新型有机硅阳离子捕收剂的合成及其对铝硅矿物的浮选特性与机理研究
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摘要
针对我国铝土矿反浮选脱硅技术的重大需求,将有机硅基团引入铝硅矿物阳离子捕收剂分子结构中,系统地进行了有机硅阳离子捕收剂的制备及其对铝硅矿物的浮选特性和机理研究。
首先,系统地研究了有机硅捕收剂的合成与表征。以卤代有机硅氧烷与脂肪叔胺为原料、碘化钾为催化剂、无水乙醇为溶剂,一步直接合成了有机硅季铵盐QAS系列捕收剂。在卤代有机硅氧烷、叔胺、碘化钾投料的摩尔配比为1.1:1.0:0.01、反应温度80℃、合成时间37h、通N2保护的条件下,合成产品转化率均达90%以上。采用六甲基二硅氧烷(MM)为封端剂,对氨乙基氨丙基二甲氧基甲基硅烷(TAS100)进行封端处理,制备了有机硅伯胺捕收剂氨乙基氨丙基三硅氧烷(TAS101)。在投料摩尔配比TAS100:MM=1:5、以10%四甲基氢氧化铵溶液为催化剂、通N：保护、恒温90℃搅拌反应8h的条件下,TAS100转化率约达90%。分别以TAS100、TAS101为原料与苄氯反应,当投料的摩尔比TAS100或TAS101：苄氯=1：1.5时,以无水乙醇为溶剂、通N2保护、恒温80℃反应8h,合成了有机硅仲胺苄基氨乙基氨丙基二甲氧基甲基硅烷(TAS550)和苄基氨乙基氨丙基三硅氧烷(QAS550)。采用化学滴定、界面张力测定、红外谱图分析、1HNMR和13CNMR核磁共振测定等分析测试技术对最终产品的结构与性能进行表征,研究表明各目的产品纯度均超过90%。
研究并揭示了有机硅捕收剂的结构与浮选性能的相互关系。研究结果表明,有机硅季铵盐QAS系列捕收剂在广泛pH范围内均是高岭石、叶蜡石、伊利石三种铝硅酸盐矿物的有效捕收剂,QAS系列捕收剂对一水硬铝石的捕收能力随着矿浆pH升高先增加而后急速减小；当pH≥11时,铝硅矿物之间表现出了良好的反浮选分离趋势；该类捕收剂对铝硅矿物的浮选性能随着主碳链的延长而降低；在捕收剂γ-(三乙氧基硅基)丙基十二烷基二甲基氯化铵(QAS222)用量4×10-4 M、NaOH调矿浆pH至11、未添加任何抑制剂的条件下,实现了一水硬铝石和高岭石人工混合矿的反浮选分离。在pH4～10广泛范围内,有机硅伯胺和仲胺捕收剂可显著增强铝硅矿物的可浮性,是铝硅矿物的有效捕收剂；有机硅伯胺TAS101对铝硅矿物的捕收力强于有机硅仲胺TAS550和QAS550；在捕收剂TAS101用量1.0×10-3 M、抑制剂可溶性淀粉500mg/L、Na2CO3调pH=8条件下,成功地进行了一水硬铝石与高岭石矿物的反浮选分离。
针对河南某Al2O3品位63.92%、铝硅比为6.07的一水硬铝石型铝土矿,以γ-(三乙氧基硅基)丙基十二/十四烷基二甲基氯化铵(QAS224)和TAS101为捕收剂,进行反浮选脱硅试验研究。小型闭路试验研究结果表明,当捕收剂γ-(三乙氧基硅基)丙基十二/十四烷基二甲基氯化铵(QAS224)用量700g/t、NaOH调矿浆pH至11,原矿经一次粗选两次精选两次扫选,获得了Al2O3品位67.79%、Al2O3回收率81.72%、A/S为9.67的浮选精矿；当捕收剂TAS101用量720g/t、Na2CO3调矿浆pH至11、可溶性淀粉用量1320g/t时,原矿同样经一次粗选两次精选两次扫选,浮选精矿A/S为9.58,其A1203品位和回收率分别为68.52%、83.34%；当QAS224用量540g/t,TAS101用量180g/t,Na2CO3调矿浆pH至11,可溶性淀粉用量1320g/t时,浮选流程不变,获得了浮选精矿A/S为10.34、Al2O3,品位68.98%、Al2O3回收率85.42%的选别指标,组合捕收剂脱硅效果优于单一用药。各浮选精矿质量均满足拜耳法氧化铝生产工艺给料要求。
研究并揭示了有机硅季铵盐捕收剂QAS222与矿物作用机理。研究结果表明,在矿浆pH=11的碱性条件下,QAS222通过静电物理作用、氢键作用、化学吸附与矿物表面的Si、0、Al等原子作用,使矿物表面产生了更多Si-O-Si、Si-O、Si-O-Al键,从而牢固地吸附于高岭石、叶蜡石和伊利石三种铝硅酸盐矿物表面,使其矿物表面ζ-电位正移、接触角增大、疏水性和可浮性增强,而此时QAS222很难在一水硬铝石矿物表面发生吸附,因此,铝硅矿物表面之间出现了明显的疏水性和可浮性差异,从而实现了铝硅矿物的反浮选分离。
在矿浆广泛pH范围内,TAS101可较好地改善铝硅矿物表面的疏水性和可浮性,淀粉是一水硬铝石矿物的选择性抑制剂；受淀粉抑制后,一水硬铝石矿物很难再吸附捕收剂TAS101,因此可浮性较差；而淀粉基本不影响高岭石、叶蜡石、伊利石的浮选；以TAS101为捕收剂、淀粉为抑制剂,可有效地实现铝硅矿物的浮选分离。机理研究表明,捕收剂TAS101的硅基团起疏水作用,其在一水硬铝石矿物表面主要发生静电物理吸附,而在高岭石、叶蜡石和伊利石矿物表面则发生静电吸附和氢键作用。
To the significant demand of desilication of bauxite ores by reverse flotation in China, a kind of new cationic organosilicon surfactant was developed as collector of aluminosilicate minerals. The synthesis of this collector was studied on, as well as its flotation performance and mechanism on diaspore and aluminosilicate minerals.
