CN112919892B - 一种无机陶瓷膜支撑体材料及其制备方法 - Google Patents
一种无机陶瓷膜支撑体材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 239000012528 membrane Substances 0.000 title claims abstract description 50
- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 57
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000012798 spherical particle Substances 0.000 claims abstract description 42
- 239000002245 particle Substances 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 29
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- 239000002994 raw material Substances 0.000 claims abstract description 28
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010881 fly ash Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims description 28
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 16
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 13
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 11
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 11
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 4
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开了一种无机陶瓷膜支撑体材料及其制备方法，预先将木炭粉在成球仪中形成球核，喷洒PVA溶液，加入混合均匀的粉料，得到具有球形外观的莫来石前驱体假性球形颗粒，烧制后成为疏松多孔的莫来石纤维原位形成的类球状外形颗粒，再以该材料为原料并添加粉煤灰、粘结剂，经搅拌、陈腐后，挤制成型并烧制得到。本发明创新地制备出了一类具有开口气孔的莫来石纤维原位形成的类球状外形颗粒，并将其应用在无机陶瓷膜中作为支撑体材料，极大地改善支撑体材料的渗水性能，有望替代商品化的陶瓷膜支撑体材料为密闭的球状氧化铝颗粒的现状，且利用沙漠黄砂制备陶瓷材料对环境的保护起到了促进作用，有效地节约了资源，具有较大的经济和社会价值。
Description
技术领域
本发明涉及无机陶瓷膜支撑体材料技术领域，具体地说，是一种无机陶瓷膜支撑体材料及其制备方法。
背景技术
多孔陶瓷膜是一种具有梯度孔结构的多孔陶瓷材料，通常是由孔径和厚度均逐渐减小的支撑体、过渡层和起分离作用的顶层膜组成。作为支撑体，除了要为顶层膜提供必要的机械强度外，还必须具有优异的渗透性能和耐酸碱腐蚀性能。目前商品化的陶瓷膜支撑体材料多采用高纯的Al2O3为原料在高于1700℃烧制而成，其显微结构为具有球形颗粒的封闭式Al2O3球，强度较高，但渗透性能还有待于进一步改善，该类商品化的支撑体过高的烧成温度以及高纯原料正是造成目前陶瓷膜高成本的主要原因之一。因此，作为膜载体的支撑体材料在可保证其理化性能的同时必须从降低能耗、节约成本、大幅度降低高纯原料的资源消耗、绿色环保的角度出发进行加以改良。莫来石(Mullite)材料因其具有低的热膨胀系数、高的耐磨特性、抗化学腐蚀性强、在低温和高温环境强度大等一系列优异性能，有着极大的应用前景。
发明内容
本发明的目的是提供一种用低品位原料沙漠黄砂、固体废弃物粉煤灰和工业原料氢氧化铝制备具有开口气孔的莫来石纤维原位形成的类球状外形颗粒，并将其应用在无机陶瓷膜作为支撑体材料，从而替换商品化的密闭氧化铝实心球支撑体材料，提高渗水通量，加快过滤效率。
本发明的第一个目的，提供一种无机陶瓷膜支撑体材料。
