-83份、锌镁合金粉0.6-1.3份、石墨2-4份、晶须0.8-1.4份、氧化铬1-2份、苯酚6-10份、纳米二氧化硅4-6份、表面活性剂2-5份和芋头3-10份。
作为本发明进一步的方案:晶须采用碳化硅、硫酸钙、碳酸钙、氧化锌和硼酸铝中的至少一种,晶须的长度为1-3厘米。
作为本发明进一步的方案:该多孔陶瓷还包括竹炭纤维1.6-3.5份。
所述比表面积大的多孔陶瓷的制备方法,具体步骤如下:
步骤一,将锌镁合金粉加入过量的盐酸溶液中,并不断地磁力搅拌,待锌镁合金粉完全溶解时用去离子水洗涤,然后置于氢氟酸溶液中搅拌60-90分钟,再用去离子水多次洗涤,真空干燥4-8小时,干燥温度为70-86摄氏度,再置于分散剂中分散,磁力搅拌1-3个小时,得到分散液;
步骤二,将苯酚加入到质量分数为50-65%的乙醇溶液中,再加入一定量的氨水,在25-28摄氏度的恒温条件下搅拌10-30分钟,待苯酚全部溶解后加入表面活性剂,继续在25-28摄氏度的恒温条件搅拌20-45分钟,然后加入过量的甲醛溶液,在25-28摄氏度的恒温条件搅拌12-15小时,将溶液转移至高压反应釜,在65-84摄氏度下进行水热反应,待反应结束后自然冷却至室温,离心洗涤分离冷冻干燥后获得第一产物;
步骤三,将芋头粉碎成碎屑,再将芋头碎屑放进玻璃容器内并加入质量分数为26-30%的盐酸浸没,加热至90-95摄氏度并且保持30-40秒,快速降温后过滤分离,得到盐酸混合溶液,将盐酸混和溶液减压低温浓缩至稀稠,然后加入质量分数为90-95%的乙醇溶液稀释,并不断搅拌,稍作静置产生芋头果胶沉淀,将玻璃容器上层的酒精过滤倒掉,再次加入等量酒精稀释、搅拌、过滤和沉淀,得到芋头果胶;
步骤四,将石墨粉碎至3-8um,然后将石墨粉倒入分散液中进行搅拌,得到第二产物;
步骤五,将酚醛树脂、氧化铝、硼砂、方解石、钠闪石、陶土、晶须、氧化铬和纳米二氧化硅进行球磨并且过240-300目筛子,得到第三产物;
步骤六,将第一产物、芋头果胶、第二产物和第三产物混合并且加入适量去离子水,混合成泥状,在惰性气氛下以3-6摄氏度/分钟的速率升温至640-680摄氏度并且保持5-8小时,再以10-15摄氏度/分钟的速率升温至960-1080摄氏度并且保温6-12小时,再用8-15摄氏度/分钟的速率降温至520摄氏度并且保温25-40分钟,最后再以3-5摄氏度/分钟的速率降温至120-150摄氏度,最后再进行炉冷,即可得到成品。
作为本发明进一步的方案:步骤五中球磨的球料比为6-9:1,球磨温度为36-45摄氏度。
与现有技术相比,本发明的有益效果是:本发明原料来源广泛,制备工艺简单,通过芋头果胶、多孔的稳定体系等物质相互作用,得到的陶瓷具有高的孔隙率,从而增大了陶瓷的比表面积,满足了人们的使用需求。
具体实施方式
下面结合具体实施方式对本专利的技术方案作进一步详细地说明。
实施例1
一种比表面积大的多孔陶瓷,包括以下重量法的原料:酚醛树脂3份、氧化铝2.4份、硼砂8份、方解石10份、钠闪石16份、陶土75份、锌镁合金粉0.6份、石墨2份、晶须0.8份、氧化铬1份、苯酚6份、纳米二氧化硅4份、表面活性剂2份和芋头3份。晶须采用硫酸钙、碳酸钙和氧化锌的混合物,晶须的长度为2厘米。
所述比表面积大的多孔陶瓷的制备方法,具体步骤如下:
步骤一,将锌镁合金粉加入过量的盐酸溶液中,并不断地磁力搅拌,待锌镁合金粉完全溶解时用去离子水洗涤,然后置于氢氟酸溶液中搅拌68分钟,再用去离子水多次洗涤,真空干燥6小时,干燥温度为75摄氏度,再置于分散剂中分散,磁力搅拌2个小时,得到分散液;
步骤二,将苯酚加入到质量分数为58%的乙醇溶液中,再加入一定量的氨水,在26摄氏度的恒温条件下搅拌24分钟,待苯酚全部溶解后加入表面活性剂,继续在25摄氏度的恒温条件搅拌30分钟,然后加入过量的甲醛溶液,在28摄氏度的恒温条件搅拌13小时,将溶液转移至高压反应釜,在72摄氏度下进行水热反应,待反应结束后自然冷却至室温,离心洗涤分离冷冻干燥后获得第一产物;
步骤三,将芋头粉碎成碎屑,再将芋头碎屑放进玻璃容器内并加入质量分数为28%的盐酸浸没,加热至92摄氏度并且保持36秒,快速降温后过滤分离,得到盐酸混合溶液,将盐酸混和溶液减压低温浓缩至稀稠,然后加入质量分数为92%的乙醇溶液稀释,并不断搅拌,稍作静置产生芋头果胶沉淀,将玻璃容器上层的酒精过滤倒掉,再次加入等量酒精稀释、搅拌、过滤和沉淀,得到芋头果胶;
步骤四,将石墨粉碎至6um,然后将石墨粉倒入分散液中进行搅拌,得到第二产物;
步骤五,将酚醛树脂、氧化铝、硼砂、方解石、钠闪石、陶土、晶须、氧化铬和纳米二氧化硅进行球磨并且过270目筛子,得到第三产物;
步骤六,将第一产物、芋头果胶、第二产物和第三产物混合并且加入适量去离子水,混合成泥状,在惰性气氛下以4摄氏度/分钟的速率升温至640摄氏度并且保持6小时,再以12摄氏度/分钟的速率升温至980摄氏度并且保温10小时,再用12摄氏度/分钟的速率降温至520摄氏度并且保温30分钟,最后再以3摄氏度/分钟的速率降温至130摄氏度,最后再进行炉冷,即可得到成品。
实施例2
一种比表面积大的多孔陶瓷,包括以下重量法的原料:竹炭纤维2.8份、酚醛树脂6份、氧化铝4份、硼砂14份、方解石13份、钠闪石22份、陶土80份、锌镁合金粉0.9份、石墨3.5份、晶须1.2份、氧化铬1.6份、苯酚8份、纳米二氧化硅5份、表面活性剂4份和芋头7份。
所述比表面积大的多孔陶瓷的制备方法,具体步骤如下:
步骤一,将锌镁合金粉加入过量的盐酸溶液中,并不断地磁力搅拌,待锌镁合金粉完全溶解时用去离子水洗涤,然后置于氢氟酸溶液中搅拌80分钟,再用去离子水多次洗涤,真空干燥6小时,干燥温度为82摄氏度,再置于分散剂中分散,磁力搅拌2个小时,得到分散液;
步骤二,将苯酚加入到质量分数为56%的乙醇溶液中,再加入一定量的氨水,在28摄氏度的恒温条件下搅拌20分钟,待苯酚全部溶解后加入表面活性剂,继续在26摄氏度的恒温条件搅拌30分钟,然后加入过量的甲醛溶液,在26摄氏度的恒温条件搅拌13小时,将溶液转移至高压反应釜,在75摄氏度下进行水热反应,待反应结束后自然冷却至室温,离心洗涤分离冷冻干燥后获得第一产物;
步骤三,将芋头粉碎成碎屑,再将芋头碎屑放进玻璃容器内并加入质量分数为30%的盐酸浸没,加热至93摄氏度并且保持35秒,快速降温后过滤分离,得到盐酸混合溶液,将盐酸混和溶液减压低温浓缩至稀稠,然后加入质量分数为92%的乙醇溶液稀释,并不断搅拌,稍作静置产生芋头果胶沉淀,将玻璃容器上层的酒精过滤倒掉,再次加入等量酒精稀释、搅拌、过滤和沉淀,得到芋头果胶;
步骤四,将竹炭纤维和石墨粉碎至6um,然后将石墨粉和竹炭纤维粉末倒入分散液中进行搅拌,得到第二产物;
