• Volume 28,Issue 9,2011 Table of Contents
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    • >Surfactants
    • Study on the mixed solution of OBS and SDS surfactant

      2011, 28(9).

      Abstract (1227) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The effects of sodium p-perfluorous nonenoxybenzene sulfonate (OBS) fluorocarbon surfactant and sodium dodecyl sulfate (SDS) hydrocarbon surfactant mixing ratio on the solution surface tension, interface tension, spreading properties and foam properties have been investigated to find the best mixing ratio in this paper. The results show that the mixing ratio of OBS/SDS has great influence on the mixed solution properties, the cooperative effect varies with the mixing ratio. Some mixed solution—the surface tension slight increase, but the interface tension are significantly lowered, so the spreading properties are greatly improved—can spread on cyclohexane in comparison with the OBS pure solution which can’t spread on cyclohexane. When the molar ratio is 0.46:1 and the concentration is 6.17×10-3mol/L , the spreading properties are the best, the mixed solution can quickly spread on cyclohexane, and the amount of OBS is significantly reduced by 46%. When the molar ratio is 0.15:1, the synergic effects of interface property and foamability are optimum. The best spreading concentration of mixed solution, which is denoted by the sign cs, also has been studied, it is found that the spreading properties of the mixed solution at cmc are not necessarily the best, the deviation between the cmc and the cs exists, and the gap is determined by surfactants properties and mixing ratio.

    • >Review and monographs
    • Research progresses in the biocidal performance and mechanism of polydimethyldiallylammonium chloride

      2011, 28(9).

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      Abstract:In this paper, the research progresses concerning the biocidal performance and mechanism of polydimethyldiallylammonium chloride (PDMDAAC) were reviewed based on the literatures. The discussion about the biocidal performance of PDMDAAC was carried out in four aspects, such as applied fields, action objects, action modes and action effects. The information about the biocidal mechanism of PDMDAAC was summarized. Therefore, it was pointed out that the present recognition about the biocidal performance of PDMDAAC was not satisfactory, and the description about the biocidal mechanism of PDMDAAC had almost not been touched. Finally, a series of valuable suggestions were put forward for further researches on the biocidal performance and mechanism of PDMDAAC.

    • >Functional materials
    • Effects on the Bismuth-doped Tin Oxide Nano-powders Prepared by Co-precipitation

      2011, 28(9).

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      Abstract:Bismuth-doped Tin Oxide (BTO) nano-particless were prepared by chemical co-precipitation method using SnCl4.5H2O and Bi(NO3)3.5H2O as precursors and NH3.H2O as precipitant. Effects of processing parameters on particle were investigated. These parameters include reaction temperature,terminal pH,doping bismuth content, calcine temperature, and PEG-600 dispersant. The BTO precursors were studied by TG-DTA. The product particles were characterized by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The optimized conditions for preparing nanometer BTO powders were proposed: reaction temperature of 60℃, terminal pH of 3, and the calcine temperature of 600℃, the minimum resistivity of BTO powders is 3.48Ω•cm under the optimized conditions.

    • Synthesis of dihydromyrcenol-type silane coupling agent

      2011, 28(9).

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      Abstract:Using platinum complexes(Pt-PMVS) as a catalyst for hydrosilylation reaction of dihydromyrcenol with triethoxysilane, a new type of silane coupling agent, [2,6-dimethyl-8-(triethoxysilyl)octan-2-ol](DHMS) is prepared,and the target product and by-products was characterized. The effects of reaction conditions such as solvent, reaction time, reaction temperature and Pt content reaction on the target product and by-products generation were investigated. The results show that under optimized reaction condition, the DHMS is obtained with yield up to 69.7%,and the purity is higher than 98% in weight.

    • >Biological engineering
    • Enzymatic hydrolysis of corn stalk treated by ionic liquid [BMIM]Cl after steam explosion activation

      2011, 28(9).

