Page 29 - 《精细化工》2019年第11期

第 36 卷第 11 期 精 细 化 工 Vol.36, No.11
2019 年 11 月 FINE CHEMICALS Nov. 2019

功能材料
煤矸石浸渣制备白炭黑工艺优化及性能分析

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刘成龙 ，许爱华 ，夏举佩 ，郑光亚 ，李宛霖 ，梁永锋 ，马 贵
（1. 宁夏师范学院 化学化工学院，宁夏 固原 756000；2. 昆明理工大学 化学工程学院，云南 昆明
650500）
摘要：为实现煤矸石固废的资源化高效综合利用，以煤矸石浸取 Al、Fe、Ti 等元素后的浸渣为原料，利用煤矸
石浸渣-硫酸钠干法制备出水玻璃，然后采用碳化法制备白炭黑产品。借助邻苯二甲酸二丁酯（DBP）测定产品
的吸油值，并通过比表面积测定（BET）、X 射线衍射分析（XRD）、红外光谱分析（FTIR）、扫描电镜（SEM）
以及热重-差热分析（TG-DSC）等对白炭黑进行了结构表征与性能测试；考察了水玻璃质量分数、反应温度、
Na 2 CO 3 质量浓度、CO 2 通入速率对白炭黑 DBP 吸油值和比表面积的影响，在单因素实验基础上以比表面积为
主要指标，利用正交实验设计与响应曲面法联合设计优化了制备工艺。结果表明：在水玻璃质量分数为 10%、
反应温度为 77 ℃、CO 2 通入速率为 147 mL/min、Na 2 CO 3 质量浓度为 3 g/L 条件下，实验结果与响应曲面预测结
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果基本吻合，制得比表面积为 267.33 m /g、DBP 吸油值为 2.77 mL/g 的白炭黑产品。产品性能分析表明，所制
白炭黑为由非晶态物质组成的无定形态产品，产品中基本无杂质出现，纯度较高，微观形貌较好，符合 HG/T3061
—2009 中 A 类产品的要求。
关键词：煤矸石；浸渣；白炭黑；正交实验设计；响应曲面法；功能材料
中图分类号：TQ170.9; TQ127.2 文献标识码：A 文章编号：1003-5214 (2019) 11-2177-08

Process Optimization and Performance Analysis for Preparation of

Silica from Coal Gangue Leaching Residue

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LIU Cheng-long , XU Ai-hua , XIA Ju-pei , ZHENG Guang-ya ,
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LI Wan-lin , LIANG Yong-feng , MA Gui
（1. School of Chemistry and Chemical Engineering, Ningxia Normal University, Guyuan 756000, Ningxia, China;
2. Faculty of Chemical Engineering, Kunming University of Science and Technology, Kunming 650500, Yunnan, China）
Abstract: In order to realize efficient and comprehensive utilization of coal gangue solid waste, the
leaching residue after leaching Al, Fe, Ti and other elements of coal gangue was used as raw material to
prepare sodium silicate solution by sodium sulfate dry method. Then, a high value-added silica was
prepared by a carbonization method. The oil absorption value of silica was determined by dibutyl phthalate
(DBP). The structure and properties of the product was characterized by specific surface area test (BET),
X-ray diffraction (XRD), Fourier Transform infrared spectroscopy (FTIR), scanning electron microscopy
(SEM) and thermogravimetric-differential scanning calorimetry (TG-DSC) and other modern characterization
methods. The effects of sodium silicate concentration, reaction temperature, Na 2CO 3 mass concentration
and CO 2 ventilation rate on the DBP absorption value and specific surface area of silica were investigated
by single factor experiment. Subsequently, the orthogonal test design and response surface methodology
was used to optimize the preparation process of silica using specific surface area as main index. The results
indicated that the optimum process conditions were obtained as follows: the mass fraction of sodium silicate
was 10%, the reaction temperature was 77 ℃, the CO 2 ventilation rate was 147 mL/min, and the Na 2CO 3
mass concentration 3 g/L. The verification experiment results were basically consistent with the prediction
results of the response surface. Under these optimum conditions, the obtained silica had a specific surface

收稿日期：2019-04-23; 定用日期：2019-06-04; DOI: 10.13550/j.jxhg.20190348
基金项目：宁夏师范学院校级重点科研项目资助（NXSFZDC1904）
作者简介：刘成龙（1987—），男，硕士，助教，E-mail：lclmyx@163.com。