liuchao , xuexin , yinqing , lixi , baoyan , ma jianzhong , shilei
2022, 39(3).
Abstract:As a new organic polymer material, polyurethane is known as "the fifth largest plastic", which is widely used in light industry, construction, automobile, aviation and aerospace fields because of its excellent comprehensive properties. However, in the process of processing or using, it is hard to avoid structural damage due to external force, which greatly reduces the mechanical properties of its materials and the service life of its products. Reversible covalent bond is a kind of dynamic covalent bond which can realize reversible fracture and recombination under a certain conditions. Therefore, the introduction of it into the polyurethane molecular chain not only has a small impact on the mechanical properties of the material, but also can give it a self-healing function, thereby significantly improving the service life and added value of its products. In this paper, the self-healing mechanism and application research progress of self-healing polyurethane based on reversible covalent bonds are reviewed, and some problems in the research of its self-healing materials are pointed out, and the future development trend of it is prospected.
LIU xiudong , Pei Jie , WU Chun-kai
2022, 39(3).
Abstract:Abstract: Cell immobilization technology has the advantages of simple process, biocompatibility, stable operation, etc., which can effectively ensure cell viability and realize efficient cell-catalyzed production of fine chemicals. The research status and progress of traditional multi-cell immobilization methods such as surface attachment, gel embedding, and polyelectrolyte layer-by-layer self-assembled membranes in the field of fine chemical (e.g. dihydric alcohols, bioethanol, lactic acid, ester, polysaccharide) production are mainly introduced, followed with the problem analysis. Then, the mechanism, and trend of a new developing immobilization method, single-cell nano-coating, are summarized with the possible application for fine chemicals production. Finally, the technical challenges and research directions that cell immobilization technology faces in the production of fine chemicals are prospected, with a purpose to providing certain technical support for the production of fine chemicals.
XU Wen-long , WANG Sheng , BAO Yan , WANG Hai-yan , CHEN Shuang , ZHAO Zong-shan
2022, 39(3).
Abstract:The frequent occurrence of oil spills at sea and the large amount of oil-bearing and industrial wastewater cause large-scale pollution of water resources and serious damage to the balance of ecosystem. At present, more and more commercial and academic attention has been paid to the separation of oil and organic pollutants from water. Graphene-based aerogels are three dimensional macroscopical materials assembled from two-dimensional graphene sheets. Because of their high porosity, large specific surface area, low density and strong mechanical properties, it has a broad application prospect in the field of oil-water separation and has become one of the research hotspots. The latest research progress of graphene-based aerogels in structural design, assembly and drying methods are systematically summarized in this review. Its application in oil-water separation is also summarized in recent years. The research status and future research directions of graphene based aerogels in the field of oil-water separation are briefly reviewed, in order to provide a new perspective for further exploration in this field.
ZHANG Zhen , SUN Cui-zhen , LIU Ru-peng , WANG Guo-xiu , YANG Lu-bing , WU Zhen
2022, 39(3).
Abstract:PPCPs are a new type of organic pollutants. Compared with common pollutants, PPCPs have a low concentration in the aquatic environment but have a complex chemical structure, various sorts, enormous properties, and are toxic. The conventional processing technology is difficult to remove PPCPs completely. The solid-phase catalyst of heterogeneous catalytic ozonation technology can be recycled and reused and has less secondary pollution. At present, the research of this treatment technology in the field of PPCPs has been extensive. The article describes the surface reaction mechanism, free radical reaction mechanism, and synergistic reaction mechanism that the heterogeneous catalytic ozonation technology often follows to degrade PPCPs. Meanwhile, it further explained the four ways in the free radical reaction mechanism. The article briefly introduces the effects of catalysts and other factors on the degradation of PPCPs, summarizes the application progress of heterogeneous catalytic ozonation in the treatment of PPCPs, and puts forward the problems existing in the current heterogeneous catalytic ozonation technology. Ultimately, the article prospects the future research direction and application prospects of heterogeneous catalytic ozonation technology.
ZHOU Yao-hong , ZHANG Xiao-hua , XIONG Wan-ming
2022, 39(3).
Abstract:Catalytic oxidation technique is one of effective ways to realize resource utilization of lignin, which can transform lignin into aromatic aldehydes (p-hydroxybenzaldehyde, vanillin, syringaldehyde, etc.) with high functionalization. Aromatic aldehydes are important intermediates in the synthetic of dyes, perfumes and pharmaceuticals, and have great industrial application value. Herein, this review summarizes the latest research progress in the preparation of aromatic aldehydes from lignin at home and abroad through five aspects: metal catalytic oxidation, organic catalytic oxidation, electrochemical catalytic oxidation, photocatalytic oxidation and ionic liquids catalytic oxidation, and briefly elaborates the reaction process mechanism under different catalytic systems. On this basis, the direction of research regarding the value-added of lignin catalytic oxidation is prospected to develop targeted catalysts for different lignin in order to contribute to the high value utilization of lignin. Finally, it is pointed out that regulating the oxygen vacancy on the surface of metal oxides is an effective strategy to selectively catalyze the preparation of aromatic aldehydes from lignin.