Firstly, the organosilicon cationic collectors were synthesized and characterized systematically. The organosilicon quaternary ammonium collectors were obtained by one-step reaction which conducted at 80℃for 37 hours, with halogenated siloxane coupling agent:tertiary aliphatic amine:KI=1.1:1:0.01 by the mole ratio, using anhydrous ethanol as solvent, protected the reaction system with N2. The percent conversion of tertiary aliphatic amine was more than 90%. The organosilicon CH3Si(OSi(CH3)3)2(CH2)3NH(CH2)2NH2(TAS101) collector was synthesized when reaction was conducted at 90℃for 8 hours, with CH3Si(OCH3)2(CH2)3NH(CH2)2NH2(TAS 100):hexamethyldisiloxane (MM)= 1:5 by the mole ratio, using anhydrous ethanol as solvent and 10%(CH3)4NOH solution as activator, protected the reaction system with N2. The percent conversion of TAS100 was about 90%. The CH3Si(OCH3)2(CH2)3NH(CH2)2NHCH2(C6H5)(TAS550) collector was synthesized when reaction was conducted at 80℃for 8 hours, with TAS100:benzyl chloride=1:1.5 by the mole ratio, using anhydrous ethanol as solvent, protected the reaction system with N2. The collector CH3Si[OSi(CH3)3]2(CH2)3NH(CH2)2NHCH2(C6H5)(QAS550) was obtained with TAS101 took the place of TAS100 in the reaction mentioned above. Structures and properties of final products were characterized by FT-IR spectrum,1HNMR and 13CNMR et al. The purity of every new organosilicon collector was more than 90%.
The relationship of molecular structures and flotation performance of collectors were investigated. The results indicated that organosilicon quaternary ammonium was an effective collector of kaolinite, pyrophyllite and illite minerals in a wide pH range, and their collecting ability for diaspore increased firstly and then decreased drastically with the increase of pulp pH, and the optimum pulp pH for the separation of diaspore from kaolinite was around 11. The collecting ability of organosilicon quaternary ammoniums for aluminosilicate minerals receded with the lengthening of backbone in tertiary aliphatic amine. In pH=11 the diaspore was been effectively separated from kaolinite with 4×10-4 M [(C2H5O)3Si(CH2)3N(CH3)2C12H25]Cl(QAS222) as collector. In the wide range of pH=4-10, the collectors of organosilicon primary amine and secondary amine could improve the minerals'floatability remarkably. The collecting ability of primary amine TAS101 was better than that of the secondary amine TAS550 and QAS550 for aluminosilicate minerals. The diaspore and kaolinite were separated successfully in the reverse flotation with 1.0×10-3 M TAS101 collectors and 500mg/L soluble starch depressors in pulp pH=8.
