• Volume 31,Issue 3,2014 Table of Contents
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    • >Review and monographs
    • Progress in the Synthetic Process of Losartan

      2014, 31(3).

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      Abstract:Losartan was the oral non-peptide angiotensin Ⅱ receptor antagonist which was first approved by Sweden in 1994, and then approved by American Food and Drug Administration (FDA) in 2004. In recent years, Losartan has been the first-line antihypertensive drug. Structurally, Losartan was constituted by linking four structural fragment: imidazole ring (A), phenyl ring (B) and (C) as well as tetrazole ring (D). Based on the different linkage order of four ring fragment, the synthetic strategies of Losartan have been divided into five such as (B C) D A, (B C) A D, (C D) B A, (C D) (A B) and (A B) C D. In this paper, the progress in the synthetic process of Losartan has been reviewed from the perspective of five different synthetic strategies since its first discovery.

    • >Functional materials
    • Study on colloidal properties of the attapulgite soaked with natural brackish water

      2014, 31(3).

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      Abstract:Attapulgite clay was soaked with natural brackish water, and the effects of soaking time on the viscosity, rheological and suspension stability of attapulgite were intensively investigated. The results indicate that the metal ions in the brackish water were exchanged with the surface ions of attapulgite, which altered the surface charges of attapulgite and thus improved its colloidal properties. After soaking for 90 d, attapulgite exhibits the best suspension stability. After soaking for 180d, the rotary viscosity of attapulgite was increased from 1188 mPa.s to 2444 mPa.s.

    • Effect of Ethanol on Preparation and Properties of Hydrophobic and Lipophilic Resin via HIPEs Method

      2014, 31(3).

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      Abstract:Using styrene, divinylbenzene as comonomers, ammonium persulfate as initiator, hexadecyltrimethylammonium bromide as emulsifier, porous polystyrene/ divinylbenzene (PSD) was synthesized by high internal phase emulsions (HIPEs) as template. The effects of ethanol volume fraction (relative to dispersed phase) on the emulsion stability and the properties of the PSD,such as density, absorption (release) effects of liquid, and swelling ratio, were investigated. It was more difficult to form a stable emulsion with the increase of alcohol content. In addition, the density, absorption of the liquid, swelling ratio of the PSD decreased, the release of toluene increased with the increasing of alcohol. It is worth mentioning that, after the PSDs were extracted by water-ethanol, the absorption rate of water decreased to 0.26 cm3/g, while the absorption rate of toluene was still 15.60~18.42 cm3/g. Thus, we would obtain a hydrophobic and lipophilic resin from this way.

    • The interactions and swelling properties of sodium alginate/feather keratin intelligent microspheres

      2014, 31(3).

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      Abstract:Sodium alginate/feather keratin(SA/FK) microspheres were prepared by extrusion dripping method. The interactions of SA and FK were charactered by FTIR and viscosimetry. The effects of preparation conditions(m(FK): m(SA), w(CaCl2), crosslinking time)and solution properties(pH, temperature, ionic strength,)on swelling ratio were also investigated. The result indicates that, electrostatic is the main interaction and hydrogen bond supplements it. Over time, swelling rate becomes slow, and it meets equilibrium swelling at last. SA/FK microspheres have compact network structures when m(FK): m(SA)=0.60, w(CaCl2)= 7% and crosslinking time is 60 min. The equilibrium swelling ratios are 0.6, 0.6, and 0.9. The equilibrium swelling ratio rises from 0.6 to 0.9 when temperature rises from 30℃ to 45℃. The equilibrium swelling ratio rises from 0.9 to 1.1 when pH froms 1 to 7. As pH=13, it rises to 3.8. The equilibrium swelling ratio rises from 1.1 to 13.8 when ionic strength increases from 0 to 0.6mol/L. SA/FK microspheres possess the ionic strength / temperature / pH sensitivity, and it is expected to achieve new intelligent slow-release microspheres.

