CN116161980A - 疏水多孔陶瓷复合材料及其制备方法和应用 - Google Patents
疏水多孔陶瓷复合材料及其制备方法和应用 Download PDFInfo
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- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 101
- 239000002131 composite material Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title abstract description 23
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 71
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 47
- 238000001035 drying Methods 0.000 claims abstract description 37
- 239000012778 molding material Substances 0.000 claims abstract description 25
- 238000002791 soaking Methods 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 17
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 6
- 229930006000 Sucrose Natural products 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005350 fused silica glass Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
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- 238000004321 preservation Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 239000000463 material Substances 0.000 description 9
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
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- 229910021641 deionized water Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- QRPMCZNLJXJVSG-UHFFFAOYSA-N trichloro(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)[Si](Cl)(Cl)Cl QRPMCZNLJXJVSG-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
本申请提供了一种疏水多孔陶瓷复合材料及其制备方法和应用,其制备方法包括:将陶瓷原料和粘结剂混合,制备塑形料;将塑形料挤压成块状后,进行烘干、烧结处理,制备多孔陶瓷材料;将多孔陶瓷材料在含有碳源的溶液中进行浸泡处理后,干燥,制备碳源负载的多孔陶瓷材料;将碳源负载的多孔陶瓷材料热处理,制备疏水多孔陶瓷复合材料。本申请通过烧结陶瓷原料提高了多孔陶瓷材料的机械强度,通过对负载碳源的多孔陶瓷材料的热处理得到碳在多孔陶瓷材料表面及陶瓷内部都牢固结合的疏水多孔陶瓷复合材料。
Description
技术领域
本申请涉及陶瓷技术领域,特别是涉及一种疏水多孔陶瓷复合材料及其制备方法和应用。
背景技术
