聚氨酯用高羟值大豆油多元醇的合成与表征

本文以大豆油为原料,采用过氧甲酸氧化法制备了高环氧值环氧大豆油(ESO);以氢氧化锂为催化剂,并通过三羟甲基丙烷对其开环合成了高羟值的大豆油多元醇(TESO),研究了反应温度、反应时间对反应进程的影响。用傅里叶红外光谱及1HNMR对其进行表征,结果表明在在190℃下反应4h可以得到高羟基的大豆油多元醇。     

二乙醇胺开环环氧大豆油制备大豆多元醇及其性能表征

以大豆油、冰乙酸和过氧化氢为原料,硫酸为催化剂,合成了不同环氧值的环氧大豆油。再由合成的环氧大豆油与二乙醇胺在四氟硼酸作催化剂的条件下．通过开环加成反应制备了羟基值分别为261mgKOH／g、285mgKOH／g、312mgKOH／g、340mgKOH／g的4种大豆多元醇。用滴定法测定多元醇羟值,用傅立叶变换红外光谱、差示扫描量热法、热重分析法对多元醇进行了分析和表征。结果表明4种多元醇的熔点和热稳定性都随多元醇羟值增大而增大。     

废弃大豆油环氧改性制备多元醇及其表征分析

传统大豆油多元醇的合成具有反应温度高、时间久、需要添加溶剂等缺点。为了使其合成方法简单易行、节能环保,对传统多元醇合成方法进行了优化改进。以废弃大豆油(SBO)自制的环氧大豆油(ESO)为主体,以异丙醇、正丁醇、正戊醇3种一元醇为原料,四氟硼酸(HBF4)为催化剂,在室温下,不添加水和其他溶剂,通过开环反应快速生成3种羟值不同的环氧大豆油多元醇低聚物。利用傅里叶红外光谱、差示扫描量热法、热重分析法、核磁共振氢谱等对聚合产物进行表征,并对产物结构和性质进行分析。结果表明,无需添加溶剂,室温下环氧大豆油开环聚合,反应时间不超过1 min,产物羟值达406 mg/(KOH) g,环氧大豆油转化率达95. 5%。     

植物油基多元醇的合成研究

该文以环氧大豆油(ESBO)和甲醇为原料,在SO42-/ZrO2固体酸催化作用下,通过开环加成反应制备了植物油多元醇(Polyol)。借助红外、核磁共振、热分析等技术对产物结构和性质进行了分析,考察了原料配比、反应温度、反应时间和催化剂用量对ESBO转化率和多元醇合成的影响。结果表明:在反应原料配比n(甲醇)∶n(ESBO)=50∶1,反应温度373 K,反应时间2 h条件下,环氧大豆油转化率为96.8%,羟基值为198.3 mg KOH/g。     

绿色增塑剂环氧大豆油的合成与表征

用自制的催化剂合成了一种环氧大豆油。通过L16(45)正交试验考察了双氧水用量、催化剂用量、反应时间和反应温度对环氧大豆油环氧值的影响。结果表明:在双氧水用量100份、催化剂用量0.5份(大豆油用量定为100份)、反应温度50℃、反应时间12.5 h的最佳工艺条件下,产品的环氧值为6.58%,碘值为0.83 gI/100g。产品通过红外和核磁共振表征,确定大豆油被环氧化生成环氧大豆油。     

钨基催化剂体系下甲醇开环环氧大豆油制备多元醇

以环氧大豆油和甲醇为原料,通过开环加成制备植物油基多元醇。在自制的二氯二氧化钨(WO2Cl2)作催化剂、三氟甲磺酸银(Ag OTf)作助催化剂的条件下,考察了催化剂用量、助催化剂用量、反应时间、温度和醇油物质的量比等对环氧大豆油开环转化率的影响,并对产物的环氧值进行了测试。结果表明,当催化剂用量为3%(以甲醇和环氧大豆油总质量为基准,下同),三氟甲磺酸银用量为4%,反应温度为70℃,反应时间为8 h,醇油物质的量比为28∶1时,环氧大豆油的开环转化率较高,为89.13%。对开环产物进行了FTIR、1HNMR、TG以及流变性分析。通过热重分析得出,多元醇的分解温度(334℃)比环氧大豆油的分解温度(305℃)高。流变性分析得出,随着温度的升高,环氧大豆油和多元醇的黏度逐渐下降。在温度较低时,大豆油多元醇的黏度明显低于环氧大豆油的黏度。     

