异辛醇铝水解制备高纯拟薄水铝石的研究

doi:10.19964/j.issn.1006-4990.2024-0436

Abstract

Abstract:

The preparation of high-purity pseudo boehmite using aluminum isooctanol as raw material can solve the problems of pipeline blockage and high energy consumption in alcohol water separation caused by the hydrolysis of aluminum isopropoxide in industry.The influence of different hydrolysis conditions on the solubility index and gelation time of pseudo boehmite was studied by changing the hydrolysis temperature，hydrolysis time，aging temperature，and aging time during the preparation of high-purity pseudo boehmite by hydrolysis of isooctanol aluminum and combining XRD analysis of the crystal phase of the product.The results showed that changes in hydrolysis temperature，hydrolysis time，aging temperature，and aging time all affected the solubility of pseudo boehmite，with hydrolysis temperature having the most significant effect.The solubility index of pseudo boehmite obtained by hydrolysis at 95 ℃ could reach over 99.9%，and the shortest gelation time was 8 seconds.After hydrolysis at 95 ℃，different aging times and temperatures had no significant effect on the solubility index of the product，which could reach over 99.9%.To further improve the solubility of the product，the hydrolyzed product was treated in a pure water system at 110 ℃，and the gelation time was shortened to about 5 seconds，exhibiting various technical parameters comparable to commercial high-purity pseudo boehmite（SB powder）.This study provided a research foundation for the large-scale production of high-purity pseudo boehmite prepared by hydrolysis of isooctanol aluminum.

Key words: isooctanol aluminum, high-purity pseudoboehmite, solubility index, gelation time

CLC Number:

TQ133.1

TIAN Peng, JIAO Dandan, LI Fan, NING Guiling. Study on synthesis of high purity pseudoboehmite by hydrolyzing isooctanol aluminum[J]. Inorganic Chemicals Industry, 2025, 57(10): 49-54.

