• Volume 29,Issue 9,2012 Table of Contents
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    • >Review and monographs
    • The Study Progress on Biomass Sizing Agent

      2012, 29(9).

      Abstract (396) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:There are many advantages in preparing the sizing agent in the paper industry by using these biomass resources, such as the reasonable utilization of resources, cost reduction, protection of the environment and so on. The biomass sizing agents such as modified rosin, starch and modified starch, animal glue and so on are often used in the paper industry. The paper mainly introduce four kinds of biomass sizing agents, and their applied situation is also further expounded in the paper industry.

    • >Functional materials
    • Synthesis and Properties of Silicone Modified Epoxy Resin

      2012, 29(9).

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      Abstract:The good silicone modified epoxy resin was synthesized when the hydrolysis temperature was 35~40℃, the hydrolysis time was 1~1.5h ,and the hydrolysis ratio was nH2O/ncl=6:1~7:1.IR indicated that the mainly chemical reaction was occurred between hydroxyls of silicone and epoxy resin.The influence of modified and unmodified epoxy resin on mechanical properties, heat-resistant and moisture resistance was studied.The results show that when R/Si was 1.5, the tensile strength was 23.91MPa ,bending strength was 29.24MPa, the impact strenth was 10.02 KJ•m-2 and the temperatrue of 50% weight loss was 431℃,higher than those of unmodified epoxy resin by 3.86 MPa,9.49 MPa,6.18 KJ•m-2 ,30℃,respectively;At the same time,the moisture resistance of modified resin was increased.

    • Synthesis of Acrylic acid-based/Kaolinite superabsorbent polymer

      2012, 29(9).

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      Abstract:The Kaolin/(AA-AM-DMC) superabsorbent resin with cationic monomer, nonionic monomer and anionic monomer was prepared by inverse suspension method, using cyclohexane as continuous phase, N, N-methylene-bis-acrylamide as crosslinking agent, potassium persulfate as initiating agent, Span 60 as dispersing agent. The effect of the degree of neutralization of acrylic acid, Kaolin amount, DMC amount, initiating agent amount, crosslinking agent amount, and polymerization temperature were investigated. The superabsorbent resin was characterized by IR spectroscopy and SEM. Water absorption rate under the optimal conditions can reach 1827g/g and salt absorption rate can reach 146g/g.

    • Green synthesis of silver@graphene nano-composite and its antibacterial activity

      2012, 29(9).

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      Abstract:Ag@Graphene nano-composite was prepared by one step in situ synthetic method, using polyethylene glycol as reductant. Graphene oxide and silver ions were reduced at the same time under hydrothermal reaction. UV-vis spectroscopy, X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR) and transmission electron microscope (TEM) were used to characterize the as-prepared nano-composite. The results of characterization indicated that silver nanoparticles were uniformly anchored on the surface of graphene sheets and the average particle size was 30nm. Antibacterial activity was tested using E. coli as model strain. The minimal inhibitory concentration of Ag@graphene against E. coil was 100µg/mL, making the composite an outstanding and novel antibacterial material.

    • Preparation of Magnetic Microcapsules by Solvent Evaporation Method and Corresponding Properties

      2012, 29(9).

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      Abstract:In this paper, the magnetic microcapsules were prepared by means of solvent evaporation. Core material was magnetofluid whose nano OA-Fe3O4 (oleic acid modified Fe3O4) magnetic particles prepared with coprecipitation were dispersed in different solvent media. Shell material was PMMA (polymethyl methacrylate). Optimum core material and emulsifier were selected. The encapsulation parameters, including mass fraction of emulsifier, core material to shell material mass ratio and shearing emulsification rate were investigated respectively. The active ingredient, morphology, thermal property and magnetic responsiveness of OA-Fe3O4 and magnetic microcapsule were characterized by XRD, FTIR, TEM, SEM, optical microscope and VSM (vibrating sample magnetometer). The results show that the effective ingredient of nanoparticle prepared by coprecipitation is Fe3O4, which can be successfully microencapsulated. The OA-Fe3O4 exhibits monodispersity, and its particle size is 3-15nm. OA-Fe3O4 also shows superparamagnetism, and its saturation magnetization is 43.3emu/g. The optimum process parameters of preparing magnetic microcapsules as follows: Magnetofluid of OA-Fe3O4 dispersing in n-C16H34 is core material, mass fraction of emulsifier SDS (sodium dodecyl sulfonate) to total emulsion is 2%, core material to wall material mass ratio is 5:1, and shearing rate is 800r/min. The wall thickness of magnetic microcapsule is 1-2μm and the particle size is concentrated on 10±2μm. The saturation magnetization of magnetic microcapsule is 43.3emu/g, which shows good magnetism response under magnetic field.

