2011, 28(8).
Abstract:KH-570 coating nanosized Antimony Doped Tin Oxide (ATO) particles were obtained by the ATO functionalized with silicon coupling agent KH-570 in the mixed media of ethanol and deionized water. The surface structure and the property of the obtained nanosized ATO particles were characterized by a series of tests such as FTIR, XPS, TG, TEM, etc. The grafted ratio of KH-570 and the surface modified mechanism of ATO with KH570 were further discussed here. Results revealed that about 7.36-7.73wt% of KH-570 had been successfully grafted onto the surface of ATO. The lipophilicity and the dispersibility of the modified nanosized ATO particles were significantly improved which could be dispersed stably in n-butanol for more than 100h. The mechanism illuminated a network structure silicon coupling agent layer was formed on the surface of the ATO particles during the grafting reaction with the help of the supersonic wave, which gives a good performance of the lipophilicity and the dispersibility of these obtained nanosized ATO particles.
2011, 28(8).
Abstract:Abstract: In this paper, P(AA-AM-VAc)/OMMT superabsorbent composite resin was synthesized by aqueous solution polymerization based on acrylic acid(AA), acryamide(AM), vinyl acetate(VAc) and organic montmorillonite(OMMT). The optimal polymerization condition was achieved by investigating the effects of factors, such as polymerization temperature, monomer tatio, content of initiator, content of cross linker, neutralization degree of acrylic acid, and content of organic montmorillonite on the absorbency of the superabsorbent composite resin. The structure of the resin was characterized by Fourier transform infrared spectroscopy(FT-IR). The results showed that the water absorbency rate of the superabsorbent composite resin prepared under optimal condition was up to 695g/g for water and 113g/g for 0.9% salt water.
2011, 28(8).
Abstract:Glycidyl ether polyhedral oligomeric silsesquioxanes (POSS-EP) was prepared in high yield by hydrolysis and condensation of 3-glycidyloxypropyltrimethoxysilane (EPTMS). Through a thermal copolymerization between G4 PAMAM dendrimers and blends of POSS-EP and bisphenol A epoxy resin (DGEBA), a series of epoxy-based POSS/PAMAM hybrid materials was obtained. Thermal copolymerization reaction was characterized by differential scanning calorimetry (DSC) and a reaction activation energy (Ea) was calculated by Kissinger’s model. Thermal and mechanical properties for the hybrid materials obtained under different copolymerization conditions were studied by DSC, thermogravimetric analysis (TGA) and tensile test. The results revealed that owing to the presence of POSS groups and the specific role of structure-properties relationship for PAMAM tree-structure, these epoxy-based POSS/PAMAM hybrid materials exhibited excellent thermal stabilities and mechanical properties.
ZUO Fang , AN Peng , ZHENG Zhaohui , DING Xiaobin , PENG Yuxing
2011, 28(8).
Abstract:The supramolecular system was obtained using poly(N-isopropylacrylamide) with ferrocene as side groups (poly(NIPAM/FCN)) and ?-CD polymer. The inclusion action was investigated by several techniques, including 1H NMR spectra, cyclic voltammetry, UV-vis spectra and dynamic light scattering measurements. The results showed that ?-CD (or ?-CD polymer) could interact with the reduced ferrocene side groups and hardly affect the oxidized form, and the solution properties could be regulated by redox reaction.
NIU Yan-hua , TIAN Senlin , Yang Zhi
2011, 28(8).
Abstract:A novel redox-active cationic surfactant (11-Ferrocenylundecyl) trimethylammonium Bromide (hereinafter referred to FTMA) was synthesized by the main method of Friedel-Crafts reaction and Amination reaction. The synthesized target compounds were characterized by 1H NMR and 13C NMR, the purity of FTMA was 97%.Surface tensions of FTMA and FTMA+ were measured at 30℃ condition used the platinum plate method. The critical micellar concentration (CMC) values were changed from 0.6mmol/L to 1mmol/L when FTMA was oxidized to FTMA+, resulting the surface activity occurred significant changes, the surface tension value was also increased from 38.5mN•m-1 to 55.3 mN•m-1 at the concentration of the CMC. The electrochemical behavior of FTMA in 0.2 mol/L Li2SO4 solution was investigated by cyclic voltammetry methods. Results indicate that the oxidation potential and reduction potential were 0.457V and 0.4168V respectively, the ΔEp is 40.2mV, and the ratio of Ipa/Ipc is 1.26.So FTMA possessed well reversible characteristic, which realized reversibility between reduction and oxidation freely. Otherwise, we finished the changes between FTMA and FTMA+ by electrochemical method. So the surface activity of FTMA can reversible controlled through electrochemical switchable method, and it may be a new kind of surfactant which can be used to the reversible surfactant-enhanced remediation .
