• Volume 40,Issue 2,2023 Table of Contents
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    • >Fine chemical intermediates
    • Catalytic synthesis of tetrahydroquinazoline by ionic liquids in aqueous media

      2023, 40(2).

      Abstract (109) HTML (0) PDF 477.97 K (461) Comment (0) Favorites

      Abstract:A series of tetrahydroquinazoline derivatives were synthesized by cyclization condensation in aqueous medium with 1-butyl-3-methylimidazole tetrafluoroborate as catalyst, aromatic amine and 2-aminobenzaldehyde as raw materials. By exploring the reaction conditions, the optimal conditions are determined as follows: With 0.2 mmol 2-(1-pyrrolide) benzaldehyde (Ⅰa), 0.4 mmol aromatic amine (Ⅱa), 30% (based on the amount of Ⅰa, the same below) catalyst, 1 mL H2O, at 90 ℃ for 6 h, the highest yield of 81% of the product was obtained. At the same time, the universality of the substrate was investigated, and 19 tetrahydroquinazoline derivatives were synthesized from a wide range of substrates.

    • >Drug and cosmetic materials
    • Synthesis of amino acid esters of oleic acid and dodecanedioic acid and their antibacterial activities

      2023, 40(2).

      Abstract (121) HTML (0) PDF 592.38 K (418) Comment (0) Favorites

      Abstract:Glycine ethyl ester hydrochloride, L-Alanine ethyl ester hydrochloride, L-leucine ethyl ester hydrochloride, L-methionine methyl ester hydrochloride and L-tyrosine methyl ester hydrochloride were used to react with oleic acid in presence of EDC/HOBt to produce five kinds of amino acid derivatives of oleic acid. In addition, glycine ethyl ester hydrochloride and L-alanine ethyl ester hydrochloride were reacted with dodecanedioic acid to produce two amino acid derivatives of dodecanedioic acid. The results showed that seven products were synthesized with yields higher than 75%. The structures of the products were characterized by FTIR, TGA, 1HNMR and LC-MS. The dispersibilities of the products were tested, and the antibacterial activities of the products against Staphylococcus aureus and Escherichia coli were investigated. The results showed that the products were capable of dispersing in both aqueous and organic phases. Moreover, these fatty acid acyl amino acid esters showed obvious antimicrobial activities. The oleoyl leucine ethyl ester can effectively inhibit the growth of Staphylococcus aureus (the number of bacteria is decreased from 2×109 CFU/mL to 1.4×107 CFU/mL). The oleoyl tyrosine methyl ester can inhibit Escherichia coli (the number of bacteria is decreased from 2×109 CFU/mL to 1.8×107 CFU/mL).

    • Study on Influencing Factors of Crystallization Rate of hexyl 2-[4-(diethylamino)-2-hydroxybenzoyl]-benzoate

      2023, 40(2).

      Abstract (137) HTML (0) PDF 730.34 K (430) Comment (0) Favorites

      Abstract:This paper mainly studies the solubility changes of hexyl 2-[4-(diethylamino)-2-hydroxybenzoyl]-benzoate (DHHB), the most widely used sunscreen agent in different oils. Phenylethyl benzoate (226) oils have the greatest compatibility with DHHB sunscreens. After ultrasonic dissolution, the solubility is 0.241 g/mL when placed for 28 days at room temperature at 25 °C. The effect of different dissolution methods on the recrystallization of sunscreens was investigated, and it was found that the decline rate of the 28-day heating and dissolution was more than 10% lower than that of ultrasonic dissolution. It was reduced by 12.65%; the solubility changes of sunscreens were stored for 4 weeks under different storage temperatures (4℃, 25℃), and it was found that low temperatures were more likely to promote the crystallization of sunscreens. By adding emulsifiers Span 20 and Span 80, it is found that the addition of emulsifiers can significantly slow down the decline rate of the solubility of DHHB in the oil dioctyl carbonate (CC). The decline rate of the post-80s was reduced by 21.28%. By observing the crystallization behavior of sunscreen agents and XRD detection of recrystallized substances, the influence of the above conditions on the crystallization of DHHB was explored, which provided guiding significance for solving the application of DHHB in the later development of sunscreen products.

    • >Fine chemical intermediates
    • One-pot synthesis of quinoline polycyclic compounds

      2023, 40(2).

