乙醛酸电合成研究进展

较为全面地总结了乙醛酸制备的技术路线,综合评价其工艺的优缺点;详述了电合成乙醛酸工艺开发方面的情况,总结其最佳工艺条件,提出了存在的问题和今后发展的方向

A high-pressure extraction technique and its application in seed oil

设计并建立一套适用于植物油萃取的高压工艺的实验装置。在温度为12~24℃、压力约6 MPa时,以高压液体二氧化碳对沾油布条的预萃取实验表明,该装置可以在萃取温度下40 min内将油从布条中几乎萃取完毕。在温度为25~40℃、压力为0.4~1.0 MPa下,采用液化气为萃取剂,考察该工艺对完整颗粒的黄豆和花生中植物油的萃取收率。常压条件下,考察了常规使用的正己烷溶剂于不同萃取温度下对完整颗粒的黄豆和花生中植物油的萃取收率的影响。比较2种萃取方式所得同种原料的对应植物油的萃取收率的结果表明:以正己烷为溶剂,常压萃取对豆油的萃取效果较好,萃取温度在正己烷沸点时效果最佳,豆油的萃取收率达2.88%;以液化气为溶剂,采用高压萃取方式对花生油的萃取效果较好,萃取温度在40℃时,花生油的萃取收率达4.91%。An experimental apparatus for high-pressure extraction of seed oil was designed and established.At 14～24℃ and about 6 MPa the apparatus was applied to a model system:cloth adsorbed with oil;the extraction results showed the oil could be quickly extracted into liquid carbon dioxide within 40 min at different extraction temperature,indicating the availability of the technique.At 25～40℃ and 0.4～1.0 MPa the apparatus was employed to extract seed oil from unbroken soybean and peanut respectively by using liquefied-gas as the extractant.Moreover,the oil extraction from unbroken soybean and peanut were also investigated at atmospheric pressure by using conventional hexane as the extractant.The oil yields obtained from the same material by the two methods were compared and analyzed.Results showed that hexane as solvent for extracting soybean at the boiling point of hexane with the extraction rate of 2.88% was more favorable than liquefied-gas implemented at high pressure;liquefied-gas as the solvent at high pressure for extracting peanut at 40℃with the extraction rate of 4.91% was better than hexane.教育部留学回国人员科研启动基金资助项目(项目编号);; 福建省新世纪优秀人才支持计划和福建省自然科学基金资助项目(E0710026

Separation of terpenes and oxygenated compounds from citrus oil by supercritical CO_2 extraction

以冷榨柑橘精油为原料,采用gC/MS对柑橘精油原料进行定性及定量分析,确定了柑橘精油中的7种萜烯类化合物成分作为分离考察对象。实验探讨了超临界萃取压力、萃取温度、萃取时间和CO2流量等因素对含氧化合物分离效果的影响。实验结果表明,萃取相中萜烯类化合物的回收率总体上随着萃取压力、温度、时间和CO2流量的增大而增大。当萃取压力为12MPA,萃取温度为45℃,萃取时间为4H以及CO2流量为1.0l/MIn时,分离效果最佳,其萃取相中萜烯类化合物的回收率高达90.03%。Supercritical CO2 extraction was employed to separate terpenes and oxygenated compounds from citrus oil.The raw oil,the extract,and the raffinate were qualitatively and quantitatively analyzed by GC/MS,respectively,with the terpenes being represented by seven typical compounds.The influences of several experimental factors including extration pressure,extraction temperature,extraction time and CO2 flow rate on the separation of the oxygenated compounds were studied.The results indicate that the recovery rate of terpenes in the extract generally increases with the increasing of extraction pressure,temperature,time and CO2 flow rate.The optimum conditions for extracting terpenes are as follows: pressure 12 MPa,temperature 45 ℃,extraction time 4 h,and CO2 flow rate 1.0 L/min.Under these optimum conditions,the recovery rate of terpenes in the extract is 90.03%.福建省新世纪人才支持项目(0000-X04157

