2023, 40(5).
Abstract:Lignin is a kind of abundant and environment-friendly polyphenol polymer that can be used as a natural antioxidant. Meanwhile, lignin has the advantages of good light stability, UV resistance and biodegradability, how to better develop and utilize its antioxidant function has attracted extensive attention of researchers. First, this paper summarized the recent advances about the structure-activity relationship of lignin antioxidant, the influence and mechanism of lignin microstructural on its antioxidant ability were summarized, and the main problems faced by structure-activity study were discussed. Secondly, the efforts on improving the antioxidant activity of lignin were introduced from the perspectives of fractional purification, nano modification and chemical modification. Finally, by introducing the application of lignin in sunscreen, polymer functional composites and medical materials, the contribution of antioxidant property of lignin to the anti-UV ability, thermal oxygen stability and bacteriostatic activity was discussed, which could provid a reference for the preparation and application of lignin-based functional materials.
GE Jie-fang , XIONG Xiang-yuan
2023, 40(5).
Abstract:Multi-drug resistance (MDR) refers to the phenomenon that tumor cells product resistant to traditional and new chemotherapeutic drugs, which has become an important obstacle in the treatment of malignant tumors. In recent years, it has been found that nanoscale drug delivery systems (NDDS) have unique advantages in inhibiting tumor multi-drug resistance, including increasing the solubility and stability of drugs, avoiding drug efflux pumps, achieving higher drug concentrations at the target site via using lower doses and negligible toxic side effects. Therefore, NDDS emerge as an effective strategy to overcome MDR in cancer. Here, we review the types and research progress of NDDS for enhancing the uptake of anticancer drugs and selective intracellular accumulation, including targeting specific ligand functionalization systems and stimulus-responsive drug activation and release systems.
SONG Xiao nan , CHEN Ying , SHAN Shao yun , ZHI Yun fei , HU Tian ding
2023, 40(5).
Abstract:Hydroboration is one of the main ways to synthesize organoboron compounds, which has received much attention because of its mild conditions, simple operation and high atomic utilization. Materials containing noble metals such as Rh, Ir, and Pb have been the primary choice catalysts for hydroboration in the past decades, but their high cost and toxicity have limited their widespread application. In the last decade, alkaline earth metals and cheap transition metals such as Fe, Co and Ni have flourished in the field of catalytic hydroboration because of their abundant reserve, low price and high catalytic performance, thus exhibiting have a broad application potential. This paper focuses on the research progress of transition metal and alkaline earth metal-based materials catalyzing hydroboration of unsaturated hydrocarbons in recent years.
ZHANG Chengping , GUO Qin , QUAN Hengdao
2023, 40(5).
Abstract:The development methods and development status of alternatives to chlorofluorocarbons (CFCs) were introduced in this review. Currently, developed alternatives to CFCs include hydrochlorofluorocarbons (HCFCs), hydrofluorocarbons (HFCs) and hydrofluoroolefins (HFOs). Among them, HFOs have excellent environmental performance, which can be used to replace HFCs in the fields of refrigeration and foaming. The main synthetic routes of HFOs are summarized, and the best industrialization route is pointed out. However, the core patents of HFOs are monopolized by foreign developed countries, and HFOs have the risk of secondary pollution and flammability. Besides, the performance of HFOs is difficult to meet the application requirements in the fields of precision cleaning, high-end chip manufacturing process and high-voltage electrical insulation. Looking forward to the future development of CFCs substitutes, it is proposed that the future research focus will be: it is necessary to develop a new generation of alternatives to meet the country's major strategic needs so that our contry achieve precise replacement of CFCs in many fields.
LUO Yanping , JIN Caiju , DING Shunmin , CHEN Chao
2023, 40(5).
Abstract:Hydrosilylation reaction refers to the addition reaction of compounds containing Si-H bonds and compounds containing unsaturated bonds under certain conditions. It is one of the important reactions for building C-Si bonds and plays an important role in the silicone industry. In this paper, the recent research work on metal-organic frameworks (MOFs) catalyzing such reactions is reviewed, and the reactions carried out by each reaction substrate are systematically summarized and reviewed. Finally, the prospect of MOFs for catalyzing hydrosilylation reaction is given.
