• img
  • Current Issue
  • Next Issue
  • Back Issue
  • Special Issue

以实际刊发为准

    Select All
    Display Method:: |
    Volume 39,  2022 Issue 12
      Catalysis,separation and purification technology
    • Li Ming-yue, Li Huipeng

      2022,39(12), DOI:

      Abstract:

      Bi12TiO20 photocatalyst doped with Fe element was prepared by hydrothermal method, and the structure of Bi12TiO20 was modified by X-ray diffraction (XRD), ultraviolet-visible diffuse reflectance (UV-Vis DRS), scanning electron microscope (SEM), nitrogen adsorption and desorption, X-ray photoelectron spectroscopy (XPS) to characterize the morphology, microstructure and chemical valence state of the photocatalyst, and apply it to the photocatalytic degradation of methylthionine chloride (MB).The experimental results show that When the doping amount of Fe is 5%,the catalyst dosage is 0.05g, and the degradation rate of 10mg/L MB reaches 98.949%. After Fe doping, the Fe-Bi12TiO20 photocatalyst forms a new hybrid energy level, and the absorption band boundary is red-shifted, thereby improving the photocatalytic activity of the catalyst. Fe is a crystal doped in Bi12TiO20 with +3 and +2 valences middle.Fe-Bi12TiO20 photocatalyst, after repeated use for 5 times, the degradation rate of MB can still reach more than 88%, and it has excellent photocatalytic stability performance.Both h+ and·O2-are the main active species during photocatalytic degradation.This paper provides a reference for the doping modification of Bi12TiO20 materials.

    • Biological engineering
    • Guo Shang, xulina, Li Yanting, Guo Weiwei, Guo Xiaofei, Hong Shasha

      2022,39(12), DOI:

      Abstract:

      Cordyceps militaris is rich in protein, polysaccharide, cordycepin and other active components, with anti-cancer and anti-oxidation functions. In order to improve the economic value of Cordyceps militaris, the protein was extracted from its fruiting body by alkali solution and acid precipitation method, and the extraction conditions were optimized by orthogonal test. The polypeptide was obtained by digesting those protein with protein complex enzyme. And the antimicrobial and anticancer activities of those polypeptides were evaluated by measuring inhibitory zone and cytotoxicity. The results showed that the optimal extraction conditions of protein were as follows: pH 8.5, solid-liquid ratio 1:28, extraction time 210 min, extraction three times, the highest protein yield was 45.06%. The optimum enzymatic hydrolysis process of Cordyceps militaris polypeptide solution was as follows: the ratio of alkaline protease to papain was 4:3; The optimum temperature of enzymolysis was 55℃, pH 7.2, the enzyme dosage was 7000 U/mL, the enzymolysis time was 210 min, and the highest yield of peptide was 16.73%. Under these conditions, the polypeptides prepared from Cordyceps militaris (< 3.0×103 Da) showed good antibacterial activity against Escherichia coli, Bacillus subtilis and Staphylococcus aureus, with inhibitory zones of (12.08 ± 0.22), (6.67 ± 0.12) and (10.32 ± 0.23) mm, respectively. The results showed that the SAO-S (IC50 = 0.49 mg/L) and T24 (IC50 = 0.23 mg/L) were significantly inhibited by Cordyceps militaris polypeptide.

    • Drug and cosmetic materials
    • LIU Bo, GAO Hui, ZHANG Meng-dan, YANG Ping, SONG Xin-jian

      2022,39(12), DOI:

      Abstract:

      2-Amino-4,5-dimethylthiophene-3-carbonitrile was first obtained through the modified Gewald reaction with butan-2-one, malononitrile and elemental sulfur as raw materials. Then sixteen fluorinated thieno[2,3-d]pyrimidine derivatives IIIa~IIIp were synthesized by the substitution reaction of substituted benzylamines with the key intermediate 4-chloro-5,6-dimethyl-2-(trifluoromethyl)thieno[2,3-d]pyrimidine, which was prepared directly from 2-amino-4,5-dimethylthiophene-3-carbonitrile and trifluoroacetic acid in the presence of phosphorous oxychloride via one-pot procedure. The structures of these target compounds were confirmed by 1HNMR, 13CNMR, IR, MS and elemental analysis. The crystal structure of compound IIIa was determined by X-ray single-crystal diffraction. The bioassay results suggest that the target compounds IIIa, IIIc and IIIf exhibit good in vitro antitumor activity. The target compounds IIIk~IIIp with an electron-donating substituent in the benzene ring display poor antitumor activity, but the antitumor activity is better (e.g. IIIc, IIIf and IIIi) when the meta-position of the benzene ring was substituted with an electron-withdrawing group, especially a fluorine atom. The half inhibitory concentration (IC50) values of compound IIIa against MCF-7 and HepG2 cells were 2.01 μmol/L and 2.44 μmol/L, respectively, while the IC50 values of IIIc against MCF-7 and HepG2 cells were 1.44 μmol/L and 1.47 μmol/L, respectively. Both of them indicate much better antitumor activity than the control group Gefitinib.

    • Review and monographs
    • YANG Wenbing, ZHAO Huahua, SONG Huanling, YANG Jian, ZHAO Jun, YAN Liang, CHEN Li-qun, CHOU Lingjun

      2022,39(12), DOI:

      Abstract:

      Propionic acid and ethyl propionate are important chemical products and intermediates in organic synthesis. Due to the abundant ethanol resources, which could be obtained by the non-petroleum synthesis in China, the synthesis of propionate and ethyl propionate from ethanol has been extensively studied. However, the homogeneous carbonylation of ethanol encounters some problems, such as low yield, harsh reaction conditions and difficulty in separating the product from the catalyst. At present, the research on ethanol carbonylation mainly focuses on heterogeneous catalyst, includes noble metal catalyst and non-noble metal catalyst. In this paper, the research progress of the two types of catalysts is introduced in detail. The reaction mechanism of the two types of catalysts, the effects of promoters, supports and process parameters on the activity of two catalysts are emphatically described. The advantages and disadvantages of the different catalysts are pointed out and the application status of the catalysts is reviewed. Finally, the synthesis of propionic acid and ethyl propionate by the heterogeneous carbonylation of ethanol is prospected. Thus, this review could provide ideas for the design and development of catalysts with high activity and stability.

