仲丁醇铝水解制备高纯拟薄水铝石
收稿日期: 2021-11-01
网络出版日期: 2022-07-14
基金资助
大连市高层次人才创新支持计划（青年科技之星）(2018RQ15);国家重点研发计划(2021YFA1500300)
Preparation of high purity pseudo-boehmite by hydrolysis of aluminium sec-butoxide
Received date: 2021-11-01
Online published: 2022-07-14
采用仲丁醇铝为原料水解制备高纯拟薄水铝石，研究水解温度、水用量、水解时间、干燥温度对拟薄水铝石胶溶指数的影响，并结合X射线衍射（XRD）和红外光谱（IR）分析产物的结构。研究结果表明：水解温度、水用量、水解时间以及干燥温度的改变都会影响拟薄水铝石的胶溶指数，其中水解温度和水用量的影响最为明显；水解温度的提高有益于拟薄水铝石结晶，低温产物无法胶溶，当水用量不断增大时，产物的晶型从最初的无定形态过渡到拟薄水铝石相，结晶度增加，相应产物的胶溶指数也增大；水解时间的延长，有利于水解产物的晶粒长大，胶溶指数增加；提高干燥温度对产物结晶和胶溶指数的影响均较小。实验最终得到周期短、残水量少、残碳量低的最优水解条件：仲丁醇铝与水物质的量比为1∶4.0，水解搅拌时间为2 h，水解温度和干燥温度均为110 ℃。为进一步提高产物的胶溶指数，采用将水解后产物再水化法对其进行优化，胶溶指数高达99.6%，优化后产物的各项技术参数均可与商用高纯拟薄水铝石（SB粉）相媲美。该研究为仲丁醇铝水解制备拟薄水铝石的工业化提供了相应基础。
李凡 , 杨雨哲 , 田朋 , 李伟 , 宁桂玲 . 仲丁醇铝水解制备高纯拟薄水铝石[J]. 无机盐工业, 2022 , 54(7) : 78 -84 . DOI: 10.19964/j.issn.1006-4990.2021-0660
High purity pseudo-boehmite was prepared by hydrolysis of aluminium sec-butoxide.The effect of hydrolysis temperature，water dosage，hydrolysis time，and drying temperature on dispersion index was investigated.The X-ray diffraction（XRD） and infrared spectroscopy（IR） characterization were carried on to analyze the structure of product.The results showed that hydrolysis temperature，water dosage，hydrolysis time and drying temperature affected the dispersion index of the product，and the effect of hydrolysis temperature and water dosage were more obvious.The increase of hydrolysis temperature was beneficial to the growth of pseudo-boehmite crystal，and the peptizing property of products at low temperature was poor.With the increase of water dosage，the crystal form of the product was continuously improved，from the initial amorphous form to the pseudo-boehmite phase，respectively crystalline rises and the dispersion index of the product increased accordingly.Prolonging the hydrolysis time was beneficial to the grain growth of pseudo-boehmite and the increase of dispersion index.And the drying temperature had less effect on the crystallization and dispersion index.The optimal hydrolysis conditions were obtained as follows：the molar ratio of aluminum sec-butoxide to water was 1∶4.0，the hydrolysis stirring time was 2 h，and the hydrolysis temperature and drying temperature were 110 ℃.In order to further improve the dispersion index index of the product，hydration of the hydrolyzed product was used to optimize the dispersion index up to 99.6%.At the same time，other technical parameters of the optimized product were comparable with SB powder.This study provided a research basis for the industrialization of the preparation of pseudo-boehmite by the hydrolysis of aluminium sec-butoxide.
