• Volume 32,Issue 12,2015 Table of Contents
    Select All
    Display Type: |
    • >Functional materials
    • Efficient Dispersion of Single-walled Carbon Nanotubes by Block Copolymer F127

      2015, 32(12).

      Abstract (1003) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The single-walled carbon nanotubes (SWNTs) were oxidized by sulfuric acid and nitric acid to prepare carboxylated single-walled carbon nanotubes(SWNTs-COOH), and then dispersed with a amphiphilic Pluronic F127((PEO)99(PPO)65(PEO)99) triblock copolymer under the condition of magnetic stirring,shock and ultrasound to prepare the suspension of SWNTs-COOH/F127.The dispersion and stability were carried by static observation.The characterization of structure of modified SWNTs was carried out by laser particle size analyzer,scanning electron microscope,transmission electron microscopy,fourier-transform infrared spectra,UV–vis spectroscopy and Raman spectroscopy.The dispersion of SWNTs、F127 modified SWNTs、carboxylated SWNTs、carboxylated SWNTs modified by F127 was compared and the experimental results showed that after mixed acid treatment,the single-walled carbon nanotube have modified with carboxyl groups successfully.Compared with the pristine SWNTs,the dispersion and stability in water of modified SWNTs have greatly improved.The SWNTs-COOH/F127 suspension has no deposition after centrifugation for 30min with 4000r/min and can stand at room temperature for more than 30 days without flocculation.The aqueous SWNTs-COOH/F127 of high dispersibility was attempt to construct a rapid detection system.

    • Synthesis, Characterization and Performances of UV-curable Polysiloxane-modified Polyether Polyurethane Acrylate Prepolymer

      2015, 32(12).

      Abstract (604) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:An UV-curable polysiloxane-modified polyether polyurethane acrylate prepolymer (Si5E5PUA) was synthesized with polysiloxane (Q4-3667), polypropylene glycol (PPG-2000), isophorone diisocyanate (IPDI), diethanolamine and hydroxy ethyl acrylate (HEA) as raw materials. The structure of Si5E5PUA was characterized by Fourier infrared spectrometer (FT-IR), nuclear magnetic resonance (1H NMR and 29Si NMR) and gel permeation chromatograph (GPC). The viscosity, photopolymerization behavior and volume shrinkage in polymerization processes of Si5E5PUA systems with different monomers and glass transition temperatures of cured films were investigated. The results showed that the Si5E5PUA exhibited good compatibility with acrylate monomers. The systems of Si5E5PUA with different monomers had excellent photopolymerization efficiency and final double bond conversion was over 90%. The increase of functionality of the monomers could enhance the glass transition temperatures of cured films. The volume shrinkage of Si5E5PUA systems ranged from 3.3% to 5.6%.

    • >Perfumes and essences
    • Analysis on 3-acetyl-N-butyl-2-methyl-5-(1?,2?,3?,4?-tetrahydroxy-butyl) Pyrrol by Gas Chromatography-Mass Spectrometry

      2015, 32(12).

      Abstract (699) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:3-acetyl-N-butyl-2-methyl-5-(1,2,3,4-tetrahydroxy-butyl) Pyrrol was synthesized by cyclization reaction and alkylation reaction, then its structure was confirmed by 1HNMR, 13CNMR, IR and HRMS spectra. The thermo-gravimetric was studied by themogravimetry-derivative themogravimetry-differential scanning calorimetry (TG-DTG-DSC). Its pyrolysis behavior was investigated by pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) at 300, 600, 900 ℃ and the application of the target compound in cigarette flavoring was studied. The results indicated that the initial pyrolysis temperature of the target compound was 137.6℃, and the secondary pyrolysis temperature was 224.9℃. The thermal mass loss of the target compound reached about 65% at 900 ℃. 58 pyrolysis products were detected,including the flavorous substances such as 2,3-dimethyl-1H-pyrrole, 1-(1-methyl-1H-pyrrol-3-yl)-ethanone and 3-acetyl-2,4-dimethylpyrrole, and the amount of total products increased with the increase of temperature. The target compound could improve and increase aroma quality, and with the concentration of 0.003%, it showed the most appropriate flavoring effect. Possible pyrolysis mechanism of 3-acetyl-N-butyl-2-methyl-5-(1,2,3,4-tetrahydroxy-butyl) Pyrrol was preliminarily discussed, which would provide a reference for the study of its conversion behavior in cigarette combustion process.