YAO Xianrui , HUANG Rui , YU Yu-jie , TANG Yu-mu , HE Yu , LI Jian-feng
2023, 40(5).
Abstract:Hydrophobic deep eutectic solvents are recognized as potential substitute of traditional toxic and harmful organic solvents and ionic liquids due to their simple preparation, low toxicity, high thermal stability and high biodegradability. Their hydrophobicity, highly adjustable physical and chemical properties and excellent solubility of organic and inorganic compounds can meet the needs of many industrial applications. Through the synergistic effect of electrostatic interaction, ions exchange and hydrogen bond, hydrophobic deep eutectic solvents achieved efficient separation, directional catalysis and modification of the target substances. This paper summarizes the structure composition and performance influencing factors of hydrophobic deep eutectic solvents, and review the application of hydrophobic deep eutectic solvents in separation and extraction, pollutant removal, biocatalysts, material modification and food safety detection. Hydrophobic deep eutectic solvents can achieve targeted regulation of the solvent properties by changing their structure composition, then highly selective extracts various target components in a wide pH range, and simplifies the process of catalysis and modification. Their high cycle stability greatly reduces the consumption of solvent, and shows great potential to replace traditional solvents in green chemical technology. However, the synergistic mechanism between the compositions of the hydrophobic deep eutectic solvents is not clear, it is necessary to further to clarify their function mechanism in order to achieve the precise customization and efficient application of the hydrophobic deep eutectic solvents.
2023, 40(5).
Abstract:Rhodamine B (RhB) was incorporated into polyethylene glycol diacrylate (PEGDA) and ethoxylated trimethylolpropane triacrylate (ETPTA) to prepare RhB-PEGDA/ETPTA with different photonic band gaps Inverse opal structure photonic crystal composite film. The composite film was characterized by reflection spectrum and fluorescence spectrum. And the fluorescence polarization performance regulation of RhB by photonic crystal was studied. The results show that when the photonic bandgap of the photonic crystal composite film exactly matches its emission peak (595 nm), the polarization state of the emitted light is regulated successfully. When the thickness of the photonic crystal layer is 6.94 μm, the fluorescence polarization regulation effect is the best, and the polarization anisotropy value is 0. When the photonic bandgap of the inverse opal composite film matches the excitation wavelength (555 nm), the polarization anisotropy value is 0.082; when it matches red band edge of the emission peak (665 nm), the polarization anisotropy value is 0.12; When the emission peaks are uncorrelated (730 nm), the polarization anisotropy value is 0.16, similar with that of pure RhB. All these results indicate that photonic crystals with suitable bandgap can regulate the polarization state of fluorescence.
WU Denghui , LI Xin-hang , ZHAO Pei-hua
2023, 40(5).
Abstract:A novel reacting P-N intumescence flame retardant, trioxo (3-triethylphosphite- 5-chlorine- 1-triazine) glycerin (TTCTG), has been synthesized and the molecular structure was characterized by FTIR, H NMR, and 31P NMR. The thermal degradation property of TTCTG was assessed by TGA, which revealed that it was good thermal stability on the high temperature condition. The flame retardancy of cotton fabrics with different TTCTG content was investigated by using TGA, vertical flammability test, LOI, and SEM,the results showed that when the content of TTCTG was 20%, the limiting oxygen index of 20%TTCTG-CF was up to 27.3%, the flame retardancy reached the class B1 of national standard of flame retardant fabrics.The TGA results indicated TTCTG could promote the rapid decomposition of cotton fabric into char at 284 ℃, SEM showed that the surface of 20%TTCTG-CF formed the dense expansive carbon layer after combustion. After washing for 20 times, the LOI of 20%TTCTG-CF was still as high as 26.4%, reaching class B1 of national standard of flame retardant fabrics. The structure of 20%TTCTG-CF after 20 washing times was analyzed by SEM and FTIR, and the results showed that TTCTG and cotton fiber were linked by covalent bond, which gave cotton fiber excellent and lasting flame retardancy.