疏水材料由于具有疏水性,因而具有防水和自清洁的功能,在油水分离方面具有很高的价值,因此疏水材料近年来成为研究热点之一。
材料表面的表面形貌、化学性质和微观几何结构决定了材料的疏水性。制备材料的疏水表面的方法包括两类:一类是在具有低表面能的材料表面进行粗糙化处理;另一类是在具有一定粗糙结构的表面上修饰低表面能物质。
目前,疏水材料制备方法的出发点包括“材料的疏水性”和“重新设计疏水涂层”两个方面。其中,以“陶瓷材料本身的疏水性”为出发点的疏水陶瓷材料的制备方法存在所需原料较多,成本较高的特点;以“重新设计疏水涂层”为出发点也有很多研究,例如,现有技术公开了一种技术方案,将天然沸石在乙醇中超声分散,再加入全氟癸基三氯硅烷,继续超声分散后将基材浸入分散液中并干燥的制备方法得到浸泡两到三次后,基材表面即形成超疏水涂层。但是这种制备方法存在“疏水涂层与基材表面的结合力不强,容易脱落失去疏水能力”的问题。
发明内容
本申请的目的在于提供一种疏水多孔陶瓷复合材料及其制备方法和应用,用以解决疏水材料的疏水涂层与基底的结合性差的问题。具体技术方案如下:
本申请第一方面提供了一种疏水多孔陶瓷复合材料的制备方法,包括:将陶瓷原料和粘结剂混合,制备塑形料;将塑形料挤压成块状后,进行烘干、烧结处理,制备多孔陶瓷材料;将多孔陶瓷材料在含有碳源的溶液中进行浸泡处理后,干燥,制备碳源负载的多孔陶瓷材料;将碳源负载的多孔陶瓷材料热处理,制备疏水多孔陶瓷复合材料;其中,陶瓷原料包括氧化铝、熔融石英砂、氧化钛、氮化硅、碳化硅中的至少一种,粘结剂包括硅溶胶、水玻璃中的至少一种,碳源包括蔗糖、淀粉、羟乙基纤维素、聚乙二醇中的至少一种。
在本申请的一些实施方案中,疏水多孔陶瓷复合材料的孔隙率为10~30%。
在本申请的一些实施方案中,塑形料中陶瓷原料和粘结剂的质量比为4∶1~2∶1;含有碳源的溶液中碳源的质量分数为10~40%。
在本申请的一些实施方案中,硅溶胶中二氧化硅的质量分数为20~30%;水玻璃中硅酸钠的质量分数为20~30%。
在本申请的一些实施方案中,烘干的温度为80~100℃、时间为1~3h。
在本申请的一些实施方案中,烧结处理的升温速率为3~15℃/min、烧结温度为800~1200℃、保温时间为1~3h。
在本申请的一些实施方案中,浸泡处理的真空度为-0.05~-0.1MPa、时间为6~24h;干燥的温度为80~120℃、时间为0.5~2h。
在本申请的一些实施方案中,热处理的真空度为-0.05~-0.1MPa、温度为400~550℃、时间为1~3h;陶瓷原料的颗粒粒径为20~100μm。
本申请第二个方面提供了一种上述的制备方法得到的疏水多孔陶瓷复合材料。
本申请第三方面提供了一种上述疏水多孔陶瓷复合材料在油水分离方面的应用。
本申请有益效果:
本申请提供的疏水多孔陶瓷复合材料的制备方法,通过烧结陶瓷原料提高了多孔陶瓷材料的机械强度,通过对负载碳源的多孔陶瓷材料的热处理得到碳在多孔陶瓷材料表面及陶瓷内部都牢固结合的具有较大粗糙度疏水多孔陶瓷复合材料。
当然,实施本申请的任一产品或方法并不一定需要同时达到以上所述的所有优点。
附图说明
为了更清楚地说明本申请或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本申请的一些实施例,对于本领域普通技术人员来讲,还可以根据这些附图获得其他的实施例。
图1A为根据本申请的实施例1制备的多孔陶瓷材料的照片;
图1B为根据本申请的实施例1制备的多孔陶瓷材料的照片;
图1C为根据本申请的实施例1制备的多孔陶瓷材料的SEM照片;
图2A为根据本申请的实施例1制备的疏水多孔陶瓷复合材料的照片;
图2B为根据本申请的实施例1制备的疏水多孔陶瓷复合材料的照片;
图2C为根据本申请的实施例1制备的疏水多孔陶瓷复合材料的SEM照片;
图3显示根据本申请的实施例1制备的疏水多孔陶瓷复合材料与水的接触角的示意图;
图4为根据本申请的实施例1制备的疏水多孔陶瓷复合材料表面形成的液滴效果照片;
图5显示根据本申请的实施例2制备的疏水多孔陶瓷复合材料与水的接触角的示意图;
