WANG Yu-jie , JIANG Guo-qiang , SUN Jia-li , DING Fu-xin
2013, 30(1).
Abstract:Thermosensitive hydrogels are of great potential in in situ implantation for long-term controlled drug release. The present article reviewed the recent research progress in the preparation of thermosensitive hydrogel and the drug delivery system, the body response to and the degradation of the hydrogel, as well as the drug release form the hydrogel. The challenges of implant drug delivery based on thermosensitive hydrogel were presented and the solutions were discussed. The major handicaps in controlled drug delivery of the thermosensitive hydrogel include the flexible network with high water content and low mechanical strength, inducing the body inflammatory responses and invaded by the tissue after implantation, and the individual differences in the degradation and evolution of the network. Many researches developed various approaches to overcome these handicaps. The body inflammatory responses and tissue invading can be mitigated by either improving the hydrophilicity and reducing the positive charge of the hydrogel or incorporation with the anti-inflammatory peptides. The mechanical strength might be promoted by cross-linking, blending hydrophilic polymer in to the hydrogel, or preparing the interpenetrating polymer network, so that the network and water can be maintained for longer period. Further approaches to improve the controlled drug delivery involve building drug diffusion barrier on the hydrogel surface, enhancing the interaction between the drug and the polymer in hydrogel, and the combination hydrogel with drug-loaded micro/nanoparticles.
2013, 30(1).
Abstract:Sepiolite (ST) grafted poly(2 - acrylamido -2 - methylpropanesulfonic acid-co-acrylamide )high-salt superabsorbent resin was synthesized by using microwave irradiation. using sepiolite, 2 - acrylamido -2 - methylpropanesulfonic acid(AMPS) and acrylamide (AM) as raw material. The effects of the concentration of inorganic salt solution, kind of various metal ions and amount of ST on water absorbency of the superabsorbent resin were studied.We had studied the ratio of liquid absorption and water-retention properties of superabsorbent resin. Meanwhile, the microstructure of resin was charactered by FTIR,XRD and SEM. The results indicate that the water absorbency for the superabsorbent resin decreases with increasing concentration of various external saline solutions, and has the following tendency in different metal ions saline solutions:NaCl > CaCl2 > FeCl3, the superabsorbent resin capability of water absorption could be remarkably enhanced by introducing a proper amount of ST. And the superabsorbent resin has a high water-absorbent rate and a good water retentionproperties. FTIR and XRD characterization indicated that ST and organic monomer happened between the grafting copolymerization reaction, The partial monomers were inserted to the ST and the interactaction was formed in the superabsorbent resin. SEM showed that the resin had microporous and laminatestructure.
He Dong-shan , Mai Yu-liang , Yu Lin
2013, 30(1).
Abstract:In ethanol medium, one ternary complex of lanthanum was synthesized using cinnamic acid, 8-hydroxyquinoline and Lanthanum chloride heptahydrate at normal temperature. The complex was tested by EDTA titration, molar conductivity, elemental analysis, infrared spectra(IR), ultraviolet spectra(UV), DTA-TG, and 1HNMR spectra. The composition of the complex was confirmed to be LaL1(L2)2•H2O (HL1= cinnamic acid; HL2= 8-hydroxyquinoline). The antimicrobial properties of Escherichia coli, Staphylococcus aureus, Staphylococcus albus, Bacillus subtilis and Micrococcus luteus showed that: lanthanum ion, 8-hydroxyquinolin and complex had an antibacterial effect, but antibacterial effect of the complex was significantly superior to the ligands.
YU xiang , YU zhi-dong , CHENG li-hua , PAN qi
2013, 30(1).
