响应面法优化含锰钛白废水制备碳酸锰的工艺

doi:10.16085/j.issn.1000-6613.2018-1747

摘要/Abstract

摘要：

以硫酸法钛白粉生产过程产生的含锰废水为原料，以碳酸氢铵溶液为沉淀剂, 十二烷基硫酸钠为添加剂，采用液相沉淀法对废水中的锰进行资源化回收。在单因素实验基础上，采用响应面法中的Box-Behnken Design优化实验设计，分别考察了反应温度、过量系数、pH和陈化时间四因素对碳酸锰沉淀率的影响，建立了响应值与影响因素间的回归方程，并确定了优化条件为：反应温度33.3℃、过量系数1.06、pH=7.2、陈化时间2.0h，在该条件下锰的沉淀率预测值为99.30%，相应的实验值为98.90%，预测值与实验值相对误差仅0.4%，表明响应面法所建立的预测锰沉淀率的模型可靠；所得产品经电感耦合等离子体发射光谱仪（ICP-AES）分析锰含量为43.53%，符合工业碳酸锰（HG/T 4203—2011）质量标准中对碳酸锰纯度的要求。研究结果为含锰废水的资源化回收提供了新思路。

关键词: 钛白废水, 液相沉淀法, 碳酸锰, 响应面法, 回收

Abstract:

The method of liquid phase precipitation with ammonium bicarbonate solution as precipitant and sodium dodecyl sulfate as an additive was used to recover manganese from wastewaters produced from sulfate titanium dioxide preparation wastewater. Based on results of single factor tests, Box-Behnken Design，a kind of response surface methodology, was used to investigate the effects of reaction temperature, excess coefficient of ammonium bicarbonate(NH₄HCO₃), pH of the solution and aging time on the precipitation of manganese precipitation rate. Based on the regression analysis, regression equations related to response values and factors were established. The optimal process conditions were determined as follows: reaction temperature of 33.3℃, excess coefficient of 1.06, solution pH of 7.2, and aging time of 2.0h. The predicted precipitation rate of manganese was 99.30%, while the corresponding experimental result was 98.90%. The errors between the predicted and experimental value was 0.4%, which indicated that established models were accurate and reliable for the analysis and prediction of the process of the manganese precipitation rate. In the optimized conditions, the manganese content in the manganese carbonate was 43.53% by ICP-AES analysis method, which reached the standard of industrial grade product (HG/T 4203—2011). This study could provide a new idea for the resource reclamation of manganese-containing wastewater.

Key words: titanium dioxide wastewater, liquid phase precipitation method, manganese carbonate, response surface methodology, recovery

中图分类号:

TQ137.1⁺2

何海霞, 万亚萌, 陈欢哲, 杨昆鹏, 李涛, 任保增. 响应面法优化含锰钛白废水制备碳酸锰的工艺[J]. 化工进展, 2019, 38(06): 2649-2657.

Haixia HE, Yameng WAN, Huanzhe CHEN, Kunpeng YANG, Tao LI, Baozeng REN. Process optimization of preparation of manganese carbonate from manganese-containing titanium dioxide wastewater by response surface methodology[J]. Chemical Industry and Engineering Progress, 2019, 38(06): 2649-2657.

图/表 17

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组分	初始废水含量/g?L^-1	组分	初始废水含量/g?L^-1
Mn²⁺	7.7000	Cu²⁺	0.1200
Fe²⁺	5.0100	Cr³⁺	0.4900
Al³⁺	3.4000	Ni²⁺	0.0725
Ca²⁺	0.4200	Ba²⁺	0.0525
Mg²⁺	1.1900	其他离子	微量

组分	初始废水含量/g?L^-1	组分	初始废水含量/g?L^-1
Mn²⁺	7.7000	Cu²⁺	0.1200
Fe²⁺	5.0100	Cr³⁺	0.4900
Al³⁺	3.4000	Ni²⁺	0.0725
Ca²⁺	0.4200	Ba²⁺	0.0525
Mg²⁺	1.1900	其他离子	微量

组分	预处理后含量/g?L^-1	组分	预处理后含量/g?L^-1
Mn²⁺	15.700	Cu²⁺	＜0.010
Fe²⁺	0.110	Cr³⁺	＜0.010
Al³⁺	0.090	Ni²⁺	＜0.010
Ca²⁺	0.177	Ba²⁺	＜0.010
Mg²⁺	0.150	其他离子	＜0.010

组分	预处理后含量/g?L^-1	组分	预处理后含量/g?L^-1
Mn²⁺	15.700	Cu²⁺	＜0.010
Fe²⁺	0.110	Cr³⁺	＜0.010
Al³⁺	0.090	Ni²⁺	＜0.010
Ca²⁺	0.177	Ba²⁺	＜0.010
Mg²⁺	0.150	其他离子	＜0.010

水平	因子
水平	A/℃	B	C	D/h
-1	20	1.0	6.5	1.5
0	30	1.1	7.0	2.0
1	40	1.2	7.5	2.5