    • >Surfactants
    • Study on the synthesis and properties of stearic ethanolamide polyoxyethylene ether glucopyranoside

      2012, 29(9).

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      Abstract:A series of stearic ethanolamide polyoxyethylene ether glucopyranoside with different polymerization degree(n) of epoxyethane (EO) were synthesized .The structure of the products were characterized by IR and 1HNMR .Surface physicochemical properties of these products were measured .The results showed that surface tension (γcmc) varied from 30~38mN∕m and critical micelle concentration (CMC) varied from 1×10-5~10×10-5g∕ml. The relationship between surface physicochemical properties of products and polymerization degree of EO were studied systematically. The application properties such as emulsifying power(with turpentine)、foaming ability、hard water stability、absorbing and keeping moisture rate improved with the increase n of EO.

    • ulphonated fatty acid salt surfactant synthesis and flotation study for fluorite

      2012, 29(9):0-0.

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      Abstract:sulphonated fatty acid salt surfactants were prepared from the biodiesel production of illegal cooking oil by oxidation-reaction method. The optimal synthetic conditions were system introduced. Their flotation process performance for pure minerals and fluorite ore were studied.The result showed that the recovery of fluorite rise significantly with increase of pulp pH, when the pH is 9.06 and the collector density is 80mg/L, the recovery of fluorite is 97.13%.The results of bench scale -flotation indicated that by using sulfonated fatty acid salts as collector,the recovery of fluorite can reach to 98.01%,which is 1.21% higher than conventional collector oleic acid.

    • >Biological engineering
    • Study on kinetics of ABE production by continuously coupling the fermentation and pervaporation

      2012, 29(9).

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      Abstract:Acetone-Butanol-Ethanol (ABE) fermentation continuously coupling with pervaporation was conducted in a continuous and closed-circulating fermentation system by combining clostridium acetobutylicum and PDMS membrane bioreactor. The continuous fermentation was successfully lasted for 192 h, and the corresponding kinetic behaviors were studied. During the continuous fermentation, cell concentrations of 0.84~4.00 g/L, glucose concentrations of 16.08~35.15 g/L, the total solvents concentrations of 5.14~17.54 g/L in the fermentation broth and ABE productivity of 0.36 g/(L?h) were achieved. The results showed that ABE fermentation continuously coupling with pervaporation in a PDMS membrane bioreactor system is feasible and promising.

    • >Modernization technology of traditional Chinese medicines
    • Study on Antioxidant Activity of Ophiopogon japonicus Extracts by DPPH Assay

      2012, 29(9).

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      Abstract:The total saponins, total flavonoids and total proteins were extracted from Ophiopogon japonicus. The antioxidant activity of three extracts were investigated by DPPH assay. Ascorbic acid, thiourea and catechins were used as posititive control and IC50 value as the evaluating criterion of DPPH free radical scavenging capability. The results show that at the wavelength of 517 nm, the calibration curves showed good linearity in the range of 25.8~51.5 μg/mL of DPPH. The IC50 of antioxidants(ascorbic acid, thiourea and catechins) were 87.0,482.9 and 10.2 μg/mL respectively. The IC50 of the extracts from O. japonicus(total saponins, total flavonoids and total proteins) were 509.0,79.4 and 46.0 μg/mL. The strength in the order of IC50 was catechins﹥total proteins﹥total flavonoids﹥ascorbic acid﹥thiourea﹥total saponins. In addition, multi-cluster analysis show that total flavonoids, total proteins, ascorbic acid and catechins had a similar intensity of antioxidant activity, which sihgnifies that the total flavonoids and total proteins from O. japonicus had strong antioxidant activity.

    • >Perfumes and essences
    • Volatile aroma compounds of Rosa Roxburghii Tratt and Rosa sterilis

      2012, 29(9):0-0.

