3-甲基戊酸糠醇酯的合成研究

以3-甲基戊酸为原料,经酰氯化、酯化反应,合成了香料目标化合物。考察了催化剂用量、反应物配比、反应时间、反应温度等对目标化合物收率的影响,结果表明,最佳合成工艺条件为:n(3-甲基戊酰氯)∶n(吡啶)=1∶2,n(糠醇)∶n(3-甲基戊酰氯)=1∶1. 2,反应时间4 h,反应温度50℃,收率达87. 8%。利用IR、1HNMR、13CNMR对目标化合物结构进行确证。     

十一烯酰-L-谷氨酸的制备

十一烯酸分子内有双键和羧基官能团的存在,可发生许多不同的反应而制得各种精细化工中间产品。本文以三氯化磷为氯化剂制备十一烯酰氯,使十一烯酰氯与谷氨酸单钠盐反应制备了十一烯酰-L-谷氨酸。研究了十一烯酰氯制备、十一烯酰-L-谷氨酸的制备条件,结果表明,实验条件下十一烯酰氯的收率可达80%,十一烯酰-L-谷氨酸的单步收率可达97%。     

合成苯基二氯化膦影响因素的分析研究

以苯和三氯化磷为主要原料,合成苯基二氯化膦。通过正交实验优化原料配比和反应时间;确定了最佳原料配比和反应时间;通过对比优选出氯化钠为络合剂,并对其用量和粒径进行优化。结果表明,最佳反应条件为n(苯)∶n(三氯化铝)∶n(三氯化磷)∶n(氯化钠)=1.0∶1.1∶1.3∶1.6,反应时间为4 h,产率达到了91.6%。     

二聚亚麻油酰氯的合成与表征

以二聚亚麻油酸和三氯化磷为原料,经过酰氯化反应有效合成了标题化合物.通过正交实验研究了物料物质的量比、反应温度、反应时间对合成工艺的影响,确定最优工艺条件:n(二聚亚麻油酸):n(三氯化磷)=1:2.8,反应温度为70℃.反应时间6h,所得产品纯度达90%,总收率85%以上.采用IR、1HNMR和13CNMR对目标化合...     

手性拆分剂一水合-L-二苯甲酰酒石酸的合成工艺研究

以L-酒石酸、苯甲酰氯为起始原料,甲苯为溶剂,经过酯化、酐化和水解2步反应得到手性拆分剂一水合-L-苯甲酰酒石酸,并优化了工艺条件。结果表明,在n(L-酒石酸)∶n(苯甲酰氯)=1∶3.1、反应温度为120~125℃、反应时间3.5 h及酸酐水解体系为甲苯/水、n(酸酐)∶n(水)=1∶4、反应温度为100~105℃、水解时间3 h的反应条件下,目标化合物的总收率达84.1%,纯度大于99.5%。该方法反应收率高,后处理简便,污染少,工艺条件易于控制,适合工业生产。     

光稳定剂二苯甲酮合成新工艺研究

以苯甲酰氯、三氯化苄和苯为原料合成二苯甲酮,分别研究了反应温度、反应时间、原料配比、催化剂用量、溶剂的用量等条件对合成反应的影响,确定了最佳工艺条件。该方法合成二苯甲酮的最适宜的工艺条件是:反应温度120℃、反应时间12 h、n(苯甲酰氯)∶n(苯)=1∶1.7,n(苯甲酰氯)∶n(三氯化苄)=7.35∶1,催化剂用量为4.25 g(相对于0.588 mol苯甲酰氯),二苯甲酮的收率可达到94.54%以上,产品纯度二苯甲酮99.5%。     

1,4-二棕榈酰羟脯氨酸的合成工艺

对化妆品用皮肤抗衰老剂1,4-二棕榈酰羟脯氨酸的合成工艺进行了研究。重点对棕榈酰氯与羟脯氨酸缩合反应的摩尔比、反应时间、反应温度、反应介质、pH值等因素进行了考察。得到的适宜的反应条件为:丙酮体积分数为50%、n(羟脯氨酸)∶n(棕榈酰氯)=1∶2.5、pH=9～10、反应温度15℃、反应时间4h。产物经纯化后得到熔点为81～85℃的白色固体粉末。     

山苍子油直接合成柠檬腈

用山苍子油直接同硫酸羟胺反应生成柠檬肟,再加入乙酐和相转移催化剂脱水得到柠檬腈。通过正交实验确定了柠檬肟合成的最佳工艺条件为:n(山苍子油)∶n(羟胺)=1∶1·5,pH=5·5~6·0,反应温度45~50℃,反应时间3·5h,柠檬肟的产率为90·1%。柠檬腈合成工艺为:n(柠檬肟)∶n(乙酸酐)=1∶4,反应温度125~130℃,反应时间1·0h,柠檬腈的产率为78·0%。最后用IR、UV、GC谱对产品做了分析。     