2022, 39(3).
Abstract:Attapulgite is a cheap and easy-to-obtain natural clay mineral. It has large specific surface area, high cation exchange capacity, abundant surface functional groups and etc. Through different modifications of its characteristics, attapulgite can be combined with various base membranes to form a composite membrane. The advantages and disadvantages of the preparation method of attapulgite composite separation membrane are analyzed; The effects of attapulgite addition on the tensile strength, Young's modulus and elongation at break of the composite membrane were summarized; The applications of attapulgite composite membrane in CO2 separation, heavy metal separation, dye separation and oil-water separation were introduced, and its separation mechanism was analyzed. Finally, challenges as well as research directions of attapulgite composite separation membrane are prospected.
haoyupeng , liulu , zhangyuang , tangbingtao
2022, 39(3).
Abstract:The PEG/EG electro-thermal energy conversion phase change materials (PCMs) are prepared by encapsulating polyethylene glycol (PEG) into expanded graphite (EG) support materials via the vacuum impregnation method. The electro-thermal conversion and thermal properties of the composites with various EG mass fraction are further investigated. The results show that EG not only improve the thermal conductivity of the materials, but also endow it with electric conductivity. When the mass fraction of EG is 5%, the electro-thermal conversion efficiency of PEG/EG composites PCMs reach 80.6% under a voltage of 7 V. In addition, the composites exhibit good shape-stability, high phase change enthalpy value (152.2 J/g) and excellent thermal conductivity. The time of PEG/EG in storing heat process is shortened by 73% compared with pure PEG. Therefore, the composites will have a broad application prospect in electro-thermal energy conversion system and thermal energy storage fields.
2022, 39(3).
Abstract:Polyimide (PI) has attracted much attention due to its excellent comprehensive properties. The construction of high-strength aerogels by PI is of great significance for expanding its applications in high-tech fields such as aerospace, microelectronics, etc. In this work, 4,4'-oxydianiline (ODA) and 3,3',4,4'-benzophenone tetracarboxylic dianhydride (BTDA) were used as monomers to construct polyimide aerogels, and aramid nano fibers (ANFs) were introduced to enhance the skeleton of aerogels. The influences of ANFs on the chemical structure, microscopic morphology and mechanical properties of aerogels were explored through Fourier Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM). The results revealed that ANFs were combined with the precursor polyamic acid (PAA) through hydrogen bonding, and were evenly dispersed to enhance the aerogel skeleton effectively. It’s clear that the volume shrinkage rate during the aerogel preparation process effectively reduced with the introduction of ANFs. Compare to the pure PI aerogels, the volume shrinkage of aerogels with 4 wt% ANFs is reduced from 63% to 54%, the Young’s modulus increased from 1.8 MPa to 6.9 MPa, and the compression rebound rate increased by 37%.
2022, 39(3).
Abstract:A series of sulfonated poly(aryl ether sulfone)s proton exchange membranes (4SPAES-x) with four flexible side chains in repeated units were prepared by bromination and graft sulfonation. Their chemical structure was characterized by 1H NMR, and their phase morphology was analyzed by atomic force microscope. It was confirmed that the membranes had a good hydrophilic/hydrophobic phase separation morphology. The ion exchange capacity of 4SPAES-x membrane is 1.12~1.74 mmol/g, and their water absorption, swelling rate and proton conductivity are 11%~32%, 7%~22% and 21~86 mS/cm at 30 ℃, respectively, which increases with the increase of the sulfonation ratio. The maximum energy efficiency of the vanadium flow single cell assembled with 4SPAES-25 membrane is 83.3% at a current density of 40 mA/cm2, which is higher than the 81.5% of Nafion 115. In addition, the efficiency of the single cell also has good cycle stability.
2022, 39(3).
Abstract:Castor oil-based polyurethane acrylate (COPUA) was synthesized from isophorone diisocyanate (IPDI), castor oil (CO) and hydroxyethyl acrylate (HEA). Modified silica sol was prepared by sol-gel method with tetraethyl orthosilicate (TEOS) and 3- (isobutenyl oxide) propyl trimethoxysilane (MEMO). A series of modified silica sols were obtained by adjusting the ratio of TEOS to MEMO. The optimal ratio of MEMS to TEOS was determined to be 1 (MT-1). Based on this, the UV-cured COPUA/SiO2 hybrid material was obtained by changing the addition amount of MT-1. The hybrid materials and coatings were characterized by FT-IR, TEM, SEM, TGA, et al. the mechanical and surface properties of the composite coatings were also tested. The result showed that when the amount of modified silica sol is 15%(based on the mass of COPUA resin, the same below), the SiO2 particles in the coating are evenly distributed. The coating surface is smooth and flat, which can be proved by the excellent light transmittance(100.2%). The hardness of the composite coating is 5H, the adhesion is grade 0 and the flexibility is 1mm; The tensile strength of the film reaches 13.52MPa and the elongation of section is 7.49%,which has a good application prospect in the modification and protection of plastic surface.
