CN114702319A - 一种用于氧化铝纤维膜的超重力气纺方法及应用 - Google Patents
一种用于氧化铝纤维膜的超重力气纺方法及应用 Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 84
- 238000009987 spinning Methods 0.000 title claims abstract description 72
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000012528 membrane Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000000919 ceramic Substances 0.000 claims abstract description 7
- 239000012774 insulation material Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 26
- 239000002243 precursor Substances 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 6
- 229910044991 metal oxide Inorganic materials 0.000 claims description 6
- 150000004706 metal oxides Chemical class 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 2
- 238000001914 filtration Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 6
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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Abstract
本发明提供一种用于氧化铝纤维膜的超重力气纺方法及应用,通过结合离心纺丝法和气纺法技术,利用离心力和气吹双重驱动力模拟超重力的状态,再通过在两种纺丝方式的自由切换与结合,可以制得尺寸跨度从微米级到纳米级的氧化铝纤维,以及结构均匀的氧化铝纤维膜。制备的陶瓷纤维膜其纤维直径在30~40000 nm范围内可以调整,长径比≥100000,1400℃灼烧30分钟无表观灼烧痕迹。作为隔热材料使用时,热导率≤0.02 W/m·K;作为过滤膜材料,在5 cm/s的风速下,PM2.5过滤率≥99.9%。
Description
技术领域
本发明属于纤维制备技术领域,尤其是涉及一种用于氧化铝纤维膜的超重力气纺方法及应用。
背景技术
氧化铝纤维是一种高性能的无机陶瓷纤维,与普通玻璃纤维或碳化硅等无机陶瓷纤维相比,氧化铝纤维具有极好的耐高温氧化性、耐热性和超高强度等特点,其成品的融化温度最高可达2000℃,并且可以在1000℃以上的温度下长时间使用,抗拉强度最高可达2800MPa,模量达到370GPa。可以应用在高温极端工作环境和航天航空领域。
