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

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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

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Inorganic Acid-Base-Salt Committee of CIESC

Synthesis and dehydration dynamics of boehmite microcrystalline with different particle sizes

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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

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