2022, 39(3).
Abstract:As a new type of thermoset polymer, polydicyclopentadiene (PDCPD) is valued in industry for its excellent mechanical properties, improved heat resistance, and stable physical and -chemical tolerance. Research on the modification of hydrophilic properties is of importance for the expanding application of the material. Hence, copolymer PDCPD was prepared by copolymerization of dicyclopentadiene (DCPD) with 2-Propenoic acid, 2-methyl-, 2-[ [2,3, 3a, 4, 7,7a-hexahydro-4,7-methano-1H-indenyl] oxy] ethyl ester (DCPEMA) via Ring Open Metathesis Polymerization (ROMP). The research results indicated that DCPEMA copolymerized with DCPD via opening cyclopentene group and olefin double bond. Tensile strength of the copolymer was decreased from 64.3 MPa to 9.2 MPa by introducing DPCEMA. Breaking elongation of the copolymer reached 68.34% when n(DCPD) : n(DCPEMA) = 2 : 1 was applied, however, it dropped with the further increasing of the DPCEMA content. The crosslinking density of the copolymer was evaluated via swelling test. The swelling ratio of copolymer showed similar trends as breaking elongation. Moreover, the surface hydrophilicity of the copolymer could be improved dramatically with the introduction of DPCEMA.
XU Qunna , Yang Yuxi , Ma Jianzhong , Xu Xiaoyu
2022, 39(3).
Abstract:In recent years, hydrogel has attracted wide attention in biomedical and food environmental protection because of its unique network structure and versatility, among which bio-based green functional material has become an important development direction of hydrogel. The antibacterial casein-based nanocomposite hydrogel was prepared by "semi-soluble sol-gel acidification" with casein (CA) as the base, introduced nanoparticles ZnO (ZnO NPs). The experimental results showed that the as-prepared nanocomposite hydrogel had three-dimensional three-dimensional network structure with uniform pore distribution; when ZnO NPs was 3%, the swelling rate reached up to 79.19%, whilst the tensile strength and elongation at break increased to 1.9 MPa and 137.4%,respectively ; the obtained nanocomposite hydrogel showed excellent adhesion to human skin, glass, plastic, metal; and harbored surperior antibacterial properties for E. coli and S. aureus. This research can provide a good application prospect in biomedical dressings fields.
2022, 39(3).
Abstract:In this paper, we have synthesized a water-oil amphiphilic photoinitiator triethylene glycol benzoylformate (TGBF) based on benzoylformic acid and triethylene glycol, and investigated its UV-visible light absorption properties, photolysis mechanism, water solubility and ability to initiate photopolymerization by using UV-vis absorption spectrometer, electron spin resonance spectrometer and real-time infrared spectrometer. The research results show that TGBF has low molar extinction coefficients at above 300 nm, but it is able to undergo intramolecular or intermolecular hydrogen abstraction reaction to produce alkyl radicals to initiate polymerization of acrylate monomers under the irradiation of 405 nm LED. TGBF has good water solubility, and can effectively initiate polymerization of oil-based tripropylene glycol diacrylate (TPGDA) and water-based polyethylene glycol 400 diacrylate (PEG(400)DA). The final double bond conversions reach more than 80%.More importantly, TGBF has excellent ability to initiate deep polymerization of oil-based monomer TPGDA and aqueous monomer PEG(400)DA, with polymerization depths of 5.6 cm and 6.5 cm, respectively, demonstrating that it has a great potential in the field of deep-layer LED photopolymerization.
LIU Xiang , ZHANG Qian , WANG Yingdi , GAO Feng , DONG Yuming
2022, 39(3).