Abstract:Mg-Al layered double hydroxide (LDH) as a container, loaded with molybdate anions,were synthesized via the coprecipitation method. The resulting compounds were characterized by X-ray diffraction (XRD) and Raman spectra, respectively. The properties of the release of inhibitor and the inhibition mechanism were observed and analyzed by slow-release experiment. The SEM-EDS、ICP and N2 adsorption-desorption measurements demonstrated the excellent anion-exchange and adsorption capabilities for chloride ion . Polarization curves measurements showed that the filtrate as electrolyte exhibited a lower corrosion current density value due to the presence of MoO42-.The result was demonstrated that the released inhibitor can provide adequate corrosion protection, maintaining a corrosion current density at approximately 9.129A穋m-2 for magnesium alloy within 24h. The coatings containing 20% MoO42—LDH pigment keep excellent corrosion resistance by electrochemical impedance spectroscopy (EIS) during immersion in 3.5% NaCl solution.
2013, 30(1).
Abstract:To obtain the non-covalent molecular imprinted polymer with good adsorption properties, the interaction between the template molecule and functional monomer is importance. Molecular dynamics simulations and ultraviolet spectrum (UV) analysis were made to predict the interactions of the chloramphenicol (CAP) and different functional monomer (methacrylic acid (MAA), acrylicacid (AA), acrylamide (AM), methyl methacrylate (MMA)) complex. Firstly, the binding energy (ΔE) of CAP with different monomers is calculated by using the molecular dynamics method, and the ΔE follows the order of MAA>AA>AM>MMA. Secondly, the interaction strength between CAP and different monomers is studied by ultraviolet spectrum analysis, which is in the same order. Thirdly, the static adsorption experiments of the MIPMs and Non-Imprinted Polymers Microspheres (NIPMs) synthesized by using MAA, AA, AM or MMA respectively are studied, the results show that the adsorption performance of MIPMs for template are obviously better than the corresponding NIPMs, and the saturation adsorption capacity for different functional monomers have significant differences as well, which follows the order: MAA>AA>AM>MMA. Based on the experimental results, molecular mechanics calculation and UV analysis, it indicts that MAA is the most suitable functional monomer for CAP among the four monomers, and the molecular dynamics calculation and UV analysis can be used as effective tools for selecting functional monomer for the synthesis of MIPMs. Finally, molecular imprinted polymer microspheres (MIPMs) were prepared by using MAA as functional monomer. Scanning electron microscopy (SEM) shows that the obtained MIPMs has good dispersion, the average size was 8.44 μm,dispersion coefficient was 14.2%. The selectivity of MIPMs prepared by different molar ratio between CAP and MAA were studied by static adsorption method. The experimental results show that the static adsorption distribution coefficient of CAP is much higher than that of other analogs, has the obvious specific identification. In the CAP:MAA=1:4, the separation factor between CAP and Thiamphenicol (TAP) is as high as 4.57, higher than any other separation factor, this experimental result is consistent with the UV analysis results.
2013, 30(1).
Abstract:A cationic surfactant dodecylguanidine hydrochloride was synthesized and the optimized reaction conditions were: n(dodecylamine)∶n(cyanamide)∶n(hydrochloride)=1∶1.5∶1.1, refluxed for 2h in ethyl alcohol solvent. The structure of product was confirmed by IR, 1H-NMR and elemental analysis. The properties of the product were measured, such as surface activity, foaming and emulsifying power, and antimicrobial capacity. Results showed that cmc of the product is 5.5mmol/L, γcac is 24.1mN/m. The product had better foaming and lower emulsifying abilities than DTAC. The inhibitions of cell viability for Staphylococcus aureus and Escherichia coli are 100% at the concentration of 25mg/L and for Candida albicans is 99.5% at the concentration of 100mg/L respectively.
LIU Cheng-yun , RONG Ze-ming , DU Wen-qiang , WANG Yue , QU Jing-ping , LÜ Lian-hai
2013, 30(1).
Abstract:Two kinds of surfactants were used to synthesize a series of [Pd-Pt]/C bimetallic catalysts. These catalysts were characterized and used in selective hydrogenation of quinoline to 1,2,3,4-tetraquinoline. The 5wt%[Pd-Pt(1:3)]/C hold the highest activity among these catalysts. The effect of solvent,temperature,pressure and the initial concentration on the reaction was studied. The conversion of quinoline was 100% and the selectivity of 1,2,3,4-tetraquinoline was up to 100% under optimal reaction conditions: c( quinoline) = 2.4 mol /L,130℃,2.5 MPa, 50min.