| 1 | 朱洪法.催化剂载体制备及应用技术［M］.2版.北京：石油工业出版社，2014. |
| 1 | ZHU Hongfa.Preparation and application technology of catalyst support［M］.2nd ed.Beijing：Petroleum Industry Press，2014. |
| 2 | 于海斌，崔晓萌，孙彦民，等.前驱体合成方法对γ-氧化铝性质的影响研究［J］.无机盐工业，2017，49（1）：52-55. |
| 2 | YU Haibin， CUI Xiaomeng， SUN Yanmin，et al.Effects of precursor synthesis methods on properties of γ-Al2O3 ［J］.Inorganic Che- |
| 2 | Industry micals，2017，49（1）：52-55. |
| 3 | 左少卿，熊晓云，许勐，等.拟薄水铝石胶溶性影响因素的研究进展［J］.应用化工，2018，47（6）：1250-1253. |
| 3 | ZUO Shaoqing， XIONG Xiaoyun， XU Meng，et al.Research progress of the factors to impact the dispersion of pseudo-boehmite［J］.Applied Chemical Industry，2018，47（6）：1250-1253. |
| 4 | 刘建良，马爱增，潘锦程，等.拟薄水铝石路径热油柱成型制备毫米级氧化铝小球的研究［J］.石油炼制与化工，2019，50（5）：1-5. |
| 4 | LIU Jianliang， MA Aizeng， PAN Jincheng，et al.Study on preparation of millimeter-sized alumina pellets by hot oil-drop method with pseudo-boehmite［J］.Petroleum Processing and Petrochemicals，2019，50（5）：1-5. |
| 5 | 杨文建，孟广莹，李晓云，等.球形氧化铝的制备及其在丙烷脱氢催化剂中的应用［J］.无机盐工业，2020，52（6）：87-91. |
| 5 | YANG Wenjian， MENG Guangying， LI Xiaoyun，et al.Preparation of spherical alumina and its application in PDH［J］.Inorganic Chemicals Industry，2020，52（6）：87-91. |
| 6 | 孟广莹，于海斌，杨文建，等.水柱成型法制备重整载体［J］.无机盐工业，2016，48（6）：71-74. |
| 6 | MENG Guangying， YU Haibin， YANG Wenjian，et al.Preparation of reforming support by water column forming method［J］.Inorganic Chemicals Industry，2016，48（6）：71-74. |
| 7 | 左少卿，杜晓辉，熊晓云，等.拟薄水铝石制备方法的研究进展［J］.应用化工，2017，46（9）：1818-1821. |
| 7 | ZUO Shaoqing， DU Xiaohui， XIONG Xiaoyun，et al.Research progress in preparation of pseudo-boehmite［J］.Applied Chemical Industry，2017，46（9）：1818-1821. |
| 8 | MUSI? S， DRAG?EVI? ?， POPOVI? S.Hydrothermal crystallization of boehmite from freshly precipitated aluminium hydroxide［J］.Materials Letters，1999，40（6）：269-274. |
| 9 | LEE H W， PARK B K， TIAN M Y，et al.Relationship between properties of pseudo-boehmite and its synthetic conditions［J］.Jo- |
| 9 | urnal of Industrial and Engineering Chemistry，2006，12（2）：295-300. |
| 10 | VAN GARDEREN N， CLEMENS F J， ANEZIRIS C G，et al.Improved γ-alumina support based pseudo-boehmite shaped by mi- |
| 10 | cro-extrusion process for oxygen carrier support application［J］.Ceramics International，2012，38（7）：5481-5492. |
| 11 | 凯·德林，安德烈埃·布拉施.具有高α-转化温度的勃姆石氧化铝的制备方法：中国，1823009A［P］.2006-08-23. |
| 11 | DOELLING K， BRASCH A.Preparation method of boehmitic aluminas with high α-conversion temperature：CN，1823009A［P］.2006-08-23. |
| 12 | 段启伟，戴隆秀，江燮卿，等.由烷氧基铝制备催化剂载体氧化铝［J］.石油炼制与化工，1994，25（3）：1-3. |
| 12 | DUAN Qiwei， DAI Longxiu， JIANG Xieqing，et al.Production of alumina as catalyst support from aluminium alkoxide［J］.Petroleum Processing and Petrochemicals，1994，25（3）：1-3. |
| 13 | 宁桂玲，林源，丛昱，等.两步水解制取氧化铝纳米微粉的研究［J］.仪器仪表学报，1995，16（S1）：314-318. |
