• Volume 31,Issue 1,2014 Table of Contents
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    • >Functional materials
    • Preparation and Characterization of Modified Chitosan Membrane with Iodine

      2014, 31(1).

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      Abstract:The modified chitosan (RS-CTS-E) and the corresponding gel membrane were prepared by chitosan (CTS) reacted with salicylaldehyde, and then cross-linked with epichlorohydrin. The modified chitosan membrane with iodine (RS-CTS-E-I2) was prepared by modified chitosan gel membrane immersed in a certain concentration of iodine in ethanol solution. The properties of the RS-CTS-E-I2 membrane were characterized by SEM, IR, etc. The analysis of iodine content showed that the adsorption of iodine of modified chitosan gel membrane increased along with the iodine concentration of ethanol. The adsorption kinetics of iodine result showed that the equilibrium adsorption time was 6 h. The antimicrobial test result showed that the antibacterial diameters of against Staphylococcus aureus and E.coli of the RS-CTS-E-I2 membrane were (31 ± 1) mm and (30 ± 1) mm, respectively, when the iodine mass fraction of the RS-CTS-E-I2 membrane was 19.05%, the bacteriostasis degree was very significant.

    • >Rubber and plastics auxiliaries
    • Synthesis and Application of Chlorine-bromine Silicate Ester Flame Retardants

      2014, 31(1).

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      Abstract:Tribromophenol sodium was reacted with epichlorohydrin to generate tribromophenyl epoxy propyl ether, then tribromophenyl epoxy propyl ether was reacted with silicon tetrachloride to generate intermediate product tribromophenoxy chloropropoxy silicon trichloride, the intermediate product was further reacted with ethylene oxide, to generate chlorine-bromine silicate ester flame retardants. The effect of reaction temperature, time and amount ratio of substance on the reaction yield was discussed. The optimal conditions for preparation were selected as follows: n(tribromophenyl epoxy propyl ether): n(silicon tetrachloride): n(ethylene oxide) was 1:1:3.2, reaction time was 4h at 50℃. The percentage of the reaction yield could reach 98.6%. The molecular structures of the product and its flame retardant properties were characterized by means of FTIR, 1H-NMR and LOI technique. Applied Research showed that the flame retardants had good flame retardant plasticizer for PVC and other materials.

    • >Drug and cosmetic materials
    • Improved synthesis of lonidamine

      2014, 31(1).

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      Abstract:Lonidamine was synthesized from phenylhydrazine and 2,4-dichlorobenzyl bromide as the raw materials. Phenylhydrazine was acetylated, and then reacted with hydroxylamine hydrochloride, chloral hydrate and sodium sulphate to form N-acetyla-minoisonitrosoacetanilide, which was subsequently hydrolyzed to obtain 1H-indazole-3-carboxylic acid after Beckmann rearrangement and ring shrinking reaction. 2,4-dichlorobenzyl bromide was prepared by 2,4-dichlorotoluene and NBS with AIBN as catalyst, and then reacted further with 1H-indazole-3-carboxylic acid to get the product of lonidamine. The influence of process conditions on the yield of N-acetyla-minoisonitrosoacetanilide was studied by single-factor experiment and orthogonal test. The optimal conditions for the reaction were: the molar ratio of n(N-acetylphenylhydrazine), n(chloral hydrate) and n(sodium sulphate) 1:1.3:8.5, reaction temperature 90℃ and reaction time 13min. The process can get the product in 86.9% yield under the above optimized reaction conditions. The total yield of lonidamine was 31.2%. Structure of product was characterized by IR, 1H NMR and MS.

    • >Biological engineering
    • Autolysis of Ultrasonic Coupling Extraction from Waste Beer Yeast β- (1, 3) - D - Glucan Research

      2014, 31(1).

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      Abstract:Abstract: Autolysis-ultrasonic coupling method was adopted to extract β- (1, 3) -D- glucan from waster beer yeast. Firstly, single factor and orthogonal test were designed to study the effect of different autolysis promoters on yeast autolysis. The results showed that the mixture of 5% NaCl+1.5% ethyl acetate can effectively promote yeast autolysis. Furtherly, ultrasonic method was used to extract β-(1, 3)-D-glucan from the cell wall deposition harvested after autolysis. The effects of ultrasonic power, ultrasonic time and ultrasonic times were explored in 2% NaOH solvent by response surface methodology. The results indicated that the optimum parameters were ultrasonic power 550 W, ultrasonic time 33 minutes, 2 ultrasonic times. Under the above conditions, the extraction rate of β-1, 3-glucan was up to 50.5 %, which was doubled as compared with pure ultrasonic method without autolysis pretreatment.

