不同粒径薄水铝石微晶的合成及其脱水动力学分析

doi:10.19964/j.issn.1006-4990.2023-0001

Abstract

Abstract:

It is of great significance to explore the particle size regulation of boehmite and the thermal decomposition mechanism of boehmite into alumina for the synthesis of fine alumina.Pseudo-boehmite was used as a seed to assist aluminum hydroxide hydrothermal to regulate the particle size of boehmite，and the universality of this method was explored.Through the kinetic analysis of the calcination experiment and the dehydration process of boehmite with different particle sizes，the influence mechanism of particle size on the transformation process of boehmite was explored.The results showed that the addition of different proportions of pseudo-boehmite seeds could prepare boehmite microcrystalline with average particle size D50 of 2.02，0.96 and 0.66 μm，respectively.The seeds produced by different processes had the same control effect.The dehydration process of boehmite with different particle sizes was controlled by different kinetic reaction mechanisms，and as the particle size decreased，the activation energy of the dehydration process was gradually decreased.This study provided a new effective way to adjust the particle size of boehmite，and provided a theoretical basis for the preparation of fine alumina from boehmite as a precursor.

Key words: boehmite, alumina, grain size, dynamics, activation energy, crystal seed

CLC Number:

P578.4+96

TIAN Peng, ZHOU Ruohui, XU Qianjin, LIU Kunji, PANG Hongchang, NING Guiling. Synthesis and dehydration dynamics of boehmite microcrystalline with different particle sizes[J]. Inorganic Chemicals Industry, 2023, 55(11): 27-36.