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      Abstract:Volatile aroma compounds of Rosa Roxburghii Tratt and Rosa sterilis was extracted by solid-phase microextraction , identified by GC-MS technique and their relative content was ascertained by area normalization method of each constituent . There were 31 compounds be found in the extracts from Rosa Roxburghii and 32 compounds be found in the extracts from Rosa sterilis. 14 compounds were the common compounds of the two plants . The main compounds in Rosa Roxburghii were Trans,-bata.-ocimene(20.649%), Nonanal(5.029%)), 1-humulene (6.101%), , Gama-Seliene (12.733%), Hetriacontan (6.507%) The main compounds in Rosa sterilis included 3-Hexen-1-ol,acetate- (Z)-( 10.649%), Trans-,beta-ocimene(5.672%),1-humulene (10.643%), Alpha-humulene(5.911%), Gama-Seliene (18.218%), Alpha -Seliene(5.412%), Heptadecane,9-octyl- (11.573%). There are some differences in the main component of Rosa Roxburghii Tratt and Rosa sterilis . This result provided a scientific basis for utility of Rosa Roxburghii Tratt and Rosa sterilis .

    • >Food and feedstuff chemicals
    • The preparation and dynamics of glucose stearic acid esters by lipase-catalyzed reaction in non-aqueous media

      2012, 29(9).

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      Abstract:Sugar esters are widely used in the food, cosmetic, detergent and phar-maceutical industry. The preparation and it’s dynamics of glucose stearic acid esters (GSAE) by lipase-catalyzed reaction were studied in this work. The available lipase of catalytic synthesis GSAE in non-aqueous media was screened from 7 commercial lipases. To facilitate these reactions, a certain volume of glucose, stearic acid, lipase, molecular sieve 3A, solvents etc were added in 50 ml tapered bottles, respectively. The results showed that lipase Novozyme 435 proved to be efficient catalysts of enzymatic preparation GSAE, acetone was appropriate solvent, and Novozyme 435 could keep high activity in acetone. And excessive water in the reaction system obviously decreased the activity of Novozyme 435 and the yield rate of GSAE, thus it was very necessary to add defined amount moisture absorber to remove the water of substrates, solvent and reaction process. The optimized esterification reaction conditions with 0.08 g Novozyme 435, 0.8 g 3A molecular sieve, the ratio of stearic acid and glucose = 3:1, 10 ml acetone, 150r/min shaking, 45℃ reaction temperature, 5 h reaction time were good for making the produce GSAE in non-aqueous media. In the optimized condition, the maximum reaction rate Vm was 0.749 μmol/min?g, Km was 0.0203 mmol/L and the GSAE yield rate was up to 64.11%.

    • >Water treatment technology and environmental protection
    • Influence of inorganic salts on viscosity behavior and coagulation performance of Composite Coagulants

      2012, 29(9).

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      Abstract:The influences of inorganic salts on viscosity behavior and coagulation performance of composite coagulants Polyaluminum Chloride (PAC)/ Polydimethyldiallylammonium Chloride (PDM) have been researched in this paper. Furthermore, the correlation of these two influences has been deduced. Ubbelohde viscometer was used to study the influence of inorganic salts on reduced viscosity of PAC/PDM; meanwhile jar test was used to study the influence of inorganic salts on coagulation performance of PAC/PDM. The results showed that different inorganic salts have different influences on the viscosity behavior of compose coagulants and the sequence of the influence from strength to weakness was: AlCl3 > MgCl2> NaCl, and white precipitation was formed while Na2SO4 and Na3PO4 were added in the composite coagulant solutions. The jar test results indicated that, as coagulants, AlCl3 could enhance the coagulation performance of PAC/PDM obviously, NaCl and MgCl2 had no influence on the coagulation performance, and Na2SO4 weakened the performance while Na3PO4 first weakened then enhanced it. Therefore, there is no direct correlation between the influences of inorganic salts on the viscosity behavior and the coagulation performance of PAC/PDM.

    • >Acrylic series chemicals
    • RAFT microemulsion polymerization of methyl methacrylate

      2012, 29(9).

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      Abstract:In this article, a difunctional RAFT agent S, S′-bis (α, α′-dimethylacetic acid) trithiocarbonate (BDAT) was synthesized and used as chain transfer to mediate the reversible addition-fragmentation chain transfer (RAFT) polymerization of methyl methacrylate (MMA) in microemulsion. The influence of polymerization temperature and concentration of RAFT agent on the polymerization were investigated respectively, and the polymerization kinetic constants were calculated. Experimental results showed that the RAFT polymerization in microemulsion exhibited living polymerization characters. The molecular weight of products increased linearly with conversion, the polydispersity indexes remained low value, and the polymerization processes were totally under control with increasing concentration of RAFT agent. In addition, the influence of RAFT concentration on the particle size was investigated by TEM. The TEM results indicated that the particles were highly monodispersed and the particle size increased with increasing concentration of RAFT agent.

