煅烧白云石粉制备微纳米级圆片状氢氧化镁
收稿日期: 2021-03-19
网络出版日期: 2022-03-14
基金资助
国家自然科学基金(61102041);辽宁省高校创新团队支撑计划(2013010);国家科技支撑计划(2013BAB09B01);辽宁省教育厅项目(L2013169);辽宁省精细化工协同创新中心资助项目;辽宁省自然科学基金(201602582);辽宁省高等学校创新人才支持计划(LR2018078);辽宁省自然科学基金材料联合基金(20180510007);辽宁省自然科学基金指导计划项目(2019ZD0075);菱镁固废化工材料高值利用技术与基地集成示范(2020YFCI909300);辽宁省教育厅项目(LJKZ0431)
Preparation of micro-nano round flake magnesium hydroxide from calcined dolomite powder
Received date: 2021-03-19
Online published: 2022-03-14
以白云石为原料,通过氨法制备出高纯度(99.30%)圆片状的阻燃型微纳米级氢氧化镁。探究了反应温度、通氨速率、氨镁物质的量比对氢氧化镁分散性和形貌的影响,确定最佳工艺条件:反应温度为80 ℃、通氨速率为150 mL/min、氨镁物质的量比为23∶1。用扫描电镜、透射电子显微镜、X射线衍射仪、激光粒度分析仪、热重分析仪和白度仪表征产品的形貌、结构、粒度及稳定性。结果表明制得的圆片状微纳米级氢氧化镁的分散性好、晶型完整、粒度均匀,D50为2.493 μm、D90为6.132 μm、直径约为5.7 μm、厚度约为0.7 μm、长厚比约为8∶1。稳定性好、灼烧失量为31.03%、白度为97.4,高于工业氢氧化镁行业标准。
范天博 , 胡婷婷 , 韩冬雪 , 贾晓辉 , 赵一波 , 王新安 , 郭洪范 , 李莉 , 刘云义 . 煅烧白云石粉制备微纳米级圆片状氢氧化镁[J]. 无机盐工业, 2022 , 54(1) : 29 -33 . DOI: 10.19964/j.issn.1006-4990.2021-0169
Micro-nano-sized high-purity(99.30%) round flake magnesium hydroxide as the flame retardant was prepared from dolomite by ammonia method.The effect of reaction temperature,ammonia-passing rate,ammonia-magnesium molar ratio on the dispersion and morphology of magnesium hydroxide were investigated.The optimal process conditions were determined:reaction temperature was 80 ℃,ammonia-passing rate was 150 mL/min,and ammonia-magnesium molar ratio was 23∶1.The morphologies,structures,size distributions and stability of products were characterized through scanning electron microscope,transmission electron microscope,X-ray diffractometer,laser particle analyzer,thermogravimetric analyzer and whiteness meter.The results showed that the prepared round flake micro-nano-sized magnesium hydroxide flame retardant had high dispersibility,complete crystal shape,uniform particle size with D50 of 2.493 μm,D90 of 6.132 μm,diameter of about 5.7 μm,thickness of about 0.7 μm and length thickness ratio of about 8∶1.The stability was good,the ignition loss was 31.03%,and the whiteness was 97.4,which was higher than industrial magnesium hydroxide industry standard.
Key words: dolomite; round flake magnesium hydroxide; flame retardant
[1] | 罗仙平, 王金庆, 董竑君, 等. 纳米氢氧化镁的制备及表征方法研究进展[J]. 盐业与化工, 2016, 45(6):14-19. |
[2] | ZHUANG Z Y, OU X W. Interfacial engineering improved the se-lective extraction of uranyl from saline water by nano-Mg(OH)2 and the underlying mechanism[J]. ACS Sustainable Chem.Eng., 2015, 4(3):801-809. |
[3] | 王安民, 赵建海, 梅林玲, 等. 氢氧化镁混凝性能及其对印染废水处理研究进展[J]. 天津城建大学学报, 2019, 25(1):51-55. |
[4] | FAN J J, HU Y B, LI X Y. Nanoscale zero-valent iron coated with magnesium hydroxide for effective removal of cyanobacteria from water[J]. ACS Sustainable Chem.Eng., 2018, 6(11):15135-15142. |
[5] | 黄永强, 游小艇, 杨铭. 氢氧化镁对水质、底质改良的研究和应用[J]. 渔业研究, 2017, 39(2):139-146. |
[6] | 潘年明, 薛晨. 氢氧化镁乳液的制备及其在脱硫中的应用[J]. 应用化工, 2017, 46(7):1331-1334,1339. |
[7] | LIU X M, SONG K N, LIU W Z, et al. Removal and recovery of Pb from wastewater through a reversible phase transformation process between nano-flower-like Mg(OH)2 and soluble Mg(HCO3)2[J]. Environmental Science:Nano, 2019, 6:467-477. |
[8] | 韩文生, 李丽娟, 宋富根, 等. Fe3O4/Mg(OH)2复合材料的制备及形貌控制[J]. 盐湖研究, 2020, 28(3):93-98. |
[9] | 宋雪雪, 李丽娟, 姬连敏, 等. 纳米及微米级六角片状氢氧化镁的制备[J]. 盐湖研究, 2018, 26(2):66-74,80. |
[10] | 范天博, 李雪, 马超, 等. 氯化镁溶液氨气鼓泡反应制备纳米氢氧化镁[J]. 化工学报, 2010, 61(11):3025-3032. |
[11] | 厥永生, 刘跃军, 杨军. 油酸包覆针状氢氧化镁纳米粉体的制备[J]. 中国粉体技术, 2010, 16(3):50-53. |
[12] | 王明帆, 马祥伟, 游轻寒, 等. 活性氢氧化镁水热改性制备分散性氢氧化镁[J]. 无机盐工业, 2015, 47(7):29-31. |
[13] | 赵丽慈. 球形氢氧化镁的合成、磷硅改性及阻燃EVA的研究[D]. 保定:河北大学, 2015. |
[14] | 黄建翠, 凌观爽, 宗俊. 水菱镁矿制备高分散六角片状纳米氢氧化镁的新工艺条件探究[J]. 无机盐工业, 2021, 53(2):55-60. |
[15] | 张旭, 卜庆伟, 王超君, 等. 氢氧化镁表面改性与阻燃性能研究[J]. 消防科学与技术, 2018, 37(7):951-954. |
[16] | 赵连梅, 赵建海, 张强, 等. 油酸钠对纳米氢氧化镁的表面改性研究[J]. 消防科学与技术, 2007(1):80-82. |
[17] | 范天博, 姜宇, 刘露萍, 等. 一步水热法合成六方片状氢氧化镁及其生长习性分析的研究[J]. 人工晶体学报, 2017, 46(12):2319-2325. |
[18] | 崔益顺. 氢氧化镁阻燃剂制备及性能研究[J]. 无机盐工业, 2017, 49(9):38-41. |
/
〈 |
|
〉 |