In order to de-silicate from some diasporic bauxite of Henan Province, of which the Al2O3 grade and A/S were 63.92%,6.07 respectively, the closed circuit flotation experiments were conducted with the [(C2H5O)3Si(CH2)3N(CH3)2C,2H25/C14H29]C1(QAS224) and TAS101 as collectors. When the diasporic bauxite ore was processed by single-stage rougher, two-stage cleaner and two-stage scavenger with 700g/t QAS224 in pulp pH=11, A12O3 grade, A12O3 recovery and the A/S of concentrate were 67.79%,81.72%and 9.67 respectively. When the diasporic bauxite ore was processed by single-stage rougher, two-stage cleaner and two-stage scavenger with 720g/t TAS101 and 1320g/t soluble starch in pulp pH=11, A12O3 grade, Al2O3 recovery and the A/S of floating concentrate were 68.52%,83.34%and 9.58 respectively. The collecting ability of combination of QAS224 and TAS101 was stronger than each one of them. At 540g/t QAS101,180g/t TAS101 and 1320g/t soluble starch in pulp pH=11, A12O3 grade, Al2O3 recovery and the A/S of concentrate were 68.98%,85.42%and 10.34 respectively with same flowsheet. The quality of concentrates reached the feeding requirement of Bayer process.
The study on acting mechanism of the collector QAS222 with the minerals showed that there were electrostatic adsorptions, hydrogen binding and chemical adsorptions between QAS222 and the three aluminosilicate minerals in pulp pH=11, produced more Si-O, Si-O-Si and Si-O-A1 bonds and made the QAS222 adsorbed steadily in these minerals'surfaces. So the Zeta potentials increased and contact angle turned bigger and the floatability became better. Under the same conditions it was difficult to QAS222 to be adsorbed in the diaspore mineral surface. So the diaspore may be effectively separated from aluminosilicate minerals by collector QAS222 in pulp pH=11.
In pulp pH=11 TAS101 may adsorbed in the four minerals surfaces and improved their floatability. Soluble starch was effective depressor for diaspore. The diaspore mineral can not act with TAS101 if it had been depressed by soluble starch in pulp pH=11 and its floatability always was bad. The soluble starch can not change the floatability of aluminosilicate minerals. The diaspore could be effectively separated from aluminosilicate minerals with TAS101 as collector and the soluble starch as depressor in pulp pH=11. The study on acting mechanism of the TAS101 with the minerals indicated that silicon groups of TAS101 had hydrophobic interaction, and there were electrostatic adsorptions in the diaspore surface and hydrogen bond interactions as well as electrostatic adsorptions in the other three aluminosilicate minerals'surfaces.