TAN Yanyan , SHANG Xiaoyu , XIE Jinhui , ZHANG Daohai , SHAO Huiju , QIN Shuhao
2023, 40(5).
Abstract:HDPE/CSW composites were prepared by melt blending method using γ-methacryloxypropyltrimethoxysilane (KH570) modified calcium sulphate whiskers (CSW) as filler for high density polyethylene (HDPE). The effects of KH570-modified CSW on the properties of the composite HDPE/CSW were characterized by SEM, XRD, TG and DSC. The results showed that the tensile and flexural strengths of HDPE/CSW increased by 39.51% and 15.9%, respectively, compared with pure HDPE at a CSW mass fraction of 20%, and were prone to heterogeneous crystallization, which enhanced the heat resistance and crystallinity of the HDPE/CSW composites, and the crystallization behaviour showed that the HDPE/CSW composites grew as two-dimensional sheet crystals. The activation energy of thermal degradation reaction of the original HDPE was 244.11 kJ/mol, and the activation energy of thermal degradation reaction of HDPE/CSW composites decreased to 236.99 kJ/mol at 50% mass fraction of CSW, indicating that CSW enhanced the thermal degradation reaction rate of HDPE/CSW composites and extended the use range of the composites.
YANG Wei-cheng , LIU Jian , MA Hai-yan
2023, 40(5).
Abstract:Based on the Grubbs 2nd catalyst, several creative Grubbs 3rd catalysts were synthesized by reaction with pyridine ligands of different types. The structures were characterized and confirmed by 1H NMR. The bulk polymerization of dicyclopentadiene was catalyzed by the newly synthesized G3 catalysts. On the basis of controllable polymerization by adding triphenylphosphine polymerization inhibitor, polydicyclopentadiene material was prepared by mould casting method. The effects of polymerization inhibitor, different catalysts and different catalyst contents on the properties of polydicyclopentadiene material were discussed. The structure was characterized by FT-IR, TGA and DSC. p-DCPDThe results indicate the introduction of PPh3 could prolong the spot life of DCPD mixed solution with Grubbs 3rd catalysts more significantly than that with Grubbs 2nd catalyst. The newly synthesized Grubbs 3rd catalysts exhibited excellent catalytic performance for DCPD polymerization, obviously improving the mechanical properties of p-DCPD materials. Moreover, the p-DCPD manufactured from benzomethylene-[1,3-bis(trimethylphenyl)-2-imidazoline subunit]-dichloro-bis(3-methylpyridine) ruthenium(G3-5) exhibited better performance thermal stability and compact cross-linking structure.
DONG Meng-meng , WANG Chan , RAN Guo-xia , ZHANG Mi , SONG Qi-jun
2023, 40(5).
Abstract:This work develops a new method for rapid and efficient detection of sex hormones in cosmetics. Gold nanoparticles (AuNPs) with high dissipation coefficient was used as fluorescence quenchers in this detection system, rhodamine B(RB) was considered as fluorescence probe and β-cyclodextrin(β-CD) was provided as recognition element. Inclusion of RB into β-CD made fluorescence resonance energy transfer (FRET) occur through the donor (RB) and quencher (AuNPs) nearby. And then, the progesterone-induced release of RB from β-CD cavity, leads to the recovery of the fluorescence of RB. Thus the corresponding fluorescence recovery rate had a good linear relationship with concentration of progesterone in the range of 0 μmol/L-25 μmol/L,and the limit of detection is 0.15 μmol/L. The system was used for the determination of progesterone in toner, and the recoveries are from 95.3% to 101.9%, and the relative standard deviations were less than 4.2%. The fluorescence probe also response to other sex hormones such as estradiol and testosterone. It could be concluded that the system can be applied to the detection of sex hormones in cosmetics.
YU Zhi-juan , WU Jing-xiang , JIANG Jing-yang , ZHANG Chun-qing
2023, 40(5).