    • Synthesis and Chelating Property with Iron(III) Ion of 3-hydroxy-4-pyridinone Derivative

      2014, 31(3).

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      Abstract:N,N'-bis-[4-(2-methyl-3-hydroxy-4-pyridinone)-phenyl]-malonamide was prepared by microwave- assisted synthesis with methyl maltol, p-phenylenediamine, malonyl dichloride as the main raw materials. The structure of the target product was characterized by means of IR, 1H NMR, UV-Vis and MS. And the chelating property with iron (III) ion has been measured by spectrophotometric determination. At pH = 7.40, the results show that the ligand coordination with Fe3+ is 1:1 under the Tris-water-ethanol buffer solution, the apparent stability constants of the complex is logK = 7.46, it was confirmed that the novel compound was potential chelating potency for iron (III) ion.

    • Synthesis of Schiff base zinc phthalocyanines and to study the properties

      2014, 31(3).

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      Abstract:2(3),9(10),16(17),23(24)-tri-(4-phenylimine phenoxy) phthalocyanine zinc(Ⅱ) (C84H52N12O4Zn)(APc) and 2(3)-(2-methyl-8-quinolinoxy)-9(10),16(17),23(24)-tetra- (4-phenylimine phenoxy phthalocyanine zinc(Ⅱ) (C81H50N12O4Zn) (BPc) were synthesized from 4-hydroxybenzaldehyde and characterized by UV-Vis, IR, 1H NMR spectra and elemental analysis. The aggregative behavior was studied in DMF by UV-Vis. The results show that BPc is not aggregative in DMF. However, APc is aggregative in DMF at the concentration of 1.499×10-5 mol/L~2.407×10-5 mol/L. The Q-band maximum absorption peaks of APc and BPc at 672nm and 676nm, compared with the unsubstituted zinc phthalocyanine(669nm) have red shift obviously. The electrochemical properties and energy band structure are studied by cyclic voltammetry. They have low LUMO (-5.411 eV,-5.384 eV) and a deep HOMO (-4.214 eV,-4.210 eV) energy level. It is indicated that APc and BPc matches with the energy level of the nanocrystalline of TiO2.

    • Synthesis of Ni-Cr-Co Nano-oxides as Anode Electrocatalysts for Methanol Oxidation

      2014, 31(3).

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      Abstract:NiCrCo nano oxides have been synthesized by thermal decomposition method and were used as the anode electrocatalysts for direct methanol fuel cell (DMFC). The catalysts were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the particle size of nano oxides was about 20-50 nm, and the material dispersed uniformly. The activity of catalysts with different metal molar ratios and calcination temperatures on the methanol oxidation reaction were investigated by cyclic voltammetry (CV). The optimal content of the Ni:Cr:Co ratio is found to be 1:1:1.5, which exhibits significantly high current density of methanol oxidation. And the onset potential ,current density and If/Ib for methanol oxidation was 0.38 V, 19.3 mA/cm2 and 1.72, respectively. Results show that the prepared NiCrCo nano oxides electrode presents high electrocatalytic activity for methanol oxidation.NiCrCo nano oxides have been synthesized by thermal decomposition method and were used as the anode electrocatalysts for direct methanol fuel cell (DMFC). The catalysts were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the particle size of nano oxides was about 20-50 nm, and the material dispersed uniformly. The activity of catalysts with different metal molar ratios and calcination temperatures on the methanol oxidation reaction were investigated by cyclic voltammetry (CV). The optimal content of the Ni:Cr:Co ratio is found to be 1:1:1.5, which exhibits significantly high current density of methanol oxidation. And the onset potential ,current density and If/Ib for methanol oxidation was 0.38 V, 19.3 mA/cm2 and 1.72, respectively. Results show that the prepared NiCrCo nano oxides electrode presents high electrocatalytic activity for methanol oxidation.

    • Studies on Synthesis and Self-assembly Behavior of pH and CO2-Responsive Block Copolymers

      2014, 31(3).

