fangzhuqing , shidaxin , lihansheng , wuqin , 矫庆泽
2020, 37(1).
Abstract:exo-Tetrahydrodicyclopentadiene (exo-THDCPD) is a kind of high-energy density hydrocarbon fuel, which can be prepared from dicyclopentadiene by hydrogenation and isomerization reactions. In this pa-per, the current research and technical status of exo-THDCPD preparation, including the reaction princi-ple, process route, main technical parameters and so on are summarized. The types and preparation methods of hydrogenation and isomerization catalysts and the research progress of hydrogenation and isomerization processes are introduced. Finally, it is pointed out that the non-noble metal alloy catalysts are the research focus of hydrogenation catalysts. Furthermore, prolonging the life time of supported AlCl3 catalysts, improving the anti-coking performance of zeolite and reducing the production cost of ionic liquid catalysts are three research directions of isomerization catalysts. Increasing the selectivity of the bi-functional catalysts is important for the one-pot preparation of exo-THDCPD. Liquid-phase con-tinuous-flow process is expected to realize the continuous industrial production of exo-THDCPD.
2020, 37(1).
Abstract:Unlike coronene, which are flat and planar, corannulene has a bowl-like stereo structure. It can be imagined as the cap region of fullerene C60 or an end of a single-walled carbon nanotube. Coranulene has many unique properties because of its bowl-like structure. The synthesis of corannulene and derivatization of bromine-containing corannulenes are briefly introduced. In recent years, the derivatives of mono-functional groups and multi-functional groups synthesized from monobromocorannulene and tetrabromocorannulene are reviewed, which serve as precursors for numerous classes of materials and energy, such as graphitic tubes/caps, liquid crystals, dendrimers, polymers.
WEN Hui-xia , Xu Cheng-gong , Fan Bin , Li Hong-xi , DanZhenshijie , Zhao Wen-yu
2020, 37(1).
Abstract:Lithium carbonate, aluminium oxide, silicon dioxide, europium(III) oxide were used as raw materials to prepare a series of Eu3+ ion-doped LiAlSiO4 red phosphor Li1-xAlSiO4+x:xEu3+(x=0.05~0.18) by a conven-tional high-temperature solid-phase method at 1150℃. The crystal structure, particle morphology and luminescence properties of Li1-xAlSiO4+x:xEu3+ were characterized by XRD, SEM and photoluminescence spectrum. The influence of amount of Eu3+doping on the luminescence intensity, color temperature and hue of the red phosphors was investigated. The results indicated that the sample was single host when the Eu3+ doping molar fraction was below 15.0%. The sample could be excited by the near-ultraviolet band of 350~420 nm, and the strongest excitation peak was located at 394 nm. The emission spectrum showed characteristic peaks of Eu3+, at 593 nm and 616 nm, corresponding to 5D0→7F1, 5D0→7F2 transitions, re-spectively. The optimal doping molar fraction of Eu3+ corresponding to the strongest emission of sample was 12.0%. The occurrence of concentration quenching was mainly due to the quadrupole -quadrupole (q-q) interaction. The CIE coordinate of this sample is (0.6464, 0.3526), thus, it can be a candidate of red phosphor for NUV excited LEDs.
2020, 37(1).