    • YAN Yu-ting, WANG Qian, ZHOU Fang-fang, Huang Yue

      2022,39(12), DOI:

      Abstract:

      Antibiotics, as animal therapeutic agents and growth promoters, are widely used in agriculture, animal husbandry and aquatic product breeding, resulting in excessive antibiotic residues in animal and plant food, which seriously threaten human health. Therefore, detection of antibiotic residues in food is of great significance. However, the existing detection methods of antibiotic residues, such as microbiological assay, enzyme-linked immunoassay, liquid chromatography-mass spectrometry, capillary electrophoresis, usually have the disadvantages of time consuming, complex operation and high cost. As a new technology, biosensor has the advantages of being rapid and simple, high sensitivity, good selectivity and low cost, indicating great potential in the field of antibiotic residue detection. Nucleic acid probe, as a new tool for biological analysis, has been widely used in the development of biosensors. The introduction of nucleic acid probe to the biosensing detection of antibiotic residues opens up a new way for the efficient detection of antibiotic residues. The application of nucleic acid probe in the biosensing detection of antibiotic residue is reviewed from the aspects of electrochemical biosensor, fluorescence biosensor, colorimetric biosensor and other common biosensors, and the future development prospect of this field is also prospected.

    • ZHANG Qian-jie, Wang Ping-li, ZHANG Dong-mei, Jiang Wen, ZHANG Wan-ping

      2022,39(12), DOI:

      Abstract:

      Popularity of green and sustainable development among people encourages them to pursue safe, harmless and side-effect free products. No toxicity and irritation, coupled with superior biodegradability and bio-compatibility, are attributable for people’s growing attention on biomass particle emulsifier. This paper reviews the research progress of Pickering emulsions stabilized with naturally derived solid particles, including polysaccharide-based particles such as starch, chitosan, cellulose, cyclodextrin, etc., and protein-based particles such as whey protein, soy protein, and zein. etc., and other types of particles such as flavonoids, polyphenols, natural pearl powder, etc. In addition, the paper reviews the application of Pickering emulsions stabilized with natural solid particles in cosmetics, including enhancing emulsion system stability, loading bio-active ingredients and synergistic effect. Finally, the application prospect of Pickering emulsions stabilized with naturally derived solid particles is prospected.

    • Lan Tianyu, CONG Shanshan, Zhang Na, Wang Jun

      2022,39(12), DOI:

      Abstract:

      Dendritic transition metal catalysts are transition metal active centers loaded on dendritic macromolecular. Therefore, these catalysts not only have the unique artistic structure of dendrimers, but also have the functional performance of transition metal complexes, so that they can work together, and have the characteristics of homogeneous and heterogeneous catalytic systems, It has high catalytic activity and good catalytic stability in catalytic olefin polymerization. It has attracted much attention in recent years, and catalytic ethylene polymerization is one of the research hotspots. This paper is classified by their transition metal active center and summarizes the progress of dendritic transition metal catalysts in this ethylene polymerization at home and abroad in recent years, expounds the causes of various dendritic effects, and looks forward to the development prospect of dendritic transition metal catalysts for ethylene polymerization

    • LIU Tao, RUI Ting-wei, ZHU Jin-qi, SHEN Dong, YOU Yi-wen

      2022,39(12), DOI:

      Abstract:

      Excess phosphorus discharged into natural water will lead to eutrophication. Adsorption method has been extensively studied due to its economy, convenience, and efficiency. Ordered porous materials are characterized by regular pores, large surface area and pore volume, which can improve the dispersion of active species, further effectively enhancing the phosphate adsorption efficiency. The recent progress in the application of sorbents based on ordered porous materials to phosphate removal from water is summarized, including ordered porous carbon materials, ordered porous silicon materials and metal organic frameworks. The phosphate adsorption performance, main adsorption mechanism, adsorption influence factor, recovery and utilization of adsorbents based on ordered porous materials are discussed. The problems of phosphate adsorption by adsorbents based on ordered porous materials are summarized, and the future research direction and application prospect are also proposed.

    • GUAN Huanan, XING Ke, ZHANG Yue, SONG Yan, LIU Shuping

      2022,39(12), DOI:

      Abstract:

      Polyoxometalates (POMs) had a diverse structure and composition and unique performance characteristics. It was considered as a promising class of anionic materials in electrochemical biosensors and many other fields. POMs had defects such as poor electrical conductivity and low specific surface area. The preparation of POMs into polyoxometalate-based complexes with nanomaterials such as carbon-based materials, noble metals and metal organic frameworks could improve the defects of POMs and and enhance its electrocatalytic properties. Polyoxometalate-based complexes will also expand the range of applications in the field of electrochemical biosensors. This article reviewed the types and preparation methods of electrochemical biosensors with polyoxometalate-based complexes. As well as its research progress in the field of food analysis, and the future challenges and application prospects of this complexes were discussed.

    • Functional materials
    • XU Yu-qin, Zhang Yiqian, YANG Jian-jun, WU Qing-yun, WU Ming-yuan, ZHANG Jian-an, LIU Jiu-yi

      2022,39(12), DOI:

      Abstract:

      Using polyvinyl alcohol (PVA), graphene oxide (GO) and silver nitrate as raw materials, a series of reduced graphene oxide (rGO) - supported nano silver / polyvinyl alcohol antibacterial hydrogels (rGO AgNPs / PVA) (PGA) with different mass fractions of AgNPs were prepared by physical crosslinking method (freezing thawing method) without adding initiator and crosslinker. The structure and morphology of the hydrogel were characterized by FTIR and SEM, and its mechanical and biological properties were tested by tensile test and biological experiment. The results showed that the addition of reduced graphene oxide enhanced the mechanical strength of polyvinyl alcohol (PVA) hydrogel, the elongation at break of rGO AgNPs / PVA antibacterial hydrogel was about 60% higher than that of PVA hydrogel, and the tensile strain could reach 125%. Rheological tests showed that the storage modulus (G') and loss modulus (G') of PVA hydrogel were lower than those of rGO AgNPs / PVA hydrogel; rGO and nano silver (AgNPS) are synergistic antibacterial. The antibacterial band widths of PGA-2, PGA-3, PGA-4 and PGA-5 against Escherichia coli and Staphylococcus aureus are 0.5~4.5 mm and 0.5~5.5 mm respectively; SEM test showed that compared with PVA hydrogel, the pores of rGO agnps/pva hydrogel increased, rGO formed network structure through π - π action, and rGO agnps/pva hydrogel showed porous interconnected microstructure.

