• Volume 38,Issue 8,2021 Table of Contents
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    • >Review and monographs
    • Progress of Suzuki coupling reaction catalyzed by loaded NHC-Pd complexes

      2021, 38(8):0-0.

      Abstract (1260) HTML (0) PDF 678.93 K (95) Comment (0) Favorites

      Abstract:As an effective method of constructing carbon-carbon bonds, the Suzuki coupling reaction of palladium catalysis has been widely used in natural products, total pharmaceutical synthesis and organic synthesis industries. The currently widely used palladium-containing homogeneous catalysts have high reaction activity, but expensive palladium metal salts or complexes are not easy to be recycled, and traces remain in the target product or waste liquid, causing heavy metal pollution of the target product and environmental pollution, which greatly increases the cost of the reaction and reduces the safety of the product. Therefore, it is expected that a heterogeneous catalyst that is easy to be recycled and low in palladium leaching can be used to achieve high-efficiency and green catalysis of the reaction.The nitrogen heterocyclic carbene palladium complex (NHC-Pd) has the advantages of high reactivity and good stability in catalyzing the Suzuki coupling reaction, and is often used as the catalytic center of heterogeneous catalysts. Starting from the support materials of heterogeneous catalysts such as polymer materials, porous silicon materials, carbon-based materials, metal-organic frameworks and magnetic nanoparticles, this paper reviews the latest research progress of NHC-PD in heterogeneous catalytic Suzuki coupling reaction in recent year, which has guiding significance for the development of this research direction in the future.

    • >Functional materials
    • Ru/Al2O3 modification and catalytic hydrogenation of diisoonyl phthalate

      2021, 38(8):0-0.

      Abstract (363) HTML (0) PDF 1.42 M (100) Comment (0) Favorites

      Abstract:Ruthenium catalysts with different supports were prepared by equal volume impregnation method. Ru/Al2O3 was selected as the best catalyst for the hydrogenation of diisoononyl phthalate to diisoonyl 1,2-cyclohexane dicarboxylate. The support Al2O3 was modified by hydrothermal treatment at 140 ℃ for 4h, pore forming agent addition of 1%, binder addition of 5%, calcination at 700 ℃ for 4h. Al2O3 with different ruthenium loading amount was characterized and evaluated. The results showed that the best ruthenium loading amount was 0.3%. The conversion of diisoonyl phthalate was 98.9% and the selectivity of diisoonyl 1,2-cyclohexanedicarboxylate was 97.1% under the conditions of temperature 150 ℃, pressure 5MPa and space velocity 0.25h-1.

    • Research Progress on Self-assembly of Amphiphilic Starch

      2021, 38(8):0-0.

      Abstract (490) HTML (0) PDF 990.67 K (93) Comment (0) Favorites

      Abstract:Due to its unique amphiphilic structural characteristics, amphiphilic starches (AS) are dissolved in selective solvents can self-assemble to form spherical micelles with a core-shell structure under the push of hydrophobic force. The micelles can enclose hydrophobic guests and confine them in space to form supramolecular inclusion compounds. AS self-assembly expands the application range of starch as a carrier. This article summarizes the principles, preparation methods, and influencing factors of the self-assembly of AS, introduces the research progress in the application of this method in the fields of food, medicine, and industry, and puts forward the current problems in the field of self-assembly of AS, and possible future research directions.

    • Pyrrolidone citrate used for thickening of amino acid surfactants

      2021, 38(8):0-0.

      Abstract (483) HTML (0) PDF 1.92 M (86) Comment (0) Favorites

      Abstract:New pyrrolidone citrate surfactants(HCA-nC8P, HCA-nC12P) were constructed via acid-alkali reactions of pyrrolidone surfactants (N-octyl-2-pyrrolidone, C8P and N-dodecyl-2- pyrrolidone, C12P) with citric acid. The related factors affecting surface-active properties and the effects of different proportions of citric acid on the solubility and wetting of C8P or C12P were studied. The experiments of surface tension and electrical conductivity show that the ionic surfactants are formed, and the addition of citric acid can affect the surface activity of HCA-nC12P more than that of HCA-nC8P. When the mole ratio of C8P or C12P and citric acid increases, CMC and Γmax gradually decrease, pC20 and Amin increase. When the mole ratio is 1:1, the water solubility of HCA-1C8P or HCA-1C12P increases, and the wettability gets better as the ratio increases. Through rheological experiments, pyrrolidone citrate surfactants can well increase the viscosity of sodium lauroyl sarcosine aqueous solution. The addition of HCA-nC8P can increase the viscosity of 15 wt% sodium lauryl sarcosine aqueous solution by 10~15 times, and with the increase of carbon chain length(HCA-nC12P), the viscosity can increase to 70~80 times.