2011, 28(8).
Abstract:Three allyl-type maleate diesters have been synthesized,use three long-chain fatty alcohols (octanol, dodecanol, tetradecyl alcohol), maleic anhydride, allyl chloride as the main raw material. By orthogonal and single factor experiments, the optimum reaction conditions were obtained as follows, single-esterification reaction, n (maleic anhydride): n (long chain alcohol) = 1.10:1.00, the temperature was 85 ℃, the time was 2h; double-esterification reaction, n(octyl sodium salt of maleic acid monoester) : n (allyl chloride) = 1:2.5, the temperature was 60℃, the time was 7h, n( Dodecyl sodium salt of maleic acid monoester) : n (allyl chloride) = 1:2.0, the temperature was 60℃, the time was 6h, n (tetradecyl sodium salt of maleic acid monoester): (allyl chloride) = 1:2.0, the temperature was 65 ℃, the time was 6h. The products of each step were characterized by IR and 1HNMR.
GE Ying-yong , HOU Jing-tao , ZHANG Min , LI Hong-qiang
2011, 28(8).
Abstract:Alkyl hydroxamic acid was synthesized directly from coconut oil and hydroxylamine hydrochloride by hydroxylamine-coconut oil method under the catalysis of sodium hydroxide.The synthetic product was confirmed the existence of alkyl hydroxamic acid by qualitative detection using Fe3+ and analysising infrared spectra of coconut oil and products. The effects of the mass ratio of feed,reaction temperature,addition rate of NaOH and reaction time on the conversion rate of product were investigated.The results showed that the content of product could be up to 77.6%,when the mass ratio of feed was n(Coconut oil):n(NH2OH•HCl):n(NaOH)=1:3.30:7.26,the reaction temperature was 28℃,the addition rate of NaOH was 1.67ml/min and the reaction time was 8h. The new procedure has the advantages of not experiencing esterification with poisonous methanol,direct oximation,simple operation and environmental friendly.The alkyl hydroxamic acid was applied to low grade of phosphate floation and the good result was obtained that the concentrate grade of P2O5 was 30.55%,the recovery of P2O5 was 79.18%, tailings grade of P2O5 was 6.89%,which showed that the alkyl hydroxamic acid has a good selection performance. on the low grade phosphate rock flotation.
2011, 28(8).
Abstract:Using the raw materials to produce biological and chemical combination production and biomass energy have become a global strategy for sustainable development. In this study, corn stover was pretreated by using the newly steam explosion to separate the components at first. Then zinc chloride solution was used to destruct the crystallinity of cellulose. Based on the single factor experiments, the effects of zinc chloride concentration, pretreatment time and temperature were investigated by response surface methodology. A mathematical model was established and analyzed to describe the relationships between the studied factors and the response of the cellulose solubility of corn stover. The structures of untreated/treated corn stalk were detected by Scanning Electron Microscope (SEM) and X-ray diffraction (XRD) .The optimum pretreatment parameters were as follows: zinc chloride concentration of 87%, pretreatment time of 49 min and pretreatment temperature for 139℃. Under the optimum conditions, cellulose solubility of corn stover of 1g was up to 0.762g.
LIN Yuan , LIN Li-qin , LIN Wen-shuang , HUANG Jia-le , HE Ning , WANG Hai-tao , SUN Dao-hua , LI Qing-biao
2011, 28(8).
Abstract:Quasi-spherical silver nanoparticles (AgNPs) were synthesized by the extracts of different medicinal plants including Syzygium aromaticum, Cornus officinalis, Prunus mume and Sanguisorba officinalis, and were characterized by UV-Visible spectroscopy, transmission electron microscopy and X-ray diffraction. When pH values of the extracts were adjusted to 10, the biosynthesized AgNPs were well-dispersed and highly stable, and are relatively small in size. Thus obtained AgNPs were found to demonstrate good antibacterial activity against Escherichia coli and Staphylococcus aureus, with minimum inhibition concentrations of 1.69 and 3.38 μg/mL required, respectively.
