NaVO3-NH4Cl-H2O体系下NH4VO3溶析结晶工艺

doi:10.19964/j.issn.1006-4990.2023-0371

Abstract

Abstract:

The anti-solvent crystallization technology of NH₄VO₃was proposed to deal with the problems of long induction period and low product yield in the process of NH₄VO₃ cooling crystallization.By using ethanol as anti-solvent and NH₄Cl as precipitator，the effects of volume ratio of ethanol-leaching solution，NH₄Cl initial concentration and temperature on the product yield were investigated by response surface methodology based on single factor experiment and the regression equation for predicting the product yield was obtained.The results showed that the regression equation could predict the product yield well.There was only a significant interaction between the volume ratio of ethanol-leaching solution and the initial concentration of NH₄Cl.The influence of three factors on the product yield from high to low was volume ratio of ethanol-leaching solution，initial concentration of NH₄Cl，temperature.The NH₄VO₃ products with yield greater than 95% were prepared under the conditions of crystallization time of 150 min，NH₄Cl initial concentration of 0.68 mol/L，temperature of 278.15~288.15 K and volume ratio of ethanol-leaching solution of（1.5:1）~（2:1）.The product morphology was flower-like structure with the size of 5~10 μm.

Key words: anti-solvent crystallization, response surface methodology, ammonium metavanadate, ethanol

CLC Number:

TQ420.6

LI Chunli, ZHANG Huanhuan, CHENG Zhuo, TANG Xiuhua, ZHANG Fengzhen, YE Yuling. Anti-solvent crystallization process of NH₄VO₃ in NaVO₃-NH₄Cl-H₂O solution system[J]. Inorganic Chemicals Industry, 2024, 56(5): 39-44.

Figures/Tables 9

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Table 1

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References 17

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序号	A（温度）/ K	B（NH₄Cl初始浓度）/（mol∙L^-1）	C（乙醇-浸取液体积比）	η/%
序号	A（温度）/ K	B（NH₄Cl初始浓度）/（mol∙L^-1）	C（乙醇-浸取液体积比）	实验值	计算值
1	288.15	0.68	1.5:1	96.09	98.44
2	283.15	0.51	1.5:1	87.40	89.14
3	288.15	0.51	2.0:1	97.54	96.94
4	278.15	0.34	1.5:1	84.98	82.63
5	283.15	0.34	2.0:1	98.02	98.20
6	288.15	0.34	1.5:1	71.95	72.37
7	283.15	0.68	1.0:1	93.19	93.01
8	283.15	0.51	1.5:1	86.91	89.14
9	283.15	0.68	2.0:1	95.12	93.37
10	283.15	0.34	1.0:1	46.35	48.10
11	283.15	0.51	1.5:1	90.78	89.14
12	283.15	0.51	1.5:1	92.23	89.14
13	278.15	0.68	1.5:1	97.05	96.63
14	278.15	0.51	2.0:1	93.19	95.36
15	288.15	0.51	1.0:1	68.08	65.91
16	278.15	0.51	1.0:1	75.33	75.93
17	283.15	0.51	1.5:1	88.36	89.14

来源	平方和	自由度	均方和	F值	P值	显著性分析
模型	2 914.88	9	323.88	46.65	<0.000 1	**
A	35.70	1	35.70	5.14	0.057 7	不显著
B	803.09	1	803.09	115.67	<0.000 1	**
C	1 273.04	1	1 273.04	183.36	<0.000 1	**
AB	36.43	1	36.43	5.25	0.055 8	不显著
AC	33.57	1	33.57	4.84	0.063 8	不显著
BC	618.38	1	618.38	89.07	<0.000 1	**
A²	1.66	1	1.66	0.24	0.639 9	不显著
B²	4.13	1	4.13	0.59	0.466 0	不显著
C²	104.15	1	104.15	15.00	0.006 1	**
残差	48.60	7	6.94
失拟误差	27.80	3	9.27	1.78	0.289 6	不显著
纯误差	20.80	4	5.20
总变异	2 963.48	16

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Anti-solvent crystallization process of NH₄VO₃ in NaVO₃-NH₄Cl-H₂O solution system

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Anti-solvent crystallization process of NH4VO3 in NaVO3-NH4Cl-H2O solution system