      Abstract (198) HTML (0) PDF 700.59 K (479) Comment (0) Favorites

      Abstract:Quinoline, as an advantageous skeleton of drug modification, has important application value in the field of innovational drug research and development, and the methodological studies on its structural modification has also attracted much attention. In view of this, a one-pot method to synthesize a series of novel quinoline polycyclic compounds were constructed with 5-fluorosubstituted-4-chloroquinoline derivatives and binucleophilic reagents as the starting materials. The key step of this method is the reaction of 4-chloro-5-fluoroquinoline-3-carboxylates with ortho-substituted anilines (binucleophilic reagents) in N,N-dimethylformamide, and in the presence of deacid reagents to complete a cascade substitution of chlorine and fluorine under heating conditions, to afford diversified quinoline polycyclic derivatives without separating the mono-substituted intermediates. The method is simple and efficient, does not require any catalysts, and with good tolerance of various functional groups. The structures of the products were confirmed by 1H NMR, 13C NMR and high resolution mass spectrum (HRMS).

    • >Functional materials
    • Preparation and Properties of PIN/PAN Polymer Electrolyte Film

      2023, 40(2).

      Abstract (136) HTML (0) PDF 1.29 M (398) Comment (0) Favorites

      Abstract:PIN/PAN(Polyindole/Polyacrylonitrile)films were prepared by electrospinning to replace cellulose paper(C-P)in paper-based aluminum air and applied to thin film aluminum air batteries. This study analyzed the influence of PIN content on the ionic conductivity and liquid absorption rate of thin film electrolyte. The surface morphology and chemical composition of PIN/PAN films were analyzed by SEM and FTIR. The ionic conductivity and discharge characteristics of thin film electrolyte were analyzed by electrochemical workstation and battery test system. The results show that PIN/PAN thin film electrolyte can effectively improve the performance of thin film aluminum air battery. At 3 mA cm-2,5 mA cm-2and7 mA cm-2, the discharge time is about 21%, 27% and 34% higher than that of paper-based aluminum air battery, and the discharge time is related to the liquid absorption rate and ionic conductivity of thin film electrolyte. The ionic conductivity of electrolyte prepared by 4% PIN/PAN film is 6.7×10-4 S.cm-1, and it has good adsorption capacity for alkaline solution. The highest liquid absorption rate is 496%,which is 3.3 times higher than that of cellulose paper.

    • >Review and monographs
    • Research progress of iron-based oxygen reduction catalysts in fuel cells

      2023, 40(2).

      Abstract (89) HTML (0) PDF 1.40 M (464) Comment (0) Favorites

      Abstract:Cathode oxygen reduction reaction is one of the core reactions of fuel cells. At present, the catalyst for catalyzing oxygen reduction reaction is usually the noble metal platinum. However, its high cost, poor tolerance to methanol, and easy carbon monoxide poisoning limit its widespread use. Therefore, it is essential to research non-platinum-based catalysts. Iron-based catalysts are favored due to their excellent catalytic activity, high stability, good methanol tolerance, and low price, and they are the most promising alternatives to platinum-based catalysts. In this paper, the research status, catalytic mechanism and factors affecting the activity of several types of iron-based oxygen reduction catalysts are reviewed. Then, the problems to be solved and the development direction of various catalysts are also proposed.

    • >Electro-organic chemistry and industry
    • Core-shell NF@Ni3S4@CoFe-LDHs electrode for Urea-Assisted Oxydrogen Reaction in Alkaline Media

      2023, 40(2).

      Abstract (88) HTML (0) PDF 1.59 M (402) Comment (0) Favorites

      Abstract:The anodic oxygen evolution reaction (OER) of hydrogen production from electrolytic water requires a high over potential to overcome the slow kinetics. Therefore, urea oxidation reaction (UOR) with a theoretical overpotential of 0.37 V was used to decrease the anodic overpotential. Hydrothermal and electrochemical deposition methods were used to construct heterogeneous core-shell structure NF@Ni3S4@CoFe-LDHs catalytic electrode which used in basic urea solution. Due to the synergistic effect of hierarchical structure and heterogeneous species at the interface, the adsorption of intermediate products and the desorption of protons on the electrode surface are accelerated, and the decomposition energy barrier of water and urea molecules is greatly reduced. In the mixed solution of x mol/L urea (x=0.1, 0.33 and 0.5) with 1mol/L KOH, it only need 100 mV overpotential to drive 10mA/cm2 current density. In 0.33 mol/L alkaline urea solution, the NF@Ni3S4@CoFe-LDHs can driven 116mA higher than that in 1mol/L KOH solution, and it can operate stably for 20 h while maintaining good circularity. The catalytic electrode has good application prospects in hydrogen production from alkaline water and urea wastewater treatment.

    • >Review and monographs
    • Application of MOFs materials in catalysts for CO2 hydrogenation

      2023, 40(2).