图6显示根据本申请的实施例3制备的疏水多孔陶瓷复合材料与水的接触角的示意图;
图7显示根据本申请的实施例4制备的疏水多孔陶瓷复合材料与水的接触角的示意图;
图8显示根据本申请的实施例5制备的疏水多孔陶瓷复合材料与水的接触角的示意图;
图9显示根据本申请的实施例6制备的疏水多孔陶瓷复合材料与水的接触角的示意图;
图10显示根据本申请的实施例7制备的疏水多孔陶瓷复合材料与水的接触角的示意图;
图11为根据本申请的实施例1制备的疏水多孔陶瓷复合材料重复使用前A部分和使用20次后B部分的SEM照片的对比图。
具体实施方式
下面将结合本申请中的附图,对本申请中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本申请一部分实施例,而不是全部的实施例。基于本申请中的实施例,本领域普通技术人员基于本申请所获得的所有其他实施例,都属于本申请保护的范围。
本申请提供了一种疏水多孔陶瓷复合材料的制备方法,包括:将陶瓷原料和粘结剂混合,制备塑形料;将上述塑形料挤压成块状后,进行烘干、烧结处理,制备多孔陶瓷材料;将上述多孔陶瓷材料在含有碳源的溶液中进行浸泡处理后,干燥,制备碳源负载的多孔陶瓷材料;将上述碳源负载的多孔陶瓷材料热处理,制备疏水多孔陶瓷复合材料;其中,上述陶瓷原料包括氧化铝、熔融石英砂、氧化钛、氮化硅、碳化硅中的至少一种,上述粘结剂包括硅溶胶、水玻璃中的至少一种,上述碳源包括蔗糖、淀粉、羟乙基纤维素、聚乙二醇中的至少一种。
本申请提供的疏水多孔陶瓷复合材料的制备方法,通过烧结陶瓷原料提高了多孔陶瓷材料的粗糙度,通过对负载碳源的多孔陶瓷材料的热处理得到碳在多孔陶瓷材料表面及陶瓷内部都牢固结合的疏水多孔陶瓷复合材料。
在本申请的一些实施方案中,上述疏水多孔陶瓷复合材料的孔隙率为10~30%。
在本申请的一些实施方案中,上述塑形料中陶瓷原料和粘结剂的质量比为4∶1~2∶1;上述含有碳源的溶液中碳源的质量分数为10~40%。
在本申请的一些实施方案中,上述硅溶胶中二氧化硅的质量分数为20~30%;上述水玻璃中硅酸钠的质量分数为20~30%。
在本申请的一些实施方案中,上述烘干的温度为80~100℃、时间为1~3h。
在本申请的一些实施方案中,上述烧结处理的升温速率为3~15℃/min、烧结温度为800~1200℃、保温时间为1~3h。
在本申请的一些实施方案中,上述浸泡处理的真空度为-0.05~-0.1MPa、时间为6~24h;上述干燥的温度为80~120℃、时间为0.5~2h。
在本申请的一些实施方案中,上述热处理的真空度为-0.05~-0.1MPa、温度为400~550℃、时间为1~3h;上述陶瓷原料的颗粒粒径为20~100μm。
本申请还提供了一种上述制备方法得到的疏水多孔陶瓷复合材料。
本申请提供的疏水多孔陶瓷复合材料中的多孔陶瓷材料的表面粗糙度高,碳源在高温热处理的过程中生成的碳活性高,能够与多孔陶瓷材料紧密地结合,进而使得碳在多孔陶瓷材料的表面及内部的结合牢固,能够长久稳定地保持优异的疏水性能,并且陶瓷复合材料的机械强度高,耐摩擦。
本申请还提供了一种上述疏水多孔陶瓷复合材料在油水分离方面的应用。
本申请中多孔材料的孔隙率是使用压汞法测试得到的。
本申请中制备得到的疏水多孔陶瓷复合材料可以重复使用,重复使用方法为:每次多孔陶瓷复合材料使用后,分别用去离子水,酒精超声清洗2遍。然后,经过100℃干燥后用于下次使用。
实施例1
<制备疏水多孔陶瓷复合材料>
将50g粒径为100μm的氧化铝颗粒和质量分数为30%的硅溶胶按质量比为4∶1混合均匀,制备塑形料;
将所得塑形料在直径为3cm的模具中挤压成圆柱型块体,所得圆柱型块体在100℃的烘箱中烘干1h后,在马弗炉内以5℃/min的升温速率升温至1200℃,保温1h进行烧结处理,制备多孔陶瓷材料;
将所制备的多孔陶瓷材料浸泡于50mL质量分数为30%的蔗糖溶液中,抽真空,真空度为-0.08MPa,浸泡处理6h后,在80℃的烘箱中干燥2h,制备碳源负载的多孔陶瓷材料;
将所制备的碳源负载的多孔陶瓷材料在管式炉内,在真空度为-0.09MPa的真空中,以5℃/min的升温速率升温至500℃,保温2h进行热处理,制备疏水多孔陶瓷复合材料。
