微晶菱镁矿蒸氨及水化动力学研究

doi:10.11949/0438-1157.20221587

化工学报 ›› 2023, Vol. 74 ›› Issue (4): 1578-1586.DOI: 10.11949/0438-1157.20221587

• 催化、动力学与反应器 • 上一篇下一篇

微晶菱镁矿蒸氨及水化动力学研究

衣思敏¹(), 马亚丽¹^,²^,³^,⁴, 刘伟强¹, 张金帅¹, 岳岩¹, 郑强¹^,²^,³^,⁴, 贾松岩¹^,²^,³^,⁴, 李雪¹^,²^,³^,⁴()

^1.沈阳化工大学化学工程学院，辽宁沈阳 110020
^2.教育部资源化工与材料重点实验室，辽宁沈阳 110020
^3.辽宁省化工应用技术重点实验室，辽宁沈阳 110020
^4.辽宁省镁钙资源无机功能材料工程研究中心，辽宁沈阳 110020

收稿日期:2022-12-09 修回日期:2023-02-26 出版日期:2023-04-05 发布日期:2023-06-02
通讯作者: 李雪
作者简介:衣思敏（1998—），女，硕士研究生，y06100319@163.com
基金资助:
2020—2022年辽宁省普通本科高等学校校际合作项目（辽教发[2020]28号文件）;2021—2023年辽宁省科技厅创新能力提升联合基金项目(2021-NLTS-12-04);辽宁省自然科学基金项目(2022-BS-210)

Study on ammonia evaporation and hydration kinetics of microcrystalline magnesite

Simin YI¹(), Yali MA¹^,²^,³^,⁴, Weiqiang LIU¹, Jinshuai ZHANG¹, Yan YUE¹, Qiang ZHENG¹^,²^,³^,⁴, Songyan JIA¹^,²^,³^,⁴, Xue LI¹^,²^,³^,⁴()

^1.College of Chemical Engineering, Shenyang University of Chemical Technology, Shenyang 110020, Liaoning, China
^2.Key Laboratory of Resource Chemicals and Materials, Ministry of Education, Shenyang 110020, Liaoning, China
^3.Liaoning Provincial Key Laboratory of Chemical Application Technology, Shenyang 110020, Liaoning, China
^4.Liaoning Magnesium-Calcium Inorganic Functional Materials Engineering Research Center, Shenyang 110020, Liaoning, China

Received:2022-12-09 Revised:2023-02-26 Online:2023-04-05 Published:2023-06-02
Contact: Xue LI

摘要/Abstract

摘要：

为加强微晶菱镁矿的深入研究，分别以微晶菱镁矿经高温煅烧所得微晶MgO和辽宁某工厂轻烧MgO为原料进行蒸氨、沉镁、煅烧得到MgO，并进行水化实验。采用水合法考察了MgO活性对蒸氨动力学的影响，探究了反应温度、固液比对产品粒径及水化率的影响，考察了不同固液比所得产品形貌，并对水化曲线进行分析，确定了不同镁源的水化反应控制类型。结果表明：二者的蒸氨反应都受扩散控制；在100℃、9 h条件下，固液比为1/5时，微晶MgO水化产品呈完整的六方片状结构，而轻烧MgO水化产品的片状结构大小不一且不规整；二者水化反应均属于化学反应控制类型。此研究为微晶菱镁矿的利用发展提供了新思路。

关键词: 微晶菱镁矿, 粉体技术, 蒸氨反应, 热解, 动力学

Abstract:

In order to strengthen the further study of micrystalline magnesite, the microcrystalline MgO obtained from calcined microcrystalline magnesite and the light burned MgO from a factory in Liaoning are used as raw materials for steaming ammonia, precipitating magnesium and calcinating to obtain MgO, and conduct hydration experiment. The effect of MgO activity on ammonia evaporation kinetics was investigated by water method, and the effects of reaction temperature and solid-liquid ratio on particle size and hydration rate of products were investigated, the morphologies of products with different solid-liquid ratios were investigated, and hydration curves were analyzed to determine the hydration reaction control types of different magnesium sources. The results show that the evaporation of ammonia in both of them is controlled by diffusion. Under the conditions of 100℃ and 9 h, when the solid-liquid ratio is 1/5, the microcrystalline MgO hydration product has a complete hexagonal sheet structure, while the sheet structure of the lightly burned MgO hydration product is different in size and irregular. Both hydration reactions belong to the internal diffusion chemical reaction control type. This study provides a new idea for the utilization and development of micrystalline magnesite.

Key words: microcrystalline magnesite, powder technology, ammonia evaporation reaction, pyrolysis, kinetics

中图分类号:

TQ 132.2

衣思敏, 马亚丽, 刘伟强, 张金帅, 岳岩, 郑强, 贾松岩, 李雪. 微晶菱镁矿蒸氨及水化动力学研究[J]. 化工学报, 2023, 74(4): 1578-1586.

Simin YI, Yali MA, Weiqiang LIU, Jinshuai ZHANG, Yan YUE, Qiang ZHENG, Songyan JIA, Xue LI. Study on ammonia evaporation and hydration kinetics of microcrystalline magnesite[J]. CIESC Journal, 2023, 74(4): 1578-1586.

图/表 12

表1 不同MgO主要成分

Table 1 Main components of different MgO

成分	微晶MgO主要成分含量/%	轻烧MgO主要成分含量/%
MgO	96.15	75.83
CaO	1.55	7.21
SiO₂	0.24	10.25
Fe₂O₃	0.05	2.04

表2 不同原料所得水化MgO中活性MgO含量

Table 2 Active MgO content in hydrated MgO obtained from different raw materials

样品编号	以微晶MgO为原料活性MgO含量/%	以轻烧MgO为原料活性MgO含量/%
1	75.15	56.14
2	76.52	56.35
3	76.47	54.77
平均值	76.05	55.75

图1 不同原料Mg2+浸出率曲线

Fig.1 Curve of leaching rate of Mg2+ from different raw materials

图2 不同温度下不同原料蒸氨反应拟合关系

Fig.2 The fitting relation of ammonia evaporation reaction of different raw materials at different temperatures

图3 不同原料蒸氨lnk-1/T关系曲线

Fig.3 lnk-1/T of ammonia of different raw materials

图4 反应温度、固液比对产品粒径的影响

Fig.4 Effect of reaction temperature and solid-liquid ratio on particle size of product

图5 反应温度、固液比对水化率的影响

Fig.5 Effect of reaction temperature and solid-liquid ratio on hydration rate

图6 反应温度为100℃、反应时间为3 h的水化产物SEM图

Fig.6 SEM images of hydration products at reaction temperature of 100℃ and reaction time of 3 h

图7 反应温度为100℃、反应时间为3 h的水化产物XRD谱图

Fig.7 XRD patterns of hydration products at reaction temperature of 100℃ and reaction time of 3 h

图8 不同原料水化曲线

Fig.8 Hydration curves of different raw materials

图9 不同温度下不同原料水化反应拟合关系

Fig.9 The fitting relation of hydration reaction of different raw materials at different temperatures