无机陶瓷纤维的制备方法主要包括浸渍法、静电纺丝法、熔融法、溶胶-凝胶法、甩丝法等。其中,溶胶-凝胶法由于反应条件温和、制备成本低、所得制品纯度高等特点,应用更为广泛。利用溶胶-凝胶法制备氧化铝纤维主要包括三个步骤:纺丝前驱体的制备、凝胶纤维的制备和热处理。当纺丝前驱体形成后,即可运用不同的纺丝方式获得凝胶纤维,这些方法主要由干法纺丝、气纺法和离心纺丝法等。干法纺丝是通过储液罐的气体压力和计量泵产生的压力,将纺丝前驱体挤出喷丝板,并在加热甬道中干燥成凝胶纤维。它能够制备连续长纤维,纤维直径均匀,通常只能制得微米级纤维。离心纺丝法是利用高速旋转产生的离心力将溶胶从小孔或狭缝甩出,再在高温氛围中固化成凝胶纤维的一种方法。它具有设备简单、纺丝条件易控制、纤维直径较小等特点。气纺法是以高速气流作为驱动力,溶胶经喷丝孔挤出后在高速气流的驱动下形成射流,收集于接收装置上。它具有生产效率高、纤维直径较小等特点。后两种方法通常用于制备陶瓷纤维膜,虽然能够制得纤维直径较小的氧化铝纤维,但是其尺寸只能达到微米级到亚微米级,相对于纳米纤维其尺寸还是偏大,不适宜用于高端产品的过滤材料和催化剂等载体材料上。
发明内容
本发明第一个目的在于,针对现有技术中存在的不足,提供一种用于氧化铝纤维膜的超重力气纺方法。
为此,本发明的上述目的通过如下技术方案实现:
一种用于氧化铝纤维膜的超重力气纺方法,包括如下步骤:
S1、纺丝前驱体的制备
将氧化铝溶胶与至少一种不同于氧化铝溶胶的其他金属氧化物溶胶混合,并使得两种或多种溶胶混合均匀;加入一定量的纺丝助剂,再次混合均匀;在一定温度下陈化直至粘度为1~3000Pa·s,得到合适的纺丝前驱体;
S2、超重力强化气纺凝胶纤维的制备
将步骤S1制备得到的纺丝前驱体加入超重力强化气纺设备中,在离心力或/和气流的驱动力下,实现前驱体射流的单一/双重牵伸,并在热空气下固化成凝胶纤维;
(3)凝胶纤维膜的热处理
将步骤S2制得凝胶纤维膜进行除水、除聚合物和陶瓷化,最后降温得到氧化铝陶瓷纤维。
在采用上述技术方案的同时,本发明还可以采用或者组合采用如下技术方案:
作为本发明的优选技术方案:步骤S1中,氧化铝溶胶与其他金属氧化物溶胶的质量比为0.99:0.01~0.50:0.50。
作为本发明的优选技术方案:步骤S1中,其他金属氧化物溶胶为:氧化镁、氧化钙、氧化镧、氧化钇、氧化硅、氧化锌、氧化钛、氧化锰、氧化镍或氧化硼中的任意一种或多种。
作为本发明的优选技术方案:步骤S1中,纺丝助剂为聚乙烯吡咯烷酮、聚环氧乙烷、聚氧化乙烯、聚乙烯醇中的任意一种。
作为本发明的优选技术方案:步骤S1中,陈化温度为50~100℃。
作为本发明的优选技术方案:步骤S1中,陈化时间为1~40小时。
作为本发明的优选技术方案:步骤S2中,超重力强化气纺过程控制为:
喷丝板温度为20~60℃,转盘转速为200~12000r/min,气体压力为1~30MPa,气流温度为20~150℃,气流流速为3~600m/min,纺丝环境氛围相对湿度为10%~60%。
作为本发明的优选技术方案:步骤S3中,热处理过程控制为:
以0.1~3℃/min的升温速率从室温升温到500~800℃,在此温度保温1~3小时;再以2~20℃/min的升温速率升温至1200~1600℃,在此温度下保温0.5~5小时,然后降温至室温,得到氧化铝陶瓷纤维。
本发明第二个目的在于,针对现有技术中存在的不足,提供利用前文所述的用于氧化铝纤维膜的超重力气纺方法所制备得到的氧化铝纤维膜作为隔热材料的应用。
本发明还有一个目的在于,针对现有技术中存在的不足,提供利用前文所述的用于氧化铝纤维膜的超重力气纺方法所制备得到的氧化铝纤维膜作为过滤材料的应用。
本发明提供一种用于氧化铝纤维膜的超重力气纺方法及应用,通过结合离心纺丝法和气纺法技术,利用离心力和气吹双重驱动力模拟超重力的状态,再通过在两种纺丝方式的自由切换与结合,可以制得尺寸跨度从微米级到纳米级的氧化铝纤维,以及结构均匀的氧化铝纤维膜。制备的陶瓷纤维膜其纤维直径在30~40000nm范围内可以调整,长径比≥100000,1400℃灼烧30分钟无表观灼烧痕迹。作为隔热材料使用时,热导率≤0.02W/m·K;作为过滤膜材料,在5cm/s的风速下,PM2.5过滤率≥99.9%。