可聚合甲基丙烯酰氧丙基磷酸酯的合成

以三氯氧磷、三乙胺、丙烯酸羟丙酯(HPA)等为原料,通过多步法合成了一种磷酸酯反应型乳化剂。实验对原料配比、反应时间、反应温度等进行讨论,得到最佳工艺条件,并用红外光谱对产品进行结构表征。结果表明,合成甲基丙烯酰氧丙基磷酸酯中间体,选择n(三氯氧磷)∶n(三乙胺)∶n(HPA)=1.1∶1.3∶1,反应时间为1.5h,反应温度为25℃,第二步水解反应温度0~15℃,水解物料比为n(中间体产物)∶n(三乙胺)∶n(水)=1∶1.4∶1.2时,最终产物收率最高,可达98.80%。     

2-萘二硫醚制备新工艺研究

以2-萘磺酰氯为原料,以碘化钾/亚硫酸氢钠/甲酸组成的还原体系制备标题化合物,产物的结构经~1HNMR和~(13)CNMR表征。通过单因素和正交试验,考察反应物物质的量比、反应温度、反应时间等对收率的影响,最终确定合成标题化合物的最优条件为:n(2-萘磺酰氯)∶n(亚硫酸氢钠)=1∶4、n(2-萘磺酰氯)∶n(甲酸)=1∶3. 5、n(2-萘磺酰氯)∶n(碘化钾)=1∶2. 5、水作为溶剂、反应温度为100℃、反应时间2. 5 h,产品收率为69. 7%,纯度可达96%以上。该方法原料易得、操作简单,并实现了对还原剂的部分循环利用,为工业化奠定了基础。     

我国脂肪酸的生产和应用

简要介绍脂肪酸的分类、原料来源、生产工艺、品种以及用途。并对我国脂肪酸的生产现状进行了分析。重点介绍了脂肪酸在我国橡胶工业中、塑料助剂等领域的应用,脂肪酸甲酯作为表面活性剂在不同领域的广泛应用,最后还简述了癸二酸和改性醇酸树脂应用。     

酸液体系的研究现状分析和现场应用

酸化解堵与压裂改造相比,它具有施工相对简单和成本相对较低等特点,所以酸化解堵是一项各油田广泛使用的油气田增产技术。酸化解堵技术已有将近100历史,现已研制出具有不同特点的酸液体系,如乳化酸、泡沫酸、固体酸、多氢酸等,基本能满足复杂地质条件对酸液的要求。     

油酸的精制研究

油酸酰胺是一种很好的塑料添加剂 ,可用作塑料加工成型时的脱膜剂、润滑剂。油酸的原料来源很广 ,牛油、羊油、猪油等动物油油脂以及大豆油、花生油、棕榈油等植物油脂中都含有大量的油酸。由于油酸的来源和生产方法多种多样 ,因此其所含的脂肪酸种类及含量都不尽相同。除油酸外 ,还有亚油酸、亚麻酸等高不饱和脂肪酸。针对油酸中因含有大量的多不饱和组分如亚油酸、亚麻酸而容易产生氧化泛黄的问题 ,采取了尿素络合法对原料油酸进行精制 ,以减少原料中亚油酸、亚麻酸组分的含量。经气相色谱验证 ,产品达到了应用指标 ,提高了产品的抗氧性。     

The Growth‐Inhibiting Effects of Beef Fatty Acids on MCF‐7 Cells Are Influenced Mostly by the Depot Location and Inconsistently by the Biohydrogenation Intermediate Content

Biohydrogenation intermediates (BHI) including conjugated linoleic acid (CLA) isomers are formed during ruminal biohydrogenation of polyunsaturated fatty acids (PUFA) in ruminants. Although many studies have examined the anticarcinogenic effects of CLA, few studies have reported the anticarcinogenic properties of BHI in their natural form found in dairy and beef fats. The present study compared the growth‐inhibitory effects of fatty acids from beef perirenal fat (PRF) or subcutaneous fat (SCF) with low or high levels of BHI in MCF‐7 human breast cancer cells. Cells were exposed for 72 h to media containing increasing doses (50 to 400 μM) of different beef fat treatments. Fatty‐acid analysis showed that BHI were readily incorporated into cell phospholipids (PL) in a treatment‐dependent manner, but higher BHI in PL did not consistently inhibit growth. Culturing with low‐BHI PRF or high‐BHI PRF did not lead to growth inhibition, but low‐BHI SCF inhibited growth, and inhibition was further increased by high‐BHI SCF. Other classes of fatty acids may, therefore, be interacting with BHI resulting in differential effects on growth inhibition in human breast cancer cells.     