化工原理的纵横向实验教学改革

针对化工原理实验教学中存在的弊病，运用多层次的纵向教学及灵活开放的横向教学，收到了较好的教学效果

Extraction of insecticidal toosendanin from meliaceae by supercritical CO_2

王宏涛(1968-),男,博士,副教授,主要研究方向为天然产物的提取分离等, E-mail: [email protected]。[中文文摘]苦楝素是楝科植物中制备植物源农药的主要杀虫成分。针对不同种源楝树的皮、叶及果实,采用溶剂浸提法提取筛选苦楝素含量较高的种源作为实验原料,采用乙醇提取,考察液固质量比、提取时间和提取次数等参数对苦楝素提取率的影响。当液固质量比为25∶1、提取时间为4 h、提取次数为3次时,苦楝素的提取率达18%。进一步采用超临界CO2萃取考察压力、温度、萃取时间、原料粒径和夹带剂等参数对苦楝素萃取率的影响,当温度为40℃、压力为20 MPa、时间为2.0 h、原料粒径为40目、夹带剂乙醇质量为CO2质量的12.5%时,苦楝素的萃取率达43.5%。在对萃取液结晶纯化中成功分离得到质量分数达98%的苦楝素。[英文文摘]Toosendanin is the main insecticidal component of meliaceae plants for producing botanical insecticides.The extraction of toosendanin from the parks,leaves and fruits of the various meliaceae plants was studied by using ethanol,and the part of the meliaceae plants with the maximal mass fraction of toosendanin was selected as experimental materials.The effects of the mass ratio of liquid to solid,extraction time,and extraction times on the yield of toosendan were investigated by using ethanol extraction method. The yield of toosendanin is up to 18% at them ass ratio of liquid to so lid of 25:1, extraction time of 4h and extract ing 3 times. The effects of pressure, temperature, extraction time, and the partic le size of materials and the dosage of mod if iers on the yield of toosendanin w ere investigated bym eans of supercritical CO2 extraction. The yield of toosendan in is up to 43.5% when ethanol is used as mod ifier with its mass 12.5% of CO2 mass at temperature 40,pressure 20 MPa,extraction time 2h and material particle size 40 mesh. The toosendanin crystal with mass fraction 98% was separated from the extracts by using crystalliza tionm ethod.福建省新世纪人才支持计划项

Electrosynthesis of glyoxylic acid in a static bed reactor with cooled cathode

以过饱和草酸水溶液为阴极液,盐酸溶液为阳极液,在阴极冷却固定床电化学反应器内草酸电解合成乙醛酸。考察了电流密度、电极和电解液温度、阴极材料对合成乙醛酸时空产率和电流效率的影响。结果表明,阴极冷却固定床反应器是一种较理想的反应器,用石墨板作阳极,铅作阴极,电流密度为400.5A/m2,阴极空速u0=0.505m/s,电解温度为20℃左右时,电解1.5h,在阴极可得到质量分数为5.45%的乙醛酸溶液,平均时空产率可达0.12kg/dm3·h以上。Glyoxylic acid was produced by electroreduction of oxalic acid in the static bed reactor with cooled cathode. The cathodic and anodic electrolytes were super-saturated oxalic acid and hydrochloric acid aqueous solutions. The current efficiency and time-space yield of glyoxylic acid were studied under different current densities, temperatures of cathode and electrolyte,materials of cathode. The results indicated that the cooled cathode static bed reactor is an excellent reactor. The average space-time yield of glyoxylic acid is over 0.12 kg/dm~3·h and the concentration of glyoxylic acid can reach 5.45% after 1.5 h electrolysis with cathode of lead and anode of graphite board under conditions of temperature 20℃,superficial flow rate of 0.505 m/s and current density of 400.5 A/m~2 in the cooled cathode static bed reactor.福建省自然科学基金资助项目(F99029

Composite microparticles of ibuprofen/lipid generated by supercritical fluids from their melts

采用CO2及N2辅助的气体饱和溶液微粒形成技术制备布洛芬/肉豆蔻酸、布洛芬/三棕榈酸甘油酯复合微粒,考察它们的形态、颗粒分布以及复合微粒中药物的溶出情况。N2辅助过程制得的布洛芬(质量分数5%)/肉豆蔻酸复合微粒与用该过程得到的纯肉豆蔻酸大小及粒径分布大致相同,而CO2辅助过程制得的布洛芬/肉豆蔻酸复合微粒却要比该过程得到的纯肉豆蔻酸的粒径要大,分布也较宽;CO2及N2辅助形成的布洛芬/肉豆蔻酸复合微粒无缓释效果。用N2辅助制备得到的含20%布洛芬(质量分数)的复合微粒保持了三棕榈酸甘油酯微粒化后的颗粒形貌,粒径更大;用CO2辅助制备得到的含20%布洛芬的复合微粒其粒径比三棕榈酸甘油酯微粒化后的颗粒粒径要小,粒径分布更窄;布洛芬/三棕榈酸甘油酯复合微粒具有缓释效果,而且用N2辅助制备的布洛芬含量为5%的复合微粒比布洛芬含量为20%的复合微粒溶出慢。Using the CO2-assisted and N2-assisted atomization processes,ibuprofen/lipid composite microparticles can be produced;the lipid includes myristic acid(MA) and tripalmitin(TP).The ibuprofen(5% in mass ratie)/MA composite microparticles show similar particle sizes to that of pure MA from the N2-assisted process,while the composite microparticles have a large particle size and particle size distribution,compared to that of pure MA from the CO2-assisted process.The dissolution reveals no controlled release of ibuprofen for the ibuprofen/MA composite microparticles either from the N2-assisted process or from the CO2-assisted process.For the ibuprofen/TP system,the obtained composite microparticles containing 20%(in mass) ibuprofen show similar particle morphology,while has a larger particle size(PS) than that of the pure myristic acid particles in the case of N2-assisted process.Nevertheless,the microparticles from the CO2-assisted process has a small PS and narrow PSD,compared to that of the pure myristic acid particles.The obtained ibuprofen/TP composite microparticles containing 5% or 20% ibuprofen show an evidently controlled drug release.For example,the drug release is only 20% in 500 min for the ibuprofen/TP microparticles containing 20% ibuprofen,prepared by the CO2-assisted process.国家自然科学基金资助项目(20406015);; 福建省新世纪优秀人才支持计划;; 福建省自然科学基金资助项目(2007J0167

