本文選題：大孔吸附樹脂 + 硫酸銨��； 參考：《江南大學》2015年碩士論文

【摘要】：羥基乙酸同時兼具酸性、堿性兩種性質,在合成生物降解材料、化學清洗劑及日用化工產品等方面得到廣泛應用。目前國內企業(yè)主要采用羥基乙腈水解法生產羥基乙酸,產品純度低,無法滿足其在有機合成、醫(yī)藥和化妝品行業(yè)上的要求,因此亟需建立簡單、方便、高效的方法來分離提純羥基乙酸。本文采用吸附分離技術研究硫酸銨與羥基乙酸混合液中兩組分的分離提純。在吸附過程中硫酸銨比羥基乙酸提前穿透,而在解吸過程中羥基乙酸比硫酸銨延遲解吸。根據此特性,利用大孔吸附樹脂對混合液進行吸附及解吸實驗,在吸附過程中提純硫酸銨組分,在解吸過程中提純羥基乙酸組分,最終達到兩組分分離提純的目的,同時對兩組分的吸附進行理論分析,為吸附分離技術在混合液中分離提純硫酸銨與羥基乙酸的應用提供理論指導。本文主要研究及結論如下:1.硫酸銨與羥基乙酸混合液中兩組分的分析方法研究本文在甲醛法、酸堿滴定法基礎上引入乙酰丙酮分光光度法,甲醛與乙酰丙酮反應生成有色物質3,5-二乙�；�-1,4-二氫吡啶(DEDHP),測定體系吸光度,改進并建立了混合液中測定硫酸銨和羥基乙酸含量的分析方法:DEDHP分光光度~酸堿滴定聯(lián)合定量分析法。探討了硫酸銨含量、羥基乙酸含量、乙醇濃度、p H值、溫度、時間等因素對該方法測定兩組分含量的影響。該方法適宜條件:p H=5~7,CGA0.9 mg·m L-1,60℃恒溫15 min,測定波長414 nm;兩組分含量測定的相對偏差分別小于1.5%、1.8%。2.大孔吸附樹脂對混合液中兩組分的分離研究分別采用動態(tài)吸附法及解吸法考察了樹脂各性能(極性、孔徑、比表面積)對混合液中硫酸銨與羥基乙酸的吸附、解吸規(guī)律,以穿透容量差(ΔQ)、硫酸銨純化率(ηs)、飽和容量差(ΔQe)、羥基乙酸純化率(ηq)為考察指標,研究吸附過程中硫酸銨的分離及解吸過程中羥基乙酸的分離。根據組分ΔQ與ΔQe的變化規(guī)律發(fā)現(xiàn)樹脂極性越大、比表面積越大或孔徑約為160A°時,樹脂對兩組分的分離能力越強,結合純化率的變化規(guī)律,發(fā)現(xiàn)樹脂HPD950具有最佳分離效果,并確定了分離提純的適宜條件,1)吸附實驗:40℃,料液流速1.5 m L·min-1;2)解吸實驗:40℃,20%的乙醇~水溶液為洗脫液,洗脫流速1.6 m L·min-1。在此條件下,硫酸銨純化率ηs0.9、ηs1.0(純度90%、100%)分別約為51、85 mg·g-1,羥基乙酸純化率ηq0.7(純度70%,工業(yè)級)、ηq0.99(純度99%,醫(yī)藥級)分別約為262、123 mg·g-1。3.HPD950樹脂吸附分離混合液中兩組分的機理研究采用靜態(tài)吸附法研究兩組分在樹脂HPD950上的吸附行為,考察不同溫度、樹脂粒徑、料液濃度對吸附過程的影響,進行吸附熱力學及動力學研究;探究兩組分在吸附過程中的吸附機理。熱力學研究中,樹脂HPD950對硫酸銨的吸附過程符合Langmuir等溫吸附模型,對羥基乙酸的吸附過程符合Freundlich等溫吸附模型,且均為優(yōu)惠吸附;兩組分的吸附過程均為自發(fā)進行(ΔG0)的熵增加(ΔS0)物理放熱(ΔH0,|ΔH|40 k J·mol-1)過程。動力學研究中,兩組分的吸附均為準二級速率動力學過程,擴散過程由顆粒內擴散控制,動力學總方程分別為:硫酸銨：（RTFCr F ×?ù?é-×××=-+---17499exp0786.0)1(213123/29620.0）羥基乙酸:（tRTFCr F ×?ù?é-×××=-+---20521exp1961.0)1(2)1(3123/22554.）
[Abstract]:Hydroxy acetic acid, which has two properties of acid and alkaline, has been widely used in the synthesis of biodegradable materials, chemical cleaning agents and daily chemical products. At present, hydroxy acetonitrile is used to produce hydroxy acetic acid in domestic enterprises. The purity of the products is low, which can not meet the requirements in the organic synthesis, medicine and cosmetics industry. It is urgent to establish a simple, convenient and efficient method to separate the purified hydroxy acetic acid. In this paper, the separation and purification of two components in the mixture of ammonium sulfate and hydroxy acetic acid are studied by adsorption separation technology. The adsorption and desorption experiments of the mixture with macroporous adsorption resin were used to purify the ammonium sulfate component during the adsorption process and to purify the hydroxy acetic acid component during the process of desorption and finally achieve the purpose of separating and purifying the two components. At the same time, the adsorption of the two components was theoretically analyzed to separate and purify ammonium sulfate and hydroxyl in the mixture solution. The application of acetic acid provides theoretical guidance. The main research and conclusion are as follows: 1. analysis methods of two components in the mixture of 1. ammonium sulfate and hydroxy acetic acid in this paper, the acetacetone spectrophotometric method is introduced on the basis of the formaldehyde method, acid base titration, and the reaction of formaldehyde and acetacetone to produce coloured substance 3,5- two acetyl -1,4- two hydropyridine (DEDH P) to determine the absorbance of the system and to improve and establish an analytical method for the determination of the content of ammonium