结晶紫碱性褪色反应在假二元微乳液体系近临界区的动力学和微乳液液膜法萃取镍离子的研究
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摘要
自从1869年英国物理学家安德鲁斯发现临界现象以来,相变和临界现象的研究一直非常活跃,人们发现,截然不同的物理体系在临界点附近都有十分相似的奇异行为。而临界效应对于溶液中的化学反应同样具有重要影响,二元体系近临界区中的化学反应已有大量研究,但在假二元微乳液体系中的化学反应还没有报道。本论文的第一部分用紫外-可见分光光度计研究了结晶紫在水/AOT/正癸烷和水/CTAB/正丁醇假二元微乳液体系远离临界区和近临界区的碱性褪色反应动力学,探讨了临界效应对化学反应动力学的影响。
微乳液是高度分散的体系,颗粒很小,有很大的传质面积以及很高的传质效率,因而利用微乳液作为液膜来进行物质的提取分离,不仅具有快速、高效的优点,而且能克服乳状液的不稳定、易溶胀、破乳难等特点、具有良好的应用前景。镍是工业上十分重要的原料,在催化剂、电池、合金等方面都有广泛的应用,因此本论文第二部分还研究了微乳液液膜在萃取镍离子中的应用。
论文的具体内容包括:
(1)研究了结晶紫在水/AOT/正癸烷(LCST,低临界点)ω=40.8和ω=45.2(水与表面活性剂的物质的量之比)假二元微乳液体系远离临界区和近临界区的碱性褪色反应动力学。发现当温度远低于假二元体系的低临界点时,反应速率常数符合Arrhenius公式;当温度在低于临界点0.255-1.382 K之间时,反应速率常数高于Arrhenius公式推导值,即出现加速现象(Speeding up),不符合临界慢化(Critical slowlng down);而且越接近临界点,反应速率常数波动幅度越大。另外,发现拟合的临界指数x=0.322±0.028(ω=40.8)和x=0.340±0.034(ω=45.2)都接近于0.326(3DIsing模型的β值),不吻合G-W理论的判断。
(2)研究了结晶紫在水/CTAB/正丁醇(UCST,高临界点)ω=146假二元微乳液体系远离临界区和近临界区的碱性褪色反应动力学。发现当温度远高于假二元体系的高临界点时,化学反应速率常数符合Arrhenius公式;当温度在高于临界点0.646-2.282 K之间时,反应速率常数低于Arrhenius公式推导值,符合临界慢化(Critical slowing down),而且越接近临界点,反应速率常数波动幅度越大,另外,发现拟合的临界指数为x=0.124±0.028接近于0.11(3DIsing模型的α值),吻合G-W理论的判断,属于弱慢化。
(3)分别在两个微乳液体系中研究了CV~+两种分子构型的变化规律,发现不论是在水/AOT/正癸烷(LCST)体系中还是在水/CTAB/正丁醇(UCST)体系中,当温度处于在T_c~0到T_c之间时I_(λ590)/I_(λ550)(两个特征峰的吸收强度比值)都受到近临界效应的影响,当体系的温度在逐渐靠近T_c时I_(λ_590)/I_(λ550)随温度的升高而增大,然后在最靠近T_c处I_(λ590)/I_(λ550)又迅速降低。
(4)分别研究了水/AOT/正癸烷微乳液液膜对标准镍溶液和工业镍溶液中镍离子的萃取和回收,考察了微乳液液膜组成、pH值、微乳液液膜与镍溶液的质量比、搅拌时间等实验参数对萃取率的影响,以及反萃取时pH值和短链醇对反萃取率和消除微乳体系乳化的影响。发现AOT和正癸烷的质量比在7/3到6/4之间时,只要适当调整pH值就可以实现对镍离子的有效萃取,而且微乳液液膜可以多次循环萃取。当在pH为9-10范围内萃取9次时,Ni~(2+)的最大富集浓度可达到44.17g/L,即为工业镍溶液(0.4230g/L)浓度的104倍。
Since Andrews,the British physicist,found the critical phenomena in1869,the research field of phase transition and critical phenomena has been very active.For different systems,it is found that their properties are similar in the vicinity of respective critical point.And the critical effect on chemical reactions is also very important.At present there are many reports about reactions just in binary solutions,but reactions in the pseudo-binary microemulsions near critical point have not yet been reported.The first part of this thesis was the kinetic study of alkaline fading of crystal violet in water/AOT/n-decane and water/CTAB/n-butanol pseudo-binary microemulsion near and far away from respective critical point by UV-visible spectrometer.