大豆油基聚酯多元醇的合成及其在聚氨酯泡沫中的应用

以大豆油、苯酐、对苯二甲酸和小分子醇为原料,通过酯化–酯交换反应,制得了酸值0.5mg/g的大豆油基聚酯多元醇。通过FTIR(傅里叶变换红外)、~1H-NMR(核磁共振氢谱)的结构表征,确认了大豆油成功引入聚酯分子链中。同时,考察了大豆油用量对聚酯多元醇品质和聚氨酯泡沫性能的影响。结果表明,原料体系中含有质量分数15%～25%大豆油合成的聚酯多元醇时外观及加工性能较好,由其制备的聚氨酯泡沫的低温尺寸稳定性优异。     

固体超强酸树脂催化合成环氧大豆油的工艺研究

以固体超强酸树脂为催化剂合成了环氧大豆油,分别对催化剂用量、反应温度、过氧化氢用量、乙酸用量及反应时间进行单因素和正交试验,并通过极差分析对环氧化过程中显著影响环氧值的因素进行统计分析。结果表明:最佳的合成工艺条件为反应温度70℃、催化剂用量(以大豆油质量为基准,下同)0.45%、过氧化氢用量85%、乙酸用量7.5%、反应时间4.5h,在此工艺条件下环氧大豆油环氧值可达6.55%。     

环氧大豆油无溶剂法合成研究

介绍了一种环氧大豆油的无溶剂法合成工艺．通过正交实验方法优选了合成工艺条件；讨论了甲酸用量、双氧水用量及滴加速度、催化剂用量、反应温度、反应时问等对产物环氧值的影响。     

磁性固体酸催化制备高羟值植物油基多元醇

以ZrOCl_2·8H_2O和纳米Fe_3O_4为原料,用共沉淀法制备了ZrO_2/Fe_3O_4载体,并以浸渍法将SO_4~(2–)负载于ZrO_2/Fe_3O_4载体上作为活性中心,制得SO_4~(2–)/ZrO_2/Fe_3O_4催化剂。利用FTIR、EDS、XRD等对催化剂的组成、结构、表面酸性、磁性能进行了表征。将此磁性固体酸催化剂应用于甘油作为开环剂的环氧大豆油制备多元醇反应体系中,考察了催化剂用量、温度、反应时间等对开环转化率及产物羟值的影响。结果表明,最佳反应条件为:催化剂用量为环氧大豆油质量的1%,反应温度80℃,反应时间6 h。在该条件下环氧大豆油开环转化率达99%,产物羟值达365 mg KOH/g。     

氢过氧化大豆油还原制备羟基大豆油

用亚硫酸钠还原氢过氧化大豆油制备羟基大豆油,并考察了溶剂种类,溶剂浓度,温度,还原剂亚硫酸钠量及还原时间对反应的影响.在实验条件下,最佳工艺条件为：15℃、以88.2 ％（V/V体系）的乙醇为溶剂、n（Na2SO3）∶n（-OOH）=1.2∶1、反应1.5h.氢过氧化大豆油的转化率达95.8％.     

超声波提取大豆种子中大豆异黄酮的研究

研究了利用超声波提取大豆种子中大豆异黄酮,建立了一种快速测定大批量大豆种子中大豆异黄酮含量的方法.结果表明,提取大豆异黄酮的最佳条件为:提取剂为75%乙醇,料液比为1∶20,提取时间为40 min,提取次数为2次.     

Functionality of dialyzed soybean extract

The soybean extract that was dialyzed against distilled and deionized water and adjusted to pH 7.5 (dialyzed soybean extract; d-SE) gave a transparent liquid after heating. The heated d-SE had less beany flavor and formed a translucent gel by heating again with 0.2 M NaCl. Gelation occurred at a lower protein concentration with NaCl than that of the original soybean extract. The dynamic viscoelasticity showed that the translucent gel from the heated d-SE was melted and gelled by the repetition of heating and cooling, indicating reversible gelsol transition. Cryoprecipitation could be avoided by the heating of d-SE. A gel was formed at 30°C by incubation of d-SE with NaCl. These properties of soybean extract may offer new applications as a food ingredient.     

