磁性纳米材料改性树状大分子水处理剂的合成及性能研究
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摘要
目前,我国东部大部分油田都进入高含水期,三次采油技术的运用给油田带来了可观的经济效益,但也使含油污水的组成和稳定性发生了很大的变化,使用单一的水处理剂和常规的水处理方法处理污水已很难奏效,因此研究开发新型的、高效的、复合型水处理剂已成为科研工作者研究的热点。本论文在探索合成磁性纳米四氧化三铁和PAMAM树状大分子的最适宜反应条件基础上,利用PAMAM树状大分子的特殊结构包覆磁性纳米四氧化三铁颗粒制得PF系列磁性纳米材料改性树状大分子水处理剂。
本课题在研究合成磁性四氧化三铁的基础上,通过正交实验探索了柠檬酸钠改性合成磁性纳米四氧化三铁的最适宜反应条件:搅拌速度800r/min,n(Fe2+)/n(Fe3+)/n(OH-)=1/1.8/8,氨水浓度为0.25mol/L,铁盐浓度为0.75mol/L,反应温度为50℃,n(柠檬酸钠)/n(总铁)=0.75。并通过红外光谱、X射线粉末衍射仪、扫描电子显微镜、透射电子显微镜和动态光散射粒度仪对产物进行了表征分析,证明合成产物是粒径在20nm左右的磁性四氧化三铁颗粒。
利用发散法合成了PAMAM树状大分子,详细研究了合成低代数PAMAM树状大分子的最适宜条件。0.5代PAMAM树状大分子的合成最适宜条件为:反应时间18h,反应温度30℃,n(EDA)/n(MA)=1/8,溶剂甲醇30%;1.0代PAMAM树状大分子合成的最适宜条件为:反应时间24h,反应温度25℃,n(0.5G)/n(EDA)=1/12,溶剂甲醇20%。通过此反应条件重复进行迈克尔加成和酯的酰胺化反应,可以依次得到2.0代、3.0代PAMAM树状大分子。采用红外光谱分析(IR)、1H-NMR、元素分析等表征手段对各代产品进行表征,结果证明合成产物是目标分子结构。通过合成的各代PAMAM和现场药剂罗曼哈斯处理孤岛四号联井排来液除油实验表明,合成的3.0代PAMAM除油效果最佳,在加剂量为70 mg/L时除油率可达到85.1%,悬浮物从138 mg/L降到73 mg/L,除油效果远远好于现场药剂罗曼哈斯。
探索了不同反应条件对合成磁性纳米材料改性树状大分子水处理剂的影响,得到合成PF系列水处理剂的最适宜条件为:n(PAMAM)/n(总Fe)=0.5,反应温度70℃,pH值8～9,包覆时间30min。通过红外光谱、透射电子显微镜和振动样品磁强计对磁性纳米材料改性树状大分子水处理剂进行了表征分析,证明得到的产物是粒径为30nm左右的四氧化三铁颗粒,且具有超顺磁性。最适宜条件下合成的PF-0.5水处理剂在加剂量为80mg/L时,可将孤四联污水含油量从1328.1mg/L降到42.1mg/L,悬浮物从143mg/L降到61mg/L。PF-0.5水处理剂适用性研究表明对孤岛三个联合站的污水有一定的普遍适应性。
At present, most oilfields in eastern China have entered in the period of high moisture content. Using EOR technology in the oilfield has brought considerable economic benefits, but also the composition of oily wastewater and stability of great changes have taken place. Single wastewater conventional treatment reagent and sewage treatment method have been hard work. So, research and development of new, highly efficient, complex wastewater treatment reagent has become a hot work to scientific research workers. In this paper, based on the research of the optimum reaction conditions of magnetic nano-meter Fe3O4 and PAMAM dendrimers, we utilize the special structure of PAMAM dendrimers coated magnetic nanometer Fe3O4 particle to be the PF series of magnetic nano-material modified dendrimer wastewater treatment reagent.
