CN109081688A - 一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法 - Google Patents
一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法 Download PDFInfo
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- CN109081688A CN109081688A CN201810981934.6A CN201810981934A CN109081688A CN 109081688 A CN109081688 A CN 109081688A CN 201810981934 A CN201810981934 A CN 201810981934A CN 109081688 A CN109081688 A CN 109081688A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 58
- 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 title claims abstract description 35
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 35
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 45
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 102000035118 modified proteins Human genes 0.000 claims abstract description 13
- 108091005573 modified proteins Proteins 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 8
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 235000019241 carbon black Nutrition 0.000 claims description 7
- 239000006229 carbon black Substances 0.000 claims description 7
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- 239000010433 feldspar Substances 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- 235000012222 talc Nutrition 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 7
- 238000005452 bending Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011022 opal Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000454 talc Substances 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000010811 mineral waste Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
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Abstract
本发明涉及一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，包括以下步骤：（1）按照改性蛋白土、氢氧化铝、ρ‑氧化铝、氧化铝纤维和烧结助剂重量比为3:4:0.9:0.1:0.1将原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；（2）将粉料加水，配制成固含量为55%的陶瓷浆料；（3）将把制备好的陶瓷浆料迅速倒入一定形状的模具中浇铸成型，并真空脱气，除去浆料中的气泡，然后把样品置于在室温下干燥48h后得到陶瓷生坯；（4）将陶瓷生坯烧结，冷却，即得莫来石多孔陶瓷。本发明的莫来石陶瓷制备工艺简单、工艺易于控制、制备过程污染小和生产成本低的特点；所制备的莫来石多孔陶瓷强度高、开气孔率高。
Description
技术领域
本发明涉及一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，属于无机陶瓷材料领域。
背景技术
由于具有良好的化学稳定性、较高的常温和高温强度、优异的耐热冲击性和良好的流体透过性能，莫来石多孔陶瓷在热气过滤、熔融金属过滤、催化剂载体和热绝缘等领域表现出广阔的应用前景。不同铝质原料对形成的针状莫来石的微观结构、相组成和性能有着重要影响。江东亮等人(中国专利，专利公开号CN101037345)以白炭黑和氧化铝为主要原料，采用凝胶冷冻干燥法制备莫来石多孔陶瓷。袁磊等人(中国专利，专利公开号CN103833400)以含氧化铝和二氧化硅的矿物或固体废弃物，工业氧化铝为原料，外加淀粉和铵盐作为造孔剂在1400～1600℃烧结，制备得到自生纤维增强的莫来石多孔陶瓷。王慧等人(中国专利，专利公开号CN101012767)以磷酸、氢氧化铝和莫来石纤维为原料采用湿法成型，于1000～1300℃烧结得到高孔隙率的莫来石纤维多孔陶瓷。但是普遍存在莫来石多孔陶瓷空隙率与强度的矛盾，空隙率高，强度低。
发明内容
本发明提供了一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，解决了现有莫来石多孔陶瓷空隙率与强度的矛盾，空隙率高，强度低的问题。
为解决上述技术问题，本发明采用的技术方案为：
一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土、氢氧化铝、ρ-氧化铝、氧化铝纤维和烧结助剂重量比为3:4:0.9:0.1:0.1，将原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)将均匀粉料与水混合，配制成固含量为55％的陶瓷浆料；
(3)将把制备好的陶瓷浆料迅速倒入一定形状的模具中浇铸成型，并真空脱气，除去浆料中的气泡，然后把样品置于在室温下干燥48h后得到陶瓷生坯；
(4)将陶瓷生坯烧结，冷却，即得莫来石多孔陶瓷。
进一步，本发明的一种优选方案：所述的烧结助剂，按照重量份计，包括30-40份生滑石、50-60份长石、1份氧化铈、3-5份白炭黑。
进一步，本发明的一种优选方案：所述的改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
进一步，本发明的一种优选方案：所述的烧结为：以1℃/min的速率缓慢升温至300℃，然后以2℃/min，升温至800℃，5℃/min升至1500℃保温4小时烧结，然后随炉冷却。
本发明的有益效果：
蛋白土又称蛋白石，是一种含水非晶质或胶质的活性二氧化硅，是一种无定形硅质矿物。其化学组成为SiO2.nH2O，其中所Si为无定形结构，主要成份除Si外还含少量氧化铁、氧化铝、锰、铜和有机杂质等。蛋白石岩是由极微小的蛋白石球体组成，有较发育的孔隙，具有孔隙度高，吸水性强，吸附性好等特点。经过改性处理，SiO2含量由79％升至90％，且空隙率大幅提高。采用蛋白土作为主料，作为造孔剂，可以有效的提高莫来石陶瓷的空隙率，降低粘结剂的用量，进而提高产品的强度。
