常压盐溶液-丁二酸转晶体系中pH对α-CaSO4·0.5H2O的影响
收稿日期: 2019-07-18
网络出版日期: 2020-02-26
Effect of pH on α-CaSO4·0.5H2O in salt solution at atmospheric pressure-succinic acid crystal transfer system
Received date: 2019-07-18
Online published: 2020-02-26
以磷石膏为原料,丁二酸为转晶剂,采用常压盐溶液法制备α-CaSO4·0.5H2O的体系中,在温度为103 ℃、反应时间为3 h、丁二酸掺量为0.05%(质量分数)、氯化钠质量分数为15%的条件下研究pH对制备α-CaSO4·0.5H2O的影响。结果表明:当pH为7.0~9.0时,可以得到长径比为1∶1~3∶1的短柱状α-CaSO4·0.5H2O晶体。FT-IR和XPS表征结果显示,合适的pH条件下,丁二酸电离出适量的羧酸根离子吸附于α-CaSO4·0.5H2O晶体晶面上与钙离子络合,减缓了α-CaSO4·0.5H2O晶体在晶面上的生长速度,减小了晶体长径比。XRD和TEM表征结果证实,羧酸根离子吸附于α-CaSO4·0.5H2O晶体的(204)晶面上与钙离子络合。
关键词: 磷石膏; α-CaSO4·0.5H2O; 丁二酸; 常压盐溶液法
丁峰 , 窦焰 , 郑之银 , 刘荣 , 崔鹏 . 常压盐溶液-丁二酸转晶体系中pH对α-CaSO4·0.5H2O的影响[J]. 无机盐工业, 2020 , 52(1) : 82 -86 . DOI: 10.11962/1006-4990.2019-0096
α-CaSO4·0.5H2O was prepared with phosphogypsum as raw material and succinic acid as crystal transfer by salt solution at atmospheric pressure.The effect of pH on the preparation of α-CaSO4·0.5H2O was studied under the conditions of reaction temperature of 103 ℃,reaction time of 3 h,mass fraction of succinic acid of 0.05% and mass fraction of sodium chloride of 15%.Results showed when the pH was at 7.0~9.0,the short columnar α-CaSO4·0.5H2O crystals that the aspect ratio between 1∶1~3∶1 was obtained.The results of FT-IR and XPS showed that the range of succinic acid ionization out just the right amount of carboxylic acid root complexing adsorption on the Ca 2+ of α-CaSO4·0.5H2O crystal surface when the system was in an appropriate pH range,the growth velocity of the crystal suface was slowed down and the aspect ratio of the crystal was reduced.XRD and TEM characterization results confirmed that carboxylic acid ions were complexated and adsorbed on the(204) crystal surface of α-CaSO4·0.5H2O crystal.
[1] | 刘红霞 . 常压盐溶液法α-半水脱硫石膏的制备及晶形调控研究[D]. 重庆:重庆大学, 2010. |
[2] | Wu X Q, Tong S T, Guan B H , et al. Transformation of flue-gas-de-sulfurization gypsum to α-hemihydrated gypsum in salt solution at atmospheric pressure[J]. Chinese Journal of Chemical Engineering, 2011,19(2):349-355. |
[3] | 彭家惠, 张建新, 瞿金东 , 等. 有机酸对α-半水脱硫石膏晶体生长习性的影响与调晶机理[J]. 硅酸盐学报, 2011,39(10):1711-1718. |
[4] | 沈卓贤 . 脱硫石膏在常压盐溶液中制备α-半水石膏的转晶剂作用研究[D]. 杭州:浙江大学, 2008. |
[5] | Mi Y, Chen D, Wang S . Utilization of phosphogypsum for the preparation of α-calcium sulfate hemihydrate in chloride-free solution under atmospheric pressure[J]. Journal of Chemical Technology & Biotechnology, 2018,93(8):2371-2379. |
[6] | Li F, Liu J, Yang G , et al. Effect of pH and succinic acid on the morphology of α-calcium sulfate hemihydrate synthesized by a salt solution method[J]. Journal of Crystal Growth, 2013,374:31-36. |
[7] | Pan Z, Lou Y, Yang G , et al. Preparation of calcium sulfate dehydrate and calcium sulfate hemihydrate with controllable crystal morphology by using ethanol additive[J]. Ceramics International, 2013,39(5):5495-5502. |
[8] | Zhao W, Gao C, Zhang G , et al. Controlling the morphology of calcium sulfate hemihydrate using aluminum chloride as a habit modifier[J]. New Journal of Chemistry, 2016,40(4):3104-3108. |
[9] | Duan Z, Li J, Li T , et al. Influence of crystal modifier on the preparation of α-hemihydrate gypsum from phosphogypsum[J]. Construction & Building Materials, 2017,133:323-329. |
[10] | 方羊, 窦焰, 孙祥斌 , 等. Al 3+对水热法制备α-CaSO4·0.5H2O晶须的影响 [J]. 高校化学工程学报, 2017,31(2):413-419. |
[11] | Zhang X, Wang J, Wu J , et al. Phase-and morphology-controlled crystallization of gypsum by using flue-gas-desulfurization gypsum solid waste[J]. Journal of Alloys and Compounds, 2016,674:200-206. |
[12] | Guan B, Jiang G, Wu Z , et al. Preparation of α-calcium sulfate hemihydrate from calcium sulfate dihydrate in methanol-water solution under mild conditions[J]. Journal of the American Ceramic Society, 2011,94(10):3261-3266. |
[13] | 栾扬, 赵志曼, 全思臣 , 等. 基于密度泛函理论研究磷建筑石膏晶体表面吸附丁二酸转晶机理[J]. 材料导报, 2018,32(12):2118-2123. |
[14] | Wu X Q, Tong S T, Guan B H , et al. Transformation of flue-gas-de-sulfurization gypsum to α-hemihydrated gypsum in salt solution at atmospheric pressure[J]. Chinese Journal of Chemical Engineering, 2011,19(2):349-355. |
[15] | Tan H, Dong F . Morphological regulation of calcium sulfate hemihydrate from phosphogypsum[J]. Materialwissenschaft und Werks-tofftechnik, 2017,48(11):1191-1196. |
[16] | Ma B G, Ru X H, Lu S W , et al. Preparation of α-calcium sulfate hemihydrate from phosphogypsum in CaCl2 solution under atmospheric pressure[J]. Advanced Materials Research, 2012,554/555/556(7):570-574. |
/
〈 |
|
〉 |