Abstract:Two-dimensional N-TiO2/Ti3C2 photocatalytic composites were synthesized by simple solvothermal reaction, via aluminum titanium carbide, hydrofluoric acid, sodium fluoroborate were used as raw materials and urea was used as nitrogen source, in which TiO2 nanosheets were grown in-situ on highly conductive Ti3C2 MXenes (two dimensional transition metal carbide) nanosheets and meanwhile nitrogen element was doped into TiO2. The catalyst samples were characterized by X-ray diffractometer, scanning electron microscope, transmission electron microscopy, X-ray photoelectron spectrometer, UV-Vis diffuse reflectance spectrometer, photoluminescence spectrometer, etc. The results showed that N-TiO2/Ti3C2 composites showed significantly enhanced photocatalytic degradation ability toward RhB under visible light irradiation, and the degradation rate constant of N-TiO2/Ti3C2 was 8.41 times higher than that of pure TiO2 and degradation ratio was 96.3% within 150min. This is mainly because the doping of nitrogen element narrowed the band gap of TiO2 and extended the light response range to the visible light region. At the same time, the in-situ growth of TiO2 nanosheets formed a close contact interface by Ti3C2 MXenes nanosheets with excellent electrical conductivity, which promoted the separation and migration of photogenerated carriers. The results of free radical trapping experiments and electron spin resonance tests showed that •O2- and •OH were the main active species for RhB degradation in the N-TiO2/Ti3C2 photocatalytic system. In addition, N-TiO2/Ti3C2 composites possess good stability and reusability.
2022, 39(3).
Abstract:In this study, low-cost dimethyldimethoxysilane was used as the main raw material to prepare and synthesize polydimethylsiloxane (PDMS) through hydrolysis condensation reaction, and then it was introduced into castor oil-based waterborne polyurethane (CWPU-SOP) to prepare modified castor oil-based waterborne polyurethane (PDMS/CWPU-SOP) with antifouling performance. The results showed that when the amount of PDMS was 8%, the contact angle of PDMS/CWPU-SOP film was increased by 25? to 110?, and the water absorption of PDMS/CWPU-SOP film was decreased by 7% to 15%. PDMS improved the film's hydrophobicity and water resistance. PDMS/CWPU-SOP film can roll freely on the surface of different acid and alkaline droplet without leaving any trace, with a certain antifouling performance.
XIE Fan , GAO Kun , ZHUO Long-hai , CHEN Shan-shan , MA Qin , JIA Feng-feng , LU Zhao-qing
2022, 39(3).
Abstract:In this study, RGO was obtained by chemical hydrothermal reduction method, and ANF was prepared by chemical splitting method. With ANF with high mechanical properties as matrix, RGO with strong electrical properties was introduced, and RGO/ANFs composite aerogel with compressible spring back and high electromagnetic shielding efficiency was prepared by freeze-drying method. The effects of different amounts of RGO on the microstructure, electrical conductivity, mechanical properties and electromagnetic shielding properties of RGO/ANFs aerogels were systematically studied. The results showed that when the mass fraction was 20 wt.%, the electrical conductivity of the system was as high as 15.84 S/cm, and the electromagnetic shielding efficiency could reach 22 dB. When the 30% compression strain, the compressive stress could reach 21 kPa. The spongy porous structure increased the multiple reflection of the incident electromagnetic wave and improved the electromagnetic shielding performance, making the three-dimensional RGO/ANFs composite aerogel an ideal and efficient electromagnetic shielding material with both mechanical properties and electromagnetic shielding performance. The composite aerogel with both electromagnetic shielding and mechanical properties is expected to be used in communication, microelectronics, aerospace and other fields.
2022, 39(3):0-0.
Abstract:The g-C3N4/Bi2MoO6 precursor was prepared by solvothermal method with melamine, sodium molybdate dihydrate and bismuth nitrate pentahydrate as raw materials, then loaded Ag3PO4 nanoparticles by coprecipitation method, the g-C3N4/Bi2MoO6/Ag3PO4 composite was obtained. The composite was characterized by XRD, FTIR, XPS, SEM and UV-Vis DRS. Tetracycline hydrochloride (TC) was used as the target degradation, the results showed that the degradation rate of 10 mg/L TC reached 93% in 50 min under visible light irradiation. The corresponding rate constant was 0.033 min-1, which was higher than g-C3N4, Bi2MoO6 and Ag3PO4 with 33 times, 3.6 times and 1.5 times, respectively, showing that the g-C3N4/Bi2MoO6/Ag3PO4 composite had the best catalytic performance among all the catalyst. After four cycles with g-C3N4/Bi2MoO6/Ag3PO4, the degradation rate of TC was 71%, higher than Ag3PO4, indicating that the g-C3N4/Bi2MoO6/Ag3PO4 composite had better stability. According to the experimental results of free radical capture, the main active species in the process of TC degradation were ·OH- and ·O2–. Finally, the possible degradation mechanism and degradation path were supposed.
DU Meng , XU Xiang , JIANG Shan , ZHENG Nan , LIU Dehua , SONG Wang-ze
2022, 39(3):0-0.
