• Volume 37,Issue 2,2020 Table of Contents
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    • >Review and monographs
    • New development of photoinitiators for UV-LED curing system

      2020, 37(2).

      Abstract (1645) HTML (0) PDF 706.77 K (0) Comment (0) Favorites

      Abstract:The research progress of photoinitiatios that used in UV-LED curing system was reviewed, which including traditional photoinitiators and their derivatives (thioxanenones, diphenylmethyl ketones and acylphosphine oxides), photoinitiators of new groups (carbazolidyl, naphthalimide, phenazinyl, phenylmalinyl, imidazolidyl and triazinyl) and macromolecular photoinitiators. The stability of photoinitiator can be improved through the modification of traditional photoinitiator and synthesis of macromolecular photoinitiator. The absorption wavelength of the new photoinitiator has a good match with the emission wavelength of UV-LED curing, while this kind of photoinitiator often needs auxiliary agent. Furthermore, the influence of oxygen inhibition on photocuring system is described, the shortcomings of photoinitiators are pointed out and the development and the application of photoinitiators in the future is prospected

    • Research Progress on the Reaction Mechanism of Methanol to Hydrocarbons

      2020, 37(2).

      Abstract (787) HTML (0) PDF 2.18 M (0) Comment (0) Favorites

      Abstract:Methanol to hydrocarbon (MTH) reaction is an important way to prepare various hydrocarbons from non-oil routes, which has important basic research and industrial application value, and has become one of the research hotspots of coal-based alternative energy sources. However, there is still much debate about the understanding of the reaction mechanism of methanol-based hydrocarbons and the confirmation of reaction steps. The complex reaction network limited the analysis and verification of the reaction mechanism, thus slowing down the design of the reactor and development process of technology in these reactions. In this review, the main progress of the reaction mechanism of MTH in recent years is summarized from the two aspects: direct mechanism and indirect mechanism. The double-cycle catalytic mechanism of the hydrocarbon pool accepted widely was highlighted. The MTH hydrocarbon pool mechanism involved six major chemical processes: olefin methylation, olefin cracking, hydrogen transfer, cyclization, aromatic methylation and aromatic dealkylation. A systematic understanding of the mechanism of the reaction provides a theoretical basis, with accurately designing crystal shape, size, pore structure of the catalyst, as well as regulating of the distribution of acidic sites, which lays a foundation for the establishment of the catalytic structure-activity relationship of this complex reaction. This is of great significance to the industrialization process of the development of coal chemical industry.

    • Research Progress on Anti-skin Photoaging of Plant Extracts

      2020, 37(2).

      Abstract (545) HTML (0) PDF 431.73 K (0) Comment (0) Favorites

      Abstract:Abstract: Ultraviolet (UV) radiation is a major cause of skin photoaging. In recent years, the prevention of UV damage to the skin has been valued by the public, and the exploring of the photoaging prevention active substances has become a research hotspot. This article introduces the effect of UV on the skin and the mechanisms of photoaging. Different pathways are reviewed, including UV absorption, anti-oxidation, regulation of extracellular matrix synthesis and decomposition, inhibition of pigmentation, relief of skin inflammation and regulation of autophagy of different plant extracts delay the ageing of the skin light effect, in order to provide reference for the research and application of natural plant photoprotective functional cosmetics.

    • >Functional materials
    • Synthesis and Thermal Behavior of 5-Cyano-4-Aminoimidazole

      2020, 37(2).

      Abstract (588) HTML (0) PDF 496.51 K (0) Comment (0) Favorites

      Abstract:Imidazole based energetic compounds are one of the important directions on high energy compounds, and 5-cyano-4-aminoimidazole is the key intermediate for the design and synthesis of novel tetrazoyl imidaz-ole high energy and high nitrogen content compounds. With 5-carboxamide-4-amino imidazole (AICON) as raw material, the target compound 5-cyano-4-aminoimidazole (AICN) was obtained by its dehydration reaction with phosphoryl trichloride (POCl3). Through optimization of reaction system, reaction tempera-ture, reaction time and molar ratio, the yield and HPLC purity of AICN could achieve higher than 65% and 99.5%, respectively. Besides, the target compound was characterized by NMR, IR and element anal-ysis, and its thermal properties were investigated by TG. Results showed that the optimum reaction condi-tions was as follows: taking POCl3 as dehydrant, n(AICON) : n(POCl3) was 1:10, and reaction heating mode was that the reaction temperature rised rapidly to 80-85 ℃, maintained for 30 minutes, then de-creased to 70-75 ℃, and maintained for 1-1.5 h; there were two mass loss stages of AICN existed in the range of 40-1000 ℃, the corresponding decomposition temperature regions were 40-400 ℃ and 400-1000 ℃, the corresponding mass losses were 19.8% and 60.7%, and the peak values of thermal de-composition temperatures was 256.5 ℃ and 698.4 ℃, respectively, which indicated that 5-cyano-4-aminoimidazole had good thermal stability.

    • Preparation and Properties of Luminescent Thermo-sensitive Hydrogel doped with Upconversion Nanoparticles

      2020, 37(2).

