异丙醇有机定量分析方法建立

用酰化方法对异丙醇有机定量分析方法建立。选择了合适酰化试剂及用量、标准溶液浓度大小、反应时间、反应温度等一系例条件作比较。采用了乙酸酐-高氯酸-吡啶酰化法,乙酸酐-乙乙酸钠酰化法,邻苯二甲酸-吡啶法,分别对异丙醇作具体分析。试验结果,用高氯酸吡啶作催化剂,方法简便,准确度高。用乙酸钠作催化剂,方法较复杂,但可防止伯胺、仲胺干扰,含量稍偏低。用邻苯二甲酸可以防止醛、酚干扰,准确度较高,但酰化试剂用量大,反应时间长。     

Utilization of wastewater from zeolite production in synthesis of flotation reagents

The application of waste alkali liquids as a substitute of sodium hydroxide for the saponification to improve the collection performance of fatty acids was investigated by saponification reaction test and flotation test. The results of the saponification reaction test indicated that the optimal conditions for the saponification were stirring rate of 55 r/min, initial temperature of 40 °C and stirring time of 45 min. Meanwhile, the laboratory scale and industrial scale flotation experiments showed that the fatty acid salt synthesized by wastewater achieved an index comparable to fatty acid sodium synthesized by sodium hydroxide. As a consequence, it was feasible to replace sodium hydroxide with the wastewater from zeolite production for fatty acid saponification. The cross-border utilization of waste alkali liquids not only reduced environmental pollution, but also produced excellent economic benefits.     

蚕蛹油不饱和脂肪酸提取及氧化稳定性研究

以蚕蛹毛油为原料,采用常压碱水皂化制取混合脂肪酸,溶剂法分离高纯度蚕蛹油不饱和脂肪酸。首先在超量碱、皂化温度、皂化时间单因素实验的基础上采用响应面实验优化常压碱水皂化工艺,得到最佳皂化条件为恒定碱液质量分数15%,超量碱45%,皂化温度98℃,皂化时间3.3 h;其次通过甲醇溶剂法得到高纯度蚕蛹油不饱和脂肪酸工艺条件为恒定结晶温度-10℃,料液比为1∶2.4(混合脂肪酸与溶剂甲醇质量比),甲醇溶液质量分数90%,结晶时间30 min;最后脱色后得到蚕蛹油不饱和脂肪酸产品,并对其理化指标测定。产品在不同贮存条件下保存32 d考察其氧化稳定性,结果表明在4℃条件下避光保存并添加抗氧化剂的产品稳定性最好。     

A Novel Sample Preparation Method Using Rapid Nonheated Saponification Method for the Determination of Cholesterol in Emulsified Foods

Abstract: In this study, nonheated saponification was employed as a novel, rapid, and easy sample preparation method for the determination of cholesterol in emulsified foods. Cholesterol content was analyzed using gas chromatography with a flame ionization detector (GC‐FID). The cholesterol extraction method was optimized for maximum recovery from baby food and infant formula. Under these conditions, the optimum extraction solvent was 10 mL ethyl ether per 1 to 2 g sample, and the saponification solution was 0.2 mL KOH in methanol. The cholesterol content in the products was determined to be within the certified range of certified reference materials (CRMs), NIST SRM 1544 and SRM 1849. The results of the recovery test performed using spiked materials were in the range of 98.24% to 99.45% with an relative standard devitation (RSD) between 0.83% and 1.61%. This method could be used to reduce sample pretreatment time and is expected to provide an accurate determination of cholesterol in emulsified food matrices such as infant formula and baby food. Practical Application: A novel, rapid, and easy sample preparation method using nonheated saponification was developed for cholesterol detection in emulsified foods. Recovery tests of CRMs were satisfactory, and the recoveries of spiked materials were accurate and precise. This method was effective and decreased the time required for analysis by 5‐fold compared to the official method.     

Supercritical Carbon Dioxide Extraction of Marigold Lutein Fatty Acid Esters: Effects of Cosolvents and Saponification Conditions

Extraction of lutein fatty acid esters from marigold flower using supercritical carbon dioxide (SC-CO₂) with cosolvent was investigated. Without the cosolvent, the total xanthophylls yield increased with increasing temperature and pressure of SC-CO₂, and the optimal condition was found to be at 60°C and 40 MPa. At this condition, the highest total xanthophylls percent recovery was 74.4 ± 0.9%. Palm oil was found to be a more efficient cosolvent than soybean oil, olive oil, and ethanol, resulting in a 16% increase in the total xanthophylls recovery to 87.2 ± 4.4% when 10% (w/w) of palm oil was used. Furthermore, saponification of the oleoresin for 3 h at 75°C with 40% w/v KOH solution at the oleoresin to solution ratio of 1 g to 2 ml was found to suitably convert lutein fatty acid esters into free lutein.     

茶油脱臭馏出物中甾醇精制的研究

采用乙醇萃取VE,皂化法提取茶油脱臭馏出物中甾醇化合物,以正己烷为结晶溶剂对甾醇化合物进行重结晶。VE最佳萃取参数:液料比3:1,搅拌时间30min,萃取温度55℃,搅拌速度80r/min。甾醇最佳的提取工艺条件:碱料比1(KOH):5,醇料比15(乙醇):1,皂化时间3h,温度85℃;最佳结晶工艺条件:液料比3:1,溶剂正己烷,结晶温度-2℃,结晶时间24h,三次重结晶后精制甾醇的纯度可以达到89.3%。     

水箱拉丝机润滑剂的研制

以生产实际为基础,介绍不同钢丝拉拔与润滑剂配合的生产性试验,分析润滑剂成分对拉丝生产的影响。研制出用水箱拉丝机生产中高碳光面钢丝和镀锌钢丝皂液的配方,给出皂液性能控制的3个技术指标,介绍皂液的生产、维护、化验方法。     

环己酮生产中皂化废碱液的资源化利用及处理

介绍了环己烷液相氧化法生产环己酮过程中皂化废碱液的资源化利用及处理方法,该方法的工艺步骤为:向皂化废碱液中通入足量的二氧化碳气体进行碳酸化反应,固液分离后提取碳酸氢钠,经煅烧后获取碳酸钠;蒸发分离残液,脱出其中50%的水分,脱出的水经生化处理达标排放;在蒸发残液中加入硫酸进行亲电取代反应,固液分离后提取硫酸钠和皂化油,同时处理反应过程中产生的废气;将皂化油在蒸馏釜内进行蒸馏,提取一元有机酸和清洁燃料油。