煤矸石浸渣制备白炭黑工艺优化及性能分析
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TQ170.9;TA536.4

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宁夏师范学院校级重点科研项目资助(NXSFZDC1904)


Process Optimization and Performance Analysis for Preparation of Silica from Coal Gangue Leaching Residue
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Scientific Research Project of Ningxia Normal University (NXSFZDC1904)

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    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)测定吸油值、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;以水玻璃浓度、反应温度、Na2CO3质量浓度、CO2通入速率为考察因素进行了单因素实验,在单因素实验基础上以比表面积为主要指标进行了正交实验设计与响应曲面法联合设计优化制备工艺。结果表明:在水玻璃质量分数为10 %、反应温度为77℃、CO2通入速率为147 mL/min、Na2CO3质量浓度为3 g/L条件下,实验结果与响应曲面预测结果基本吻合,制得比表面积为267.33 m2/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。

    Abstract:

    In order to realize the efficient and comprehensive utilization of coal gangue solid waste, the coal gangue leaching residue - sodium sulfate dry method was chosen to prepare sodium silicate solution with the acid leaching residue as raw materials,which was generated after valuable elements extraction from coal gangue. A high value-added silica product was prepared by a carbonization method. Determination of dibutyl phthalate oil absorption value, specific surface area test X-ray diffraction, Fourier Transform infrared spectroscopy, scanning electron microscopy and thermogravimetric analysis - differential scanning calorimetry and other modern characterization methods were used to characterize the properties of silica. The concentration of sodium silicate, reaction temperature, the Na2CO3 mass concentration and CO2 ventilation rate were investigated by single factor test. Based on the single factor test, the orthogonal test design and response surface methodology were used to optimize the preparation process with specific surface area as the main index. The results indicate that the optimum process conditions are as follows: the sodium silicate mass fraction 10%, the reaction temperature 77 °C, and the CO2 ventilation rate 147 mL/min, and Na2CO3 mass concentration 3%, the verification experiment results are basically consistent with the prediction results of the response surface, under this condition, the silica product with specific surface area of 267.33 m2•g-1 and DBP oil absorption value of 2.77 mL•g-1 can be obtained. The product performance analysis shows that the product is an amorphous product composed of amorphous materials. The product has no impurities, high purity and good micro-morphology, which meets the requirements of Class A products in standard HG/T3061-2009.

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引用本文

刘成龙.煤矸石浸渣制备白炭黑工艺优化及性能分析[J].精细化工,2019,36(11):

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  • 收稿日期:2019-04-23
  • 最后修改日期:2019-06-03
  • 录用日期:2019-06-04
  • 在线发布日期: 2019-09-27
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