磷钼杂多酸的合成研究

介绍了磷钼杂多酸的合成。通过正交试验探讨了反应物料量比、三氧化钼浓度、反应温度和反应时间对产物产率的影响。结果表明,最适宜的反应条件为:反应物量比n(三氧化钼)∶n(磷酸)=12∶1.0、反应温度t=70℃、反应时间7 h、三氧化钼与水的质量比1∶8。经红外光谱分析及熔点测定确定所得产品为磷钼杂多酸化合物。并以磷钼杂多酸取代硫酸作催化剂制备乙酸乙醋来研究其催化活性,并与硫酸做催化剂进行对比实验收率为70.75%,超过硫酸催化剂水平。     

Fatty Acid Profiles in Sunflower Grains During Storage in Different Environments

This study aimed to evaluate the fatty acid profiles of sunflower oil extracted from hybrid grains produced and stored in different environments. The trials were conducted in Teresina (Piauí), Vilhena (Rondônia), and Jaguariúna (São Paulo) in randomized complete block design with 4 replicates. After harvesting, grains from 1 high oleic and 3 traditional hybrids were packed in kraft paper bags and stored in a covered shed and in a cold chamber up to 12 months. The fatty acid profiles were determined by gas chromatography after 0, 4, 8, and 12 months of storage. Analyses of variance were conducted in a split‐plot design, with hybrids being considered as whole plots and storage times as subplots. Tukey's test was performed to compare hybrids and regression analyses for storage times. The initial fatty acid profile of the grains of the same hybrid varied depending on the production location. The grain storage of high oleic and traditional sunflower hybrids during 12 months in covered shed and in cold chamber resulted in little changes in oil fatty acid profiles, regardless of the initial contents. These changes occurred only for linoleic and palmitic acids.     

Fatty Acid Profiles of Oil Obtained from Mid-Oleic Sunflowers Grown in Tropical Region

This study aimed to verify whether the fatty acid profiles of mid-oleic genotypes grown in the tropical region of Brazil fit the Codex Alimentarius and to examine the possibility of using traditional inbred lines to produce high-oleic hybrids. For this purpose, we assessed the fatty acid profile of six mid-oleic hybrids grown in environments with different minimum temperatures during oil formation in the achenes. The tests were conducted between 2015 and 2017 in an experimentally randomized complete block design with four replications. The oleic, linoleic, palmitic, and stearic acid contents were determined using gas chromatography. The mid-oleic hybrids presented varying levels of fatty acids, with oleic acid ranging between 43.6% and 84.6%, linoleic acid between 8.5% and 45.6%, palmitic acid between 3.9% and 5.7%, and stearic acid between 2.2% and 6.2%. Some of the fatty acid values were outside the ranges established by the CODEX STAN 210-1999 and were characteristic of high-oleic type sunflowers. This finding shows that we can take advantage of the potential of combining traditional inbred lines to produce high-oleic hybrids for faster and more economical breeding programs in these environments.     

Quality of Sunflower Oil Obtained in the Main Producing Region of Brazil: Adherence to the Codex Alimentarius

The objective of this work was to evaluate the quality of the oil extracted from sunflower achenes grown in Campo Novo de Parecis, the main producing region of Brazil, to optimize its use by the processing and food industries. In addition, the fatty acid profiles of the oil were checked for their adherence to the CODEX STAN 210–1999. Traditional and high-oleic genotypes were grown between 2014 and 2017 during trials with a randomized complete block experimental design with four replications. The contents of oleic, linoleic, palmitic, and stearic acids were determined using gas chromatography. The fatty acid profiles of traditional genotypes were observed to be outside the ranges established by the CODEX, with an oleic acid content above 39.4% and linoleic, palmitic, and stearic acid values lower than 48.3%, 2.7%, and 5.0%, respectively, as well as high-oleic sunflower oil with a stearic acid content of less than 2.6%. The availability of this information can, on the one hand, positively impact industries and encourage the use of better quality raw materials that are more technologically and nutritionally adequate. On the other hand, the commercialization of sunflower oil with a fatty acid profile outside the ranges established by CODEX can be difficult, because the contents are out of specification due to the climatic conditions in the cropping region.     

质子酸催化合成α-氯代十二酸工艺研究

采用廉价的浓硫酸为催化剂,氧气为自由基捕集剂,以十二酸为原料,经氯化合成α-氯代十二酸。系统考察了反应温度、催化剂用量、氯气流量、氧氯比、反应时间等因素的影响,得到最佳工艺条件:十二酸20 g,在反应温度135℃、催化剂10%、氯气流量50 mL·min-1、vO2/vCl2=1∶2、反应时间3 h,可实现十二酸基本完全转化,目标产物α-氯代十二酸选择性达到94.5%。     

草酸作助剂磷钨酸催化H2O2氧化环己醇合成己二酸

在无有机溶剂、无相转移催化剂条件下,以草酸作助剂,采用磷钨酸催化过氧化氢氧化环己醇的方法来制备己二酸。考察了磷钨酸用量、反应时间、反应温度、过氧化氢用量及草酸用量对己二酸的分离产率的影响,得到最佳工艺条件,即环己醇10.51 mL、磷钨酸0.6 mmol/L、草酸1.0 mmol/L,H2O2(30%)70 mL,温度85℃、时间8 h,己二酸的最大分离产率为77.83%,纯度为99.9%。