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      Abstract:For improving the yield of reducing sugars from corn stalk enzymatic hydrolysis,the steam explosion was selected as an activation method,ionic liquid [BMIM]Cl was used as a further treatment step, the influence of steam explosion pressure and time on the the yield of reducing sugars was evaluated. The results showed that after activating with a steam pressure of 2.6 MPa for 90 seconds treatment, the yield of reducing sugars from [BMIM]Cl treated corn stalk can increase by 84.03% compare to activated corn stalk and by 286.83% compare to untreated corn stalk. The relative content of cellulose in [BMIM]Cl treated corn stalk increased by 64.86%. X-ray diffraction analysis (XRD) and Scanning electronic microscopy (SEM) indicated that the structure of [BMIM]Cl treated corn stalk changed into amorphous. The changes of structure lead to the cellulase attach on easier. So it came to the conclusion that corn stalk treated by [BMIM]Cl and activated by steam explosion can enhancing the yield of reducing sugars significantly.

    • >Modernization technology of traditional Chinese medicines
    • Optimization of oil extraction from Gonocaryum lobbianum (Merr.) Kurz fruit and Analysis of its fatty acids

      2011, 28(9).

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      Abstract:The extraction rates for oil from Gonocaryum lobbianum (Merr.) Kurz fruit using three different methods, saxhlet extraction, ultrasonic extraction, and accelerated solvent extraction, were compared. The optimal ultrasonic processing conditions were explored by orthogonal experiments. The oil extracted by three methods was analyzed respectively using GC-MS, and their compositions and relative content of each fatty acid were determined. The optimal conditions for extraction consist of material-liquid ratio at 1:9, extracting duration of 10 min, ultrasonic output power of 400W, and 70℃ temperature.The highest oil yield was 31.21% under these conditions. GC-MS analysis showed that fruit oil extracted by three methods contained 7,9,and 8 kinds of fatty acids respectively; The fatty acid with the largest content was 13-Octadecenoic acid(70.86,68.71,69.92%), followed by Hexadecanoic acid(17.58,19.95,18.73%), then Octadecadienoic acid (Z,Z)-( 5.12,6.00,5.96%), The total contents of unsaturated fatty acids were 80.61,78.68,79.88%.

    • >Catalysis,separation and purification technology
    • Preparation of nickel-vanadium catalysts and their photocatalytic performance

      2011, 28(9).

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      Abstract:Ni-V-O/SiO2 catalysts were prepared by impregnation methods and characterized by XRD, UV-Vis and pyridine adsorbed FTIR. The effects of treatment temperature and Ni-V ratio of the catalysts on photocatalytic catalysis of carbonylation for methonal with carbondioxide were investigated under UV irradiation. The results indicated that the selectivity of methyl formate (MF) and dimethyl carbonate (DMC) could be up to 77.6% when the catalyst with 6:4 of Ni-V ratio was treated at 60 °C. Pyridine-FTIR analyses revealed that the catalyst surface contained Lewis acid sites and the acid content obtained by calculation was 1.85 mmol/g. The surface L acid strength was the major factor to influence the selectivity of carbonylation products.

    • The effect of ZnO on hydrogenolysis performance for glycerol of CuO-ZnO/ Al2O3 catalyst

      2011, 28(9).

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      Abstract:CuO-ZnO/Al2O3 catalysts supported on alumina was prepared by impregnation. XRD, XPS and TPR methods were used to characterize the distribution and chemical forms of CuO and ZnO impregnated on the catalyst. The results showed that copper oxide was the main active component, zinc oxide acted as a promoter in CuO-ZnO/Al2O3 catalysts. ZnO could modify the interaction between copper oxide and the supporter to reduce the reduction temperature of copper oxide. Hence, the hydrogenolysis performance for glycerol of the catalysts was improved. The Cu species in defect of electron was the hydrogenolysis active sites for the hydrogenolysis of glycerol. With a weight loading of 12% of CuO and Cu/Zn molar ratio of 1:1.5 in the catalystst. The conversion of glycerol was up to 97.82%, whereas the selectivity for 1,2-propanediol was nearly to 94%.

    • >Perfumes and essences
    • Preparation of Optically Active Acyloins by Sharpless Asymmetric Dihydroxylation

      2011, 28(9).