      Abstract (226) HTML (0) PDF 4.86 M (649) Comment (0) Favorites

      Abstract:As one of the major greenhouse gases, CO2 has caused a series of environmental problems, such as global warming. CO2 conversion to valuable products is of great significance to alleviating global climate issues. Methanol is not only a high energy fuel but an important chemical intermediate. CO2 hydrogenation to methanol is a feasible way to realize CO2 recycling. However, at present, there are a series of problems such as low selectivity, low CO2 conversion rate and low methanol synthesis rate. Thus, the development of efficient and highly selective catalysts is critical to realize the industrial application of CO2 hydrogenation to methanol. In recent years, metal-organic framework (MOFs) materials have attracted extensive attention in the field of catalysis due to their structural diversity and design flexibility. In this paper, we reviewed the advantages, synthesis methods and research progress of MOFs catalysts in the field of CO2 hydrogenation to methanol. Furthermore, the challenges and prospects of the application of MOFs catalysts in this field were also discussed.

    • >Functional materials
    • Synthesis and electrochemical properties of yttrium-doped lithium titanate/graphene nanocomposites

      2023, 40(2).

      Abstract (165) HTML (0) PDF 1.18 M (546) Comment (0) Favorites

      Abstract:With graphene as the base, tetrabutyl titanate, lithium hydroxide and yttrium nitrate as raw material, cetyl ammonium bromide as the surfactant, the nanocomposite precursor was synthesized by solvothermal method, and then the yttrium-doped lithium titanate/graphene nanocomposite was synthesized by calcination under the atmosphere of nitrogen. The morphology, structure and composition of the nanocomposite were characterized by SEM, XRD, EDS, Raman Spectroscopy, etc. The results show that yttrium doped lithium titanate / graphene nanocomposites were formed by coating flake lithium titanate on graphene sheets. The nanocomposite was used as anode material of the lithium-ion battery, and its electrochemical properties were studied by cyclic voltammetry and constant current charge-discharge cycle method. The results show that under the charge-discharge current density of 100 mA/g, the initial charge-discharge capacity of the nanocomposite is 145.5mAh/g, the capacity fading is almost 0 after 100 cycles of charge-discharge cycle, 1.59% after 200 cycles, and 3.24% after 300 cycles, which is significantly improved compared with the graphite anode whose capacity retention rate is only about 80%. Further research found that the doping of yttrium and the compositing of graphene can reduce the polarization degree of lithium titanate electrode in the charge and discharge cycle and improve the cycle performance of the material.

    • Preparation and properties of self-healing hydrogels based ondynamic borate bonds/hydrogen bonds

      2023, 40(2).

      Abstract (102) HTML (0) PDF 5.30 M (940) Comment (0) Favorites

      Abstract:A novel phenylboronic acid ionic liquid (PBA-IL) monomer was designed, and the self-healing hydrogel (PAM/PBA-IL/CNF) with semi-interpenetrating network was prepared by a one-step polymerization of acrylamide (AM) and PBA-IL in the presence of TEMPO-oxidized CNFs. The chemical structure of PBA-IL was analyzed by 1H NMR. The chemical structure and physical morphology of the hydrogel were characterized by FTIR, XPS and SEM. The mechanical properties and self-healing properties were tested by tensile test and self-healing experiment. The results showed that the PBA-IL monomer and the hydrogel were successfully prepared, and the hydrogel exhibited excellent self-healing properties. When the mass fraction of PBA-IL was 30%, the self-healing efficiency of PAM/PBA-IL3/CNF hydrogel was 95.43% (within 150 min). And the tensile strength (319.5 kPa) and elongation at break (1950.3%) of the self-healed PAM/PBA-IL3/CNF hydrogel approached that of the original hydrogel. The self-healing properties of PAM/PBA-IL/CNF hydrogels were attributed to the synergistic effect of the boronate bonds formed by the PAM/PBA-IL copolymers with the cis-diols on the CNFs chain and the multiple hydrogen bonds inside the hydrogels.

    • Preparation and oil-water separation properties of hydrophobic peanut shell/polyurethane composite foam

      2023, 40(2).

      Abstract (93) HTML (0) PDF 1.60 M (430) Comment (0) Favorites

      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.

    • >Modernization technology of traditional Chinese medicines
    • Effect of drying method on kinetics and volatile components of red date

      2023, 40(2).

