聚环氧琥珀酸环氧化条件优化及阻垢剂性能评价方法研究
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摘要
本论文研究了聚环氧琥珀酸(PESA)的合成工艺,对其合成过程中的环氧化条件进行了优化,并采用核磁共振对其结构进行了表征;依据2007年3月开始实施的中华人民共和国化工行业标准HG/T 3823—2006《聚环氧琥珀酸(盐)》测定了聚环氧琥珀酸的物理性质。通过对碳酸钙沉积法和电导滴定法的对比试验研究,提出了针对反渗透阻垢剂的快速评价方法,并以此评价了PESA对碳酸钙、硫酸钙、硫酸钡和硫酸锶的动态阻垢性能。
本文以马来酸酐为原料,钨酸钠为催化剂,双氧水为氧化剂,氢氧化钠为引发剂,采用溶液聚合的方法,合成PESA。通过对PESA合成过程中环氧化条件的优化,改善和提高了聚环氧琥珀酸产品的性能,使其对碳酸钙的平均阻垢率提高5%以上。
采用核磁共振对合成的产品进行结构表征。依据HG/T 3823—2006《聚环氧琥珀酸(盐)》对合成的聚环氧琥珀酸物理性质的测定结果为:固含量:41.51%,密度(20℃):1.34 g/cm3,极限黏数:0.033dL/g,pH值(10g/L水溶液):11.31,均符合HG/T 3823—2006标准要求。本文还对PESA中起阻垢作用的基团——羧基的含量进行了测定,结果为21.45%。
通过对电导滴定法和碳酸钙沉积法的试验比较,电导滴定法与碳酸钙沉积法试验结果保持一致,并且电导滴定法的重现性要明显好于碳酸钙沉积法,且具有操作简单方便、试验周期短的优点。碳酸钙沉积法和电导滴定法结果均表明,PESA具有多元阻垢性能,且对碳酸钙、硫酸钙、硫酸钡和硫酸锶的阻垢性能良好。
对反渗透的动态试验表明,自制PESA动态多元阻垢性能良好,可以保证反渗透系统的正常运行。
It is studied the optimize synthesizing method of polyepoxysuecinic acid (PESA), and optimized the epoxidation conditions, made structure token by nuclear magnetic resonance (NMR), measured physical performance of PESA due to Chemical Industrial Standard of the PRC——HG/T 3823—2006< Polyepoxysuecinic acid(salt)>.Using methods of conductivity titration and calcium carbonate deposition to evaluating the diversification scale inhibition, and comparing the results of these two methods,and proposing a fast evaluation method for RO scale inhibitors. We uses this fast evaluation method to evaluating PESA’s performance for carbonate scale, calcium sulfate scale, barium sulfate scale and strontium sulfate scale.
This study uses maleic anhydride as raw material, sodium tungstate as catalyst, hydrogen peroxide as oxidation agent and sodium hydroxide as initiator to synthesis PESA though solution polymerizing. Through futher study of epoxidation conditions, optimize synthesis PESA which performance better than before. The scale inhibition ratio of optimizing PESA are 5% higher than before.
It is made structure token by NMR. Due to the standard HG/T 3823—2006< Polyepoxysuecinic acid(salt)>,this study measured physical performance of self-made PESA. The results of experiment show that self-made PESA’s solid content is 41.51%, density is 1.34 g/cm3, limit viscosity is 0.033dL/g,and pH(10g/L liquid) is 11.31.All the physical performance above are according with the request in HG/T 3823—2006.In addition, this study measured carboxyl content of PESA which is the main group to inhibiting scales. The carboxyl content of self-made PESA is 21.45%.
Comparing the methods of calcium carbonate deposition and conductivity titration, their results has consistency and the conductivity titration’s reproducibility is better than the calcium carbonate deposition’s. And the conductivity titration has many advantages, such as convenient operating, short cycle of test. Both results of calcium carbonate deposition and conductivity titration show that PESA has diversification scale inhibition, and its scale inhibition for calcium carbonate scale, calcium sulfate scale, barium sulfate scale and strontium sulfate scale are good.
Results of dynamic method show that self-made PESA has good dynamic diversification scale inhibition,it could ensure the normal operation of Reverse Osmosis System.