Abstract:Photosensitizers played crucial roles in photodynamic therapy (PDT) and most of them owned the macrocyclic and conjugated structures, which would lead to undesired aggregation-induced quenching (ACQ) effect. To solve the ubiquitous ACQ effect and strong hydrophobicity of photosensitizers, in this work, a series of water-soluble polyporphyrins (P-1O, P-3O, and P-5O) were prepared using different flexible chains containing ether groups. Upon screening, P-5O owned best water-solubility, highest singlet oxygen yield (1.95 folds vs porphyrin monomer), and could self-assembled into nanoparticles (NPs) with the particle size of 100 nm in a carrier-free manner. Such NPs had excellent stability upon different pH values, serum, dilution folds, freeze-drying, and incubation time. In vitro photo/dark toxicity results indicated that the NPs had low dark-toxicity in both tumor cells (Hep1-6) and normal cells (293T) (cell viability higher than 80%). The NPs had obvious photo-toxicity in Hep1-6 cells(cell viability fewer than 30%), indicating the typical anti-cancer PDT effect.
2022, 39(3).
Abstract:Abstract: In order to study the structure control method and structure-activity relationship of multi-branched cationic polyurethane surfactants with multiple long alkyl chains, isophorone diisocyanate (IPDI), N-methyldiethanolamine, cetyl alcohol and bromine Substituted alkanes are used as raw materials to prepare a series of multi-branched long-chain alkyl quaternary ammonium polyurethane surfactants (SC2、SC3、SC4). The structure of the product was confirmed by infrared spectroscopy, gel chromatography and proton nuclear magnetic resonance spectroscopy. The critical surface tension, Krafft point, foamability, emulsification and salt resistance were tested. Due to the difference in polarity between monomers, products and solvents, cationic polyurethane surfactants (SC3) with three-branched long-chain alkyl groups cannot be obtained according to the formulation design. The product is a mixture of SC2 and SC4. The surface tension (γCMC) of the cationic polyurethane surfactant (SC2) with dihexadecyl group is 23.61mN/m, the corresponding critical micelle concentration (CMC) is 0.30×10-3mol/L, and the Krafft point is 23. ℃; The surface tension (γCMC) of the cationic polyurethane surfactant (SC4) with four hexadecyl groups is 30.35mN/m, the CMC is 0.25×10-3mol/L, and the Krafft point is 41℃; at the same time, the product It has high surface activity and good emulsification, foaming and salt tolerance. The results show that for surfactants with complex structures, the preparation method based on the reaction of isocyanate with hydroxyl is simple and reliable. Keywords: polyurethane surfactants; hyperbranched; cationic; structure-activity relationship
WU Ying , LIU Qing , TANG Wen , WANG Jiaqi , WANG Shuangdan , HOU Furong
2022, 39(3):0-0.
Abstract:The antioxidant, whitening, antibacterial activities, cytotoxicity and skin permeability effects of volatile oil of Salvia miltiorrhiza, dandelion extract and their complexes were tested, and the synergistic effects of S. miltiorrhiza volatile oil and dandelion extract were investigated. The results showed that the antioxidant activity of the complexes was stronger than that of the two alone, and slightly higher than that of the positive control VC. The results of enzyme kinetics showed that the inhibitory effect of volatile oil on tyrosinase activity was stronger than that of arbutin, the positive control. The inhibitory type of volatile oil on tyrosinase was competitive, and the inhibition constant KI was 0.0049 mg/L. There was no antagonistic effect between volatile oil and dandelion on tyrosinase activity. The inhibitory effect of the complexes on Staphylococcus aureus were better than that of the single component, which was comparable to the positive control, streptomycin sulfate. The extract had no cytotoxicity when the concentration reached 100 mg/L. After complexing the S. miltiorrhiza volatile oil and dandelion extract, the cumulative permeability of dandelion extract was greater than when acting alone, and the volatile oil of S. miltiorrhiza promoted the transdermal absorption of dandelion extract. The results showed that the complex of S. miltiorrhiza volatile oil and dandelion extract had synergistic antioxidant and antibacterial effects, no obvious cytotoxicity, better skin permeability, and could be used as a natural active substance in food, cosmetics and other fields.
HUANG Wen-rui , TANG Chao-fan , TAO Yu-feng , HAN Juan , WU Jiacong , WANG Yun
2022, 39(3).
Abstract:The green deep eutectic solvents(DESs) synthesized by choline chloride(ChCl) were applied to extract the total flavonoids, total quercetin and quercetin from Chrysanthemum indicum L.. Firstly, four kinds of DESs with excellent performance were synthesized and their physical properties were characterized. Secondly, urea-choline chloride with the best extraction effect was used as the solvent to optimize several parameters affecting the extraction amount. The extraction conditions were as follows: water content of 30%, extraction time of 45 min, solid-liquid ratio of 1:50 g/mL, extraction temperature of 60 ℃. At this time, the extraction yields of total flavonoids, total quercetin and quercetin were 72.32 mg/g, 12.97 mg/g and 10.06 mg/g, respectively, which were better than traditional organic solvents. Finally, the SEM and XRD results showed that the crystal structure of the Chrysanthemum indicum L. did not change significantly during the extraction process. DESs can dissolve the lignin on the surface of Chrysanthemum indicum L., which makes it have stronger cell-breaking effect and leads to easier dissolution of flavonoids.