      Abstract (4543) HTML (0) PDF 3.08 M (15) Comment (0) Favorites

      Abstract:Water-dispersive upconversion nanoparticles(UC@PEI NPs) were synthesized by hydrothermal method using polyethyleneimine(PEI) as surface modification agent. The effects of solvent components, reaction time, PEI molecular weight and addition amount on luminescence intensity were investigated and characterized. The results showed that the optimal synthesis conditions were V(H2O):V(EG) = 1:1, PEI(Mw = 10000) was added 1.2 g, and reacted at 200 ℃ for 8 h. Subsequently, in the presence of UC@PEI NPs and poly(N-isopropylacrylamide)(PNIPAM), acrylamide, N,N'-methylenebisacrylamide were copolymer-ized by free radical polymerization to prepare composite hydrogel. The morphology, mechanical strength and luminescent thermo-sensitive were characterized by SEM, tensile testing machine and luminescence spectrometer. The results showed that composite hydrogel with the interpenetrating network structure still remained intact after repeated dehydration and swelling, and the average dehydration ratio and swelling ratio were 81.18% and 61.38%; the strain under stress was 251.10%, and the mechanical strength was 38.09 kPa; under the excitation of 980 nm NIR laser, the luminescence intensity at 540 nm(Er3+, 4S3/2 → 4I15/2) decreases by 42.64% when the temperature rises from 20 ℃ to 48 ℃, and the luminescence intensity can be reversibly recovered when the temperature decreases. This shows that the composite hydrogel has the properties of reversible upconversion luminescent thermo-sensitive, good material stability, good stretchability, and has a certain mechanical strength.

    • Synthesis and properties of a class of high transparent polyimides containing methyl structure

      2020, 37(2).

      Abstract (599) HTML (0) PDF 592.83 K (0) Comment (0) Favorites

      Abstract:A series of soluble methyl-containing polyimides (MPI) were prepared by a one-step high-temperature copolymerization using 2,6-diaminotoluene(TDA), 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride(ODPA) and 3,3',4,4'-biphenyltetracarboxylic dianhydride(BPDA) as monomers and m-cresol as the solvent. Their structures and properties were tested by FTIR, 1HNMR, DSC, TGA, UV, etc. The series of methyl-containing polyimides had good solubility in NMP, DMAc, DMSO, DMF, CH2Cl2 and CHCl3 at room temperature, and their solubility decreased as increasing of the content of biphenyl anhydride. The obtained films showed good optical transmission properties, and the transmittance at the ultraviolet light wavelength of 450 nm was above 74%, and the cutoff wavelengths were around 350 nm. The series of polyimides also had good thermal properties. The initial decomposition temperatures of this series of MPI were more than 457 °C, and their glass transition temperatures were in the range of 260 °C~285 °C. The elastic modulus, tensile strength and elongation at break of the prepared films were in the range of 1.7~2.1 GPa, 89.7~120.6 MPa and 19.7%~28.4%, respectively.

    • Preparation and Application of bi-functional BaTiO3/CA films

      2020, 37(2).

      Abstract (396) HTML (0) PDF 1.14 M (0) Comment (0) Favorites

      Abstract:Bi-functional BaTiO3/CA films were prepared with 500 nm BaTiO3 microspheres and cellulose acetate. SEM, contact angle meter, and UV-visible spectrophotometer were used to characterize them. The effect of BaTiO3 morphology, mass ratio of CA to BaTiO3, mixing time, different surfactants and dosages, solid content and films thickness on morphology, diffusion performance and light reflectivity of bi-functional films were studied. The optimal condition for preparing the bi-functional film were as follows: BaTiO3 was 500 nm microspheres. Mass ratio of CA to BaTiO3 was 0.05. Mixing time was more than 4 h. Surfactants was Triton X-100 which dosages was 20 μL/ 10 g (Triton X-100/ BaTiO3). Solid content was 44.9% and film thickness was 0.4 mm. Bi-functional films prepared in the condition were smooth and thermal stable. The light reflectivity of the bi-functional BaTiO3 film in the 460~800 nm range was higher than 97.5%. Serum diffused in the bi-functional BaTiO3 film reacted in the reagent film and then formed uniform colorful spots. The SD of the diameter of the five parallel samples was 0.055, which showed a good repeatability. The linear range of GLU and URIC reagents prepared with BaTiO3/CA bi-functional films was wider than that prepared with TiO2/CA films.

    • Preparation and Electrochemical Performance of Graphene/SnO2/Si@PPy Composite

      2020, 37(2).

      Abstract (420) HTML (0) PDF 1.69 M (0) Comment (0) Favorites

      Abstract:Graphene/SnO2 (GS) composites were synthesized from graphene oxide and SnCl2 by microwave hydrothermal method. Using ammonium persulfate as initiator, the coating structure of Si@PPy (SP) was prepared by in situ oxidation polymerization of pyrrole on the surface of Si powders. Graphene/SnO2/Si@PPy (GSSP) composites were prepared by microwave hydrothermal assembly method. The morphology and structure of GS, SP and GSSP were characterized by SEM, TEM, XRD, Raman and BET. The half-cells were assembled with GSSP composite as anode, and then the electrochemical properties were tested, such as rate performance, cyclic performance, CV and EIS. The results showed that the GSSP composite had excellent rate performance. At a current density of 100 mA/g, the average specific capacity of discharge and charge is 948.44 mAh/g and 869.63 mAh/g, respectively. Under the current density of 1000 mA/g, the specific capacity retention rate after 400 cycles of discharge and charge was up to 90.69% and 89.34%.