Preparation of Tripalmitin Micronization by Supercritical Fluids Technique

利用气体饱和溶液微粒形成技术实验装置,分别用超临界n2和超临界CO2制备三棕榈酸甘油酯微粒,探讨压力、温度以及喷嘴大小等工艺参数对微粒(粒径、粒径分布和形貌)的影响。结果表明:n2辅助过程得到的微粒基本为球状;预膨胀压力越高,粒径越小,粒径分布越窄;100μM喷嘴下制得的微粒粒径最小,且分布较均匀。CO2辅助过程得到的微粒部分为球状,部分为针状和片状;预膨胀压力越高,粒径越小,粒径分布越窄;喷嘴直径大小对微粒平均粒径及粒径分布影响不大;预膨胀温度升高,颗粒的粒径稍微增大。CO2辅助过程得到的微粒粒径比n2辅助过程得到的微粒粒径稍大,但两者的粒径分布相差不大。Generation of tripalmitin microparticles from its melts was investigated by using both supercritical CO2 and supercritical N2.The effects of various operating conditions,such as the pre-expansion pressure,pre-expansion temperature,and nozzle size on the particle morphology,particle size and particle size distribution(PSD) were investigated.Results showed that microspheres were obtained from the N2-assisted process,the particle size decreased and PSD narrowed with the increasing of the pre-expansion pressure,nozzle size showed no obvious effect on the microparticles,and pre-expansion temperature should be less than 72 ℃ to obtain solid particles.From the CO2-assited process,spherical,lamellate and needle-like particles were obtained,the particle size decreased,PSD narrowed with the increasing of the pre-expansion pressure,nozzle size showed no obvious effect on the particles and the pre-expansion temperature slightly increased the average size of particles.Particles' PSD from supercritical CO2 was close to that from supercritical N2

化工实验教学体系模块化构建探索与实践

厦门大学化学工程与技术实验教学中心以培养化工专业创新性人才为目标,结合化工学科知识结构分布及实验教学的特点,对化工实验的教学内容、教学模式及师资队伍建设进行了改革,构建了"层次化、模块化"的教学体系,切实有效地提高了实验教学质量,以期培养新型工科人才。福建省本科高校教育教学改革研究项目(FBJG20170300

Separation and identification of auraptene from grapefruit peel oil

橙油素是广泛存在于柑橘类果实中的天然抗癌活性成分。选用SP70大孔吸附树脂分离纯化葡萄柚精油中的橙油素,该树脂对于橙油素的吸附容量和解吸率分别达到14.53 Mg/g和83.32%,并成功地从树脂床层的洗脱液中结晶分离出橙油素晶体。对所得晶体分别采用差示扫描量热仪(dSC)、紫外吸收光谱(uV)、红外吸收光谱(Ir)、电喷雾质谱(ESI-MS)进行定性分析,分析结果与橙油素标准品相符合。进一步采用高效液相色谱(HPlC)对所得晶体进行定量分析,结果表明所得晶体中橙油素的质量分数可达85%。Auraptene exists widely in the peels and juice sacs of citrus species and is reported to be an effective inhibitor of chemical carcinogenesis in some rodent models.The separation and purification of auraptene from the grapefruit peel oil was performed by SP70 macroporous resin adsorption.The amount adsorbed and the recovery of auraptene were 14.53 mg/g and 83.32% respectively.Auraptene was crystallized out from the concentrated eluate of macroporous resin bed successfully.Differential scanning calorimetric(DSC),ultraviolet spectrum(UV),infrared spectroscopy(IR) and electrospray ionization mass spectroscopy(ESI-MS) were all used to analyze the obtained crystals qualitatively.The analytical results are in accordance with that of auraptene standard.Furthermore,high performance liquid chromatography(HPLC) was utilized to quantify auraptene of the crystals obtained.The mass fraction of auraptene in the obtained crystals can reach 85%.福建省新世纪人才支持项目(0000-X04157