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      Abstract:Multi-responsive block copolymer poly(dimethylamino-2-ethyl methacrylate)-block-poly(lactide) (PDMAEMA-b-PLA) was synthesized by Ring-opening Polymerization (ROP) and Reversible Addition-Fragmentation Chain Transfer Polymerization (RAFT). Structures of the block copolymers were conformed by 1H-NMR and FTIR. The self-assembly of the block copolymers and their particle sizes and morphologies changed with CO2 and pH responses were investigated by ultraviolet spectrophotometer (UV-Vis), zeta potential and particle size analyzer and SEM. Results showed that the block copolymers have pH sensitivity and CO2 responsibility, and the responsibilities to environment can be recycled at least three times.

    • >Surfactants
    • Synthesis and Characterization of Methyl Diethanolamine Fatty Acid Di-ester

      2014, 31(3).

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      Abstract:The esterification reactions between the fatty acids with different alkyl chain length and the N-methyl diethanolamine were investigated. The reaction conditions were optimized by orthogonal experiments with lauric acid as materials. The effects of reaction temperature, catalyst dosage, molar ratio of raw materials and reflux temperature on the esterfication were examined, and the optimized reaction condition were determined as following: reaction temperature of 200 oC, catalyst dosage of 0.3%(mass ratio of catalyst/total raw materials), n(lauric acid) : n(N-methyl diethanolamine)=1.8:1, reflux temperature 70 oC. Under the optimized condition, the mass fraction of methyl diethanolamine lauric acid di-ester in the product was more than 98%. In addition, the conditions of esterification reactions between the fatty acids with different alkyl chain length and N-methyl diethanolamine were optimized. Under the optimized condition, the mass fraction of fatty acid diethanolamine di-ester in all of these products was greater than 98%. The products were characterized by IR and 1HNMR.

    • Microwave synthesis of a perfluoroalkyl-containing quaternary ammonium salt

      2014, 31(3).

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      Abstract:A novel perfluoroalkyl-containing quaternary ammonium salt was synthesized from N-methyl diethanolamine and perfluorinated hexyl ethyl iodide by microwave technique. The structure of the product was characterized by fourier transform infrared spectroscopy, mass spectrometry and nuclear magnetic resonance spectrum. The effect of solvent dosage, microwave power, reactant mole ratio and reaction time on reaction conversion rate were studied. The Central-Composite mathematical relational model between conversion rate of N-methyl diethanolamine and effect factors was established to optimize the synthesis technique of the product. The optimum synthesis conditions were as follow: perfluorinated hexyl ethyl iodide 0.015mol, N-methyl diethanolamine 0.01mol, solvent dosage 50wt%(10ml), microwave power 582.49 W, reaction time 2.5 h. Under the optimal condition, in a short reaction time, only 10.42% of the conventional heating time, the conversion rate of MDEA was 89.15%.

    • Preparation and Surface Activity of A Silicon Surfactant

      2014, 31(3).

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      Abstract:Preparation and surface activity of 2-methyl-2-perfluorononenyloxyethoxycarbonyl ethyl- methyldipolyethoxylsilicane (V) were investigated. 2-methyl-2-perfluorononenyloxyethoxycarbonyl ethyl methyldichlorosilicane (III) was synthesized from 2-perfluorononenyloxyethyl methacrylate (I)and methyldichlorosilicane (II) by hydrosilication in the presence of H2PtCl6. III reacted with polyglycol (IV)to give non-surfactant V which was characterized by FTIR and MS. its surface activities were investigated. The critical micelle concentration (CMC) of aqueous solution of V was 0.22 g/L, surface tension of which at CMC (γcmc) was 19.5 mN/m. The reaction conditions of hydrosilication were optimized. n (I ): n (II) = 1∶1.2, I and II reacted in THF at 50℃ in the presence of 20 ppm H2PtCl6 for 24h to give III at yield 68.0%. V is a fluorosilicon surfactant with high activity.