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      Abstract:Five optically active acyloins were prepared by Sharpless dihydroxylation of silyl enol ethers as intermediates starting from the corresponding ketones. 4-heptanone, 5-nonanone, 2,6-dimethyl-4-heptanone, 5-Methyl-3-hexanone and 4-Phenyl-2-butanone reacted with Me3SiCl or Me3SiI under the presence of different bases to give a kinetically controlled or thermally stable silyl enol ether. The obtained silyl enol ethers were oxidized through Sharpless asymmetric dihydroxylation using AD-mix- or  to give (S)-acyloins in >62% ee or (R)-acyloins in >75% ee respectively except the silyl enol ether derived from 5-methyl-3-hexanone. This silyl enol ether were oxidized to give (R)-acyloin whether AD-mix- or  was used. AD-mix- gave a 16% ee while AD-mix- gave a 76% ee. However, the silyl enol ether was oxidized by Oxone and Shi’s catalyst derived from D- or L-fructose to give (R)-acyloin in a 75% ee of (S)-acyloin in a 73% ee respectively.

    • Synthesis of Benzaldehyde Glycol Acetal by the Modified Expandable Graphite under Microwave Irradiation

      2011, 28(9).

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      Abstract:Abstract: Modified expandable graphite was prepared and used in the synthesis of benzaldehyde glycol acetal under microwave irradiation. The factors were investigated through orthogonal experiment. The optimum conditions were as follows: molar ratio of benzyladehyde to glycol 1:2.5, mass ratio of the catalyst to the total reactants 2.04%, microwave irradiation power 300W, irradiation time 20.0 min, and the amount of cyclohexane was 6mL, the yield of acetal reached 87.6%; and the activity of the catalyst remains basically unchanged after used 4 times. The catalyst was studied by SEM and XRD, which showed that interlayer compound was instituted by sulfuric acid molecules inserting the graphite’s layers.

    • >Food and feedstuff chemicals
    • Study on Extraction of collagen from donkey skin and its properties

      2011, 28(9).

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      Abstract:Citric-soluble collagen (CSC) and pepsin-soluble collagen (PSC) were successfully extracted from donkey skin, and the characterization of the collagens was investigated and compared. The results showed that both collagens exhibited a maximum absorbance at 234nm, but little absorbance near to 280nm. FTIR measurement of ASC and PSC were quite similar, and suggested the existence of triple-helix structure. Based on sodium dodecyl sulfate-polyacrylamide gel electrophoretic(SDS-PAGE) patterns, both samples were identified as type I collagen, containing two different α chains (α1 and α2). But thermal transition temperature of PSC (65.3℃) was slightly higher than the corresponding ASC (51℃) though the DSC(differential scanning calorimetry) detection. The hydroxyproline determination showed the purity of ASC was higher than that of PSC.

    • >Leather chemicals
    • Preparation and Properties of Graft Copolymer of Degraded Starch and HPA-CAE with HRP Catalysis

      2011, 28(9).

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      Abstract:Hydroxypropyl acrylate-citrate (HPA-CAE) was prepared by esterification of citric acid and hydroxypropyl acrylate. Then a graft copolymer was synthesized by copolymerization of degraded starch and HPA-CAE using horseradish peroxidase (HRP) /H2O2/acetylacetone (ACAC) as catalyst. The effects of amount of HRP, H2O2, ACAC and CA-HPA on grafting efficiency (GE) and grafting percentage (GP) were investigated. The optimum graft copolymer was synthesized by graft copolymerization of 50 g degraded starch (wt 15%) with 13.9 g CA-HPA in the presence of 6.4 mg HRP/4.7 mL H2O2/1.2g ACAC. The structure of the copolymer was characterized by FTIR and NMR. The applied results showed that the retanned leather had the merits of softness, fine grain and uniform thickness.

    • The Current Situation and Research of Ambient Cross-linking Systems in Acrylic Resin Leather Finishing

      2011, 28(9).

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      Abstract:Achieving macromolecular chain ambient cross-linking to form a network structure in acrylic resin leather coating process is a kind of widely adopted current technical ideas and methods. The mechanisms and ways of that are also hot spots in the current acrylic resin emulsion preparation research field. This paper reviews that the current situation of ambient cross-linking systems in acrylic resin leather finishing and emphatically introduces the research of late-model ambient cross-linking systems in that.