本文以马来酸酐为原料,钨酸钠为催化剂,双氧水为氧化剂,氢氧化钠为引发剂,采用溶液聚合的方法,合成PESA。通过对PESA合成过程中环氧化条件的优化,改善和提高了聚环氧琥珀酸产品的性能,使其对碳酸钙的平均阻垢率提高5%以上。
采用核磁共振对合成的产品进行结构表征。依据HG/T 3823—2006《聚环氧琥珀酸(盐)》对合成的聚环氧琥珀酸物理性质的测定结果为:固含量:41.51%,密度(20℃):1.34 g/cm3,极限黏数:0.033dL/g,pH值(10g/L水溶液):11.31,均符合HG/T 3823—2006标准要求。本文还对PESA中起阻垢作用的基团——羧基的含量进行了测定,结果为21.45%。
通过对电导滴定法和碳酸钙沉积法的试验比较,电导滴定法与碳酸钙沉积法试验结果保持一致,并且电导滴定法的重现性要明显好于碳酸钙沉积法,且具有操作简单方便、试验周期短的优点。碳酸钙沉积法和电导滴定法结果均表明,PESA具有多元阻垢性能,且对碳酸钙、硫酸钙、硫酸钡和硫酸锶的阻垢性能良好。
对反渗透的动态试验表明,自制PESA动态多元阻垢性能良好,可以保证反渗透系统的正常运行。
It is studied the optimize synthesizing method of polyepoxysuecinic acid (PESA), and optimized the epoxidation conditions, made structure token by nuclear magnetic resonance (NMR), measured physical performance of PESA due to Chemical Industrial Standard of the PRC——HG/T 3823—2006< Polyepoxysuecinic acid(salt)>.Using methods of conductivity titration and calcium carbonate deposition to evaluating the diversification scale inhibition, and comparing the results of these two methods,and proposing a fast evaluation method for RO scale inhibitors. We uses this fast evaluation method to evaluating PESA’s performance for carbonate scale, calcium sulfate scale, barium sulfate scale and strontium sulfate scale.
This study uses maleic anhydride as raw material, sodium tungstate as catalyst, hydrogen peroxide as oxidation agent and sodium hydroxide as initiator to synthesis PESA though solution polymerizing. Through futher study of epoxidation conditions, optimize synthesis PESA which performance better than before. The scale inhibition ratio of optimizing PESA are 5% higher than before.
It is made structure token by NMR. Due to the standard HG/T 3823—2006< Polyepoxysuecinic acid(salt)>,this study measured physical performance of self-made PESA. The results of experiment show that self-made PESA’s solid content is 41.51%, density is 1.34 g/cm3, limit viscosity is 0.033dL/g,and pH(10g/L liquid) is 11.31.All the physical performance above are according with the request in HG/T 3823—2006.In addition, this study measured carboxyl content of PESA which is the main group to inhibiting scales. The carboxyl content of self-made PESA is 21.45%.
Comparing the methods of calcium carbonate deposition and conductivity titration, their results has consistency and the conductivity titration’s reproducibility is better than the calcium carbonate deposition’s. And the conductivity titration has many advantages, such as convenient operating, short cycle of test. Both results of calcium carbonate deposition and conductivity titration show that PESA has diversification scale inhibition, and its scale inhibition for calcium carbonate scale, calcium sulfate scale, barium sulfate scale and strontium sulfate scale are good.
Results of dynamic method show that self-made PESA has good dynamic diversification scale inhibition,it could ensure the normal operation of Reverse Osmosis System.
引文
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[15]孙咏红,周晓慧,马磊,等.绿色阻垢剂聚环氧琥珀酸的合成.大连铁道学院学报.2004,25(1):93-95
[16]王风云,吕志芳,董伟,等.聚环氧琥珀酸钠的合成及阻垢性能.应用化学.2001,18(9):746-748
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[19] Brown J Michael,etal .Methods of controlling scale formation in aqueous systems.USA,US5062962,1991
[20]侯振宇,张秋禹,李丹,等.聚环氧琥珀酸钠的合成及其阻垢性能研究.工业用水与废水.2006,37(2):73-76
[21]刘汉玉,梅平,陈武,等.绿色阻垢剂聚环氧琥珀酸的合成试验研究.长江大学学报(自科版)理工卷.20074(2):38-39
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[23] Patel S,Nicol A J.Developing a cooling water inhibitor with multifunctional deposit control properties.Material Performance.1996:41
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[27] Suitor J W, Marner W J, Ritter R B.The history and status of research in fouling of heat exchanger in cooling water servied.Can J Chem.Eng.1997,55:374
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