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针对鞣花酸在实际生产过程中耗时长、纯度低等问题,以单宁酸为基质采用液气射流氧化法制备鞣花酸,考察了金属离子、单宁酸浓度、反应温度和反应时间对鞣花酸得率及纯度的影响。进一步探究了溶剂法、结晶法、碱溶酸沉法、反溶剂法对鞣花酸纯度的影响,并通过高效液相色谱、红外光谱、紫外可见分光光谱和热重对鞣花酸高纯度的样品进行表征。结果表明,其制备的较优工艺条件为:2.5%单宁酸溶液中引入金属离子Na (即NaOH)调节反应液pH至8.5,反应温度20℃,反应时间6 h,该条件制备的鞣花酸经碱溶酸沉后产率为46.72%、纯度84.55%;选取甲醇溶剂洗涤法在65℃条件下处理1h,鞣花酸的纯度达98.13%,回收率为75.03%,提高了鞣花酸的热稳定性。液气射流氧化法与溶剂洗涤法相结合,大幅缩短制备鞣花酸的反应时间并明显提高其纯度,有望在工业生产中提高鞣花酸的生产效率并拓宽其在医药和化妆品领域的应用。 相似文献
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《工程塑料应用》2015,(10)
利用五倍子单宁酸氧化制备鞣花酸,通过响应曲面法优化了合成工艺。采用乙酰氯对其进行外酯化,并与可生物降解材料聚丁二酸丁二酯(PBS)复合,探讨了鞣花酸酯化物(EAE)对PBS结晶形态、热稳定性、力学性能和亲疏水性的影响。结果表明,鞣花酸合成的最佳工艺条件为过硫酸铵0.6 g、碱溶p H=9、反应时间24 h,在此条件下鞣花酸的产量为1.34 g/10 g五倍子粉末。傅里叶变换红外光谱(FTIR)分析表明,鞣花酸及其酯化物均为目标合成物。复合材料FTIR分析表明EAE与PBS只进行了物理共混,两者相似相容。同时,EAE对PBS起到了成核剂的作用,使得复合材料的球晶尺寸变小,热稳定性、拉伸强度、疏水性较PBS均有所提高,断裂伸长率相应降低。 相似文献
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紫外分光光度法测定鞣花酸含量的研究 总被引:6,自引:1,他引:5
研究了用紫外分光光度法测定鞣花酸含量的一种新方法。其技术关键是将鞣花酸试样溶于适量稀碱配制分析试液,从而解决了鞣花酸不溶于水和难溶于多数有机溶剂的难题。确定了鞣花酸的紫外特征吸收峰的测定波长为 357 nm;验证了新方法在测定条件下试液浓度与吸光度之间的线性关系,并测算了测量误差;进行了新方法测定值的稳定性试验。研究结果表明,该方法具有操作较为简便、耗用溶剂少、分析成本较低、测定结果误差小等特点,适用于鞣花酸工业生产质量监控的产品含量分析。 相似文献
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主要研究了4种吐温系列非离子表面活性剂对鞣花酸的增溶作用,其中以Tween-20的增溶效果最好。随Tween-20溶液浓度的增大,鞣花酸增溶量逐渐增大,但Tween-20溶液浓度达到10.00 g/L以上时,鞣花酸增溶量则呈现逐渐下降的趋势。35℃时鞣花酸在10.00 g/L的Tween-20溶液中的增溶浓度达到238.59 mg/L,比鞣花酸饱和水溶液浓度(10.12 mg/L)大了近24倍。随着温度的提高,鞣花酸在Tween-20溶液中的增溶量也略有升高。鞣花酸Tween-20增溶体系对ABTS·和DPPH·的清除率IC50分别为0.31 mg/L和0.92 mg/L,而Vc对ABTS·和DPPH·的清除率IC50则为3.32 mg/L和2.40 mg/L。结果表明在表面活性剂的作用下,大幅提高了鞣花酸的增溶量,而且同时保持了鞣花酸优异的抗氧化性能。通过粒径分析和透射电镜实物验证,鞣花酸Tween-20增溶体系的平均粒径为(272.5±3.62)nm。 相似文献
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Daniel Swern A. J. Stirton J. Turer P. A. Wells 《Journal of the American Oil Chemists' Society》1943,20(11):224-226
Summary Fat-soluble fatty acid monoesters of 1-ascorbic acid (vitamin C) and d-isoascorbic acid have been prepared from lauric, myristic,
palmitic, and stearic acids in 40–50 per cent yields.
Evidence has been presented to show that only the primary hydroxyl group of each of the ascorbic acids has been esterified.
Antioxidant properties of these esters are being studied.