    • Synthesis and anti-aging evaluation of fructosazine

      2021, 38(8):0-0.

      Abstract (410) HTML (0) PDF 1.78 M (111) Comment (0) Favorites

      Abstract:Fructosazine was synthesized from D-gluctose by 4 steps,including Amadori rearrangement, isopropylidene protection, cascade reaction of hydrodebenzylation and oxidative aromatization catalyzed by Pd/C, and removal of isopropylidene protection. The structure of the key intermediate isopropylidene fructosazine was characterized by NMR, MS, X-ray single crystal diffraction. The MTT method was used to determine the effect of fructosazine on the viability of human fibroblast cells (2BS cells). Compared with the control group, 2BS cell viability was significantly enhanced 25% by 1 μmol/L fructosazine. The aging marker β-galactosidase (SA-β-Gal) method was used to evaluate the anti-aging activity of fructosazine. The blue staining rate of early-senescent and mid-senescent 2BS cells, which were continuously cultured with 1 μmol/Lfructosine, were 14% and 19% less than that of the control group respectively. The results showed that fructosazine had anti-aging activity on 2BS cells in the early or middle stage of aging.

    • The fabrication of photonic crystal structurally colored films by mixing different sized silica nanoparticles

      2021, 38(8):0-0.

      Abstract (814) HTML (0) PDF 2.83 M (69) Comment (0) Favorites

      Abstract:247 nm and 285 nm SiO2 nanoparticles with good dispersibility were synthesized using a Stöber-based solvent varying method, and different structural colors films were obtained by controlling the mixing ratio of the two sized silica nanoparticles. When the proportion of 247 nm SiO2 increased, the color gradually appeared blue-shift, but due to the influence of uncorrelated light scattering, the color of the photonic crystal films are lighter. To solve the problem, the ink was added to the silica suspension, when concentration of the ink increased, the lightness of the film decreased, the saturation increased and the saturation is the highest when the mass fraction of ink was 0.06%. The article made specific analysis on the influence of particle size, mixing ratio and ink content on structural color, the study found that the structural color of the photonic crystal was affected by the particle size and conformed to the Bragg formula, the different mixing ratio changed the average particle size of SiO2, thus formed different colors.The method of producing different structural colors from two particle sizes of SiO2 is simpler and quicker, and can be applied to pigments and coatings for dyeing.

    • Pickering emulsion stabilized solely by hydrophilic SiO2 Nanoparticles

      2021, 38(8):0-0.

      Abstract (549) HTML (0) PDF 10.39 M (209) Comment (0) Favorites

      Abstract:Pickering emulsions were successfully stabilized by highly hydrophilic silica nanoparticles (SiO2 NPs) near the isoelectric points. We found that vigorous mixing of SiO2 NPs suspensions of with oil, van der Waals forces between particles and oil droplets are sufficient to trap SiO2 NPs in close proximity to oil-water interfaces when the pH of suspensions equal to isoelectric points, and O/W Pickering emulsions were stabilized. Increasing the concentrations of SiO2 NPs or decreasing the oil phase volume fractions leads to a higher particle absorbing amount at the oil/water interface, higher viscosity of the continuous phase as well as the formation of a three-dimensional network structure between the emulsion droplets, thereby improving the stability of the emulsions. The emulsions perform good pH responsiveness benefiting from the protonation and deprotonation of silanol on the surface of SiO2 NPs under varying pH.

    • Synthesis of Anisole from Phenol and Dimethyl Carbonate catalyzed by solid base KF/MgAl-LDO

      2021, 38(8):0-0.

      Abstract (398) HTML (0) PDF 542.79 K (84) Comment (0) Favorites

      Abstract:The solid base catalysts MgAl-LDO and KF/MgAl-LDO doped with different alkali metal halides(MX) were prepared by MgAl-LDHs as precursor. XRD characterization and Hammett titration were carried out, and the catalytic activity for the synthesis of anisole from phenol and dimethyl carbonate was investigated. The results showed that the Mg/Al molar ratio, precipitation pH and calcination temperature of MgAl-LDHs all affect the structure and basicity of the catalyst, and the droping of KF greatly increases the base amount of the catalyst, especially the strong base amount of H0(11-15), which is mainly provided by KMgF3 and K2CO3. The catalyst of KF/MgAl-LDO with the KF mass fraction of 33% showed the best catalytic performance. When the molar ratio of DMC to phenol was 2:1, the catalyst dosage is only 1 wt%(based on the phenol mass), reaction temperature is 200 ℃, reaction time is 4 h, the yield of anisole was 95.2%. The research of the relation between the activity and the basicity showed that the activity of the catalyst was positively correlated with the total base amount, and the strong base site of H -(11~15) had the highest catalytic performance.