Abstract:A-DOA/CNTs materials were obtained by synergistic modification of carbon nanotubes (CNTs) with dopamine (DOA) in a weakly basic system by oxidative self-polymerization and γ-aminopropyltriethoxysilane (APTES) hydrolysis and condensation reaction. Polyurethane prepolymer with double bond and semi-blocked end was synthesized by isophorone diisocyanate (IPDI), polycarbonate polyol (PCDL), Dihydroxymethyl butyric acid (DMBA), pentaerythritol triacrylate (PETA). The A-DOA/CNTs modified FPUA composite emulsion was prepared by emulsion copolymerization of vinyl monomers such as organic fluorine and other residual isocyanate groups and covalent polycondensation and crosslinking of the modified CNTs surface active groups. The results are as follows: When the amount of A-DOA/CNTs is 0.75% and the amount of organic fluorine monomer is 12%, the thermal decomposition temperature of A-DOA/CNTs/FPUA composite film is 329?C when the thermal weight loss is 10%. Compared with the thermal decomposition temperature of PUA film, the thermal decomposition temperature of PUA film is 292?C, and 37?C is increased. At this time, the dynamic storage modulus of composite film at -55?C is the best value, and the glass transition temperature is 83?C, which significantly improves the thermal stability of the film. The water absorption of A-DOA/CNTs/FPUA film is 5.2%, the water contact angle is 103.1? , the tensile strength is 23.3 MPa, the elongation at break is 352%, and the comprehensive performance is the best.
2020, 37(1).
Abstract:Synthesized from isophorone diisocyanate (IPDI) and polyoxypropylene diol (PPG), Waterborne polyurethane (WPU) was prepared as a carbon source in the preparation of carbon dots (CDs) with hydrothermal method. Carbon dots (CDs) with different mass fractions were added to the reaction system of isophorone diisocyanate (IPDI) and polyadipate 1,4-butanediol diol (PBA) to prepare carbon dots/waterborne polyurethane composite materials. The structure and properties of the composite materials were characterized by fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), ultraviolet-visible absorption spectroscopy (UV), fluorescence spectroscopy and the mechanical properties tests. The results showed that the thermal stability, fluorescence performance and mechanical strength of the composite films were improved with the addition of carbon dots.When the mass fraction of carbon dots was 0.5%, the quantum yield and fluorescence lifetime of the composite film were 4.15% and 2.43 ns, respectively. The tensile strength and elongation at break of the films were 36.80MPa and 660%, respectively, which were 29.7% and 33.3% higher than those with no carbon dots added.
Nie Sheng-nan , Wu Li-jun , Liu Ying-han , Zhang Hao
2020, 37(1).
Abstract:In order to improve the surface corrosion resistance of the heat exchanger without affecting the heat transfer efficiency, graphene, graphite powder, epoxy resin, and other materials were used to prepare the composite coating of high thermal conductivity and anti-corrosion on the surface of heat exchangers. After sulfuric acid corrosion test, heat conduction test, and bonding strength test, these conclusions are drawn: The anti-corrosion of the coating increases with the increase of graphene content and its corrosion rate will reach the minimum value 0.2338mg/(cm2·h) when the graphene mass fraction is 0.06%, and its corrosion resistance is much stronger than that of 304 stainless steel, which corrosion rate is 1.5 mg/(cm2·h); the thermal conductivity increases with the increase of graphite powder content, and will reach the maximum value 35.848 W/(m·K) when the graphite mass fraction is 8%; the bonding strength of the coating reaches ASTM grade 5B.
CHU Yun-chen , ZHANG Xue-min , WANG San-fan
2020, 37(1).
Abstract:A conventional method for preparing a polyvinylidene fluoride (PVDF) homogeneous cation exchange membrane is improved. The PVDF homogeneous cation exchange membrane was directly prepared by using initiators and sulfonation with concentrated sulfuric acid. A series of PVDF cation exchange membranes using the initiator benzoyl peroxide (BPO) and/or 2,2'-azobis(2-methylpropionitrile) (AIBN) were prepared by solvent evaporation. The effects of different initiators and their contents on the membrane structure and membrane properties were investigated. The physical morphology and chemical structure of PVDF cation exchange membranes were analyzed by thermal field emission scanning electron microscopy (FE-SEM) and Fourier Transform infrared spectroscopy (FTIR). The results show that PVDF and styrene form a semi-interpenetrating network structure in the cation exchange membrane containing BPO. In the cation exchange membrane containing AIBN, styrene is grafted on the linear PVDF chain and forms a phase separation structure. The structure and properties of the PVDF cation exchange membrane are affected by the content of AIBN and BPO. When the AIBN content is 0.25 g and the BPO content is 0.1 g, the membrane resistance of the ion exchange membrane reaches a minimum of 4.2 Ω∙cm^2. The ion exchange capacity is up to 1.6 meq/g; when the AIBN content is 0.15 g and the BPO content is 0.1 g, the migration number of the ion exchange membrane is 95.15%. The effects of different initiators and their contents on membrane resistance and migration number were further verified by cyclic voltammetry and chronopotentiometry.