Abstract:In this paper, anionic copolymerization of butadiene and styrene with n-butyllithium (n-BuLi) as initiator and 2, 2-bis (5-methyl-2-tetrahydrofuranyl) propane (BMTFP), ethyl tetrahydrofurfuryl ether (ETE) and ditetrahydrofuranyl propane (DTHFP) as polar regulators was carried out under different dosage of regulator and polymerization temperatures. The microstructure, molecular weight and its distribution of styrene-butadiene copolymer were characterized by 1H-NMR and GPC. The results showed that there was no side reaction in BMTFP polymerization system and the molecular weight distribution of copolymer was narrow, which was consistent with the characteristics of living? anionic polymerization. BMTFP has a strong ability to regulate the microstructure of styrene-butadiene copolymer. When the polymerization temperature was 50℃ and the BMTFP/ n-BuLi (mole ratio) was 2/1, the content of 1,2- structure in styrene-butadiene copolymer can reach 69.7%, and the content of styrene microblock tends to 0. Under the same experimental condition, BMTFP, ETE and DTHFP were at the same level in terms of their ability to regulate the microstructure of styrene butadiene copolymers. However, the raw materials required for BMTFP synthesis were bio-based platform compounds. From the aspects of environmental protection, energy security and potential economic value, BMTFP has a broad development prospect in the preparation of solution styrene butadiene rubber with high vinyl content.
GUO Song , SUN Yisi , YANG Weicheng , SHI Huijuan , MA Haiyan , LUO Yong
2023, 40(5).
Abstract:This paper reported the preparation of poly(dicyclopentadiene-co-cyclooctadiene) microfluidic chips. Elastomer PDCPD copolymer was synthesized by ring opening metathesis polymerization of dicyclopentadiene (DCPD) with cyclooctadiene (COD) which was introduced as comonomer. when the mass ration of DCPD: COD was 1 : 1, as-synthesized copolymer showed the similar elastomeric properties as PDMS and excellent fidelity of replication at microscale. We achieved persistent bonding between copolymer and PDCPD based on the polymerization activity of semi-cured gel. Chips fabricated by copolymer can be connected in a simple, effective manner which similar to that of PDMS chips. Monodispersed droplets were obtained using copolymer microfluidic chips and the size of the microdroplets can be tuned via changing the flow rate of continue phase.
LI Ying , SHI Hongling , WANG Zhe , RAN Luni , XUE Chuan , TANG Cunduo
2023, 40(5).
Abstract:L-2-aminobutyric acid (L-ABA) is an important pharmaceutical intermediate and food additive. In order to achieve the efficient biosynthesis of L-ABA, two recombinant Escherichia coli strains carrying threonine deaminase, leucine dehydrogenase and different formate dehydrogenases encoding genes were established by using a dual plasmid co-expression system of pACYCDuet-1 and pET28a, which were named as E. coli BL21(DE3)/ pACYCDuet-1-EsLeuDH-EcTD: pET28a- CbFDH and E. coli BL21(DE3)/ pACYCDuet-1-EsLeuDH-EcTD: pET28a- CbFDHM, respectively. After induction, the two recombinant E. coli strains successfully expressed three target enzymes. The results showed that the expression levels of L-threonine deaminase and L-leucine dehydrogenase in the two recombinant E. coli strains were basically the same. The expression level of formate dehydrogenase in the latter was 342 IU/mL, which was significantly higher than 196 IU/mL in the former. In the 50 mL reaction system, 200 mM L-threonine was reacted at 220 rpm and 30 ℃ for 8 hours, the yield of L-ABA was 71% in the former and 85% in the latter. The results showed that increasing the expression level of formate dehydrogenase could significantly improve the synthesis efficiency of L-ABA. After the reaction temperature was optimized, the yield of L-ABA reached 90% catalyzed at 220 rpm and 30 ℃ for 8 hours. This study laid a solid theoretical foundation for the large-scale conversion and value-added of L-threonine and the biosynthesis of L-ABA in the future.
ZHANG Chunyan , SU Jiajun , YIN Hui , YAO Chenxi , XIAO Jun , LUO Jianxin
2023, 40(5).