    • Preparation and Performance Characterization of Superhydrophobic Near- infrared Absorption Coating

      2020, 37(2).

      Abstract (617) HTML (0) PDF 1.50 M (0) Comment (0) Favorites

      Abstract:Through reasonable coating structural design, polydimethylsiloxane(PDMS)/Sm2O3 composite coating with superhydrophobic property was prepared by scratch coating method using nano-SiO2, PDMS and Sm2O3 particles as micro-nano structural modifier, adhesives and functional pigments, respectively. The effects of the ratio of PDMS to Sm2O3, the addition amount of nano-SiO2 and the surface micro-nano structural layer on the coating properties were discussed. The results show that the ratio of PDMS to Sm2O3 (mass ratio) has an important effect on the coating properties. When m(PDMS):m(Sm2O3)=6:4, the reflectance of the coating to the 1.06 μm near-infrared light can be as low as 58.8%. The water contact angle can reach 113°, which is significantly higher than the conventional polyurethane-based near-infrared absorption coatings. The superhydrophobic property of the coating can be achieved by coating a PDMS/SiO2 micro-nano structural layer with a distinct papillary structure on the surface of the PDMS/Sm2O3 composite coating. After the surface of PDMS/Sm2O3 composite coating is coated by PDMS/SiO2 micro-nano structural layer with SiO2 mass fraction of 30%, the water contact angle can be increased to 158°, the roll angle can be as low as 4°, and has lower reflectance (61.4%) to the 1.06 μm near-infrared light.

    • Synthesis and Characterization of Zirconium-Based MOFs and Catalytic Preparation of Biodiesel

      2020, 37(2):0-0.

      Abstract (1345) HTML (0) PDF 1.26 M (1) Comment (1) Favorites

      Abstract:UiO-66 and its derivatives were synthesized by solvothermal synthesis of different organic ligands, such as terephthalic acid, 2-nitroterephthalic acid, 2-aminoterephthalic acid and 2-hydroxyterephthalic acid. In the synthesis, formic acid, acetic acid, benzoic acid and hydrochloric acid were used as different modulators to modulate the structure of zirconium-based MOFs. The zirconium-based MOFs were characterized by XRD, SEM and FT-IR. The effects of different modulators and additions on the morphology and structure of zirconium-based MOFs were investigated. It was found that the different modulators have different effects on the formation of zirconium-based MOFs. The hydrochloric acid and acetic acid mixture modulators can significantly improve the crystallinity of UiO-66. When the molar ratio of the regulator to ZrCl4 was 30, the benzoic acid modulator can obtain uniform UiO-66 octahedral crystal with dimensions of 500 nm, the formic acid modulators increased the specific surface area of UiO-66 from 1173.3 m2/g to 1973.8 m2/g. Three kinds of zirconium-based MOFs were selected as esterification reaction catalysts to obtain esterified oil. UiO-66-NH2 has good catalytic activity, and its free fatty acid conversion rate was 50.7%. The yield of biodiesel obtained by the reaction of KOH catalyzed esterification oil was 51.6%, and the methyl ester rate was as high as 99% or more.

    • Preparation and Responsive Properties of γ-FeOOH-g-PDMAEMA Stabilized Pickering Emulsion

      2020, 37(2):0-0.

      Abstract (501) HTML (0) PDF 2.69 M (1) Comment (0) Favorites

      Abstract:Initiator modified γ-FeOOH nanoparticles (γ-FeOOH-Br) were prepared by using FeSO4·7H2O as precursor, 2-bromoisobutyric acid as surface modifier with the aids of ethylenediamine under pH=9. Subsequently, double-responsive poly(2-(dimethylamino) ethyl methacrylate) (PDMAEMA) was grafted from γ-FeOOH-Br nanoparticles by surface initiated atomic transfer radical polymerization (SI-ATRP) method to obtain γ-FeOOH-g-PDMAEMA particle brushes, which were further used as a Pickering emulsifier to prepare Pickering emulsion. The obtained products were characterized systematically by SEM, TEM, FT-IR, TGA, Zeta potential, and particle size analyzer. The stability, pH and temperature response of particle brushes stabilized Pickering emulsion were studied. The results showed that the morphologies of both γ-FeOOH-Br and γ-FeOOH-g-PDMAEMA were needle-like. The size of γ-FeOOH-Br was about 700 nm long and about 50 nm wide, and the length and width of γ-FeOOH-g-PDMAEMA was increased to 710 nm and 80 nm, respectively. Due to the successful grafting of PDMAEMA onto the surface of initiator modified γ-FeOOH nanoparticles, γ-FeOOH-g-PDMAEMA emulsifier had a LCST of 35 ℃. The as-prepared Pickering emulsions were highly stable and demonstrated reversible pH and temperature dual responsiveness.

    • >Modernization technology of traditional Chinese medicines
    • Study on chemical constituents and antitumor activity of Amenone vitifolia

      2020, 37(2).