    • YUAN Chengke, FENG Yongqiang, LIU Wanwan, FENG Weihang, CHEN Junsheng, WANG Hai, Zhang Weibing, Dong Wenwei, CAO Liyun, HUANG Jianfeng

      2022,39(12), DOI:

      Abstract:

      Polyimide is widely concerned in the field of engineering polymer materials. The development of a new type of polyimide film material with high temperature resistance and good hydrophobicity is an important breakthrough to promote the engineering application of high-performance polymer materials in electric vehicles and other high-tech fields. In this work, the composite polyimide film was synthesized by a two-step method, and the polyimide film was modified by nano-ZrO2 powder. The structure and morphology of the composite film were characterized by means of XRD, SEM, energy spectrum, infrared spectroscopy, etc. and the thermal stability, hydrophobicity and tensile strength of the composite film were tested. The results showed that the addition of nano-ZrO2 enhanced the interaction between polyimide molecular chains, and the heat resistance of polyimide was significantly improved. The decomposition temperature was increased by 20 ℃, the water contact Angle was increased by 60%, and the hydrophobicity was improved. This work provides a new idea for the development of novel high-performance polyimide polymer materials.

    • LIU Jing, YANG Lubing, LI Chen, CHEN Yongkai, ZHANG Zhen, WEI Wenhua

      2022,39(12), DOI:

      Abstract:

      Monolayer tungsten trioxide nanosheets (ML-WO3) were prepared via the space-confined strategy and then compounded with TiO2 to obtain ML-WO3/TiO2 nanomaterials, which were used for the photocatalytic degradation of rhodamine B under simulated solar light. The compositional structure and optical features of ML-WO3/TiO2 were characterized by means of SEM, TEM, HRTEM, XRD, UV-Vis and PL. The results showed that the ML-WO3/TiO2 overcame the defect of large band gap of pure TiO2 and exhibited stronger absorption performance than ML-WO3 and TiO2 in the full wavelength solar light, and there was a remarkable synergistic relationship between ML-WO3 and TiO2. The active species capture experiments showed that .OH and .O2- free radicals were the main active species for RhB degradation. The Z-scheme heterojunction charge transfer pathway constructed between ML-WO3 and TiO2 can ensure efficient separation and recombination of photogenerated carriers. The photocatalytic activity of the ML-WO3/TiO2 composites could still approach 80% after 5 cycles of experiments, with good photochemical stability. The possible degradation pathway of RhB was speculated by the detection of RhB intermediates by HPLC-MS.

    • YOU Hou-mei, ZHAO Ke-xin, XIE Ying-ying, ZHANG Xiang-kun, ZHU Bao-lin, Tian Weiliang

      2022,39(12), DOI:

      Abstract:

      Based on solid agglomeration or stacking of organic fluorescent dyes, which leads to fluorescence quenching, luminescence, and weakening of stability, the method of exfoliation and supramolecular assembly is used to prepare solid fluorescent ultra-thin film emitters. First, vermiculite nanosheets were prepared by shear exfoliation, and their particle size distribution was controlled at 30-300 nm. Then, vermiculite organic-inorganic vermiculite was obtained by layer-by-layer supramolecular assembly with organic fluorescent dyes (rhodamine 6G and rhodamine B). fluorescent film. It was found by comparative experiments that a uniform luminescent fluorescent film could not be obtained without adding vermiculite nanosheets. The SEM of the vermiculite organic-inorganic fluorescent film shows that the organic fluorescent dyes and vermiculite are evenly distributed, which overcomes the fluorescence quenching of the agglomeration or stacking of the organic fluorescent dyes, and realizes the controllable fluorescence brightness.

    • REN Long-fang, TANG Zheng, HU Yan, QIANG Tao-tao

      2022,39(12), DOI:

      Abstract:

      In order to improve the hydrophobic properties of polyurethane foam (PUF), peanut shell powder (PSP) was firstly modified by hexadecyltrimethoxysilane (HDTMS) to prepare the hydrophobic modified peanut shell powder (H-PSP). The testing results of water contact angle showed that the water contact angle of modified H-PSP was increased from 0° of PSP to 145.2°. Then, PUF loaded with H-PSP composites (H-PSP-PUF-n, n is the mass fraction of H-PSP in polyurethane prepolymer PPU) were prepared by prepolymer method. The structure and properties of H-PSP-PUF-n were characterized and tested. The results showed that the loading of H-PSP on PUF improved the surface roughness and mechanical properties of foams. The optimal loading capacity of H-PSP was optimized to be 10% of the mass of PPU (H-PSP-PUF-10). Compared with PUF, the static water contact angle of H-PSP-PUF-10 reached to 142.4°, which was higher 50.4° than that of PUF. The oil-water separation experiments of dichloromethane, petroleum ether, kerosene, xylene and hexamethylene were carried out. The results showed that the adsorption capacity of H-PSP-PUF-10 for different oils was 7~9 g/g, as well as it had good oil-water selectivity. After 15 cycles of adsorption-desorption, the adsorption capacity of H-PSP-PUF-10 for different oils was about 6.5~8.0 g/g, which had excellent recyclability.