    • >Functional materials
    • Synthesis of benzamides Containing Active structure of Capsaicin and their Bacteriostatic activity and Antifouling Capability

      2014, 31(1).

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      Abstract:Four benzamide compounds(HDDB、THBHB、HMBB、HBOMB) containing active structure of capsaicin were synthesized and their structures were confirmed by IR spectroscopy and 1HNMR. The bioassay results showed that all the four compounds possessed good antibacterial activity, with MIC value of HBOMB for Escherichia Coli and Staphylococcus aureus were 0.0625mg/mL and 0.1250mg/mL. And they were also studied as antifouling agents in antifouling paint, test panels immersed for 120 days were only covered with a few Balanus.

    • >Fine chemical intermediates
    • The research in the synthesis of γ-nitro ester compounds by solvent-free ball-milling method

      2014, 31(1).

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      Abstract:A calcium nitrate prompted solvent-free Michael addition reaction of nitroalkenes with malonate esters to synthesize γ-nitro ester compounds by ball-milling method has been developed. The reaction is carried out at a frequency of 20Hz,and takes 30min to complete conversion. Nitroalkenes and their derivatives reacted with malonate esters obtain the target product with the yield of more than 80% , especially when there are two electron-withdrawing groups in the ortho position of the phenyl ring of nitrostyrene, the yield is up to 95%.

    • reparation and Characterization of Al2O3-AlClx-3 Catalyst and Its Catalytic Performance for Oxidation of Alcohol

      2014, 31(1).

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      Abstract:Using cotton as template, an efficient and highly recyclable porous tubular catalyst Al2O3-AlClx-3 was prepared by chemical tailor with hydrochloric acid. The structure of Al2O3-AlClx-3 catalyst was characterized by field emission scanning electron microscopy and X -ray photoelectron spectroscopy. Applying Al2O3-AlClx-3 catalyst in the oxidation of alcohol under optimized conditions, several parameters such as solvent system, catalyst amount, reaction temperature, and reaction time were screened. It was found that Al2O3-AlClx-3 catalyst is available for the oxidation of alcohol to corresponding aldehyde or ketone with higher conversion and selectivity using Oxone?as an oxidant. Basing on the literatures and experimental result,we have proposed a possible mechanism for the alcohol oxidation.

    • >Special dyes and pigments
    • Preparation of Nanoscale TiO2/PMMA Composite Particles by Miniemulsion Polymerization

      2014, 31(1).

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      Abstract:The nanoscaleTiO2/PMMA composite particle was prepared via miniemulsion polymerization. The influences of co-emulsifier, emulsifier, monomer and initiator on properties of the dispersion were investigated. The results show that hexadecane (HD) was more effective to inhibit the Ostwald effect than that of cetyl alcohol (CA) and dodecanol(LA). When the mass ratio of MMA and TiO2, HD and MMA, DNS-86 based on the whole dispersion, was 60%, 6% and 2%, respectively, the particle size of nanoscale TiO2/PMMA composite particle was 185nm, which was similar to that of pre-emulsion under these conditions. The white ink prepared by nanoscale TiO2/PMMA composite showed higher hiding power and stability than that of by nanoscale TiO2.

    • >Functional materials
    • Synthesis and Properties of Dendritic Poly(amine-ester) with Polyoxyethylene Chain

      2014, 31(1).