YAO Yuan-yong , BHADURY Pinaki-shankar , XUE Wei
2013, 30(1).
Abstract:The intermedia 1c of (R)-3,3’-Bis(diphenylhydroxyl)-2,2’-dihydroxy[1,1’] binaphthalenyl had been obtained by modification of (R)-BINOL at 3,3’ positions under the interaction of n-BuLi, and then had been converted successfully into the potent axially dissymmetric binaphthyl phosphoric acid 2a through selective hydroxyls protection, and phosphonation. The yield arrived to 52%.
SUN Yin-he , HUANG Ren-liang , XING Xiao-xiao , QI Wei , SU Rong-xin , HE Zhi-min
2013, 30(1).
Abstract:A pretreatment method via aqueous ammonia was used before the extraction of solanesol from tobacco leaves. The result of component analysis for tovacco leaves demonstrated that the pretreatment is necessary, and HPLC, MS and SEM analysis illustrated that the positive effect of pretreatment was obvious. The ammonia leaching could dissolve lignin, destroy the cell wall of tobacco, release the solanesol, change the solanesyl ester into solanesol, and dissolve some of the impurities, thereby significantly ehanced the extraction of solanesol and simplified the subsequent purification process. After ammonia pretreatment, the equilibrium time of extraction shortened from 3h to 1.5h, the extraction yield was increased from 89.24% to 104.63%, and the purity of extract increased from 16.72% to 21.03%.
SUN Wei-feng , ZHOU Zhi-lei , YIN Chun-yan , CHEN Mao-shen , LI Yue , ZHONG Fang
2013, 30(1).
Abstract:The comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry was applied to analyze the volatiles of Artemisia argyi leaves extract. 210 components were detected and 65 compounds were identified with high similarity. Most of them were terpenes and their oxygenated derivatives. The pyrolysis of the Artemisia argyi leaves extract was investigated with TG-DSC and pyrolysis apparatus. TG curve showed that the main weight loss occurred between 145~643℃, among which the volatiles lost at 145~465℃ and complex pyrolysis occurred at 465~643℃. The pyrolysis products of different temperatures were identified. The results showed that most of the volatiles including terpenes, alcohols and aliphatic hydrocarbons were directly transferred via distilling. Flavoring substances (furans) as well as harmful compounds (carbonyl compounds, naphthalene, indene) were generated at the pyrolysis zone of 600~900℃.
2013, 30(1).
Abstract:Based on the micron level size of microencapsules prepared by In-situ polymerization method with urea formaldehyde resin as wall material,nano-capsules were prepared with urea-formaldehyde resin as shell,sandalwood fragrance as core and Tween80 as emulsifier.Shell/core ratio, size of emulsified essence,solid content were studied as single effect factor .Three factors’ level was ranged by evaluation of particle size and distribution.It showed that when the system solid content was less than 1%, shell/core ratio of 2:1-5:1, emulsified fragrance particle size for 50-200 nm,well-distributed nano-capsules can be obtained. A quadratic polynomial model between the size of UF partials and the three factors was established by using response surface methodology.In addition, R2 value of the model is 0.9927,while the relative deviation of the verification experiment were within 6%,which showed the model to have good effectiveness in predicting protease production.
2013, 30(1).
Abstract:Ticagrelor, which is a small molecule anti-clotting drug by oral with high selectivity,is platelet activity without the metabolic activation. However, (1 R, 2 S)-2- (3, 4-difluorophenyl)cyclopropanamine is an important intermediate of ticagrelor. The synthetic conditions of the key-step of Corey-Chaykovsky Asymmetric Cyclopropanation reaction were improved based on the reference. The best condition is that: L-menthol as chiral auxiliary agents ; trimethylsulfonium iodide as sulfur-ylide reagent; DMSO: THF = 4: 1 as reaction solvent; reaction temperature was 10 ℃; 10 % CuI as reaction catalyst; the yield is 60.5 %. Based on the reaction, the total yield of the five steps was 20%.
2013, 30(1).