无味环氧豆油的合成技术研究

本文阐述无味环氧豆油的合成技术，将精制大豆油，乙酸与其它辅料按配方比例投入反应釜，再慢慢滴加双氧水，使之环氧化反应，待反应完全后，经水洗，中和，脱水等一系列工艺，制成无味环氧豆油成品。这种合成方法，工艺简单，产品质量稳定优良。     

Ion chromatographic determination of phosphorus and tungsten in epoxidized soybean oil

Soybean oil has been epoxidized with hydrogen peroxide in the presence of catalytic amounts of trioctylmethyl-ammonium tetra(diperoxotungsto)phosphate. A fast ion-exchange chromatographic method with suppressed conductivity detection has been developed for determining residual contents of tungsten and phosphorus in the oil. Tungsten and phosphorus could be determined at concentrations of 66 and 11 ppm, respectively. At tungsten and phosphorus concentrations of 1000 and 50 ppm, measured repeatabilities were 1.3 and 1.5%, respectively.     

Rigid,thermosetting liquid molding resins from renewable resources. I. Synthesis and polymerization of soy oil monoglyceride maleates

In this study, rigid thermoset polymers were prepared from radical copolymerization of the soybean oil monoglyceride maleates with styrene. In the first part of the study, soybean oil monoglycerides (SOMGs) were obtained from the reaction of soybean oil with glycerol at 220–240°C with an optimization of the reaction to maximize the monoglyceride yield. In the following step, SOMG were reacted with maleic anhydride at temperatures around 100°C to produce the SOMG maleate half esters. Different catalysts and different reaction conditions were examined to increase the maleate half esters' yields. The reactions were followed by IR and ¹H NMR, and the products were characterized by mass spectrometry. In the final step, the radical initiated copolymerization of the SOMG maleates with styrene produced rigid, thermoset polymers. The emulsion copolymerization of the SOMG maleates with styrene was also carried out successfully without the addition of an emulsifier. The obtained polymers were characterized by IR and the crosslinked network structure of the copolymers was examined with the swelling behavior in different solvents. Mechanical properties of the cured resin such as T_g, dynamic flexural modulus, and surface hardness were also determined. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 69–77, 2001     

大豆异黄酮的纯化工艺研究

采用大孔吸附树脂、硅胶、葡聚糖凝胶及反相硅胶RP-18等4种填料的柱层析法纯化大豆异黄酮。结果表明,四种层析填料的纯化效果均较好,大豆异黄酮纯度达30％以上,其中以葡聚糖凝胶为填料的柱层析法分离纯化效果最佳,纯度可达55．45％,提取率为90％。     

Volatile by-products during heat polymerization of soybean oil

Volatile by-products during heat polymerization of soybean oil at 330°C were analyzed using GC-MS and NMR. Color and viscosity changes were monitored for the heat-polymerized soybean oil and the by-products. About 90% (w/w) of the by-products were decanoic, palmitic, linoleic, oleic, and stearic acids and cis-9-tricosene. The by-products also contained small amounts of 3-eicosene, 9,17-octadecadienal, and cyclotetracosene. The weight percentage of decanoic acid increased with reaction time, whereas those of other components showed no trends.     

Soybean drying in fluidized bed. effect on the hydratable and nonhydratable phosphatide concentration in crude and degummed crude oil

The content of nonhydratable phosphatides in soybean crude oil is increased by phospholipase D activity during the oil-making process. Enzyme inhibition would allow to minimize them. Recently harvested soybeans with high moisture levels require adequate drying to store safely. Simultaneous soybean drying and phospholipase D inactivation in a single operation when applying a thermal treatment by the fluidized-bed technique was evaluated. The process conditions for performing the drying and a complete enzyme inhibition on soybeans, with an initial moisture content between 7.4 and 20.6% wet basis, similar to that at the time of the harvest, were fluidizing and drying medium temperature between 110 and 140°C, and a drying time between 1 and 2 min. For the treated soybeans, the phosphorus content increased up to 223% in crude oil and decreased 17% in degummed crude oil with regard to the values of the control sample.     

大豆蛋白复合纤维中异黄酮含量的检测

对大豆异黄酮的结构性能进行了论述,并采用高效液相色谱法(HPLC)对大豆蛋白复合纤维中异黄酮含量进行了检测分析。结果表明:异黄酮主要以糖苷型结构存在于大豆蛋白复合纤维分子中;经洗涤后,异黄酮含量仍然很高。