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      Abstract:Dendritic poly(amine-ester) with polyoxyethylene chain (PAE-PEO-A和PAE-SAA-PEO-A)is synthesized from a dendrimer with 8 primary amine as the terminal group[PAE(NH2)8] and poly(ethylene oxide) [PEO-A(454)] or sodium acrylate(SAA) and poly(ethylene oxide). Effects of reaction temperature, reaction time and ratio of reactants on the yield of products were discussed by orthogonal experiment. The structure of products was identified by FTIR. The surface tension of dendritic poly(amine-ester) with polyoxyethylene chain and their solubilization effects for benzoic acid and salicylic acid were determined. It was found that when reaction temperature reaction temperature was 65℃, reaction time was 96 h, n [PAE(NH2)8] : n [PEG-A(454)]=1:16, CH3OH as solvent, the yield was 88.30%. The critical micelle mass concentration of PAE-PEO-A solution was 0.0075 g/L. Its lowest surface tension was 43.8 mN/m. PAE-PEO-A has a solubilization of benzoic acid and salicylic acid. Solubilization capacity increased with increasing the number of surface functional groups and concentrations. It was found that when reaction temperature reaction temperature was 50℃, reaction time was 96h, n[PAE(NH2)8] : n (SAA) : n[PEO-A(454)] =1:12:8, CH3OH as solvent, the yield was 48.83%. It was found that PAE-SAA-PEO-A has good water solubility and surface activity. PAE-SAA-PEO-A has good solubilization of benzoic acid and salicylic acid, especially salicylic acid. PAE-SAA-PEO-A solution exhibits obviously solubilization effect for salicylic acid which is about 2.4 times that of PEG-400 at same concentration of 0.500g /L.

    • Effect of Preparation Method on the Performance of Li4Ti5O12

      2014, 31(1).

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      Abstract:Spinel Li4Ti5O12 powders are prepared by solid state reaction, thermal polymerization method and sol-gel. The phase identification, surface morphology, and electrochemical properties of the powders are investigated by X-ray diffraction, scanning electron microscopy, galvanostatic charge-discharge experiments and electrochemical impedance spectroscopy. The results show that the powders prepared by sol-gel are pure Li4Ti5O12. The powders prepared by solid state reaction and thermal polymerization method are impure with TiO2 phase. The grain size of the powders prepared by sol-gel is about 80 nm, which is much samller than the powders prepared by solid state reaction and thermal polymerization method. The capacities of the Li4Ti5O12 powders prepared by solid state reaction, thermal polymerization method and sol-gel are 161.6mAh/g, 165.9mAh/g and 171.5mAh/g, respectively. Their capacity retentions afer being cycled 25 times for the powders prepared by solid state reaction and thermal polymerization method are 84.7% and 87.7%, which are smaller than that of 94.3% for the powders prepared by sol-gel. The Li4Ti5O12 powders prepared by sol-gel shows the best electrochemical properties.

    • >Review and monographs
    • Research on the application situations of Pickering emulsion in oil field

      2014, 31(1).

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      Abstract:With the continuous development of nanotechnology, Pickering emulsion, with its unique advantages, is widely used in a various fields such as food, cosmetics, medicine and so on. Pickering emulsion has been commonly applied in oil field and this technique is quite mature abroad, but few researches on the oil filed have been conducted in China. This paper first elaborates the mechanism of Pickering emulsion's formation and stabilization, and then discusses the factors that affect Pickering emulsion's stability and rheology. Finally, this paper clarifies current applications of Pickering emulsion in oil fields and forecasts its prospects. The conclusions of this paper can be summarized as following: (1) Due to Pickering emulsion’s unique stability, the demulsification technology will be a significant research direction. (2)The in-depth research on solid nanoparticles emulsifiers which is sensitive to environmental stimulus will better promote the use of Pickering emulsion in oil fields. (3) In order to promote the universal application of Pickering emulsion in oil field, researchers are suggested to focus on the modification of nano-SiO2 and nano-CaCO3.

    • >Functional materials
    • Preparation of Ortho Substituted Perylene Bisimides Derivatives and Electron Transport Study

      2014, 31(1).

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      Abstract:Perylene bisimides derivatives 3 and 4 were synthesized at the 2, 5, 8, 11-positions of the perylene core under Ir-catalysis. The structure of the compounds were characterized by means of 1H NMR,13C NMR and HRMS.Compared to compound 1 a hypsochromic shift in the absorption and emission is observed for the derivatives 3 and 4, the tetrachloro derivative showing a greater shift than the tetrabromo one. Their LUMO values are -4.18 eV and -4.16 eV, which are significant low than compound 1. The thermogravimetric analysis (TGA) indicates that all of them have good thermal stability with decomposition temperatures more than 370℃. Electron mobilities were measured by the method of space charge limited current (SCLC). By introducing the halo atom at the ortho position, their films become ordered and they exhibit good electron mobilities, which is up to 3.05 ?10-4 cm2 V-1 s-1 for compound 3.

    • Synthesis and Properties Double-ended Tridentate Ligand La(Ⅲ) gel Polymer

      2014, 31(1).