<性能测试>
将实施例1制备的多孔陶瓷材料进行形貌分析,结果见图1A、图1B和图1C。
根据图1A和图1B所示的氧化铝多孔陶瓷材料的照片图,实施例1制备的氧化铝多孔陶瓷材料的颜色为白色,具有多孔结构,表面粗糙。
根据图1C所示的氧化铝多孔陶瓷材料的SEM照片,实施例1制备的氧化铝多孔陶瓷材料的内部具有多孔结构,粒径在80μm左右。
将实施例1制备的疏水多孔陶瓷复合材料进行形貌和疏水性的分析,结果见图2A、图2B、图2C、图3和图4。
根据图2A和图2B所示的疏水多孔陶瓷复合材料的照片图,实施例1制备的疏水多孔陶瓷复合材料为黑色,疏水多孔陶瓷复合材料的表面及内部都是均匀的黑色。
根据图2C所示的疏水多孔陶瓷复合材料的SEM图,实施例1制备的疏水多孔陶瓷复合材料的陶瓷颗粒表面附有一层或多层的碳,但是没有堵塞陶瓷的孔道,影响疏水多孔陶瓷复合材料的粗糙度。
根据图3所示的疏水多孔陶瓷复合材料与水的接触角θ约为117.7°,说明实施例1制备的疏水多孔陶瓷复合材料的疏水性良好。
根据图4所示的疏水多孔陶瓷复合材料表面形成的液滴效果,进一步证明了实施例1制备的疏水多孔陶瓷复合材料的疏水性良好。
实施例1制备的疏水多孔陶瓷复合材料的孔隙率为26.1%。
实施例1制备的疏水多孔陶瓷复合材料,被用于油水分离实验,并进行重复使用测试,经过20次循环使用,其表面SEM照片如图11所示,其中,图11中的A部分是实施例1中所制备的疏水多孔陶瓷复合材料使用前的SEM照片,图11中的B部分是实施例1中所制备的疏水多孔陶瓷复合材料经过20次使用后的SEM照片,通过图11中A部分和图11中的B部分可以看出使用前和经过20次使用后的表面形态已经内部孔道结构并没有明显的变化,这说明,该多孔陶瓷材料具有优秀稳定性能,可以重复使用,降低成本。
实施例2
<制备疏水多孔陶瓷复合材料>
将50g粒径为50μm的氧化铝颗粒和质量分数为30%的硅溶胶按质量比为2∶1混合均匀,制备塑形料;
将所得塑形料在直径为3cm的模具中挤压成圆柱型块体,所得圆柱型块体在100℃的烘箱中烘干1h后,在马弗炉内以5℃/min的升温速率升温至1000℃,保温1h进行烧结处理,制备多孔陶瓷材料;
将所制备的多孔陶瓷材料浸泡于50mL质量分数为40%的蔗糖溶液中,抽真空,真空度为-0.08MPa,浸泡处理6h后,在80℃的烘箱中干燥2h,制备碳源负载的多孔陶瓷材料;
将所制备的碳源负载的多孔陶瓷材料在管式炉内,在真空度为-0.09MPa的真空中,以5℃/min的升温速度升温至500℃,保温2h进行热处理,制备疏水多孔陶瓷复合材料。
<性能测试>
实施例2制备的疏水多孔陶瓷复合材料的孔隙率为18.5%。
实施例2所制备的疏水多孔陶瓷复合材料与水的接触角θ如图5所示,约为120.2°,说明实施例2制备的疏水多孔陶瓷复合材料的疏水性良好。
实施例3
<制备疏水多孔陶瓷复合材料>
将50g粒径为100μm的熔融石英砂颗粒和质量分数为20%的硅溶胶按质量比为2∶1混合均匀,制备塑形料;
将所得塑形料在直径为3cm的模具中挤压成圆柱型块体,所得圆柱型块体在100℃的烘箱中烘干1h后,在马弗炉内以5℃/min的升温速率升温至800℃,保温1h进行烧结处理,制备多孔陶瓷材料;
将所制备的多孔陶瓷材料浸泡于50mL质量分数为30%的淀粉溶液中,抽真空,真空度为-0.05MPa,浸泡处理5h后,在80℃的烘箱中干燥2h,制备碳源负载的多孔陶瓷材料;
将所制备的碳源负载的多孔陶瓷材料在管式炉内,在真空度为-0.08MPa的真空中,以5℃/min的升温速率升温至500℃,保温2h进行热处理,制备疏水多孔陶瓷复合材料。
<性能测试>
实施例3制备的疏水多孔陶瓷复合材料的孔隙率为23.7%。
实施例3所制备的疏水多孔陶瓷复合材料与水的接触角θ如图6所示,约为118.2°,说明实施例3制备的疏水多孔陶瓷复合材料的疏水性良好。
实施例4
<制备疏水多孔陶瓷复合材料>
将50g粒径为20μm的氧化钛颗粒和质量分数为30%的硅酸钠溶液按质量比为2∶1混合均匀,制备塑形料;
