研究香樟树枝叶乙醇提取物的化学成分.采用硅胶柱色谱、Sepha—dex LH一20凝胶柱色谱、半制备高效液相色谱进行分离纯化,根据理化常数和波谱数据鉴定化合物的结构.从樟树中分离到4种化合物单体,分别是①芝麻素,②1,5-辛二烯-3-羟基-3-甲基-7-酮,③二甲基罗汉松脂素,④9-氧代橙花叔醇.化合物①、③是木质素类化合物,化合物②、④是萜烯类化合物.其中化合物①、②、③首次在该植物中得到.用滤纸片法测定了化合物①—④对立枯丝核菌、黄瓜枯萎病菌、玉米大斑病和禾谷镰刀菌的抗菌活性,结果显示化合物②、④有较好的抗菌活性,化合物①有微弱的抗菌活性.
以乙基纤维素(EC)为载体材料,萘普生为包埋药物,采用O/W型乳化-溶剂挥发法制备了包封率较高的EC/萘普生复合载药微球,利用正交试验优化制备工艺,得出当EC与萘普生的质量比为3:1,EC用量2.5%,聚乙烯醇用量0.8%,吐温-80用量0.4%时是复合微球的最佳制备工艺,在该工艺条件下药物包封率达到88.97%.通过扫描电子显微镜(SEM)、激光粒度分析、傅里叶变换红外光谱(FT-IR)对复合微球的形态和结构进行了分析表征.SEM显示复合微球的形态顺滑,激光粒度分析表明复合微球平均粒径为14.014μm,复合微球的FT-IR谱图中既有EC的特征峰,又有萘普生的特征峰,但没有新基团产生,表明EC包覆萘普生过程中未产生新化合物.体外释放实验表明复合微球的累积释药率随溶出介质pH值的增大而增大,在溶出介质pH值为9时,复合微球的累积释药率最大,达到82.5%,缓释性能较好.
Three lignosulfonate fractions ( LG-1, LG-2 and LG-3 ) were obtained by ultrafiltration with two cut-off molecular weight membrane of 6000 and 20000 u. The yield, purity, molecular weight and hydrophilic group content of lignosulfonate fractions were characterized and the performances of lignosulfonate fractions as dust suppressant were also compared. The results showed that ultrafiltration could effectively fractionate the lignosulfonate and the yields of LG-1, LG-2 and LG-3 were 58. 32% , 24. 50% and 17. 18% , respectively. The weight average molecular weights of the three fractions were 4841, 15239 and 37768 and the polydispersities were 2. 78, 2. 40 and 2. 06, respectively. With the increase of lignosulfonate molecular weight, the ash and sulfonic acid group content decreased while the total sugar content increased. The ultrafiltration fractionation had significant effects on the performance of lignosulfonate as dust suppressant. With the increase of molecular weight cut-off, the water absorption capacity, compression strength and anti-wind erosion ability of lignosulfonate increased by 96. 43% , 55. 11% and 63. 07% , respectively, which suggested that lignosulfonate fraction LG-3 with higher molecular weight performed better as dust suppressant. SEM analysis suggested that after spraying of lignosulfonate solution, a bonding layer was formed between sand grains and played the role of cohesiveness and incrustation for the sand grains. Moreover, the phenomenon was more obvious with the increase of lignosulfonate molecular weight.
Water dispersible rosin-based polyester polyol ( WDRPP) was prepared through the method of first fractional melting reaction and then reflux,using maleopimaric anhydride ( MPA) ,neopentyl glycol ( NPG) ,trimethylolpropane ( TMP) ,isophthalic acid (IPA), adipic acid (AA) and 5-sulfoiso-phtalic acid mono sodium salt (5-SSIPA) as raw materials. Effects of reaction time,the amount of catalyst, n(—OH)∶n(—COOH) and the amount of hydrophilic monomer on the reactions were investigated. The products were characterized by fourier transform infrared spectroscopy ( FT-IR) and 13 C NMR. The heat resistance of WDRPP was studied using thermogravimetric analyzer ( TG ) . The thermal degradation kinetic data were analyzed using Coats-Redfem method,and the kinetic parameters were obtained. The results showed that WDRPP with excellent thermostability and the WDRPP dispersion with good stability were obtained when reaction time was 5. 5 h(melting reaction time of 3 h and reflux time of 2. 5 h), the amount of catalyst was 0. 10%, n(—OH)∶n(—COOH) was 1. 4∶1,and the amount of hydrophilic monomer was 2. 86%, respectively. It was found that the temperature at maximum weight loss rate was 406. 7 ℃, the reaction activation energy of pyrolysis was 64. 65 kJ/mol,and the linear curves of thermal degradation kinetics fitted well (R2 =0. 997 3). This indicated that the thermal degradation process of WDRPP followed the law of first-order kinetic reaction. FT-IR and 13C NMR results demonstrated that WDRPP was prepared successfully.