Microemulsion as an extracting membrane not only has many excellent and outstanding advantages,including small and highly dispersed particles,large mass transfer area and high mass transfer efficiency,but also overcomes the disadvantages of emulsion,including the instability, easily swelling,and hard demulsification.Nickel,as a very important industrial raw material of the catalysts,batteries,alloys,ect.,has a wide range of applications,so in the second part of this thesis microemulsion as a novel extraction method of nickel ion was examined.
The specific content of the thesis as following:
(1) Kinetic studys of alkaline fading of crystal violet reaction were investigated in water/AOT/ n-decane(LCST,lower critical solution temperature)ω=40.8 andω=45.2(n_(water)/n_(surfactant) molar ratio) near and far away from respective critical point.When the temperature was much lower than T_C(low critical point of the solution),the reaction rate constant obeyed the Arrhenius equation.But when the temperature was less than T_C about 0.200-1.500 K,namely near critical region,the reaction rate constant deviated from Arrhenius equation and appeared to Speeding up phenomenon,which wasn't consistent with the theories of critical slowing down in dynamic critical phenomena.The fitted critical exponents,including x= 0.322±0.028(ω=40.8) and x=0.340±0.034(ω=45.2),were also not in agreement with G-W's theory.
(2) The kinetic investigation of alkaline fading of CV had also been examined in water/CTAB/ n-butanol(UCST,upper crical solution temperature)ω=146 psuedo-binary microemulsion. The reaction rate constant was in good line with the Arrhenius equation when the temperature was much higher than T_C(upper critical point of the solution),and it appeared the critical slowing down when the temperature got closed to T_C,just above it in range of 0.646-2.282 K.The fitted critical exponents,x=0.124±0.028 closed to 0.11(the value ofαin 3DIsing model),was also in agreement with G-W's theory.
(3) As a byproduct of kinetic investigation of alkaline fading of CV in pseudo-binary microemulsions,we had observed that comparative amount of two isomers of CV changed in both LCST and UCST microemulsions.I_(λ590)/I_(λ550),the intensity ratio of the maximum absorption wavelength to the shoulder,switched from increasing to decreasing in the nearest region of T_c,was influnced by the critical effect.
(4) In order to test the extracting effect of water/AOT/n-decane microemlsion as a novel liquid membrane to nickel ion,we had devised two experiments,including the standard nickel ion solution and the industrial one.We found the extraction and anti-extraction rate were influenced by the experimental parameters including not only liquid membrane composition, pH,the quality ratio of the membrane to nickel ion solutions,but also stirring time.The results showed that when the composition of the liquid membrane,the quality ratio of AOT to n-decane,was between 7/3 and 6/4,the microemulsion was very efficient to the extraction of nickel ion solution,and could be recycled several times to utilize as long as the proper pH value was adjusted.After extracting the industrial nickel ion solution 9 times with pH in the range of 9-10,nickel ion concentration was up to 44.170 g/L,104 times to the original industrial nickel ion concentration(0.423 g/L).
微乳液是高度分散的体系,颗粒很小,有很大的传质面积以及很高的传质效率,因而利用微乳液作为液膜来进行物质的提取分离,不仅具有快速、高效的优点,而且能克服乳状液的不稳定、易溶胀、破乳难等特点、具有良好的应用前景。镍是工业上十分重要的原料,在催化剂、电池、合金等方面都有广泛的应用,因此本论文第二部分还研究了微乳液液膜在萃取镍离子中的应用。
论文的具体内容包括:
(1)研究了结晶紫在水/AOT/正癸烷(LCST,低临界点)ω=40.8和ω=45.2(水与表面活性剂的物质的量之比)假二元微乳液体系远离临界区和近临界区的碱性褪色反应动力学。发现当温度远低于假二元体系的低临界点时,反应速率常数符合Arrhenius公式;当温度在低于临界点0.255-1.382 K之间时,反应速率常数高于Arrhenius公式推导值,即出现加速现象(Speeding up),不符合临界慢化(Critical slowlng down);而且越接近临界点,反应速率常数波动幅度越大。另外,发现拟合的临界指数x=0.322±0.028(ω=40.8)和x=0.340±0.034(ω=45.2)都接近于0.326(3DIsing模型的β值),不吻合G-W理论的判断。
(2)研究了结晶紫在水/CTAB/正丁醇(UCST,高临界点)ω=146假二元微乳液体系远离临界区和近临界区的碱性褪色反应动力学。发现当温度远高于假二元体系的高临界点时,化学反应速率常数符合Arrhenius公式;当温度在高于临界点0.646-2.282 K之间时,反应速率常数低于Arrhenius公式推导值,符合临界慢化(Critical slowing down),而且越接近临界点,反应速率常数波动幅度越大,另外,发现拟合的临界指数为x=0.124±0.028接近于0.11(3DIsing模型的α值),吻合G-W理论的判断,属于弱慢化。
(3)分别在两个微乳液体系中研究了CV~+两种分子构型的变化规律,发现不论是在水/AOT/正癸烷(LCST)体系中还是在水/CTAB/正丁醇(UCST)体系中,当温度处于在T_c~0到T_c之间时I_(λ590)/I_(λ550)(两个特征峰的吸收强度比值)都受到近临界效应的影响,当体系的温度在逐渐靠近T_c时I_(λ_590)/I_(λ550)随温度的升高而增大,然后在最靠近T_c处I_(λ590)/I_(λ550)又迅速降低。