      Abstract (91) HTML (0) PDF 549.21 K (466) Comment (0) Favorites

      Abstract:Drying red dates through hot air drying, vacuum freeze drying and microwave vacuum drying, the volatile components of date slices were analyzed using headspace solid-phase microextraction-gas chromatography-mass spectrometry and electronic nose, and the effects of the three drying methods on the color, kinetics and volatile components of date slices were compared. The experimental results showed that hot air drying and microwave vacuum drying have greater influence on the color of date slices, and vacuum freeze drying can better maintain the original color; by fitting the kinetic equations, the Page model was found to be the most suitable mathematical model for predicting the drying characteristics of the three drying methods of date slices; significant differences in the types and relative contents of volatile components of date slices by drying, there were a total of 19 volatile components that were identical in date slices before and after drying. The volatile substances mainly included acids, esters, alcohols, aldehydes, ketones, hydrocarbons, heterocyclic substances and other compounds, and the relative contents of volatile components of acids and alkanes in date slices increased significantly after drying, while aldehydes and heterocyclic substances decreased significantly. The electronic nose results showed that the aroma characteristics of the dried date slices were different from those of fresh red date, and the aroma characteristics of hot air drying and microwave vacuum drying were closer and caramel aroma characteristics of date slices dried by microwave vacuum was more prominent. Compared with hot air drying and vacuum freeze drying, microwave vacuum drying is more suitable for preparing dried date slices because of its higher efficiency, lower energy consumption and less time consuming.

    • Comparison of deproteinization methods of alkaline-extracted crude polysaccharide from Bletilla striata and its antioxidant activity

      2023, 40(2).

      Abstract (162) HTML (0) PDF 657.21 K (541) Comment (0) Favorites

      Abstract:The alkaline-extracted crude polysaccharide from Bletilla Striata (BSP-A) was used to compare the effect of protein removal by TCA method, TCA+n-butanol method, macroporous resin AB-8 adsorption method, papain method, Sevage method, and three-phase separation method. The polysaccharide retention and protein removal yield were used as important indicators, and the polysaccharide structure and biological activity were explored to determine a more suitable method for polysaccharide purification. The results showed that Sevage, papain, and three-phase separation methods could retain more than 80% of polysaccharides with relatively mild reactions. TCA method, TCA+n-butanol method, and macroporous resin AB-8 adsorption method had the best results in deproteinization, of which the highest could reach 90%. Different deproteinization methods slightly affected the molecular weight of BSP-A, while the three-phase separation method and TCA+n-butanol method affected the composition ratio of mannose and glucose of BSP-A. These six methods affected the zeta potential and FT-IR characteristics of BSP-A, among which the papain and Sevage methods could better retain the antioxidant activity. In general, Sevage method was a polysaccharide deproteinization method with good retention of polysaccharide structure and activity but low deproteinization efficiency, and it can be one of the compelling methods to remove free protein from BSP-A.

    • >Catalysis,separation and purification technology
    • Snowflake Cu2S/defective UiO-66 p-n heterojunction for photocatalytic reduction of Cr(VI)

      2023, 40(2).

      Abstract (108) HTML (0) PDF 1.61 M (498) Comment (0) Favorites

      Abstract:To solve the problems of poor visible light response and rapid electron-hole recombination of metal-organic skeleton material UiO-66, snowflake Cu2S was used as the substrate for the defect control of UiO-66, as a result, Cu2S/defective UiO-66 composite photocatalyst with p-n heterojunction was prepared by solvothermal method. The photocatalytic reduction of Cr(VI) in K2Cr2O7 solution was investigated. The results of SEM, XRD and XPS showed that the defective UiO-66 grew uniformly on Cu2S. A tight p-n heterojunction between Cu2S and defective UiO-66 was formed, which improved the utilization rate of the material to visible light and promoted the effective separation of photogenerated electron-hole pairs. Under visible light irradiation, the reduction rate of 20 mg 28% Cu2S/defective UiO-66 composite photocatalyst (28% is loading amount of defective UiO-66, based on the mass of generated Cu2S) for 50 mL 20 mg/L K2Cr2O7 solution reached to 98.92%, as well as the reduction rate of Cr(VI) still reached 96.27% after 5 cycles. The synergistic effect of defect regulation and heterojunction construction can not only effectively solve the problem of easy agglomeration of defective UiO-66 nano-catalyst, but also improve the photocatalytic reduction performance of UiO-66.

    • Dinuclear aluminum complexes bearing anilido-aldimine ligands: synthesis, structures, and ring-opening polymerization catalysis of ε-caprolactone

      2023, 40(2).