2011, 28(8).
Abstract:The volatile compounds were extracted in the different parts of Melilotus indica (Linn.) All. by microwave-assisted headspace solid-phase micro-extraction(MAE-HS-SPME). Their constituents were analyzed and identified by gas chromatography-mass spectrometry combined with Kovats retention index. The results showed that 43 volatile constituents in the stem, 44 in the leaf and 71 in the flower of Melilotus indica (Linn.) All. were separated and identified. Accounting for 89.92 %、83.12% and 90.77% of the total peak areas, respectively. Which is the main component in stem 3,4-dihydrocoumarin (5.97%),dihydrocoumarin (55.29%) and Hexadecanal (4.44%). And in the leaves 3,4-dihydrocoumarin (11.84%) and dihydrocoumarin (48.15%). And in the flowers 3,4-dihydrocoumarin (6.08%),dihydrocoumarin (27.44%),p-isopropylanisole (6.20%) and thymol (5.19%). It was also observed that there were significant differences in the relative contents of three parts.
汪洪武 , LIU Yan-qing , WEI Shou-lian , YAN Zi-jun , ZHU Hong-liu
2011, 28(8).
Abstract:In this paper, the constituents of essential oils which extracted with hydrodistillation from the herbal pair Cortex Magnoliae Officinalis -Herba Ephedrae (CMO-HE) and its signal herbs were analyzed by capillary GC-MS and elucidated based on the standard mass spectral data. 44, 38 and 39 kinds of volatile components were identified respectively. Relative mass fractions of the constituents were determined by area normalization method. The identified relative contents of essential oils were 98.42%, 99.07% and 99.21%, respectively. It is further demonstrated that 28 and 25 volatile constituents of CMO-HE are from that of single herb CMO and HE, respectively. Ten kinds of new volatile compounds in CMO-HE are produced because of the chemical reactions and physical changes occurred in the process of decocting two single herbs.
2011, 28(8).
Abstract:The identification of aroma compounds, formed from the model reactions of L-ascorbic acid and L-cysteine with or without urea at two different initial pH values (5.0, 8.0) and 140?癈 for 2h, was performed using a solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) technique. The effect of urea on aroma compounds was investigated. 47 aroma compounds were identified. The results showed that sulfur-containing compounds such as alicyclic S compounds, thiophenes and thienothiophenes were the most abundant compounds. Other compounds identified were furans, thiazoles and pyrazines. The addition of urea into the reaction mixture in general caused a reduction or disappearance in content of some sulfur-containing compounds at pH8.0, but caused a increase at pH5.0. On the other hand, it facilitated the generation of several nitrogen-containing volatiles such as pyrazine, methylpyrazine, ethylpyrazine, 2,6-dimethylpyrazine and other alkyl pyrazines which are known to elicit roasty and nutty flavor notes at pH8.0. A plausible explanation for this phenomenon is that ammonia can be released from urea upon heating and the formed ammonia competes with hydrogen sulfide to react with Maillard reaction precursors to produce nitrogen-containing compounds such as alkylpyrazines.
YU Jing , YU Liang-min , RUAN Xiu , LI Xia
2011, 28(8).
Abstract:N,N’-di-allyl-dithiodipropionamide(ALPD)has been synthesized with allylamine and dithiodipropionmethyl by amidation , and its structure has been confirmed by IR spectroscopy and 1HNMR. Considering molar ratio of the reactants, amount of the catalyst, dropping time of dithiodipropionmethyl and reaction time impact on the yield of ALPD; researching the antibacterial effects of ALPD. The optimum reaction conditions are n(allylamine): n(dithiodipropionmethyl)=3:1, the amount of catalyst triethylamin is 2.5mL, dropping time of dithiodipropionmethyl is 2.5h, reaction time is 48h, yield is 88.4%. The MICs of ALPD are 0.1250g/L, 0.0625 g/L with Staphylococcus aureus, Escherichia coli. The ALPD can be introduced into the macromolecular by polymerization.
2011, 28(8).