    • Synthesis and performances of a novel oil-based surfactant sodium dodecanoyl diphenyl sulfide sulfonate

      2014, 31(3):0-0.

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      Abstract:Oil-based surfactants have received widespread attention because of their lower cost and environmental friendly. A novel oil-based surfactant sodium dodecanoyl diphenyl sulfide sulfonate was synthesized from lauroyl chloride and diphenyl sulfide by F-C acylation reaction, followed by sulfonation and neutralization. Structures and contents of the intermediate and the final product were identified by means of FT-IR and 1H NMR and HPLC. Some performances of the surfactant, such as Krafft point (TK), surface tension (γ), critical micelle concentration (cmc), and electrolyte resistance were measured. TK of the surfactant is lower than 0 oC, and cmc and γcmc are respectively 4.38×10-4 mol/L and 37.63 mN/m at 25 oC. The LSDP of the surfactant is 26% (wt%), and it can soluble in aqueous solution of 9.7%(wt%) NaOH, 14.5%(wt%) CaCl2, 24.3%(wt%) NaCl and 30.9%(wt%) HCl, respectively. The experimental results showed that the surfactant has excellent water solubility at low temperature, good lime soap dispersing power and strong electrolyte resistance.

    • >Biological engineering
    • Study on Ion exchange coupling with Electrodialytical Desalination of 1, 3-Propanediol fermentation broth in Pilot-plant Level

      2014, 31(3).

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      Abstract:The desalination of fermented broth containing 1,3-propanediol by ion exchange coupling with electrodialysis was studied. Based on the laboratory-scale desalination experiment, the electrodialytical desalination, ion exchange resin, and the coupling process were also investigated. It is showed that the 1,3-PDO loss was 11.41% by electrodialysis. Among various cationic and anionic resins, LSI296 and LSI010 were used to pilot level by comparing pH, conductivity and exchange volume. The efficiency of desalination was improved to 96.2%, and the loss of 1,3-PDO was decreased to 5.88% by ion exchange coupling with electrodialysis.

    • >Catalysis,separation and purification technology
    • Synthesis of Novel Br鴑sted-Lewis Acidic Ionic Liquids and Used as Catalysts in Rosin Dimerization

      2014, 31(3).

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      Abstract:A Brønsted acidic ionic liquid mim•HCl was synthesized as an intermediate by protonating N-methyl imidazole with Brønsted acid donor hydrochloric acid. And a group of dual acidic ionic liquid 1-hydro-3-methylimidazole chloride chloroironinates (1-x)[mim•HCl]x[FeCl3] (where x is the mole fractions of the Lewis acid) was synthesized from the reaction of mim•HCl and a Lewis acid donor FeCl3. The acidities of the group were characterized and compared to each other by FT-IR in virtue of pyridine and acetonitrile molecular probe, respectively. The dual acidic ionic liquids were then employed to catalyze rosin dimerization. A dimeric rosin acid with a softening point of 102.4 oC was obtained using (1-x)[mim•HCl]x[FeCl3](x=0.64) as catalyst, which was 15 oC higher than that without using catalyst. The catalytic activity became weaker after the fifth use.

    • >Perfumes and essences
    • Rheological Experiment and Parameter Fitting of Rose Fragrance-Loaded Polybutylcyanoacrylate Nanocapsules

      2014, 31(3).

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      Abstract:The change of wall material content (0.4%、0.6%、0.8%), fragrance content (0.4%、0.6%、0.8%) and emulsifier content (2%、3%、4%) had respectively an influence on the rheology of rose fragrance-loaded polybutylcyanoacrylate (PBCA) nanocapsules via emulsion polymerization. Steady state test showed that apparent viscosity decreased to 0.006 Pa.s with the increase of shear rate from 0.001 s-1 to 500 s-1, which presented shear thinning rheological property of pseudoplastic fluid; apparent viscosity increased 10 times with the increase of wall material content, fragrance content and emulsifier content. Dynamic test indicated that enhanced viscoelasticity resulted from the increase of fragrance content and emulsifier content; dynamic modulus had complex changes with the increase of wall material content. The steady state rheological curves of different formulation rose fragrance nanocapsules were fitted well by Cross equation and Carreau equation, and the standard error was mostly controlled within 10.