Abstract:Poly(p-phenylene sulfonic acid) microspheres were prepared by a simple, green and controllable method, and used as solid acid catalysts for the synthesis of biodiesel. Firstly, poly (p-phenylene sulfonic acid) microspheres (PSS) were prepared by soap-free emulsion polymerization with water as medium, styrene (St) as the matrix monomer, divinylbenzene (DVB) as the cross-linking monomer, sodium p-phenylene sulfonate (NaSS) as functional monomer, methacrylic acid (MAA) as the water-soluble monomer, and potassium persulfate (KPS) as the initiator. The obtained microspheres were characterized by FT-IR, XPS, SEM, TGA and DSC, and their particle size, zeta potential, specific surface area and acid density were investigated. The effects of NaSS, DVB and KPS contents on the structure and properties of the microspheres were discussed. Then, PSS was used as solid acid catalyst to catalyze the esterification of oleic acid/methanol to synthesize biodiesel. The conversion rate of oleic acid could reach 86.4% when the ratio of methanol to oleic acid is 10:1, the amount of PSS is 2% of the mass of oleic acid, the reaction temperature is 80 ℃, and the reaction time is 6 h. As a solid acid catalyst, PSS has good reusability, and the conversion of oleic acid has not decreased significantly after 4 cycles.
WEN Na , HU Meifeng , LI Deli , CHANG Yue , ZHA Fei
2023, 40(5).
Abstract:Abstract:PGS(PEI)/CaIn2S4 composites was prepared by a one-pot hydrothermal method using polyethyleneimine (PEI) modified palygorskite (PGS(PEI)) and CaIn2S4 precursor as raw materials. The physicochemical properties of PGS(PEI)/CaIn2S4 composites were characterized by means of XRD, SEM, N2 adsorption-desorption, UV-Vis DRS and PL. The growth mechanism of the composite was described and the feasibility of photocatalytic degradation of various dyes was tested. PGS(PEI) is embedded in flower-like nano-CaIn2S4.The maximum specific surface area, pore volume and pore diameter of PGS(PEI)/CaIn2S4 (modified PGS mass ratio of 60%) are 138.6 m2/g, 0.49 cm3/g and 14.20 nm, respectively. The photogenerated carrier separation rate of composite increases attributing to the built-in electric field between PGS(PEI) and CaIn2S4 and the photoelectron transformation by PEI. Thephotocatalytic activity of 60% PGS(PEI)/CaIn2S4 for methylic orange (MO) degradation is higher than CaIn2S4 under the visible light. The degradation rate of MO is 96.9% for 60 min. The superoxide free radicals (.O2-) play an important role in the photodegradation process.
Zhang Wan-ping , LI Xuyan , SUN Zhiyong , WANG Lu , ZHANG Yuhong , HUANG Huoxing , ZHANG Dongmei
2023, 40(5).
Abstract:Carbonic acid is a biological effector molecule with broad application prospects in skin care and skin disease intervention. The hydration conversion effect of carbonic acid precursor molecule CO2 in aqueous medium is the key to the formation of carbonic acid, however, the factors affecting its hydration conversion have not been fully studied. Based on cosmetics, the effects of rheology modifiers, ionic strength, humectants, and emulsifiers on CO2 hydration conversion in aqueous environment were studied respectively; the cytocompatibility and human efficacy of CO2 minimalist formula system were discussed. The results show that the hydration conversion effect of CO2 decreases with the increase of the viscosity of the rheology modifier; it decreases with the increase of the ionic strength; the enhancement of the polarity of the polyol molecule is beneficial to the hydration conversion of CO2; the change of the molecular structure of the emulsifier affects the hydration conversion effect. In addition, the CO2 medium system showed excellent cytocompatibility to human keratinocytes, and the minimalist formula system containing CO2 lowered the skin pH, increased the skin moisture content, but increased the trans epidermal water loss rate. This research provides a research idea for the development of CO2 products and provides theoretical and application support for CO2 skin care applications.
YAN Ya-qian , ZHANG Yu-zhi , FU Hao , ZHANG Yu-xuan , WANG Dong-dong , YANG Li , LI Meng , WANG Chang-tao
2023, 40(5).