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      Abstract:Using nitrogen rich 2,6-bibenzimidazole-4-hydroxypyridine reacted with 1,6-dibromohexane and 1,8-dibromo-octane the double-ended tridentate ligand 1,6-bis-(2,6-bis(benzimidazolyl)pyridyloxy)hexane and 1,8-bis-(2,6-bis(benzimidazolyl)pyridyloxy)octane were synthesized. Temperature and chemical stimuli-responsive La(Ⅲ) polymer gel with distinct luminescence could be obtained through the ligand and metal ions self-assembly. MR spectra indicate successful synthesized the monomer and the ligand, the TG and XRD were applied to test the performance of polymer. Experiments showed that the polymer gels have reversible temperature stimuli-responsive, and chemical stimuli-responsive when added formic acid. Optical performance reach showed, under UV irradiation, the polymer gels have a distinct luminescence, and maximum emission peaks are located at 419 nm.

    • >Fine chemical intermediates
    • Synthesis and characterization of trans-4-(trans-4′-n-propylcyclohexyl)cyclohexyl aldehyde

      2014, 31(1).

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      Abstract:Abstract:More than 98% purity of trans-4-(trans-4′-n-propylcyclohexyl)cyclohexyl aldehyde was obtained via hydrogenation,acidolysis and isomerization reaction with trans-4-(4′- n-propylcyclohexyl)-benzaldehyde propylene glycolacetal as the starting material, the total yield was 39.2%, the structure of the target compound was confirmed by 1HNMR, IR and GC-MS. The hydrogenation reaction conditions of trans-4-(4′-n-propylcyclohexyl)-benzaldehyde propylene glycolacetal were investigated,the results of the condition experiments showed that the reaction effect was best when Ru/C was as the catalyst, ethanol was as the reaction solvent,m[trans-4-(4′- n-propylcyclohexyl)-benzaldehyde propylene glycolacetal]:m(Ru/C) was 1 g : 0.09 g,the hydrogenation pressure was 3.5 MPa,the reaction temperature was 35~40 ℃.

    • Synthesis of 1-bromo-6-cyano-2-naphthol

      2014, 31(1).

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      Abstract:6-Bromo-2-naphthol (4) was prepared from 2-naphthol (2) via a two-step one-pot process in a yield of 89.0%; then 6-cyano-2-naphthol (5) was synthesized from 4 under the feeding ratio of n(CuCN):n(4)=1.5:1 in a yield of 91.2%. In the end, the bromination reagents Br2 and NBS were both adopted to prepare 1-bromo-6-cyano-2-naphthol (1) from 5. In the case of Br2 as bromination reagent, acetic acid as solvent, n(Br2):n(5) = 1:1, the yield is 89.8%;and this process is low-cost and suitable for industrialization. In the case of NBS as bromination reagent, acetonitrile as solvent, n(NBS):n(5)=1.00:1.03, the yield is 99.2%; this method is mild, simple, efficient for laboratory-scale preparation in which the problems of volatilization and high inhalation toxicity of Br2 are avoided.

    • >Catalysis,separation and purification technology
    • Components distribution of cinnamon oil by steam distillation separation

      2014, 31(1).

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      Abstract:The aim of this study was to optimize operating conditions to extract benzaldehyde, cinnamaldehyde, phenylpropyl aldehyde, cinnamyl acetate, and o-methoxy cinnamic aldehyde from cinnamon oil by steam distillation. A single factor experiment was conducted to investigate the influence of three main factors including particle size, temperature, and time on the yield and content of the ingredients. To explore the relationship between factors influencing yield and content of the ingredients, the operating conditions were further optimized using the orthogonal experiment with yield and content of cinnmaldehyde as criteria. The optimized parameters of the extracting processes were as follows: 20 mesh, temperature 168 oC, and time 1.5 h. It gave 2.08% yield and 91.50% content of cinnamaldehyde. The repeated experiments also indicated the same results were obtained with good quality on the base of optimized parameters.

    • >Fine chemical intermediates
    • A Simple and Green Method Preparing Fullerenol

      2014, 31(1).

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      Abstract:In order to solve the problem of the poor solubility of fullerene in water, A method preparing water-soluble fullerenol has been realized based on the fullerene oxides in this paper. In detail, the fullerene oxides were oxidized further and hydrolyzed by H2O2 to form more hydroxyl groups on fullerene cage under 50℃.,synthesized fullerenol successfully.The solubility of fullerenol is 59.8 mg/mL.Charactized and analysed the product.This paper has provided a novel method of preparing fullerenol.