Figures/Tables 14

Table 1

Fig.1

Table 2

Fig.2

Fig.3

Fig.4

Table 3

Table 4

Fig.5

Fig.6

Table 5

Fig.7

Table 6

Table 7

References 41

1	STAMIRES D， O'CONNOR P， PEARSON G，et al.Process for the preparation of quasi-crystalline boehmites from inexpensive precursors：US，6689333［P］.2004-02-10.
2	KARGER-KOCSIS J， LENDVAI L.Polymer/boehmite nanocomposites：A review［J］.Journal of Applied Polymer Science，2018，135（24）：45573.
3	NISHIMURA S， LE S D， ASAI Y，et al.Boehmite-derived aluminum oxide catalyst for a continuous intramolecular aldol condensation of 2，5-hexanedione to 3-methyl-2-cyclopentenone in a liquid-flow reactor system［J］.Chemistry Letters，2022，51（2）：131- 134.
4	RAVINDRAN A R， LADANI R B， ZAVABETI A，et al.Liquid metal synthesis of two-dimensional aluminium oxide platelets to reinforce epoxy composites［J］.Composites Science and Technology，2019，181：107708.
5	曹伟娜，任昆仑，李莉，等.勃姆石改性PET复合材料的阻燃和增强机理研究［J］.中国塑料，2019，33（7）：32-37.
	CAO Weina， REN Kunlun， LI Li，et al.Flame retardancy and reinforcing mechanism of boehemite-modified PET composites［J］.China Plastics，2019，33（7）：32-37.
6	虞瑞雷，叶定坤，叶耀挺，等.勃姆石协同氢氧化镁阻燃尼龙复合材料及其制备方法和应用：中国，110343383B［P］.2022-04-01.
7	WANG Yuan， WANG Qiulin， WEI Xiuqin，et al.A novel three-dimensional boehmite nanowhiskers network-coated polyethylene separator for lithium-ion batteries［J］.Ceramics International，2021，47（7）：10153-10162.
8	ZHONG Guobin， WANG Yong， WANG Chao，et al.An AlOOH-coated polyimide electrospun fibrous membrane as a high-safety lithium-ion battery separator［J］.Ionics，2019，25（6）：2677-2684.
9	WANG Yuan， WANG Qiulin， LAN Yu，et al.Aqueous aluminide ceramic coating polyethylene separators for lithium-ion batteri- es［J］.Solid State Ionics，2020，345：115188.
10	LIU Kefan， YANG Chengyuan， LI Xiaogang，et al.Controllable coaxial coating of boehmite on the surface of polyimide nanofiber membrane and its application as a separator for lithium-ion batteries［J］.Energy Technology，2022，10（4）：2100982.
11	GOONERATNE R， IROH J O.Thermomechanical and pre-ignition properties of multicomponent poly（vnylidene fluoride）/aluminum oxide/single-walled carbon nanotube hybrid nanocomposites［J］.Journal of Composites Science，2022，6（12）：380.
12	NOWECK K， SCHIMANSKI J， JUHL J，et al.Boehmitic aluminas，and high-temperature stabile and highly porous aluminum oxides in a pure phase which are obtained therefrom：US，6773690［P］.2004-08-10.
13	川上义贵，曾我部康平，梅田铁.氧化铝和使用其的汽车催化剂的制造方法：中国，109476493A［P］.2021-06-11.
14	苏少龙，李晓云，杨文建，等.一种球形氧化铝的制备方法：中国，109179465B［P］.2021-02-23.
15	NASU T， ASUMA A.Alumina powder for sintering：JP，2020105047A［P］.2020-07-09.
16	CIGANE U， PALEVICIUS A， JANUSAS G.Vibration-assisted synthesis of nanoporous anodic aluminum oxide（AAO） membranes［J］.Micromachines，2022，13（12）：2236.
17	VEIGA L P DA， JEANGUENAT C， LISCO F，et al.Ultrathin ALD aluminum oxide thin films suppress the thermal shrinkage of battery separator membranes［J］.ACS Omega，2022，7（49）：45582-45589.
18	尾崎裕谦，安东博幸.氧化铝和含有其的浆料、和氧化铝多孔膜、层叠隔板、非水电解液二次电池及其制造方法：中国，109119576B［P］.2020-01-03.
19	HARMENING T， SCHONEBORN M， JAGER A K.Alumina bismuth catalyst support and method for its production field of the invention：EP，3827897A1［P］.2021-06-02.
20	吴永峰.勃姆石高温煅烧相变及溶出活性研究［J］.世界有色金属，2020（4）：9-10.
	WU Yongfeng.Study on the phase transition and digestion performance of boehmite at high temperature［J］.World Nonferrous Metals，2020（4）：9-10.
21	YANG Yongyu， TIAN Peng， GAO Tingting，et al.Synthesis of controlled-particle-size boehmite for coating lithium-ion battery separators［J］.New Journal of Chemistry，2023，47（5）：2211-2220.
22	杨永钰，田朋，周若辉，等.氢氧化铝活化对水热法制备勃姆石的影响［J］.无机盐工业，2022，54（9）：55-62.
	YANG Yongyu， TIAN Peng， ZHOU Ruohui，et al.Effect of gibbsite activation on preparation of boehmite by hydrothermal method［J］.Inorganic Chemicals Industry，2022，54（9）：55-62.