    • Preparation and Dynamics Researches of SS-g-P(AA/AM)/PGS Superabsorbent Resin

      2012, 29(9):0-0.

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      Abstract:A low cost superahsorbent resin, SS-g-P(AA/AM)/PGS, based on the natural sorghum straw (SS, particle size>180 mesh) as the source of cellulose, was prepared by grafting copolymerization of acrylamide (AM) and partly-neutralized acrylic acid (AA) on the chain of SS mixed with palygorskite (PGS). The copolymerization was carried out using N, N?methylene double acrylamide (MBA) as crosslinking agent and potassium persulfate (KSB) as initiator. The morphology and structure were characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The water-absorption capability as well as the thermal stability of the polymers were also characterized. The results show that the superabsorbent resin bears the maximum absorption amount of 273.0 g/g for distilled water and 66.7 g/g for tap water when the total adding amount of palygorskite and sorghum straw accounts for 19.8% in SS-g-P (AA/AM)/PGS. The dynamics behavior of the resin was also well investigated through the observation of swelling features, and was found that a Fickon and a non-Fickon diffusion model were accordance with the absorption of distilled water and tap water, respectively.

    • >Special dyes and pigments
    • Preparation of Fluorescent Disperse Dye Paste and Its Stability

      2012, 29(9).

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      Abstract:Fluorescent disperse paste was prepared with four kinds of benzopyran fluorescent disperse dye and naphthalene sulfonic derivative dispersing agent using wet grinding process and their stability property was assessed for inkjet printing ink. Particle sizes and fluorescence intensity of the obtained four kinds of dye paste decreased with prolonging the grinding time. The absorbance ratio of the fluorescent disperse pink BG centrifuged for 50 min was 78.1%, indicating that pink BG paste performed excellent centrifugal stability. The particle sizes of all the fluorescent disperse dye paste increased after stored for 5 d at 55℃. The fluorscent disperse orange BG presented better thermal property as its particle size increased by only 7.5%. The fluorescence intensity of dye paste also reduced after heated. From all the discussions, the fluorescent disperse pink BG performed excellent stability to apply in the preparation of inkjet printing ink.

    • >Adhesives
    • Preparation and study on the properties of Polyurethane-Type polymeric thioxanthone photoinitiators

      2012, 29(9).

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      Abstract:Polyurethane-Type polymeric photoinitiators containing side-chain thioxanthone and in-chain coinitiator amine were synthesized through step polymerization of diisocyanate, 2-(2, 3-dihydroxy)propoxy-thioxanthone (HPTX) and N-methyl diethanolamine. The thioxanthone and coinitiator amine structures were successfully introduced into the backbones of polymeric photoinitiators. FT-IR and 1H NMR analyses confirmed the structures of polymeric photoinitiators. UV-Vis spectra showed the macromolecular chain have no obvious effect on the maximal absorption of thioxanthone moieties. Photopolymerization of polyurethane acrylate resin (PUA), initiated by Polyurethane-Type polymeric thioxanthone photoinitiators, was studied through photo differential scanning calorimetry (photo-DSC). The results indicate that PU-IMTX is the most efficient photoinitiator for the photopolymerization of PUA among the photoinitiators synthesized in this article.

    • Effect of CTAB on the application performance of starch-based wood adhesive

      2012, 29(9):0-0.

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      Abstract:The effects of cetyl trimethyl ammonium bromide (CTAB) on shear strength, viscosity, mobility and storage stability of starch-based wood adhesive were studied. The action mechanisms of CTAB were preliminarily discussed. It was showed that, although CTAB addition resulted in slight decrease in shear strength of starch-based wood adhesive, the mobility and the storage stability of adhesive could be improved significantly. 1.5%(w/w, dry starch basis) of CTAB led to good application performance of starch-based wood adhesive. The results of differential scanning calorimeter(DSC) and scanning electron microscopy (SEM) suggested that action mechanisms of CTAB might be to hinder the aggregation of starch molecules, which inhibited the short-term and long-term retrogradation of starch.

    • >Fine chemical intermediates
    • Synthesis of 3-methoxy-4-benzyloxyphenethylamine Hydrochloride

      2012, 29(9).