本发明的第二个目的，提供一种无机陶瓷膜支撑体材料的制备方法。
为实现上述第一个目的，本发明采取的技术方案是：
一种无机陶瓷膜支撑体材料，采用成球仪预先以木炭粉制备球核，在球核上喷洒PVA溶液，再以球核粘附莫来石前驱体粉料，得到假性莫来石球形颗粒前驱体，所述莫来石前驱体粉料由沙漠黄砂、氢氧化铝、五氧化二钒和氟化铝组成；将假性莫来石球形颗粒前驱体平铺于耐热板进行烧制；将烧制后得到的莫来石球形颗粒通过筛分出不同级别的大小颗粒；选用不同大小级配组的莫来石球形颗粒，添加粉煤灰，添加PVA粘结剂后经搅拌、陈腐后采用挤制成型得到支撑体材料坯体，并于1100℃烧制而成。
在上述无机陶瓷膜支撑体材料中，优选的，所述莫来石前驱体粉料组成如下：沙漠黄砂35～65份、氢氧化铝65～35份、五氧化二钒4份，氟化铝3份。
在上述无机陶瓷膜支撑体材料中，优选的，所得的假性莫来石球形颗粒前驱体，经筛选其类球状的颗粒粒径控制在600μm以内。
在上述无机陶瓷膜支撑体材料中，优选的，所述假性莫来石球形颗粒前驱体平铺于耐热板进行烧制，其中烧成制度为：室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制。
在上述无机陶瓷膜支撑体材料中，优选的，经烧制后的莫来石球形颗粒通过筛分出不同级别的大小颗粒，分别为50～200μm、200～400μm、400～600μm。
在上述无机陶瓷膜支撑体材料中，优选的，选用不同大小级配组的莫来石球形颗粒，按照小球：中球：大球＝3:5:2颗粒级配，外加15wt％的粉煤灰，添加PVA粘结剂后经搅拌、陈腐后采用挤制成型得到支撑体材料坯体，并于1100℃保温30分钟烧制而成。
在上述无机陶瓷膜支撑体材料中，优选的，所述PVA溶液的浓度为5％。
在上述无机陶瓷膜支撑体材料中，优选的，所制备的无机膜陶瓷支撑体材料渗水通量为14.8～19.2t/m2.h(0.1MPa)。
为实现上述第二个目的，本发明采取的技术方案是：
一种无机陶瓷膜支撑体材料的制备方法，包括如下步骤：
(1)木炭粉置于成球仪中，并喷洒PVA溶液，启动成球仪得到不同粒径的木炭粉球核；
(2)按照重量份取原料：沙漠黄砂35～65份、氢氧化铝65～35份、五氧化二钒4份，氟化铝3份，将上述原料充分的混合均匀；
(3)将1)中所制得的球核置于盘中，喷洒PVA溶液，并不断搅拌，将2)中均匀混合的粉体加入盘中并不断搅拌，获得假性莫来石球形颗粒前驱体；
(4)将3)中制得的假性莫来石球形颗粒前驱体经室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制；
(5)将4)中烧制后获得的莫来石球形颗粒进行筛分，颗粒大小级配分别为小球50～200μm、中球200～400μm、大球400～600μm；
(6)按照重量比小球：中球：大球＝3:5:2，并外加15wt％的粉煤灰，添加PVA粘结剂后经搅拌、陈腐后采用挤制成型无机陶瓷膜支撑体材料坯体，并于1100℃保温30分钟进行烧制。
本发明选择来源广泛的低品位原料沙漠黄砂，固体废弃物粉煤灰、工业原料氢氧化铝作为合成莫来石支撑体材料的原料，通过首先预制成型木炭粉球核，再将混合均匀的莫来石前驱体粉料加入，通过粘附后形成为假性的莫来石球形颗粒前驱体，经煅烧后，添加固体废弃物粉煤灰，经挤制成型烧制可得到颗粒疏松多孔、颗粒间充满间隙的一类特殊微结构的支撑体材料，从而大大地提高渗水通量，加快过滤，缩短分离的时间。一方面可以利用固体废弃物与低品位原料替代日益枯竭的高岭、瓷石类自然资源，降低原材料的生产成本；另一方面提高了固体废弃物与低品位原料的高附加值，同时对环境起到了一定的保护作用。固体废弃物原料因其来源广泛，价格低廉，利用其原位合成具有开口气孔的莫来石纤维形成的类球状外形颗粒，并将其应用在无机陶瓷膜作为支撑体材料，实现了固废原料充分利用的理念。
本发明创新地制备出了一类具有开口气孔的莫来石纤维原位形成的类球状外形颗粒，并将其应用在无机陶瓷膜作为支撑体材料的制备方法，极大地改善支撑体材料的渗水性能，从而有望替代商品化的陶瓷膜支撑体材料为密闭的球状氧化铝颗粒的现状，而且利用沙漠黄砂制备陶瓷材料，不仅可以替代正日益枯竭的高岭土类瓷质原料，还对环境的保护起到了促进作用，有效地节约了资源，具有较大的经济和社会价值。
附图说明
附图1是本发明实施例2所制支撑体材料的扫描电镜照片。
具体实施方式
下面结合具体实施方式，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明记载的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1具有开口气孔的莫来石纤维原位形成的类球状外形颗粒无机陶瓷膜材料