23	POPESCU C.Integral method to analyze the kinetics of heterogeneous reactions under non-isothermal conditions A variant on the Ozawa-Flynn-Wall method［J］.Thermochimica Acta，1996， 285（2）：309-323.
24	ZHANG Jianjun， REN Ning.A new kinetic method of processing TA data［J］.Chinese Journal of Chemistry，2004，22（12）：1459-1462.
25	杨仲禹.一种材料热分析动力学参数的获取方法：中国，113008931A［P］.2021-06-22.
26	NAQVI S R， TARIQ R， HAMEED Z，et al.Pyrolysis of high-ash sewage sludge：Thermo-kinetic study using TGA and artificial neural networks［J］.Fuel，2018，233：529-538.
27	任宁，张秀芳，白继海，等.Popescu法研究一水合乙酸铜的热分解动力学［J］.河北师范大学学报，2005，29（6）：584-587.
	REN Ning， ZHANG Xiufang， BAI Jihai，et al.Study on thermal decomposition kinetics of copper acetate dihydrate with popescu method［J］.Journal of Hebei Normal University（Natural Science），2005，29（6）：584-587.
28	XU Bingan， SMITH P.Dehydration kinetics of boehmite in the temperature range 723-873 K［J］.Thermochimica Acta，2012，531：46-53.
29	彭志宏，李琼芳，周秋生.氢氧化铝脱水过程的动力学研究［J］.轻金属，2010（5）：16-18.
	PENG Zhihong， LI Qiongfang， ZHOU Qiusheng.Studies on dehydration kinetics of aluminium hydroxide［J］.Light Metals，2010（5）：16-18.
30	KAZANTSEV S O， BAKINA O V， PERVIKOV A V，et al.Antimicrobial activity and sorption behavior of Al₂O₃/Ag nanocomposites produced with the water oxidation of bimetallic Al/Ag nanoparticles［J］.Nanomaterials，2022，12（21）：3888.
31	ABDOU N Y， SABRY M， EL-FARAMAWY N.Thermoluminescence characteristics of different phase transitions from nanocrystalline alumina［J］.Journal of Radioanalytical and Nuclear Chemistry，2022，331（9）：3865-3876.
32	NAMPI P P， GHOSH S， WARRIER K G.Calcination and associated structural modifications in boehmite and their influence on high temperature densification of alumina［J］.Ceramics International，2011，37（8）：3329-3334.
33	高振昕，贺中央，郑小平，等.拜尔法三水铝石受热相变的形貌特征［J］.硅酸盐学报，2008，36（S1）：117-123.
	GAO Zhenxin， HE Zhongyang， ZHENG Xiaoping，et al.Phase transformation and morphology of bayer-gibbsite during heating［J］.Journal of the Chinese Ceramic Society，2008，36（S1）：117-123.
34	张智慧，李楠，阮国智. γ-Al₂O₃和α-Al₂O₃与其对应的氢氧化物对合成尖晶石的影响［J］.耐火材料，2007，41（1）：33- 36.
	ZHANG Zhihui， LI Nan， RUAN Guozhi.Influence of γ-Al₂O₃ and α-Al₂O₃ and their corresponding hydroxides on synthesis of spinel［J］.Refractories，2007，41（1）：33-36.
35	WANG Haipeng， XU Bingan， SMITH P，et al.Kinetic modelling of gibbsite dehydration/amorphization in the temperature range 823-923 K［J］.Journal of Physics and Chemistry of Solids，2006，67（12）：2567-2582.
36	范伟东，李旺兴，韩东战，等.粒度对氢氧化铝低温相变动力学的影响［J］.化工进展，2020，39（3）：1101-1107.
	FAN Weidong， LI Wangxing， HAN Dongzhan，et al.Influence of particle size on kinetics of low temperature phase transformation of aluminum hydroxide［J］.Chemical Industry and Engineering Progress，2020，39（3）：1101-1107.
37	OKADA K， NAGASHIMA T， KAMESHIMA Y，et al.Effect of crystallite size of boehmite on sinterability of alumina ceramics［J］.Ceramics International，2003，29（5）：533-537.
38	OKADA K， NAGASHIMA T， KAMESHIMA Y，et al.Effect of crystallite size on the thermal phase change and porous properties of boehmite［J］.Journal of Colloid and Interface Science，2002，248（1）：111-115.
39	黎少华，袁方利，胡鹏，等.薄水铝石粒度对煅烧形成α-Al₂O₃粉体的影响［J］.过程工程学报，2006，6（4）：580-584.
	LI Shaohua， YUAN Fangli， HU Peng，et al.Influence of boehmite particle size on the formation of α-alumina powder by calcination［J］.The Chinese Journal of Process Engineering，2006，6（4）：580-584.
40	关昕，王晶，史忠祥.水热法制备薄水铝石粉体及其脱水动力学分析［J］.大连交通大学学报，2018，39（4）：77-82.
	GUAN Xin， WANG Jing， SHI Zhongxiang.Preparation and kinetics of dehydration of boehmite by hydrothermal treatment［J］.Journal of Dalian Jiaotong University，2018，39（4）：77-82.
41	回佳琦.Al（OH）₃制备Al₂O₃过程中动力学模拟及低温煅烧工艺研究［D］.西宁：青海大学，2019.
	HUI Jiaqi.Kinetic calculation and low-temperature calcination process of Al（OH）₃ prepared Al₂O₃ ［D］.Xining：Qinghai University，2019.

