CN104307641B - 一种氨基三唑硫酮类捕收剂的应用 - Google Patents
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Abstract
本发明公开了一种氨基三唑硫酮类捕收剂的应用,该应用是将氨基三唑硫酮类化合物作为矿物浮选捕收剂应用于从含铜、银或金矿物的矿石中浮选回收有价金属,该氨基三唑硫酮类捕收剂相对现有技术中的常用浮选捕收剂能有效改善铜、银或金矿物的富集和回收能力。
Description
技术领域
本发明涉及一种氨基三唑硫酮类捕收剂的应用,属于金属选矿领域。
背景技术
氨基三唑硫酮类化合物及其衍生物具有良好的杀菌、抑菌、调节植物生长、螯合金属等性质。在生物医药领域,此类化合物用于消炎、镇静、抗焦虑、抗微生物、抗真菌;在农业领域,用作高效低毒的除草剂、杀虫剂和植物生长调节剂;在防腐领域,其用作金属缓蚀剂。
Jack和Ned以3-酰胺基二硫代氨基甲酸钾为原料对氨基三唑硫酮的三种合成方法进行了研究(Jack R.Reid,Ned D.Heindel.Improved syntheses of 5-substituted-4-amino-3-mercapto-(4H)-1,2,4-triazoles[J].Heterocyclic Chem,13,925(1976))。Beyer和Kroger用脂肪酸与二氨基硫脲在回流或熔融条件下反应制得烷基三唑硫酮(BeyerH.,Kroger,C.F.Liebigs Ann.Chem.1960,637,135),该方法合成过程简单,收率最高可达到87%。Romualdas等人用熔点低的酯类代替羧酸与二氨基硫脲反应,制得烷基三唑硫酮,收率最高为78%(Smicius R,Burbuliene M M,Jakubkiene V,et al.Convenient way to5-substituted 4-amino-2,3-dihydro-4H-1,2,4-triazole-3-thiones[J].Journal ofheterocyclic chemistry,2007,44(2):279-284)。
Jaap评述了金属与1,2,4-三唑配体的单、寡和多核螯合物(JaapG.Haasnoot.Mononuclear,oligonuclear and polynuclear metal coordinationcompounds with1,2,4-triazole derivatives as ligands[J].Coordination Chemistryreviews.200-202(2000)131-185)。Robert等报道了Mn、Fe、Co和Ni金属原子与3-甲基-4-氨基-1,2,4-三唑-5-硫酮中的S原子和N原子结合形成含高氯酸根或硝酸根的双五元环结构(如式3),而Cu原子的螯合物尽管与Mn和Fe原子的相似,但所有的原子都是反式的,给电子基团相对于基底都是顺式排列形成平面结构(如式4)(Robert W.Clark,PhilipJ.Squattrito,Ashok K.Sen,Surendra N.Dubey,et al.Structural trends in a seriesof divalent transition metal triazole complexes[j].Inorganica Chimica Acta293(1999)61–69)。Yi等人报道了烷基三唑硫酮-镉金属螯合物的一维、二维及三维单晶结构,并认为Cd属于交界酸,可与N或S或与两者同时配位(Long Yi,Bin Ding,Bin Zhao,PengCheng,Dai-Zheng Liao,Shi-Ping Yan,and Zonghui Jiang.Novel Triazole-BridgedCadmium Coordination Polymers Varying from Zero-to Three-dimensionality[J].Inorg.Chem.2004,43,33-43)。
Liu等研究了3-烷基-4-氨基-5-巯基-1,2,4-三唑在铁表面吸附行为及其防腐性能(Xiuyu Liu,Shenhao Chen,Hongyan Zhai,Lixia Shen,Juanjuan Z hou,Ling Wu.Thestudy of self-assembled films of triazole on iron electrodes usingelectrochemical methods,XPS,SEM and molecular simulation[J].Electrochemitrycommunications 9(2007)813-819)。王鹏研究了3-十一烷基-4-氨基-5-巯基-1,2,4-三唑在铜币表面的吸附机理及其防腐性能,认为氨基三唑硫酮通过π(C=N)键和S原子的p轨道与铜的d轨道成键(王鹏.铜质币腐蚀变色机理及抗变色工艺研究[D].大连:大连理工大学,2009)。
目前,现有技术中并没有关于氨基三唑硫酮类杂环化合物用作浮选捕收剂的报道,
发明内容
本发明的目的是在于提供一种氨基三唑硫酮类捕收剂在金属矿物浮选方面的应用,该氨基三唑硫酮类化合物能有效提高含铜、银或金矿物的矿石中有价金属的富集和回收效率。