      Abstract (91) HTML (0) PDF 646.29 K (522) Comment (0) Favorites

      Abstract:The anilido-aldimine chelating ligands (1R,2R)-[(NHAr)C6H4CH=N]2C6H10 (Ⅱ: Ar = C6H5; Ⅲ: Ar = 2,6-Me2C6H3) reacted with Al(CH3)3 to afford dinuclear aluminum complexes (Ⅳ, Ⅴ), respectively. All the complexes were characterized by 1H and 13C NMR spectroscopies. Complex Ⅴ was additionally characterized by single crystal X-ray diffraction analyses. The X-ray analysis reveals that the molecular contains two aluminum centrals and single ligand. Catalysis of the aluminum complexes Ⅳ, Ⅴ towards the ring-opening polymerization of ε-caprolactone was investigated in the presence of benzyl alcohol. All the polymerization reactions proceed in a controlled/living manner. The conversion exceeds 97% within 1.5 min using n(ε-caprolactone)∶n(BnOH)∶n(Ⅳ or Ⅴ) =200∶4∶1. Turn over frequency for Ⅳ is 7840 h–1, and for Ⅴ is 9700 h–1, much higher than the ethyl-bridged binuclear aluminum complex (1152 h-1) and the mononuclear amine-imine aluminum complex (2550 h-1). The polymerization reactions proceed in a controlled manner.

    • >Drug and cosmetic materials
    • Fabrication of glucose-responsive double drug delivery system for the release of insulin and cyclic adenosine monophosphate

      2023, 40(2).

      Abstract (85) HTML (0) PDF 1.56 M (409) Comment (0) Favorites

      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
    • Structure and properties of regenerated microcrystalline cellulose from ethanol grading

      2023, 40(2).

      Abstract (185) HTML (0) PDF 698.84 K (563) Comment (0) Favorites

      Abstract:Graded regeneration microcrystalline cellulose (MCC) were obtained by adding anhydrous ethanol with various weight in NaOH/ urea solution of MCC. The degree of polymerization of the regenerated MCC was determined by viscometer method. The structure, crystallinity, thermal stability and morphology of regenerated MCC were characterized by FTIR, XRD, XPS, TGA and SEM respectively.The results showed that the degree of polymerization of regenerated MCC decreased from 203 to 77 with the increasing grading times with ethanol. The SEM results showed that morphology of MCC changed from smooth rod fiber structure to rough and porous structure after regeneration. FTIR and XRD results indicated that the crystallization phase of regenerated MCC changed from typeⅠto type Ⅱ, and the amorphous region increased. After the third time grading by ethanol, the crystallinity of MCC decreased from 64.4% to 31.9%. XPS results showed that in regenerated MCC the binding energy and relative content of free hydroxyl group increased, resulting in the decreasing trend of crystallinity. TG results showed that the thermal stability of regenerated MCC decreased with the increasing grading times, and the initial decomposition temperature decreased from 310 °C to 257 °C after the third-time regeneration.

    • >Electro-organic chemistry and industry
    • Preparation and methanol electrooxidation performance of composite Pd-Co/CNT catalyst

      2023, 40(2).

      Abstract (58) HTML (0) PDF 1.52 M (474) Comment (0) Favorites

      Abstract:Pd nanocatalyst is an excellent anode catalyst for alkaline direct methanol fuel cell. The performance of the Pd catalyst can be improved through synergistic effect by adding a transition metal. Carbon nanotube supported non-alloyed Pd-Co bimetallic nano-catalysts were prepared by a step-by-step ethylene glycol reduction method, and their performances for methanol electrooxidation were investigated. The results show that the introduction of Co can improve the dispersion of Pd nanoparticles so as to increase the electrochemical surface area of the catalyst, and significantly improve the kinetic property of the catalyst. The cyclic voltammetry test showed that the peak current density of methanol oxidation over Pd-Co/CNT(1:0.2) catalyst was about 2.7 times that of Pd/CNT catalyst. The chronoamperometry test indicated that Pd-Co/CNT(1:0.2) catalyst had a lower activity decay rate than Pd-Co/CNT catalyst, showing a strong anti-poisoning ability. The improvement in the performance of Pd-Co/CNT catalyst is attributed to the synergistic interaction between Pd and Co. Yet, the current protocol can be used to grow and assemble other multi-metallic catalysts.

    • Electrochemical behavior and removal of copper in the hydrometallurgical recycling process of waste lead-acid battery

      2023, 40(2).

      Abstract (85) HTML (0) PDF 1.57 M (494) Comment (0) Favorites

      Abstract:The electrochemical behavior and purification method and principle of typical Cu2+ impurity in the recovery process of waste lead paste based on Methanesulfonic acid (MSA) were studied. The research results show that Cu2+ is preferentially precipitated over Pb2+ in the electrolysis process, resulting in a decrease in the purity of electrolytic lead, a decrease in the current efficiency of lead reduction and an increase in energy consumption. The existence of Cu2+ changes the nucleation mechanism of Pb2+, thus making the reduction potential of Pb2+ shift positively. Based on the principle of removing copper with lead powder, the fluidized purification process is proposed to replace the traditional stirring replacement method according to the characteristics of lead methanesulfonate system, which solves the problems of the large consumption of lead powder, high purification cost, and low efficiency. When the particle size of lead powder is 100 ~ 150 mesh, the temperature is 20 ℃, the flow rate is 8 ~ 10 m/h, and the height of the filled lead powder column is 0.6 ~ 0.7 cm. The removal rate of Cu2+ can reach more than 90% in the purification process of actual leaching solution from waste lead paste.