    • Polyvinyl alcohol (PVA)/kaolin hemostatic membranes based on electrospin technology

      2021, 38(8):0-0.

      Abstract (405) HTML (0) PDF 2.56 M (94) Comment (0) Favorites

      Abstract:Solidified the polyvinyl alcohol water solution with different ratio of kaolin to fabricate hemostatic membranes by electrospinning. The SEM and EDS images showed that kaolin had been distributed on the membranes’ fibers. The hemostatic performance experiments showed that membranes made from10% PVA (mass ratio)/2% kaolin (mass ratio) solution performed best on hemostatic quality. It coagulate pig blood in vitro by 254 ± 2 s, and the blood loss and clotting time on SD rats’ hepatic injury experimentwere 167 ± 9 s and 0.21 ± 0.05 g, respectively. The further study on the hemostatic mechanisms, PK2 showed that it could decrease 7.2% and 4.7% clotting time on the APTT (activated partial thromboplastin time) and PT (prothrombin time) tests comparing with the controls, respectively, and it formed strong blood clots about 8 minutes. Combining with the low cytotoxicity and low hemolysis ration, it could be concluded that the PVA/kaolin electrospun membranes had high prospect on commercial application.

    • Research progress of CO2 capture materials

      2021, 38(8):0-0.

      Abstract (507) HTML (0) PDF 5.44 M (93) Comment (0) Favorites

      Abstract:Global warming caused by excessive CO2 emissions has become a primary issue in the environmental crisis, and hence it is imperative to achieve the strategic objectives of peak carbon dioxide emissions and carbon neutrality proposed by our nations. To solve this problem, a variety of CO2 capture and storage technologies have been adopted by numerous scientific researchers. This article focuses on major CO2 adsorbents, such as carbon-based materials, zeolites, metal organic framework materials, hydrotalcite materials, metal oxides and supporting amine-based materials, etc. Moreover, the latest research progress of CO2 adsorbents, including the adsorption mechanism, performance advantages and disadvantages, directions of improvement and current challenges, has been introduced in detail, and prospects for future development of the adsorption materials have been provided.

    • Research progress of electrospinning nanofiber membrane in air filtration

      2021, 38(8):0-0.

      Abstract (616) HTML (0) PDF 1.85 M (124) Comment (0) Favorites

      Abstract:Electrospinning nanofiber membrane has the advantages of small pore size, high porosity and well fiber uniformity, which makes it show great application potential in the fields of air filtration and personal protection. This paper briefly introduces the principle, equipment and technological parameters of electrospinning and summarizes the latest research results at home and abroad on the preparation of high-efficiency, low-resistance and functional new air filter materials (antibacterial, degradable, hydrophobic and high-temperature resistant functions) by electrospinning in recent years. The existing problems in existing research and future research development directions are analyzed and discussed.

    • Sonochemical fabrication and photocatalytic properties of Au-modified nano ZnO

      2021, 38(8):0-0.

      Abstract (341) HTML (0) PDF 1.65 M (93) Comment (0) Favorites

      Abstract:Au modified ZnO nanoparticales (Au/ZnO) were successfully prepared by a simple sonochemical method, without adding any active agent. The as-prepared products were characterized by SEM, TEM, XRD, PL, UV-VIS, UV-DRS and BET. The results show that Au3+ is directly reduced on the surface of ZnO to form nanoparticles by sonochemical method, and Au nanoparticles preferentially grow along the surface of ZnO, thus forming a close interface structure between the two materials. The modification of Au nanoparticles makes the UV peak at 384 nm shifts to blue and its intensity is obviously weakened, meanwhile, the intensity of visible luminescence peak decreases until it disappears, indicating that the photo-generated charges are effectively separated. With an appropriate amount of gold decoration, the UV light absorption capacity of the Au/ZnO was significantly enhanced, and a certain degree of visible light absorption appeared, indicating that the light utilization rate has been improved. Photocatalytic experiments show that Au/ZnO can effectively degrade methyl orange and methyl blue solutions. Kinetic analysis of the photodegradation properties using ln(ρ/ρt)=kt linear fitting shows that as the amount of Au is 0.5% (based on the amount of ZnO substance, the same below), the first order degradation reaction rate constant of methylene blue and methyl orange is 4.26 and 2.38 times of pure ZnO, respectively, and their degradation can reach 100%.

