活性氧化铝催化剂载体的光固化浆料制备与成型

doi:10.15541/jim20210604

无机材料学报 ›› 2022, Vol. 37 ›› Issue (3): 297-302.DOI: 10.15541/jim20210604

活性氧化铝催化剂载体的光固化浆料制备与成型

周港怀¹, 刘耀²(), 石原¹, 刘绍军¹()

1.中南大学粉末冶金研究院, 长沙 410083
2.萍乡学院机械电子工程学院, 萍乡 330073

收稿日期:2021-09-30 修回日期:2021-10-26 出版日期:2022-03-20 网络出版日期:2021-11-12
通讯作者: 刘耀, 讲师. E-mail: liuyao1985@csu.edu.com; 刘绍军, 教授. E-mail: liumatthew@csu.edu.cn
作者简介:周港怀(1997-), 男, 硕士研究生. E-mail: 193312100@csu.edu.cn
基金资助:
江西省自然科学基金(20212BAB204048);江西省重点研发计划(20213BBE53049)

Slurry Preparation and Stereolithography for Activated Alumina Catalyst Carrier

ZHOU Ganghuai¹, LIU Yao²(), SHI Yuan¹, LIU Shaojun¹()

1. Powder Metallurgy Research Institute, Central South University, Changsha 410083, China
2. College of Mechanical and Electronic Engineering, Pingxiang University, Pingxiang 330073, China

Received:2021-09-30 Revised:2021-10-26 Published:2022-03-20 Online:2021-11-12
Contact: LIU Yao, lecturer. E-mail: liuyao1985@csu.edu.com; LIU Shaojun, professor. E-mail: liumatthew@csu.edu.cn
About author:ZHOU Ganghuai (1997-), male, Master candidate. E-mail: 193312100@csu.edu.cn
Supported by:
Jiangxi Provincal Natural Science Foundation(20212BAB204048);Key Research and Development Program of Jiangxi Province(20213BBE53049)

摘要/Abstract

摘要：

为制备具有高效化学催化反应和复杂精细结构的活性氧化铝催化剂载体, 制备出低粘度、高均匀性和高固相含量的光固化浆料, 通过粒度分析和流变测试等手段, 研究树脂配比和偶联剂改性剂改性活性氧化铝表面对粉末粒度分布和浆料的稳定性、均匀性和流变性的影响。当w(HEA) : w(HDDA) : w(TMPTA) : w(modified-EA)=1.5 : 1.0 : 2.5 : 5.0时, 预混液在剪切速率为1 s^-1时的粘度仅为0.35 Pa·s; 粉末改性后KH560高分子链附着在活性氧化铝表面, 使得活性氧化铝由亲水性改性为疏水性, 提高浆料的均匀性和稳定性, 并使粉末之间产生空间位阻, 降低粉末团聚, 其平均直径从4.43 μm降低至3.89 μm; 采用浸润混合法制备固相含量为52%(质量分数)的浆料并成功打印。脱脂烧结后的活性氧化铝样品保持了复杂异形薄壁结构, 其开孔率和密度分别为51.3%和1.93 g/cm³。

关键词: 光固化成型, 活性氧化铝, 粉末表面改性, 流变性能

Abstract:

In order to prepare activated alumina catalyst carrier with efficient chemical catalytic reaction and complex fine structure, we prepared a low viscosity, high uniformity and high solid content stereolithographic slurry. Effects of resin ratio and coupling agent modification on the particle size distribution of activated alumina and the stability, uniformity and rheological properties of slurry were studied by particle size analysis and rheological test. When w(HEA) : w(HDDA) : w(TMPTA) : w(modified-EA)=1.5 : 1.0 : 2.5 : 5.0, the viscosity of premix at shear rate 1 s ^-1 is only 0.35 Pa·s. After powder modification, KH560 polymer chain attached to surface of activated alumina, changing the activated alumina from hydrophilic to hydrophobic, which improved the uniformity and stability of slurry, caused steric hydration between powders and reduced powder agglomeration, leading the average diameter of activated alumina being decreased from 4.43 μm to 3.89 μm. Slurry with solid content of 52% (in mass) was prepared by wetting mixing method and then successfully printed. Debounded and sintered activated alumina samples maintains a complex irregular thin-walled structure, and their porosity and density are 51.3% and 1.93 g/cm³, respectively.

Key words: stereolithography, activated alumina, powder surface modification, rheological property

中图分类号:

TQ174

周港怀, 刘耀, 石原, 刘绍军. 活性氧化铝催化剂载体的光固化浆料制备与成型[J]. 无机材料学报, 2022, 37(3): 297-302.

ZHOU Ganghuai, LIU Yao, SHI Yuan, LIU Shaojun. Slurry Preparation and Stereolithography for Activated Alumina Catalyst Carrier[J]. Journal of Inorganic Materials, 2022, 37(3): 297-302.

图/表 7

图1 光固化成型机器的三维结构示意图(a)和活性氧化铝打印模型图(b)

Fig. 1 Three-dimensional structure diagram of stereolithographic machine (a) and print model diagram of activated alumina (b)

图2 活性氧化铝粉末的XRD图谱

Fig. 2 XRD pattern of activated alumina

图3 偶联剂改性活性氧化铝机理图

Fig. 3 Mechanic diagram of activated alumina modified by coupling agent

图4 质量分数为2%的KH550、KH560和KH570偶联剂改性后活性氧化铝的粒度分布图(a)和平均颗粒直径图(b)

Fig. 4 Particle size distribution (a) and average particle diameter (b) of activated alumina diagram after 2% (mass percentage) KH550, KH560 and KH570 coupling agent modification

图5 不同活性稀释剂配比树脂粘度曲线

Fig. 5 Viscosity diagrams of resin with different monomer ratios

图6 改性活性氧化铝和树脂不同混合方式的浆料黏度图

Fig. 6 Viscosity diagram of slurry with different mixing methods of modified activated alumina and resin. Inset shows the enlarged curues under shear rate less than 70 s-1

图7 光固化活性氧化铝样品脱脂烧结后样品照片(a)和光固化活性氧化铝脱样品脂烧结后的SEM照片(b)

Fig. 7 Stereolithographic activated alumina sample diagram (a) after debounding and sintering and SEM image (b) of stereolithographic activated alumina sample after debounding and sintering

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活性氧化铝催化剂载体的光固化浆料制备与成型

Slurry Preparation and Stereolithography for Activated Alumina Catalyst Carrier

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