    • >Water treatment technology and environmental protection
    • Preparation of UiO-66-NH2/MoS2@PUF for absorption of Cr(Ⅵ)

      2023, 40(2).

      Abstract (112) HTML (0) PDF 5.93 M (537) Comment (0) Favorites

      Abstract:In order to solve the problem of difficult recovery of metal-organic skeleton material UiO-66 in water and further improve the adsorption efficiency of UiO-66 to Cr(Ⅵ), molybdenum disulfide (MoS2) was doped to prepare UiO-66-NH2/MoS2. Then, the composite material was uniformly grown on polyurethane foam (PUF) by in-situ growth method to prepare the composite material UiO-66-NH2/MoS2@PUF. UiO-66-NH2/MoS2@PUF were characterized by XRD, SEM, TEM, TGA and BET. The results showed that UiO-66-NH2/MoS2 was uniformly loaded on the surface of PUF and the loading rate was up to 28%. The application experiment results showed that when pH was 4, the removal rate of Cr(Ⅵ) reached to 89%. After 5 cycles of adsorption, the removal rate of UiO-66-NH2/MoS2@PUF to Cr(Ⅵ) still was 83%, which indicated that UiO-66-NH2/MoS2@PUF had good recyclability. The concentration of Zr(Ⅳ) in the residual solution after Cr(Ⅵ) adsorption was analyzed. The concentration of Zr(Ⅳ) was 0.0785 mg/L, which indicated that the leakage of Zr(Ⅳ) during the adsorption process can be negligible and proved that UiO-66-NH2/MoS2@PUF had excellent chemical stability. The results showed that quasi-second-order kinetic model and Langmuir model can describe the adsorption process of UiO-66-NH2/MoS2@PUF to Cr(Ⅵ) well.

    • Preparation and properties of solvent-resistant composite nanofiltration membrane with PDA-UiO-66 interlayer

      2023, 40(2).

      Abstract (97) HTML (0) PDF 3.94 M (678) Comment (0) Favorites

      Abstract:In this study, dopamine and UiO-66 nanoparticles were co-deposited on polyetherimide (PEI) base membrane crosslinked by 1,6-hexamethylenediamine to construct PDA-UiO-66 nanocomposite interlayer, and the solvent-resistant composite nanofiltration membrane (TFN-U) was prepared by interfacial polymerization on the interlayer. The membrane structure was characterized and analyzed by FTIR, XRD, SEM, AFM, water contact angle meter, etc. Meanwhile, the influence of UiO-66 mass concentration on the solvent resistance, pollution resistance and operation stability of TFN-U membrane was explored. The results show that the introduction of PDA-UiO-66 nanocomposite interlayer can improve the permeation flux of TFN-U membrane. When the mass concentration of UiO-66 nanoparticles is 0.2 g/L, the pure water flux of TFN-U2 membrane is increased to 63.83 L/(m2 h) and the methanol flux is 28.50 L/(m2 h), and the rejection rate of Congo red aqueous solution and Congo red methanol solution can still maintain 98.24 and 93.16%. After soaking in anhydrous ethanol, acetone, ethyl acetate, n-hexane and DMF for 24 hours, the rejection rate of Congo red remained above 94%, and the flux recovery rate reached 78.1%. After continuously filtering Congo red methanol solution for 24 hours, the methanol flux of the membrane was 14.13 L/(m2 h) and the rejection rate was 98.29%, which indicated that TFN-U2 membrane had good solvent resistance, pollution resistance and certain stability.

    • Cerium-nitrogen modified hydrochar for efficient degradation of Tetracycline hydrochloride via potassium persulfate activation

      2023, 40(2).

      Abstract (91) HTML (0) PDF 1.73 M (486) Comment (0) Favorites

      Abstract:Advanced Oxidation Process is widely used in the field of organic pollution degradation, but some problems still exist such as poor catalytic durability and low atomic utilization, which hinder the improvement of its activation performance. In this paper, cerium nitrogen modified hydrochar(Ce-N-HTC) with high catalytic performance was prepared by microwave hydrothermal method from cow dung, urea (C2H4N4) and cerium nitrate hexahydrate (Ce (NO3) 3·6H2O). The performance of the catalyst was evaluated by activating potassium persulfate to degrade tetracycline hydrochloride (TCH). When pH is 7.0,Ce0.3-N-HTC can degrade TCH up to 90.32% in 70 minutes, and bicarbonate ion has a great influence on the degradation rate of TCH. Competitive radical quenching experiment and electron paramagnetic resonance (EPR) experiment showed that the catalyst could degrade tetracycline through radical (·OH) and Noradical (1O2). After 6 cycles of experiments, the degradation rate of TCH can still be maintained above 75%, indicating that the prepared Ce-N-HTC has good stability and recoverability.