    • >Drug and cosmetic materials
    • Synthesis, characterization and biological activities of Ru(II)–dmso complexes with heterocyclic hydrazones ligands

      2014, 31(3).

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      Abstract:Two [Ru(Ⅱ)Cl2(DMSO)2L1,2] type complexes were synthesized by mixing precursor complex cis-[RuCl2(DMSO)4] and heterocyclic aldehyde benzoyl hydrazone in ethanol (L1 is pyridine-4-formaldehyde benzoylhydrazone, L2 is furan-2-carboxaldehyde benzoylydrazone) .The new complexes were characterized by elemental analysis, IR spectra , UV-Vis spectra and 1HNMR. The electrochemical behavior of the complexes was studied with the help of cyclic voltammetry, Results indicate that [Ru(Ⅱ)Cl2(DMSO)2L2)] of five strains were used in the experiment has strong antibacterial activity.The antibacterial activity of complexes was detected by agar diffusion method and the anticancer activity of complexes was detected by MTT method, Results showed [Ru(Ⅱ)Cl2(DMSO)2L1] expression of growth promoting effect on cells, [Ru(Ⅱ)Cl2(DMSO)2L2)]Show the promotion before inhibition effect.

    • Synthesis of Strontium Ranelate

      2014, 31(3).

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      Abstract:Citric acid was reacted in concentrated sulfuric acid to product acetone- dicarboxylic acid. Methyl tetraester of ranelic acid was produced from acetonedicarboxylic acid by esterification reaction, cyclization reaction and alkylation reaction. Finally, strontium ranelate was synthesized from methyl tetraester of ranelic acid by hydrolysis reaction and salt formation. Orthogonal experiments and single factor experiments were developed to deter- mine the optimal conditions. The yield of the process is 37.9%. All compounds were con- firmed by H1-NMR, elemental analysis and XRD.

    • >Food and feedstuff chemicals
    • Self-assembly and Release Behavior of Vc-loaded β-conglycinin Nanoparticles

      2014, 31(3).

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      Abstract:β-conglycinin nanoparticles were prepared by self-assembly with desolvation method. The effect of protein concentration, volume ratio of ethanol to protein solution and amount of glutaraldehyde on nano-size was studied using turbidity method, and the release behavior of Vc embedded in the nanoparticles was determined. The results showed that the nanoparticles had better dispersity when the protein concentration, the volume ratio of ethanol to protein solution and the amount of glutaraldehyde (1.5 g/L) was 10-12 g/L, 4:1 and 0.5 mL, respectively. The nano-size was mainly around 350-380 nm. Vc in crosslinked nanoparticles released smoothly while Vc in uncrosslinked nanoparticles had a sudden accelerated phenomenon in the release rate, and the release mechanism of Vc in pH3.0 and 7.4 buffer solutions was Fickian diffusion and anomalous transport, respectively.

    • >Water treatment technology and environmental protection
    • Preparation of MgO/η-Al2O3 solid base catalyst for the hydrolysis of urea from wastewater

      2014, 31(3).

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      Abstract:MgO/η-Al2O3 solid base catalysts with η-Al2O3 as carrier were prepared and used for catalytic hydrolysis of urea in wastewater. X-ray diffraction and N2-BET techniques were applied to characterize the crystal structure and surface properties of catalysts, and back titration method was used to determine the basic sites amount. The effects of MgO loading amount (mass fraction), catalyst dosage, temperature of oil bath and reaction time on urea hydrolysis were respectively investigated. The results show that MgO/η-Al2O3 exhibits excellent catalytic activity for urea hydrolysis, and the urea removal rate increases with MgO loading amount and reaches the maximum when the loading amount is 14.29%. Under the condition of catalyst dosage of 40 g/L, temperature of 170 ℃ and reaction time of 8 h, a low urea concentration of 9.04 mg/L which has met the emission requirement (10 mg/L) is obtained by using 14.29% MgO/η-Al2O3 as catalyst. Furthermore, according to the results of stability tests, MgO/η-Al2O3 demonstrates a good recycling ability.