      Abstract (527) HTML (0) PDF 532.03 K (0) Comment (0) Favorites

      Abstract:The 70% ethanol extract of Anemone vitifolia in Enshi area of HuBei province was isolated and purified by column chromatography on silica gel, Sephadex LH-20 and preparative liquid chromatography. Structures were proved by physicochemical properties, NMR and MS.The antitumor activity was tested by MTT assay. Results 10 compounds, including lignin, flavonoidsand saponins, were obtained from 70% ethanol extract of Anemone vitifolia , and were identified trachelogenin (Ⅰ), arctigenin (Ⅱ), chlorogenic acid (Ⅲ), astragalin (Ⅳ), isoquercitrin (Ⅴ), tiliroside (Ⅵ), tracheloside (Ⅶ), arctiin (Ⅷ), salicin (Ⅸ) and dioscin (Ⅹ). CompoundsⅠ~Ⅱ、Ⅵ~Ⅶ、Ⅸ were isolated from the genus Amenone for the first time; Compounds Ⅰ~Ⅶ、Ⅸ、Ⅹ were isolated  from Amenone vitifolia for the first time. Compounds Ⅱ、Ⅷ、Ⅸ、Ⅹ inhibited the proliferation of HeLa cells with inhibition rates of 10.5%, 7.0%, 0.5% and 88.0% at 100 μmol/L, and the inhibition rate of compound Ⅹ was higher than that of the positive control cisplatin by 80.5%.

    • Optimization of Extraction of Total Phenolics and Total Flavonoids from Fruits of Phellodendron amurense by Response Surface Method and Their Antioxidant Activity

      2020, 37(2).

      Abstract (694) HTML (0) PDF 1.39 M (0) Comment (0) Favorites

      Abstract:On the basis of single-factor test, the extraction conditions of total phenolics (TP) and total flavonoids (TF) from fruits of Phellodendron amurense were analyzed and optimized by the Box-Behnken design, and studied the antioxidant activity of the extracts to determine their correlation. Results showed that, the optimal extraction conditions are as follows: ethanol volume fraction 43%, extraction temperature 72 ℃, pH value 11, ultrasonic power 500 W, liquid/material ratio 30:1 (mL/g), and extraction time 40 min. The yield of TP (expressed as mg of Gallic acid (GA) per gram P. amurense fruit) and TF (expressed as mg of rutin (RT) per gram P. amurense fruit) were 7.09 ± 0.38 mg GA/g and 20.41 ± 0.47 mg RT/g under these conditions. Results showed that there is a significant correlation between in vitro antioxidant activity and contents of TP and TF(P<0.01).and TF(P<0.01). This work would provide a basis for the further development of P. amurense.

    • >Catalysis,separation and purification technology
    • The catalytic performance of highly dispersed nickel-silica catalyst in quinoline hydrogenation

      2020, 37(2).

      Abstract (843) HTML (0) PDF 2.51 M (0) Comment (0) Favorites

      Abstract:A series of nickelphyllosilicate derived Ni-PS-AEH-x (different calcination temperatures, the same below) catalysts with a loading of 10% (mass fraction of ruthenium in a catalyst, the same below) nickel were prepared by ammonia evaporation hydrothermal method using nickel nitrate and silica sol as raw material. Ni-PS-AEH-400 was found to have the best catalytic performance by investigating the hydrogenation performance of different nickel-based catalysts. By investigating the influence of reaction conditions, the optimal reaction conditions were as follows: molar ratio of quinoline : Ni is 30 : 1, reaction temperature was 100 ℃, hydrogen pressure was 3 MPa, reaction time was 120 min, and the quinoline conversion rate was 99.0%, the yield of 1,2,3,4-tetrahydroquinoline was 95.4%.The structure, composition and morphol-ogy of catalysts were characterized by XRD, TEM, N2 adsorption-desorption, H2-TPR, and XPS. The re-sults indicated that Ni-PS-AEH-400 exhibited better catalytic performance, attributed to larger specific surface area, active particle higher dispersion and stronger interaction between the active particles and the support compared with Ni/SiO2-IMP prepared by impregnation method.

    • Synthesis and Catalytic Properties of [(N-Heterocyclic carbene) Pd (ferrocenyl-allyl) Cl]

      2020, 37(2).

      Abstract (525) HTML (0) PDF 523.47 K (0) Comment (0) Favorites

      Abstract:[(N-Heterocyclic carbene)Pd(ferrocenyl-allyl)Cl] II was prepared easily in good yield by simple addition of THF solution of 1, 3-bis (2, 6-diisopropylphenyl) imidazolium chloride (IPrHCl) to chloride-bridged ferrocenyl-allyl-Pd dimer I at room temperature. The one-pot synthesis avoids multi-step reactions employing free carbene. Complex II was characterized by IR, 1H NMR, 13C NMR, MS and HRMS. Additionally, the detailed structure has been determined by single-crystal X-ray analysis. Complex II was stable to air and moisture, and displayed high catalytic activities for the Suzuki-Miyaura coupling reaction of a variety of aryl chlorides with aryl boronic acids with catalyst loadings of 0.4 mol % at 70 oC, and the Buchwald-Hartwig amination of chlorobenzene with various amines in the presence of 0.5 mol% complex II at 100 oC.

