• Volume 36,Issue 1,2019 Table of Contents
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    • >Review and monographs
    • Research Progress on Supercritical CO2 Microemulsions and Its Application in Textiles

      2019, 36(1):0-0.

      Abstract (1145) HTML (0) PDF 534.08 K (1605) Comment (0) Favorites

      Abstract:The formation principle and evaluation indicators of supercritical CO2 microemulsion were introduced based on the basic properties of supercritical CO2 fluid. The research and development status of fluorine surfactants and hydrocarbon surfactants in supercritical CO2 microemulsion was summarized specially. Moreover, the latest application progress of supercritical CO2 microemulsion system in textile was reviewed, and its application values in the clean processing of textile materials such as pretreatment, dyeing, finishing and fiber modification were obtained. It is indicated that the application of supercritical CO2 microemulsion in the textile, material, chemistry, biology and other fields should be broadened by strengthening the research on the basic theory of supercritical CO2 microemulsion and by establishment supercritical CO2 / ionic liquid microemulsion system.

    • >Functional materials
    • Preparation of Aminated Gelatin Nanoparticles Used to Stabilize Pickering Emulsion

      2019, 36(1).

      Abstract (746) HTML (0) PDF 3.12 M (0) Comment (0) Favorites

      Abstract:Fairly monodispersed aminated gelatin nanoparticles (AGNPs, PDI ≈ 0.068) were prepared by a two-step desolvation method using amino-modified type B as raw material. The particle is positively charged (ζ ≈ 35 mV), with an average size of 240 nm. The effects of pH on the size and dispersity of AGNPs is investigated in the preparation process. It shows that the optimized reaction condition is pH = 4, which can endow the AGNPs with a smaller particle size (≈ 240 nm) and uniform distribution. The results from atomic force microscopy (AFM), scanning electron microscope (SEM) and transmission electron microscopy (TEM) showed that the AGNPs exhibited spherical morphology with a narrow particle size distribution. And compared with gelatin nanoparticles (GNPs), the rigid structure and homogeneity of AGNPs is enhanced. Moreover, the higher three-phase contact angle of AGNPs (θow = 67° ± 5°) than that of GNPs (θow = 31° ± 6°), as evaluated by surface wettability analysis, indicates the increased surface hydrophobicity and capability for the stabilization of O/W Pickering emulsion. Pickering emulsion stabilized by AGNPs can store at 4 ℃ for 9 months without stratification, possessing good storage stability.

    • Constrution and Properties of Fluorosilicone Anti-fingerprint Transparent Coating

      2019, 36(1).

      Abstract (973) HTML (0) PDF 1.24 M (0) Comment (0) Favorites

      Abstract:Abstract: The trifluoropropyl vinyl silicone oil (FVSA) was prepared by ring-opening reaction from 1,3,5-tris(3,3,3-trifluoropropyl)methylcyclotrisiloxane(D3F), tetramethylcyclotetrasiloxane (D4vi) and hexamethyldisiloxane(MM). Alkoxy modified fluorinated polysiloxane (FVT) was prepared by hydrosilylation addition with trimethoxysilane (TMS) and (FVSA).The nano-modified fluorosilicone resin (FVT-SiO2) was obtained via fractional hydrolysis and polycondensation with FVT, tetraethyl orthosilicate (TEOS) and 1H,1H,2H,2H-perfluorooctyltrimethoxysilane (POTS). The transparent anti-fingerprint coating was prepared with FVT-SiO2 as a film forming material. The structure, morphology and performance of the products were characterized by FTIR, AFM and SEM, and the influence of reaction conditions of fractional hydrolysis on the contact angle of coating was discussed. The results showed that: after FVT and TEOS were reacted in 2h, the POTS was added to the further fractional reactions, and the spherical FVT-SiO2 were obtained which dispersed homogeneously with diameter approximately 150nm. Moreover, when the mass concentration of treating solution of FVT-SiO2 was 2wt% and the number of layers was 3, the coating showed optimal transparency, adhesion , hydrophobicity and oleophobicity. The water and oil contact angles reached 138.5°and 109°, respectively.

    • Modification of Waterborne Polyurethane by p-Hydroxybenzoic Acid-Oligochitosan

      2019, 36(1).