Abstract:Lactobacillus plantarum and Saccharomyces cerevisiae were used to prepare two kinds of dayrose fermentation broth. By monitoring the scavenging capacity of DPPH radical, hydroxyl radical and total antioxidant capacity of the two fermentation broth, it was found that the antioxidant capacity of the fermentation broth was stronger than that of the aqueous extract (blank control). At the cellular level, both fermentation broth showed repair effects on UVB-induced injury cells, and compared to the cell model group after UVB irradiation, the activities of collagen type ⅰ (COL-1) and catalase (CAT) were increased. In the experiments of tyrosinase activity inhibition,the daylily fermentation broth showed good whitening effect compared with the water extract. According to the expression levels of inflammatory factors IL-6, TNF-a and COX-2 in HaCaT cells, the expression level of inflammatory factors in the sample group was significantly lower than that in the model group, indicating that the anti-inflammatory ability of daylily fermentation broth was greater than that of water extract. The results of chick chorioallantoic membrane test (HET-CAM) showed that there was no bleeding phenomenon before and after treatment, and the daylily fermentation broth was not irritating. Finally, it was concluded that the two kinds of daylily fermentation can be used as natural plant raw materials for cosmetics, which have strong antioxidant, anti-inflammatory and whitening functions on the skin, and also have good human safety.
CAO Ning , LU Dan , ZHANG Jian-bin , ZHUANG Zi-cong , LU Jian-mei
2023, 40(5).
Abstract:flecainide acetate was synthesized from methyl 5-bromo-2-iodobenzoic acid via Ullmann aryl etherification, amide condensation, salification. The total yield was 52.1% (based on methyl 5-bromo-2-iodobenzoic acid). The optimistic condition of Ullmann aryl etherification reaction was established. The reaction conditions were obtained as follows: when{[(phen)2Cu][OCH2CF3]Cu} is used as ligand. The reaction was stirred in DMF at 110℃for 12 hours. The yield of key intermediate is 60.1%. The total yield of flecainide acetateis 54.0%, and the purity is 99.93%. The structure of flecainide acetate and the important intermediates were confirmed by MS, 1H NMR.
HAN Liu , WU Haoxiong , GAO Liancong , YANG Yuxin , CHANG Sheng , SUN Xin
2023, 40(5).
Abstract:Twenty-three (E)-4-(3-(2-bromophenyl) acryyl) phenyl - substituted benzenesulfonic ester derivatives were designed and synthesized based on the pharmacophore combination principle (yield: 60.9 to 80.3%), and their structures were confirmed by 1H NMR, MS and 13C NMR. The in vitro antitumor activity of the target compound was evaluated by MTT assay using 5-fluorouracil and imatinib as positive control, human cervical cancer Hela cells, human lung cancer A549 cells and human chronic myelocytic leukemia K562 cells as test cell lines. Target compound Vp exhibited the strongest A549 cell proliferation inhibitory activity (IC50 = 7.53 μmol/L), better than the positive control drug 5-fluorouracil (IC50 = 8.1 μmol/L), target compound Vt exhibited the strongest inhibitory activity of K562 cell proliferation inhibition (IC50 = 4.47 μmol/L), target compound Vd exhibited the strongest Hela cell proliferation inhibitory activity (IC50 = 4.53 μmol/L), than positive control drug 5-fluorouracil (IC50 = 13.5 μmol/L) is approximately 3 times stronger, and the target compound Vd also exhibits strong proliferation inhibitory activity against A549 cells (IC50 = 8.0 μmol/L) and K562 cells (IC50 = 7.81 μmol/L), which deserves further study.
2023, 40(5).