Abstract:The star-shape anionic/non-ionic polyurethane-acrylate (SPUA) was prepared via “arm-first” technique, the effects of the content of non-ionic extender (PEG 600) on the properties of emulsion and film after UV curing were researched, and the structure of SPUA was confirmed by FT-IR. Results show that: The content of PEG 600 change obviously particle size distribution, surface tension and rheology behavior of emulsion. Micro-phase separation of SPUA is not obvious, and compatibility between soft segment and hard segment is good. With increasing content of PEG 600, ultimate strength, solvent-resistance of film after UV curing, glass transition temperature(Tg) of soft segment raise, which elongation at break, tensile-recovery ratio, water-resistance, thermal stability of film after UV curing decline.
ZHANG Meng-meng , XIE Li-ping , ZHOU Peng , LI Rui-hai
2011, 28(8).
Abstract:The synthesis of tributyl citrate catalyzed by cation exchange resin modified by SnCl4 was investigated.As shown in the results of Fourier transform infrared spectrum and X-Ray fluorescence spectrum, the skeleton structure has not changed and loading factor of Sn4+ is 13.47% after modified by SnCl4. The optimization of reaction parameters was performed ,showing that maximum yield of tributyl citrate of 97.3% could be obtained under the conditions that temperature was 155 ℃,duration was 6 h,molar ratio of n-butanol to citric acid was 4.1:1 and catalyst amounts was 4.5%(based on the total mass of reactants).The catalyst could be reused 8 times without any disposal and the yield still reached 96%.
2011, 28(8).
Abstract:A silicon-halogen synergistic flame retardant plasticizer benzyl trichloroethyl silicate was synthesized by using silicon tetrachloride, benzyl alcohol and ethylene oxide as raw materials. The effect of reaction time, temperature and amount ratio of substance on product yield was discussed.The optimal conditions for preparation r were selected as follows: n(silicon tetrachloride):n(benzyl alcohol) was 1: 1; n(silicon tetrachloride):n(ethylene oxide) was 1: 3.2; reaction time was 2h at 30℃ and the percentage of product yield could reach 98%. The molecular structures of benzyl trichloroethyl silicate and its related performance measurement were determined by means of FTIR,1H NMR and LOI technique.
2011, 28(8).
Abstract:A new linear-chain polyether-aminosiloxane (LPEAS) was synthesized by the reaction of epoxy polyether terminated polydimethylsiloxane with N, N-dimethyl-propanediamine. The Chemical structure of LPEAS was characterized by IR and 1H-NMR.Then the particle sizes, particle sizes distribution were investigated by transmission electron microscope (TEM) and other instruments. The effects of its viscosity, amino value and the amount of the emulsion on the performance of treatment of cotton fabrics were also studied. The results showed that average particle size of LPEAS emulsion was only 27nm, cotton fabric featured hydrophilicity improved, the bending rigidity of fabric decreased, and the whiteness of the fabrics remained the same,when the viscosity of LPEAS was 0.950 Pa•s, amino value was 0.3 mmo1/g ,the amount of the emulsion was 10kg/t,and curing at 100℃for 5min following 160℃for 30 seconds.
2011, 28(8).
Abstract:The solvent-free cationic silicone modified polyurethane /polyacrylate composite emulsion(PAU) were prepared by isophorone diisocyanate(IPDI),polytetrahydrofuran glycol(PTMG1000), N-methyldiethanolamine(MDEA), trimethylolpropane(TMP) and othermaterials, with silane coupling agent (KH550) . The chemical structure of PAU and properties of emulsions were characterized by FT - IR , TG, XRD, TEM and so. The results showed that : when n (-NCO): n (- OH) = 1.07, m (St): m (BA) = 1:2, MDEA content was 5.50%, TMP content was 0.55%, KH550 content was 0.69%, it synthesizes polyurethane with the expected structure, and the addition of silicone enhanced flexibility of the membrane.
WANG Ai-qin , ZHAI Nai-hua , Wang Wen-bo , Zheng Yi-an
2011, 28(8).