      Abstract (698) HTML (0) PDF 919.52 K (0) Comment (0) Favorites

      Abstract:p-Hydroxybenzoic acid grafted oligochitosan (p-HBzA-g-OCS) was obtained by the graft copolymerization of p-hydroxybenzoic acid (p-HBzA) and oligochitosan (OCS). The waterborne polyurethane modified by p-HBzA-g-OCS (HOCS-WPU) was prepared reacting p-HBzA-g-OCS as a crosslinker with polyurethane prepolymer (PPU). The structure of samples was confirmed by FTIR and UV-Vis, its properties were analyzed by DLS, mechanical properties, XRD, TGA and radical scavenging assay of ABTS and DPPH. The results showed that a smaller particle size of HOCS-WPU emulsion was 57.85 nm. Compared to the unmodified WPU, the tensile strength of the film increased from 14.03 MPa to 16.85 MPa, the crystallinity of the polyurethane declined from 3.57% to 3.45%, and the initial decomposition temperature increased from 204.6 ℃ to 216.7 ℃ when 2% of p-HBzA-g-OCS (based on the total mass of the synthetic PPU starting materials) was added. The free radical scavenging assay results showed that ABTS and DPPH radical scavenging assay of HOCS-WPU reached 62% and 35% when the mass concentration of the polymer was 2.5 g/L. The antioxidant activity of HOCS-WPU was significantly better than that of the unmodified WPU.

    • Performance and Construct of UV Blocking Superhydrophobic Fabric Coating

      2019, 36(1).

      Abstract (786) HTML (0) PDF 830.77 K (0) Comment (0) Favorites

      Abstract:Polyurethanes with double bonds were prepared by hydroxy fluorosilicone oil, Pentaerythritol triacrylate(PETA) as a raw material. The ultraviolet absorbers(UVA400) and nanosilica particles were added to the finishing solution to improve the UV protection and surface roughness of the coating. The ultraviolet(UV) blocking and superhydrophobicity fabric coating was fabricated by UV light initiate double bond radical polymerization. FTIR and SEM analysis show that fluorosilanes and PETA are introduced into the polyurethane molecular chain. The surface of the fabric has micro-nano-shaped projections, and the rough surface coating was constructed. Hydrophobic and UV protective tests of coated fabrics show that the coated fabric with excellent superhydrophobicity and UV protection performance when w(silicon dioxide)=15.0% and w(UVA400)=1.5%, the coated fabric has a water contact angle of 154°, roll angle of 9°, ultraviolet protection factor(UPF) value of 72, and transmittance of ultraviolet A(UV-A)band was 2.96%. And the coated fabric after accelerated aging test 120h, the contact angles was 155°, the UPF values was 117, the transmittance of the UV-A band was 2.68%, respectively, and with excellent durability.

    • Synthesis of HPCS-AM-DAC and its Flocculating Properties

      2019, 36(1):0-0.

      Abstract (719) HTML (0) PDF 1.94 M (0) Comment (0) Favorites

      Abstract:In this paper,hydroxypropyl chitosan(HPCS),acrylamide(AM) and acryloyloxyethyltrimethylammonium chloride (DAC) were used as raw materials to synthesize the HPCS-AM-DAC. The structures and morphologies of the compounds were characterized by FTIR, 1HNMR, XRD and SEM. The influences of reaction temperature, Ammonium nitrate dosage, monomer dropping time and DAC dosage on cationic degree and intrinsic viscosity were investigated.The results showed that under the conditions of H2O 25 mL, AM dosage 2 g, HPCS dosage 1 g, reaction temperature 70℃, initiator dosage 1.7% (based on the mass of HPCS, the same below), dropping time of monomers 35 min, and DAC dosage 3.5 g, both cationic degree and intrinsic viscosity of the product reached a good value of 63.01% and 468.81 mL/g. The flocculation experiments of kaolin simulated wastewater were carried out with CTS, homemade HPCS, HPCS-AM-DAC and commercial cationic polyacrylamide (CPAM). The effect of flocculation system pH and flocculation dosage on the removal rate of turbidity was investigated.In kaolin simulated wastewater with a turbidity of 200 NTU, the results showed that the suitable pH range for flocculation of HPCS-AM-DAC was 2~6, and the dosage range was 2mg/L~5mg/L.Under these conditions, the turbidity removal rate is above 96%. Based on the zeta potential, floe particle size and flocculation XPS analysis, the flocculation mechanism of HPCS-AM-DAC on simulated kaolin wastewater is the synergistic effect of electrical neutralization and adsorption and bridging.

    • Grind-strengthened solvent-free synthesis of sucrose fatty acid esters

      2019, 36(1):0-0.

      Abstract (880) HTML (0) PDF 599.06 K (0) Comment (0) Favorites

      Abstract:A grind-strengthened strategy was developed for the solvent-free synthesis of sucrose fatty acid esters (SE). The effect of grinding time, emulsifier, reaction time, reaction pressure and catalyst dosage on yields and production distributions of SE were investigated by using sucrose and fatty acid methyl ester as reactants. The generated SE was purified by using water washing and alcohol extraction. And they were characterized by the analysis of Fourier Transform Infrared Spectroscopy (FTIR) and High Performance Liquid Chromatography-Evaporative Light Scattering Detector (HPLC-ELSD). The results showed that the grinding pretreatment could reduce the particle size of reaction dispersion (D50) to 5 μm and effectively enhanced the solvent-free transesterification reaction of sucrose esters. Under the optimized conditions a fatty acid methyl ester conversion of 91.2% and a SE yield of 61.6% were achieved, in which the grinding time was 60 min, the dosage of potassium stearate was 10%, the dosage of potassium carbonate was 2.0%, the reaction was conducted under the pressure of 0.5 kPa for 6 h. The amount of SE reached up to 81.9% in the purified product, and its free sugar was 0.6%, acid value was 3.0 mg KOH/g, water content was 0.2%, ash content was 0.5%, and all these indicators completely accorded with the Food and Agriculture Organization / World Health Organization (FAO/WHO) standard.