本发明提供了一种氨基三唑硫酮类浮选捕收剂的应用,该应用是将具有式1结构的氨基三唑硫酮类化合物应用于从含铜、银或金矿物的矿石中浮选回收有价金属;
其中,
R为C1~C17的烷烃基、或者为C2~C17的烯烃基,或者为具有式2结构的烷氧醚基;
R1为亚乙基或亚丙基,n为1~10;
R2为C3~C17的烷烃基、或者为C2~C17的烯烃基。
本发明的氨基三唑硫酮类化合物的应用还包括以下优选方案:
R优选为C1~C17的直链烷烃基,或C5~C7的环烷基,或C10~C17单烯烃基。
R1优选为亚乙基,n为2~9。
R2优选为C3~C17的直链烷烃基、或者为C10~C17的单烯烃基。
最优选的氨基三唑硫酮类化合物中R为甲基、乙基、丙基、戊基、己基、环己基、庚基、壬基,正十一烷基、正十三烷基、正十五烷基、正十七烷基或8-十七烯基;n为2~6;R2为丙基、戊基、己基、庚基、壬基,正十一烷基、正十三烷基、正十五烷基、正十七烷基或8-十七烯基。
本发明的氨基三唑硫酮类化合物可通过相应的有机羧酸与二氨基硫脲在回流或熔融条件下反应而制得。
本发明的有益效果:本发明首次将氨基三唑硫酮类化合物应用于矿物中的有价金属浮选捕收,特别适用于含铜、银或金矿物的矿石中有价金属的富集和回收,相对于现有的常用捕收剂能提高有价金属回收率。
具体实施方式
以下实施例旨在进一步说明本发明内容,而不是对本发明的保护范围的限定。
实施例中所有的份数和百分数除另有规定外均指质量。实施例中对矿物的浮选捕收过程都是常规过程,只是采用本发明的氨基三唑硫酮类化合物替换常规捕收剂。以下实施例中采用的氨基三唑硫酮类化合物都采用现有技术中的常规方法制备得到,通过相应的有机羧酸与二氨基硫脲在回流或熔融条件下反应而制得。实施例1
在3-己基-4-氨基-1,2,4-三唑-5-硫酮浓度为5×10-5mol/L,矿浆pH为7.3,起泡剂甲基异丁基甲醇(MIBC)的浓度为15mg/L,N2气流速为200mL/min,对粒径为-0.076mm~+0.038mm的黄铜矿浮选3分钟,此时黄铜矿的浮选回收率达到97.9%。
实施例2
在3-己基-4-氨基-1,2,4-三唑-5-硫酮浓度为3×10-4mol/L,矿浆pH为8.2,起泡剂MIBC的浓度为15mg/L,N2气流速为200mL/min,对粒径为-0.076mm~+0.038mm的孔雀石浮选3分钟,此时孔雀石的浮选回收率为99.5%。
实施例3
新疆某氧化-硫化铜矿样,原矿含Cu 0.91%,其中氧化铜含量0.52%,硫化铜含量0.39%。试验流程:一次粗选一次扫选。磨矿细度:-0.074mm80%;药剂条件:粗选硫化钠1200克/吨,扫选硫化钠200克/吨,其余药剂条件及其结果见表1。表1的试验结果表明,3-烷基-4-氨基-1,2,4-三唑-5-硫酮捕收剂取得了比丁黄药、辛基羟肟酸和丁黄药+辛基羟肟酸更高的铜回收率和铜品位(粗精矿)。
表1 3-烷基-4-氨基-1,2,4-三唑-5-硫酮捕收剂浮选氧化-硫化铜矿石试验结果
实施例4
江西某斑岩铜矿石矿样,原矿含铜0.41%,含硫1.81%,含金0.16g/t。试验流程:一次粗选;磨矿细度:-0.074mm占65%;药剂条件:石灰用量800克/吨,矿浆pH值为8.0,其余药剂条件及其结果见表2。表2的试验结果表明,本发明的3-烷基-4-氨基-1,2,4-三唑-5-硫酮捕收剂取得比常用捕收剂戊黄药更高的铜、金浮选回收率。
表2 3-烷基-4-氨基-1,2,4-三唑-5-硫酮捕收剂浮选斑岩铜矿条件及其结果
*单位g/t
实施例5
四川某冶金铜炉渣样,原矿含铜2.81%。试验流程:一次粗选;磨矿细度:-0.074mm占90%;药剂条件:石灰用量500克/吨,矿浆pH值为7.2,其余药剂条件及其结果见表3。表3的试验结果表明,本发明的3-烃基-4-氨基-1,2,4-三唑-5-硫酮与丁黄药组合使用能取得比常用单独用丁黄药更高的铜浮选回收率。
表3 3-烃基-4-氨基-1,2,4-三唑-5-硫酮捕收剂浮选冶金铜渣条件及其结果
Claims (5)
1.一种氨基三唑硫酮类浮选捕收剂的应用,其特征在于,将具有式1结构的氨基三唑硫酮类化合物应用于从含铜、银或金矿物的矿石中浮选回收有价金属;
其中,
R为C1~C17的烷烃基或C5~C7的环烷基,或者为C2~C17的烯烃基,或者为具有式2结构的烷氧醚基;
R1为亚乙基或亚丙基,n为1~10;
R2为C3~C17的烷烃基、或者为C2~C17的烯烃基。
2.根据权利要求1所述的应用,其特征在于,R为C1~C17的直链烷烃基或C10~C17单烯烃基。
3.根据权利要求1所述的应用,其特征在于,R1为亚乙基,n为2~9。
4.根据权利要求1所述的应用,其特征在于,R2为C3~C17的直链烷烃基、或者为C10~C17的单烯烃基。
5.根据权利要求1~4任一项所述的应用,其特征在于,R为甲基、乙基、丙基、戊基、己基、环己基、庚基、壬基,正十一烷基、正十三烷基、正十五烷基、正十七烷基或8-十七烯基;n为2~6;R2为丙基、戊基、己基、庚基、壬基,正十一烷基、正十三烷基、正十五烷基、正十七烷基或8-十七烯基。
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