图10 不同原料水化lnk-1/T关系曲线

Fig.10 lnk-1/T curves of hydration of different raw materials

参考文献 34

1	李志勋, 冯润棠, 田晓利,等. 水化方式对微晶菱镁矿制备高纯氢氧化镁的影响[J]. 耐火材料, 2018, 52(3):213-216.
	Li Z X, Feng R T, Tian X L, et al. Effect of hydration process on preparation of high purity magnesium hydroxide from microcrystalline magnesite[J]. Refractories, 2018, 52(3):213-216.
2	田晓利, 李志勋, 冯润棠,等. 煅烧制度对微晶菱镁矿制备高致密度烧结镁砂性能的影响[J]. 耐火材料, 2022, 56(5):400-406.
	Tian X L, Li Z X, Feng R T, et al. Effect of calcination schedule on properties of high density sintered magnesia prepared from microcrystalline magnesite[J]. Refractories, 2022, 56(5):400-406.
3	王刚, 夏志豪, 李希艳,等. 不同气氛下流化床菱镁矿轻烧产物特性研究[J]. 化工学报, 2022, 73(8):3699-3707.
	Wang G, Xia Z H, Li X Y, et al. Effect of atmosphere on active performance of light-burned magnesium oxides from calcined magnesite in fluidized bed[J]. CIESC Journal, 2022, 73(8):3699-3707.
4	杨翠杰, 赵华, 徐恺,等. (NH₄)₂SO₄浸取轻烧粉的控制过程[J]. 矿产综合利用, 2016(5):66-68, 42.
	Yang C J, Zhao H, Xu K, et al. Study on controlling process of (NH₄)₂SO₄ leaching of light-calcined powder[J]. Multipurpose Utilization of Mineral Resources, 2016(5):66-68, 42.
5	巴浩静, 白丽梅, 赵文青,等. 轻烧镁制备及深加工研究进展[J]. 矿产保护与利用, 2017(1):84-89.
	Ba H J, Bai L M, Zhao W Q, et al. Review on preparation and processing of caustic calcined magnesit[J]. Conservation and Utilization of Mineral Resources, 2017(1):84-89.
6	范天博, 姜宇, 陈思,等. TRIZ理论在轻烧粉氨气法制备氢氧化镁过程中的应用研究[J]. 无机盐工业, 2019, 51(5):23-27, 44.
	Fan T B, Jiang Y, Chen S, et al. Application of TRIZ theory in preparation of magnesium hydroxide by light burning ammonia[J]. Inorganic Chemicals Industry, 2019, 51(5): 23-27, 44.
7	吴易梅, 孙玉柱, 路贵民,等. 结晶-水热法制备六角片状氢氧化镁[J]. 高校化学工程学报, 2019, 33(2):425-434.
	Wu Y M, Sun Y Z, Lu G M, et al. Preparation of hexagonal sheet magnesium hydroxide flake by a crystallization-hydrothermal method[J]. Journal of Chemical Engineering of Chinese Universities, 2019, 33(2):425-434.
8	赵丽, 王立艳, 肖姗姗,等.氢氧化镁阻燃剂制备研究进展[J]. 无机盐工业, 2018, 50(3):16-19.
	Zhao L, Wang L Y, Xiao S S, et al. Research progress in preparation of magnesium hydroxide flame retardant[J]. Inorganic Chemicals Industry, 2018, 50(3):16-19.
9	李雪, 程沛, 侯睿,等. 轻烧粉氨气法制备氢氧化镁阻燃剂的研究[J]. 无机盐工业, 2016, 48(11):21-24.
	Li X, Cheng P, Hou R, et al. Preparation of Mg(OH)₂ with caustic calcined magnesia through ammonium circulation[J]. Inorganic Chemicals Industry, 2016, 48(11):21-24.
10	姚建平, 范天博, 王健,等. 氨状态对氨法制备氢氧化镁颗粒性质的影响[J]. 化工学报, 2012, 63(1):314-319.
	Yao J P, Fan T B, Wang J, et al. Influence of ammonia state on particle characterization of magnesium hydroxide prepared via ammonia method[J]. CIESC Journal, 2012, 63(1):314-319.