    • Preparation and Properties of Tung Oil - based Photoinitiator

      2019, 36(1):0-0.

      Abstract (902) HTML (0) PDF 741.03 K (1484) Comment (0) Favorites

      Abstract:Tung oil anhydrides(TOM1∽TOM3)and tung acid anhydrides were synthesized via the Diels-Alder reaction of tung oil、tung acid with maleic anhydride (MA).Under the catalysis of triethylamine, TOM and TAM molecules were reacted with the hydroxyl groups of Irgacure2959 to produce four photo-cleavage photoinitiators (TOMG1∽TOMG3, TAMG).The structure of initiator was characterized by FT-IR and 1H NMR spectroscopy. The Photo bleach of prepared photoinitiator was analyzed by UV visible spectroscopy. The photopolymerization dynamics of 1, 6-hexanediol diacrylate initiated by prepared photoinitiator or Ingancure2959 were studied by real-time FT-IR technology. The results show that TOMG3 has the best photo initiated performance with respect to Irgacure2959 and the synthesized tung oil-based photoinitiators. The UV curing gum of HDDA,、PUA and TOMG3 in a mass ratio of 46: 46: 8 (effective photoinitiator group content 2.14 wt%) were cured under irradiation of 28mW/cm2UV lamps in 60 seconds with gel rate of 96%. The hardness and flexibility of curing film was 6H and 5mm, respectively. The adhesion to the glass was zero level.

    • Fabrication of UiO-66 Membranes for the Separation of n-butane/i-butane

      2019, 36(1):0-0.

      Abstract (1239) HTML (0) PDF 6.39 M (546) Comment (0) Favorites

      Abstract:Continuous UiO-66 membrane was fabricated on alumina support by pre-coating ZrO2 layer and seeding secondary growth. The structure and morphology of membrane were characterized by XRD and SEM. The membrane integrity was examined by testing the permeance of gas under T=298 K and P=0.08 MPa. The effects of operating pressure and operating temperature on the permeation selectivity of UiO-66 membranes were investigated. As a result, pre-coating ZrO2 layer helped to obtain a continuous uniform UiO-66 membrane of about 5 μm in thickness. Reverse permeation properties were found of i-C4H10 and n-C4H10 on UiO-66 membrane. At 25 ?C and 0.08 MPa, the permeation selectivity of the membrane for i-C4H10/n-C4H10 were 3.60, with the corresponding permeance of 4.39?10-7 mol/(m2?s?Pa) and 1.22?10-7 mol/(m2?s?Pa).

    • >Surfactants
    • Synthesis and Application Properties of Gemini Cationic Surfactant With Diamide Groups

      2019, 36(1).

      Abstract (671) HTML (0) PDF 820.30 K (0) Comment (0) Favorites

      Abstract:A Gemini cationic surfactant with diamide groups (ADQ-12) was synthesized using Lauric acid, N, N-dimethyl-1, 3-propanediamine and 1, 3-dichloro-2-propanol as raw materials under the action of sodium carbonate. Product was characterized by FTIR and 1HNMR, the surface/ interfacial activities and application performance were researched. The results showed that ADQ-12 has critical micelle concentration(CMC value is 1.41×10-4 mol/L) that are 1~2 orders of magnitude lower than conventional single cationic surfactants and γCMC is 32.26 mN/m; When the surfactant concentration is 0.05 g/L, the interfacial tension of kerosene/water(IFT) could be reduced to ultra-low level (4.1×10-3 mN/m), which is much lower than 2 mN/m of hexadecyl trimethyl ammonium bromide(CTAB); ADQ-12 showed strong resistance to calcium and magnesium ions(>60 g/L) in the case of concentration of 1.0 g/L; The antibacterial rate of ADQ-12 against on S. aureus and E. coli was still 100% when surfactant concentration is 10 mg/L, which is greater efficacy than didecyl dimethyl ammonium chloride(DDAC); The biodegradation of ADQ-12 after 7 days was higher than 99% and showed the excellent biodegradability.

    • >Biological engineering
    • CoMFA, CoMSIA and HQSAR studies of HEPT as HIV-1 Reverse Transcriptase Inhibitors

      2019, 36(1).