MPP-2K-WPU, PP-2K-WPU and D270-2K-WPU were prepared by crosslinking of hydrophilic-modified polyisocyanate with maleopimaric acid modified polyester polyol ( MPP) , polyester polyol ( PP) and Bayhydrol D270 polyester polyol dispersion, respectively. The products were characterized by FT-IR and DSC. The influences of n(—NCO)∶n(—OH) and type of polyol component on contact angle, surface free energy and water resistance of 2K-WPU films were investigated. The experimental data were analyzed using Equation of State method and Owens-Wendt-Rabel-Kaelble method. The results showed that water series test liquid (water, water-diiodomethane) was better to describe the surface properties of 2K-WPU, if it was compared with formamide series test liquid ( formamide, formamide-diiodomethane) . With increasing of n(—NCO)∶n(—OH) , the surface free energy of MPP-2K-WPU decreased firstly and then increased, and the water resistance increased firstly and then decreased. MPP-2K-WPU exhibited the minimum surface free energy and the strongest water resistance when the n(—NCO)∶ n(—OH) was 1. 5∶1. Compared with two kinds of control samples (PP-2K-WPU and D270-2K-WPU), the surface free energy of MPP-2K-WPU was the minimum, and its water resistance was the best.
Dialdehyde nanocellulose (DNC) was prepared using sodium periodate as an oxidant from nanocellulose (NC). Gold nanoparticles/NC catalyst was further synthesized by using DNC as reducing agent and template. The preparation conditions, chemical structure and crystal structure of catalysis was characterized by UV-vis (ultraviolet visible) spectra, FT-IR (Fourier transform infrared) spectra and XRD (power X-ray diffraction). In addition, the oxidation state and size of gold nanoparticles on the surface of cellulosic carrier was determined by XPS and TEM (transmission electron microscopy). The catalytic performance of the synthesized catalysis was investigated by the reduction of 4-nitropheol with sodium borohydride as a model reaction. It was found that the conversion ratio could be up to 94% after reacting for 55 min, and the catalytic rate constant of catalysis in the reaction was calculated to be 0.073 min-1.
纤维素是自然界中储量丰富的天然可再生资源,因具有可再生性、生物相容性好、环境友好等诸多优点而备受研究者青睐.综述了国内外关于纤维素在离子液体中溶解与再生的研究成果,并探讨了离子液体作为纤维素溶剂可能面临的挑战,对离子液体应用于纤维素溶解的工业化前景进行了展望.
以Yb(OTf)3为催化剂,聚氧乙基-α-生育酚癸二酸酯(PTS)为助溶剂,水为溶剂,经三组分[脱氢枞胺(1)、亚磷酸二乙酯(2)和芳醛(3a ~ 3f)]缩合反应合成了6个含脱氢枞基的α-氨基膦酸酯衍生物(4a~4f),产率65%~75%,其结构经1H NMR,FT-IR和EI-MS确证.考察了溶剂和助溶剂对4a产率的影响.结果表明:在最优反应条件[以水为溶剂,11 mmol,2 1.2 mmol,3a 1 mmol,Yb(OTf) 30.01 mmol,PTS 2 mL,于室温反应1 h]下,4a产率71%.Yb(OTf)3循环使用5次,4a产率64%.
综述了制备纤维素纳米晶体的几种化学方法,包括酸解法、氧化法、酶解法等,并讨论了这几种方法的优缺点.重点介绍了纤维素纳米晶体负载无机纳米粒子复合材料的制备和在催化、酶固定、抗菌剂等方面的应用.
以蔗渣浆为原料,通过2,2,6,6-四甲基哌啶(TEMPO)催化氧化后,超声波处理制备纳米纤维素(NCC),再经冷冻干燥制备了纤维素气凝胶.通过透射电子显微镜(TEM)、傅里叶红外光谱(FT-IR)、热重分析(TG)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)对NCC及其气凝胶形态和结构等进行了研究.TEM显示超声波作用30 min得到的NCC长度为100 ~400 nm,直径为20 nm左右;XRD显示氧化后NCC晶型仍为纤维素Ⅰ型;TG显示NCC相对蔗渣原料热稳定性降低;SEM显示NCC水悬浊液中,NCC质量分数为0.1%时,冷冻干燥得到的纤维素气凝胶为三维网状结构,NCC质量分数大于0.1%时,纤维素气凝胶为"蜂窝状"多孔结构.
采用细乳液两步法制备PSA(压敏胶)用松香衍生物包覆的核/壳型丙烯酸酯乳液.着重探讨了细乳液的聚合条件、氢化松香二甘醇酯(HR-DGE)掺量等对乳液及其PSA性能的影响.研究结果表明:PSA用乳液的最佳聚合条件是w(HR-DGE)=5%、w(APS)=0.8%(均相对于单体总质量而言)、保温时间为2~3 h和保温温度为85℃,此时单体转化率相对最高(>95%);当w(HR-DGE)=4%时,PSA的初粘力和持粘力俱佳;随着HR-DGE掺量的增加,PSA用乳液对BOPP薄膜的润湿性增大、相对分子质量(Mr)下降、Mr分布变窄和玻璃化转变温度(Ts)呈先降后升态势,并且PSA的初粘力略有升高、持粘力明显下降.