    • Study on the Removal and Kinetics of Parafuchsin from Aqueous Solution by calcined-β-CD-Fe-LDHs

      2014, 31(3).

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      Abstract:In this article, β-cyclodextrin (β-CD) intercalated ferrum-containing hydrotalcite was fleetly prepared by the technology of the microwave-crystallization and low saturated state of coprecipitation. The purposed sample of β-CD-Fe-LDHs and calcined-β-CD-Fe-LDHs were characterized by XRD, IR and SEM. The results show that the synthesized β-CD-Fe-LDHs with the flexible slice have the structure of LDHs. The calcined product is uniform particle state. Calcined-β-CD-Fe-LDHs was then applied to the removal of parafuchsin. The effects of photocatalyst types, the reaction temperature, parafuchsin mass concentration and cycle life on the parafuchsin removal were investigated. It is shown the percentage of removal for parafuchsin solution of 50 mg/L can reach 95.70% under the optimum conditions, and the removal rate can reach 79.99% even after 5 cycles. The kinetics cuvres of removal show that the removal is first-order kinetics model before 40 minutes under different photocatalyst mass concentrations and parafuchsin mass concentrations. The results suggest that calcined-β-CD-Fe-LDHs can be used as a novel and efficient photocatalyst for the removal of parafuchsin.

    • >Rubber and plastics auxiliaries
    • The Influence of Tetrahydropyrrole Spirocyclic Phosphoramidate on the Flame Retardancy and Mechanical Property of Cotton Fabrics

      2014, 31(3).

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      Abstract:Abstract: Tetrahydropyrrole Spirocyclic Phosphoramidate, a kind of flame retardant synthesized by ourselves, was used in cotton fabrics flame retardant finishing combined with polyacrylate resin adhesive. The flame retardant finishing conditions were optimized by orthogonal design method. It was found that the better finishing conditions are: the ratio of flame retardant and adhesive is 1.5:1(w:w), the ratio of cotton fabric and flame retardant adhesive is 60:40, the cure temperature is 140 ℃ and the cure time is 1.5min. Under the better condition, the LOI of the cotton raises from 18.2% to 28.9%, the flame retardant level reaches B1 level, and the breaking force increases from 364N(warp-wise)and 320N(across warp)to 917N(warp-wise)and 472N(across warp)N, which indicates that TPSP improves not only cotton’s flame retardancy but also the strength. Thermogravimetric Analysis results show that the cotton’s initial decomposition temperature reduces from 314.5℃ to 287.6℃,down 26.9℃ and the residue at 600℃ increases from 0.29% to 38.87%,up 38.58%, which indicates that TPSP improves effectively cotton charred form performance.

    • Synthesis of fire retardancy hexakis(4- acylhydrazone-2-methoxyphenoxy)-cyclotriphosphazene and its application in fire retardancy of ABS resin

      2014, 31(3):0-0.

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      Abstract:Hexakis (4-formyl-2-methoxyphenoxy)-cyclotriphosphazene (I) was prepared by hexachlorocyclotriphosphazene and 4-hydroxy-3-methoxy-benzaldehyde. Hexakis (4-formyl -2 -methoxy-phenoxy)-cyclotriphosphazene (I) then reacted with substituted hydrazides to give hexakis(4- acylhydrazone-2-methoxyphenoxy)-cyclotriphosphazene ( IIa - IIg). The structures of IIa – IIg were confirmed by elementary analyses, IR, 1H NMR, 13C NMR, and MS spectra. Fire- resistant ABS resin were prepared by compound IIa – IIg and ABS resin, and the limited oxygen index (LOI) and UL 94 were tested. The results showed that they exhibited flame retardant effect, especially IIe, IIf exhibited a significant flame retardant effect.

