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聚环氧琥珀酸的合成工艺优化及中试试验研究.pdf
李霞
学位类型硕士 ; 硕士
导师吴怀之
2012
学位授予单位中国科学院研究生院
学位授予地点北京
学位专业化学工程
关键词聚环氧琥珀酸 环氧琥珀酸 离子色谱法 阻垢率 中试
其他摘要聚环氧琥珀酸(PESA)是国际公认无磷、非氮、易生物降解的绿色多元阻垢缓蚀剂。PESA可应用范围很广,特别适用于高硬度、高碱性水系中,但在我国其合成技术还处在实验室水平,存在工艺路线不成熟、生产条件因反应过程剧烈而不易控制、反应中间体产率因副反应容易进行而难以控制,以及最终产物质量不稳定等行业技术难题,离工业生产还有一定距离。本论文从工艺、检验、设备与控制四个方面开展了PESA关键技术研究。本研究通过正交试验对聚环氧琥珀酸的合成工艺条件进行了优化,得到了环氧化反应最佳条件为:环氧化pH值为7、氧化剂用量1:1.0、环氧化温度65 、环氧化时间1.5 h;最佳聚合工艺条件为:pH值为12引发剂用量与环氧琥珀酸摩尔比为1:0.15、聚合温度90 、聚合时间2 h对相关检测技术进行了研究,建立了一种利用离子色谱法同时测定环氧琥珀酸合成液中酒石酸、马来酸、环氧琥珀酸、富马酸的方法,测量相对标准偏差为0.30%~2.64%采用氯化溴加成法和碱化-溴加成法测定合成体系中马来酸(盐)含量,与离子色谱分析结果比较,取得了理想的分析效果,相对标准偏差RSD%<5%;开发了用含盐酸的氯化镁饱和溶液作为加成试剂测定环氧值的新方法,并探讨了其最佳反应条件,在反应温度为60 、反应时间为45 min时测量结果的相对误差和精密度都在1%以内;改进了PESA阻垢率测定方法——碳酸钙沉积法(GB/T 16632-2008),将镁离子作为复合指示剂来指示终点颜色变化,使滴定终点从紫红色到蓝色的跃迁明显,提高了滴定终点敏锐度,测定相对标准偏差RSD%<1%,加标回收率在99.5%~100.5%之间。建立了50/PESA 生产装置,系统装备90%以上过程实现全自动运行,反应条件与过程参数控制波动范围小于15%所合成中间体环氧琥珀酸纯度达到97%以上,产品PESA阻垢率在用量为20 mg/L时即达到了90%以上,30 mg/L时达到了98%以上。; Polyepoxysuccinic acid (PESA) is well-known as an non-phosphorus, non-nitrogen, easily biodegradable "green" multivariate scale and corrosion inhibitor. PESA has a wide range of application especially in the high hardness and highly-alkaline water systems. In our country, there are many industrial technical problems in its immature sythesis technology. For example, it is difficult to control the violent reaction process production conditions, and the production rate of the reaction intermediate from side reaction is not easily to be controlled. In addition, the quality of the final product is unreliable as we all know. In this thesis, PESA key technology research is carried out from the following four aspects such as technology, equipment, control and inspection.Based on the orthogonal experiments, polyepoxysuccinic acid synthesis conditions were optimized. The optimal conditions for epoxidation were listed as follows:  pH value at 7, the oxidant at 1:1.0, epoxidation temperature 65 °C and epoxidation time 2 h. The optimal polymerization reaction conditions were listed as follows: pH value at 12, the molar ratio of catalyst over maleic anhydride of 1:0.15, polymerization temperature 90 °C and polymerization time 2 h.By means of the relevant instrumental characterization, a new method was established combining the ion chromatography with quantification of the dosage concentrations of synthetic solution epoxy succinic acid, tartaric acid, maleic acid, epoxy succinic acid and fumaric acid. The relative experimental standard deviation was ranging from 0.30% to 2.64%. By bromine addition method and alkaline chlorination - bromine addition method, the synthetic system of maleic acid (salt) content is determined. Compared with the result of ion chromatography analysis, the relative standard deviation RSD<5%. A new method and optimum measuring conditions were developed using hydrochloric acid-containing magnesium chloride saturation solution as addition reagents to determinate the epoxy value. When the reaction temperature and reaction time were 60 °C and 45 min, respectively, the measuring relative error and accuracy was less than 1%. PESA scale inhibition rate analytical method - calcium carbonate deposition method (GB/T 16632-2008) got improved. Using magnesium- chrome black T to indicate the color change, we made the transition point very evident from amaranth to blue, and improved the sensitivity of titration end point. This method had a higher accuracy and precision, making the RSD < 1% and the standardized recovery range from 99.5% to 100.5.The production facility was established with an annual production capacity of 50 tons PESA. More than 90% of the system process was equipped with fully-automatic operation. The fluctuation range of the reaction conditions and process parameters was less than 15%. The purity of epoxy succinic acid intermediate was above 97%. The scale inhibition rates of PESA with dosing amounts of 20 mg/L and 30 mg/L reached more than 90% and 98%, respectively.
作者部门公共技术服务中心
学科领域公共技术
公开日期2012-11-30
学位类型硕士 ; 硕士
语种中文
文献类型学位论文
条目标识符http://ir.qibebt.ac.cn/handle/337004/1427
专题中试技术服务中心
推荐引用方式
GB/T 7714
李霞. 聚环氧琥珀酸的合成工艺优化及中试试验研究.pdf[D]. 北京. 中国科学院研究生院,2012.
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