首先,系统地研究了有机硅捕收剂的合成与表征。以卤代有机硅氧烷与脂肪叔胺为原料、碘化钾为催化剂、无水乙醇为溶剂,一步直接合成了有机硅季铵盐QAS系列捕收剂。在卤代有机硅氧烷、叔胺、碘化钾投料的摩尔配比为1.1:1.0:0.01、反应温度80℃、合成时间37h、通N2保护的条件下,合成产品转化率均达90%以上。采用六甲基二硅氧烷(MM)为封端剂,对氨乙基氨丙基二甲氧基甲基硅烷(TAS100)进行封端处理,制备了有机硅伯胺捕收剂氨乙基氨丙基三硅氧烷(TAS101)。在投料摩尔配比TAS100:MM=1:5、以10%四甲基氢氧化铵溶液为催化剂、通N：保护、恒温90℃搅拌反应8h的条件下,TAS100转化率约达90%。分别以TAS100、TAS101为原料与苄氯反应,当投料的摩尔比TAS100或TAS101：苄氯=1：1.5时,以无水乙醇为溶剂、通N2保护、恒温80℃反应8h,合成了有机硅仲胺苄基氨乙基氨丙基二甲氧基甲基硅烷(TAS550)和苄基氨乙基氨丙基三硅氧烷(QAS550)。采用化学滴定、界面张力测定、红外谱图分析、1HNMR和13CNMR核磁共振测定等分析测试技术对最终产品的结构与性能进行表征,研究表明各目的产品纯度均超过90%。
研究并揭示了有机硅捕收剂的结构与浮选性能的相互关系。研究结果表明,有机硅季铵盐QAS系列捕收剂在广泛pH范围内均是高岭石、叶蜡石、伊利石三种铝硅酸盐矿物的有效捕收剂,QAS系列捕收剂对一水硬铝石的捕收能力随着矿浆pH升高先增加而后急速减小；当pH≥11时,铝硅矿物之间表现出了良好的反浮选分离趋势；该类捕收剂对铝硅矿物的浮选性能随着主碳链的延长而降低；在捕收剂γ-(三乙氧基硅基)丙基十二烷基二甲基氯化铵(QAS222)用量4×10-4 M、NaOH调矿浆pH至11、未添加任何抑制剂的条件下,实现了一水硬铝石和高岭石人工混合矿的反浮选分离。在pH4～10广泛范围内,有机硅伯胺和仲胺捕收剂可显著增强铝硅矿物的可浮性,是铝硅矿物的有效捕收剂；有机硅伯胺TAS101对铝硅矿物的捕收力强于有机硅仲胺TAS550和QAS550；在捕收剂TAS101用量1.0×10-3 M、抑制剂可溶性淀粉500mg/L、Na2CO3调pH=8条件下,成功地进行了一水硬铝石与高岭石矿物的反浮选分离。
针对河南某Al2O3品位63.92%、铝硅比为6.07的一水硬铝石型铝土矿,以γ-(三乙氧基硅基)丙基十二/十四烷基二甲基氯化铵(QAS224)和TAS101为捕收剂,进行反浮选脱硅试验研究。小型闭路试验研究结果表明,当捕收剂γ-(三乙氧基硅基)丙基十二/十四烷基二甲基氯化铵(QAS224)用量700g/t、NaOH调矿浆pH至11,原矿经一次粗选两次精选两次扫选,获得了Al2O3品位67.79%、Al2O3回收率81.72%、A/S为9.67的浮选精矿；当捕收剂TAS101用量720g/t、Na2CO3调矿浆pH至11、可溶性淀粉用量1320g/t时,原矿同样经一次粗选两次精选两次扫选,浮选精矿A/S为9.58,其A1203品位和回收率分别为68.52%、83.34%；当QAS224用量540g/t,TAS101用量180g/t,Na2CO3调矿浆pH至11,可溶性淀粉用量1320g/t时,浮选流程不变,获得了浮选精矿A/S为10.34、Al2O3,品位68.98%、Al2O3回收率85.42%的选别指标,组合捕收剂脱硅效果优于单一用药。各浮选精矿质量均满足拜耳法氧化铝生产工艺给料要求。
研究并揭示了有机硅季铵盐捕收剂QAS222与矿物作用机理。研究结果表明,在矿浆pH=11的碱性条件下,QAS222通过静电物理作用、氢键作用、化学吸附与矿物表面的Si、0、Al等原子作用,使矿物表面产生了更多Si-O-Si、Si-O、Si-O-Al键,从而牢固地吸附于高岭石、叶蜡石和伊利石三种铝硅酸盐矿物表面,使其矿物表面ζ-电位正移、接触角增大、疏水性和可浮性增强,而此时QAS222很难在一水硬铝石矿物表面发生吸附,因此,铝硅矿物表面之间出现了明显的疏水性和可浮性差异,从而实现了铝硅矿物的反浮选分离。
在矿浆广泛pH范围内,TAS101可较好地改善铝硅矿物表面的疏水性和可浮性,淀粉是一水硬铝石矿物的选择性抑制剂；受淀粉抑制后,一水硬铝石矿物很难再吸附捕收剂TAS101,因此可浮性较差；而淀粉基本不影响高岭石、叶蜡石、伊利石的浮选；以TAS101为捕收剂、淀粉为抑制剂,可有效地实现铝硅矿物的浮选分离。机理研究表明,捕收剂TAS101的硅基团起疏水作用,其在一水硬铝石矿物表面主要发生静电物理吸附,而在高岭石、叶蜡石和伊利石矿物表面则发生静电吸附和氢键作用。
To the significant demand of desilication of bauxite ores by reverse flotation in China, a kind of new cationic organosilicon surfactant was developed as collector of aluminosilicate minerals. The synthesis of this collector was studied on, as well as its flotation performance and mechanism on diaspore and aluminosilicate minerals.