This subject explore the best conditions of synthesis the Fe3O4 powder modified by sodium citrate through the orthogonal experiment on the basis of the synthesis of magnetic Fe3O4 powder: stirring speed 800 r/min, n (Fe2+)/n(Fe3+)/n(OH-) = 1/1.8/8, the concentration of ammonia is 0.25 mol/L, iron salt concentrations is 0.75 mol/L, the reaction temperature is 50℃, n(Sodium Citrate)/n(Total Fe) = 0.75. And through infrared spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy and dynamic scattering particle size instrument to analysis, the product is proved to be the magnetic Fe3O4 around 20 nm in diameter.
PAMAM dendrimers have been synthesized by divergent method, and the most optimum conditions have been detailedly studied on synthesis of low-generation PAMAM dendrimers. The optimum reaction conditions of synthesis 0.5 PAMAM dendrimers: reaction time 18h, reaction temperature 30℃, n(EDA)/n(MA)=1/8, solvent methanol 30%; The optimum reaction conditions of synthesis 1.0 generation PAMAM dendrimers are as follows: reaction time 24h, reaction temperature 25℃, n(0.5G)/n(EDA)=1/12, solvent methanol 20%. Repeated Michael addition and Ester Amide reaction, it can be followed by 2.0 generation, 3.0 generation PAMAM dendrimers. Using infrared spectroscopy (IR), 1H-NMR, elemental analysis of various methods, the products are characterized to be the target molecular structure. Through the degrease experiments on well liquid drainage from Gudao 4th joint station by the pharmaceutical Luomanhasi and PAMAM dendrimers, it shows that the 3.0 generation PAMAM has the best results in oil removal rate to 85.1 % at the additive dose of 70 mg/L, and the suspended solids are removed from 138 mg/L reduced to 73 mg/L. The deoiling effect is far better than those of the scene pharmacy Luomanhasi.
Explore the effect of different conditions on synthesis of the magnetic nano-material modified dendrimer wastewater treatment reagent. We obtained the best conditions on synthesis of PF series wastewater treatment reagent: n (PAMAM)/n(Total Fe) = 0.5, reaction temperature 70℃, pH value 8～9, coating time 30min. Through the infrared spectrum, transmission electron microscopy and vibration sample magnetometer, the nano-material modified dendrimer wastewater treatment reagent is characterized to be Fe3O4 powder around 30nm, And has paramagnetic. The PF-0.5 wastewater treatment reagent can remove the oil in water from 1328.1mg/L to 42.1mg/L at the additive dose of 80mg/L, suspended solids from 143mg/L down to 61mg/L. Study on the applicability of PF-0.5 wastewater treatment reagent shows that it has certain rifely adaptability to the sewage of three Gudao joint station.
本课题在研究合成磁性四氧化三铁的基础上,通过正交实验探索了柠檬酸钠改性合成磁性纳米四氧化三铁的最适宜反应条件:搅拌速度800r/min,n(Fe2+)/n(Fe3+)/n(OH-)=1/1.8/8,氨水浓度为0.25mol/L,铁盐浓度为0.75mol/L,反应温度为50℃,n(柠檬酸钠)/n(总铁)=0.75。并通过红外光谱、X射线粉末衍射仪、扫描电子显微镜、透射电子显微镜和动态光散射粒度仪对产物进行了表征分析,证明合成产物是粒径在20nm左右的磁性四氧化三铁颗粒。
利用发散法合成了PAMAM树状大分子,详细研究了合成低代数PAMAM树状大分子的最适宜条件。0.5代PAMAM树状大分子的合成最适宜条件为:反应时间18h,反应温度30℃,n(EDA)/n(MA)=1/8,溶剂甲醇30%;1.0代PAMAM树状大分子合成的最适宜条件为:反应时间24h,反应温度25℃,n(0.5G)/n(EDA)=1/12,溶剂甲醇20%。通过此反应条件重复进行迈克尔加成和酯的酰胺化反应,可以依次得到2.0代、3.0代PAMAM树状大分子。采用红外光谱分析(IR)、1H-NMR、元素分析等表征手段对各代产品进行表征,结果证明合成产物是目标分子结构。通过合成的各代PAMAM和现场药剂罗曼哈斯处理孤岛四号联井排来液除油实验表明,合成的3.0代PAMAM除油效果最佳,在加剂量为70 mg/L时除油率可达到85.1%,悬浮物从138 mg/L降到73 mg/L,除油效果远远好于现场药剂罗曼哈斯。
探索了不同反应条件对合成磁性纳米材料改性树状大分子水处理剂的影响,得到合成PF系列水处理剂的最适宜条件为:n(PAMAM)/n(总Fe)=0.5,反应温度70℃,pH值8～9,包覆时间30min。通过红外光谱、透射电子显微镜和振动样品磁强计对磁性纳米材料改性树状大分子水处理剂进行了表征分析,证明得到的产物是粒径为30nm左右的四氧化三铁颗粒,且具有超顺磁性。最适宜条件下合成的PF-0.5水处理剂在加剂量为80mg/L时,可将孤四联污水含油量从1328.1mg/L降到42.1mg/L,悬浮物从143mg/L降到61mg/L。PF-0.5水处理剂适用性研究表明对孤岛三个联合站的污水有一定的普遍适应性。