Abstract:The Pickering emulsions of four essential oils stabilized by modified citrus and whey pectin composite nanoparticles were prepared by high-pressure homogenization method after irradiation modification of pectin. The emulsions were characterized by Malvern laser particle size analyzer, SEM, FTIR and Haake torque rheometer, and the emulsions and antibacterial effects were evaluated by drug sensitivity tests. The results showed that the emulsification ability of the irradiated modified pectin was significantly enhanced which the emulsion stability was increased to 548.11 m2/g. FITR spectra characterized the groups of the emulsions,corroborating the formation of aggregates and the successful encapsulation of essential oils. The particle size of the emulsions ranged from 829 nm to 1147 nm and were stable after centrifugation and stay more than 90% storage for 77 days. The emulsions encapsulated different essential oils in the range of 5.81% to 21.54% with loadings of 0.81% to 5.81%. The four emulsions showed significant inhibition of two food microorganisms (Escherichia coli and Staphylococcus aureus) with inhibition circles ranging from 7.51 to 34.98 mm. The modified citrus pectin-lactalbumin based Pickering emulsions were stable in structure and encapsulated essential oils with good slow release efficacy and antibacterial activity, which provides theoretical guidance for the establishment of emulsion systems and delivery of antimicrobial essential oils This provides a theoretical guide for the establishment of emulsion systems and the delivery of antimicrobial essential oils and a promising application pathway.
ZHANG Jiang-hua , WANG Ting , YAO JiaShan , TANG Jingjing , MA Jia , ZHANG Wei , LI Zixuan , ZHOU Da-yong , SUN Le-le
2023, 40(5).
Abstract:A kind of zinc-loaded silica-coated iron oxide (Zn-Fe3O4@SiO2) material was prepared by sol-gel and impregnation methods, and their textural and magnetic properties were characterized by SEM, TEM, XPS, Py-FTIR, VSM and EDS techniques. The as-prepared Zn-Fe3O4@SiO2 was used to catalyze the acidolysis of soybean lecithins (SLs) with short-chain fatty acids (propionic acid and butyric acid) to synthesize novel emulsifiers of short-chain structured phospholipids (SCSPLs). Otherwise, the main physicochemical properties of the targeted SCSPLs were studied as well. Resultingly, it was identified that the thus-synthesized core-shell Zn-Fe3O4@SiO2 magnetic microspheres contained amounts of active zinc moieties, which effectively facilitated the synthesis of SCSPLs. When the m(SLs)∶m(C3:0)∶m(C4:0)=1∶4∶4, the catalyst dosage was 5% of total mass of raw materials, the reaction temperature was 50 ℃, and the reaction time was 5 h, the maximum short-chain fatty acid incorporation of SCSPLs reached 78.15%±1.08% with 35.43%±0.62% of propionic acid and 42.72%±0.55% of butyric acid. Meanwhile, Zn-Fe3O4@SiO2 could be easily separated with an external magnetic field and be recycled for 5 times without obvious deactivation. Moreover, the targeted SCSPLs showed greatly enhanced emulsifying and dispersing properties, and oxidative stability in comparison with raw SLs.
ZHANG Meng-di , Zhang Wei , YAO Ji-ming
2023, 40(5).
Abstract:In order to improve the efficiency of electrocoagulation of indigo dyeing wastewater, and determine the optimal conditions formation conditions of hydrolyzed metal salts. The Al-Ferron timed spectrophotometry was used to investigate the effect of initial pH value, coexisting anion species, and current density on the distribution of aluminum salts during electrocoagulation. The changes of floc Zeta potential, termination pH, system current and conductivity were also monitored. The dissolution and corrosion of the electrode were observed microscopically, and the electrochemical behavior was analyzed by measuring the electrode polarization curve and electrochemical impedance spectroscopy using an electrochemical workstation. The results showed that the optimal initial pH value range was 6 ~ 7 during the electrocoagulation, when the content of Alb with the dominant flocculation form is higher; the addition of chloride ions inhibited the electrode passivation and enhanced the electrocoagulation reaction rate; the low current density was beneficial to the uniform corrosion of electrodes and the existence of Alb. When the current density was 15mA/cm2, the content of Alb in the system could reach 4.76mg/L, which could produce a good flocculation effect.
XIE Qiuhua , JIANG Yazhen , ZHANG Zhihua , CUI Li , WANG Ping , YU Yuanyuan
2023, 40(5).