WEI Xue-ling , ZOU Xiang-yu , BAO Wei-wei , AI Tao-tao , LI Wen-hu , Jiang Peng
2022, 39(3).
Abstract:Transition metal compounds, particularly layered double hydroxides (LDH), are considered as the most promising electrocatalysts owing to their unique two-dimensional layer structures and tunable components. CoNi-LDH was constructed from cobalt nitrate hexahydrate, nickel nitrate hexahydrate, urea and ammonium fluoride by hydrothermal method. CoNi-LDH was etched in sodium nitrate and ferric chloride trihydrate solution at 100 ℃ by fast interface engineering to form FeOOH/CoNi-LDH. SEM, XPS and TEM were used to characterize the morphology and phase of FeOOH/CoNiLDH, and the electrocatalytic oxygen evolution performance was tested in 1 mol/LKOH electrolyte. The results showed that the rough heterogeneous nanorods of FeOOH@CoNi-LDH greatly increase the number of active sites and the conversion rate of active substances. When the current density was 100 mA/cm2, the over potential was 291 mV, meanwhile, Tafel slope was 48 mV/dec. The electrode had good cycle stability and at least 100 h durability.
WU Qi , ZOU Lianghua , HU Xueyi , XIA Yongmei
2022, 39(3).
Abstract:Four analogues of cannabidiol (CBD) were synthesized from Friedel-Crafts alkylation with α-phellandrene as alkylation reagent, phloroglucinol or alkylphenol as the nucleophilic receptor under the catalysis of ferric chloride. Meanwhile, other eight cannabinol analogues were synthesized by O-alkylation with alkyl bromide using 8,9-dihydrocannabidiol (H2CBD) and 2,2,8,9-tetrahydrocannabinol (2,2,8,9-THC). The antioxidant activities of CBD and its analogues were characterized by DPPH, ABTS free radical scavenging ability and inhibition on lipid oxidation, and their antibacterial activities against four bacteria were studied. The relationship between the structure of the analogues and the properties was investigated. The reduction of phenolic hydroxyl groups on the benzene ring resulted in weakening of the antibacterial and antioxidant activity. The results showed that analog I, due to its polyphenolic structure, performed better antioxidant capacity than CBD did, and its EC50 values of DPPH and ABTS free radical scavenging were 23.8% and 25.1% of that of CBD, respectively; which is even slightly lower than that of VC. Analogues I presented good antibacterial activity against the assayed bacteria with the minimum antibacterial concentration (MIC) lower than 100 μg/mL; whereas other analogs exhibited no antibacterial activity against the above bacteria at the assayed concentrations. Overall, phenolic hydroxyl group maybe essential for antioxidant and antibacterial activity of CBD analogues.
2022, 39(3).
Abstract:Nicofluprole is a novel fluorinated phenylpyrazole nicotinamide insecticide successfully developed and marketed by Bayer. The mechanism of action has not been reported yet. The synthetic method for Nicofluprole was explored, and its insecticidal activities were tested. Nicofluprole was prepared with aniline and 5-bromo-2-chloronicotinic acid as starting materials, and its structure was confirmed by 1H NMR, 13C NMR和MS compared with the literature hydrogen spectrum data of Nicofluprole. This synthetic route has a higher total yield and lower cost. Nicofluprole has higher insecticidal activity against the lepidoptera pests (Plutella xylostella and armyworm), the homoptera pest (Myzus persicae) and the Acarina pest (Tetranychus cinnabarinus). The lethal rate of Nicofluprole can reach 100% against Plutella xylostella at 2.5 mg/L, 100% against armyworm at a concentration of 10 mg/L and 71% against Tetranychus cinnabarinus at 5 mg/L. Nicofluprole also had a good control effect on Myzus persicae at a concentration of 10 mg/L.
2022, 39(3).
Abstract:Lignite as a low-grade coal resource utilization rate is not high, but lignite has humic acid composition. From the view of low-rank coal resources reuse, humic acid extracted from lignite can be used as raw material of chemical fertilizer and extracted residue can be used as carbon source to synthesize MnS@C composite with MnS nanoparticles. When applied to the anode material of lithium-ion batteries (LiBs), The specific surface area and pore volume of MnS@C composite are 117.19m2/g and 0.044mL/g, respectively and it shows high specific capacity of 830 mAh/g after 200 cycles at 0.1 A/g, excellent rate capability with capacity values of 644, 522, 427, 399, 373 and 348 mAh/g at current desities of 0.2, 0.4 0.8 1.0 1.2 and 1.6 A/g, respectively, remarkable cycle performance of maintaining about 99% after 200 cycles at 0.1 A/g. The exceptional electrochemical performance of MnS@C is due to the existence of carbon matrix, which can not only buffer the volume expansion of MnS nanoparticles in the process of lithiation/delithiation, but also show the great potential for high-performance LiBs, and make a great contribution to the high-value utilization of lignite.