将所得塑形料在直径为3cm的模具中挤压成圆柱型块体,所得圆柱型块体在100℃的烘箱中烘干1h后,在马弗炉内以5℃/min的升温速率升温至1000℃,保温1h进行烧结处理,制备多孔陶瓷材料;
将所制备的多孔陶瓷材料浸泡于50mL质量分数为40%的聚乙烯纤维素溶液中,抽真空,真空度为-0.06MPa,浸泡处理12h后,在80℃的烘箱中干燥2h,制备碳源负载的多孔陶瓷材料;
将所制备的碳源负载的多孔陶瓷材料在管式炉内,在真空度为-0.08MPa的真空中,以5℃/min的升温速率升温至500℃,保温2h进行热处理,制备疏水多孔陶瓷复合材料。
<性能测试>
实施例4制备的疏水多孔陶瓷复合材料的孔隙率为11.9%。
实施例4所制备的疏水多孔陶瓷复合材料与水的接触角θ如图7所示,约为129.8°,说明实施例4制备的疏水多孔陶瓷复合材料的疏水性良好。
实施例5
<制备疏水多孔陶瓷复合材料>
将50g粒径为20μm的碳化硅颗粒和质量分数为30%的硅溶胶溶液按质量比为3∶1混合均匀,制备塑形料;
将所得塑形料在直径为3cm的模具中挤压成圆柱型块体,所得圆柱型块体在100℃的烘箱中烘干1h后,在马弗炉内以5℃/min的升温速率升温至1000℃,保温1h进行烧结处理,制备多孔陶瓷材料;
将所制备的多孔陶瓷材料浸泡于50mL质量分数为40%的聚乙烯纤维素溶液中,抽真空,真空度为-0.08MPa,浸泡处理24h后,在80℃的烘箱中干燥2h,制备碳源负载的多孔陶瓷材料;
将所制备的碳源负载的多孔陶瓷材料在管式炉内,在真空度为-0.05MPa的真空中,以5℃/min的升温速率升温至500℃,保温2h进行热处理,制备疏水多孔陶瓷复合材料。
<性能测试>
实施例5制备的疏水多孔陶瓷复合材料的孔隙率为14.2%。
实施例5所制备的疏水多孔陶瓷复合材料与水的接触角θ如图8所示,约为128.6°,说明实施例5制备的疏水多孔陶瓷复合材料的疏水性良好。
实施例6
<制备疏水多孔陶瓷复合材料>
将50g粒径为50μm的氮化硅颗粒和质量分数为30%的硅溶胶溶液按质量比为4∶1混合均匀,制备塑形料;
将所得塑形料在直径为3cm的模具中挤压成圆柱型块体,所得圆柱型块体在100℃的烘箱中烘干1h后,在马弗炉内以5℃/min升温速率升温至900℃,保温1h进行烧结处理,制备多孔陶瓷材料;
将所制备的多孔陶瓷材料浸泡于50mL质量分数为40%的蔗糖溶液中,抽真空,真空度为-0.08MPa,浸泡处理12h后,在80℃的烘箱中干燥2h,制备碳源负载的多孔陶瓷材料;
将所制备的碳源负载的多孔陶瓷材料在管式炉内,在真空度为-0.05MPa的真空中,以5℃/min的升温速率升温至500℃,保温2h进行热处理,制备疏水多孔陶瓷复合材料。
<性能测试>
实施例6制备的疏水多孔陶瓷复合材料的孔隙率为20.8%。
实施例6所制备的疏水多孔陶瓷复合材料与水的接触角θ如图9所示,约为122°,说明实施例6制备的疏水多孔陶瓷复合材料的疏水性良好。
实施例7
<制备疏水多孔陶瓷复合材料>
将50g粒径为50μm的氮化硅颗粒和质量分数为20%的硅酸钠溶液按质量比为2∶1混合均匀,制备塑形料;
将所得塑形料在直径为3cm的模具中挤压成圆柱型块体,所得圆柱型块体在100℃的烘箱中烘干1h后,在马弗炉内以5℃/min的升温速率升温至800℃,保温1h进行烧结处理,制备多孔陶瓷材料;
将所制备的多孔陶瓷材料浸泡于50mL质量分数为40%的聚乙二醇溶液中,抽真空,真空度为-0.05MPa,浸泡处理12h后,在80℃的烘箱中干燥2h,制备碳源负载的多孔陶瓷材料;
将所制备的碳源负载的多孔陶瓷材料在管式炉内,在真空度为-0.08MPa的真空中,以5℃/min的升温速率升温至500℃,保温2h进行热处理,制备疏水多孔陶瓷复合材料。
<性能测试>
实施例7制备的疏水多孔陶瓷复合材料的孔隙率为17.3%。
实施例7所制备的疏水多孔陶瓷复合材料与水的接触角θ如图10所示,约为121.6°,说明实施例7制备的疏水多孔陶瓷复合材料的疏水性良好。