11	孙晓君, 丁珂, 仇龙,等. 以轻烧粉制备六方片状氢氧化镁[J]. 硅酸盐学报, 2019, 47(4):538-544.
	Sun X J, Ding K, Qiu L, et al. Preparation of hexagonal-sheet magnesium hydroxide by surfactant free method[J]. Journal of the Chinese Ceramic Society, 2019, 47(4):538-544.
12	吴丹, 张琦, 王玉琪,等. 轻烧粉在氯化铵体系中的萃取实验研究[J]. 应用化工, 2021, 50(2):415-418.
	Wu D, Zhang Q, Wang Y Q, et al. Experimental study on extraction of light burning powder in ammonium chloride system[J]. Applied Chemical Industry, 2021, 50(2):415-418.
13	丁珂, 孙晓君, 李会杰,等. 氧化镁蒸氨反应的动力学和机理研究[J]. 无机盐工业, 2019, 51(11):31-35.
	Ding K, Sun X J, Li H J, et al. Study on kinetics and mechanism of ammonia evaporation reaction of magnesium oxide[J]. Inorganic Chemicals Industry, 2019, 51(11):31-35.
14	朱云, 王善忠, 胡建锋. 水热法制备阻燃剂氢氧化镁[J]. 有色金属, 2007(3): 30-32, 36.
	Zhu Y, Wang S Z, Hu J F. Hydrothermal preparation of flame retardant Mg(OH)₂ [J]. Nonferrous Metals, 2007(3): 30-32, 36.
15	梁晓正, 马玉新, 李鸣铎,等. 外力环境对氧化镁水化产物性能的影响[J]. 有色金属工程, 2020, 10(6):1-8.
	Liang X Z, Ma Y X, Li M D, et al. Effect of external force on properties of products prepared from hydration of MgO[J]. Nonferrous Metals Engineering, 2020, 10(6): 1-8.
16	白丽梅, 邢智博, 张俊,等. 氧化镁常压水合法制备氢氧化镁的过程分析[J]. 非金属矿, 2017, 40(4):1-3.
	Bai L M, Xing Z B, Zhang J, et al. The process analysis of hydrating magnesium oxide to prepare magnesium hydroxide under the ordinary pressure[J]. Non-Metallic Mines, 2017, 40(4):1-3.
17	黄娜娜, 李会杰, 仇龙,等. 菱镁矿氨法制备氢氧化镁及活性氧化镁水化动力学研究[J]. 盐科学与化工, 2020, 49(2):29-32.
	Huang N N, Li H J, Qiu L, et al. Study on hydration kinetics of magnesium hydroxide and active magnesium oxide prepared by magnesite ammonia process[J]. Journal of Salt Science and Chemical Industry, 2020, 49(2):29-32.
18	刘欣伟, 冯雅丽, 李浩然,等. 菱镁矿制备轻烧氧化镁及其水化动力学研究[J]. 中南大学学报(自然科学版), 2011, 42(12):3912-3917.
	Liu X W, Feng Y L, Li H R, et al. Preparation of light-burned magnesia from magnesite and its hydration kinetics[J]. Journal of Central South University (Science and Technology), 2011, 42(12):3912-3917.
19	王利莎. 氧化镁水合法制备阻燃级氢氧化镁研究[D]. 天津: 天津科技大学, 2012.
	Wang L S. Research on hydration preparation of fire-retardant level magnesium hydrate from magnesium oxide[D]. Tianjin: Tianjin University of Science & Technology, 2012.
20	白炳华. 微晶菱镁矿制备高纯轻质氧化镁研究[D]. 西安: 西安建筑科技大学, 2021.
	Bai B H. Research of preparation of high purity light magnesium oxide from microcrystalline magnesite[D]. Xi'an: Xi'an University of Architecture and Technology, 2021.
21	张诗英. 菱镁粉MgO活性测定方法研究: Cl^－测定法[J]. 武汉工业大学学报, 1994, 16(3): 114-117.
	Zhang S Y. The study of determination method in magnisia activity[J]. Journal of Wuhan University of Technology, 1994, 16(3): 114-117.
22	王素平. 高活性氧化镁的制备与吸附性能的研究[D]. 天津: 天津大学, 2015.