LIU Tian-yi , LONG Jia-peng , LIANG Bing
2022, 39(3).
Abstract:A silicon-containing compatilizer (K-ADR) was synthesized from chain extender (ADR 4370s) and silane coupling agent (KH550) and applied in talc reinforced PTAT matrix composites. The structure of K-ADR was characterized by FTIR, 1HNMR and TGA, and the effects of solvent type. The PBAT/K-ADR/talc composite was prepared by melting blending with a torque rheometer, and the rheological properties, mechanical properties, microstructure of impact section and element distribution of the composite were characterized. The results showed that the best performance was obtained when the K-ADR contentwas6‰. The tensile strength, impact strength and bending modulus of this component are 19.11MPa, 67.68KJ/m2 and 378.36MPa. Compared with pure PBAT, the properties of the composites are improved by 5.3%, 110.7% and 346.7%, respectively. The water vapor transmittance coefficient (WVP) and oxygen transmittance coefficient (OP) of the composite films are 5.70*10-12g·cm/cm2·s and 3.17*10-13cm3·cm/(cm2·s·Pa), which are reduced to 2.1% and 1.0% of those of the pure PBAT samples, respectively.
2022, 39(3):0-0.
Abstract:A novel benzoxazine monomer, using polydatin as phenol source and furfurylamine as amine source (PDA-fa) was successfully synthesized. 1H nuclear magnetic resonance spectroscopy (1H NMR) and Fourier transform infrared spectroscopy (FT-IR) were carried out to confirm the structure of PDA-fa. The curing behaviors were investigated by differential scanning calorimetry (DSC) and in situ FT-I. PDA-fa exhibits an endothermic peak at 183 ℃. The C=C bond and furan structure can be crosslinked during the ring-opening polymerization of oxazine ring. Additionally, the thermal property of poly(PDA-fa) and the surface property of benzoxazine membrane were further investigated. The glass transfer temperature of poly(PDA-fa) is 230℃(DSC) and 231 ℃(TMA). The value of Td5 and Td10 are 306 and 338 ℃, respectively, and a char yield at 800 ℃ is as high as 61%. The surface free energy of the completely cured benzoxazine membrane is calculated to be 43.6 mJ/m2.
LI Shuai , XIAO Laihui , WANG Yigang , CHEN Jie , NIE Xiaoan
2022, 39(3).
Abstract:In this study, the waterborne hyperbranched epoxy resin (HE-32) is synthesized using glycerol triglycidyl ether and diethylene glycol , the waterborne polyamide (PA236) is synthesized using adipic acid and diethylene triamine, then graft PA236 onto HE-32 to get modified waterborne polyamide PA236G, finally, 2~4% waterborne curing agent is added to obtain the creping adhesive CA-21. The analysis of HE-32, PA236 and PA236G using 1H-NMR, 13C-NMR, FTIR and GPC confirmed that the polymer was successfully synthesized and PA236 was successfully grafted onto HE-32; The thermal properties of the three products have been tested by thermogravimetric analysis, and the thermal stability of PA236G has been greatly improved. Finally, the film performance and mechanical properties of CA-21 were tested. The results showed that the average shear strength of CA-21 can reach 0.17 MPa, and the adhesion to the substrate can reach 171.16 N, which proved it has the potential to be used as a viscous agent.
ZUO Tian-peng , CHENG Xiao-wei , WU-Hao , LIU-Peng , ZHANG Chun-mei , LIU Kai-qiang , HUANG-Sheng
2022, 39(3):0-0.
Abstract:A type of layered composite retarder, boric acid root intercalated hydrotalcite(Mg/Al-BA-LDH)was synthesized by ion exchange reaction between boric acid and magnesium aluminum lamellar dihydroxides(Mg/Al-CO3-LDH)which was prepared by coprecipitation method ,in order to well overcome the problems of abnormal cementing slurry and the strength of the cement paste developing slowly at the top of the long-sealing section cementing of the commonly used retarders.The structure was characterized by XRD、FTIR and SEM,results show that the prepared Mg/Al-BA-LDH has a good crystallite, and the interlayer spacing is 0.92nm at pH=4.5.At the same time,the comprehensive performance of the cement slurry system with Mg/Al-BA-LDH was evaluated.The experimental results show that the retarder can effectively adjust the thickening time of the cement slurry at 90 ℃~170℃,and the thickening curve is stable, indicating right-angle thickening.The compressive strength of cement stone containing Mg/Al-BA-LDH was greater than 14MPa at low temperature for 24h, and the strength can reach 33.97mpa after 7d when the content is 0.5%( Dosage is based on cement quality).After curing under different temperature difference conditions, the compressive strength of the top cement stone develops normally and meets the construction requirements, which could be applied to long sealing and large temperature range cementing operation. The filling of hydrotalcum material and the crystal effect played a leading role in the process of cement hydration, thus promoting cement hydration and effectively alleviating the slurry compressive strength decline caused by retarding effect.
