响应曲面法优化碳热还原重铬酸钠制备超细氧化铬

doi:10.19964/j.issn.1006-4990.2022-0752

Abstract

Abstract:

The high purity ultrafine chromium oxide was prepared by carbothermal reduction method optimized by response surface method using sodium dichromate separated and extracted from chromium-containing electroplating sludge as precursor.It effectively avoided the disadvantages of environmental pollution caused by a large amount of chromium-containing waste produced in the production process of traditional processes，and achieved the goal of comprehensive utilization of chromium resources and zero pollution emission.The effects of n（C）/n（Na₂Cr₂O₇），reaction time and reaction temperature on RE_Cr（Ⅵ） were investigated.On this basis，the response surface method was used to optimize the selection，and the reactants and reduction products were characterized by thermogravimetric analyzer and X-ray diffractometer.The mechanism of carbothermal reduction was discussed.The results showed that the optimum reduction conditions were n（C）/n（Na₂Cr₂O₇）=4，reaction time of 2 h，reaction temperature of 550 ℃，and the RE_Cr（Ⅵ） reached 99.947%.The significant order from big to small of the influence of various factors on RE_Cr（Ⅵ） was：n（C）/n（Na₂Cr₂O₇），reaction temperature，reaction time.The mechanism of carbothermal reduction was that Na₂Cr₂O₇ was first reduced to Cr₂O₃ and Na₂CO₃ by carbon black during the reduction process，then molten Na₂Cr₂O₇ neutralized Na₂CO₃ to form Na₂CrO₄，and finally Na₂CrO₄ was further reduced to Cr₂O₃ by carbon black.At the same time，the reaction temperature should not be too high，too high reaction temperature would promote the transformation of Cr₂O₃ to NaCrO₂.The purity of the prepared Cr₂O₃ product was more than 99%，and the average particle size was 214.246 nm，which met the first-class quality index of industrial chromium trioxide and met the high-value utilization requirements of materials such as plasma spraying and chrome green pigments.

Key words: carbothermal reaction, chromium oxide, sodium dichromate, response surface methodology

CLC Number:

TQ136.11

ZHANG Zhiqiang, CUI Kangping, CHEN Xing, LI Haiyang. Optimization of preparation of ultrafine chromium oxide by carbothermal reduction of sodium dichromate by response surface methodology[J]. Inorganic Chemicals Industry, 2023, 55(10): 136-144.

Figures/Tables 14

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水平	影响因子
水平	A n（C）/n（Na₂Cr₂O₇）	B 反应时间/h	C 反应温度/℃
-1	1	1	400
0	3	2	500
1	5	3	600

序号	影响因子			实验值/ %	预测值/ %
序号	A	B/h	C/℃	实验值/ %	预测值/ %
1	3	2	500	93.19	93.80
2	5	2	600	99.90	101.36
3	1	3	500	85.35	85.66
4	5	3	500	95.65	98.58
5	5	1	500	95.65	95.34
6	3	2	500	92.13	93.80
7	1	1	500	83.96	84.58
8	3	3	600	99.54	98.71
9	1	2	600	87.13	87.65
10	5	2	400	88.65	88.13
11	3	2	500	95.63	93.80
12	3	2	500	92.36	93.80
13	1	2	400	79.60	78.14
14	3	1	400	84.34	85.17
15	3	1	600	98.62	97.47
16	3	3	400	87.12	88.27
17	3	2	500	95.70	93.80

方差来源	平方和	自由度	均方差	F值	P值	显著性
模型	612.71	9	68.08	21.70	0.000 3	极显著
A	280.37	1	280.37	89.39	<0.000 1	极显著
B	9.33	1	9.33	2.97	0.128 2	不显著
C	258.55	1	258.55	82.43	<0.000 1	极显著
AB	1.17	1	1.17	0.371 9	0.561 3	不显著
AC	3.46	1	3.46	1.10	0.328 5	不显著
BC	0.864 9	1	0.864 9	0.275 7	0.615 7	不显著
A²	42.40	1	42.40	13.52	0.007 9	极显著
B²	0.713 0	1	0.713 0	0.227 3	0.648 1	不显著
C²	13.77	1	13.77	4.39	0.047 4	显著
残差	21.96	7	3.14	—	—
失拟项	9.76	3	3.25	1.07	0.456 5	不显著
纯误差	12.19	4	3.05	—	—
总离差	634.66	16	—	—	—

指标		w（Cr₂O₃）/ %	w（水溶性铬）/%	w（水分）/ %	w（水溶物）/ %	pH（100 g/L 悬浮液）	吸油量/ g	w（粒径>0.045 mm 粒子）/%
Ⅰ类	优等品	≥99.0	≤0.005	≤0.15	≤0.1	6~8	15~25	≤0.1
	一等品	≥99.0	≤0.03	≤0.15	≤0.3	5~8	15~25	≤0.2
	合格品	≥98.0	≤0.03	≤0.3	≤0.4	5~8	15~25	≤0.3
Ⅱ类	优等品	≥99.0	≤0.005	≤0.15	≤0.2	—	≤20	≤0.2
	一等品	≥99.0	≤0.03	≤0.15	≤0.3	—	≤25	≤0.2
	合格品	≥98.0	≤0.03	≤0.3	≤0.5	—	≤25	—
本文产品		99.53	0.004	0.0	0.1	7.5	23	0.1

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Optimization of preparation of ultrafine chromium oxide by carbothermal reduction of sodium dichromate by response surface methodology

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