    • >Water treatment technology and environmental protection
    • The research on storage stability of composite coagulants PAC/PDM

      2011, 28(9).

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      Abstract:To research the storage stability of composite coagulants PAC/PDM prepared using Polyaluminum Chloride (PAC) and Polydimethyldiallylammonium Chloride (PDM), Al-Ferron complexation timed spectrophotometry was used to test the changes of the species distribution of Aluminum in the composite coagulations before and after stored at room temperature or at 80℃ in water bath, and the jar test was also used to evaluate their variation of coagulation performance. The results showed that none obvious change of the species distribution of Aluminum in the composite coagulants, caused by stored in different time at room temperature or at 80℃,could been observed. The jar test results indicated that the obvious changes of removal efficiency in turbidity and CODMn of composite coagulants resulted from storage were still not measured. Therefore, composite coagulants PAC/PDM had behaved a good storage stability.

    • >Papermaking chemicals
    • Preparation and Application of Water-in-Water Type Cationic Polyacrylamide Emulsion as Flocculation

      2011, 28(9).

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      Abstract:Water-in-water type cationic polyacrylamide (CPAM) emulsions with low viscosity, high polymer content and high stability were synthesized by radical copolymerization of acrylamide(AM),Methacrylatoethyl trimethyl ammonium chloride (DMC) and N,N′-methylenediacrylamide (MBA) as the monomers in the polyethylene glycol 20000(PEG 20000)solution. The effects of PEG2000,DMC, initiator(KPS),polymerization temperature on viscosity were studied; Kaolin flocculating tests shows:Under the condition the temperature is 40℃~50%,the reaction time 5 hours ~8 hours, w(PEG20000)=80%、w(KPS)= 0.8%,when w(MBA)=0.3%,w(DMC)= 10%,the product has better flocculating performance and good stability. Transmission electron microscope(TEM)shows spherical droplets and stripe shape droplets dispersed throughout aqueous dispertion.Infrared spectrum shows the synthesized polymer chain contents AM chain unit 、DMC chain unit and MBA chain unit.

    • >Special dyes and pigments
    • Syntheses and Characterization of a Series of Nickel Bis(dithiolene) Near-IR Dyes

      2011, 28(9).

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      Abstract:Four nickel bis(dithiolene) complexes with different substituent groups were synthesized and characterized. The physical and chemical properties of the complexes were systematically studied. The UV-Vis-NIR spectra showed strong and broad absorptions in the NIR region (700~1100 nm). The substituent effect and solvent effect of the complexes were investigated. The electron donating substituent results in the red-shifted absorption band, while the electron withdrawing substituent results in the hypsochromic-shifted absorption band. The red-shifted absorption band was observed as increasing the polarity of the solvent. The electrochemical properties were investigated by both of cyclic voltammetry/differential pulse voltammetry (CV/DPV). Furthermore, the HOMO and LUMO energy levels of the dyes were obtained by Density Functional Theory (DFT) calculations. TG studies revealed the good thermal stability of the complexes.

    • >Building chemicals
    • Preparation of silane modified fluorinated polyacrylate emulsion and its surface properties of nano-coatings

      2011, 28(9).

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      Abstract:A fluorinated polyacrylate (DLHK) emulsion was prepared by copolymerization of dodecafluoroheptyl methacrylate (DFMA), lauryl acrylate (LA), 2-hydroxypropyl methacrylate(HPMA) and 3-(methylacryloxyl)propyltri- methoxy silane (MPMS) in the presence of anionic/nonionic surfactants. The structure and physicochemical properties of DLHK were characterized by Infrared spectrum (IR), 1H-nuclear magnetic resonance (1H-NMR) and Transition electron microscopy (TEM). Then the DLHK emulsion was utilized to prepare the fluorocarbon coating and effects of temperature and dosage of emulsion on surface properties of coating were discussed. Results show that the DLHK latexes possess core-shell structures with an average particle size of 131nm and zeta potential of -24.09 mV. The coating displays favorable water repellency and water contact angle on its surface is 128°when dosage of emulsion and curing temperature are 25g and 150℃, respectively.

