共沸回流法制备α-半水石膏工艺研究
收稿日期: 2021-10-08
网络出版日期: 2022-07-14
基金资助
工信部产业技术基础公共服务平台(2020-0107-3-1)
Study on process of preparing α-hemihydrate gypsum by azeotropic reflux method
Received date: 2021-10-08
Online published: 2022-07-14
为消除副产石膏对环境的危害,提高副产石膏的利用价值,采用共沸回流法以工业废酸石膏为原料,经过浆料配制、投加共沸溶剂、转晶反应以及抽滤烘干得到α-半水石膏,并对α-半水石膏的最佳合成工艺进行了探究。通过X射线衍射仪(XRD)、扫描电镜(SEM)对产物进行表征。重点研究了共沸溶剂浓度、温度、固液比、pH对副产石膏的转晶过程、转晶产物组成及结构的影响,并通过单因素实验以及正交实验得到最佳实验条件。结果表明:在共沸溶剂体积分数为70%、转晶温度为120 ℃、固液质量比为1∶6、pH为5、反应时间为3 h时可以制得长径比约为1∶1、抗折强度(2 h)为5.6 MPa、烘干抗压强度为43 MPa的α-半水石膏,满足JC/T 2038—2010《α型高强石膏》α40强度等级。
徐成 , 沈介发 , 郝宇宁 , 吴炳辉 , 马晓明 , 刘建武 , 严生虎 , 张跃 . 共沸回流法制备α-半水石膏工艺研究[J]. 无机盐工业, 2022 , 54(7) : 117 -123 . DOI: 10.19964/j.issn.1006-4990.2021-0597
In order to eliminate the harm of by-product gypsum to the environment and improve the utilization value of by-product gypsum,the azeotropic reflux method was used to take industrial waste acid gypsum as raw material to obtain α-hemihydrate gypsum through slurry preparation,azeotropic solvent addition,crystal conversion reaction,and suction drying,and the best synthesis process of α-hemihydrate gypsum was explored.The product was characterized by X-ray diffractometer(XRD) and scanning electron microscope(SEM).The effects of azeotropic solvent concentration,temperature,solid-liquid ratio,and pH on the conversion process of by-product gypsum,the composition and structure of the conversion product were mainly researched,and the best experimental conditions were obtained through single-factor experiments and orthogonal experiments.The results showed that when the concentration of azeotropic solvent was 70%,the crystal transition temperature was 120 ℃,the solid-to-liquid ratio was 1∶6,the pH was 5,and the reaction time was 3 h,the aspect ratio could be about 1∶1,and flexural resistance could be obtained.The α-hemihydrate gypsum with a strength(2 h) of 5.6 MPa and a drying compressive strength of 43 MPa met the α40 strength grade of JC/T 2038—2010“α-type high-strength gypsum”.
1 | 崔玉民,殷榕灿.染料废水处理方法研究进展[J].科技导报,2021,39(18):79-87. |
1 | CUI Yumin, YIN Rongcan.The progress of treatment methods of dye wastewater[J].Science & Technology Review,2021,39(18):79-87. |
2 | 李崇,周俊,刘瑶,等.我国废硫酸产生及综合利用现状[J].过程工程学报,2018,18(S1):24-34. |
2 | LI Chong, ZHOU Jun, LIU Yao,et al.Emission and comprehensive utilization of spent sulfuric acid in China[J].The Chinese Journal of Process Engineering,2018,18(S1):24-34. |
3 | 卢静昭,赵斌,陈学青,等.利用脱硫石膏制备高品质二水石膏[J].人工晶体学报,2016,45(1):97-103. |
3 | LU Jingzhao, ZHAO Bin, CHEN Xueqing,et al.Preparation of the high-quality gypsum by dihydrate FGD[J].Journal of Synthetic Crystals,2016,45(1):97-103. |
4 | 杨林,张冰,周杰,等.磷石膏制备α型高强石膏及其转化过程研究[J].建筑材料学报,2014,17(1):147-152. |
4 | YANG Lin, ZHANG Bing, ZHOU Jie,et al.Preparation of α-high strength gypsum using phosphogypsum and transformation of phosphogypsum to α-high strength gypsum[J].Journal of Building Materials,2014,17(1):147-152. |