    • >Functional materials
    • Synthesis of Multi-benzene Dendritic Molecule and Fluorescence Effect Research it to Fluorophores

      2015, 32(12).

      Abstract (728) HTML (0) PDF 0.00 Byte (1) Comment (0) Favorites

      Abstract:Pyromellit-tetra-diethanol amine (PTDA) was synthesized with pyromellitic dianhydride (PMDA) and diethanol amine (DEA) as raw materials. Multi-benzene dendritic Molecul(PTDA-3,5-DAC)was prepared PTDA using 3,5-dihydroxybenzoic acid(3,5-DAC) modifying PTDA. Its structure was identified PTDA means of FTIR and NMR. In the energy transfer systems of PTDA-3,5-DAC and fluorophores (Eosin B, Rhodamine B, Titan yellow and Methylene blue), the changes of fluorescence intensity were studied. The results showed that the optimum conditions were determined as following: reaction temperature was 160 ℃, reaction time was 4 h, catalyst dosage was 2.0 %, catalyzer was toluene sulfonic acid. The extent of reaction is 75.67 %. The fluorescence of fluorophores decreased when PTDA-3,5-DAC was added into Eosin B' and Methylene blue' DMF solutions. The fluorescence of fluorophore increased then decreased when PTDA-3,5-DAC was added into Rhodamine B' DMF solution. The fluorescence of fluorophore lesser increased when PTDA-3,5-DAC was added into Titan yellow' DMF solution.

    • >Catalysis,separation and purification technology
    • The Preparation of Ru/C Catalysts and Catalytic Quinoline Hydrogenation Performance Research

      2015, 32(12).

      Abstract (1051) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Use first dipping adsorption with KBH4 reduction method of the preparation of 5%Ru/C catalysts which have been characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and high resolution transmission electron microscopy (TEM). Results show that dispersion degree of 5%Ru/C catalyst is high, the average grain size of metal ruthenium 2 ~ 3 nm. In quinoline hydrogenation reaction, the catalyst showed high catalytic activity. With water as solvent,, at 100 ℃, reaction 1 h ,2 MPa hydrogen pressure, the conversion of quinoline was 100% and the selectivity of 1, 2, 3, 4 -tetraquinoline was up to 100%,TOF for 338h-1 .

    • >Fine chemical intermediates
    • Novel Synthesis of 2,6-dihydroxy-3,5-dinitrotoluene

      2015, 32(12).

      Abstract (781) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:2,6-dihydroxy-3,5-dinitrotoluene (MDNR) is one of key intermediate for poly(p-phenylene methyl benzobisoxazole) (MPBO) . In this paper, 2,6-dichloro-3,5-dinitrotoluene (DCDNT) was first prepared through the nitration of 2,6-dichlorotoluene with a purity of 99.79% and yield of 98.40%, then methoxylated with CH3O- to obtain 2,6-dimethoxy-3,5-dinitrotoluene (DMDNT) with a purity of 96.90%,and a yield of 88.36%; Finally, MDNR was successfully synthesized by the acid demethylation of DMDNT, and its purity was 99.40%,the yield was 93.15%. MDNR was identified by FT-IR, MS and 1H-NMR. This process has advantages of cheap raw materials, convenient operation, excellent product quality, the total yield of more than 80%, easy to industrialization,etc. which provides the source of key intermediate for further development of methyl modified PBO fiber.

    • >Functional materials
    • Acid stimuli-responsive silica nano-container and release in vitro

      2015, 32(12).

      Abstract (854) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In order to study the effect of intelligent nano-container’s release function in imitation of the condition of Lysosome and Endosome, an acid stimuli-responsive intelligent nano-container using the ketal chain as a stimuli-responsive unit was prepared using Mesoporous Silica Nanoparticles (MSNs) as a carrier, adsorbing fluorescent macromolecular Rhodamine B and encapsulated at the place of MSNs’s mesoporous by β-cyclodextrin with 2-(2-bromo-ethoxy)-2-(2-azido-ethoxy) propane. The functionalized surface of MSNs was demonstrated by Nuclear Magnetic Resonance (NMR), Fourier Transform Infrared Spectrometer (FTIR) and Thermo Gravimetric Analysis (TGA). The releasing performances of Rhodamine B at different pH values were monitored by RF-5201 spectrophotometer and the drug loaded in the intelligent nano-container is 15.23 mg/g which was measured by Ultraviolet-Visible Spectrophotometer (UV-Vis). The intelligent nano-containers constructed by assembly-technology realized “zero release” under neutral condition and remarkable release under acidic condition—suitable release in imitation of the condition of Lysosome and Endosome and this research has extensive application prospects in terms of targeting tumor cells.