Figures/Tables 8

Fig.1

Table 1

Fig.2

Table 2

Fig.3

Table 3

Table 4

Table 5

References 26

[1]	DANILEVICH V V， KLIMOV O V， NADEINA K A，et al.Novel eco-friendly method for preparation of mesoporous alumina from the product of rapid thermal treatment of gibbsite［J］.Superlattices and Microstructures，2018，120：148-160.
[2]	李凡，杨雨哲，田朋，等.仲丁醇铝水解制备高纯拟薄水铝石［J］.无机盐工业，2022，54（7）：78-84，104.
	LI Fan， YANG Yuzhe， TIAN Peng，et al.Preparation of high purity pseudo-boehmite by hydrolysis of aluminium sec-butoxide［J］.Inorganic Chemicals Industry，2022，54（7）：78-84，104.
[3]	HWANG K T， LEE H S， LEE S H，et al.Synthesis of aluminium hydrates by a precipitation method and their use in coatings for ceramic membranes［J］.Journal of the European Ceramic Society，2001，21（3）：375-380.
[4]	田朋，李伟，杨雨哲，等.异丙醇铝水解制高纯拟薄水铝石［J］.无机盐工业，2022，54（2）：54-59.
	TIAN Peng， LI Wei， YANG Yuzhe，et al.Preparation of high purity pseudo-boehmite by hydrolysis of aluminium isopropanol［J］.Inorganic Chemicals Industry，2022，54（2）：54-59.
[5]	YOLDAS B E.Hydrolysis of aluminium alkoxides and bayerite conversion［J］.Journal of Applied Chemistry and Biotechnology，1973，23（11）：803-809.
[6]	杨永佳，张新昇，李金，等.大孔拟薄水铝石和γ-Al₂O₃ 载体制备研究进展［J］.过程工程学报，2021，21（10）：1156-1166.
	YANG Yongjia， ZHANG Xinsheng， LI Jin，et al.Research progress in preparation of large pore pseudoboehmite and γ-Al₂O₃ carri-er［J］.The Chinese Journal of Process Engineering，2021，21（10）：1156-1166.
[7]	FU Wenjing， WEI Cundi， ZUO Jing，et al.A facile temperature-controlled “green” method to prepare multi-kinds of high-quality alumina hydrates via a Ga-In-Sn-alloyed aluminum-water interface reaction［J］.ACS Omega，2022，7（23）：19775-19783.
[8]	ALIZADEH ARASI M， SALEM A， SALEM S.Nano-porous hydrosodalite fabrication via hydrothermal modification of processed Kaolin by boehmite：Aluminum source effect on physico-chemical characteristics of product［J］.Advanced Powder Technology，2020， 31（6）：2379-2384.
[9]	MUKHAMED′YAROVA A N， NESTEROVA O V， BORETSKY K S，et al.Influence of the obtaining method on the properties of amorphous aluminum compounds［J］.Coatings，2019，9（1）：41.
[10]	刘袁李.异丙醇铝水解制备催化用拟薄水铝石和氧化铝［D］.大连：大连理工大学，2020.
	LIU Yuanli.Preparation of pseudo boehmite and alumina for catalysis by hydrolysis of aluminum isopropoxide［D］.Dalian：Dalian University of Technology，2020.
[11]	DUAN Ning， ZHANG Xiangtai， LU Chenglong，et al.Effect of rheological properties of AlOOH Sol on the preparation of Al₂O₃ nanofiltration membrane by sol-gel method［J］.Ceramics International，2022，48（5）：6528-6538.
[12]	CHEN Long， SU Sijie， TIAN Peijing，et al.Effect of PMMA on the structure and transmittance of porous alumina antireflection coating prepared by sol-gel and template method［J］.Ceramics International，2024，50（7）：12591-12597.
[13]	HUANG J， CHO Y， WANG V，et al.Dielectric-on-dielectric achieved on SiO₂ in preference to W by water-free chemical vapor depositions with aniline passivation［J］.ACS Applied Materials & Interfaces，2023，15（21）：26128-26137.
[14]	RODRIGUEZ-OLGUIN M A， ATIA H， BOSCO M，et al.Al₂O₃ nanofibers prepared from aluminum Di（sec-butoxide）acetoacetic ester chelate exhibits high surface area and acidity［J］.Journal of Catalysis，2022，405：520-533.
[15]	LIN Yan， LUO Li， YANG Zhirong，et al.Controlled engineering of high-purity pseudo-boehmite with large pore volume by aluminum alkoxide hydrolysis：Mechanistic understanding and reforming catalysis［J］.Chemical Engineering Science，2024，298：120372.
[16]	XU Huan， LIU Cui， GUO Wei，et al.Sodium alginate/Al₂O₃ fiber nanocomposite aerogel with thermal insulation and flame retardancy properties［J］.Chemical Engineering Journal，2024，489：151223.
[17]	李伟.异丙醇铝水解制高纯拟薄水铝石［D］.大连：大连理工大学，2022.
	LI Wei.Preparation of high-purity pseudo boehmite by hydrolysis of aluminum isopropoxide［D］.Dalian：Dalian University of Technology，2022.
[18]	纪洪波，许学翔，张林，等.高纯氧化铝的制备工艺［J］.化工进展，2006，25（6）：712-713.
	JI Hongbo， XU Xuexiang， ZHANG Lin，et al.Process for producing high-pure alumina［J］.Chemical Industry and Engineering Progress，2006，25（6）：712-713.
[19]	ZHANG Tieqing， JUNG S， KIM Y B.Hydrogen production system through dimethyl ether autothermal reforming，based on model predictive control［J］.Energies，2022，15（23）：9038.
[20]	MENG Fanhui， LI Baozhen， ZHANG Jinghao，et al.Role of Zn-Al oxide structure and oxygen vacancy in bifunctional catalyst for syngas conversion to light olefins［J］.Fuel，2023，346：128351.
[21]	RIVERO-ANTÚNEZ P， CANO-CRESPO R， SÁNCHEZ-BAJO F，et al.Reactive SPS for sol-gel alumina samples：Structure，sintering behavior，and mechanical properties［J］.Journal of the European Ceramic Society，2021，41（11）：5548-5557.
[22]	LI Jing， WANG Ning， ZHUANG Yanhong，et al.Preparation of high permeability γ-Al₂O₃ ultrafiltration membranes from pseudo-boehmite industrial precursor［J］.Ceramics International，2023，49（17）：28943-28953.
[23]	MOHAMMADLOU T， BABALUO A A， KHOSHFETRAT A B.Preparation of high flux mesoporous γ-alumina membranes for whey proteins isolation：Peptizing agent（acetic acid） and binder （PEG） effects［J］.Ceramics International，2022，48（15）：21235-21244.
[24]	LIU Yi， JIA Lu， LIN Yi，et al.Catalytic combustion of toluene over Cu-Mn mixed oxide catalyst［J］.Journal of Chemical Engineering of Japan，2018，51（9）：769-777.
[25]	贾睿.球形氧化铝的制备、表征及性能模拟［D］.沈阳：沈阳工业大学，2021.
	JIA Rui.Preparation，characterization，and performance simulation of spherical alumina ［D］.Shenyang：Shenyang University of Technology，2021.
[26]	GÜLDENPFENNIG A， DISTASO M， PEUKERT W. In situ investigations on the amorphous to crystalline phase transformation of precursors for methanol synthesis catalysts［J］.Chemical Engineering Journal，2019，369：996-1004.