      Abstract (637) HTML (0) PDF 751.18 K (0) Comment (0) Favorites

      Abstract:Comparative Molecular Field Analysis ( CoMFA), Comparative Molecular Similarity Indices Analysis (CoMSIA) and the hologram quantitative structure-activity relationship (HQSAR) for 1-[(2-hydroxyethyloxy)methyl]-6-phenylthio thymidine (HEPT) derivatives were used to have molecular active conformation selection,molecular alignment,as well as the establishment of corresponding 3D-QSAR model. The model established by this method has a good ability to predict these compounds. The cross-validated q2 value of CoMFA model is 0.565 and the non-cross-validated r2 value is 0.892. The best q2 value of CoMSIA Model is 0.636 and r2 value is 0.953. The most effective HQSAR model was obtained that the q2 value of 0.876, the r2 value of 0.929, and the best hologram length value is 97. Seven highly active HEPT compounds were designed based on the three-dimensional Contour maps and the HQSAR color code map, Observations derived from these QSAR modeling study may be provided a theoretical reference for designing more active HEPT derivatives.

    • Purification, Structure and Properties of Polysaccharides from Lumpfish Cartilage

      2019, 36(1).

      Abstract (664) HTML (0) PDF 1.04 M (0) Comment (0) Favorites

      Abstract:In this study, lumpfish cartilage as raw material,The polysacccaride of Lumpfish cartilage was extracted by water extraction, and Sevag method was used to deproteinization. The purification of polysaccharide was carried by DEAE-52 cellulose and Sephadex G-75,after dialyzed and freezed,three component polysaccharides were obtained, the three polysaccharides composition were analyzed. Full-wavelength UV was used to scan, the heparin titer of the three polysaccharides was measured by the azure A colorimetric method. The structural of FCPS-3 was analysized by infrared and nuclear magnetic resonance, the FCPS-3 molecular weight was determined by GPC. The results showed that the polysaccharide content of all three components exceeded 90%, the protein content was less than 3%, and the uronic acid content exceeded 60%.The full-wavelength UV scanning of the three polysaccharides showed that the three polysaccharides had no characteristic absorption peaks at 260 nm and 280 nm, indicating that none protein and nucleic acids were contained in three polysaccharides.The heparin titer of FCPS-3 was the highest, 1.365 U/mg, and FCPS-1 and FCPS-2 were low. Characteristic showed FCPS-3 was acid polysaccharides and contained sulfate as β-glucopyranose. the FCPS-3 Mw was 175700 Da, the Z average molecular weight was 253032 Da, and the Mn was 121885 Da.When the concentration was 5 mg/ml, DPPH•, ABTS•, OH• free radical scavenging activity of the FCPS-3 was 78.63%, 96.26%, 93.15% , respectively.

    • The Application of Corn Gluten Meal hydrolysate in Xanthan Fermentation

      2019, 36(1).

      Abstract (648) HTML (0) PDF 691.72 K (0) Comment (0) Favorites

      Abstract:To apply enzymatic hydrolysate of corn gluten meal (CGM) as nitrogen source to xanthan fermentation, we discussed the effect of protease type, enzymatic hydrolysate dosage and enzyme dosage on productive rate and viscosity of xanthan. Then, the optimal nitrogen source combined with CGM hydrolysate and the ratio of CGM hydrolysate to soybean protein were optimized by single factor experiment. The results indicated that alkaline protease pretreatment had a better effect on the following xanthan fermentation than other proteases. Productive rate and viscosity of xanthan were 24.4g/kg and 4235cp when CGM dosage was 6% and enzyme dosage was 8kU. The single factor experiments showed that soybean protein combined with CGM hydrolysate as nitrogen source was better than other proteins. Furthermore, the optimal ratio of CGM hydrolysate to soybean protein was 4:6. Under above conditions, productive rate and viscosity of xanthan could reach 32.4g/kg and 5833cp, which were consistent with the value of soybean protein as the sole nitrogen source. This study provides a new idea for the reuse of corn gluten meal and a possible low-cost approach for xanthan fermentation.

    • >Catalysis,separation and purification technology
    • MIL-100 (Fe) Catalyzed Self-Condensation of n-Valeraldehyde

      2019, 36(1).

      Abstract (829) HTML (0) PDF 1.43 M (0) Comment (0) Favorites

      Abstract:Abstract: Metal-organic frameworks MIL-100(Fe) catalyst was prepared by hydrothermal method using ferric nitrate and benzene tricarboxylic acid as raw materials. Its structure was characterized by XRD, SEM and BET. The catalytic performance of MIL-100(Fe) for n-valeraldehyde self-condensation to 2-propyl-2-heptenal was evaluated. The components existing in the reaction system were identified by GC-MS analysis. The effect of reaction conditions on 2-propyl-2-heptenal synthesis was investigated and the suitable reaction conditions were determined as follows: a weight percentage of MIL-100(Fe)=15% (benchmarked against the quality of n-valeraldehyde, the following is the same), reaction temperature of 130 ℃, and reaction time of 8 h. Under the above conditions, the conversion of n-valeraldehyde was 73.5%, and the yield and selectivity of 2-propyl-2-heptenal were 63.2% and 86.0%, respectively. The MIL-100(Fe) catalyst could be reused for four times without a significant loss in its catalytic activity. XRD, FTIR analysis showed that the catalyst structure did not collapse. Lastly a possible reaction network of n-valeraldehyde self-condensation catalyzed by MIL-100(Fe) was established based on speculation of the side-reactions.