    • Preparation of Iron Oxide by Precursor Method and Its Catalytic Performance

      2020, 37(2).

      Abstract (547) HTML (0) PDF 1.16 M (0) Comment (0) Favorites

      Abstract:Fe3O4(named as Fe3O4-PR) was prepared by the precursor method from FeSO4 ,a byproduct of titanium dioxide, and it was used as a catalyst to catalyze the degradation of active brilliant red X-3B by H2O2. The effects of pH, H2O2 dosage and Fe3O4-PR dosage on the catalytic degradation reaction were investigated. And it was explored that the catalytic activity and stability of Fe3O4-PR. Finally, the mechanism of the catalytic degradation reaction was investigated. XRD, FT-IR, SEM and particle size analysis showed that the multi-faceted three-dimensional structure Fe3O4 with an average particle size of 410 nm could be successfully prepared by the precursor method. Under the conditions of pH=3, H2O2 dosage of 3 mM and Fe3O4-PR dosage of 1g/L, the degradation rate of reactive brilliant red X-3B was 97%, and the TOC removal rate was 47%. Fe3O4-PR not only has good stability, but also has better catalytic activity than Fe3O4(namedasFe3O4-CO) prepared by traditional chemical coprecipitation. The mechanism investigation shows that the catalytic degradation reaction occurs at the active site on the catalyst surface, and the redox cycle exists in the degradation process. ?OH is the main active material.

    • >Perfumes and essences
    • Effects of Enzymes on Taste of the Braised Pork Flavoring

      2020, 37(2).

      Abstract (455) HTML (0) PDF 1.62 M (0) Comment (0) Favorites

      Abstract:The effects of enzyme on the taste of the thermal reaction flavoring,the braised pork flavoring were investigated. Free amino acids in hydrolysate were analyzed by high performance liquid chromatography(HPLC). The taste of braised pork flavoring were analyzed by sensory evaluation and electronic tongue. The results showed that,the contents of bitter amino acids were the highest with 29.32 g/L,followed by the contents of umami amino acids with 10.21 g/L. The correlation analysis of sensory evaluation and electronic nose showed that the samples could be distinguished from each other by principal component analysis (PCA).

    • >Drug and cosmetic materials
    • Synthesis and Antioxidant Properties of Ferrocenyl Imid-azo[1,2-a]pyridine Compounds

      2020, 37(2).

      Abstract (683) HTML (0) PDF 641.74 K (0) Comment (0) Favorites

      Abstract:Five ferrocenyl imidazo[1,2-a]pyridine compounds were synthesized by Groeb-ke-Blackburn-Bienaym? three-component-reaction (GBB-3CR) among 2-aminopyridine, ferro-cenecarboxaldehyde, and isocyanide with LaCl3 being catalyst in ethanol. The structure of the com-pounds were confirmed by proton magnetic resonance (1H NMR), carbon-13 magnetic resonance (13C NMR), and ultra high performance liquid chromatograph electrospray ion source mass spec-trometer (UHPLC-ESI-MS). Antioxidant abilities of the obtained compounds were evaluated by in-hibiting HO?- and Cu2 /glutathione (GSH)-induced oxidation of DNA. The radical-scavenging prop-erties of the obtained compounds were estimated by quenching 2,2?-azinobis(3-ethylbenzothiazoline-6-sulfonate) cationic radical (ABTS?) and 2,2?-diphenyl- 1-picrylhydrazyl (DPPH?), and then the effects of substituents on the antioxidant properties of fer-rocenyl imidazo[1,2-a]pyridine compounds could be explored. The results showed that the TBARS percentages of five compounds were 65.4%~93.7% in inhibiting HO?- induced oxidation of DNA. The TBARS percentages of five compounds were 25.6%~62.5% in inhibiting GS?- induced oxidation of DNA. All five ferrocenyl imidazo[1,2-a]pyridine compounds could scavenge ABTS? and DPPH?. The compounds VI containing two ferrocenyls exhibits higher activity than other compounds in quenching radicals and inhibiting radicals induced oxidation of DNA.

    • >Food and feedstuff chemicals
    • Comparison of quality and electronic nose analysis of Camellia oleif-era Abel seed oil extracted by different methods

      2020, 37(2).