(4)分别研究了水/AOT/正癸烷微乳液液膜对标准镍溶液和工业镍溶液中镍离子的萃取和回收,考察了微乳液液膜组成、pH值、微乳液液膜与镍溶液的质量比、搅拌时间等实验参数对萃取率的影响,以及反萃取时pH值和短链醇对反萃取率和消除微乳体系乳化的影响。发现AOT和正癸烷的质量比在7/3到6/4之间时,只要适当调整pH值就可以实现对镍离子的有效萃取,而且微乳液液膜可以多次循环萃取。当在pH为9-10范围内萃取9次时,Ni~(2+)的最大富集浓度可达到44.17g/L,即为工业镍溶液(0.4230g/L)浓度的104倍。
Since Andrews,the British physicist,found the critical phenomena in1869,the research field of phase transition and critical phenomena has been very active.For different systems,it is found that their properties are similar in the vicinity of respective critical point.And the critical effect on chemical reactions is also very important.At present there are many reports about reactions just in binary solutions,but reactions in the pseudo-binary microemulsions near critical point have not yet been reported.The first part of this thesis was the kinetic study of alkaline fading of crystal violet in water/AOT/n-decane and water/CTAB/n-butanol pseudo-binary microemulsion near and far away from respective critical point by UV-visible spectrometer.
Microemulsion as an extracting membrane not only has many excellent and outstanding advantages,including small and highly dispersed particles,large mass transfer area and high mass transfer efficiency,but also overcomes the disadvantages of emulsion,including the instability, easily swelling,and hard demulsification.Nickel,as a very important industrial raw material of the catalysts,batteries,alloys,ect.,has a wide range of applications,so in the second part of this thesis microemulsion as a novel extraction method of nickel ion was examined.
The specific content of the thesis as following:
(1) Kinetic studys of alkaline fading of crystal violet reaction were investigated in water/AOT/ n-decane(LCST,lower critical solution temperature)ω=40.8 andω=45.2(n_(water)/n_(surfactant) molar ratio) near and far away from respective critical point.When the temperature was much lower than T_C(low critical point of the solution),the reaction rate constant obeyed the Arrhenius equation.But when the temperature was less than T_C about 0.200-1.500 K,namely near critical region,the reaction rate constant deviated from Arrhenius equation and appeared to Speeding up phenomenon,which wasn't consistent with the theories of critical slowing down in dynamic critical phenomena.The fitted critical exponents,including x= 0.322±0.028(ω=40.8) and x=0.340±0.034(ω=45.2),were also not in agreement with G-W's theory.
(2) The kinetic investigation of alkaline fading of CV had also been examined in water/CTAB/ n-butanol(UCST,upper crical solution temperature)ω=146 psuedo-binary microemulsion. The reaction rate constant was in good line with the Arrhenius equation when the temperature was much higher than T_C(upper critical point of the solution),and it appeared the critical slowing down when the temperature got closed to T_C,just above it in range of 0.646-2.282 K.The fitted critical exponents,x=0.124±0.028 closed to 0.11(the value ofαin 3DIsing model),was also in agreement with G-W's theory.
(3) As a byproduct of kinetic investigation of alkaline fading of CV in pseudo-binary microemulsions,we had observed that comparative amount of two isomers of CV changed in both LCST and UCST microemulsions.I_(λ590)/I_(λ550),the intensity ratio of the maximum absorption wavelength to the shoulder,switched from increasing to decreasing in the nearest region of T_c,was influnced by the critical effect.
(4) In order to test the extracting effect of water/AOT/n-decane microemlsion as a novel liquid membrane to nickel ion,we had devised two experiments,including the standard nickel ion solution and the industrial one.We found the extraction and anti-extraction rate were influenced by the experimental parameters including not only liquid membrane composition, pH,the quality ratio of the membrane to nickel ion solutions,but also stirring time.The results showed that when the composition of the liquid membrane,the quality ratio of AOT to n-decane,was between 7/3 and 6/4,the microemulsion was very efficient to the extraction of nickel ion solution,and could be recycled several times to utilize as long as the proper pH value was adjusted.After extracting the industrial nickel ion solution 9 times with pH in the range of 9-10,nickel ion concentration was up to 44.170 g/L,104 times to the original industrial nickel ion concentration(0.423 g/L).
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