    • >Perfumes and essences
    • Pyrolysis Constituents of Volatile Oil of Trollius Chinensis Bunge by Supercritical CO2 extraction and its Application in Cigarette Flavoring

      2014, 31(1).

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      Abstract:In order to develop a new natural cigarette flavor, Trollius chinensis Bunge was extracted with supercritical CO2 method, then the volatile oil was pyrolyzed under simulated condition of process of smoking. The pyrolytic products were measured and analyzed by Py/GC-MS method and its applications to cigarette flavoring were studied as well. The results showed that: 1) 43, 41 and 37 constituents were identified in the pyrolytic products at 300℃, 600℃, 900℃, respectively. They were mainly aldehydes, alkenes, acids and ketones which have their characteristic flavor. 2)The volatile oil of Trollius chinensis Bunge extracted with supercritical CO2 was characterized by enhancing the aroma quality and volume of smoke, reducing irritancy and improving the aftertaste.

    • >Drug and cosmetic materials
    • Improved synthesis of Cetirizine Hydrochloride

      2014, 31(1).

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      Abstract:This novel is aimed at optimizing and improving the synthesis route of Cetirizine Hydrochloride. The new synthesis route use chlorobenzene and benzoyl chloride as starting materials, through Friedel-crafts reaction, carbonyl reductive reaction, chlorination, nucleophilic substitution, obtained the product. Compared with the original synthesis route, this synthesis route shortened one reaction step, reduced the cost of raw materials, The total yield of Cetirizine Hydrochloride was increased from 20.9% to 24.87%. The structure of product was characterized by IR, 1H NMR and MS.

    • >Surfactants
    • Synthesis of Stearic Acid Triethanolamine Ester over Solid Acid Catalyst Al-SBA-15

      2014, 31(1).

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      Abstract:Al-SBA-15 solid acid catalysts with Si/Al ratio ranging from 15 to 50 were prepared and used for the catalysis of esterification of stearic acid with triethanolamine. The Al-SBA-15 (Si/Al=25) catalyst exhibited high activity and selectivity in the esterification, the acid value of the esteramine were reduced to 1.78 mgKOH/g and content of mono-esteramine and di-esteramine reached 84.79%. The activity of Al-SBA-15 (Si/Al=25) was not obviously changed when the catalyst reused 6 times. The results indicated that the catalyst showed good stability during the esterification reaction. The structure and acidity of the catalysts were characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms (BET), transmission electron microscopy (TEM) and pyridine in situ FTIR. These results showed that Al-SBA-15(Si/Al=25) kept the structure of SBA-15, and had large surface area, uniform channels, and the same time Lewis and Brønst acid sites were presence on the surface of the catalysts.

    • Preparation of poly (ether-ester) modified silicone

      2014, 31(1).

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      Abstract:Poly (ether-ester) modified silicone oil was synthesized by fourteen acid allyl polyether ester and low hydrogen silicone,using H2PtCl6 as catalyst.The chemical structure was characterized by IR.The effects of reaction temperature,time and the molar ratio of reactants on the hydrosilation reaction were investigated. Surface tension of poly (ether-ester)modified silicone solution at different mass concentration was determined. The defoaming performance of the defoamer emulsion was studied.The results showed that:reaction temperature was 85℃,reaction time was 6h,molar ration of n(C=C):n(Si-H) was 1.30:1, the conversion rate of Si-H could reach 87.6%.The defoaming time of the emulsion was 5s,bubble restrain height was 300mL.

    • >Perfumes and essences
    • Synthesis of 4-(4-Acetyl-5-methyl-1H-pyrrol-2-yl)-2′3′4′- trihydroxybutyl Strawberry Acid and its flavoring Application in Unblended Cigarette

      2014, 31(1).