Preliminary tests on the esters have indicated that they may have useful properties as interfacial modifiers. 相似文献
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This study reports the electrohydrodimerization of pyruvic acid to 2,3-dimethyltartaric acid in sulphuric acid medium (0.5 M H2SO4) on a lead cathode. The main products detected were lactic acid and 2,3-dimethyltartaric acid. The selectivity towards the formation of 2,3-dimethyltartaric acid was studied vs. pyruvic acid concentration in sulphuric acid solution, at −1.1 V vs. MSE. The best selectivity of 2,3-dimethyltartaric acid reached 69% for an initial concentration of 1.7 M pyruvic acid. The yield of pyruvic acid was 84%. 相似文献
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Shigenobu Kishino Jun Ogawa Yoriko Omura Kenji Matsumura Sakayu Shimizu 《Journal of the American Oil Chemists' Society》2002,79(2):159-163
After screening 14 genera of lactic acid bacteria, Lactobacillus plantarum AKU 1009a was selected as a potential strain for CLA production from linoleic acid. Washed cells of L. plantarum with high levels of CLA production were obtained by cultivation in a nutrient medium with 0.06% (wt/vol) linoleic acid (cis-9,cis-12-octadecadienoic acid). Under the optimal reaction conditions with the free form of linoleic acid as the substrate, washed
cells of L. plantarum produced 40 mg CLA/mL reaction mixture (33% molar yield) from 12% (wt/vol) linoleic acid in 108 h. The resulting CLA was
a mixture of two CLA isomers, cis-9,trans-11 (or trans-9,cis-11)-octadecadienoic acid (CLA1, 38% of total CLA) and trans-9,trans-11-octadecadienoic acid (CLA2, 62% of total CLA), and accounted for 50% of the total FA obtained. A higher yield (80% molar
yield to linoleic acid) was attained with 2.6% (wt/vol) linoleic acid as the substrate in 96 h, resulting in CLA production
of 20 mg/mL reaction mixture [consisting of CLA1 (2%) and CLA2 (98%)] and accounting for 80% of total FA obtained. Most of
the CLA produced was associated with the cells (ca. 380 mg CLA/g dry cells), mainly as FFA. 相似文献
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以正丁醇为内标,氢火焰离子化检测器测定,建立了气相色谱法直接进样测定乳酸催化制备丙烯酸反应液中乳酸和丙烯酸含量的方法。在载气(N2)流速为30mL·min^-1,氢气流速为88mL·min^-1,空气流速为300mL·min^-1,进样器和离子室温度为160℃,柱温为150℃的10%PEG-20M(3m×3mml填充柱上能实现很好的分离。乳酸和丙烯酸测定方法的线性相关系数分别为0.9994和0.9996,相对标准偏差分别为O.74%和0.56%,平均回收率分别为97.35%-1197.60%,检出限分别为8.62mg·L^-1和1.21mg·L^-1方法简便、快速、准确。 相似文献
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开发研究了氯乙酸副产盐酸的精制工艺及盐酸中有机杂质的紫外分光光度分析方法。副产盐酸经酸洗、吸收、蒸馏得高纯盐酸。中试结果表明 ,工艺合理 ,精制盐酸达到GB 32 0 - 93规定的工业用合成盐酸标准 相似文献
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介绍炼厂酸性气制硫酸装置的工艺过程。由于实供气源与设计值有较大出入,二氧化碳浓度偏高, 并且夹带烃类物质较多,使装置无法正常运行。通过对酸性气进行预处理后,一次开车成功,各项工艺指标均达到设计要求,遇酸性气流量突降时可补充适量硫磺,维持正常生产。 相似文献
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Edwin S. Olson 《Journal of the American Oil Chemists' Society》1977,54(2):51-53
The performic acid oxidation of linoleic acid has been shown to form 9,12-dihydroxy-trans-10,11-methylene-heptadecanoic acid (I) after hydrolysis of the formate ester. A sequence of reactions led to the identification of dimethyl-trans-1,2-cyclopropanedicarboxylate by gas liquid chromatography. Spectroscopic evidence is presented for thetrans geometry in I. Failure of the monoepoxide of linoleic acid to give the formate ester of I suggests the alternative that a homoallylic carbonium ion is formed directly upon attack of the peroxide reagent. 相似文献
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Dr. J. R. Ochoa 《Journal of Applied Electrochemistry》1993,23(9):910-914
The electrosynthesis of iminodiacetic acid by electrooxidation of nitrilotriacetic acid in undivided cells has been studied using Zn, Cu, PbO2, DSA®O2, DSA®Cl2, C, Ni and porous carbon as anodes. Results show that the synthesis is possible in both acid and basic mediums. The best results were obtained in aqueous 40% w/w sulphuric acid with porous carbon RVC-4000 as anode and SUS 316 as cathode, at 60 °C, 400 mA cm-2 and charge 95% of theoretical. Under these conditions, nitrilotriacetic acid conversion was 92%, current efficiency 80% and selectivity 85%. Loss of selectivity was due to chemical side reaction between iminodiacetic acid and HCHO electrogenerated in the electrolysis. 相似文献