    • Preparation of temperature-responsive controlled-release antioxidant composite membrane based on temperature-sensitive liposomes of rosemary essential oil

      2021, 38(8):0-0.

      Abstract (327) HTML (0) PDF 3.62 M (100) Comment (0) Favorites

      Abstract:Using synthetic phospholipid DPPC and cholesterol as membrane materials, the rosemary essential oil (REO) temperature-sensitive liposomes (t-L) were prepared by ether injection method, The temperature-sensitive liposomes were added to the chitosan-pululan solution, and BOPP was used as the base membrane to prepare an antioxidant composite membrane. The encapsulation efficiency, particle size distribution, PDI dispersion coefficient, phase transition temperature and atomic force microscopy of rosemary temperature-sensitive liposomes were measured. Measure the release rate of essential oil in the film to verify the temperature response characteristics of the film. The results showed that the average encapsulation efficiency of the prepared temperature-sensitive liposomes was 65.6%, the average particle size was 164.8nm, the average polydispersity index (PDI) was 0.163, and the switching temperature was 38.5℃ and 41.8℃. The anti-oxidant composite film released 94.1% in 7 days at 42℃, it has a significant temperature response control release effect.

    • Research progress of nitrogen-containing carbon materials for acetylene hydrochlorination

      2021, 38(8):0-0.

      Abstract (363) HTML (0) PDF 5.70 M (91) Comment (0) Favorites

      Abstract:Due to mercury pollution and its shortage resources, the research and development of novel, eco-friendly and efficient mercury-free catalysts for acetylene hydrochlorination is the key to realize the green and sustainable development of polyvinyl chloride industry. Nitrogen-containing carbon materials with excellent performance as catalyst supports provide a new idea for the research of mercury-free catalysts for acetylene hydrochlorination, which is also one of the research hotspots in this field. In this work, the application of nitrogen-containing carbon materials in acetylene hydrochlorination reaction are summarized and the research directions in the future of N-containing carbon materials in acetylene hydrochlorination are discussed.

    • Preparation and in vitro release of pH-responsive astaxanthin chitosan microspheres

      2021, 38(8):0-0.

      Abstract (336) HTML (0) PDF 530.35 K (92) Comment (0) Favorites

      Abstract:Water-soluble carboxymethyl chitosan was prepared by chemical modification of N,O- carboxymethyl chitosan with chloroacetic acid and chitosan as raw materials. Carboxymethyl chitosan microspheres and carboxymethyl chitosan microspheres loaded with astaxanthin were prepared by emulsion method. The morphology, dispersion and particle size of carboxymethyl chitosan microspheres were investigated. The results show that the optimal preparation conditions of microspheres are as follows: The content of carboxymethyl chitosan (based on water phase mass, the same below) was 1.0%, the volume ratio of oil to water was 1∶1, the content of Span 80 (based on oil phase volume, the same below) was 4.0%, the content of glutaraldehyde (based on oil phase volume, the same below) was 7.5%, and the shear rate was 4000 r/min., IR test showed that the microspheres were successfully loaded with astaxanthin, and the loading rate and encapsulation rate were 10.74% and 67.24%, respectively, when the initial astaxanthin dosage was 20mg.The release rates of astaxanthin microspheres loaded in simulated gastric juice and simulated intestinal juice were 10% and 85%, respectively. Carboxymethyl chitosan can be used as a drug carrier.

    • Green synthesis and antioxidation activities of coumarin-3-carboxylic acids

      2021, 38(8):0-0.

