5—单硝酸异山梨醇酯的合成研究（II）

山梨醇经脱水，酯化，硝酸酯化及皂化，合成了５－单硝酸异山梨醇酯，山梨醇脱水反应：山梨醇与硫酸质量比为１：０．０１４，二甲苯作带水剂，反应温度１４０℃，反应时间３．５ｈ，得异山梨醇（Ｉ）收率６９％，酯化反应：异山梨醇，冰乙酸及对甲基苯磺酸质量比为１：０．４９：０．０３４，溶剂Ｓ兼作带水剂，回流反应，得２－乙酸异山峰果醇酯混合物（ＩＩ），在１０℃，Ⅱ与硝酸质量比为１：０．３６，２ｈ内进行硝酸酯化，得２     

5-单硝酸异山梨醇酯的合成研究(Ⅱ)

山梨醇经脱水、酯化、硝酸酯化及皂化,合成了５ 单硝酸异山梨醇酯。山梨醇脱水反应：山梨醇与硫酸质量比为１∶００１４,二甲苯作带水剂,反应温度１４０℃,反应时间３５ｈ,得异山梨醇（Ⅰ）,收率６９％;酯化反应：异山梨醇、冰乙酸及对甲基苯磺酸的质量比为１∶０４９∶００３４,溶剂Ｓ兼作带水剂,回流反应,得２ 乙酸异山梨醇酯混合物（Ⅱ）;在１０℃,Ⅱ与硝酸质量比为１∶０３６,２ｈ内进行硝酸酯化,得２ 乙酸 ５ 硝酸异山梨醇酯混合物（Ⅲ）;Ⅲ在５０℃、ｐＨ＝１０～１２条件下皂化１５ｈ,得５ 单硝酸异山梨醇酯。总收率２５％。     

2-醋酸异山梨醇酯的合成研究

由山梨醇经脱水、酯化而合成了2-醋酸异山梨醇酯,山梨醇脱水收率达70%,酯化过程分别采用了乙酸和乙酸酐作为酰化剂进行酯化反应.酯化产物经处理后,2-醋酸异山梨醇酯纯度可达85%,经重结晶纯度为97.7%.     

载体型固体酸催化制备异山梨醇

采用不同的载体,制备了多种固体酸催化剂,并对其催化山梨醇脱水的反应活性进行了研究,进一步对催化效果较好的固体酸进行反应条件优化,考察了催化剂用量、反应压力、反应温度和反应时间对山梨醇脱水反应的影响。结果表明,以活性炭为载体的固体酸催化剂催化性能较好。在反应压力为6.3 k Pa,催化剂和山梨醇质量比为1:4,温度为140℃,山梨醇脱水反应6 h的条件下,异山梨醇的收率较高,为91.0%。     

一种二羧酸异山梨醇酯增塑剂的制备方法

正一种二羧酸异山梨醇酯增塑剂的制备方法,该方法以异山梨醇和一元酸为原料,在催化作用下,65℃~250℃,进行酯化反应,反应0.5h~48h。经减压蒸馏,得到二羧酸异山梨醇酯产品。二羧酸异山梨醇酯是一种无毒增塑剂,可替代邻苯二甲酸酯用于电线电缆护套、农用地膜等聚氯乙烯制品的生产。该方     

活性炭负载对甲苯磺酸催化合成山梨醇聚氧乙烯醚油酸酯

以活性炭负载对甲苯磺酸作催化剂,山梨醇聚氧乙烯醚和油酸为原料,合成山梨醇聚氧乙烯醚油酸酯。考察了催化剂用量、反应温度、反应时间等条件对反应的影响。较优的合成条件为:真空脱水,催化剂用量为总物质量的0.25%,反应温度为130～135℃,反应时间为3.0 h,满足指标要求。     

一种连续化生产三醋酸甘油酯的工艺及装置

正本发明公开了一种连续化生产三醋酸甘油酯的工艺,包括以下步骤:a)将甘油、醋酸、带水剂、催化剂组成的混合物送入反应器内140℃~170℃进行酯化反应;b)将所述酯化反应的反应产物送入脱水塔,进行共沸蒸馏脱水,所述脱水塔塔顶温度为85℃~90℃。同时,本发明还公开了一种用于制备三醋酸甘     

优质失水山梨醇单硬脂酸酯的合成

以山梨醇和硬脂酸为原料,采用先醚化后酯化的二步法合成失水山梨醇单硬脂酸酯。研究了各主要影响因素对目标产物的色泽和三项指标(酸值、羟值、皂化值)的影响,研究发现醚化催化剂的种类影响目标产物的色泽;产物的皂化值随硬脂酸与山梨醇物质的量比的减小而减小;产物的羟值随醚化脱水增多而下降。研究得到了适宜的反应条件,即醚化反应条件:温度165℃、时间70min、WH3PO4+KH2PO4=0.60％;酯化反应条件:温度195～200℃、WNa2CO3=0.70％～0.80％、时间180min。经分析,实验得到的目标产物和扩试产物三项指标均合格,产物为乳白色。单酯和双酯的质量分数大于国内同类产物。     