    • >Fine chemical intermediates
    • Synthesis of ethyl 2-(3-chloro-2-pyridinyl)-5-oxo-3-pyrazolidinecarboxylate

      2011, 28(9).

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      Abstract:2,3-dichloropyridine was synthesized from 3-aminopyridine by substitution and diazotization, which reacted with hydrazine to give 3-chloro-2 (1H)-pyridinone by electrophilic substitution.The resultant can be used in the next reaction without purification. Under the protection of nitrogen,absolute ethanol as solvent, Ethyl 3-chloro-2(1H)-pyridinone hydrazone reacted with diethyl maleate to give 2-(3-chloro-2-pyridinyl)-5-oxo-3-pyrazolidinecarboxylate, the total yield was 48.0%. Structure of the products were confirmed by IR and 1H NMR.The synthesis process was optimized, optimization of the reaction conditions were found as follows (base on 228.57 mmol 3-chloro-2(1H)-pyridinone hydrazone): under no water and oxygen, speed of dropping diethyl maleate was 10s/d , reflux 1h, the yield was 80.1%.

    • Synthesis and Biological Activity of Rotenone Oxime Amino Carbamates

      2011, 28(9).

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      Abstract:Four rotenone oximino carbamates derivatives were synthesized from natural rotenone with two steps. Their structures were clearly established by 1H NMR spectra. Compound 3b exhibited 68.3% mortality against Mythimna separata at 1.00 mg/mL, and 60.0% inhibition rate against Erysiphe graminis at 0.50 mg/mL,.

    • Synthesis of Methylphenyldichlorosilane with a Homogeneous Catalyst

      2011, 28(9).

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      Abstract:Methylphenyldichlorosilane was synthesized using methyldichlorosilane and chlorobenzene as raw materials and chloroform as the catalyst by an adaptation of the gas phase catalytic condensation method. The reaction yield and selectivity were measured by gas chromatography. The influences of the temperature, pressure and space time on the yield and selectivity were studied. The optimal reaction conditions were: temperature = 600℃, pressure > 0.5MPa, and space time = 32.2s ~ 70.4s. The highest product yield and selectivity were, respectively, 32.8% and 34.3%, which were obtained with the reaction condition of 0.56wt% CHCl3, 600 ℃, 0.7MPa and 56.3s space time.

    • Synthesis of 4-acetoxystyrene via catalytichydrogenation method

      2011, 28(9).

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      Abstract:Abstract: 4-acetoxystyrene(Ⅳ) was synthesized from 4-hydroxyacetphenone(Ⅰ) by acetlytion, catalytichydrogenation and dehydration with an overall yield of 68.7%. The structure of intermediate and target products was elucidated by spectrum techniques including 1HNMR and IR. The catalytichydrogenation process was optimized, and the suitable conditions were found as following: T=80℃, P=3Mpa and stir rate=600r/min, using Raney-Ni(mRaney-Ni:m4-acetoxyacetophenone=10%) as the catalyst and ethanol(V ethanol:m4-acetoxyacetophenone=4ml/g) as the solvent. The yield is 83.1% under the above conditions. The yield of the dehydration is 85.0% with Nafion-H as catalyst.

    • Synthesis of dodecyl glycidyl ether by phase transfer catalysis

      2011, 28(9).

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      Abstract:In the presence of phase-transfer catalyst, dodecyl glycidyl ether was synthesized from lauryl alcohol and dichloropropanol. The catalyst type, mole ratios, time and reaction temperature were investigated to optimize the reaction conditions. The optimum reaction condition were obtained as follows: n(lauryl alcohol ):n( dichloropropanol )=1:1.60, at 50 ℃ for 4 h and tetrabutyl ammonium bromide as phase tranfer catalysis, the yield of dodecyl glycidyl ether was 73.2%. The structure of product was characterized by IR and NMR. The yield of dodecyl glycidyl ether was calculated by measure its epoxy value.