      Abstract (387) HTML (0) PDF 439.82 K (89) Comment (0) Favorites

      Abstract:In order to optimize the synthesis methods of coumarin-3-carboxylic acids and investigate their antioxidant properties, eighteen coumarin-3-carboxylic compounds were obtained via the reaction of meldrum’s acid and various salicylaldehydes without catalyst in water. The structures of the obtained compounds were confirmed by 1HNMR and 13CNMR, and the antioxidant activities were evaluated by inhibiting DNA oxidation reaction by hydroxyl radical (HO•), reductive glutathione radical (GS•) and 2,2′-azobis(2-methylpropionamidine) dihydrochloride (AAPH), aiming at exploring antioxidant abilities of different types and positions of the substitutes. The results showed that this approach is green and efficiently, and can tolerate substrates with diverse functional groups. The yields of the eighteen coumarin-3-carboxylic compounds were with ranged from 54.3% to 95.6%. All the compounds exhibited strong activities to protect DNA against oxidation induced by HO•, GS• and AAPH. The absorbance percentages of thiobarbituric acid reactive substances (TBARS) were 69.42%~93.39%, 75.23%~99.45% and 66.62%~97.72%, respectively. In reaction of inhibiting HO•, GS• and AAPH induced oxidation of DNA, the TBARS percentages of hydroxyl substituted compounds (compounds XV ~ XVIII) were 69.42% ~ 77.67%, 75.23% ~ 82.87% and 66.62% ~ 75.08%, respectively. The TBARS percentages of hydroxyl substituted compounds were far less than the other coumarin-3-carboxylic compounds (compounds I ~ XIV). The results indicated that hydroxyl substituted coumarin-3-carboxylic acids showed similar TBARS percentages to water-soluble vitamin E, and can be used as potential antioxidants.

    • Suzuki Coupling Reaction Catalyzed by Palladium Supported on Mesoporous Titanium Dioxide in Continuous Flow

      2021, 38(8):0-0.

      Abstract (279) HTML (0) PDF 1.83 M (109) Comment (0) Favorites

      Abstract:0.1 wt%~1.0 wt% heterogeneous Pd/m-TiO2 catalysts were prepared by Sol-Gel method using PdCl2 and n-butyl titanate as raw materials, PVP as metal protective agent, F127 as template agent. The structure was characterized by BET, XRD and TEM. The results showed that the catalysts had an ordered mesoporous structure with 8 nm~10 nm pore size distribution, 11.3 nm~13.3 nm palladium particle size and good dispersion. Then Pd/m-TiO2 catalyst was fixed by micro-packed reactor to catalyzed Suzuki coupling reaction in continuous flow. The optimal continuous flow process was determined: mixed solvent of DMF and water (V:V=1:1, 400 mL), base K3PO4(n碱:n溴苯=1.5:1) , 0.20 mL/min flow rate, 0.10 mol/L bromobenzene, 0.12 mol/L phenylboronic acid, 0.15 mol/L K3PO4, 0.7 wt% palladium loading and 80 ℃ reaction temperature. The yield of Suzuki coupling reaction was 99% in 6.8 min residence time. The catalyst still maintained good catalytic activity after repeated use.

    • Preparation of magnesium-triphenylamine based MOF for synergistic Lewis acid and photoredox catalysis

      2021, 38(8):0-0.

      Abstract (469) HTML (0) PDF 1.45 M (165) Comment (0) Favorites

      Abstract:Self-assembly between Lewis acidic Mg2+ and photoredox tricarboxytriphenyl amine (H3TCA) constructs a metal organic framework Mg-TCA. SC-XRD was used to determine the crystal structure. UV-vis spectrum indicates that Mg-TCA has a good absorption ability in visible light region. CV,UV-vis and FL measurements indicate that the redox potential of the photoexcited Mg-TCA is -1.95 V (vs. SCE). Mg-TCA can effectively allow access to a wide range of α-alkyl-acetophenones (30%~82%) under the synergistic Lewis acid and photoredox catalysis, and the reaction conditions is shown as below: styrene substrate (0.2 mmol), NHPI ester (0.3 mmol), Mg-TCA (0.01 mmol), DMSO (2 mL), irradiated by 405 nm LED for 24 h at N2 atmosphere. The catalyst can be reused for three times without deactivation, and its structure remains intact before and after use. Mechanism studies indicate a synergistic Lewis acid and photoredox catalysis process within this transformation, the Lewis acidic nodes of Mg-TCA can bind and absorb NHPI ester, putting the NHPI ester approximate to the photoredox catalytic center within Mg-TCA, thus improving the catalytic efficiency.

    • NH3-SCR performance over bimetal exchanged Cu-Mn/SSZ-39 catalyst

      2021, 38(8):0-0.