    • Preparation and adsorption properties of polyamine modified dialdehyde chitosan

      2023, 40(2).

      Abstract (404) HTML (0) PDF 1.06 M (614) Comment (0) Favorites

      Abstract:In this work, an environmentally friendly polydopamine-modified dialdehyde chitosan (PDA/DCS) was synthesized by the polydopamine (PDA) grafted with dialdehyde chitosan (DCS). The DCS was prepared via sodium periodate selective oxidation of the chitosan (CS). In order to characterize the micro morphology and chemical structure of the modified chitosan, SEM, FTIR, and other tests were performed. The adsorption abilities were studied using the carmine as a model pollutants. As the results revealed, the CS molecular was produce the covalent binding with PDA due to the formation of the aldehyde group by sodium periodate oxidation reaction. A key factor in the improved adsorption abilities of DCS and PDA/DCS was the selective oxidation treatment. Compared with the pristine CS, the crystallinity of DCS dropped sharply, while the porosity and specific surface area were increased. In addition, the microstructure of PDA/DCS presents a dense porous structure. The adsorption processes of DCS and PDA/DCS both followed the quasi-second-order kinetic equation and Langmuir isothermal model. Moreover, the adsorption rate and capacity of PDA/DCS were significantly enhanced in comparison to the DCS. When the initial mass concentration of dye is 700 mg/L, the maximum monolayer adsorption capacity of PDA/DCS was 1194.4 mg/g. Even after the fifth recycling, the synthetic adsorbent can still reach 616.90 mg/g adsorption capacity.

    • >Dyeing and finishing auxiliaries
    • Synthesis of siloxane oligomer and its application in foam dyeing

      2023, 40(2).

      Abstract (76) HTML (0) PDF 823.74 K (441) Comment (0) Favorites

      Abstract:Abstract: In order to improve the dyeing properties of cotton fabric via foam dyeing and photocuring, a siloxane oligomer containing unsaturated double bonds was synthesized. A suitable foam system containing yellow anthraquinone dye, siloxane oligomer, photoinitiator of Diphenyl (2,4,6-trimethylbenzoyl) phosphine oxide(TPO), and surfactant of sodium dodecyl sulfate(SDS) for foam dyeing of cotton fabrics was designed. The chemical structure and molecular weight distribution of siloxane oligomers was analyzed by 1H-NMR and GPC. The chemical structure of siloxane oligomer and dyed cotton fabric was characterized by FTIR. The morphology of dyed cotton fabric was observed by SEM. The effects of amount of oligomer, amount of dye, concentration of surfactant, amount of photoinitiator on foam performance and dyeing performance were discussed. The results showed that K/S value of 5.70 , the colo fastness to soaping and to dry /wet rubbing of 4-5, ultraviolet protection factor >50 and water contact angle of 110.1°were achieved under the conditions of the concentration of dye solution of 30 g/L, the ratio of oligomer/dye of 2:1, the concentration of SDS of 2 g/L, TPO amount of 5% on the mass of monomer, and UV irradiation time of 5 min. The siloxane oligomer undergoes radical polymerization through the unsaturated double bonds on the side groups and silanol group coupling and crosslinking to achieve color fixation and gives the fabric good hydrophobic properties and anti - ultraviolet properties.

    • >Papermaking chemicals
    • Preparation and properties of high strength and high modulus polyethylene fiber/plant fiber paper-based composite materials

      2023, 40(2).

      Abstract (68) HTML (0) PDF 1.39 M (483) Comment (0) Favorites

      Abstract:High strength and high modulus polyethylene (UHMWPE) staple fiber and softwood pulp were used as raw materials to prepare UHMWPE fiber paper-based composites materials by wet forming technology combined with resin impregnation and hot pressing. The effects of base paper preparation technology and hot pressing technology on UHMWPE fiber paper-based composite materials were investigated. The results show that, in a certain range, the mechanical properties of paper-based composites materials are improved and the pore size distribution is more uniform with the increase of quantity, beating degree of softwood pulp and proportion of softwood pulp. Phenolic resin impregnation and hot pressing treatment can further improve the mechanical properties of paper-based composite materials (tensile index increased by 3.8 times), and has lower dielectric constant and dielectric loss factor.