      Abstract (513) HTML (0) PDF 639.88 K (0) Comment (0) Favorites

      Abstract:Gas chromatography-mass spectrometry and chemical methods were used to determine the physical and chemical indicators and main sense of Camellia oleifera Abel seed oil extracted by different methods. The Camellia oleifera Abel seed oil extracted by three methods was analyzed and distinguished through using electronic nose technology. The results showed that there were significant differences in many phys-ical and chemical indicators of Camellia oleifera Abel seed oil extracted by different methods. The acid value, iodine value and peroxide value of the Camellia oleifera Abel seed oil extracted by the supercritical method were lower than two other Camellia oleifera Abel seed oil, and the peroxide value was signifi-cantly different from two other Camellia oleifera Abel seed oil; The neutral color indicators of three Ca-mellia oleifera Abel seed oil had significant differences. The Camellia oleifera Abel seed oil extracted by the cold pressing method was the lowest and the Camellia oleifera Abel seed oil extracted by the leaching method was the highest. The Camellia oleifera Abel seed oil extracted by the leaching method was lowest and the Camellia oleifera Abel seed oil extracted by the cold pressing method was the highest. The fatty acid composition and the production rate of the three Camellia oleifera Abel seed oil also differed, and fatty acid composition of the Camellia oleifera Abel seed oil extracted by Supercritical CO2 method was the highest, but the production rate of the leaching method was the highest. The results of the saponifica-tion values indicated that the differences were not significant. The principle component analysis of the Camellia oleifera Abel seed oil analyzed and distinguished by electronic nose technology showed that the main component cumulative variance contribution rate was 99.62%. The results of discriminant factor analysis showed that the cumulative contribution of the principal component was 100.00%, and the dis-criminant index was 88. The electronic nose technology can accurately identify Camellia oleifera Abel seed oil extracted by different processing methods.

    • Application of Multiple Headspace Solid Phase Microextraction in Quantification of Volatile Compounds in Daqu

      2020, 37(2).

      Abstract (676) HTML (0) PDF 1.16 M (0) Comment (0) Favorites

      Abstract:Headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) was used to analyze the medium high temperature Daqu in Gujing Gongjiu, and a total of 108 volatile compounds were identified. By examining the β values of the compounds under different sample amounts, multiple headspace solid-phase microextraction (MHS-SPME) was applied to quantify the aldehydes and ketones, phenols, nitrogen, furans, lactones, terpenes at the 35 and 50 mg samples, and a total of 46 compounds were quantified. The recoveries of the method ranged from 76.83%-133.11%, the limits of detection (LOD) were lower than 103.818 ppb, and the relative standard deviation (RSD%) were less than 21.34%, which showed the method had good sensitivity and repeatability. The experimental results showed that MHS-SPME could be applied to the quantitative analysis of these 46 compounds in Daqu. The contents of measured compounds ranged from 3645.79?442.43 ng/g (3-methyl-2(5H)-furanone) to 6.32?1.03 ng/g (3-ethylbenzaldehyde). This method provided a new idea for quantifying the volatile components in Daqu, and the results also provided data support for the enterprise to improve the Daqu quality evaluation system.

    • >Electro-organic chemistry and industry
    • Two-pot Synthesis of Carbon/Nitrogen double-doped Interconnected Fe3O4 Lithium Battery Anodes

      2020, 37(2).

      Abstract (538) HTML (0) PDF 1.02 M (0) Comment (0) Favorites

      Abstract:In this paper, interconnected Fe3O4of carbon/nitrogen double-doped(Fe3O4/C/N)was prepared by a simple and efficient two-pot method. Profiting from the advantages of carbon/nitrogen double-doped and massively interconnected nanoarchitecture, Fe3O4/C/N was characterized and analyzed by XRD, XPS, TG, SEM and TEM.Fe3O4/C/N show excellent reversible capacity and exceptional cycle performance when used as anode materials for lithium ion batteries.The initial coulomb efficiency of Fe3O4/C/N is 73.9% and maintain capacity of 516mA•h/g after 210 cycles at current density of 0.2 A/g. The capacity retention is 64.6%, which equivalent to a small capacity decay of 0.17% per cycle. Therefore, as an anode material, Fe3O4/C/N has excellent application in lithium-ion batteries.

    • >Water treatment technology and environmental protection
    • Preparation of cellulose membrane with high adsorption capacity and its adsorption performance for Pb2

      2020, 37(2).

      Abstract (568) HTML (0) PDF 1.51 M (0) Comment (0) Favorites

      Abstract:Cellulose membrane was prepared by phase conversion method (L-S method) with cellulose as raw material, sodium hydroxide, urea and thiourea as solvent system, the effects of coagulation bath type, H2SO4 volume percentage, solidification temperature and solidification time on the adsorption capabilities of cellulose membrane for Pb2 were studied; the microstructure of the cellulose membrane was characterized by SEM, FTIR and XRD; the thermal properties of cellulose membrane was analyzed by thermogravimetric analyzer (TG). The results show that coagulation bath is H2SO4, the volume percentage of H2SO4 is 7 %, the solidification temperature is 40 ℃, and the solidification time is 120 min, the adsorption capacity of cellulose membrane to lead ions reach the maximum, which is 343.0 mg/g. The structure of cellulose membrane changes from a closely packed sheet to a three-dimensional network structure, and C=O bond and N—H bond generates in cellulose membrane. Crystal form of part cellulose in the cellulose membrane changes from type I to type II, and the crystallinity decreases; compared with cellulose, the thermal stability of cellulose membrane is improves to some extent.

    • Preparation and Adsorption Properties of Composites POSS/ TX-10 /Bent

      2020, 37(2).