      Abstract (581) HTML (0) PDF 2.51 M (112) Comment (0) Favorites

      Abstract:Abstract: Using SSZ-39 as support, Cu-Mn/SSZ-39 zeolite catalysts with different Cu/Mn mole ratio were prepared by ion-exchange method for selective catalytic reduction of NO by NH3 (NH3-SCR). The structures, morphologies and surface acidities of the catalysts were characterized by XRD, SEM, N2 adsorption-desorption , NH3-TPD, H2-TPR ,XPS and ICP techniques. The results show that Cu2 provides the major active sites. The catalysts exchanged with Cu2 have the good catalytic activities and N2 selectivities. The moderate exchange of Mn2 /3 increases the concentration of acid sites, especially the weak Lewis acid sites. The Cu-Mn/SSZ-39 catalysts show the good low temperature NH3-SCR activities and hydrothermal stability. When the mole ratio of Cu:Mn is 1:0.6, Cu-Mn(0.6)/SSZ-39 has the excellent low light-off temperature (T50 is 125 ℃), wide temperature window from 184 ℃ to 433 ℃, and the N2 selectivity reaches above 90% at below 450 ℃. After hydrothermal aging, the initial original crystal structure, morphology and NH3-SCR activity of Cu-Mn(0.6)/SSZ-39-A are well maintained, showing a good hydrothermal stability.

    • >Catalysis,separation and purification technology
    • Bi0/Bi2O2CO3/N-TiO2 composite material: preparation and photocatalytic performance

      2021, 38(8):0-0.

      Abstract (616) HTML (0) PDF 1.92 M (114) Comment (0) Favorites

      Abstract:A solvothermal method using TiO2 nanobelts as a substrate, ethylenediamine as a reducing agent and a nitrogen source to synthesize the photocatalytic composite Bi0/Bi2O2CO3/N-TiO2 is proposed. The obtained material was characterized by XRD, SEM, TEM etc. In the architecture of the composite, compound quantum dots combined with Bi0 and Bi2O2CO3 (1.40~1.50 nm) uniformly grew on the surface of TiO2 nanobelts (NBs). Compared with TiO2 (30.95%), Bi0/Bi2O2CO3/N-TiO2 realized a more efficient degradation of Rhodamine B (95.02%) under visible light irradiation. Finally, the active species-trapping experiments was carried out to explore the main active species. In the photoreaction, h+ and •OH may be the main active species.

    • >Drug and cosmetic materials
    • Preparation of biomimetic adhesive polydopamine eugenol antibacterial microcapsules

      2021, 38(8):0-0.

      Abstract (639) HTML (0) PDF 8.10 M (99) Comment (0) Favorites

      Abstract:Polydopamine eugenol microcapsules (PDA@EO) with controllable size were prepared by emulsion template interfacial polymerization using eugenol (EO) as the core material and dopamine (DA) as the shell material. The chemical structure, morphology, size and its distribution, and properties of the microcapsules were characterized by FTIR, TG, UV-Vis, SEM and TEM. The results showed that the microcapsules had regular spherical shape with size ranging from 55 to 94 nm. The encapsulation efficiency and the encapsulation capacity ware 25.35% and 0.6288 g/g, respectively. The cumulative release rate reached 68.39% after 24 h. The excellent adhesive property of PDA@EO microcapsules on different surfaces was verified by a comparative study. When treated with common bacteria in the site of oral infection Staphylococcus aureus (S·aure) and Escherichia coli (E·coli) for 24 hours, the growth of the cells was inhibited, PDA@EO Compared with free eugenol, the antibacterial activity of microcapsules increased by 36.84% and 35.52%, respectively; when the concentration of the microcapsule reached 2.0 g/L, the antibacterial activity of PDA@EO microcapsules against both bacteria was more than 99%.

    • >Food and feedstuff chemicals
    • Synthesis of long wavelength hydrogen peroxide fluorescent probe and its application in food safety detection

      2021, 38(8).

      Abstract (74) HTML (0) PDF 1.19 M (202) Comment (0) Favorites

      Abstract:A hydrogen peroxide fluorescent probe TC-BOR was designed and synthesized based on hemicyanine fluorophore with borate as the recognition group,and its structure was characterized by 1HNMR, 13CNMR and HRMS. The result shows that the product after reaction with H2O2 (TC-OH) fluoresces at 723 nm, with 55-fold NIR fluorescence enhancement, a rapid response within 7 min and low detection limit of 2.27 μmol·L-1. Subsequently, TC-BOR was used for the qualitative and quantitative determination of hydrogen peroxide in food and living cells, which provided a new method for the rapid detection of H2O2 in food.

    • Production of structured phospholipids rich in short-chain fatty acids catalyzed by SO3H-functionalized carbon/silica materials

      2021, 38(8).