水解温度/℃	w（氧化铝）/%	胶溶指数/%	成胶时间
30	68.53	6.80	不凝胶
45	68.40	19.13	不凝胶
60	69.35	67.61	不凝胶
75	74.75	91.84	不凝胶
90	76.60	97.44	约1 d
95	78.70	>99.90	17 s

水解时间/ h	w （氧化铝）/%	胶溶指数/ %	成胶时间/ s
0.5	76.71	>99.9	150
1.0	77.67	>99.9	110
1.5	77.86	>99.9	80
2.0	76.86	>99.9	45
3.0	79.26	>99.9	21
4.0	79.26	>99.9	17

陈化温度/ ℃	w（氧化铝）/ %	胶溶指数/ %	成胶时间/ s
70	77.70	>99.9	>900
75	77.46	>99.9	900
80	77.85	>99.9	690
85	77.75	>99.9	510
90	78.00	>99.9	195
95	76.71	>99.9	150

水解时间/ h	陈化时间/ h	w（氧化铝）/ %	成胶时间/ s
1	5	77.30	21
2	4	78.60	20
3	3	77.30	17
4	2	77.80	17
5	1	78.30	16
6	0	77.27	14
9	0	78.01	11
12	0	78.80	8

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Study on synthesis of high purity pseudoboehmite by hydrolyzing isooctanol aluminum

RichHTML

PDF (PC)

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 8

References 26

Related Articles 15

Metrics

Comments

Recommended 0

[1]	LI Lei, LI Yuelei, CHANG Hao. Study on sintering mechanism of dense fine-grained alumina ceramics [J]. Inorganic Chemicals Industry, 2025, 57(10): 75-80.
[2]	MENG Qingjie, CAO Lingling, HUO Guoyou, ZHENG Huaili, SUN Manli. Study on preparation of PAC by a new gel method and its algal removal effect [J]. Inorganic Chemicals Industry, 2025, 57(10): 81-89.
[3]	WANG Minrui, TIAN Guiying, ZHANG Ao, GE Junjie, ZHANG Lei, XIANG Jun, TANG Na. Study on granulation optimization for Al-based lithium adsorbent and its lithium recovery performance from brine [J]. Inorganic Chemicals Industry, 2025, 57(3): 36-42.
[4]	LIU Xinlong, YANG Zhenyu, HAO He, LIU Shuxin, WU Chenyang, WANG Xingli, MA Qingqing. Study on shaped 4A zeolite synthesized with aluminum extraction residue by fly ash [J]. Inorganic Chemicals Industry, 2025, 57(3): 78-85.
[5]	ZHANG Yanyan, LI Donghong, LIU Yonghe, ZHANG Yang, KANG Le, WANG Yi. Study on surface treatment of alumina filler [J]. Inorganic Chemicals Industry, 2025, 57(1): 77-82.
[6]	LÜ Lingshuang, CAO Wenhao, YU Ruixian, WANG Shouzhi, WANG Guodong, ZHU Yajun, DU Jiachen, XU Xiangang, ZHANG Lei. Research on purification process of AlN source material by two-step sintering method [J]. Inorganic Chemicals Industry, 2024, 56(12): 51-55.
[7]	REN Xuechang, FENG Hao. Study on dissolution process of sintered clinker by aluminum ash alkali method with ultrasound irritation [J]. Inorganic Chemicals Industry, 2024, 56(6): 119-126.
[8]	ZHANG Yaqi, CHEN Xiping, SUN Ningning. Study on preparation process of cryolite from anode carbon slag by catalytic decarburization [J]. Inorganic Chemicals Industry, 2024, 56(3): 91-97.
[9]	TIAN Peng, XU Jingang, XU Qianjin, LIU Kunji, PANG Hongchang, NING Guiling. Preparation of nano-alumina slurry and its application in modifying lithium-ion battery cathode material [J]. Inorganic Chemicals Industry, 2023, 55(12): 43-49.
[10]	LIU Wei, XU Yan, CHEN Yongsheng, SUN Chunhui, ZHANG Jingcheng, ZHU Jinjian, LIU Yang. Effect of alkaline earth metals on performance of Cu/Al₂O₃ ester hydrogenation catalyst [J]. Inorganic Chemicals Industry, 2023, 55(9): 140-144.
[11]	WANG Mengdi, LUO Jin, WU Wei, ZHOU Jinghui, WANG Jing, SUN Yanmin, YU Haibin. Study on preparation of γ-Al₂O₃ by microreaction and its properties for methyl orange adsorption [J]. Inorganic Chemicals Industry, 2023, 55(9): 66-74.
[12]	PANG Fei, XU Yingrui, CHAI Chunling, SHEN Jingjing, BAI Liguang, ZHAO Xiaodong. Overview on recycling of waste activated alumina in production of hydrogen peroxide by anthraquinone process [J]. Inorganic Chemicals Industry, 2023, 55(6): 1-7.
[13]	WANG Lijuan, YAN Kezhou, GUO Zhiqiang, ZHAO Zhonghe, GUO Yanxia, CHENG Fangqin. Preparation of poly-aluminum chloride from acid leaching liquor of red mud-coal gangue activated by sodium salt [J]. Inorganic Chemicals Industry, 2023, 55(4): 76-83.
[14]	LI Xing,QIN Jun,LU Qing,XU Yong,ZHANG Lijin. Effect of α/γ-alumina on structure and properties of synthesized Mg-Al hydrotalcite [J]. Inorganic Chemicals Industry, 2022, 54(12): 51-59.
[15]	YANG Yongyu,TIAN Peng,ZHOU Ruohui,XU Qianjin,LIU Kunji,NING Guiling. Effect of gibbsite activation on preparation of boehmite by hydrothermal method [J]. Inorganic Chemicals Industry, 2022, 54(9): 55-62.