    • >Catalysis,separation and purification technology
    • Ir-N@C Catalyzed N-alkylation of Amines with Primary Alcohols in Water

      2015, 32(12).

      Abstract (907) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The stable, easy recoverable heterogeneous catalyst Ir-N@C ( 5 wt % Ir content) is obtained by impregnation with commercial carbon powder. The factors for the N-alkylation reaction including different iridium catalysts, reaction temperature, reaction time, bases are investigated. Experiment results suggested that the N-alkylation of amines with primary alcohols could be efficiently catalyzed in water using iridium catalyst with n (Ir) : n (1,10-Phenanthroline) = 1 : 2. In recycling experiment, the catalyst shows good stability and the catalytic activity is not obviously decreased. The catalyst is characterized by XRD, TEM, XPS, BET.

    • >Surfactants
    • Preparation and Surface Activity of Fluorosilicon Surfactant

      2015, 32(12).

      Abstract (946) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: Preparation and surface activity of 2-methyl-2-[perfluoro-2-methyl-3-oxocaproyloxyl] ethoxycarbonyl ethylmethyldipolyethoxylsilicane (V) were investigated. 2-methyl-2-[perfluoro-2- methyl-3-oxocaproyloxyl] ethoxycarbonyl ethylmethyldichlorosilicane (III) was synthesized from 2-[perfluoro-2-methyl-3-oxocaproyloxyl] ethyl methacrylate (I)and methyldichlorosilicane (II) by hydrosilication in the presence of Karstedt catalyst. III reacted with polyglycol (IV)to give non-surfactant V which was characterized by FTIR and MS and its surface activities were investigated. The reaction conditions of hydrosilication were optimized. n (I ): n (II) = 1.2∶1, I and II reacted in THF at 50℃ in the presence of 0.5% Karstedt catalyst( calculated by quality of I ) for 28h to give III at conversatin 68.2 %. The critical micelle concentration (CMC) of aqueous solution of V was 0.52 g/L, surface tension of which at CMC (γcmc) was 22.8 mN/m. Glass surface treated by THF solution of V shows excellent hydrophobic and good oilphobic performances.

    • >Oil field chemicals and petroleum additives
    • Synthesis of Graft Copolymer of betain onto Hydroxypropyl Guar Gum

      2015, 32(12).

      Abstract (667) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A graft copolymer of betain onto hydroxypropyl guar gum was prepared by using ceric nitrate as initiator. The product structure was characterized though IR. The effects of graft reaction temperature.,graft reaction time, initiator concentration, m(betain): m(HPG) on thickening properties of product was investigated. It was indicated that monomer transfer rate was 36.5% and the product molecular could be 1.28?06. The product of 0.5% concentration in aqueous solution could be dissolved completely within 20 minutes and viscosity was 75mPas. The solution viscosity kept increasing with the increasing of salt concentration if salinity was less than 10%. No precipitate appeared during the process.

    • >Drug and cosmetic materials
    • Synthesis of (R)-4-benzyl-2-((R)-1-(3,5-bis(trifluoromethyl)phenyl)ethoxy)morpholin-3-one and Dynamic Kinetic Resolution of its Asymmetric Transformation

      2015, 32(12).

      Abstract (836) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Using 4-benzyl-2-hydroxy-3-one as a starting material, a diastereoisomers of 4-b-enzyl-2-((R)-1-(3,5-bis(trifluoromethyl)phenyl)ethoxy)morpholin-3-one was prepared by two-st-ep reaction. Then the dynamic kinetic resolution of its asymmetric transformation was use-d to convert it into chiral pure (R)-4-benzyl-2-((R)-1-(3,5-bis(trifluoromethyl)phenyl)ethoxy)morpholin-3-one under potassium t-butoxide as the alkaline conditions. The ratio of the co-nverted chiral product and diastereomer is 96:4, which has greatly utility value in the pro-cess of the industrial preparation of neural excitation peptide 1 (NK-1) receptor blockers(Aprepitant).

    • >Oil field chemicals and petroleum additives
    • Synthesis and Evaluation of a copolymer with modified β-cyclodextrin used in acid fracturing

      2015, 32(12).