      Abstract (118) HTML (0) PDF 0.00 Byte (88) Comment (0) Favorites

      Abstract:A kind of sulfonic acid-functionalized carbon/silica (C/Si-SO3H) material was successfully synthesized at low temperature via chemically activating organic sulfonic acid precursors, which was used for catalytic production of structured phospholipids rich in short-chain fatty acids by interesterification of soybean lecithin with ethyl propionate or methyl butyrate. The influences of reaction temperature, reaction time, catalyst amount and catalyst recyclability on interesterification were investigated in detail. Besides, the structure and surface acid properties of the as-prepared C/Si-SO3H catalyst were studied by FT-IR, Raman and Boehm titration method to establish its structure-performance relationship. The results showed that a large amount of Brӧnsted acid sites were grafted onto the C/Si-SO3H surface, suggesting its prominent catalytic activity for production of structured phospholipids rich in short-chain fatty acids. Correspondingly, the propionic acid or butyric acid incorporation was up to 18.33% or 16.23% at 40 ℃ within 6 h when the catalyst loading was 7%. Notably, C/Si-SO3H catalyst was recycled for 5 times without obvious deactivation.

    • >Electro-organic chemistry and industry
    • Low temperature self-propagating combustion synthesis and electrochemical properties of Li1.2Fe0.2Mn0.6O2 nanoparticles

      2021, 38(8).

      Abstract (175) HTML (0) PDF 1.30 M (77) Comment (0) Favorites

      Abstract:Abstract: Li1.2Fe0.2Mn0.6O2 nanoparticles were synthesized by self-propagating combustion at low temperature of 450℃(LFMO-450). Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscope (TEM) and galvanostatic charge-discharge tests were applied to analyze the crystal structure, micromorphology, ultrastructure and electrochemical properties of Li1.2Fe0.2Mn0.6O2 nanoparticles. The results show that simple LFMO-450 has a well-ordered layered α-NaFeO2 and are evenly distributed between 45~88 nm particles. The galvanostatic charge and discharge method test results show that the specific discharge capacity of the LFMO-450 at 0.1, 0.2, 0.5, 1 and 2C is, respectively, up to 237.5, 170.7, 124.1, 101.9 and 82.8 mA·h/g between 2.0 and 4.8 V at room temperature, which shows good rate performance. Under 1C rate, the specific discharge capacity of the sample is 106.4 and 87.8 mA·h/g for the first time and after 60 cycles, and the capacity retention rate is 82.5%, which shows good cycle performance.

    • >Dyeing and finishing auxiliaries
    • Synthesis of UV-curable branched polyurethane dispersant

      2021, 38(8):0-0.

      Abstract (590) HTML (0) PDF 764.28 K (92) Comment (0) Favorites

      Abstract:The polyurethane dispersant was designed into a hyperbranched structure, and a series of UV-curable branched polyurethane dispersants (BPUs) were synthesized by introducing pigment anchoring groups and acrylic groups into the ends of the polyurethane. This structure endowed the dispersant a self-adhesive effect to improve the fastness of printing. The molecular structure and performance of the dispersant were analyzed by infrared spectroscopy, gel chromatography. The pigment paste prepared with BPUs as the dispersant displayed good dispersion performance, uniform particle size distribution and low viscosity. The smallest particle size change within 5 days of high temperature storage was within 20 nm, and the centrifugal stability at 3000 rpm was above 92%. Using this color paste for direct printing, its washing fastness was maintained at 3~4 level, which was about 2 levels higher than commercial dispersants.

    • >Special dyes and pigments
    • Synthesis of water-based high-pigment dispersion ink emulsion by RAFT polymerization

      2021, 38(8).

      Abstract (106) HTML (0) PDF 657.57 K (84) Comment (0) Favorites

      Abstract:In order to develop the high-pigment dispersion ink emulsion, 3-Allyloxy-2-hydroxy-1-propane sulfonic acid salt (COPS-1) and 2-acrylamide-2-methylpropanesulfonic acid (AMPS) were used to prepare polymeric emulsifiers and polyacrylate emulsions by Reversible addition fragmentation chain transfer (RAFT) polymerization. The structure and properties of the polymeric emulsifiers were characterized by FT-IR, GPC and critical micelle concentration analysis. The influence of RAFT agent dosage, hydrophilic monomer ratio of polymeric emulsifier, hydrophilic monomer amount on the properties of emulsions and coating films were investigated, which revealed that the polymer emulsifiers prepared by RAFT polymerization have good emulsifying properties and narrow molecular weight distribution. The optimal amount of RAFT reagent is 0.6% of the monomer amount, the optimal ratio of the hydrophilic monomer is m(COPS-1)∶m(AMPS)∶m(AA)=1∶2∶3, and the optimal acid amount is 25%. Analysis of the glass transition temperature and particle morphology of the emulsion shows that the latex particles have two glass transitions and are uniformly dispersed.