Abstract:A fast swelling superabsorbent composite was prepared in the 10t reactor by aqueous free-radical polymerization using acrylic acid (AA) as the monomer, attapulgite (APT) as the inorganic nano-scale composite, potassium persulfate (KPS)/ascorbic acid as the initiator and N,N'-methylene-bis-acrylamide (MBA) as the crosslinking agent. The results indicate that the optimum reaction conditions were as follows: AA concentration of 42% (w/w), initiate temperature of 50oC, foaming agent content of 0.2% (w/w) and MBA content of 0.1% (w/w), which the absorption rate is 43s in distilled water and the absorption ratio is 16 g/g under 2 KPa in physiological saline. By using the heat originated from the acid and alkali neutral reaction and the polymerization reaction, the active ingredient of the superabsorbent was enhanced from 42% (w/w) to 52% (w/w). Compared with traditional technology, this technology can reduce the vapor consumption and save energy about 1,640,000 kJ/ acrylic acid/ton.
2011, 28(8).
Abstract:Polyurethane-acrylate hybrid emulsions (PUAs) were prepared by in situ emulsion polymerization method with toluene diisocyanate (TDI-80), polyether binary alcohol (N210), dimethylol propionic acid (DMPA) as the main raw materials, castor oil (C. O.) and aliphatic epoxy resin (RE) as crosslinking agents. Polyacrylate (PA) emulsions were prepared by emulsifier-free polymerization, following to afford the PU/PA blend emulsions by mechanically mixing with polyurethane(PU). The effects of the dosage of C.O., RE on the properties of the hybrid emulsions and films, and sodium 1-allyloxy-2- hydroxypropyl sulfonate (COPS-1) on the properties of the blend emulsions and films were investigated. The results state that the PUAs and PU/PAs present excellent performances when the emulsions were prepared under the following conditions, that is, the percent of C.O. and RE to dried PU was 5.0% -7.0% and 2.0% -3 .0 % (wt%) respectively and the percent of COPS-1 to all monomers was 2.0%. The properties such as flexibility, the elongation at break and adhesion of PUA are superior to that of PU/PA, except the hardness and the cost of PUA is lower and higher respectively. Infrared spectroscopy showed that almost all -NH- of PUA and PU/PA were formed to hydrogen bonds. From TEM, the core-shell particle of PUA could be obtained with lower size. From AFM scanning, the existence of micro phase separation between hard segment and soft segment of PUA was observed.
2011, 28(8).
Abstract:The hydroxyl phosphate as a functional monomer was synthesized by GMA and phosphoric acid at a low temperature, followed copolymerization with acrylic monomers to prepare a styrene-acrylic emulsion. The modified styrene-acrylic emulsion were characterized by IR、SEM, Tafel and particle size analysis and the performance of its film was tested . The results showed, the waterborne anti-corrosion emulsion reaction system was stabile and the particle diameter of emulsion is about 100nm having relatively narrow distribution. When the dosage of hydroxyl phosphate was 4%,the coating was prepared by the emulsion with the best corrosion resistance and overall performance, without flash-rust resistant appearance. The corrosion current of the paint film was 1.376×10-8A, which is better than the commericial waterborne anti-corrosion coating film on the anti-corrosion properties.
ZHANG Tian-yong , HE Meng , LI Bin , WANG Xiao , DU Jing , DUAN Yong-jie , YIN Guan
2011, 28(8).
Abstract:Method of liquid sulfonation in o-dichlorobenzene as a solvent was used in place of solid baking sulfonation. Sodium 1-amino-4-naphthalene sulfonate was prepared through ammonium salifying by 1-naphthylamine and sulfuric acid, transposition sulfonation and salifying(Na2CO3) in the presence of Tween 60 as a surfactant and o-dichlorobenzene. Effects of the solvents, the sulfonation reaction time, surfactants, recycle times of mother liquor were investigated. The optimum conditions were found as follows: 1-naphthylamine 35.8g, 80% sulfuric acid 33.6g, o-dichlorobenzene 150mL, Tween 60 1.5g, sulfonation time 6h, yield of sodium 1-amino-4-naphthalene sulfonate 90.6%.
HU Yu-feng , LÜ Chun-xu , LUO Jun
2011, 28(8).
Abstract:Abstract: An efficient method for the synthesis of p-nitrofluorobenzene using highly effective anhydrous tetrabutylammonium fluoride (TBAFanh.) via the fluorodenitration processes is reported. TBAFanh. and p-dinitrobenzene were simply stirred together in an anhydrous solution of THF at room-temperature lead to yields of p-nitrofluorobenzene can reach more than 98%. The nucleophilic fluorinating method has the advantages of surprisingly mild reaction conditions, high yields, easy work-up and little side reaction.