	Wang S P. Study on the synthesis and adsorption properties of high active MgO[D]. Tianjin: Tianjin University, 2015.
23	孙世清, 谢维章. 用热分析方法研究MgO的活性[J]. 硅酸盐学报, 1986, 14(2): 226-232.
	Sun S Q, Xie W Z. Study on the activity of MgO by thermal analysis[J]. Journal of the Chinese Ceramic Society, 1986, 14(2): 226-232.
24	李广垠, 李志坚, 徐娜,等. 轻烧氧化镁活性对烧结镁砂性能的影响[J]. 硅酸盐通报, 2018, 37(5):1699-1703.
	Li G Y, Li Z J, Xu N, et al. Effect of light burned magnesia activity on properties of sintered magnesia[J]. Bulletin of the Chinese Ceramic Society, 2018, 37(5):1699-1703.
25	董金美, 余红发, 张立明. 水合法测定活性MgO含量的试验条件研究[J]. 盐湖研究, 2010, 18(1):38-41.
	Dong J M, Yu H F, Zhang L M. Study on experimental conditions of hydration methods of determining active magnesium oxide content[J]. Journal of Salt Lake Research, 2010, 18(1):38-41.
26	He G X, Zhao Z W, Wang X B, et al. Leaching kinetics of scheelite in hydrochloric acid solution containing hydrogen peroxide as complexing agent[J]. Hydrometallurgy, 2014, 144/145: 140-147.
27	肖永丰, 陈爱国, 张雨薇,等. 粉煤灰提铝硅渣碱溶脱硅反应及其动力学[J]. 硅酸盐通报, 2021, 40(2):542-547.
	Xiao Y F, Chen A G, Zhang Y W, et al. Desilication reaction and kinetics of aluminum-extracting silicon slag in NaOH solution[J]. Bulletin of the Chinese Ceramic Society, 2021,40(2):542-547.
28	Zheng Y J, Chen K K. Leaching kinetics of selenium from selenium-tellurium-rich materials in sodium sulfite solutions[J]. Transactions of Nonferrous Metals Society of China, 2014, 24(2):536-543.
29	Amaral L F, Oliveira I R, Salomão R, et al. Temperature and common-ion effect on magnesium oxide (MgO) hydration[J]. Ceramics International, 2010, 36(3):1047-1054.
30	Kato Y, Yamashita N, Kobayashi K, et al. Kinetic study of the hydration of magnesium oxide for a chemical heat pump [J]. Applied Thermal Engineering, 1996, 16(11):853-862.
31	Birchal V S, Rocha S D F, Mansur M B, et al. A simplified mechanistic analysis of the hydration of magnesia [J]. The Canadian Journal of Chemical Engineering, 2001, 79(4):507-511.
32	郭杰, 刘百宽, 田晓利,等. 微晶菱镁矿制备高纯氢氧化镁水化工艺研究[J]. 非金属矿, 2019, 42(5):45-48.
	Guo J, Liu B K, Tian X L, et al. Study on hydration process of preparing high purity magnesium hydroxide from microcrystalline magnesite[J]. Non-Metallic Mines, 2019, 42(5):45-48.
33	孔会民, 邹来禧, 刘远,等. 以轻烧氧化镁制备六角片状氢氧化镁的研究[J]. 无机盐工业, 2022, 54(1):39-44.
	Kong H M, Zou L X, Liu Y, et al. Study on preparation of hexagonal plates of magnesium hydroxide by light-burned magnesium oxide[J]. Inorganic Chemicals Industry, 2022, 54(1):39-44.
34	翟学良, 杨永社. 活性氧化镁水化动力学研究[J]. 无机盐工业, 2000, 32(4): 16-18.
	Zhai X L, Yang Y S. Study of hydrolization kinetics of activated MgO[J]. Inorganic Chemicals Industry, 2000, 32(4): 16-18.

