本文選題：蒽醌法 + 降解物�。� 參考：《湘潭大學(xué)》2017年碩士論文

【摘要】：蒽醌法是生產(chǎn)雙氧水的主要方法。在生產(chǎn)雙氧水過程中,工作液中容易產(chǎn)生降解物,如不進(jìn)行再生處理,將引起2-乙基蒽醌和四氫-2-乙基蒽醌(EAQ和H4EAQ有效蒽醌)含量的降低,降解物含量的增多,這不僅會導(dǎo)致工作液物理性質(zhì)的改變,使雙氧水產(chǎn)品質(zhì)量下降,還會減少雙氧水的產(chǎn)量。針對以上問題,本文對用于雙氧水工作液再生的新型再生劑制備方法和雙氧水工作液中四氫-2-乙基蒽醌和2-乙基蒽醌及降解物的定量分析方法進(jìn)行了研究。首先,本文利用擬薄水鋁石和MgO為原料制備了用于雙氧水工作液蒽醌降解物再生的新型再生劑。通過研究新型再生劑捏合酸堿介質(zhì)種類及濃度、水熱處理時間和MgO含量等制備條件對再生劑再生效果的影響,采用面積歸一法分析了工作液中有效蒽醌百分含量變化情況,并與原始工作液和工廠目前使用氧化鋁料球再生劑再生后的工作液進(jìn)行了對比。結(jié)果表明,用5%硝酸溶液捏合、12h的水熱處理時間和加入10%MgO含量制備的再生劑再生效果較好,有效蒽醌百分含量達(dá)97.55%,與原始工作液和經(jīng)工廠再生劑氧化鋁料球再生后的工作液相比分別提高了0.53%、0.28%。其次,建立了一種雙氧水工作液中EAQ、H4EAQ和降解物總量的液相色譜定量分析方法。在ShimadzuLC-20A液相色譜儀上,采用Agilent ZORBAX SIL柱,選取正己烷-二氯甲烷-乙酸乙酯體系作流動相,利用硝基苯為內(nèi)標(biāo)物,苯為內(nèi)標(biāo)物溶劑,EAQ和H4EAQ標(biāo)準(zhǔn)物與內(nèi)標(biāo)物的面積比與標(biāo)準(zhǔn)物濃度在30~140mg/L范圍內(nèi)呈線性相關(guān)系,線性相關(guān)系數(shù)大于0.9999。該法在保留時間漂移和峰面積發(fā)生變化的情況下,測定雙氧水工作液中EAQ和H4EAQ的含量,定量結(jié)果相對標(biāo)準(zhǔn)偏差在1%以內(nèi),回收率在99~102%之間。而降解物的計算方法是由面積歸一法與有效蒽醌總量關(guān)聯(lián)得到,即降解物各峰面積之和/(2-乙基蒽醌+四氫-2-乙基蒽醌)面積之和×(2-乙基蒽醌+四氫-2-乙基蒽醌)測定總量,計算得降解物含量。論文最后研究了正相液相色譜法中保留時間漂移的影響因素和解決辦法。采用單因素實驗法,考察了流動相組成和溫度變化對保留時間的影響。在分析過程中,選取了正己烷-二氯甲烷-乙酸乙酯和正己烷-二氧六環(huán)流動相體系對雙氧水工作液進(jìn)行了研究,結(jié)果表明,流動相組分中含有揮發(fā)性組分時保留時間漂移影響明顯;當(dāng)流動相組分中含有易揮發(fā)性溶劑時環(huán)境溫度和柱溫的改變對保留時間的漂移影響明顯。并針對影響保留時間漂移的因素,提出了對應(yīng)的解決辦法。
[Abstract]:Anthraquinone method is the main method to produce hydrogen peroxide. In the process of producing hydrogen peroxide, degradation products are easy to be produced in the working liquid. If not treated by regeneration, the contents of 2-ethylanthraquinone and tetrahydro-2-ethylanthraquinone (EAQ and H4EAQ effective anthraquinone) will decrease, and the content of degradable substances will increase. This will not only lead to the change of the physical properties of the working fluid, but also reduce the production of hydrogen peroxide. In order to solve the above problems, the preparation method of new regenerating agent and the quantitative analysis method of tetrahydro-2-ethylanthraquinone and 2-ethylanthraquinone in hydrogen peroxide working liquid were studied in this paper. Firstly, a new regeneration agent was prepared by using pseudo-boehmite and MgO as raw materials for the regeneration of anthraquinone degradation in hydrogen peroxide working fluid. By studying the effects of preparation conditions such as the type and concentration of kneading acid-base medium, hydrothermal treatment time and MgO content on the regeneration effect of regenerator, the change of effective anthraquinone content in working liquid was analyzed by area normalization method. The results were compared with the original working liquid and the regenerated liquid of alumina ball regenerator. The results showed that the regeneration effect of regenerator prepared by kneading 5% nitric acid solution for 12 h and adding 10%MgO content was better. The effective anthraquinone content reached 97.55%, which increased 0.53% and 0.28% compared with the original working liquid and the working liquid regenerated by alumina ball, respectively. Secondly, a liquid chromatographic method for quantitative analysis of EAQ- H4EAQ and total amount of degradation in hydrogen peroxide working solution was established. In ShimadzuLC-20A liquid chromatograph, Agilent ZORBAX SIL column was used, n-hexane-dichloromethane ethyl acetate system was selected as mobile phase, and nitrobenzene was used as internal standard. There was a linear phase relationship between the area ratio of the standard substance and the concentration of the reference material in the range of 30~140mg/L, and the linear correlation coefficient was greater than 0.9999. With the change of retention time and peak area, the content of EAQ and H4EAQ in hydrogen peroxide solution was determined. The relative standard deviation of the quantitative results was less than 1% and the recovery rate was between 99 and 102%. However, the method of calculating the degradable substance is obtained by the correlation between the total amount of effective anthraquinone and the area normalization method, that is, the sum of the total area of the degradation product, that is, the sum of the total area of each peak area of the degradable product, namely, the sum of the area of the degradation product is the sum of the area of the degradation product 脳 2-ethylanthraquinone tetrahydro-2-ethyl anthraquinone). The content of degradation matter was calculated. Finally, the influence factors and solutions of retention time drift in normal phase liquid chromatography were studied. The influence of mobile phase composition and temperature on retention time was investigated by single factor experiment. In the process of analysis, the mobile phase system of n-hexane-dichloromethane acetate and n-hexane-dioxane ring mobile phase was selected to study the hydrogen peroxide working liquid. When the mobile phase contains volatile components, the retention time drift is obviously affected, and when the mobile phase component contains volatile solvents, the change of ambient temperature and column temperature has a significant effect on the retention time drift. According to the factors that affect the retention time drift, the corresponding solutions are put forward.
【學(xué)位授予單位】：湘潭大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TQ123.6

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