      Abstract (983) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: Maleic anhydride(MAH) and β-cyclodextrin(β-CD) were chosen to synthetize vinyl β-cyclodextriny monomer(MAH-β-CD) through alcoholysis reaction, and the quaternary Copolymer was synthesized by the free radical polymerization in aqueous solution, using MAH-β-CD, acrylamide(AM), 2-methyl-2-Acrylic amide propyl sulfonic acid(AMPS) and dimethyl-diallyl-ammonium chloride(DMDAAC) as monomers. The optimum conditions achieved by orthogonal experiment and single factor experiments were that the m(MAH-β-CD):m(AM):m(AMPS): m(DMDAA) was 1:69:20:10, the reaction temperature was 45℃, the monomer concentration was 20%, the polymerization reaction continues 6 h, pH value was 7, and the dosage of initiator was 0.4%(the total mass of monomer).The structures of copolymer were characterized by IR and UV-Vis absorption spectra, indicating that the synthetic product was the target product. The evaluating results showed that the acid dissolving time of 0.8% PAADM is 100 min; Comparison PAADM and PDMC showed that the thermal stability and the slow rate of PAADM were good, and the consistency of the consistency was good.

    • >Leather chemicals
    • Preparation of Modified Hyperbranched Polyglycerols and Its Application in Fatliquoring

      2015, 32(12).

      Abstract (825) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Hyperbranched polyglycerol (HBPG) of generation three was synthesized by ring-opening multibranching polymerization method using glycerol and glycidol as materials and sodium methoxide as catalyst. Oleic acid was then used to modify HBPG with different content to obtain a series of products named HBPG-X. FT-IR and 1H NMR were employed to characterize structures of HBPG and HBPG-X. Then HBPG-X and commercially available fatliquoring agent SK-70 were used in fatliquoring process of sheep skin garment leather. The results showed that the softness and mechanical properties of all treated leather were increased compared with original leather. HBPG-1 showed best effect on softness of the fatliquored leather which was similar with SK-70.

    • >Water treatment technology and environmental protection
    • Preparation and performance test of hydrophobically associating cationic starch-nano SiO2 flocculant CSSADD

      2015, 32(12).

      Abstract (916) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Taking soluble starch as the base material, the research introducing AM, the functional cationic monomer DMDAAC, hydrophobic monomer C16DMN+ and nano-SiO2 to synthesize a hydrophobically associating cationic starch-nano SiO2 composite polymer flocculant, and then the chemical structure of CSSADD was demonstrated by IR, XRD, TG and SEM. The reaction conditions were optimized by the method of single factor variable, and the study showed that the graft monomers molar ratio was AM:DMDAAC:C16DMN+=84.5:15:0.5, acidity control in PH value was 5~6, when nano-SiO2 and starch quality ratio scale was 1:3, starch andmonomers quality ratio scale was 1:3, the mass of initiator was 0.5% of total monomers, the reaction temperature was 45℃, and the reacting time was 3 hours, the CSSADD’s performance was best. The performance test indicated that when the PH value of kaolin suspension was 6 and the mass of CSSADD was 3mg/L, the upper transmittance approached 98.3%.

    • >Functional materials
    • Preparation and antibacterial ability of n-HA/PVA/CS porous composite hydrogel

      2015, 32(12).

      Abstract (912) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:[Objective] This paper studied the preparation, properties and specially antibacterial ability of n-HA/PVA/CS composite hydrogel which aims to provide theory evidence to support its further uses in artificial cornea scaffold materials. [Methods] Physical cross-linking was adopted to prepare composite hydrogel. Then composite hydrogel was studied by testing its moisture content, mechanical properties and micro structure. Turbidimetric and plate counting method were adopted to do researches about the minimum inhibitory concentration and the inhibitory rate of n-HA/PVA/CS after early exploration. At the same time, the different inhibitory rate between Gram-positive bacteria S.aureus and Gram-negative bacteria E.coli were be analyzed. [Results] n-HA/PVA/CS composite hydrogel was evenly spread three-dimensional porous structure, moisture content was 75%, the tensile strength was 0.26 MPa. n-HA/PVA/CS composite hydrogel had strong antibacterial ability after disposed by 2% acetic acid.The MIC of n-HA/PVA/CS on S.aureus cells and E.coli cells both were 0.5g/L. When the concentration of n-HA/PVA/CS was 2.0g/L, the inhibitory rate of S.aureus and E.coli reached 84% and 99%, respectively. When the concentration of n-HA/PVA/CS was 2.5g/L, the inhibitory rate reached 100%.Therefore, n - HA/PVA/CS composite hydrogel was expected to become the artificial cornea scaffold material with excellent performance.