    • Synthesis of polycarbonate diol catalyzed rare earth metal-organic framework Yb-BTC

      2019, 36(1).

      Abstract (869) HTML (0) PDF 1.02 M (1) Comment (0) Favorites

      Abstract:A rare earth metal-organic framework Yb-BTC was prepared from Yb(NO3)3•5H2O and 1,3,5-benzenetricarboxylic acid (H3BTC) by the solvothermal method and characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), N2 absorption-desorption isotherm (BET) and Fourier transform infrared spectroscopy (FTIR). The results showed that Yb-BTC was a typical microporous material with specific surface area of 560 m2/g and pore size of 1.84 nm, and Yb-BTC had uniform particle size, its size was about 2 μm. The activity of Yb-BTC for preparation of polycarnonate diol (PCDL) via the transesterification between diphenyl carbonate (DPC) and 1,5-pentanediol (PDO) was investigated, and was compared with those of catalysts reported such as triethylamine, zinc acetate, tetra-n-butyl titanate and titanium oxide bis(2,4-pentanedionate). The results exhibited that the catalytic activity of Yb-BTC was equivalent to that of titanium catalyst. When the molar ratio of PDO to DPC was 1.2, the amount of Yb-BTC was 0.05% ( the amount accounting for mass percent of DPC), the time of atmospheric transesterification at 180~185 ℃ was 2 h, the time of vacuum polycondensation at 160 ℃ was 4 h, and PCDL with the number-average relative molecular mass of 2300 g/mol and the hydroxyl value of 49.3 mg KOH/g were obtained.

    • Effect of Mn Content on 1-Methoxy-2-propanol Dehydrogenation over Cu-Mn-Al Catalysts

      2019, 36(1):0-0.

      Abstract (789) HTML (0) PDF 841.12 K (322) Comment (0) Favorites

      Abstract:A series of Cu-Mn-Al catalysts with different Mn content were synthesized by co-precipitation method using Cu(NO3)2, Mn(NO3)2, Al(NO3)3 and Na2CO3 as raw material. The samples were characterized by BET, XRD, SEM, TEM, H2-TPR and NH3-TPD. The catalytic activity was tested by 1-methoxy-2-propanol dehydrogenation to methoxyacetone in a fixed bed reactor. The results showed that Mn content had great effect on the pyhsico-chemical properties of Cu-Mn-Al catalysts. The addition of appropriate Mn promoted the dispersion of Cu, changed the reducibility and reduced surface acidity. When n(Cu):n(Mn):n(Al)=2.0:3.5:1.0, the surface acidity of Cu-Mn-Al catalyst was the lowest and Cu-Mn-Al catalyst had lower reduction temperature. Under the reaction conditions of reaction temperature 260 ℃, reaction pressure 1atm, 1-methoxy-2-propanol feed with 5% mass fractions of water and liquid hourly space velocity 2.5 h-1, the conversion of 1-methoxy-2-propanol was 61.57%, the selectivity of methoxyacetone was 96.83%, and the selectivity of main byproduct acetone was 1.20%.

    • >Drug and cosmetic materials
    • Synthesis and Antitumor Activity of Pinanyl Thiazole?Hydrazone Derivatives

      2019, 36(1).

      Abstract (846) HTML (0) PDF 1.95 M (0) Comment (0) Favorites

      Abstract:Pinanyl thiazole hydrazone derivatives 4a~n were synthesized from nopinone via addition, condensation and cyclization, and their structures were characterized by FTIR, 1HNMR, 13CNMR and HRMS. The antitumor activities of compounds 4a~n against four human cancer cell lines including HepG2, RPMI-8226, A549 and MDA-MB-231 were evaluated in vitro. The test results showed that compounds 4a had best antitumor activity against the above four cancer cell, IC50 values for HepG2, RPMI-8226, A549 and MDA-MB-231 as low as 5.8, 8.8, 7.1 and 10.6 μmol/L, respectively; compound 4c also had stronger activity and the IC50 values was 8.9, 8.7, 7.3 and 9.7 μmol/L, respectively. Cell apoptosis and cell cycle experiments results indicated that as the concentrations of compound 4a increased from 0 to 40 μmol/L, the total apoptotic rate of A549 cells increased from 6.5% to 47.2%, and the number of cells in G2/M phase increased from 13.5% to 51.7%. The above results indicated that compound 4a effectively fuelled A549 cells apoptosis in a dose-dependent manner and arrested the cell cycle at the G2/M phase.