乙酸异丁香酚酯的合成研究

采用催化法合成乙酸异丁香酚酯。对影响酯化反应的主要因素,如催化剂的选择、催化剂用量、酯化温度和酯化时间等进行研究,得出了在无水碳酸钠催化下酯化反应的适宜条件为：酯化温度95℃~100℃,催化剂用量为异丁香酚的3%,异丁香酚和醋酐用量比为1：1.2（摩尔比）,酯化反应时间3h。     

聚氧乙烯山梨醇酐单硬脂酸酯的合成与应用

以山梨醇和硬脂酸为原料,经脱水、酯化、醚化制得聚氧乙烯山梨醇酐单硬脂酸酯,它具有良好的活性,已广泛应用于食品、日化、医药、机械加工等领域。     

Many Drugs of Abuse May Be Acutely Transformed to Dopamine,Norepinephrine and Epinephrine In Vivo

It is well established that a wide range of drugs of abuse acutely boost the signaling of the sympathetic nervous system and the hypothalamic–pituitary–adrenal (HPA) axis, where norepinephrine and epinephrine are major output molecules. This stimulatory effect is accompanied by such symptoms as elevated heart rate and blood pressure, more rapid breathing, increased body temperature and sweating, and pupillary dilation, as well as the intoxicating or euphoric subjective properties of the drug. While many drugs of abuse are thought to achieve their intoxicating effects by modulating the monoaminergic neurotransmitter systems (i.e., serotonin, norepinephrine, dopamine) by binding to these receptors or otherwise affecting their synaptic signaling, this paper puts forth the hypothesis that many of these drugs are actually acutely converted to catecholamines (dopamine, norepinephrine, epinephrine) in vivo, in addition to transformation to their known metabolites. In this manner, a range of stimulants, opioids, and psychedelics (as well as alcohol) may partially achieve their intoxicating properties, as well as side effects, due to this putative transformation to catecholamines. If this hypothesis is correct, it would alter our understanding of the basic biosynthetic pathways for generating these important signaling molecules, while also modifying our view of the neural substrates underlying substance abuse and dependence, including psychological stress-induced relapse. Importantly, there is a direct way to test the overarching hypothesis: administer (either centrally or peripherally) stable isotope versions of these drugs to model organisms such as rodents (or even to humans) and then use liquid chromatography-mass spectrometry to determine if the labeled drug is converted to labeled catecholamines in brain, blood plasma, or urine samples.     

ICP-MS法测定地球化学样品中As、Cr、Ge、V等18种微量痕量元素的研究

建立了测定地球化学样品中包括As、Cr、Ge、V等18种微量、痕量元素的ICP-MS方法。地化试样用HF-HNO3混酸分解后,以1 1 HNO3溶解干渣。由于制样不使用盐酸,避免了Cl对As、Cr、Ge、V的质谱干扰。用国家一级地球化学标准物质GBW 07309制备溶液优化仪器工作参数,并用于校准。方法测定限(6s)为:0.007~6.4μg/g,精密度(RSD%,n=12)为:29%~9.4%,经过国家一级地球化学标准物质的分析验证,结果与标准值吻合。方法已应用于国土资源调查的试样分析。     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.     

基于ATRP法制备的触角状亲水性羟胺树脂的吸硼性能的研究

以大分子引发剂氯乙酰化聚苯乙烯微球(PS-acyl-Cl)经原子转移自由基聚合(ATRP)法引发丙烯酰胺(AM)和甲基丙烯酸缩水甘油酯(GMA)单体的共聚接枝,制得一种触角状亲水性环氧载体(PS-acyl-g-P(AM-co-GMA)),再经二乙醇胺(DEA)的环氧基开环胺化反应,得到一种含多个-NCH2CH2OH螯合配基的多齿-五元螯合环的触角状亲水性羟胺树脂(PS-acyl-g-P(AM-co-GMA)-DEA)。将此树脂用于硼吸附研究,结果表明,PS-acyl-g-P(AM-co-GMA)-DEA树脂对硼的吸附满足Langmuir方程,为单分子层吸附;饱和吸附量约为37.7 mg·g-1,且树脂5 min即可达到吸附平衡,与其它已报道的吸硼树脂相比,该树脂具有更高的吸附量和吸硼速率。吸附动力学研究表明,树脂吸附硼的过程主要由颗粒扩散过程控制。重复使用5次后该树脂的吸附量基本不变,解吸率均在90%以上,重复使用性能良好。