    • YU Yanchao, CHEN Xinyi, BA Xinyu, LI Yanping, LIU Yang, ZENG Yubo

      2022,39(12), DOI:

      Abstract:

      A fluorescent probe NSS of benzothiazole derivatives was synthesized using 2-mercaptobenzothiazole as raw material and the structure was characterized by IR, MS, 1H NMR, 13C NMR. The fluorescence spectroscopy studies demonstrated that the probe NSS showed fast-response, high selectivity and good anti-interference ability towards Zn2+ ion through the significant fluorescence enhancement effect in the DMSO solution. The fluorescence intensity of probe NSS had a good linear relationship with the concentration of Zn2+ (0~11 μmol/L), and the detection limit could reach 19.1 nmol/L. The bingding stoichiometry of probe NSS with Zn2+ was 1:1, which was confirmed by Job's plot analysis and MS. Meanwhile, complex NSS-Zn2+ had obviously fluorescence intensity quenched response to glyphosate while suffering from a slight interference in the presence of other organophosphorus pesticides. The quenching efficiency reached a maximum of 99.4%, and the detection limit of complex NSS-Zn2+ to glyphosate was 16.0 nmol/L (2.68 ng/mL). In addition, probe NSS was succesfully used in the detection of Zn2+ and glyphosate in the actual water samples, the method had potential application in the field of environmental detection.

    • Yuanye, Yangjianjun

      2022,39(12), DOI:

      Abstract:

      The schiff base containing aromatic disulfide bond was successfully synthesized by the reaction of salicylic aldehyde and 2, 2-diaminodiphenyl disulfide ether. The schiff base was reacted with polytetrahydrofuranediol, isophorone diisocyanate,2, 2-dihydroxymethyl butyric acid and 1, 4-butanediol. The characterization of the schiff base and polyurethane film was performed by 1HNMR and FTIR. The results showed that the self-healing waterborne polyurethane with aromatic Schiff base and aromatic disulfide bond was successfully synthesized. The self-healing ability of polyurethane was characterized by scratch test and healing test. The results showed that swPU-2 had the best scratch healing effect and self-healing rate. After 12h healing at room temperature, swPU-2 film's scratch disappeared, and after 24h healing at room temperature, the self-healing rate of polyurethane film could reach 95.8%

    • HUANG Yi-ran, CHEN Xiao-ting, PAN Nan, WANG Lian-zhu, LIU Zhi-yu, ZHOU Chang-yi

      2022,39(12), DOI:

      Abstract:

      The Zein/chitosan (CS) composite film with high content of Zein was prepared by casting method, and the film was blended and modified by composite additives [m(glycerol):m(polyethylene glycol 400)=1:1]. The effects of the additive amount of the composite additives (0, 0.5%, 1.0%, 1.5%, 2.0%, respectively, based on the total solution mass) on the mechanical, optical and thermal properties of the film were studied. The morphology and structure of the film were characterized by SEM and FTIR. The results showed that the composite additives could achieve the plasticizing effect by weakening the intermolecular force between Zein and CS, and the comprehensive mechanical properties of the film are improved. With the increase of the additive amount of the composite additives, the elongation at break of the film gradually increased, and the tensile strength decreased and then increased, the WVP increased gradually, the water contact angle decreased gradually, and the hydrophilicity of the film increased. Compared with the film without composite additives, when the concentration of composite additives reached 1.5%, the tensile strength decreased by 27.40%, the breaking elongation increased by 39.87%. The barrier performance decreased, and the WVP increased by 29.10%. Through the observation of SEM and DSC, the compatibility between Zein and CS was improved after adding composite additives, and the surface of the prepared film was more flat and smooth. with high content of Zein, the Zein/CS film has the best performance when the concentration of the composite additive is 1.5%. Adding curcumin to zein/cs composite membrane could effectively improve the oxidation resistance of the film, and with the increase of curcumin content, the proportion of bound water in the film increased, and the mechanical properties of the composite membrane were better than those without curcumin.

    • Surfactants
    • CHEN Shuang, GAO Shengsong, KANG Yaoming, LI Zengxia, TIAN Xiaowen, WANG Mian

      2022,39(12), DOI:

      Abstract:

      The effects of n-butanol content and oil-water ratio on the microemulsion phase behavior of diesel oil and distillate oil at 350~395℃, 395~450℃ and 450~500℃ were investigated using isoctyl polyoxyethylene ether-5 (E1305) as surfactants. The results showed that the phase of microemulsion system changed from Winsor I →Winsor III →Winsor II with the increase of n-butanol content.The optimum solubilizing parameter (SP*) decreases while the optimum alcoholicity (A*) increases with the increase of oil phase distillation temperature. For the system with low contents of N-butanol and E1305, the phase changes from micelle solution type → Winsor-like II → Winsor IV→Winsor I with the increase of oil-water ratio. For the system with lower n-butanol content and higher E1305 content, the phase changes directly from micelle solution to Winsor I microemulsion with the increase of oil-water ratio. For the system with higher n-butanol content, the phase states change from Winsor II →Winsor III →Winsor I with the increase of oil-water ratio. The oil-water ratio required for phase transformation is related to the surfactant content and the distillation temperature of the oil phase.

    • WANG Tong, MA Xiao-jing, SHAO Jun-qian, ZHU Hui-xia, WANG Huai, YAO Ri-sheng

      2022,39(12), DOI:

      Abstract:

      The effects of pretreatment methods of wheat straw on sophorolipids (SLs) fermentation by Starmerella bombicola were investigated, and the fermentation parameters were optimized. Dilute acid pretreatment (DAP), sodium hydroxide pretreatment (SHP) or sulfur trioxide microthermal explosion pretreatment (STMEP) were chosen to pretreat wheat straw to enhance the following enzymatic saccharification. Then, the saccharification liquids were used for SLs fermentation, respectively. Glucose supplement and activated carbon detoxification were used to improve SLs production. The results showed that SHP was the most favorable method for enzymatic saccharification of wheat straw, and the glucose content reached 61.30 g/L, followed by STMEP and DAP, with glucose content of 48.33 g/L and 40.00 g/L, respectively. The total content of inhibitors in STMEP saccharification liquid was the lowest, followed by SHP and DAP. S. bombicola could directly use the above saccharification solution to produce SLs, but the fermentation characteristics were different. Compared to the control chemical synthesis medium, SHP and STMEP saccharification medium were more conducive to acidic sophorolipid (ASL) accumulation, and the yield increased by 74.27% and 92.33% to 100.45 g/L and 110.86 g/L. Glucose addition and activated carbon detoxification could further improve SLs production. For SHP saccharification medium, glucose addition combined with activated carbon detoxification further increased ASL production to 124.49 g/L; For STMEP saccharification medium, lactonic sophorolipid (LSL) production was further increased to 32.02 g/L, which was similar to the LSL fermentation level of chemical synthesis medium. Therefore, wheat straw had potential for SLs production, and different pretreatment methods and fermentation methods can be used to obtain different types of SLs. The present study is benificial to reduce the production cost of SLs and expand its application field.