      Abstract (454) HTML (0) PDF 807.29 K (0) Comment (0) Favorites

      Abstract:A novel composites (POSS/TX-10/Bent) were prepared by composite modification of bentonite with polyhedral oli-gomeric silsesquioxane (POSS) and TX-10 nonionic surfactant as modifiers, the adsorption effect of POSS/TX-10/Bent on methylene blue was also investigated in detail. Composition and structure of composite modi-fied bentonite were characterized by XRD, XPS, EA, FTIR, SEM. The results showed that POSS and TX-10 nonionic surfactants successfully inserted into the interlayer of bentonite, which increased the interlayer spacing and hydropho-bicity of the composites. The optimum conditions were 30 ︒C, pH 6.52 (initial value), dosage 5 g/L and adsorption time 180 min., the adsorption capacity of composite modified bentonite for methylene blue was much higher than that of unmodified bentonite. The adsorption process is more in accordance with the pseudo-second-order kinetic model and the adsorption isotherm coincides with Langmuir, adsorption is a spontaneous endothermic process. The theoretical maximum adsorption capacity of the POSS/TX-10/Bent on methylene blue is 253.81 mg/g.

    • >Rubber and plastics auxiliaries
    • Mixed End-capped Waterborne Polyurethane With Pro/hydrophobic Chain Ends

      2020, 37(2).

      Abstract (563) HTML (0) PDF 518.80 K (0) Comment (0) Favorites

      Abstract:Abstract:Polyurethane prepolymer(PPU) was synthesized with isophorone diisocyanate(IPDI), poly(1,4-butanediol adipate) diol(PBA2000) and 2,2-dimethylol propionic acid(DMPA). Partially blocked hydroxy silicone oil(MPSi) was used as a hydrophobic end-capping agent, and the same molar amount of glycine(Gly) as MPSi was used as a hydrophilic end-capping agent to jointly cap PPU to synthesize a mixed-capped water-based polyurethane(MEPU) with pro-/hydrophobic chain end. The effects of r value〔n(IPDI)∶n(PBA2000)〕, DMPA content(based on the total quality of IPDI and PBA2000), and MPSi content(based on the total mass of the PPU) on MEPU performance were studied. The results showed that when r=3.0, w(DMPA)=5%, w(MPSi)=15%, MEPU emulsion is stable and transparent, compared with un-modified waterborne polyurethane, the water absorption rate of the MEPU decreased from 16.7% to 9.5%; water contact angle increased from 74.5° to 92.6°; initial decomposition temperature increased from 264℃ to 293℃; tensile strength increased 0.11 MPa; elongation at break increased by 5.81%. The water resistance and heat resistance of the film are significantly improved with the basis of not changing the stability of the emulsion.

    • >Oil field chemicals and petroleum additives
    • Synthesis and Denitrogenation Performance of Acetamide-based Coordinated Ionic Liquid

      2020, 37(2).

      Abstract (445) HTML (0) PDF 554.86 K (0) Comment (0) Favorites

      Abstract:Inexpensive acetamide (CH3CONH2)-based ionic liquids were synthesized by coordinating CH3CONH2 with anhydrous ZnCl2 at a molar ratio of 1:0.3, 1:0.4, 1:0.5, and its structure was characterized with FT-IR spectroscopy. The removal performance for basic and non-basic nitrogen of the ILs from model diesel oil containing quinoline and indole was studied. Experiment results showed that IL CH3CONH2-0.3ZnCl2 exhibited a better denitrogenation performance, and the removal efficiencies of quinoline and indole were 96.8% and 68.1% at temperature of 50℃, 1:3 (w/w) IL: oil, extraction time of 20min and settling time of 2h, respectively. It was found by further study that indole removal efficiency can reach 97.6 % with the IL after 4-stage extraction. Moreover, the quinoline removal efficiency can still reach 91.5% during five recycles of the IL.

    • Preparation and performance evaluation of Slurry thickener for supramolecular polymer clean fracturing fluid

      2020, 37(2).

      Abstract (720) HTML (0) PDF 504.77 K (0) Comment (0) Favorites

      Abstract:several problems have long existed in continuous preparation and injection of fracuturing fluid with dry thickening agents. Those problems include dusting, non-homogeneity of the fracturing fluid (such as generation of solid particles and gel congolmerates of dry thickening agents when dissolving in water ), and long dissolution time of thickening agnets etc. Based on the application of BCG, a mature supramolecular polymer thickener, a thickener was developed, which was composed of liquid paraffin, methanol, emulsifier, dispersant and thickener. The performance test shows that the hydration time of the thickener is only 0.8min, and there is no "fish-eye" in the dissolution process, so it can be prepared quickly in the field. Preparation of fracturing fluid has good heat resistance shear reisstance ability, when using a concentration of 1.6%, constant temperature under 170℃, 170S-1 shear 2 h, final viscosity stability at around 40 mpa s, in addition, the fracturing fluid has excellent suspended sand performance, and under the condition of different temperatures can be completely break. The breaking fluid has low surface tension and residue content. The properties of the fracturing fluid prepared by the thickener are equivalent to the fracturing liquid phase prepared by the dry powder thickener.

    • >Special dyes and pigments
    • Optimizating Synthesis Process of N, N-dibutyl m-aminophenol

      2020, 37(2).