Abstract:A new type of amphiphilic chitosan was synthesized by the attachment of succinyl group and lauroyl group to the CS backbone. Modification was confirmed by FTIR and 1H-NMR.The degree of succinyl,substitution was 41.27%, and the degree of lauroyl substitution was 6.32%. Lauroyl-succinyl chitosan (LSCS) can dissolved at pH<3.0 and pH>6.5,and its solubility decreased in isoelectric point and nearby pH range. The LSCS with long alkyl chain can aggregate in water solution through inter-molecular interaction, so their solutions viscosity increased significantly with the increasing of concentration, and as their concentration was up to 2wt%,, it presents gel-like behavior. The gel was sensitive to NaCl. As the concentration of NaCl increased, the strength of gel decreased.
2013, 30(1).
Abstract:An environmentally benign process has been established for the production of ibuprofen methyl ester, with ibuprofen and methanol as reactants, p-toluene sulfonic acid (PTSA) as catalyst, and glycerol as the adsorbent of water and the solvent of catalyst. The immiscibility of glycerol and ibuprofen methyl ester was exploited in this benign process. The chromatography was used to isolate the products. For whole the process, there is no effluent need to be discharged, neither the synthesis, nor the purification. The reaction conditions have been optimized as follows: the optimal molar ratio of reactants was ibuprofen: methanol: glycerol = 1:10.2:1.4; the optimal amount of PTSA was 1% (w/w) of ibuprofen; optimal reaction time was 4 h; optimum stirring speed was 300r/min. At the optimized condition, the conversion rate can be reached at 97.1%, the yield greater than 95%. Detected by LC/MS, the purity of ibuprofen methyl ester was 99.9%.
2013, 30(1).
Abstract:(S)-10-(1-carbamoylcyclopropyl)-9-fluoro-3-methyl-7-oxo-3,7-dihydro-2H -[1,4]-oxazino[2,3,4-ij]quinoline-6-carboxylic acid, the senior intermediate of pazu- floxacin, was synthesiszed from (S)-ethyl 10-(cyanomethyl)-9-fluoro-3-methyl- 7-oxo-3,7-dihydro-2H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylate, via a one-pot reaction of cyclopropanation and cyanide hydrolyzation. The reaction conditions were optimized as follows: n (Compound II): n(1,2-dichloroethane): n (Benzyltriethylam monium chloride):n(NaOH) = 1:1.5:0.43:16.7,stirred in water for 5h at room temperature and then reflux for 2h. The method has the advantages of mild reaction condition, safety, low cost, and environmental friendly.
LIU Yu-ting , WANG Jie , YIN Da-wei
2013, 30(1).
Abstract:In this paper, two Schiff bases(a and b) of acetylferrocene and two heterocyclic amines(4-aminoantipyrine,2-amino-5-mercapto-1,3,4–thiadiazole)have been synthesized,the rate of production was 85.8% and 72.6% respectively.The structures of these two compounds were characterized by IR,1H NMR and elemental analysis. Finally, the primary antibacterial activities have been screened for these two compounds against three bacterias(Staphylococcus aureus, Escherichia coli, Bacillus subtilis),the result were compared with the antibacterial activity of non- heterocyclic Schiff base(c). Finally, the result indicate that Schiff bases exhibited antibacterial activities against these three bacterias, and bacteriostatic effect along with the increase of the Schiff bases concentration and enhancement.In addition, heterocyclic Schiff bases (a, b ) against on the above three kinds of bacteria bacteriostatic activity are obviously superior to the non-heterocyclic Schiff base (c).
2013, 30(1).
Abstract:A new type adsorbent was prepared by impregnating Zr(Ⅳ) on collagen fiber (ZrCF) and its adsorption performance to remove fluoride and phosphate in aqueous solution was investigated. It was illustrated that ZrCF had a excellent ability of adsorbing both fluoride and phosphate. In the range of pH 4~9, ZrCF maintained a higher adsorption capacity for fluoride, and the maximum adsorption of phosphate was obtained in pH 3.0~6.0. The Langmuir equation could fit the adsorption isotherm of fluoride and phosphate well, and the datum of adsorption rate could be well described by the pseudo-second-order rate model. The coexisting anions such as Cl-, NO3-, CO32- and SO42- had little effect on adsorption of fluoride and phosphate. Column adsorption experiment indicated that ZrCF had more strong affinity to phosphate.