样品	化学组成	D50/μm
AH-01DG	Al（OH）₃	2.23
H-WF-1	Al（OH）₃	1.58
H-WF-5	Al（OH）₃	5.70
H-WF-10	Al（OH）₃	8.70
H-WF-25-SP	Al（OH）₃	27.6
Seed1	AlOOH·xH₂O	—
Seed2	AlOOH·xH₂O	—
Seed3	AlOOH·xH₂O	—
Seed4	AlOOH·xH₂O	—

样品	D10	D25	D50	D75	D90	D99
1#	1.35	1.62	2.02	2.54	3.09	4.20
2#	0.72	0.84	0.96	1.20	1.46	1.69
3#	0.49	0.56	0.66	0.81	1.06	1.38

样品	第一阶段			第二阶段
样品	起始点/ K	终止点/ K	质量损失率/%	起始点/ K	终止点/K	质量损失率/%
1#	303.15	642.08	0.068	651.03	846.47	15.189
2#	303.15	637.14	0.414	650.31	852.04	14.841
3#	303.15	635.69	0.716	655.10	832.69	14.486

样品	第二吸热峰t_p/K	样品	第二吸热峰t_p/K
1#	812.64	3#	793.83
2#	808.86

β/ （K·min^-1）	1#		2#			3#
β/ （K·min^-1）	α_m （Tm=769.1 K）	α_n （Tn=782.3 K）	α_m （Tm=771.3 K）	α_n （Tn=784.1 K）		α_m （Tm=761.3K）	α_n （Tn=771.2 K）
5	0.350	0.650	0.450	0.750	0.450		0.750
10	0.182	0.324	0.254	0.448	0.264		0.425
15	0.101	0.191	0.151	0.263	0.125		0.222
20	0.075	0.152	0.141	0.225	0.116		0.180
25	0.119	0.180	0.115	0.183	0.118		0.176

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Synthesis and dehydration dynamics of boehmite microcrystalline with different particle sizes

RichHTML

PDF (PC)

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 14

References 41

Related Articles 15

Metrics

Comments

Recommended 0

模型	样品1#		样品2#			样品3#
模型	相关系数	截距	相关系数	截距		相关系数	截距
D1	0.965 3	-0.080 9	0.993 6	-0.080 8	0.984 8		-0.095 8
D2	0.953 7	-0.062 9	0.984 8	-0.075 6	0.972 0		-0.084 5
D3	0.941 2	-0.022 1	0.969 0	-0.031 7	0.955 1		-0.034 1
D4	0.949 3	-0.016 4	0.979 8	-0.021 0	0.966 3		-0.023 1
D5	0.920 0	-0.053 1	0.936 0	-0.103 2	0.924 9		-0.106 6
R2	0.997 1	-0.001 5	0.969 8	0.009 7	0.994 6		-0.002 5
R3	0.997 1	-0.001 0	0.969 8	0.006 4	0.994 6		-0.001 6
C1.5	0.960 0	-0.100 9	0.978 9	-0.152 9	0.965 5		-0.173 9
C2	0.946 7	-0.350 7	0.961 4	-0.618 0	0.948 1		-0.668 5
A1	0.974 0	-0.105 3	0.993 3	-0.130 7	0.982 7		-0.165 7
A1.5	0.987 2	-0.014 6	0.998 5	-0.017 8	0.994 4		-0.049 3
A2	0.987 7	0.025 4	0.996 5	0.024 9	0.997 4		-0.002 1
A3	0.969 9	0.051 8	0.988 8	0.050 0	0.969 9		0.051 8
P1	0.997 1	-0.003 1	0.969 8	0.019 3	0.997 1		-0.003 1
P2	0.952 9	0.065 4	0.874 7	0.076 1	0.952 9		0.065 4
P3	0.830 2	0.074 7	0.780 6	0.078 0	0.830 2		0.074 7
P4	0.692 9	0.071 5	0.695 3	0.071 3	0.692 9		0.071 5