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      Abstract:Vanillin was first treated with benzyl bromide for the benzylation, the aldehyde condensed with nitromethane, then reduced with sodium borohydride in the presence of boron trifluoride etherate to give 3-methoxy-4-benzyloxyphenethylamine which was lastly treated with hydrochloric ethyl acetate to give the final compound. The effects of reagent mole ratio, reaction temperature and time on the yield of the condensation were studied, and also the effects of reducing agent proportion and reaction time on the yield of the reduction were studied. The total yield could reach up to 79.4% in four steps, and the structure of the target was confirmed by means of ESI-MS and 1H-NMR.

    • Biocatalytic Production of 2- Aminobutyric acid using "One-pot" process

      2012, 29(9).

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      Abstract:With Threonine deaminase (L-TD) and leucine dehydrogenase (L-LeuDH) obtained by cloning and expression as biocatalyst, the natural amino acid was converted into unnatural amino acid using the "one-pot" process. Finally, the product was obtained by crystallization with a total yield of 84%.The configuration of the product obtained was confirmed by LC-MS and 1H-NMR, and the ee > 99.9%. This process uses cheap raw materials and enzymes, and avoids the intercurrent extraction and separation, providing a good prospect for an efficient and low-cost 2-aminobutyric acid production process.

    • Synthesis and crystalline structure of triethylamonium tris(perfluorophenyl)-p-hydroxyphenylborate

      2012, 29(9).

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      Abstract:Triethylammonium (p-hydroxyphenyl) tris (pentafluorophenyl) borate (a) was successfully synthesized by deprotection of triethylammenium (4-(tert-Butyldimethyl silanyloxyphenyl) tris(pentafluorophenyl) borate (b) in Et3N·3HF-THF solution, wherein (b) was obtained by reacting tris(pentafluorophenyl) borane with (4-((tert-butyldimethylsilyl) oxy) phenyl) magnesium bromide. Under the optimized reaction conditions, in which the molar ratio of 4-TBDMSO-C6H4MgBr/(C6F5)3B, NEt3∙HCl/B and NEt3∙3HF/B is 3:1, 5.7:1 and 1.3:1 respectively , the molar yield of (a) borate is 54.2% on the basis of tris(pentafluorophenyl) borane and 19F NMR purity is 99.2%. Furthermore, crystal of this compound was obtained for the first time and X-ray single crystal diffraction analysis revealed that the compound crystallizes in Orthorhombic, space group Pbca.

    • Synthesis and Characterization of 2,7-Dibromo-N-octylcarbazole

      2012, 29(9):0-0.

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      Abstract:2,7-Dibromo-N-octylcarbazole (3) was synthesized from 4,4,-dibromobiphenyl by nitration, the Cadogan cyclization and N-alkylation. Nitration of 4,4,-dibromobiphenyl by HNO3 with n(4,4,-dibromobiphenyl)︰n(HNO3)=1.0︰4.0 gave 4,4,-dibromo-2-nitrobiphenyl (1) with a yield of 97% at 75 ℃ for 5 h. The cyclization of 1 by triphenylphosphine with n(4,4,-dibromo-2- nitrobiphenyl) : n(triphenylphosphine)=1.0 : 3.0 gave 2,7-dibromocarbazole (2) with a yield of 68% in Schlenk flask. N-alkylation of 2 by bromooctane with n(2,7-dibromocarbazole) : n(bromooctane)=1.0 : 1.5 gave the title product with a yield of 85% under the alkaline conditions. The structure of the product was characterized by IR, elementary analysis and 1H NMR spectra.

    • Synthesis of Ethylene Glycol Monoethyl Ether Acetate with Ceric Sulfate Tetrahydrate as Catalyst

      2012, 29(9):0-0.

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      Abstract:Ethylene glycol monoethyl ether acetate was synthesized from ethylene glycol monoethyl ether and acetic acid with ceric sulfate tetrahydrate as catalyst and cyclohexane as water entrainer. Its structure was confirmed by IR,1HNMR. Effects of molar ratio of ethylene glycol monoethyl ether to acetic acid, the variety and dosage of catalyst , the amount of water entrainer, reaction temperature and reaction time on the yield of the product were studied.Based on 0.2 mole ethylene glycol monoethyl ether,results at acetic acid/ ethylene glycol monoethyl ether molar ratio of 1.5:1, ceric sulfate tetrahydrate / ethylene glycol monoethyl ether mass ratio of 0.05:1,amount of cyclohexane (used as water entrainer) 9 mL, reaction temperature 130℃,for 2 hours reaction time give the highest yield of ethylene glycol monoethyl ether acetate above 97%.