sulfate and hydroxy acetic acid in the mixture: DEDHP spectrophotometric titration combined with quantitative analysis. The effects of ammonium sulfate content, hydroxy acetic acid content, ethanol concentration, P H value, temperature, time and other factors on the determination of the content of the two components are discussed. Suitable conditions: P H=5~7, CGA0.9 mg. M L-1,60 C at constant temperature 15 min, measuring wavelength 414 nm; the relative deviation of two components content determination is less than 1.5%. The separation of two components in the mixture of 1.8%.2. macroporous adsorption resin is studied by dynamic adsorption method and desorption method, respectively, to investigate the properties of tree fat (polarity, pore diameter, specific surface area) in the mixture. The adsorption and desorption of ammonium sulfate and hydroxy acetic acid, by penetration capacity difference (delta Q), ammonium sulphate purification rate (ETA s), saturation capacity difference (delta Qe) and hydroxy acetic acid purification rate (ETA q) as the investigation index, the separation and desorption of ammonium sulfate in the process of adsorption were studied. According to the variation of delta Q and delta Qe, the greater the polarity of the resin was found, the greater the polarity of the resin. The greater the specific surface area or the diameter of the aperture is about 160A degrees, the stronger the separation ability of the resin to the two components. The optimum separation effect of the resin HPD950 is found, and the suitable conditions for separation and purification are found, and 1) the adsorption experiment is 40, 1.5 m L. Min-1; 2) desorption experiment: 40, 20% ethanol solution is elution Liquid and elution flow rate of 1.6 m L. Min-1., the purification rate of ammonium sulfate, ETA s0.9, ETA s1.0 (purity 90%, 100%), is about 51,85 mg. G-1, the purification rate of hydroxy acetic acid (purity 70%, industrial grade), ETA q0.99 (purity 99%, pharmaceutical grade) is about two components of 262123 mg / g-1.3.HPD950 resin adsorption separation mixture respectively. The adsorption behavior of two components on resin HPD950 was studied by adsorption. The effects of different temperature, resin particle size and concentration of material on the adsorption process were investigated. Adsorption thermodynamics and kinetics were studied. The adsorption mechanism of two components in the adsorption process was investigated. In thermodynamic study, the adsorption process of resin HPD950 to ammonium sulfate was in accordance with Langmuir isothermal absorption. The adsorption process of hydroxy acetic acid conforms to the Freundlich isothermal adsorption model, and the adsorption process is preferential adsorption. The adsorption process of the two components is spontaneous (delta G0) entropy increase (delta S0) physical exothermic (delta H0, Delta H|40 K J. Mol-1). In the kinetic study, the adsorption of the two components is all quasi two rate kinetics process and the diffusion process is from the grain In grain diffusion control, the dynamic equations are: ammonium sulfate: (RTFCr F *?? * * * * * =-+---17499exp0786.0) 1 (213123/29620.0) hydroxy acetic acid: (tRTFCr F * * * * * * * =-+---20521exp1961.0) 1 (2) 1 (3123/22554.)

【學位授予單位】：江南大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TQ028;TQ424

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