At present, most oilfields in eastern China have entered in the period of high moisture content. Using EOR technology in the oilfield has brought considerable economic benefits, but also the composition of oily wastewater and stability of great changes have taken place. Single wastewater conventional treatment reagent and sewage treatment method have been hard work. So, research and development of new, highly efficient, complex wastewater treatment reagent has become a hot work to scientific research workers. In this paper, based on the research of the optimum reaction conditions of magnetic nano-meter Fe3O4 and PAMAM dendrimers, we utilize the special structure of PAMAM dendrimers coated magnetic nanometer Fe3O4 particle to be the PF series of magnetic nano-material modified dendrimer wastewater treatment reagent.
This subject explore the best conditions of synthesis the Fe3O4 powder modified by sodium citrate through the orthogonal experiment on the basis of the synthesis of magnetic Fe3O4 powder: stirring speed 800 r/min, n (Fe2+)/n(Fe3+)/n(OH-) = 1/1.8/8, the concentration of ammonia is 0.25 mol/L, iron salt concentrations is 0.75 mol/L, the reaction temperature is 50℃, n(Sodium Citrate)/n(Total Fe) = 0.75. And through infrared spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy and dynamic scattering particle size instrument to analysis, the product is proved to be the magnetic Fe3O4 around 20 nm in diameter.
PAMAM dendrimers have been synthesized by divergent method, and the most optimum conditions have been detailedly studied on synthesis of low-generation PAMAM dendrimers. The optimum reaction conditions of synthesis 0.5 PAMAM dendrimers: reaction time 18h, reaction temperature 30℃, n(EDA)/n(MA)=1/8, solvent methanol 30%; The optimum reaction conditions of synthesis 1.0 generation PAMAM dendrimers are as follows: reaction time 24h, reaction temperature 25℃, n(0.5G)/n(EDA)=1/12, solvent methanol 20%. Repeated Michael addition and Ester Amide reaction, it can be followed by 2.0 generation, 3.0 generation PAMAM dendrimers. Using infrared spectroscopy (IR), 1H-NMR, elemental analysis of various methods, the products are characterized to be the target molecular structure. Through the degrease experiments on well liquid drainage from Gudao 4th joint station by the pharmaceutical Luomanhasi and PAMAM dendrimers, it shows that the 3.0 generation PAMAM has the best results in oil removal rate to 85.1 % at the additive dose of 70 mg/L, and the suspended solids are removed from 138 mg/L reduced to 73 mg/L. The deoiling effect is far better than those of the scene pharmacy Luomanhasi.
Explore the effect of different conditions on synthesis of the magnetic nano-material modified dendrimer wastewater treatment reagent. We obtained the best conditions on synthesis of PF series wastewater treatment reagent: n (PAMAM)/n(Total Fe) = 0.5, reaction temperature 70℃, pH value 8～9, coating time 30min. Through the infrared spectrum, transmission electron microscopy and vibration sample magnetometer, the nano-material modified dendrimer wastewater treatment reagent is characterized to be Fe3O4 powder around 30nm, And has paramagnetic. The PF-0.5 wastewater treatment reagent can remove the oil in water from 1328.1mg/L to 42.1mg/L at the additive dose of 80mg/L, suspended solids from 143mg/L down to 61mg/L. Study on the applicability of PF-0.5 wastewater treatment reagent shows that it has certain rifely adaptability to the sewage of three Gudao joint station.
引文
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