样品	a	b	R²	E/（kJ·mol^-1）	A/（10¹² min^-1）
1#	35.373	-273 91	0.985 6	227.732	236.6
2#	31.296	-241 44	0.965 4	200.326	12.70
3#	30.600	-230 93	0.992 8	191.992	3.094

[1]	ZHENG Kexin, WANG Haifeng, WANG Jiawei, ZHOU Xingjie, PEI Zhengqing, LU Ju, MA Dehua. Study on leaching and kinetics of rhododengite in Jingxi area of Guangxi [J]. Inorganic Chemicals Industry, 2025, 57(1): 51-57.
[2]	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.
[3]	TIAN Peng, ZHANG Haoran, XU Jingang, MOU Chenxi, XU Qianjin, NING Guiling. Study on aluminum sol modified anode and cathode materials for lithium ion batteries [J]. Inorganic Chemicals Industry, 2024, 56(9): 44-53.
[4]	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.
[5]	XIANG Mengqi, MENG Hua, WANG Ye, MENG Xianzhang, BAI Yuhang, WANG Yujunyao, ZHANG Yidan. Study on kinetic of iron leaching from titanium gypsum and its cyclic acid leaching process [J]. Inorganic Chemicals Industry, 2024, 56(1): 114-120.
[6]	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.
[7]	LUO Wenbo, LI Heng, LÜ Jun, YANG Linguang, ZHAO Xingfan, LONG Xiao. Study on recovery of silicon and aluminum from industrial silicon slag [J]. Inorganic Chemicals Industry, 2023, 55(9): 94-99.
[8]	KANG Le, JING Maoxiang, LI Donghong, HU Xinyu, JIA Chunyan. Study on preparation and electrochemical performance of lithium aluminate nanorods modified solid electrolyte [J]. Inorganic Chemicals Industry, 2023, 55(8): 65-70.
[9]	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.
[10]	DING Hongyu, ZHONG Jianchu, WANG Hongzhi, ZHANG Shuang. Hydrothermal synthesis of talc by crystal seed induction method [J]. Inorganic Chemicals Industry, 2023, 55(5): 59-65.
[11]	TIAN Xiaoli, LI Zhixun, FENG Runtang, ZHANG Jie, ZHENG Quanfu, SHI Xuwu, DU Yongbin. Study on thermal decomposition behavior of Tibetan Kamado microcrystalline magnesite [J]. Inorganic Chemicals Industry, 2023, 55(3): 60-65.
[12]	XU Jingyao,ZHOU Xiaoli,SUN Jinghui,CAO Alin,QING Peilin. Study on preparation of flake α-alumina based on mixed molten salt at low temperature [J]. Inorganic Chemicals Industry, 2023, 55(2): 73-78.
[13]	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.
[14]	TENG Jiayang, FENG Qingge, ZHANG Xuan, QIN Fanghong, FENG Jinghang, HU Jiawen, CHEN Chaohong. Study on preparation of pseudo-boehmite from aluminum dross resource treatment [J]. Inorganic Chemicals Industry, 2023, 55(11): 130-138.
[15]	GUO Xueqin, DENG Xiaochuan, ZHU Chaoliang, FU Xin, WANG Ruirui, MA Wanxia, FAN Jie, ZUO Fangtao, QING Binju. Study on preparation of modified diatomite loaded ammonium phosphomolybdate composite adsorbent and its adsorption performance of Cs⁺ [J]. Inorganic Chemicals Industry, 2023, 55(11): 19-26.