| 13 | NING Guiling， LIN Yuan， CONG Yu，et al.Preparatlon of ultrafine Al2O3 particles by two-step hydrolysis of Al（OC3H7）3 using sol-gel technigue［J］.Chinese Journal of Scientific Instrument，1995，16（S1）：314-318. |
| 14 | 宁桂玲，田朋，田俊英，等.一种制备高纯度拟薄水铝石的方法：中国，104192880A［P］.2014-12-10. |
| 14 | NING Guiling， TIAN Peng， TIAN Junying，et al.A method for preparing high purity pseudoboehmite：CN，104192880A［P］.2014-12-10. |
| 15 | 陈军军.异丙醇铝的水解过程及其水热产物的煅烧过程分析［D］.大连：大连交通大学，2014. |
| 15 | CHEN Junjun.Hydrolysis kinetic of aluminum isopropoxide and the effects of hydrothermal process on properties of product［D］.Dalian：Dalian Jiaotong University，2014. |
| 16 | 王晶.金属醇盐法高纯氧化铝制备工艺及性能［M］.北京：冶金工业出版社，2015. |
| 16 | WANG Jing.Preparation process and properties of high-purity alumina by metal alkoxide method［M］.Beijing：Metallurgical Industry Press，2015. |
| 17 | 吕振辉，薛冬，佟佳，等.异丙醇铝制备拟薄水铝石和氧化铝［J］.石油化工，2017，46（5）：536-542. |
| 17 | Zhenhui Lü， XUE Dong， TONG Jia，et al.Preparation of pseudoboehmite and alumina through the hydrolysis of aluminium isopropoxide［J］.Petrochemical Technology，2017，46（5）：536-542. |
| 18 | 佟佳，吕振辉，薛冬，等.异丙醇铝水解制备氧化铝研究［J］.当代化工，2017，46（9）：1803-1806，1810. |
| 18 | TONG Jia， LV Zhenhui， XUE Dong，et al.Study on synthesis of alumina through hydrolysis of aluminum isopropoxide［J］.Contemporary Chemical Industry，2017，46（9）：1803-1806，1810. |
| 19 | 沈善文.可控制备高纯介孔氧化铝及其甲烷化催化应用［D］.大连：大连理工大学，2017. |
| 19 | SHEN Shanwen.Controllable fabrication of high-purity mesoporous alumina and its methanation application［D］.Dalian：Dalian University of Technology，2017. |
| 20 | 刘袁李.异丙醇铝水解制备催化用拟薄水铝石和氧化铝［D］.大连：大连理工大学，2020. |
| 20 | LIU Yuanli.Synthesis of catalysis pseudobohmite and alumina from aluminium isopropoxide［D］.Dalian：Dalian University of Technology，2020. |
| 21 | 孟广莹，于海斌，王康，等.海藻酸辅助制备氧化铝小球过程的影响因素研究［J］.化学工程，2015，43（12）：1-5. |
| 21 | MENG Guangying， YU Haibin， WANG Kang，et al.Influencing factors of spherical alumina prepared by alginate method［J］.Chemical Engineering（China），2015，43（12）：1-5. |
| 22 | 苗壮，史建公，郝建薇，等.拟薄水铝石的胶溶性与结构的关系［J］.石油学报：石油加工，2016，32（3）：493-500. |
| 22 | MIAO Zhuang， SHI Jiangong， HAO Jianwei，et al.Relationship between peptization and structure of pseudo-boehmite［J］.Acta Petrolei Sinica：Petroleum Processing Section，2016，32（3）：493-500. |
| 23 | LIU Pengchao， ZHU Yizheng， MA Jinghong，et al.Effect of boeh- |
| 23 | mite sol on the crystallization behavior and densification of mullite formed from a sol-gel precursor［J］.Progress in Natural Science：Materials International，2013，23（2）：145-151. |
| 24 | 黄树楷，辛秀兰，徐宝财.拟薄水铝石胶溶机理的探究［J］.工业催化，2017，25（12）：55-59. |
| 24 | HUANG Shukai， XIN Xiulan， XU Baocai.Study on the peptization mechanism of pseudo-boehmite［J］.Industrial Catalysis，2017， |
| 24 | 25（12）：55-59. |
| 25 | 张欣，陈建章，谢文.拟薄水铝石中水的存在形式及对其溶胶性能的影响［J］.人工晶体学报，2018，47（5）：996-999. |
| 25 | ZHANG Xin， CHEN Jianzhang， XIE Wen.Water states and its effect on the peptizing properties of the pseudo-boehmite［J］.Journal of Synthetic Crystals，2018，47（5）：996-999. |
/
| 〈 |
|
〉 |