编辑推荐 0

Metrics

阅读次数

全文

113

HTML			PDF

最新录用	在线预览	正式出版	最新录用	在线预览	正式出版
4	1	10	19	0	79

来源	本网站	其他网站

次数	83	30
比例	73%	27%

摘要

213

最新录用	在线预览	正式出版

32	1	180

来源	本网站	其他网站

次数	120	93
比例	56%	44%

[1]	金正浩, 封立杰, 李舒宏. 氨水溶液交叉型再吸收式热泵的能量及分析[J]. 化工学报, 2023, 74(S1): 53-63.
[2]	程成, 段钟弟, 孙浩然, 胡海涛, 薛鸿祥. 表面微结构对析晶沉积特性影响的格子Boltzmann模拟[J]. 化工学报, 2023, 74(S1): 74-86.
[3]	肖明堃, 杨光, 黄永华, 吴静怡. 浸没孔液氧气泡动力学数值研究[J]. 化工学报, 2023, 74(S1): 87-95.
[4]	毕丽森, 刘斌, 胡恒祥, 曾涛, 李卓睿, 宋健飞, 吴翰铭. 粗糙界面上纳米液滴蒸发模式的分子动力学研究[J]. 化工学报, 2023, 74(S1): 172-178.
[5]	于宏鑫, 邵双全. 水结晶过程的分子动力学模拟分析[J]. 化工学报, 2023, 74(S1): 250-258.
[6]	吴雷, 刘姣, 李长聪, 周军, 叶干, 刘田田, 朱瑞玉, 张秋利, 宋永辉. 低阶粉煤催化微波热解制备含碳纳米管的高附加值改性兰炭末[J]. 化工学报, 2023, 74(9): 3956-3967.
[7]	范孝雄, 郝丽芳, 范垂钢, 李松庚. LaMnO₃/生物炭催化剂低温NH₃-SCR催化脱硝性能研究[J]. 化工学报, 2023, 74(9): 3821-3830.
[8]	郑佳丽, 李志会, 赵新强, 王延吉. 离子液体催化合成2-氰基呋喃反应动力学研究[J]. 化工学报, 2023, 74(9): 3708-3715.
[9]	汪林正, 陆俞冰, 张睿智, 罗永浩. 基于分子动力学模拟的VOCs热氧化特性分析[J]. 化工学报, 2023, 74(8): 3242-3255.
[10]	杨越, 张丹, 郑巨淦, 涂茂萍, 杨庆忠. NaCl水溶液喷射闪蒸-掺混蒸发的实验研究[J]. 化工学报, 2023, 74(8): 3279-3291.
[11]	曾如宾, 沈中杰, 梁钦锋, 许建良, 代正华, 刘海峰. 基于分子动力学模拟的Fe₂O₃纳米颗粒烧结机制研究[J]. 化工学报, 2023, 74(8): 3353-3365.
[12]	李锦潼, 邱顺, 孙文寿. 煤浆法烟气脱硫中草酸和紫外线强化煤砷浸出过程[J]. 化工学报, 2023, 74(8): 3522-3532.
[13]	张蒙蒙, 颜冬, 沈永峰, 李文翠. 电解液类型对双离子电池阴阳离子储存行为的影响[J]. 化工学报, 2023, 74(7): 3116-3126.
[14]	何宣志, 何永清, 闻桂叶, 焦凤. 磁液液滴颈部自相似破裂行为[J]. 化工学报, 2023, 74(7): 2889-2897.
[15]	周继鹏, 何文军, 李涛. 异形催化剂上乙烯催化氧化失活动力学反应工程计算[J]. 化工学报, 2023, 74(6): 2416-2426.

微晶菱镁矿蒸氨及水化动力学研究

Study on ammonia evaporation and hydration kinetics of microcrystalline magnesite

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

图/表 12

参考文献 34

相关文章 15

编辑推荐 0

Metrics

本文评价