    • Catalysis,separation and purification technology
    • MA Shou Xiao, Zhu kai

      2022,39(12), DOI:

      Abstract:

      We developed a superheated steam distillation (SSD) strategy for the extraction of Chinese fir essential oil with Chinese fir root cuttings as raw materials. The conditions were listed as follows: feed 350 g, steam flow 650 mL/h, distillation for 4 hours, different extraction temperatures as 130 ± 5 ℃, 160 ± 5 ℃, 190 ± 5 ℃, 220 ± 5 ℃, 250 ± 5 ℃ and 280 ± 5 ℃ respectively. The results showed that the yield of superheated steam was increased 2-4 folds comparing with that of atmospheric steam distillation (SD). The essential oil of Cunninghamia lanceolata has the smell of wood and ointment. However, the compounds with low boiling point in the components of the essential oil decrease with the increase of extraction temperature. Also, acidic compounds were observed in the mixture with acidic smell. On the other hand, increasing the steam temperature led to the decrease of cedanol in essential oil from 49.99% to 25.41%, increase of α-cedrene from 16.61% to 30.14%, and increase of β-cedrene from 4.10% to 11.92%. This SSD strategy could dramatically improve the oil yield from Chinese fir essential oil. Furthermore, variation of the extraction temperature could provide the oil with different chemical components, which can meet the different needs of the product.

    • WANG Jiasheng, ZHANG Ying, YE Hongyang, WANG Wanhui, BAO Ming

      2022,39(12), DOI:

      Abstract:

      Subnano-Pd@SiO2 core shell materials were prepared by a one-pot method in a microemulsion made up of cetyltrimethyl ammonium bromide/n-butanol/cyclohexane with newly prepared Pd(NO3)2 solution as raw material. Pd subnanoclusters with an average size of 0.7 nm are uniformly dispersed in the entire SiO2 nanospheres with a high loading amount of 4% on the basis of the mass of SiO2. The physico-chemical properties of the Subnano-Pd@SiO2 were characterized by TEM, XRD, XPS, and N2 adsorption-desorption. The catalytic performances of Subnano-Pd@SiO2 for the hydrogenation reaction of aromatic nitro compounds were investigated. The results showed a 99.5% yield of aniline was achieved through the hydrogenation of nitrobenzene under mild reaction conditions of 50 ℃ and 1.0 MPa H2 for 4 h. Meanwhile, Subnano-Pd@SiO2 was efficient for the hydrogenation of various aromatic nitro compounds to give high yields (98.5%~100%) of arylamines. The activity of Subnano-Pd@SiO2 did not decrease significantly even after being recycled for 4 times.

    • LI feng, MAO haili, XU ping, ZENG chenglu

      2022,39(12), DOI:

      Abstract:

      Lignin was isolated from Camellia oleifera shell by lactic acid-based deep eutectic solvent (DES). The structure, thermal stability and antioxidant activity of lignin samples were investigated. The results showed that TEBAC/LA and Bet/LA DES exhibited excellent capability of solubilizing lignin from biomass. The yield of lignin was 77.87% and 59.49% after pretreatment at 120 ℃ for 5 h, respectively. UV and FTIR analyses show that the benzene ring structure of lignin remains complete and with syringl and guaiacyl units. Compared to TEBAC/LA, the lignin samples extracted by Bet/LA presented low relative molecular mass, low polydispersity index and homogeneous structure. The weight loss rate, weight loss temperature and pyrolysis product of the two lignin are different, indicating that there are significant differences in the thermal stability of different lignin. Moreover, the two lignin samples showed distinct antioxidant activity. The capability of Bet/LA sample to scavenge DPPH radical were up to 84.57%.

    • LIANG Hui, LI Changbo, ZHAO Guozheng, WANG Shuo, XU Hongzhu, SUN Zikai

      2022,39(12), DOI:

      Abstract:

      A series of CeO2/g-C3N4 composite catalytic materials were prepared by microwave-assisted double template method and soft template method, and the materials were characterized by XRD, N2 adsorption-desorption, XPS, SEM and TEM, and their wet catalytic properties were investigated. The results showed that the D-CeO2/g-C3N4 composites prepared by the double-template method exhibit the characteristics of cubic-phase CeO2 and laminated g-C3N4, with large specific surface area and pore size, which are mesoporous structures and the presence of Ce3+ and Ce4+ on the surface, which are favorable to the formation of oxygen vacancies. The D-CeO2/g-C3N4(7.5) sample obtained after adding 1 g of block copolymer F127, using anhydrous ethanol solution as the solvent and adjusting the mixture to be alkaline, and microwave radiation reaction for 120 min had a complete and homogeneous structure with the best morphological characteristics. The COD removal rate of 100 mg/L phenol solution could reach more than 80% when the reaction temperature was controlled at 75 ℃, D-CeO2/g-C3N4(7.5) was injected at 0.7 g, H2O2 was injected at 0.5 mL, and the initial pH was 5. The D-CeO2/g-C3N4(7.5) composite catalytic material could still achieve more than 60% catalytic degradation after five times of use.