    • Synthesis of Raspberry-like Composite Microsphere of Ag/Polystyrene- Acrylonitrile and its Catalytic Performance

      2015, 32(12).

      Abstract (1065) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Monodisperse polymer microspheres P(St-AN) were prepared through two-steps polymerization stabilized with polymerizable anion-charged monomer Sodium Styrene Sulfonate (NaSS). The influence of acrylonitrile dropping time on particle size and dispersity were discussed. Using the P(St-AN) particles as template, raspberry-like Ag/P(St-AN) composites were obtained by chemical deposition. Composition, structure, morphology and catalytic performance of the composite particles were characterized by fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, and UV-visible spectroscopic techniques. The results revealed that the P(St-AN) template particles were uniform spherical particles when the acrylonitrile were dropped 1~3 h after the reaction beginning. The particle size was between 600 nm and 800 nm. The obtained Ag/P(St-AN) were of uniform structure and Ag nanoparticles of face centered cubic crystal structure were well coated on the surface of the particles with good dispersity and stability. The Ag/P(St-AN) composite particles were used as the catalyst in 4-nitrophenol reduction to 4-aminophenol with NaBH4 as the reducer, and the reduction was significantly enhanced.

    • >Fine chemical intermediates
    • Synthesis of Chiral 2,2'-Bis(diphenylphosphino)-1,1'-binaphthalene

      2015, 32(12).

      Abstract (852) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:(S)-(-)-2,2'-bis(diphenylphosphino)-1,1'-binaphthalene was prepared in three steps. (S)-(-)-1,1'-binaphthyl-2,2'-diol was firstly protected by trifluoromethanesulfonic anhydride, then after cross coupling with diphenylphosphine oxide, the title compound was synthesized by reduced with trichlorosilane. Structure characterization of the intermediates was conducted by methods of 31PNMR、1HNMR and HRMS. The optimum reaction conditions were determined as follows: n (Ⅱ) : n (Ph2PH=O) : n (DABCO) : n (Ni(dppe)Cl2) : n (HSiCl3) = 1 : 2.1 : 2.5 : 0.1 : 3. In the coupling step, the reaction temperature and time was 100 ℃ and 48 h, respectively. After reduced by trichlorosilane under reflux condition for 5 h, (S)-BINAP was got with the yield of 82.3% and 99.3% e.e..

    • >Functional materials
    • Structure control and property of solvent-free reactive layer for coated urea

      2015, 32(12).

      Abstract (639) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Triethanolamine (TEA) was used to modify solvent-free reactive layer of polyaryl polymethylene isocyanate (PAPI) and polyester polyol system for obtaining coated urea. The crosslink density, crystallization morphology, thermal stability and molecular structure of the films were characterized by the swelling method, differential scanning calorimetry (DSC), thermal gravimetric analysis (TG/DTG) and attenuated total reflection-fourier transform infrared spectroscopy (ATR-FTIR), respectively. And the effect of the mass fraction of TEA on controlled-release property of coated urea was investigated. The results showed that the crosslink density and glass transition temperature of the film increased with the increase in mass fraction of TEA. The degree of hydrogen bonding of carbonyl groups in the film was reduced after TEA was added, but the CH2 bending vibration absorption was enhanced. When the mass fraction of TEA was 2.6%,the control release duration of coated urea was extended by at least 25 d, compared with coated urea without modification treatment.

    • >Surfactants
    • Synthesis and Properties of 1-(threetrimethylsilylmethyl)-3-decyl imidazolium Chloride

      2015, 32(12):0-0.

      Abstract (1105) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A kind of ionic liquid surfactant 1-(threetrimethylsilylmethyl)-3-decyl imidazolium chloride was prepared in an unmodified microwave oven by quaternary ammonium reaction of chloromethyltrimethylsilane with N-decyl imidazole, which was synthesized using imidazole, sodium hydroxide and bromodecane as materials through alkylation reaction. The structure of the intermediate and the target product were characterized by IR、1HNMR and 13CNMR. At the same time, the thermal stability, foaming properties and surface activities of the target product were measured. The results show that complete decomposition temperature of 1-(threetrimethylsilylmethyl)-3-decyl imidazolium chloride was 297℃. The foaming power increased with increasing concentration of the surfactant, but the foam stability at different concentration was low. Moreover, the critical micelle concentration (cmc) of the ionic liquid surfactant was 4.12mmol/L and the surface tension at cmc was 25.13mN/m at 25 ℃.

