对叔丁基苄硫醇的合成与浮选机理研究
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摘要
采用黄药与对叔丁基苄氯酯化反应生成黄原酸酯,再用乙胺氨解,得到硫氨酯和对叔丁基苄硫醇。考察了温度、酯化时间、氨解时间、黄药摩尔比、乙胺摩尔比对反应的影响。结果表明,在常温下酯化4 h、氨解2 h、黄药和乙胺与对叔丁基苄氯摩尔比为1. 1∶1. 1∶1为最佳条件。并通过单矿物浮选实验、吸附量测定实验、接触角测定、红外光谱分析、XPS分析等手段,对对叔丁基苄硫醇捕收剂进行了浮选性能和浮选机理的研究,结果表明,对叔丁基苄硫醇在矿物表面发生了化学吸附。
The esterification of xanthate with( 4-( tert-butyl) phenyl) chloride to give xanthogenate,and then ethylamine solution is added to give the thionocarbamates and 4-tert-butylbenzyl mercaptan. The effects of temperature,esterification time,ammonolysis time,xanthate molar ratio,and ethylamine molar ratio on the reaction were researched. The results showed that under the optimum conditions of esterification at room temperature for 4 h and ammonolysis for 2 h,the molar ratio of xanthate and ethylamine to( 4-( tert-butyl) phenyl) chloride was 1. 1∶ 1. 1∶ 1. The flotation performance and flotation mechanism of 4-tertbutylbenzyl mercaptan collector were studied by means of single mineral flotation experiment,adsorption amount measurement experiment,contact angle measurement,spectrum analysis and XPS analysis. The results show that 4-tert-butylbenzyl mercaptan chemisorbed on the mineral surface.
The esterification of xanthate with( 4-( tert-butyl) phenyl) chloride to give xanthogenate,and then ethylamine solution is added to give the thionocarbamates and 4-tert-butylbenzyl mercaptan. The effects of temperature,esterification time,ammonolysis time,xanthate molar ratio,and ethylamine molar ratio on the reaction were researched. The results showed that under the optimum conditions of esterification at room temperature for 4 h and ammonolysis for 2 h,the molar ratio of xanthate and ethylamine to( 4-( tert-butyl) phenyl) chloride was 1. 1∶ 1. 1∶ 1. The flotation performance and flotation mechanism of 4-tertbutylbenzyl mercaptan collector were studied by means of single mineral flotation experiment,adsorption amount measurement experiment,contact angle measurement,spectrum analysis and XPS analysis. The results show that 4-tert-butylbenzyl mercaptan chemisorbed on the mineral surface.
引文
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[17] Liu S,Zhong H,Liu G,et al. Cu(I)/Cu(II)mixed-valence surface complexes of S-[(2-hydroxyamino)-2-oxoethyl]-N,N-dibutyldithiocarbamate:Hydrophobic mechanism to malachite flotation[J]. Journal of Colloid and Interface Science,2018,512:701-712.
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[3] Mikhlin Y,Karacharov A,Tomashevich Y,et al. Cryogenic XPS study of fast-frozen sulfide minerals:Flotation-related adsorption of n-butyl xanthate and beyond[J]. Journal of Electron Spectroscopy&Related Phenomena,2016,206(22):65-73.
[4] Zhang X,Qian Z,Zheng G,et al. The design of a macromolecular depressant for galena based on DFT studies and its application[J]. Minerals Engineering,2017,112:50-56.
[5] Ma X,Hu Y,Zhong H,et al. A novel surfactant S-benzoylN,N-diethyldithiocarbamate synthesis and its flotation performance to galena[J]. Applied Surface Science,2016,365:342-351.
[6] Zhao G,Peng J,Zhong H,et al. Synthesis of novel ether thionocarbamates and study on their flotation performance for chalcopyrite[J]. Minerals,2016,6(3):97-112.
[7]王彦军,刘学勇,张平军.新型硫化矿捕收剂烯丙基硫氨酯合成与选矿应用研究[J].矿业工程,2016,14(6):33-37.
[8]刘广义,任恒,詹金华,等. 3,3'-二乙基-1,1'-一缩二乙二醇二羰基双硫脲的合成、表征与性能[J].中国有色金属学报,2013,23(1):290-296.
[9] L Guangyi,Hong Z,X Liuyin,et al. Improving copper flotation recovery from a refractory copper porphyry ore by using ethoxycarbonyl thiourea as a collector[J]. Minerals Engineering,2011,24(8):817-824.
[10]储春利,蒋中刚,唐道文.难浸金矿硫脲浸出试验研究[J].有色金属(冶炼部分),2014(3):37-39.
[11] Long X,Chen Y,Chen J,et al. The effect of water molecules on the thiol collector interaction on the galena(Pb S)and sphalerite(Zn S)surfaces:A DFT study[J]. Applied Surface Science,2016,389:103-111.
[12] Roy S,Datta A,Rehani S. Flotation of copper sulphide from copper smelter slag using multiple collectors and their mixtures[J]. International Journal of Mineral Processing,2015,143:43-49.
[13]张珍明.高纯度对叔丁基苄硫醇的合成[J].化工时刊,2000(7):42-44.
[14]王倩,王崇磊,崔波,等.对叔丁基苄硫醇的新工艺研究[J].化学与黏合,2013,35(5):62-66.
[15] Ricci A,Buuhoi N P. Odour and chemical constitution of some structural analogues of tertbutylated 1-tetralones[J]. Bulletin De La Societe Chimique De France,1967(10):3634-3636.
[16]李述文,范如霖.实用有机化学手册[M].上海:上海科学技术出版社,1981.
[17] Liu S,Zhong H,Liu G,et al. Cu(I)/Cu(II)mixed-valence surface complexes of S-[(2-hydroxyamino)-2-oxoethyl]-N,N-dibutyldithiocarbamate:Hydrophobic mechanism to malachite flotation[J]. Journal of Colloid and Interface Science,2018,512:701-712.