    • >Adhesives
    • Effect of side chain long alkyl on adhesion of waterborne polyurethane on non-polar substrate

      2023, 40(2).

      Abstract (41) HTML (0) PDF 609.58 K (499) Comment (0) Favorites

      Abstract:A series of waterborne polyurethane emulsions containing long-chain alkyl groups in side chains were prepared using polyneopentyl adipate (PNA), dimer acid polyester polyol (BY3026) and isophorone diisocyanate (IPDI) as the main raw materials. The structure of the film was characterized by infrared test, and the properties of the emulsion and films were analyzed by tests such as particle size, mechanical stretching, water absorption, contact angle and adhesion on biaxially oriented polypropylene film (BOPP). The results show that when the mass ratio of BY3026 to PNA increases from 0% to 60%, the particle size of the emulsion increases, the water resistance of the film increases, and the surface energy first decreases and then increases, the tensile strength and elongation at break decreased from 52.6 MPa and 2607.2% to 38.7 MPa and 1911.2% respectively. When m(BY3026):m(PNA)=2:5, polyurethane has the best compatibility with BOPP film, the surface energy is 35.41 mJ/m2, and the T-peel strength on BOPP film is 2.98 N/25 mm.

    • >Building chemicals
    • Synthesis and corrosion inhibitory of N,N '-bis(4,6-diamino acid-1,3,5-triazinyl)-hexanediamine

      2023, 40(2).

      Abstract (80) HTML (0) PDF 1.51 M (498) Comment (0) Favorites

      Abstract:Four kinds of corrosion inhibitors, N,N'-bis[4,6-bis(2-aminoacetoxy)-1,3,5-triazinyl]-hexanediamine (TFYJ), N,N'-bis[4,6-bis (3-aminopropionyl)-1,3,5-triazinyl)]-hexanediamine (TFBJ), N,N'-bis[4,6-bis(4-aminobutyryl)-1 ,3,5-triazinyl)]-hexanediamine (TFDJ), N,N'-bis[4,6-bis(6-aminocaproic acid)-1,3,5-triazinyl)] -Hexylenediamine (TFJJ),was designed and synthesized by cyanuric chloride、amino acid(2-aminoacetic acid、3-aminopropionic acid、4-aminobutyric acid、6-aminocaproic acid)、1,6-hexanediamine. Its structure was characterized by FT-IR、1H NMR and MS. The corrosion inhibition of 45# carbon steel in 1 mol/L HCl was tested by weight loss method,electrochemical method and the corrosion inhibition mechanism was ananlyzed. The results showed that four types of target corrosion inhibitor had excellent corrsion inhibition effect on 45# carbon steel in 1 mol/L HCl. Preferably,the corrosion inhibition rate of TFJJ(100 mg/L)at 20 ℃ could reach 98.37 %(weight loss method). The Tafel curve showed that it was a mixed corrosion inhibitor,dominated by cathodes. The adsorption thermodynamics showed that TFJJ conformed to the Langmuir isotherm adsorption equation, and the adsorption process was mainly chemical adsorption. EHOMO, ELUMO, Fukui index, etc. of TFJJ were obtained by quantitative calculation, which proved that the corrosion inhibition of TFJJ occured on the N atom of the triazine ring and amino group, and the C and O atoms of the carboxylic acid group. Compared with the commercially available NUEF485, the corrosion inhibition rate of the product synthesized in this paper is increased by 5.25 %~9.44 %, and it still had good hard water resistance under 600 mg/L hard water.

    • >Fine chemical intermediates
    • Process and simulation of synthesis of cyclic carbonate in microreactor

      2023, 40(2).

      Abstract (102) HTML (0) PDF 1.09 M (664) Comment (0) Favorites

      Abstract:The continuous microreactor process for the synthesis of cyclic carbonates by the coupling reaction of epoxide and CO2 was designed, using an intramolecular bifunctional catalyst. The effects of catalyst loading, temperature, pressure, and ratio of CO2 to epoxide on the coupling reaction were investigated. The experimental results show that the epoxide can be efficiently converted to the corresponding cyclic carbonate even at mild conditions (120 °C, 1.5 MPa), lower catalyst concentrations (0.5‰ mol), the conversion rate of epoxide can reach 78% within 30 s. Under the same conditions, the continuous microreactor process exhibited 1.8 times efficiency to that of the traditional tank reaction process. These results indicate that the designed microchannel reaction process can significantly enhance the gas-liquid mixing mass transfer during the reaction. Fluent software was used to simulate the gas-liquid mixing in the microreactor for exploring the effect of different working conditions on the CO2-epoxide mixing. Combined with the analysis of experimental results, it is shown that the gas disturbance plays a key factor in affecting gas-liquid mixing.