本申请提供的疏水多孔陶瓷复合材料中的多孔陶瓷材料的表面粗糙度高,碳源在高温热处理的过程中生成的碳活性高,能够与多孔陶瓷材料紧密地结合,进而使得碳在多孔陶瓷材料的表面及内部的结合牢固,能够长久稳定地保持优异的疏水性能,并且机械强度高,耐摩擦,可以多次重复利用。
需要说明的是,在本文中,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。
以上所述仅为本申请的较佳实施例,并非用于限定本申请的保护范围。凡在本申请的精神和原则之内所作的任何修改、等同替换、改进等,均包含在本申请的保护范围内。
Claims (10)
1.一种疏水多孔陶瓷复合材料的制备方法,其特征在于,包括:
将陶瓷原料和粘结剂混合,制备塑形料;
将所述塑形料挤压成块状后,进行烘干、烧结处理,制备多孔陶瓷材料;
将所述多孔陶瓷材料在含有碳源的溶液中进行浸泡处理后,干燥,制备碳源负载的多孔陶瓷材料;
将所述碳源负载的多孔陶瓷材料热处理,制备疏水多孔陶瓷复合材料;
其中,所述陶瓷原料包括氧化铝、熔融石英砂、氧化钛、氮化硅、碳化硅中的至少一种,所述粘结剂包括硅溶胶、水玻璃中的至少一种,所述碳源包括蔗糖、淀粉、羟乙基纤维素、聚乙二醇中的至少一种。
2.根据权利要求1所述的制备方法,其特征在于,
所述疏水多孔陶瓷复合材料的孔隙率为10~30%。
3.根据权利要求1所述的制备方法,其特征在于,
所述塑形料中陶瓷原料和粘结剂的质量比为4∶1~2∶1;
所述含有碳源的溶液中碳源的质量分数为10~40%。
4.根据权利要求1所述的制备方法,其特征在于,
所述硅溶胶中二氧化硅的质量分数为20~30%;
所述水玻璃中硅酸钠的质量分数为20~30%。
5.根据权利要求1所述的制备方法,其特征在于,
所述烘干的温度为80~100℃、时间为1~3h。
6.根据权利要求1所述的制备方法,其特征在于,
所述烧结处理的升温速率为3~15℃/min、烧结温度为800~1200℃、保温时间为1~3h。
7.根据权利要求1所述的制备方法,其特征在于,
所述浸泡处理的真空度为-0.05~-0.1MPa、时间为6~24h;
所述干燥的温度为80~120℃、时间为0.5~2h。
8.根据权利要求1所述的制备方法,其特征在于,
所述热处理的真空度为-0.05~-0.1MPa、温度为400~550℃、时间为1~3h;
所述陶瓷原料的颗粒粒径为20~100μm。
9.一种根据权利要求1~8任一项所述的制备方法得到的疏水多孔陶瓷复合材料。
10.权利要求9所述的疏水多孔陶瓷复合材料在油水分离方面的应用。
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JP2005263531A (ja) * | 2004-03-17 | 2005-09-29 | Dainatsukusu:Kk | カーボンの疎水化熱処理方法 |
CN1901989A (zh) * | 2003-12-31 | 2007-01-24 | 康宁股份有限公司 | 具有疏水涂层的陶瓷结构 |
CN107555963A (zh) * | 2016-06-30 | 2018-01-09 | 南京理工大学 | 一种超疏水陶瓷的制备方法 |
CN113795472A (zh) * | 2019-01-12 | 2021-12-14 | 纽约州立大学研究基金会 | 陶瓷泡沫、其制造方法及其用途 |
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CN1901989A (zh) * | 2003-12-31 | 2007-01-24 | 康宁股份有限公司 | 具有疏水涂层的陶瓷结构 |
JP2005263531A (ja) * | 2004-03-17 | 2005-09-29 | Dainatsukusu:Kk | カーボンの疎水化熱処理方法 |
CN107555963A (zh) * | 2016-06-30 | 2018-01-09 | 南京理工大学 | 一种超疏水陶瓷的制备方法 |
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