CHEN Hong-yu , yuqianqian , yangjianjun
2022, 39(3):0-0.
Abstract:Sulfonated polyaniline (Spani) was synthesized from chlorosulfonic acid, aniline and ammonium persulfate. Go was reduced by polyethyleneimine (PEI) to synthesize PG composites. SPG composites were prepared by combining Spani with PG using the active site on go. Waterborne epoxy anticorrosive coatings were prepared by blending SPG with waterborne epoxy resin. The structure of SPG composites was characterized by FT-IR and XRD. The results showed that the amino group on Pei successfully combined with go, and Spani successfully increased the layer spacing of PG; The corrosion resistance of waterborne epoxy coating was measured by salt spray and electrochemical experiments, and the physical properties of the coating were analyzed. The results show that when 2wt% SPG is added (the amount is based on the total mass of epoxy resin and curing agent, the same below), the waterborne epoxy anticorrosive coating has the best corrosion resistance, and the corrosion efficiency can reach 99.19%. Compared with pure EP, the corrosion current density decreases from1080 nA?cm-2 to 307 nA?cm-2, and the corrosion voltage increases from -0.840mV to -0.347mV
2022, 39(3).
Abstract:An One-pot reaction based on Algar-Flynn-Oyamada (AFO) reaction for synthesis flavonols was optimizated. Hydroxyacetophenone and the corresponding Benzaldehyde were treated as raw materials, the molar ratio of reactants, alkali, reaction solvent, reaction time, and reaction temperature were optimized through single factor test, the factors and levels, which have a greater impact on the yield of flavonols, had been screened out. On this basis, the response surface design was used for establishing a mathematical model, which could predict the flavonols’ One Pot Synthesis Process, and the mothed details were: n(corresponding benzaldehyde):n(hydroxyacetophenone):n(NaOH)=1:1.2:10.2, ethanol as solvent (0.0982 mol?L-1), reflux at 80℃ for 3h, after cooling, 35% H2O2 (0.1253 mol?L-1) and H2O (0.1253 mol?L-1) were added(the reactant aldehyde as standard), and then The reaction continued for another 3 hours at 25℃. It had been verified that the simplified synthesis process had greatly stability and extremely simply, which could effectively increase the yield of flavonols about 8.41%~23.89% and provide a method basis for the convenient synthesis of flavonols.
2022, 39(3):0-0.
Abstract:In the presence of dimethylallyl diphosphate, FgaPT2 was used to catalyze the synthesis of C-4 prenylated indole diketopiperazine. The synthesized product has been tested for anti-tumor, anti-bacterial, anti-fungal, and antioxidant activity. For the product with the highest biological activity, the feasibility of site-directed mutagenesis to increase the yield of enzyme synthesis was studied. The results showed that FgaPT2 enzyme catalyzed the synthesis of 7 C4-prenylated indole diketopiperazines, and FgaPT2 has a certain selectivity for substrates. C4-Prenylation significantly improves the biological activity of indoledikepiperazine, especially the prenylation product 6b. Site-directed mutagenesis of Arg244 showed that 52.6% of FgaPT2 mutants increased the synthesis yield of 6b. Kinetic parameters verify the interaction between 6a and mutant FgaPT2, which can increase the conversion rate of isoprenyl groups.
YANG Feng-ke , YUAN Shi-shen , ZHANG Yong-fu , NIU Peng-cheng , RU Yu-qing , GAO Wei-wei
2022, 39(3):0-0.
Abstract:A green synthesis method of p-chlorobenzaldehyde, an important fine chemical intermediate, was reported. p-Chlorobenzaldehyde was achieved through the catalytic oxidation of p-chlorobenzyl alcohol. Hydrogen peroxide and copper salt were used as oxidant and catalyst, respectively. The effects of the type and amount of copper salt, the amount of hydrogen peroxide, the dropping time and the reaction temperature on the yield of p-chlorobenzaldehyde were investigated. The optimum reaction conditions were obtained as follows: copper acetate was used as the catalyst, n[Cu(OAc)2] : n(p-chlorobenzyl alcohol) : n(H2O2) = 1 : 100 : 300, water as the solvent, reaction temperature and time were 96 ℃ and 2 h, respectively. The conversion rate was 93.1%, the selectivity for generating p-chlorobenzaldehyde was 97.7%, and the yield was up to 91.0%. The catalyst-containing water phase was recycled, and the yield could still reach above 85% after 5 cycles. The method has the advantages of green and environmentally friendly oxidant, recyclable catalyst and solvent, no waste acid production, which is suitable for industrial production.