Abstract:Dye-free coloration of wool fabric was performed by using the Maillard reaction between reducing sugars and wool keratin. SDS-PAGE gel electrophoresis, spectrophotometry, DNS method and K/S value of the colored wool fabric were used to investigate the reaction between sugars and keratin, the effect of reducing sugar type and reaction conditions on the coloring property of wool fabric. The results showed that new glycoproteins with higher molecular weight were formed from the reaction between reducing sugar and wool keratin and the absorbance value at 540nm of the reaction solution changed obviously, which indicated that colorants were produced via the Maillard reaction between sugars and keratin. A stronger color yield of the colored fabric was obtained with xylose than that of galactose and glucose. The appropriate conditions for wool coloring were at 90℃ and pH=9. The colored yield of increased 23.0% after H2O2 pretreatment of wool fabric. The color fastness to washing and brushing and dry/wet rubbing fastness of the colored fabric via Maillard reaction were excellent with 4-5, 5, 5, 5 degree, respectively, but the color fastness to light is only 2 degree.
ZHANG Zhenming , LIU Chi , HUANG Wen-jing , ZHANG Shu-hang , SUN zhi-xu , Li Run-lai
2023, 40(5).
Abstract:Long-chain dialkyl amine containing hydroxyl groups was synthesized with peach aldehyde as substrates, Ti(n-OBu)4 as catalyst, NaBH4 as reductant, ammonium chloride/triethylamine as amine sources. The effects of catalyst and reaction temperature on the yield of reductive-amination were investigated. The optimized procedure was obtained as follows: reaction was carried out at 20 ℃ for 24 hours, n(peach lactone)∶n(NH4Cl)∶n(Et3N)∶n(Ti(n-OBu)4)∶n(NaBH4)=1.0∶1.45∶1.45∶1.45∶2.0,to give the titled compound with a yield of 57.7%. The structure of the product was characterized by FTIR, 1HNMR, 13CNMR and MS. The final process was validated and executed at up to 100 g scale with the yield of 61.5%.
XU Xi-xi , GU Gui-zhou , JAING Lin-shi , LI Zheng
2023, 40(5).
Abstract:Parafuchsin was synthesized by a two-step catalytic method. Firstly, para-nitrotoluene was used as the starting material, and sodium polysulfide was combined with ethanol as the organic solvent and N, N-dimethylacetamide(DMA) as the amine catalyst. The results showed that n (DMA) : n (p-nitrotoluene) =3:13 reaction effect was the best. Then, under the catalyst of alcohol based catalyst polyethylene glycol 400 (PEG-400), it reacted with aniline and hydrochloric acid to produce para-magenta crude product. The effects of material ratio, reaction temperature and reaction time on the yield of para-magenta crude product were investigated. The results showed that n (PEG-400) : n (p-nitrotoluene) =2: 300, n (p-nitrotoluene) : n (aniline) : n (hydrochloric acid) = 1: 5.9:2.8, reaction at 110 ℃ for 4 h, the yield of para-magenta crude was 85.6% .In the process of parafuchsin purification, the effects of reaction temperature and time on the mass fraction of parafuchsin were investigated, The results showed that the mass fraction of parafuchsin reached 99.3% after reaction at 130℃ for 3h. The wastewater from parafuchsin production is mainly aniline. After rectification, 89.3% of aniline can be recovered. The process has the characteristics of green, high efficiency and environmental protection, and is conducive to industrial popularization.
WU Xiaochun , HE Yong , YUE Zhiwei , MAO Yexiang , ZHANG Hongmo
2023, 40(5).
Abstract:The solvent-free synthesis process of 2-chloroethyl ethyl ether was improved. Using triethylamine as the catalyst for the reaction of 2-ethoxyethanol with thionyl chloride, the obtained product was washed with saturated sodium bicarbonate solution, saturated sodium chloride solution and dried with anhydrous sodium sulfate to obtain 2-chloroethyl ethyl ether. The structure of product was characterized by 1H-NMR and GC-MS. The effects of molar ratio of reactants, reaction temperature and reaction time on the chromatographic purity and yield of the product were investigated by one-variable at-a-time optimization approach. After optimization, the molar ratio of 2-ethoxyethanol : thionyl chloride : triethylamine was set to 1.0 : 1.3 : 0.3, the reaction temperature was 70 °C, and the reaction time was 4 h. Under this process, the product yield over 90.2% and the chromatographic purity over 99.4%,the assay over 99.2% were obtained after pilot-scale amplification of kilograms.