      Abstract (680) HTML (0) PDF 478.59 K (0) Comment (0) Favorites

      Abstract:The preparation of N, N-dibutyl-m-aminophenol from m-aminophenol and n-chlorobutane using water as solvent was optimized. The results showed that the optimized conditions for the synthesis of N,N-dibutyl-m-aminophenol were the following: n(m-aminophenol): n(n-chlorobutane): n(CuI)=1: 2: 0.06, reaction time of 6.5 h, reaction temperature of about 105~110 ℃ and reaction pressure of about 0.2~0.5 MPa. Under these conditions, the yield of the N, N-dibutyl-m-aminophenol was up to 96.7% and the purity that was determined by liquid chromatography was above 99%. By the fine control of the reaction pressure and the pH of reaction solution, the selectivity of 98.5% was achieved. In this work, the formation of the two side-products including 3-(butylamino)phenol and 3-butoxy-N,N-dibutylaniline was effectively inhibited via the control of the reaction pressure and the pH value of re-action solution. This optimized synthesis process provides a new idea for the fabrication of N,N-di-n-butyl m-aminophenol.

    • >Adhesives
    • Synthesis and application properties of BPS-BPA phenolic epoxy resin

      2020, 37(2).

      Abstract (684) HTML (0) PDF 1.70 M (0) Comment (0) Favorites

      Abstract:Bisphenol S-BPA phenolic epoxy resin was synthesized using bisphenol A phenolic resin (BPA phenolic resin) and 4, 4-dihydroxydiphenyl sulfone (BPS) under the bridge of epichlorohydrin and the Catalysis of tetrabutylammonium bromide (TBAB). Then, its chemical structure and molecular weight were character-ized by FTIR, 1H NMR, GPC, energy spectrum analysis, etc. The results showed that the target product was successfully prepared and showed good temperature resistance, and its Mw was 4355. In addition, the effects of reaction temperature, reaction time, material ratio and NaOH content on the epoxy value of the target product were also discussed. The optimum process conditions for the target product obtained by or-thogonal experimental design are: reaction temperature 110 ?C, reaction time 2.5 h, material ratio 1:0.9, NaOH content 18 ml. Under these conditions, the epoxy value of the synthesized product was 0.718%. Finally, an adhesive was obtained by adding a curing agent to the target product. This adhesive has excel-lent bonding properties. It displays a maximum adhesion of 100.66 N and an interlayer bonding strength of 0.788 N.m, which exhibits good adhesion to low-polarity polypropylene materials.

    • >Building chemicals
    • Synthesis of Fluoride-containing Silane Coupling Agents with Short Fluorocarbon Chains and their Application in Hydrophobic Coating Construction

      2020, 37(2).

      Abstract (1560) HTML (0) PDF 1.73 M (0) Comment (0) Favorites

      Abstract:Several fluoride-containing silane coupling agents with short fluorocarbon chains were synthesized via the anionic ring-opening polymerization and hydrosilylation reaction using trifluoropropylmethylcyclotrisiloxane(D3F), dimethylchlorosilane, methyldichlorosilane and vinyltrimethoxysilane(VTMS) as reactants. The substrate on the glass plate was prepared by spin-coating of nano-silica sol, and the hydrophobic coating was obtained after the modification of silane coupling agents. The effects of silane coupling agents on the hydrophobicity, adhesion, hardness and transmittance of the coatings were investigated. The results showed that for the same type fluoride-containing silane coupling agents, the contact angle increased with the fluorine content in the agents. For the fluoride-containing silane coupling agents which had the similar molecular weight and fluorine content, the coating modified by the linear type coupling agent was more hydrophobic than the one modified by the branched type. Among the fluoride-containing silane coupling agents in this work, the coating modified by the branched type with a degree of polymerization of 9(DF3) showed the biggest contact angle, about 141.6°. The adhesion level of the hydrophobic coatings in all cases reached to level 1 and the hardness reached to H, while the visible light transmittance was higher than 82.9%. The hydrophobic coatings also had good self-cleaning property.

    • >Fine chemical intermediates
    • One-Pot Two Steps Synthesis of β-Keto-Sulfones via the Enaminone Intermediate

      2020, 37(2).

      Abstract (588) HTML (0) PDF 595.98 K (1) Comment (0) Favorites

      Abstract:β-keto-sulfones are an important sulfone-containing molecules and also serves as a versatile building blocks in organic synthsis. In this paper, we developed a novel method to construct various β-keto-sulfones that formed from the radical sulfonylation of carbonyl α-Csp3-H. The present method in-cluding two steps: firstly, the ketones react with DMF-DMA to generate more reactive enaminone inter-mediate, then with the assistance of FeCl3?6H2O/TBHP system, the enaminone intermediate underwent radical addition, oxidation, nucleophilic substitution and the loss of DMF would produce the β-keto-sulfones. This methodology will provide new strategies for construct β-keto-sulfone-type products, which has advantages of simple operation, mild reaction conditions and good functional group tolerance.

    • >Other
    • Study on skin care efficacy of black tea and green tea extract

      2020, 37(2).

      Abstract (1000) HTML (0) PDF 594.39 K (1) Comment (0) Favorites

      Abstract:This experiment determined the functions of sunscreen, moisturizing, anti-oxidation, whitening and anti-aging of black tea extract and green tea extract alone and in combination, and whether the two have synergistic effects. The results showed that the black tea and green tea extracts were more effective in combination with moisturizing, anti-oxidation, whitening and anti-aging functions.