附图说明
图1为实施例1制备的氧化铝陶瓷纤维的扫描电子显微镜图。
图2为实施例1制备氧化铝陶瓷纤维膜在1400℃灼烧30分钟前的照片。
图3为实施例1制备氧化铝陶瓷纤维膜在1400℃灼烧30分钟后的照片。
具体实施方式
参照附图和具体实施例对本发明作进一步详细地描述。
实施例1
将1.2千克氧化铝溶胶溶液中加入0.2千克二氧化硅溶胶溶液,在70摄氏度循环油浴中搅拌均匀。加入500克聚乙烯醇,搅拌均匀后在60摄氏度下浓缩30小时,得到黏度为500Pa·s的纺丝前驱体。
将纺丝前驱体加入到超重力强化气纺设备进行纺丝,其工艺参数为:喷丝板温度为40℃,转盘转速为3000r/min,气体压力为5MPa,气流温度为110℃,气流流速为10m/min,纺丝环境氛围相对湿度为40%。所得凝胶纤维在以3℃/min的升温速率从室温升温到600℃,在此温度保温1小时;再以10℃/min的升温速率升温至1300℃,在此温度下保温1小时,然后降温至室温,得到氧化铝陶瓷纤维。
图1为实施例1制备的氧化铝陶瓷纤维的扫描电子显微镜图,该氧化铝陶瓷纤维表面光滑平整,纤维尺寸均匀,平均直径为550nm,长径比达到300000。实施例1氧化铝陶瓷纤维膜可以用作高温隔热材料,其热导率为0.01W/m·K。
图2、图3分别为实施例1制备氧化铝陶瓷纤维膜在1400℃灼烧30分钟前后的照片,从照片中可以看到氧化铝陶瓷纤维膜经高温灼烧后无明显灼烧痕迹。
实施例2
将1.2千克氧化铝溶胶溶液中加入0.2千克二氧化硅溶胶溶液,在70摄氏度循环油浴中搅拌均匀。加入400克聚乙烯吡咯烷酮,搅拌均匀后在60摄氏度下浓缩30小时,得到黏度为600Pa·s的纺丝前驱体。
将纺丝前驱体加入到超重力强化气纺设备进行纺丝,其工艺参数为:喷丝板温度为40℃,转盘转速为5000r/min,气体压力为10MPa,气流温度为110℃,气流流速为50m/min,纺丝环境氛围相对湿度为40%。所得凝胶纤维在以3℃/min的升温速率从室温升温到600℃,在此温度保温1小时;再以10℃/min的升温速率升温至1300℃,在此温度下保温1小时,然后降温至室温,得到氧化铝陶瓷纤维。
实施例2得到的氧化铝陶瓷纤维表面纤维尺寸均匀,平均直径为360nm,长径比达到600000。实施例2制得氧化铝陶瓷纤维膜可以用作高温过滤材料,当测试风速为5cm/s时,其PM2.5过滤率为99.95%。
实施例3-9
实施例3-9在实施例1的基础上仅改变转盘转速、气流压力、气流速度、气流温度、环境氛围相对湿度,其他步骤或者参数同实施例1,具体如下表1所示:
表1工艺与纤维尺寸的关系
对照实施例1
将1.1千克氧化铝溶胶溶液中加入0.2千克二氧化硅溶胶溶液,在70摄氏度循环油浴中搅拌均匀。加入500克聚乙烯吡咯烷酮,搅拌均匀后在60摄氏度下浓缩30小时,得到黏度为800Pa·s的纺丝前驱体。
将纺丝前驱体加入到超重力强化气纺设备进行纺丝,其工艺参数为:喷丝板温度为40℃,转盘转速为0r/min,气体压力为10MPa,气流温度为100℃,气流流速为10m/min,纺丝环境氛围相对湿度为60%。所得凝胶纤维在以3℃/min的升温速率从室温升温到600℃,在此温度保温1小时;再以10℃/min的升温速率升温至1300℃,在此温度下保温1小时,然后降温至室温,得到氧化铝陶瓷纤维。
对照实施例1得到的氧化铝陶瓷纤维表面纤维尺寸均匀,平均直径为1500nm,长径比达到500。
对照实施例2
将1.2千克氧化铝溶胶溶液中加入0.3千克二氧化硅溶胶溶液,在70摄氏度循环油浴中搅拌均匀。加入500克聚氧化乙烯,搅拌均匀后在60摄氏度下浓缩30小时,得到黏度为550Pa·s的纺丝前驱体。