    • Drug and cosmetic materials
    • Zhang Xiangyang, Wang Feifei, Tang Yucai, Shen Youming, Chen Jun

      2022,39(12), DOI:

      Abstract:

      For efficiently constructing functionalized β-aryl-δ-amino acid derivatives, starting from easily prepared 5-phthalimide-2-pentenoic acid methyl ester and arylboric acids as raw materials, nine kinds of 5-phthalimide-3-arylvalerate methyl ester were obtained via a [Rh(COD)Cl]2 catalyzed Michael reaction. And the yields were more than 95%. The obtained compounds were confirmed by 1HNMR, 13CNMR and HR-MS, respectively. Moreover, the optimum reaction conditions for synthesis of 5-phthalimide-3-arylvalerate methyl ester were as follows: methyl 5-phthalimide-2-pentenoate (0.2 mmol), arylboric acid (0.4 mmol), potassium hydroxide aqueous solution (0.1 mL, 1.0 mol/L), [Rh(COD)Cl]2 (0.005 mmol), 1,4-dioxane (1.0 ml) as solvent,reaction time of 10 hours,at the temperature 100℃. In addition, 5-phthalimide-3-p-chlorophenylvalerate methyl ester can be used for the rapid preparation of the active molecules of homobaclofen hydrochloride.

    • YAO Yongbo, ZHOU Zhijun, SHENTU Baoqing, ZHANG Junfeng, XU Huawei, ZHU Linlin

      2022,39(12), DOI:

      Abstract:

      In order to study the effect of mixing condition on the thermo-sensitivity of chitosan/ sodium β-glycerophosphate (β-GP) solutions. The β-GP solution (50 wt%) was added dropwise in the chitosan solution(2 wt%), and the viscoelastic properties of the solutions were studied by off-line rheology. It is found that the system has thermal induced sol - gel transition character when the volume ratio of chitosan solution/β-GP solution is 8/2. When more β-GP solution was added, the sol-gel transition temperatures of the chitosan/β-GP solutions are similar, but the gel structure loose. Temperature is the important influence factor for the chitosan/β-GP solution. The solution is stable at the temperature of 4 °C and forms weak gel at 25 °C after a certain time. When the temperature is above 30 °C, sol-gel transition occurs quickly.

    • Ying Wang, Lin Li, Jing Hu

      2022,39(12), DOI:

      Abstract:

      When pure essential oil used as antibacterial agents, the dosage was relatively large, the aroma was monotonous and strong, and it was easy to cause sensory discomfort or allergy. In order to solve the problems, the minimum antimicrobial concentration (MIC) of 13 kinds of essential oils was determined. Meantime, the checkerboard dilution method, inhibition zone method and sensory evaluation were used to optimal combination of compound essential oils (CEOs) based on litsea cubeba. Furthermore, the antibacterial mechanism of compound essential oil against E.coli was evaluated. The results showed that litsea cubeba and cinnamon compound essential oil (V:V=2:1) with pleasant and comfortable aroma exhibited excellent synergistic antibacterial activity against E.coli and S.aureus, and the inhibition zone diameters were (21.12±0.17) mm and (40.26±0.61) mm, respectively. Compared with single litsea cubeba essential oil and cinnamon essential oil, the compound essential oils have a more obvious inhibitory effect against E. coli. Meanwhile, the relative conductivity and bacterial cellular content (140% and 20% higher than that of litsea cubeba essential oil and cinnamon essential oil) was increased significantly, which further confirmed the destruction towards bacteria membrane and the leakage of its contents.

    • YU Chuan-ming, OU Jia-yu, DENG Cui-er, YANG Hui-lin, MAI Min-min, QIU Xin-ni, TIAN Li-fen, LI Yong, CHEN Hong

      2022,39(12), DOI:

      Abstract:

      Mesoporous silica nanospheres (MSN) was prepared by hydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) using N-hexadecyltrimethylammonium bromide (CTAB) as a template. The dual drug delivery system (Flu-G-Ins-MSN) was prepared by surface aminopropylation, phenylboration, cyclic adenosine monophosphate (cAMP) loading and gluconate insulin capping. The surface micromorphology, chemical structure, pore structure and surface charge were characterized by TEM, FTIR, XRD, N2 adsoorption-desorption, Zeta-potential analysis. Effect of stirring time on drug loading was examined. The effect of sugar sources, sugar concentration and pH on the release of insulin and cAMP was investigated. The results demonstrated that when the mass concentration of silica spheres was 10 g/L, the concentration of cAMP was 0.1 mmol/L, the drug loading could reach 25.9 μmol/g after stirring for 24 h. The release of glucose-triggered insulin and cAMP was significantly pH-dependent and increased with increasing pH. In the normal human physiological pH 7.4 environment, fructose and glucose exhibited the strongest stimulatory response to drug-loaded particles. Insulin release from 2 mg/mL drug-loaded particles stimulated with 50 mmol/L glucose for 0.5 h was up to 8.35 μmol/L, while the cAMP release for 20 h was up to 75%. The intermittent release experiments showed that glucose enables repeated stimulation of the uncapping for drug-loaded particles, and thus achieving a sustained controlled release of insulin and cAMP.

    • Food and feedstuff chemicals
    • WANG Sinian, WU Juan, LI Kunfang, GAO Jun, CHENG Yu

      2022,39(12), DOI:

      Abstract:

      To reduce the content of whey protein, heat-set mixed gels of potato protein and whey protein were prepared by partially replacing whey protein with potato protein at the ratio of 50/50 by weight. The physical properties of mixed protein gels at different total protein concentrations (40~80 g/L) were investigated by color, textural properties, moisture distribution and rheological properties. The results showed that the lowest gelation concentration of mixed protein gels was 50 g/L. Compared with whey protein gels formed at the lowest gelling concentration of 80 g/L, consumption of whey protein in those gels decreased by 2.20 times. When the protein concentration increased from 50 to 80 g/L, mixed protein gels exhibited yellow color in the appearance. Hardness and elasticity increased by 5.28 times and 5.90%, respectively, but the content of immobilized water decreased by 3.63%. The storage modulus G' showed weak relation with the frequency. Laser confocal microscopy and scanning electron microscopy showed that the mixed protein gels at the concentration of 80 g/L had uniform and compact gel network, small pore size, and clear spherical particle aggregation morphology, thus it had a higher G'. The results of FT-IR showed that the amount of β-folding and β-turn structures account for about 70% of the secondary structures in mixed protein gels. The results of solubility test showed that hydrogen bond and hydrophobic interaction made more contributions to maintaining the structure of mixed protein gels than disulfide bond.