2013, 30(1).
Abstract:The research of this thesis is conducted in micro-channel reactor and the synthesis process of preparing epoxidized fatty acid methyl esters from using fatty acid methyl esters as raw materials . Different reaction conditions including mole ratio of catalyst, resident time, amount of H2O2 and HCOOH, reaction temperature, as well as their effects on epoxidation was tested and evaluated. The optimum conditions were determined as follows:m(fatty acid methyl esters)︰m(HCOOH)︰m(H2O2)=1︰1.5︰2,temperature 40℃, the amount of catalyst 3%, reaction time 110s. The epoxy value is 4.32% under this condition.
2013, 30(1).
Abstract:Under stirring condition, the essence microcapsules were prepared through complex coacervation method by using gelatin and softener di(stearylamidoethyl) epoxypropyl ammonium acetate (ES) as wall materials for the first time. The effects of the dosage of glutaraldehyde, the mass ratio of gelatin to ES, and concentration of gelatin on the shape, size and distribution of microcapsules were studied and characterized by TEM, SEM and particle size analyzer. The results showed that essence microcapsules with regular spherical, uniform particle size distribution were obtained when the mass ratio of glutaraldehyde to gelatin and gelatin to ES were 2.2:1 and 1:0.3, respectively, and the concentration of ES was 1.5% wt%. And the mean size of dry essence microcapsules were less than 1μm. Slow-release performance test showed that the essence microcapsules had excellent slow-release performance. UV-Vis test showed that the essence-loading rate and encapsulation efficiency of cologne essence microcapsules were 41.1% and 95.3%, respectively.
CHAO Mian-ran , SU Huai-gang , LI Wei-min , WANG Xiao-bo
2013, 30(1).
Abstract:Taking diphenylamine(DPA) as the raw material, three different kinds of alkylated diphenylamine (ADPA) antioxidants were synthesized by the alkylation of the raw material with 1-hexene, 1-dodecene and styrene in the presence of anhydrous aluminum chloride respectively. The structure of ADPA was characterized by IR and GC-MS, and the thermal stability and antioxidation performance of ADPA and L57 were investigated by TG and rotary bomb oxidation test respectively. In addition, the synergistic effect between ADPA and T501 as well as ADPA and ZDDP was also studied. The results showed that the content of disubstituted DPA at the para position is more than 80%. ADPA could increase the induce time of base oils 59 times at most when the additive amount is 1%. The synergistic effect between ADPA and the traditional antioxidant was influenced by molecular structure of ADPA.
2013, 30(1).
Abstract:Two kinds of ammonium-based ionic liquid, i.e. n-butylamine nitrate and dodecylamine acetate were synthesized. The effects of ammonium-based ionic liquid and crosslinking polyether demulsifier NJ-20 complexes on the dehydration of simulated crude oil emulsion were studied. When the dosage of 200mg·L-1 and the temperature of 50°C, two demulsifier complexes reached the dehydration rate of 75% and 91% in 2 hours, respectively.Then separate polyether demulsifier NJ-20 can only reach the dehydration rate of 65% at the same conditions. When the dosage of 200mg·L-1 and the temperature of 40°C, dodecylamine acetate complexing demulsifier reached the dehydration rate of 59% in 2 hours, which is much higher than that of polyether demulsifier NJ-20, displaying strong low temperature demulsification effect.
2013, 30(1).