    • >Catalysis,separation and purification technology
    • Ag doped V2O5/TiO2 catalyst for oxidative dealkylation of 3-picoline

      2015, 32(12):0-0.

      Abstract (1154) HTML (0) PDF 0.00 Byte (87) Comment (0) Favorites

      Abstract:The effect of silver (Ag) loading on titanium-supported vanadium (Ag-V/TiO2) catalysts, prepared by impregnation method, on the oxitative dealkylation behavior of 3-picoline has been investigated. At optimum loading of 2mol % Ag was found to enhance the catalytic performance in terms of yield (80.1%) and selectivity (84.7%). As evidenced by X-ray photoelectron spectroscopy (XPS) and H2 temperature-programmed reduction (H2-TPR), Ag is attributed to promotion of the formation of surfance oxygen species and change of the valence of vanadium species (V4 /V5 ) through interaction of V and Ag, shortened the time of reduction process, increased the oxidative activity. Additionally, Ag highly dispersed on the catalysts as atom, which could formed silver oxide (Agp O oxygen species: O-, O2- and O2-) by adosorbed the O2. Thus, the selective oxidation of methylarene were modified over the Ag-V/TiO2 catalysts, which pyridine as the main product was found with few nicotinic acid.An oxidative machnism was conjectured: C-H bond was activited by V4 /V5 (oxygen species: O2-) and Agp O absorbed on the C-C bond because of the O- and O2- were strong electrophilic reactants, which attacted the site of high charge density of reacted molecule, causing the C-C bond to decompose, -CH3 was oxidatived to form COx.

    • >Building chemicals
    • Synthesis and Properties of Fluorescence Waterborne Polyurethane

      2015, 32(12):0-0.

      Abstract (965) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A novel AFC-based cationic waterborne polyurethane, very stable for long-term storage, was synthesized by importing the fluorescent agent 7-amino-4-(trifluoromethyl)coumarin (AFC) into the polyurethane chains. Structure of the WPU-AFC was confirmed by Fourier transform infrared spectroscopy (FTIR) and UV-visible absorption spectroscopy. The fluorescence intensity and average emulsion particle size for WPU-AFC were also determined. It was found that the fluorescence intensity of WPU-AFC decreased with the increasing temperature and was enhanced compared with that of AFC. The thermal stability of WPU-AFC improved compared with the WPU without AFC group.

    • >Fine chemical intermediates
    • Palladium-catalyzed Synthesis of Phenylboronate

      2015, 32(12):0-0.

      Abstract (1265) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In the preparation of pinacol(4-tert-butylbenzene)boronate by Pd-catalyzed borylation of 4-tert-buty-1-chlorobenzene,Pd2dba3 was used as catalyst,Xphos as ligand and B2(pin)2 as boron source.The effects of the quantity of boron source,different kinds of bases, ratio of the catalyst to the ligand, solvents and temperatures on the yield of the product were studied. The optimum conditions were determined as follows: n(4-tert-butyl-1-chlorobenzene) : n(Pd2dba3) : n(Xphos) : n[B2(pin)2] : n(KOAc) = 1 : 0.01 : 0.04 : 2 : 3 in EtOH at 60℃ for 1 h.The yield can reach 98%.

    • Synthesis and Antifungal Activity of Camphoric Acid-Based Diacylhydrazine Compounds

      2015, 32(12):0-0.

      Abstract (733) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Camphoric anhydride was prepared by using camphoric acid as starting material and acetic anhydride as dehydrating agent. Then, ten novel camphoric acid-based diacylhydrazine compounds 3a~3j were synthesized by the N-acylation reaction of camphoric anhydride with aromatic acylhydrazines. The synthetic conditions were investigated preliminarily. The target compounds were characterized by means of FT-IR, 1H NMR, 13C NMR and ESI-MS techniques. The preliminary bioassay showed that, at the concentration of 50 mg/L, part of the title compounds exhibited good fungicidal activity, in which compound camphoric acid-based nicotinoyl hydrazine 3h had inhibition ratio of 96.3% against Physalospora piricola (better than that of the positive control azoxystrobin).