    • Electro-organic chemistry and industry
    • LIU yaopeng, LU youluan, GAO yi, SHI zheng, HUANG wensheng, ZHENG yin

      2022,39(12), DOI:

      Abstract:

      Peanut hull activated pyrolytic carbon (PHAPC) was prepared from discarded peanut hull with NaCl as activator by a simple one-step molten salt pyrolysis method. The structure, morphology and electrochemical properties of the materials were investigated by SEM, TEM, XRD, XPS, BET, CV and EIS. Compared with peanut hull pyrolysis carbon (PHPC) without molten salt activation, PHAPC presented richer pore structure and larger specific surface area, while exhibiting superior conductibility and electrochemical properties. The PHAPC or PHPC was modified on the surface of the glassy carbon electrode (GCE). The electrochemical behavior of rutin at these electrode (PHAPC/GCE or PHPC/GCE) was investigated by DPV. The results showed that the PHAPC/GCE showed higher electrochemical activity towards rutin than the PHPC/GCE. When the concentration of rutin was within the range of 0.05~10.00 μmol/L, the electrochemical current of rutin on PHAPC/GCE showed a linear relationship, with a detection limit of 0.05 μmol/L (S/N=3) and a sensitivity of 83.61 μA?(μmol/L)-1?cm?2. Moreover, the relative standard deviation (RSD) found 3.06% indicating good reproducibility of the electrode. The standard addition method was used for the detection of rutin in rutin tablets with excellent recovery percentages from 96.0%~101.5%.

    • Water treatment technology and environmental protection
    • GUO Jinyan, MA Zhiyuan, YANG Jiaqi, LIAN Jing, NIU Yanyan, YUE Lin, GUO Yankai

      2022,39(12), DOI:

      Abstract:

      Microbial fuel cells (MFC) have the potential of generating electricity and removing nitrogen simultaneously in the treatment of nitrate containing wastewater. It is crucial to find a cathode modified material with low cost and improved performance of generating electricity and removing nitrogen for the commercial application of MFC in the field of wastewater treatment. Cuprous oxide/reduced graphene oxide (Cu2O/rGO) composite which has the advantages of excellent electrochemical properties, hold a wide application prospect in replace of Pt-based material for improving performance of microbial fuel cells (MFCs). In this study, material characterization and oxygen reduction property were conducted to analyze the synthesis of Cu2O/rGO composite materials after synthesis by reduction method. The electrochemical performance of Cu2O/rGO cathode was analyzed after it was loaded on the surface of cathode carbon cloth. The enhancement effect of Cu2O/rGO cathode on the power generation and nitrogen removal performance of MFC were investigated through the output voltage, power density and NO3--N removal rate of MFC. The mechanism of Cu2O/rGO cathode enhancing MFC performance was investigated by measuring denitrifying enzyme activity and extracellular polymer. Results showed that Cu2O/rGO which has a large number of mesoporous structures, provide more channels for electron transport, and Cu2O/rGO has better redox reversibility. Compared with Pt/C cathode, the exchange current density of Cu2O/rGO cathode increases by 33.53%, the electron transfer resistance decreases by 65.53%. The maximum average output voltage (662.54 mV), maximum power density (26.27 mW/cm2), NO3--N removal rate (83.33 mg NO3--N L/h) and average coulomb efficiency (32.02%) of Cu2O/rGO-MFC were higher than those of Pt/C-MFC (485.33 mV, 16.98 mW/cm2, 7.38%, 41.67 mg NO3--N L/h). Cu2O/rGO composite material enhance the activity of key enzymes and the content of protein-like components in denitrification of MFC cathode, improving the performance of electricity generation and nitrogen removal of Cu2O/rGO-MFC.

    • JIA Yanping, DING Xue, DU Fei, ZHANG Jian, ZHANG Hai-feng, ZHANG Lan-he

      2022,39(12), DOI:

      Abstract:

      Fe/C microelectrolysis process has low wastewater treatment efficiency and is prone to hardening problems, and is only suitable for treating acidic wastewater. In order to broaden the application range of Fe/C microelectrolysis process and improve the treatment efficiency, Fe/Mn/C ternary microelectrolysis system was constructed by adding zerovalent Mn and methyl orange (MO) simulated dye wastewater was treated. The morphology changes of iron, manganese and carbon and the compositions of surface elements were analyzed using SEM-EDS, Fourier transform infrared spectroscopy and Raman spectra. The changes of organic compounds in the wastewater were explored using UV-Vis spectra and three-dimensional fluorescence spectra before and after the reaction. Degradation performance of methyl orange was compared between Fe/Mn/C microelectrolysis and Fe/C microelectrolysis. Reaction mechanisms and reaction kinetics of methyl orange degradation were revealed using Fe/Mn/C ternary microelectrolysis system. The results showed that iron oxides, hydroxides and manganese oxides were existed on the surface of iron, manganese and carbon after the reaction. Fe/Mn/C ternary microelectrolysis broke nitrogen-nitrogen double bond of methyl orange and destroyed the structure of benzene ring. The degradation process of methyl orange conformed to second-order kinetics. After zero-valent Mn was added into Fe/C binary microelectrolysis system, the reaction efficiency constant of methyl orange degradation increased from 5.7381×10-4min?1 to 9.38336×10-4min?1. The degradation rate and degradation effect of methyl orange in the Fe/Mn/C microelectrolysis system was significantly better than those in the Fe/C microelectrolysis system.