    • >Building chemicals
    • Research on resource utilization of fluoride sludge solidified by ordinary portland cement

      2021, 38(8).

      Abstract (100) HTML (0) PDF 920.53 K (75) Comment (0) Favorites

      Abstract:The composite Portland cement was used to solidify the fluorine-containing sludge, and the cement standard test blocks with different sludge content were prepared. The effects of sludge content on the compressive strength, fluorine ion leaching amount, phase transformation and crystal morphology of the test blocks were investigated. The results show that when the amount of fluorine-containing sludge is 10%, the strength of test block is high and the amount of fluorine ion leaching is low, which is the more appropriate proportion of sludge. The 28 day compressive strength of the test block with 10% content reaches 22.2 MPa, which meets the strength requirements of general cushion, foundation, floor and structure with little stress.The fluoride ion leaching amount of 10% mixed sample under the action of groundwater and acid rain is 0.16 mg/L and 0.39 mg/L respectively, which is far less than the standard limit of 100 mg/L of hazardous waste and has high safety. Mechanism study shows that the addition of fluorine-containing sludge accelerates the hydration rate of C3A in cement, increases the amount of AFt in the early stage, and improves the early strength of the test block.

    • >Fine chemical intermediates
    • Efficient synthesis of bis(alkyl polyoxyethylene) secondary amine via one-pot method under ambient pressure

      2021, 38(8).

      Abstract (88) HTML (0) PDF 435.58 K (116) Comment (0) Favorites

      Abstract:Polyether secondary amines with polyoxyethylene ether and long-chain alkyl, have been widely used as pigment dispersing agents due to their adjustable structure, low toxicity, and good dispersibility. At present, polyether secondary amines are mainly synthesized via the reaction between polyether polyol and liquid ammonia with low yield and harsh condition. Herein, bis(C12-14 alkyl polyoxyethylene) secondary amine (S/C12-14E5) was successfully synthesized via the intermolecular deamination coupling of amine-terminated polyether with C12-C14 alkyl group (A/C12-14E5) under ambient pressure. The influences of coupling temperature, catalyst dosage, hydrogen flow rate and reaction time on the selectivity of S/C12-14E5 were systematic studied. The results showed that the average secondary amine content reached up to 97.3% when the conditions of reaction temperature was 200 ℃, the amount of catalyst was 2.5% based on the total mass of raw material, the hydrogen flow was 200 mL/min, and reaction time was 5 h. On this basis, we studied the substrate scope and scale-up reaction to demonstrate the utility of our protocol. A possible reaction mechanism was also proposed.

    • Study on clean synthesis process of 4,6-dichloropyrimidine

      2021, 38(8).

      Abstract (161) HTML (0) PDF 465.36 K (80) Comment (0) Favorites

      Abstract:In this paper, a clean process for the synthesis of 4,6-dichloropyrimidine (DCP) was reported. Firstly, 4,6-dihydroxypyrimidine (DHP) was prepared from formamide (HCONH2), dimethyl malonate [CH2(COOCH3)2] and sodium methoxide (CH3ONa) as the catalyst. When the ratio was n[CH2(COOCH3)2]:n(HCONH2):n(CH3ONa) = 1:4:4, and the reaction temperature and time were 60 ℃ and 2 h, respectively, the yield of DHP could reach 90.4%. Then, DHP was reacted with phosphorus oxychloride (POCl3) at 60 ℃ for 2 h to obtain DCP, during this reaction process, 5-ethyl-2-methylpyridine was used as the acid binder, and 1,2-dichloroethane as the solvent. The optimal molar ratio of materials was n(DHP):n(POCl3):n(5-ethyl-2-methylpyridine) = 1:2.2:1.8, the yield of DCP was up to 94.5%. Finally, the chlorinated wastewater was treated with calcium hydroxide[Ca(OH)2] and the recovery rate of the acid binder is larger than 94%. The calcium phosphate[Ca3(PO4)2] can be effectively separated from the calcium chloride (CaCl2) solution, and the recycling of waste water in the DCP production process is realized. Therefore, the wastewater could be avoided successfully and the goal of clean production of DCP was achieved.