5 | 汪潇,曹博伦,金彪,等.添加剂调控半水石膏晶体生长研究进展[J].硅酸盐学报,2020,48(1):94-103. |
5 | WANG Xiao, CAO Bolun, JIN Biao,et al.Using additives to control crystal growth of hemihydrate gypsum-A short review[J].Journal of the Chinese Ceramic Society,2020,48(1):94-103. |
6 | 胡成,向玮衡,陈平,等.丁二酸对水热合成α-半水脱硫石膏微晶形貌及力学强度的影响[J].无机盐工业,2021,53(4):76-80. |
6 | HU Cheng, XIANG Weiheng, CHEN Ping,et al.Effects of succinic acid on crystallite morphology and mechanical strength of α-hemihydrate desulfurized gypsum synthesized by hydrothermal method[J].Inorganic Chemicals Industry,2021,53(4):76-80. |
7 | LU Wenda, MA Baoguo, SU Ying,et al.Preparation of α-hemihydrate gypsum from phosphogypsum in recycling CaCl2 solution[J].Construction and Building Materials,2019,214:399-412. |
8 | 陈平,田宇,胡成.盐溶液种类和浓度对α-半水脱硫石膏合成的影响[J].无机盐工业,2020,52(10):130-134. |
8 | CHEN Ping, TIAN Yu, HU Cheng.Effect of type and concentration of salt solution on synthesis of α-semi-water desulfurization gypsum[J].Inorganic Chemicals Industry,2020,52(10):130-134. |
9 | LUO Zhao, HAN Fenglan, HUANG Xinhua.Alpha hemihydrate gypsum preparationed by atmospheric pressure salt solution method |
9 | process route[J].Applied Mechanics and Materials,2013,327:23-27. |
10 | 桂苗苗,丛钢.脱硫石膏蒸压法制α半水石膏的研究[J].重庆建筑大学学报,2001,23(1):62-65,81. |
10 | GUI Miaomiao, CONG Gang.Study on the α-hemihydrate gypsum made by desulphogypsum through autoclave process[J].Journal of Chongqing Jianzhu University,2001,23(1):62-65,81 |
11 | 罗东燕,邱树恒,陈霏,等.用蒸压法将磷石膏制备α半水石膏的研究[J].新型建筑材料,2015,42(9):23-26,46. |
11 | LUO Dongyan, QIU Shuheng, CHEN Fei,et al.Preparation of alpha hemihydrate gypsum from phosphogypsum by autoclave met- |
11 | hod[J].New Building Materials,2015,42(9):23-26,46. |
12 | 彭家惠,瞿金东,张建新,等.EDTA吸附特性及其对α半水脱硫石膏晶形的影响[J].材料研究学报,2011,25(6):566-572. |
12 | PENG Jiahui, QU Jindong, ZHANG Jianxin,et al.Adsorption characteristics of EDTA on α-hemihydrate desulfurization gypsum surface and its influence on crystal morphology[J].Chinese Journal of Materials Research,2011,25(6):566-572. |
13 | LIU Xianfeng, PENG Jiahui, ZHANG Jianxin,et al.Effect of organic diacid carbon chain length on crystal morphology of α-calcium sulfate hemihydrate in preparation from flue gas desulphurization gypsum[J].Applied Mechanics and Materials,2012, |
13 | 253-255:542-545. |
14 | SHAO Duoduo, ZHAO Bin, GAO Lili,et al.Preparation of whitening dihydrate gypsum and short columnar α-hemihydrate gypsum with FGD gypsum[J].Crystal Research and Technology,2017,52(9).Doi:10.1002/crat.201700166 . |
15 | SUN Xiangbin, ZHANG Genlei, CUI Peng.Aspect ratio-controlled |
15 | preparation of α-CaSO 4·0.5 H2O from phosphogypsum in potassium tartrate aqueous solution[J].RSC Advances,2019,9(38):21601-21607. |
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