氧氯化锆改性膨胀石墨的制备及性能研究

doi:10.3969/j.issn.1001-1935.2021.02.008

耐火材料 ›› 2021, Vol. 55 ›› Issue (2): 126-130.DOI: 10.3969/j.issn.1001-1935.2021.02.008

氧氯化锆改性膨胀石墨的制备及性能研究

王梓祎¹⁾(), 魏军从¹⁾, 郑晓艺¹⁾, 王子琦¹⁾, 涂军波¹⁾(), 郁柏松¹⁾, 苏玉庆¹⁾, 王义龙²⁾

1)华北理工大学河北省无机非金属材料重点实验室河北唐山 063210
2)唐山市国亮特殊耐火材料有限公司河北唐山 063000

收稿日期:2020-07-15 出版日期:2021-04-15 发布日期:2021-04-15
作者简介:王梓祎:女,1996年生,硕士研究生。E-mail:648347030@qq.com
基金资助:
河北省自然科学基金资助项目(E2017209164)

Preparation and properties of expanded graphite modified by zirconium oxychloride

Wang Ziyi¹⁾(), Wei Juncong¹⁾, Zheng Xiaoyi¹⁾, Wang Ziqi¹⁾, Tu Junbo¹⁾(), Yu Baisong¹⁾, Su Yuqing¹⁾, Wang Yilong²⁾

1)Hebei Province Key Laboratory of Inorganic Nonmetallic Materials,North China University of Science and Technology,Tangshan 063210,Hebei,China

Received:2020-07-15 Online:2021-04-15 Published:2021-04-15

摘要/Abstract

摘要：

为了提高膨胀石墨的石墨化度和抗氧化性,经氧氯化锆溶液真空浸渍后再经高温埋碳热处理制备了改性膨胀石墨,主要研究了改性前的石墨化度和抗氧化性及埋碳热处理温度(分别为1 550、1 600、1 650 ℃)和氧氯化锆溶液真空浸渍时间(分别为30、60、90 min)对改性膨胀石墨的石墨化度和抗氧化性的影响。结果表明:1)经改性处理,膨胀石墨的石墨化度和抗氧化性提高。2)随着埋碳热处理温度从1 550 ℃提高到1 600 ℃,改性膨胀石墨的石墨化度和抗氧化性提高;随着埋碳热处理温度从1 600 ℃提高到1 650 ℃,改性膨胀石墨的石墨化度和抗氧化性降低。3)随着氧氯化锆真空浸渍时间从30 min延长到60 min,改性膨胀石墨的石墨化度和抗氧化性提高;随着氧氯化锆真空浸渍时间从60 min延长到90 min,改性膨胀石墨的石墨化度和抗氧化性降低。4)在-0.08 MPa真空度下浸渍60 min,再在1 600 ℃埋碳热处理3 h制备的改性膨胀石墨的石墨化度和抗氧化性能最高。

关键词: 氧氯化锆, 改性处理, 膨胀石墨, 石墨化度, 抗氧化性

Abstract:

In order to improve the graphitization degree and oxidation resistance of expanded graphite,the modified expanded graphite was prepared by vacuum impregnation of zirconium oxychloride solution and high-temperature carbon embedded heat treatment.Effects of the carbon embedded temperature (1 550,1 600,and 1 650 ℃) and vacuum impregnation duration (30,60,and 90 min) on the graphitization degree and oxidation resistance of the expanded graphite were researched.The results show that:(1)after modification,the graphitization degree and oxidation resistance of the expanded graphite are improved;(2)the graphitization degree and oxidation resistance of the modified expanded graphite improve with the temperature rising from 1 550 ℃ to 1 600 ℃,but decrease from 1 600 ℃ to 1 650 ℃;(3)the graphitization degree and oxidation resistance of the modified expanded graphite improve with the vacuum impregnation duration prolonging from 30 min to 60 min,but decrease from 60 min to 90 min;(4)the graphitization degree and oxidation resistance of the modified expanded graphite prepared by impregnation at -0.08 MPa vacuum for 60 min and then carbon embedded heat treated at 1 600 ℃ for 3 h are the best.

Key words: zirconium oxychloride, modification treatment, expanded graphite, graphitization degree, oxidation resistance

中图分类号:

TQ175

王梓祎, 魏军从, 郑晓艺, 王子琦, 涂军波, 郁柏松, 苏玉庆, 王义龙. 氧氯化锆改性膨胀石墨的制备及性能研究[J]. 耐火材料, 2021, 55(2): 126-130.

Wang Ziyi, Wei Juncong, Zheng Xiaoyi, Wang Ziqi, Tu Junbo, Yu Baisong, Su Yuqing, Wang Yilong. Preparation and properties of expanded graphite modified by zirconium oxychloride[J]. Refractories, 2021, 55(2): 126-130.

图/表 8

图1 改性前及在不同温度埋碳热处理制得的改性膨胀石墨的XRD图谱

Fig.1 XRD patterns of modified EG prepared by carbon embedded heat treatment at different temperatures and before modification

图2 改性前及在不同温度埋碳热处理制得的改性膨胀石墨的拉曼光谱

Fig.2 Raman spectra of modified EG prepared by carbon embedded heat treatment at different temperatures and before modification

图3 改性前膨胀石墨的SEM照片

Fig.3 SEM photos of EG before modification

图4 在1 550 ℃埋碳热处理制得的改性膨胀石墨的SEM照片

Fig.4 SEM photos of modified EG prepared by carbon embedded heat treatment at 1 550 ℃

图5 在1 600 ℃埋碳热处理制得的改性膨胀石墨的SEM照片

Fig.5 SEM photos of modified EG prepared by carbon embedded heat treatment at 1 600 ℃

图6 在1 650 ℃埋碳热处理制得的改性膨胀石墨的SEM照片

Fig.6 SEM photos of modified EG prepared by carbon embedded heat treatment at 1 650 ℃

图7 改性前及在不同温度埋碳热处理制得的改性膨胀石墨的TG-DSC曲线

Fig.7 TG-DSC curves of modified EG prepared before and after carbon embedded heat treatment at different temperatures

图8 改性前及在氧氯化锆浸渍液中真空浸渍不同时间制得的改性膨胀石墨的拉曼光谱

Fig.8 Raman spectra of modified EG prepared before and after vacuum impregnation in zirconium oxychloride impregnation solution for different periods

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氧氯化锆改性膨胀石墨的制备及性能研究

Preparation and properties of expanded graphite modified by zirconium oxychloride

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