Abstract:A microfoam clean fracturing fluid was obtained under the acidizing fluid system by using non-ionic surfactant (SCF-18) as thickner, NaHCO3 as foam agent. The property of the system was studied. The results show that the optimum formula of acid clean fracturing fluid was 3% SCF-18 0.5% corrosion inhibitor ATMP 3.6% ammonium chloride 1% glacial acetic acid 0.5%NaHCO3. The microfoam acid clean fracturing fluid system had better temperature resistance and shear resistance performance under the condition of 90℃and 170 s-1 .The storage shear modulus G′was higher than loss shear modulus G″when the temperature below 70 ℃, which demonstrated the fracturing fluid has high viscoelasticity.The sedimentation rates of the seeds at 90℃ in the fracturing fluid was 0.7661mm穝-1, which indicated that the fracturing fluid has a better sand-carrying performance. The viscosity of microfoam clean fracturing fluid decreased 2.84 mPa?s during 40 min when the dosage of kerosene was of 5%.With the crosslinking reaction, the CO2 microfoam can apparently reduce the amount of filtration, the damage to the form and improve the flowback rate. It can be concluded that the effect of microfoam acid clean fracturing fluid system is improved.
2013, 30(1).
Abstract::Through investigating the proppant-carring time (Time) of the fracturing fluid,the optimal content of borax, complexing agent, solvent to prepare the organic boron crosslinker YJ-P had been ditermined.In addition,viscoelastic property of the fracturing system had studied by the dynamic rheology . The results showed that, when borax content was 25%, compound complexing agent ratio (m (glucose) : m (MEG)) was1:1.5, ratio of glycerol to water was 6:1 and content of crosslinking agent was 1.2% with low concentration of guanidine gum fracturing fluids, the fracturing system had the optimal proppant-carring performance, the proppant-carring time reached 27 min•mm-1.When the reaction time was determined as 4.0 h, reaction temperature as 80 ℃, the optimal proppant-carring capability of modified organic boron crosslinking agent on the low concentration guanidine gum fracturing fluid had shown up. When minimum effective concentration of guanidine gum reached 0.2%, the dynamic modulus increased with the growth of angular frequency.When the angular frequency was up to 10 rad.s- 1, the G '> G "and G' > 0.1 Pa. The fracturing fluid had optimal viscoelasticity.
WAN Xiu-qin , XU Ze-yue , XU Jian-hua , CAO Feng , XIA Yong-mei
2013, 30(1).
Abstract:Polycarboxylate macromolecule was synthesized using acrylic acid, methacrylate, sodium methallyl sulfonate and allyl polyoxyethylene ether,with ammonium persulphate used as initiator for radical aqueous solution polymerization. The polycarboxylate prolonged the gypsum plaster’s setting time. The plasters containing 0.2% polycarboxylate presented a increase of bending strength and compressive strength of 31.1% and 32.6% in 24 h, respectively. The water absorption rate of the modified plaster was 9.1% lower than that of pure plaster.
2013, 30(1).
Abstract:Sucrose-6-benzoate was synthesized from sucrose and methyl benzoate using cesium carbonate as catalyst, The influence of the catalyst tape, catalyst dosage, reaction temperature, reaction time and material ratio on the yield of the product were investigated. The optimal reaction conditions were: using cesium carbonate as catalyst with a mass fraction of 2% based on the mass of sucrose, the molar ratio n(sucrose): n(methyl benzoate) =1:4, the reaction temperature 45℃, the vacuum degree 0.05MPa, and the reaction time 5 hours. Under the optimal reaction conditions, the yield was 81.0%.
ZHANG Jiang-hua , DOU De-qiang , GAO Xin-qin
2013, 30(1).
Abstract:The deoxygenation of sulfoxides by HfCl4/NaBH4 system was investigated. The effect of reaction parameters, such as solvent, temperature, and molar ratio on the reduction was studied and discussed. According to the experimental result, when the solvent was tetrahydrofuran (THF) and the molar ratio of substrate/HfCl4/NaBH4 was 0.8/0.34/4.0, sulfoxides could be deoxygenated to sulfides in yields of 88%~99% by refluxing 0.6 h~1.5 h with HfCl4/NaBH4 system. Besides, in the oxygenation process,functional groups, such as -NO2, -OMe, -F, -Cl, and -Br groups were tolerated. This method was especially suitable for the deoxygenation of diphenyl sulfoxide and dibenzyl sulfoxide, and the yields were up to 98%~99%.