(1)将50g的木炭粉置于成球仪中，并喷洒浓度为5％PVA溶液10ml，启动成球仪得到不同粒径的木炭粉球核；
(2)按照重量份取原料：沙漠黄砂35份、氢氧化铝65份、五氧化二钒4份、氟化铝3份，将上述原料充分的混合均匀；
(3)将1中所制得的球核20g置于盘中，喷洒浓度为5％的PVA溶液4ml，并不断搅拌，紧接着将2中均匀混合的粉体20g加入盘中并不断搅拌，获得莫来石前驱体假性球形颗粒；
(4)将3中制得的假性球形颗粒经室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制；
(5)将4中烧制后的类球状莫来石颗粒进行筛分，得到颗粒大小级配分别为小球50～200μm、中球200～400μm、大球400～600μm；
(6)取5中制备的球形颗粒，按照重量比小球：中球：大球＝3:5:2称取10g，并外加15wt％的粉煤灰，添加浓度为5％的PVA粘结剂1ml后经搅拌、陈腐后采用挤制成型无机陶瓷膜支撑体材料坯体，并于1100℃保温30分钟进行烧制。
实施例2具有开口气孔的莫来石纤维原位形成的类球状外形颗粒无机陶瓷膜材料
(1)将50g的木炭粉置于成球仪中，并喷洒浓度为5％PVA溶液10ml，启动成球仪得到不同粒径的木炭粉球核；
(2)按照重量份取原料：沙漠黄砂45份、氢氧化铝55份、五氧化二钒4份、氟化铝3份，将上述原料充分的混合均匀；
(3)将1中所制得的球核20g置于盘中，喷洒浓度为5％的PVA溶液4ml，并不断搅拌，紧接着将2中均匀混合的粉体20g加入盘中并不断搅拌，获得莫来石前驱体假性球形颗粒；
(4)将3中制得的假性球形颗粒经室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制；
(5)将4中烧制后的类球状莫来石颗粒进行筛分，得到颗粒大小级配分别为小球50～200μm、中球200～400μm、大球400～600μm；
(6)取5中制备的球形颗粒，按照重量比小球：中球：大球＝3:5:2称取10g，并外加15wt％的粉煤灰，添加浓度为5％的PVA粘结剂1ml后经搅拌、陈腐后采用挤制成型无机陶瓷膜支撑体材料坯体，并于1100℃保温30分钟进行烧制。
实施例3具有开口气孔的莫来石纤维原位形成的类球状外形颗粒无机陶瓷膜材料
(1)将50g的木炭粉置于成球仪中，并喷洒浓度为5％PVA溶液10ml，启动成球仪得到不同粒径的木炭粉球核；
(2)按照重量份取原料：沙漠黄砂55份、氢氧化铝45份、五氧化二钒4份、氟化铝3份，将上述原料充分的混合均匀；
(3)将1中所制得的球核20g置于盘中，喷洒浓度为5％的PVA溶液4ml，并不断搅拌，紧接着将2中均匀混合的粉体20g加入盘中并不断搅拌，获得莫来石前驱体假性球形颗粒；
(4)将3中制得的假性球形颗粒经室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制；
(5)将4中烧制后的类球状莫来石颗粒进行筛分，得到颗粒大小级配分别为小球50～200μm、中球200～400μm、大球400～600μm；
(6)取5中制备的球形颗粒，按照重量比小球：中球：大球＝3:5:2称取10g，并外加15wt％的粉煤灰，添加浓度为5％的PVA粘结剂1ml后经搅拌、陈腐后采用挤制成型无机陶瓷膜支撑体材料坯体，并于1100℃保温30分钟进行烧制。
实施例4具有开口气孔的莫来石纤维原位形成的类球状外形颗粒无机陶瓷膜材料
(1)将50g的木炭粉置于成球仪中，并喷洒浓度为5％PVA溶液10ml，启动成球仪得到不同粒径的木炭粉球核；
(2)按照重量份取原料：沙漠黄砂65份、氢氧化铝35份、五氧化二钒4份、氟化铝3份，将上述原料充分的混合均匀；
(3)将1中所制得的球核20g置于盘中，喷洒浓度为5％的PVA溶液4ml，并不断搅拌，紧接着将2中均匀混合的粉体20g加入盘中并不断搅拌，获得莫来石前驱体假性球形颗粒；
(4)将3中制得的假性球形颗粒经室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制；
(5)将4中烧制后的类球状莫来石颗粒进行筛分，得到颗粒大小级配分别为小球50～200μm、中球200～400μm、大球400～600μm；
(6)取5中制备的球形颗粒，按照重量比小球：中球：大球＝3:5:2称取10g，并外加15wt％的粉煤灰，添加浓度为5％的PVA粘结剂1ml后经搅拌、陈腐后采用挤制成型无机陶瓷膜支撑体材料坯体，并于1100℃保温30分钟进行烧制。