    • Synthesis and Antibacterial Activities of Sulfonamides Derivatives Bearing 1, 2, 3-Triazole Moiety

      2019, 36(1):0-0.

      Abstract (874) HTML (0) PDF 425.54 K (951) Comment (0) Favorites

      Abstract:The Intermediate 2-chloro-N-(4-sulfamoylphenyl)acetamide(II) was obtained by the reaction of sulfanilamide and chloroacetyl chloride. Ten 1, 2, 3-triazolyl sulfonamides were prepared using a known one-pot procedure starting from (II), sodium azide and terminal alkynes. The target compounds were characterized by FTIR, 1H NMR, 13C NMR and ESI-MS. The minimal inhibitory concentrations (MIC) of target compounds against S.aureus and E.coli were determined with double broth dilution method. The results showed that all the tested compounds exhibited a certain antibacterial activities. In particular, 2-(4-(3-fluorophenyl)-1H-1, 2, 3-triazol-1- yl)-N-(4- sulfamoylphenyl)acetamide (IIIh) possessed similar activity against E.coli compared with the positive control drug (ciprofloxacin 0.25 μg/mL).

    • >Food and feedstuff chemicals
    • Preparation and stability of calcium iodate/sodium alginate microspheres for feeds

      2019, 36(1).

      Abstract (1739) HTML (0) PDF 1.10 M (0) Comment (0) Favorites

      Abstract:To avoid the reaction of calcium iodate with reducing substances such as vitamin c (VC) during storage and use in feeds. The microspheres of calcium iodate (Ca(IO3)2/SAMS) were prepared by improved emulsification/internal gelation with calcium iodate as core material, sodium alginate as wall material and Nano-calcium carbonate as cross linker. The Ca(IO3)2/SAMS were characterized by FTIR, SEM, TG and XRD, stability of VC solution of Ca(IO3)2/SAMS were also systematically measured. The embedding mechanism of Ca(IO3)2/SAMS were proposed according to various analysis results. The results showed that Ca(IO3)2/SAMS were spherical with a particle size of about 20-40 μm and a large number of calcium iodate were in crystalline form on the surface of Ca(IO3)2/SAMS. The half decomposition rate time (t50%) of vitamin C was 54.8 min and 78.3 min by the calcium iodate or Ca(IO3)2/SAMS, respectively. It were demonstrated that the stability of Ca(IO3)2 in feeds were improved significantly.

    • >Electro-organic chemistry and industry
    • Study on Stabilization of Alkaline Ionic Liquids in Anion-Conducting Membranes Reinforced by Nano-TiO2

      2019, 36(1).

      Abstract (575) HTML (0) PDF 953.40 K (0) Comment (0) Favorites

      Abstract:A new pyrrolidonium ionic liquid ([DMPy]OH) was synthesized with 1-Methylpyrrolidine via two-step procedure. Additionally, [DMPy]OH and nano-TiO2 were introduced into the polyvinyl alcohol (PVA) as matrix by physical doping, and then glutaraldehyde (GA) was used to cross-link PVA to obtain PVA-[ DMPy] [OH]-TiO2 composite membrane. The self-assembly effect of non-coordinating Ti4+, O2- on the surface of Nano-TiO2 and anion-cation in [DMPy]OH, and the semi-interpenetrating structure formed by GA cross-linked PVA can reduce the loss rate of ionic liquid in the membrane and increase the number of \"cationic active site\", speed up OH- migration rate, increase anionic conductivity. The existence of self-assembly between Nano-TiO2 and [DMPy]OH was confirmed by X-ray diffraction (XRD) and Mapping. The mechanical properties, thermal stability, conductivity, alkali resistance, and other properties of the composite membrane were also tested. The result indicates that PVA-[DMPy]OH]-TiO2 composite membrane has uniform morphology, the introduction of Nano-TiO2 can reduce the loss rate of IL, enhance the conductivity and mechanical properties. The experiment results show that when the [DMPy]OH mass fraction were 25wt% and Nano-TiO2 were 1wt%, the conductivity is 2.78×10-3 S.cm-1 at 80℃, the ionic liquid loss rate is 23.2% at room temperature, conductivity was 19.4% higher than that without Nana-TiO2 addition, and the loss rate of ionic liquid was also greatly decreased (about 34.3%). No obvious variety in conductivity is observed for the composite membrane after immersing in 3M KOH solution at room temperature, show that membrane has excellent alkali stability. TGA shows that membrane has good thermal stability; the initiate decomposition temperature is higher than 200oC.

    • >Leather chemicals
    • Synthesis and Tanning Properties of N, N'-bis- (4,6-dichloro -[1,3,5]- triazin-2-yl) -2,6-diaminohexanic acid

      2019, 36(1).