本发明中通过添加烧结助剂，烧结助剂优选生滑石、长石、氧化铈和白炭黑，可以有效的提高莫来石陶瓷的强度。
ρ-氧化铝是一种具有特殊晶型的氧化铝，也叫水硬性氧化铝，这种氧化铝与其它相氧化铝所不同的是，能够吸收水份重新水化转变成拜耳石或一水软铝石。这是一个强烈的放热反应。在反应后，粉状物或浆料可以变成坚硬的块状物，因此可以利用ρ-氧化铝对陶瓷浆料进行固化成型。采用ρ-氧化铝作为胶黏剂，并提供铝源，实验过程中不需要加入有机物，不需要缓慢的排胶过程，是一种低能耗、绿色环保的方法。
氧化铝纤维是一种高性能无机纤维，具有长纤、短纤、晶须等多种形式。氧化铝纤维直径10-20μm，密度2.7-4.2g/cm3，强度1.4-2.45GPa，模量190-385GPa，最高使用温度为1100-1400℃。高强度、高模量、极好的耐热性和耐高温氧化性是氧化铝纤维的突出优点。另外氧化铝纤维还拥有热膨胀系数低，抗热震性好，热导率小等优点。与其他纤维相比，氧化铝纤维可以在更高的高温下保持抗拉强度。氧化铝纤维表面活性好，容易与陶瓷基体相匹配。
采用氧化铝纤维与蛋白土复合，一方面可以有效的提高莫来石陶瓷的折弯强度，另一方面可以提高气孔率。
本发明的莫来石陶瓷制备工艺简单、工艺易于控制、制备过程污染小和生产成本低的特点；所制备的莫来石多孔陶瓷强度高、开气孔率高。
具体实施方式
下面将结合本发明实施例，对本发明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发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土、氢氧化铝、ρ-氧化铝、氧化铝纤维和烧结助剂重量比为3:4:0.9:0.1:0.1，将原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)将均匀粉料与水混合，配制成固含量为55％的陶瓷浆料；
(3)将把制备好的陶瓷浆料迅速倒入一定形状的模具中浇铸成型，并真空脱气，除去浆料中的气泡，然后把样品置于在室温下干燥48h后得到陶瓷生坯；
(4)将陶瓷生坯烧结，冷却，以1℃/min的速率缓慢升温至300℃，然后以2℃/min，升温至800℃，5℃/min升至1500℃保温4小时烧结，然后随炉冷却，即得莫来石多孔陶瓷。
烧结助剂，按照重量份计，包括30份生滑石、60份长石、1份氧化铈、5份白炭黑。
改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
实施例2
一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土、氢氧化铝、ρ-氧化铝、氧化铝纤维和烧结助剂重量比为3:4:0.9:0.1:0.1，将原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)将均匀粉料与水混合，配制成固含量为55％的陶瓷浆料；
(3)将把制备好的陶瓷浆料迅速倒入一定形状的模具中浇铸成型，并真空脱气，除去浆料中的气泡，然后把样品置于在室温下干燥48h后得到陶瓷生坯；
(4)将陶瓷生坯烧结，冷却，以1℃/min的速率缓慢升温至300℃，然后以2℃/min，升温至800℃，5℃/min升至1500℃保温4小时烧结，然后随炉冷却，即得莫来石多孔陶瓷。
烧结助剂，按照重量份计，包括35份生滑石、55份长石、1份氧化铈、4份白炭黑。
改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
实施例3
一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土、氢氧化铝、ρ-氧化铝、氧化铝纤维和烧结助剂重量比为3:4:0.9:0.1:0.1，将原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)将均匀粉料与水混合，配制成固含量为55％的陶瓷浆料；
(3)将把制备好的陶瓷浆料迅速倒入一定形状的模具中浇铸成型，并真空脱气，除去浆料中的气泡，然后把样品置于在室温下干燥48h后得到陶瓷生坯；
(4)将陶瓷生坯烧结，冷却，以1℃/min的速率缓慢升温至300℃，然后以2℃/min，升温至800℃，5℃/min升至1500℃保温4小时烧结，然后随炉冷却，即得莫来石多孔陶瓷。
烧结助剂，按照重量份计，包括40份生滑石、50份长石、1份氧化铈、3份白炭黑。
改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
对比例1
与实施例1基本相同，不同点在于：不使用烧结助剂，原料采用按照改性蛋白土、氢氧化铝、ρ-氧化铝、氧化铝纤维重量比为3:4:1:0.1。
对比例2
与实施例1基本相同，不同点在于：不使用氧化铝纤维，原料采用按照改性蛋白土、氢氧化铝、ρ-氧化铝、烧结助剂重量比为3:4:1:0.1。
测定实施例1-3和对比例1和2的性能，具体见下表。
| 开气孔率/％ | 抗弯强度/(MPa) | |
| 实施例1 | 76.6 | 54.2 |
| 实施例2 | 75.8 | 53.8 |
| 实施例3 | 76.2 | 53.6 |
| 对比例1 | 76.4 | 41.6 |
| 对比例2 | 82.2 | 47.3 |
注：折弯强度测试样为50mm×7mm×6mm的矩形条。
由上表可知，本发明的莫来石多孔陶瓷开气孔率高、抗弯强度高，相比不添加了烧结助剂的对比例1，抗弯强度提高了30％，相比不添加氧化铝纤维的抗弯强度提高了15％。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，其特征在于，包括以下步骤：
（1）按照改性蛋白土、氢氧化铝、ρ-氧化铝、氧化铝纤维和烧结助剂重量比为3:4:0.9:0.1:0.1，将原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
（2）将粉料加水，配制成固含量为55%的陶瓷浆料；
（3）将把制备好的陶瓷浆料迅速倒入一定形状的模具中浇铸成型，并真空脱气，除去浆料中的气泡，然后把样品置于在室温下干燥48h后得到陶瓷生坯；
（4）将陶瓷生坯烧结，冷却，即得莫来石多孔陶瓷。
2.根据权利要求1所述的一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，其特征在于：所述的烧结助剂，按照重量份计，包括30-40份生滑石、50-60份长石、1份氧化铈、3-5份白炭黑。
3.根据权利要求1所述的一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，其特征在于：
所述的改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为 3∶1加入浓度为 40%硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
4.根据权利要求1所述的一种氧化铝纤维增强蛋白土制备莫来石多孔陶瓷的方法，其特征在于：所述的烧结为：以1℃/min 的速率缓慢升温至 300℃，然后以2℃/min，升温至800℃， 5℃ /min升至 1500℃保温4小时烧结，然后随炉冷却。
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