步骤五,将酚醛树脂、氧化铝、硼砂、方解石、钠闪石、陶土、晶须、氧化铬和纳米二氧化硅进行球磨并且过280目筛子,得到第三产物;
步骤六,将第一产物、芋头果胶、第二产物和第三产物混合并且加入适量去离子水,混合成泥状,在惰性气氛下以6摄氏度/分钟的速率升温至660摄氏度并且保持6小时,再以15摄氏度/分钟的速率升温至1040摄氏度并且保温10小时,再用12摄氏度/分钟的速率降温至520摄氏度并且保温36分钟,最后再以4摄氏度/分钟的速率降温至140摄氏度,最后再进行炉冷,即可得到成品。
实施例3
一种比表面积大的多孔陶瓷,包括以下重量法的原料:竹炭纤维3.5份、酚醛树脂8份、氧化铝5份、硼砂18份、方解石16份、钠闪石25份、陶土83份、锌镁合金粉1.3份、石墨4份、晶须1.4份、氧化铬2份、苯酚10份、纳米二氧化硅6份、表面活性剂5份和芋头10份。晶须采用碳化硅、硫酸钙、碳酸钙、氧化锌和硼酸铝的混合物,晶须的长度为2厘米。
所述比表面积大的多孔陶瓷的制备方法,具体步骤如下:
步骤一,将锌镁合金粉加入过量的盐酸溶液中,并不断地磁力搅拌,待锌镁合金粉完全溶解时用去离子水洗涤,然后置于氢氟酸溶液中搅拌90分钟,再用去离子水多次洗涤,真空干燥6小时,干燥温度为84摄氏度,再置于分散剂中分散,磁力搅拌2个小时,得到分散液;
步骤二,将苯酚加入到质量分数为64%的乙醇溶液中,再加入一定量的氨水,在28摄氏度的恒温条件下搅拌20分钟,待苯酚全部溶解后加入表面活性剂,继续在26摄氏度的恒温条件搅拌40分钟,然后加入过量的甲醛溶液,在27摄氏度的恒温条件搅拌15小时,将溶液转移至高压反应釜,在80摄氏度下进行水热反应,待反应结束后自然冷却至室温,离心洗涤分离冷冻干燥后获得第一产物;
步骤三,将芋头粉碎成碎屑,再将芋头碎屑放进玻璃容器内并加入质量分数为30%的盐酸浸没,加热至92摄氏度并且保持36秒,快速降温后过滤分离,得到盐酸混合溶液,将盐酸混和溶液减压低温浓缩至稀稠,然后加入质量分数为94%的乙醇溶液稀释,并不断搅拌,稍作静置产生芋头果胶沉淀,将玻璃容器上层的酒精过滤倒掉,再次加入等量酒精稀释、搅拌、过滤和沉淀,得到芋头果胶;
步骤四,将竹炭纤维和石墨粉碎至5um,然后将石墨粉和竹炭纤维粉末倒入分散液中进行搅拌,得到第二产物;
步骤五,将酚醛树脂、氧化铝、硼砂、方解石、钠闪石、陶土、晶须、氧化铬和纳米二氧化硅进行球磨并且过280目筛子,球料比为8:1,球磨温度为40摄氏度,得到第三产物;
步骤六,将第一产物、芋头果胶、第二产物和第三产物混合并且加入适量去离子水,混合成泥状,在惰性气氛下以6摄氏度/分钟的速率升温至670摄氏度并且保持6小时,再以14摄氏度/分钟的速率升温至1060摄氏度并且保温11小时,再用10摄氏度/分钟的速率降温至520摄氏度并且保温30分钟,最后再以5摄氏度/分钟的速率降温至150摄氏度,最后再进行炉冷,即可得到成品。
锌镁合金粉经过酸洗后形成多孔结构,石墨可以悬浮在分散液中并且吸附在合金表面,形成多孔的稳定体系,将第一产物、芋头果胶、第二产物和第三产物利用不同温度的烧结并且烧结后进行降温时效处理,芋头果胶、多孔的稳定体系等物质相互作用,得到的陶瓷具有高的孔隙率,从而增大了陶瓷的比表面积。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外,应当理解,虽然本说明书按照实施方式加以描述,但并非每个实施方式仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施方式。