      Abstract (566) HTML (0) PDF 690.51 K (1) Comment (0) Favorites

      Abstract:N,N'-bis-(4,6-dichloro-[1,3,5]-triazin-2-yl)-2,6-diaminohexanic acid(DTDHA for short) have been synthesized by reacting cyanuric chloride(TCT) with lysine under water-mediated conditions. The orthogonal test was carried out on the three factors of molar ratio of reaction raw material, type of acid-binding agent and reaction time, and the suitable reaction conditions were raw material molar ratio n (cyanuric chloride): n (lysine) = 3: 1, KOH as acid binding agent, the reaction time 6h, the yield was 91%. The product was applied to the tanning of raw hides. The shrinkage temperature of the tanning leather was used as the inspection index. The single factor test method was used to optimize the technical conditions of the tanning process. The results showed that the optimum tanning process conditions were as follows: tanning agent dosage 20%, temperature rising from 25°C, stepwise control rising by 15°C every 2 hours, finally reaching to 55°C, total tanning for 8 hours, Under these conditions, the shrinkage temperature of the crust leather is 85.6℃. The synthetic product has a good tanning effect and belongs to a new type of organic synthesis tanning agent.

    • >Water treatment technology and environmental protection
    • Photoelectrocatalytic Performance of Polyaniline Modified Activated Carbon Particle Electrode

      2019, 36(1).

      Abstract (769) HTML (0) PDF 10.02 M (0) Comment (0) Favorites

      Abstract:Polyaniline (PANI) modified activated carbon (AC) particle electrode was prepared by in-situ polymerization method. The morphology and crystal structure of the particle electrode were studied by metalloscope, X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). And the composition was analyzed and applied to the photocatalytic degradation experiment of FBL; the factors such as compound amount, particle electrode dosage, current density, pH and initial concentration were examined for the degradation of FBL influences and studies on photocatalytic degradation kinetics of FBL. The results show that photocatalysis and electrocatalysis produce a synergistic effect; when the concentration of electrolyte Na2SO4 solution is 0.03mol?L-1, the particle electrode dosage is 9 g?L-1, the current density is 8 mA?cm-2, and the pH is 3, the removal rate of FBL with a concentration of 20 mg?L-1 reached 95.47%.

    • Scale Inhibition Performance of Chitosan Derivatives for Municipal Wastewater

      2019, 36(1).

      Abstract (549) HTML (0) PDF 928.74 K (0) Comment (0) Favorites

      Abstract:A new chitosan copolymer (CEC) was successfully synthesized by chitosan (CTS) and acrylic acid (AA) as monomer and ammonium persulfate (APS) as initiator, which copolymerization under 2% (volume fraction) glacial acetic acid solutions. The chitosan derivative was characterized by FTIR, 1H NMR. According to scale inhibition performance, the optimal synthesis conditions of CEC were selected by single factor tests, which were as follows: the mass ratio of AA: CTS was 5.30: 3.00, the reaction temperature was 75 ℃, the reaction time was 4 h and the APS mass fraction was 3%. The scale inhibition performance in secondary municipal wastewater treatment of CEC was studied and the results presented that CEC exhibited excellent inhibition performance to CaCO3 and the scale inhibition rate could reach 92.93% in the presence of 30 mg/L of CEC, which was significantly better than comercial scale inhibitor 1-hydroxy ethylidene-1,1-diphosphonic acid (HEDP). The resistance mechanism to CaCO3 was investigated by SEM and XRD, and it could be noted that the mechanism of CEC on CaCO3 was mainly lattice distortion.

    • >Rubber and plastics auxiliaries
    • Synthesis and Application of Plasticizer Dibutoxyethyl Terephthalate

      2019, 36(1):0-0.

      Abstract (1514) HTML (0) PDF 551.48 K (1683) Comment (0) Favorites

      Abstract:In this work, a plasticizer with ether bond named di (2-butoxy ethanol) terephthalate (DBETP) was synthesized by one-step transesterification using dimethyl terephthalate (DMT) and 2-butoxyethanol (EB) as raw materials. The optimum process conditions obtained by orthogonal experiment were shown in the follow: n(EB): n(DMT) = 6:1, the amount of catalyst CaO was 4.0% (based on DMT quality, the same below), reaction time was 3.0h and temperature was 140℃.The yield of the product reached 91.5%, and the structure was analyzed by FT-IR and 1H NMR spectrums. DBETP was used in the thermoplastic polyvinyl chloride (PVC), and then compared with diiooctyl terephthalate (DOTP) plasticized PVC. The performance results showed that PVC-DBETP is similar to PVC-DOTP in terms of thermal stability and pull-out resistance, but PVC-DBETP has lower glass transition temperature Tg and better tensile property, indicating that our DBETP can be used as a substitute for DOTP.

    • >Papermaking chemicals
    • Preparation and Properties of Soy Isolate Protein Based Surface Sizing Agents for Papermaking

      2019, 36(1):0-0.