The rosin products used in fluxes both at home and abroad, such as rosin, refined rosin, hydrogenated rosin, disproportionated rosin, polymerized rosin, rosin-based polyacids, rosin esters and rosin amine, were reviewed in this paper. Their properties were introduced, too. The future development of modified rosins used in fluxes was finally prospected.
Acrylate emulsion is an environmental-friendly polymer emulsion with excellent performance and board application.But it has poor heat stability,water resistance,contamination resistance and moisture permeability.Rosin was used as modified constitution,which plaied great role in improving the adhesion,water resistance and solvent resistance of acrylate emulsion.Research progress with respect to acrylate emulsion modified by rosin was reviewed from preparation and application of acrylate emulsion modified by rosin.Furthermore the tendency of the development in this field was prospected.
Fumaropimaric acid-type waterborne polyurethanes-acrylate hybird emulsion(FWPUA) were prepared from fumaropimaric acid-type waterborne polyurethanes(FWPU) and methylaerylat(MMA)、butyl acrylate(BA).Effects of initiator type,content and the amount of acrylate on properties of emulsions were studied.The products were characterized by FI-IR spectra.The properties including tensile strength,pendulum hardness,specular gloss and solvent-resistance of products were also tested.FWPUA with excellent comprehensive properties was obtained when azo-bis-isobutyronitrile and ammonium persulfate was used as composite initiator with initiator content 0.8% and the amount of acrylate 30%.
Due to its special molecular structure,Gemini surfactants possess many excellent properties over traditional surfactants,such as surface activity,critical micelle concentration,wettability,water solubility at low temperature,solubilization,rheological property,and lime soap dispersing power.Research and developmental prospects of bio-based Gemini surfactants were emphatically analyzed because of its combined characteristics of Gemini surfactants and natural products.Synthesis and applications of Gemini surfactants made from sugar,oil and rosin were introduced respectively.It is pointed out that convenient synthetic methods and effective mixed systems of Gemini and traditional surfactants will be the research focus in the near future.
Waterborne polyurethane has some drawbacks,such as poor water-resistance,low heat-resistance,low drying rate,low initial adhesion,and low solid content.Much researches to overcome these drawbacks have been carried out.Significant progress has been made in recent years.In this paper,the improvement on water resistance,heat resistance,initial adhesion,solid content and drying speed of waterborne polyurethane are summarized.
The bagasse-based adsorbent was made from bagasse,acrylic acid(AA),acrylamide(AM),and[2-(methylacryloyloxy)ethyl]trimethylammonium chloride(MAETAC)through graft copolymerization.The factors affecting the absorption capacity,such as activated time,neutralization degree of AA,initiator dosage,initiator content were discussed in detail.The optimal preparation conditions were also obtained.The adsorption capacity for Cu2+of bagasse adsorbent made under optimized synthesis condition was 58.53 mg/g,which was 12 times larger than that of bagasse.
Study on the EtOAc participated fraction from the barks of Platanus orientalis Linn. led to the isolation of ( + )-catechin, ( - )-epicatechin, ( + )-gallocatechin, ( - )-epigallocatechin, kaempferol, quercetin, afzelin, isoquercitrin, astragalin-6″-O-gallate, isoquercitrin-6″-O-gallate and tyrosol by column chromatography over Sephadex LH-20. The structures of these phenolic compounds, which have not previously been isolated from its barks, were established on the basis of spectroscopic evidences.
Chemical compositions, including proximate composition, mineral, fatty acid and monosaccharide compositions of inner barks and extractives of the Eucommia ulmoides Oliv. were studied. Carbohydrate (92.97%) was the major constituent in proximate composition of E. ulmoides inner barks. The most quantitatively abundant constituents of fatty acid, mineral and monosaccharide compositions were α-linolenic acid (27.4%), Ca (5.1769mg/g) and glucose (130.51mg/g), respectively. From the water soluble fraction of E. ulmoide inner barks, 5 compounds were isolated and their structures were elucidated as astragalin (1), isoquercetrin (2), quercetin-3-O-xyloglucoside (3), isochlorogenic acid A (4) and isochlorogenic acid C (5) by spectroscopic analyses and chemical evidence. Compounds 3 - 5 were isolated for the first time from this species.
A novel cellulose adsorbent was made from bagasse cellulose,acrylic acid(AA),acrylamide(AM),and [2-(methyl-acryloyloxy)ethyl]trimethylammonium chloride(MAETAC)through graft copolymerization.Factors affecting the adsorption capacity of the product,such as NaOH mass fraction,alkalification time,AA dosage,neutralization degree of AA and AM dosage,were discussed in detail.The optimal conditions were found to be as follows:NaOH mass fraction 30 %,alkalification time 90 min,cellulose dosage 20 %,neutralization degree of AA 60 %,AA dosage 47.3 %,AM dosage 26.3 %,MAETAC dosage 6.4 %,initiator dosage 2.6 %,reaction temperature 70 ℃,reaction time 3 h.Cu2+ adsorption of the adsorbent made under the optimized synthesis condition was 25.1 mg/g.