对比例1作为对比例，以原位形成的莫来石应用在无机陶瓷膜作为支撑体材料的制备
(1)按照重量份取原料：沙漠黄砂45份、氢氧化铝55份、五氧化二钒4份、氟化铝3份，将上述原料充分的混合均匀，并营造颗粒获得莫来石前驱体；
(2)取步骤1中的颗粒10g外加15wt％的粉煤灰，喷洒添加浓度为5％的PVA粘结剂1ml后经搅拌、陈腐后采用挤制成型得到无机陶瓷膜支撑体材料坯体；
(3)将步骤2中的无机陶瓷膜支撑体材料坯体于1200～1350℃、保温2小时烧制。
对比例2作为对比例，选用氧化铝球应用在无机陶瓷膜作为支撑体材料的制备
(1)选用的α-Al2O3来自白鸽集团，按照细颗粒：中颗粒：粗颗粒＝3:5:2的重量称取10g原料，并添加浓度为5％的PVA粘结剂1ml溶液，经陈腐后通过挤制成型得到支撑体坯体；
(2)将步骤1中的无机陶瓷膜支撑体材料坯体于1700℃、保温2小时烧制。
性能测试：将上述实施例1-实施例4及对比例1-对比例2所制备的支撑体材料进行渗水通量测试，具体测试方法如下：将所检测的支撑体陶瓷材料置于100℃烘箱中保温2小时，运用测试渗水通量设备检测各支撑体陶瓷材料的透水性能，每组检测三个试样，计算其平均值，其中测试压力为0.1MPa，所通气体为N2,所用水为纯水，记录时间为10min。测试结果如表中1所示。
表1
| 组别 | 渗水通量t/m<sup>2</sup>.h(0.1MPa) |
| 实施例1 | 17.8 |
| 实施例2 | 19.2 |
| 实施例3 | 16.4 |
| 实施例4 | 14.8 |
| 对比例1 | 11.4 |
| 对比例2 | 6.5 |
Claims (6)
1.一种无机陶瓷膜支撑体材料，其特征在于：采用成球仪预先以木炭粉制备球核，在球核上喷洒PVA溶液，再以球核粘附莫来石前驱体粉料，得到假性莫来石球形颗粒前驱体，所述莫来石前驱体粉料由沙漠黄砂、氢氧化铝、五氧化二钒和氟化铝组成；将假性莫来石球形颗粒前驱体平铺于耐热板进行烧制；将烧制后得到的莫来石球形颗粒通过筛分出不同级别的大小颗粒；选用不同大小级配组的莫来石球形颗粒，外加15wt％的粉煤灰，添加PVA粘结剂后经搅拌、陈腐后采用挤制成型得到支撑体材料坯体，并于1100℃烧制而成；所述莫来石前驱体粉料组成如下：沙漠黄砂35～65份、氢氧化铝65～35份、五氧化二钒4份，氟化铝3份；所得的假性莫来石球形颗粒前驱体，经筛选其类球状的颗粒粒径控制在600μm以内；所述假性莫来石球形颗粒前驱体平铺于耐热板进行烧制，其中烧成制度为：室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制。
2.根据权利要求1所述的无机陶瓷膜支撑体材料，其特征在于：经烧制后的莫来石球形颗粒通过筛分出不同级别的大小颗粒，分别为50～200μm、200～400μm、400～600μm。
3.根据权利要求2所述的无机陶瓷膜支撑体材料，其特征在于：选用不同大小级配组的莫来石球形颗粒，按照小球：中球：大球＝3:5:2颗粒级配，外加15wt％的粉煤灰，添加PVA粘结剂后经搅拌、陈腐后采用挤制成型得到支撑体材料坯体，并于1100℃保温30分钟烧制而成。
4.根据权利要求3所述的无机陶瓷膜支撑体材料，其特征在于：所述PVA溶液的浓度为5％。
5.根据权利要求1-4任一所述的无机陶瓷膜支撑体材料，其特征在于：所制备的无机膜陶瓷支撑体材料渗水通量为14.8～19.2t/m2.h，其中测试压力为0.1MPa。
6.一种无机陶瓷膜支撑体材料的制备方法，其特征在于：包括如下步骤：
(1)木炭粉置于成球仪中，并喷洒PVA溶液，启动成球仪得到不同粒径的木炭粉球核；
(2)按照重量份取原料：沙漠黄砂35～65份、氢氧化铝65～35份、五氧化二钒4份，氟化铝3份，将上述原料充分的混合均匀；
(3)将1)中所制得的球核置于盘中，喷洒PVA溶液，并不断搅拌，将2)中均匀混合的粉体加入盘中并不断搅拌，获得假性莫来石球形颗粒前驱体；
(4)将3)中制得的假性莫来石球形颗粒前驱体经室温～400℃采用1℃/min升温，并在最高温保温60min，随后再以5℃/min升至1200～1350℃、保温2小时烧制；
(5)将4)中烧制后获得的莫来石球形颗粒进行筛分，颗粒大小级配分别为小球50～200μm、中球200～400μm、大球400～600μm；
(6)按照重量比小球：中球：大球＝3:5:2，并外加15wt％的粉煤灰，添加PVA粘结剂后经搅拌、陈腐后采用挤制成型无机陶瓷膜支撑体材料坯体，并于1100℃保温30分钟进行烧制。
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