      Abstract (954) HTML (0) PDF 784.25 K (2162) Comment (0) Favorites

      Abstract:Using soy isolate protein (SPI) as raw material and alkenyl succinic anhydride (ASA) as hydrophobic modifier, four kinds of hydrophobic soy isolate protein (ASAn-SPI, the subscript n represented the molar rate of ASA to primary amino group of SPI, n=0.5, 1, 1.5 and 2) with different acylation degree were prepared through controlling the molar rate of ASA to primary amino group of SPI. The structures and properties of ASAn-SPI were characterized by means of primary amino content, FT-IR, UV-vis, fluorescence spectrum and hydrophobic index. The results indicated that long hydrophobic chain was successfully introduced into the SPI molecular framework, the acylation degree and hydrophobic index of ASAn-SPI increased with n and tended to be stable when n exceeded 1.5. Subsequently, ASA1.5-SPI was used in surface sizing of paper and the sizing amount was 0.77 g/m2. It was found that the initial water contact angle of ASA1.5-SPI sized paper was 132?, the retention time of water drop was 53 min. XPS and SEM analysis revealed that ASA1.5-SPI formed a rough hydrophobic layer on paper fiber surface. In addition, mechanical property tests indicated that the tensile strength of ASA1.5-SPI sized paper was increased from 0.6 kN/m to 0.67 kN/m compared with that of base paper.

    • >Fine chemical intermediates
    • Synthetic process optimization of RDEA3170

      2019, 36(1):0-0.

      Abstract (1045) HTML (0) PDF 406.89 K (1879) Comment (0) Favorites

      Abstract:4-bromo-1-naphthonitrile was obtained by a new route of bromo-magnesium exchanging reaction, synthesis and dehydration of 4-bromo-1-naphthamide using 1,4-dibromonaphthalene as starting materials. The Miyaura borylation of 4-bromine-1- naphthonitrile and its Suzuki coupling with ethyl 2-(3-bromopyridine-4-yl)thio-2-methylpropionate were realized using Pd(PPh3)2Cl2 as catalyst by a continuous reaction method. The conditions for coupling reaction and the hydrolysis of the product to produce RDEA3170 were optimized. The overall yield of RDEA3170 is 42% and the optimized synthetic process is suitable for the industrial production.

    • Catalytic Properties of Ce Exchanged Tungstosilicic Acid on the Esterification to Glycerol Monolaurate

      2019, 36(1):0-0.

      Abstract (704) HTML (0) PDF 677.21 K (1267) Comment (0) Favorites

      Abstract:A series of rare earth modified tungstosilicic acid catalysts MxH4–3xSiW12O40 (M = La, Ce, Pr, Nd, Sm; x = 1/3, 2/3, 1, 4/3) were prepared by ion exchange method. The structure, stability and acidity of the catalysts (CexH4–3xSiW12O40 ) were characterized by different analytical and spectroscopic techniques such as FT-IR, XRD, TGA-DTG and 31P MAS-NMR, and their catalytic properties were investigated on the esterification of lauric acid (LA) and glycerol (GL) to glycerol monolaurate (GML). Results showed that Ce1/3H3.0SiW12O40 catalyst had the best catalytic activity in the synthesis of GML. The rare earth metal cation (Ce) had been effectively combined to tungstosilicic acid, and the catalysts maintained the complete Keggin structure. Compared with tungstosilicic acid, the acidity of CexH4–3xSiW12O40 catalysts decreased, but the catalysts had good catalytic performance during the esterification for strong Brønsted acidity and Brønsted-Lewis acid synergy. The Ce1/3H3.0SiW12O40 was utilized to optimize the reaction conditions with 78.4% GML yield under GL/LA molar ratio of 4.0, catalyst amount (relative to LA mass) 4%, reaction temperature 423 K and reaction time 120 min. Kinetic studies revealed that the Ce1/3H3.0SiW12O40 for synthesis of GML with an apparent activation energy of 42.37 kJ/mol. The GML yield decreased to 71.4% after five consecutive, the catalyst still had superior reusability in the reaction system.

    • Palladium catalyzed hydramamine carbonylation of 2,5-Dihydrofuran

      2019, 36(1):0-0.

      Abstract (804) HTML (0) PDF 362.72 K (1020) Comment (0) Favorites

      Abstract:Tetrahydrofuran-3-formic acid and its derivatives, tetrahydrofuran-3-formamide and tetrahydrofuran-3-methonitrile are not only an important intermediate in pesticides and pharmaceuticals, such as palladium chloride as the catalyst, three phenyl phosphine as the ligand, p-toluene sulfonic acid as the promoter, and the hydramine carbonyl of aromatic amine and carbon monoxide through 2,5-dihytrofuran. A series of tetrahydrofuran -3- formamide compounds were synthesized by chemical reaction. The products were characterized by IR, 1HNMR, 13CNMR and HRMS. The adaptability of different aromatic amine substrates was investigated. When the substituents of aniline were alkyl, halogen, methoxy and nitro, the -3- formamide derivatives of tetrahydrofuran were obtained, and the yield was 54.3%~93.2%.