Firstly, the organosilicon cationic collectors were synthesized and characterized systematically. The organosilicon quaternary ammonium collectors were obtained by one-step reaction which conducted at 80℃for 37 hours, with halogenated siloxane coupling agent:tertiary aliphatic amine:KI=1.1:1:0.01 by the mole ratio, using anhydrous ethanol as solvent, protected the reaction system with N2. The percent conversion of tertiary aliphatic amine was more than 90%. The organosilicon CH3Si(OSi(CH3)3)2(CH2)3NH(CH2)2NH2(TAS101) collector was synthesized when reaction was conducted at 90℃for 8 hours, with CH3Si(OCH3)2(CH2)3NH(CH2)2NH2(TAS 100):hexamethyldisiloxane (MM)= 1:5 by the mole ratio, using anhydrous ethanol as solvent and 10%(CH3)4NOH solution as activator, protected the reaction system with N2. The percent conversion of TAS100 was about 90%. The CH3Si(OCH3)2(CH2)3NH(CH2)2NHCH2(C6H5)(TAS550) collector was synthesized when reaction was conducted at 80℃for 8 hours, with TAS100:benzyl chloride=1:1.5 by the mole ratio, using anhydrous ethanol as solvent, protected the reaction system with N2. The collector CH3Si[OSi(CH3)3]2(CH2)3NH(CH2)2NHCH2(C6H5)(QAS550) was obtained with TAS101 took the place of TAS100 in the reaction mentioned above. Structures and properties of final products were characterized by FT-IR spectrum,1HNMR and 13CNMR et al. The purity of every new organosilicon collector was more than 90%.
The relationship of molecular structures and flotation performance of collectors were investigated. The results indicated that organosilicon quaternary ammonium was an effective collector of kaolinite, pyrophyllite and illite minerals in a wide pH range, and their collecting ability for diaspore increased firstly and then decreased drastically with the increase of pulp pH, and the optimum pulp pH for the separation of diaspore from kaolinite was around 11. The collecting ability of organosilicon quaternary ammoniums for aluminosilicate minerals receded with the lengthening of backbone in tertiary aliphatic amine. In pH=11 the diaspore was been effectively separated from kaolinite with 4×10-4 M [(C2H5O)3Si(CH2)3N(CH3)2C12H25]Cl(QAS222) as collector. In the wide range of pH=4-10, the collectors of organosilicon primary amine and secondary amine could improve the minerals'floatability remarkably. The collecting ability of primary amine TAS101 was better than that of the secondary amine TAS550 and QAS550 for aluminosilicate minerals. The diaspore and kaolinite were separated successfully in the reverse flotation with 1.0×10-3 M TAS101 collectors and 500mg/L soluble starch depressors in pulp pH=8.
In order to de-silicate from some diasporic bauxite of Henan Province, of which the Al2O3 grade and A/S were 63.92%,6.07 respectively, the closed circuit flotation experiments were conducted with the [(C2H5O)3Si(CH2)3N(CH3)2C,2H25/C14H29]C1(QAS224) and TAS101 as collectors. When the diasporic bauxite ore was processed by single-stage rougher, two-stage cleaner and two-stage scavenger with 700g/t QAS224 in pulp pH=11, A12O3 grade, A12O3 recovery and the A/S of concentrate were 67.79%,81.72%and 9.67 respectively. When the diasporic bauxite ore was processed by single-stage rougher, two-stage cleaner and two-stage scavenger with 720g/t TAS101 and 1320g/t soluble starch in pulp pH=11, A12O3 grade, Al2O3 recovery and the A/S of floating concentrate were 68.52%,83.34%and 9.58 respectively. The collecting ability of combination of QAS224 and TAS101 was stronger than each one of them. At 540g/t QAS101,180g/t TAS101 and 1320g/t soluble starch in pulp pH=11, A12O3 grade, Al2O3 recovery and the A/S of concentrate were 68.98%,85.42%and 10.34 respectively with same flowsheet. The quality of concentrates reached the feeding requirement of Bayer process.
The study on acting mechanism of the collector QAS222 with the minerals showed that there were electrostatic adsorptions, hydrogen binding and chemical adsorptions between QAS222 and the three aluminosilicate minerals in pulp pH=11, produced more Si-O, Si-O-Si and Si-O-A1 bonds and made the QAS222 adsorbed steadily in these minerals'surfaces. So the Zeta potentials increased and contact angle turned bigger and the floatability became better. Under the same conditions it was difficult to QAS222 to be adsorbed in the diaspore mineral surface. So the diaspore may be effectively separated from aluminosilicate minerals by collector QAS222 in pulp pH=11.
In pulp pH=11 TAS101 may adsorbed in the four minerals surfaces and improved their floatability. Soluble starch was effective depressor for diaspore. The diaspore mineral can not act with TAS101 if it had been depressed by soluble starch in pulp pH=11 and its floatability always was bad. The soluble starch can not change the floatability of aluminosilicate minerals. The diaspore could be effectively separated from aluminosilicate minerals with TAS101 as collector and the soluble starch as depressor in pulp pH=11. The study on acting mechanism of the TAS101 with the minerals indicated that silicon groups of TAS101 had hydrophobic interaction, and there were electrostatic adsorptions in the diaspore surface and hydrogen bond interactions as well as electrostatic adsorptions in the other three aluminosilicate minerals'surfaces.
引文
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