    • Dyeing and finishing auxiliaries
    • ZHANG Meng, WU Mingyuan, WU Qingyun, YANG Jianjun, LIU Jiuyi, ZHANG Jianan

      2022,39(12), DOI:

      Abstract:

      In order to breach the bottlenecks of high solid content BiOCl crystals induced crystal fragmentation and agglomeration, square bismuth oxychloride (BiOCl) crystals with high solid content, excellent dispersisty and controllable size were prepared by using polyethylene glycol monomethyl ether-b-polymethyl methacrylate N,N-dimethylaminoethyl ester (mPEG-b-PDMAEMA) as dispersant. Pearlescent printing coatings with different pearlescent effects were obtained by using the as-prepared BiOCl crystals of varied size as pearlescent pigment and self-made waterborne polyurethane (WPU) emulsion as binder. The morphology, size distribution and crystallinity of BiOCl crystals were investigated by optical microscope, particle size distribution analyzer and XRD, respectively. The air permeability, moisture permeability, water contact angle and fastness of the pearlescent printing coatings were tested. The results showed that fragment-free BiOCl crystals of regular square exhibited high crystallinity with solid content of 10 %. The pearlescent printing coating demonstrated air permeability of > 5500 g/m2?d and moisture permeability of 15~25 mm/s-1 with the water contact angle of above 130 ° and color fastness to rubbing and washing reaching 4 or above.

    • Weng Jiali, Zhang Wei, Yu Hua

      2022,39(12), DOI:

      Abstract:

      In order to avoid the harm of capsule raw materials to the environment, degradable ethyl cellulose ether (EC) was selected as the wall material, and essential oil microcapsules were prepared by solvent evaporation. The results showed that the stirring rate had a great influence on the particle size and surface micropores of microcapsules. When the stirring rate was 1200 r/min and the mass of EC and essential oil were 1 g and 1.25 g respectively, the median particle size of the microcapsules was 70.8 μm. The embedding rate was 44.3%. Then, the prepared essential oil microcapsule was used to prepare the hygroscopic and breathable composite fabric through the wet coating process. It could be seen from the SEM that this method retained the original shape of the substrate. The flavor retention rate after 30 days of release was 39.2%. This was due to the fact that the mass fraction of Linalyl Acetate in the encapsulated essential oil increased by 27.09%, which prolonged the storage life of the essential oil. The microcapsules were uniformly and massively distributed on the surface of the stretch coated fabric, making the fragrance value as high as 382. The air permeability of the stretched and un-stretched composite fabrics was more than 600 mm/s, the fragrance retention rate was more than 35% after washing for 5 times, and the quality remains more than 96% after rubbed for 50 times. The preparation method of the composite is simple and can effectively improve the problem that the air permeability and fastness cannot be obtained at the same time.

    • Oil field chemicals and petroleum additives
    • YAN Han, YU Xiao-rong, JI Ren-jing, SHENG Zhe, YANG Huan, SU Gao-shen

      2022,39(12), DOI:

      Abstract:

      The core-shell polymer microspheres PMS@SiO2 were prepared by dry water method using hydrophobic SiO2 and aqueous phase containing monomer, initiator ,crosslinking agent and water. The effects of SiO2 hydrophobicity, the ratio of silicon and water, stirring speed and stirring time on the formation of stable dry water microreactor were investigated. The polymerization conditions of core water phase were optimized by orthogonal experiment, in which ammonium persulfate and sodium bisulfite were used as initiators ,N,N'-methylene bisacrylamide was served as a crosslinking agent. The chemical structure, thermal stability and microscopic appearance of the microspheres were respectively characterized by Fourier transform infrared spectroscopy(FTIR), thermogravimetric analyzer(TGA), laser particle size analyzer, scanning electron microscope (SEM) and transmission electron microscope(TEM), its water swelling and flooding performance were also evaluated. The results showed that the best preparation condition of core-shell polymer microspheres PMS@SiO2 were as follows: the mass ratio of SiO2-R812S and water phase was 1:10, the stirring speed and stirring time were respectively 12,000 r/min and 120 s, the amount of crosslinking agent and initiators were respectively 0.1% and 0.15%, the reaction temperature was 50 ℃ and the reaction time was 4 h. The microspheres were hydrated at 90 ℃ for 20 days, and its expansion times was about 5.0. Compared with the conventional polymer microspheres PMS, PMS@SiO2 showed slower expansion. The results of physical model displacement experiment indicated that the plugging ratio of PMS@SiO2 could reach 90.39%, the residual resistance coefficient was 10.409, and the recovery rate can be increased by 34.02%. The recovery rate of PMS@SiO2 was 11.89% higher than that of PMS, with good profile control and displacement performance.

    • Fine chemical intermediates
    • ZHAO Guodong, WU Wenju, YU Yanchao, BAI Yulong, YOU Jun

      2022,39(12), DOI:

      Abstract:

      β-cyano ketones are important fine chemical intermediates, in which cyano groups can be converted into amides, amines, carboxylic acids and their derivatives, aldehydes, ketones, alcohols, nitrogen-containing heterocycles, etc. Using cheap and low-toxic acetone cyanohydrin as the cyanogen source, the efficient preparation of β-cyano ketone was achieved through the conjugate cyanation reaction of α,β-unsaturated carbonyl compounds. The influence factors such as the type and amount of base, temperature, solvent, and the amount of acetone cyanohydrin on the reaction were investigated. Results showed that the optimal experimental conditions were obtained as follows: LiOH·H2O was used as the base, the amount of substance ratio of reaction substrate, acetone cyanohydrin, and LiOH·H2O was 1:2.5:1.6, DMF and H2O in a volume ratio of 4:1 was used as solvent, and the reaction temperature was 60 °C. Under the optimal conditions, the highest yield of β-cyano ketone was 98%. Further investigation of the scope of substrates showed that the corresponding β-cyano ketones could be obtained from 16 chalcone derivatives in the yield of 85%~98%.

    Select All
    Display Method:: |
    Select All
    Display Method:: |
Submit
Metadata retrieval
Organizers:China Haohua (Dalian) Research & Design Institute of Chemical Industry Co., Ltd.
Edited Published:
Editor in Chief:HAN Jianguo
Associate editor:CHEN Qu
Address:201 Huangpu Road, Hi-Tech Zone, Dalian
Phone:86-411-84699773, 84685669
ISSN:1003-5214