    • >Special dyes and pigments
    • Research on pH sensitivity of fluorescein derivatives and its photostabilities

      2014, 31(3).

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      Abstract:In this paper, 2’,7’-dihalofluorescein (DFF, DCF and DBF) were synthesized by the Diels-Alder reaction of 4-haloresorcinol with phthailc anhydride in the persence of methanesulfonic acid as catalyzer, and their structures were characterized. The pH titrations indicate that the dependences of fluorescent properties for these compounds on pH were extremely sensitive in the absorption spectra and the fluorescence spectra. The absorption intensities at 490, 502 and 505 nm, and the fluorescent intensities at 517, 526 and 530 nm in DFF, DCF and DBF increased with pH increasing, respectively. When the pH > 10, the absorption intensities and fluorescent intensities slightly decreased and then kept constant. The result shows that the thermodynamic pKa values and fluorescence quantum yields of DFF, DCF and DBF are 4.7, 5.1 and 6.6, and 0.97, 0.94 and 0.67, respectively. The photodegradation experiment indicated that photostabilities were DFF﹥DCF﹥FL﹥DBF in order.

    • >Fine chemical intermediates
    • Synthesis of iodo-substitued aromatic compounds in a micro-channel reactor

      2014, 31(3).

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      Abstract:The process for preparation of iodo-substitued aromatic compounds by iodination of diazonium salt and potassium iodide was investigated in self-made PTFE-microreactor. The effects of the inner diameter of microchannel reactors, current, capacity resident time and reaction temperature on yield were performed. The optimum conditions were determined as follows: the inner diameter of micro-channel reactors 0.8mm, total flow rate 1004.8μL/min, reaction temperature 20℃, reaction time 75s. The yield of iodobenzene was 79.0% under these conditions. The STC in micro-channel reactor was 9.41?03 mol?m?3?h?1, more than 100 times of that in a regular reactor. The optimum reaction conditions were also applied in the preparation of other iodo-substitued aromatic compounds in microreactor.

    • Study on the Synthetic Process of Dimethyldiallylammonium Chloride

      2014, 31(3).

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      Abstract:The effect of raw material ratios on the yield and polymerization reactivity of monomer dimethyldiallylammonium chloride(DMDAAC) was researched in this paper. DMDAAC was prepared by one-step method using dimethylamine, allyl chloride and sodium hydroxide as raw material. The yield of monomer and the intrinsic viscosity of its copolymer DMDAAC-co-AM with cationicity of 10% were used as assessment indexes, and the effect of raw material ratios on them was researched systematically, using the polymerization of DMDAAC-co-AM as template reaction . The results showed that, the raw material ratios had direct influence not only on the yield of DMDAAC monomer, but also on the polymerization reactivity in copolymerization. And the yield calculated based on DMA was 92.7% and the intrinsic viscosity of the copolymer was 12.8dL/g when the optimal raw material ratio was nAC:nNaOH:nDMA =2.08:0.965:1. The products of DMDAAC monomer and coplolymer were characterized by IR and NMR. The results established an experimental basis for the further development of DMDAAC monomer products with high yield, high purity, and high reactivity.

    • Synthesis of 3-(methylimino)benzofuran-2(3H)-one oxime

      2014, 31(3):0-0.

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      Abstract:1-(2-Hydroxyphenyl)-2-nitroethanone were synthesized through ring opening reaction of 4-Hydroxy-3-nitrocoumarin and the subsequent decarboxylation. Treating it with methoxyamine hydrochloride gave 1-(2-hydroxyphenyl)-2-nitroethanone O-methyl oxime, which underwent closing reaction mediated by sodium carbonate and gave 3-(methylimino)benzofuran-2(3H)-one oxime. Structures of all intermediates and target product were characterized by 1H NMR. The total yield was 70.4% and purity was as high as 99.2%. The synthetic process has features in high yield, easy operation, which are very promising in industrialization.