Claims (5)
1.一种比表面积大的多孔陶瓷,其特征在于,包括以下重量法的原料:酚醛树脂3-8份、氧化铝2.4-5份、硼砂8-18份、方解石10-16份、钠闪石16-25份、陶土75-83份、锌镁合金粉0.6-1.3份、石墨2-4份、晶须0.8-1.4份、氧化铬1-2份、苯酚6-10份、纳米二氧化硅4-6份、表面活性剂2-5份和芋头3-10份。
2.根据权利要求1所述的比表面积大的多孔陶瓷,其特征在于,所述晶须采用碳化硅、硫酸钙、碳酸钙、氧化锌和硼酸铝中的至少一种,晶须的长度为1-3厘米。
3.根据权利要求1所述的比表面积大的多孔陶瓷,其特征在于,该多孔陶瓷还包括竹炭纤维1.6-3.5份。
4.一种如权利要求1-3任一所述的比表面积大的多孔陶瓷的制备方法,其特征在于,具体步骤如下:
步骤一,将锌镁合金粉加入过量的盐酸溶液中,并不断地磁力搅拌,待锌镁合金粉完全溶解时用去离子水洗涤,然后置于氢氟酸溶液中搅拌60-90分钟,再用去离子水多次洗涤,真空干燥4-8小时,干燥温度为70-86摄氏度,再置于分散剂中分散,磁力搅拌1-3个小时,得到分散液;
步骤二,将苯酚加入到质量分数为50-65%的乙醇溶液中,再加入一定量的氨水,在25-28摄氏度的恒温条件下搅拌10-30分钟,待苯酚全部溶解后加入表面活性剂,继续在25-28摄氏度的恒温条件搅拌20-45分钟,然后加入过量的甲醛溶液,在25-28摄氏度的恒温条件搅拌12-15小时,将溶液转移至高压反应釜,在65-84摄氏度下进行水热反应,待反应结束后自然冷却至室温,离心洗涤分离冷冻干燥后获得第一产物;
步骤三,将芋头粉碎成碎屑,再将芋头碎屑放进玻璃容器内并加入质量分数为26-30%的盐酸浸没,加热至90-95摄氏度并且保持30-40秒,快速降温后过滤分离,得到盐酸混合溶液,将盐酸混和溶液减压低温浓缩至稀稠,然后加入质量分数为90-95%的乙醇溶液稀释,并不断搅拌,稍作静置产生芋头果胶沉淀,将玻璃容器上层的酒精过滤倒掉,再次加入等量酒精稀释、搅拌、过滤和沉淀,得到芋头果胶;
步骤四,将石墨粉碎至3-8um,然后将石墨粉倒入分散液中进行搅拌,得到第二产物;
步骤五,将酚醛树脂、氧化铝、硼砂、方解石、钠闪石、陶土、晶须、氧化铬和纳米二氧化硅进行球磨并且过240-300目筛子,得到第三产物;
步骤六,将第一产物、芋头果胶、第二产物和第三产物混合并且加入适量去离子水,混合成泥状,在惰性气氛下以3-6摄氏度/分钟的速率升温至640-680摄氏度并且保持5-8小时,再以10-15摄氏度/分钟的速率升温至960-1080摄氏度并且保温6-12小时,再用8-15摄氏度/分钟的速率降温至520摄氏度并且保温25-40分钟,最后再以3-5摄氏度/分钟的速率降温至120-150摄氏度,最后再进行炉冷,即可得到成品。
5.根据权利要求4所述的比表面积大的多孔陶瓷的制备方法,其特征在于,所述步骤五中球磨的球料比为6-9:1,球磨温度为36-45摄氏度。
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