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      Abstract:Abstract: Under alkaline conditions in aqueous solution, 2-methyl -3-acetyl-5-1′, 2′, 3′, 4′-tetrahydroxy butyl pyrrole was obtained by the reaction of D-glucosamine hydrochloride with acetyl acetone at reflux for 8h, then 4-(4-acetyl-5-methyl-1H-pyrrol-2-yl)-2′3′4′-trihydroxybutyl strawberry acid was synthesized by esterification, which was reacted with 2-methyl -3-acetyl-5-1′, 2′, 3′, 4′-tetrahydroxy butyl pyrrole and Strawberry Acid. The structures of all the compounds were confirmed by 1H NMR、13C NMR、IR and HR MS spectra. Then the pyrolysis of the target product was studied at 300, 600, 900°C, respectively, and the application of the products in unblended cigarette flavoring were studied as well. The results showed that variety of characteristic flavor substances were detected at three temperatures. It is proved that when the target was ammount to 0.2% in tobacco, which could play an important role in enhancing the aroma quality and volume of smoke, reducing irritancy and improving the aftertaste.

    • >Drug and cosmetic materials
    • Synthesis of 2,6-Dimethyl-3-aryl-4(1H)-quinolones under Microwave Irradiation

      2014, 31(1).

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      Abstract:A simple and efficient method was developed for the synthesis of 2,6-dimethyl-3-aryl-4(1H)-quinolones via the acylation and cyclization of N-(4-methylphenyl)acetamide with substituted phenylacetic acids under microwave irradiation. The reaction conditions of acylation and cyclization were optimized, and the reaction time was shortened enough. N-(4-Methyl-2-(2-arylacetyl)phenyl)acetamides were synthesized with 85.7%~91.3% yields by the acylation of N-(4-methylphenyl)acetamide and substituted phenylacetic acids using BF3?Et2O as catalyst under the conditions of microwave irradiation, 80 ℃ and 15 min. In the presence of sodium tert-butanolate and tert-butanol, the cyclization of N-(4-methyl-2-(2-arylacetyl)phenyl)acetamides under microwave irradiation and reflux condition were completed within 20 min giving the target compounds 2,6-dimethyl-3-aryl-4(1H)-quinolones in 89.2%~94.3% yields. The structures of the target compounds were identified by IR, 1H NMR spectra and elemental analysis.

    • Synthesis and hydrolysis of propranolol hydrochloride derivatives

      2014, 31(1).

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      Abstract:Propranolol hydrochloride was synthesized from α-naphthol, epoxy chloropropane and isopropylamine via a serial of reactions included etherification, eliminate, ammoniation and salt formation. Then, its two derivatives, O-acetyl propranolol hydrochloride (compound 4) and polyacrylic acid immobilized propranolol hydrochloride (compound 7), were prepared by the reaction of propranolol hydrochloride with acetyl chloride and polypropylene chloride, respectively. Their structures were characterized by melting point, IR, 1H-NMR, and single-crystal X-ray diffraction analysis. The hydrolysis results under acidic conditions indicated that the releasing rate of propranolol hydrochloride in compounds 4 and 7 within 8 h was 15.18% and 17.86%, respectively. Compared with compound 4, the polymeric carrier of compound 7 is not easy to be absorbed by the body and can be expected as prodrug for clinical application.

    • >Leather chemicals
    • Study on the Synthesis of Acrylate Modified Aqueous Polyurethane Emulsion and Film Properties

      2014, 31(1).

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      Abstract:With IPDI, PCDL,DMPA,TEA,MMA and BA as the basic raw materials, hybrid emulsion of waterborne polyurethane-acrylate(WPUA) was prepared by in-situ emulsion copolymerization method in this paper. The effects of PU content, quality ratio of MMA and BA, the n(-NCO)/n(-OH) and the amount of DMPA on the properties of the emulsion and coating film were systematically studied. The results showed that when the PU quality score was 80%, the initial molar ratio of the -NCO and -OH value was 6.0,using DMPA mass fraction at 5%, and the m(MMA):m(BA) at 4:6, the WPUA hybrid emulsion showed a stable performance.Compared with the bibulous rate of 24.75% of the unmodified PU film,the water absorption of the WPUA film was reduced by 60.4%,reaching to 9.80%,and the tensile strength of the modified film increased by 1.53 times of the PU film,reaching to 28.9MPa.All the results show that the stable WPUA emulsion was prepared,and it exhibits superior performance properties in water resistance and physical and mechanical properties.

    • >Water treatment technology and environmental protection
    • Effect of Different Dispersants on Properties of Poly(aspartic acid) Superabsorbent Polymer

      2014, 31(1).