将纺丝前驱体加入到超重力强化气纺设备进行纺丝,其工艺参数为:喷丝板温度为40℃,转盘转速为3000r/min,不使用气吹,纺丝环境氛围相对湿度为60%。所得凝胶纤维在以3℃/min的升温速率从室温升温到600℃,在此温度保温1小时;再以10℃/min的升温速率升温至1300℃,在此温度下保温1小时,然后降温至室温,得到氧化铝陶瓷纤维。
对照实施例2得到的氧化铝陶瓷纤维表面纤维尺寸均匀,平均直径为2300nm,长径比达到1000。
比较实施例1和实施例2,表明本发明通过改变纺丝工艺参数可以获得纳米级、高长径比氧化铝纤维,并且该纤维膜的热导率低、过滤效率高。比较实施例1、对照实施例1和对照实施例2,可以看出本发明可以通过自由切换与结合离心力和气吹双重驱动力两种纺丝方式,制得尺寸跨度从微米级到纳米级的氧化铝纤维。
上述具体实施方式用来解释说明本发明,仅为本发明的优选实施例,而不是对本发明进行限制,在本发明的精神和权利要求的保护范围内,对本发明做出的任何修改、等同替换、改进等,都落入本发明的保护范围。
Claims (10)
1.一种用于氧化铝纤维膜的超重力气纺方法,其特征在于:所述超重力气纺方法包括如下步骤:
S1、纺丝前驱体的制备
将氧化铝溶胶与至少一种不同于氧化铝溶胶的其他金属氧化物溶胶混合,并使得两种或多种溶胶混合均匀;加入一定量的纺丝助剂,再次混合均匀;在一定温度下陈化直至粘度为1~3000 Pa·s,得到合适的纺丝前驱体;
S2、超重力强化气纺凝胶纤维的制备
将步骤S1制备得到的纺丝前驱体加入超重力强化气纺设备中,在离心力或/和气流的驱动力下,实现前驱体射流的单一/双重牵伸,并在热空气下固化成凝胶纤维;
(3)凝胶纤维膜的热处理
将步骤S2制得凝胶纤维膜进行除水、除聚合物和陶瓷化,最后降温得到氧化铝陶瓷纤维。
2.根据权利要求1所述的用于氧化铝纤维膜的超重力气纺方法,其特征在于:步骤S1中,氧化铝溶胶与其他金属氧化物溶胶的质量比为0.99:0.01~0.50:0.50。
3.根据权利要求1所述的用于氧化铝纤维膜的超重力气纺方法,其特征在于:步骤S1中,其他金属氧化物溶胶为:氧化镁、氧化钙、氧化镧、氧化钇、氧化硅、氧化锌、氧化钛、氧化锰、氧化镍或氧化硼中的任意一种或多种。
4.根据权利要求1所述的用于氧化铝纤维膜的超重力气纺方法,其特征在于:步骤S1中,纺丝助剂为聚乙烯吡咯烷酮、聚环氧乙烷、聚氧化乙烯、聚乙烯醇中的任意一种。
5.根据权利要求1所述的用于氧化铝纤维膜的超重力气纺方法,其特征在于:步骤S1中,陈化温度为50~100℃。
6.根据权利要求1所述的用于氧化铝纤维膜的超重力气纺方法,其特征在于:步骤S1中,陈化时间为1~40小时。
7.根据权利要求1所述的用于氧化铝纤维膜的超重力气纺方法,其特征在于:步骤S2中,超重力强化气纺过程控制为:
喷丝板温度为20~60℃,转盘转速为200~12000 r/min,气体压力为1~30 MPa,气流温度为20~150℃,气流流速为3~600 m/min,纺丝环境氛围相对湿度为10%~60%。
8.根据权利要求1所述的用于氧化铝纤维膜的超重力气纺方法,其特征在于:步骤S3中,热处理过程控制为:
以0.1~3℃/min的升温速率从室温升温到500~800℃,在此温度保温1~3小时;再以2~20℃/min的升温速率升温至1200~1600℃,在此温度下保温0.5~5小时,然后降温至室温,得到氧化铝陶瓷纤维。
9.根据权利要求1-8中任意一项所述的用于氧化铝纤维膜的超重力气纺方法所制备得到的氧化铝纤维膜作为隔热材料的应用。
10.根据权利要求1-8中任意一项所述的用于氧化铝纤维膜的超重力气纺方法所制备得到的氧化铝纤维膜作为过滤材料的应用。
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