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      Abstract:In the process of synthesis of poly(aspartic acid) superabsorbent polymer, de-ionized water,methanol,ethanol and n-butanol were added into the solution of PSI, respectively, and a homogeneous system was achieved. After that, 1,6-hexamethylene diamine acted as cross-linking agent was added. Finally, biodegradable superabsorbent resin with three-dimensional structure was prepared. For further identification of microstructures of this resin, transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and thermo-gravimetry analyses (TG) had been used. In this paper, by comparing the influence of these four kinds of dispersants on the water absorption performances of PAsp resin, it was concluded as follows: whichever dispersant, when added moderately, could markedly improve the water-swelling ratio of PASP resin, whereby, water was prefer. The PAsp polymer using water as dispersant had a 945 g.g-1 water-swelling ratio in de-ionized water and 94 g.g-1 in a 0.9% sodium chloride solution; While n-butyl alcohol was served as dispersant, there was a higher fluid absorption rate for the PAsp resin, which could reach swelling equilibrium in 7 hours. In addition, when mixed solvent composed of deionized water and n-butanol, the mass ratio of which was 7:3, was used as dispersant, the water absorption performance of resin was superior to pure water and pure butanol. The resin could reach swelling equilibrium in 6 hours, and its water-swelling ratio in deionized water was up to 1004 g.g-1.The absorbent properties for PAsp resin would gradually decrease with the increasing of drying times. After 5 times, the swelling ratio of PAsp could still achieve 400 g.g-1, indicating that the resin had a good repeated bibulous performance.

    • >Rubber and plastics auxiliaries
    • Synthesis and applications of aluminium hypophosphite flame retardant

      2014, 31(1).

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      Abstract:A novel halogen-free flame retardant aluminium hypophosphite (PAH) was synthesized by sodium hypophosphite monohydrate and aluminum sulfate octadecahydrate as base material. The optimal reaction conditions were obtained:The reaction temperature being 90 ℃, the molar ratio of sodium hypophosphite monohydrate to aluminium sulfate octadecahydrate being 7.5:1.0 and the reaction time being 3 h,the yield of aluminium hypophosphite was up to 98.5%.The structure of product was characterized by means of infrared spectrometer and inductively coupled plasma atomic emission spectrometer. The application of PAH to polyurethane foam was investigated.The results show that the flame retardant polyurethane foam has LOI 30 and UL94 V-0.This method was simple, environmental and easy to realize industrialization.

    • New Method for the Synthesis of an UV Absorber

      2014, 31(1).

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      Abstract:New method for the synthesis of UV absorber bis-(1,2,2,6,6-tetramethyl-4- piperidinyl)ester phenyl-(3,5-di-tertbutyl -4-hydroxybenzyl)malonitic acid was developed. Bis-(1,2,2,6,6- pentamethyl-4-piperidinyl)ester phenylmalonic acid was synthesized from diethyl phenylmalonate and N-methyl-2,2,6,6-tetramethyl-4-piperidinol catalyzed by micronano-K2CO3 in toluene, and then it reacted with 4-hydroxy-3,5-di-t-butylbenzyl chloride catalyzed by micronano-K2CO3 in ethanol to give the target product. The influence factors were investigated. The optimized overall yield was 80 %. The target product was characterized by means of 1H NMR and 13C NMR.

    • >Fine chemical intermediates
    • Synthesis and characterization of co-modified silicone oil with long-chain alkyl ester and epoxy ether

      2014, 31(1).

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      Abstract:Co-modified silicone oil with long-chain alkyl ester and epoxy ether (PEESO) was synthesized using hydrosilylation of poly (hydromethyl, dimethyl) siloxane (PHMS) with stearyl methacrylate (SMA), allyl epoxy (poly) ether in the presence of platinum ((trimethyl)cyclopentadienylplatinum) catalyst. The effect of reactive conditions,such as dosage of catalyst, molar ratio of reactants, reaction temperature and time, on the Si-H conversion rate was discussed well. By orthogonal experiment and the corresponding single factor experiments, the preferential experimental conditions were obtained as follows. The amount of catalyst is 0.004% of material mass, the molar ratio of PHMS and alkene compounds 1:1.05, the reaction temperature 72℃, reaction time 3h. The molecular structure of the product was determined by FTIR and 1H-NMR. The experimental results indicated that the chain of long-chain alkyl ester and epoxy (poly) ether is grafted in the chain of polysiloxane.