LIULI , liufangfang , xinghongli , liuxinwei , zhaotianjiao
2020, 37(1).
Abstract:BPO-DMA and BPO-DMA-Co(II) curing systems were used to perform solidification and isothermal differential scanning calorimetry (DSC) tests on the Polyrster putty, and the curing time, curing performance, curing degree, the reaction activation energy can be explored, It is confirmed that the introduction of Co(II) in the BPO-DMA system not only made the poly putty curing speed fast, the good air drying property, and the adhesion was excellent, but also reduced the reaction activation energy of the isothermal curing and increased the curing degree; The curing reaction process of the BPO-DMA-Co(II) curing system on the Poly putty was studied by non-isothermal DSC, The curing parameters and curing temperature of the curing system were calculated by Kissinger extreme value method, FWO integration method and T-β (temperature-heating rate extrapolation )method. At the same time, according to the Friedman calculation method, it is determined that the BPO-DMA-Co(II) curing system complies with the autocatalytic curing model,and the kinetic equation is calculated according to linear regression, the results show that the data are in good agreement with the experimental measurements.
ZHOU Xi , ZHANG Zhi-min , WANG Ruo-nan , TU Wei-ping , HU Jian-qing
2020, 37(1).
Abstract:A series of bio-based degradable fluorescent polyesters (BBPP-Cys and BBPP-Ser) were synthesized from natural bio-based materials such as castor oil (CO), citric acid (CA) and L-cysteine (L-cys) or L-serine (L-ser).The structure and fluorescence characteristics were characterized by FTIR, 1HNMR, UV-vis spectra and fluorescence spectra. At the same time, the water contact angle, particle size, mechanical properties, degradation properties and cytotoxicity of the polyesters were measured. The results showed that the unique six-membered ring structure suspended on the polyesters backbone were responsible for their fluorescent properties. BBPP-Cys samples had the strongest UV absorption at 265 nm, and their fluorescence emission signal was the strongest at 445 nm. For BBPP-Ser samples, their strongest UV absorption and fluorescence emission were at 266 nm and at 460 nm, respectively. The synthesized polyesters had good hydrophilicity and small particle size, the tensile strength ranged from 1.21 MPa to 1.95 MPa. The degradation rate of the samples in 0.1 mol/L NaOH solution reached over 60% in 7 days. The cytotoxicity of fluorescent polyesters was tested by MTT assay. The results demonstrated that the cell viability of the synthesized fluorescent polyesters was all greater than 90%, indicating that they had good biocompatibility.
2020, 37(1).
Abstract:BiVO4/MIL-100(Fe) composites were prepared by one-pot hydrothermal method using NH4VO3, Bi(NO3)3•5H2O, 1,3,5-benzenetricarboxylic acid and Fe(NO3)3•9H2O as raw materials. The structure, morphology, specific area and optical property of BiVO4/MIL-100(Fe) composites were characterized by XRD, SEM, N2 adsorption-desorption, UV-Vis DRS and PL. The composites had larger specific surface area. XRD results showed that BiVO4 had mixed crystal structure of monoclinic phase and tetragonal phase. The absorption intensity of BiVO4/MIL-100(Fe) composites for visible light was higher than that of MIL-100(Fe). The recombination rate between photogenerated electrons and holes decreased after the composites absorbed visible light. Different materials were used as catalysts for the photodegradation of crystal violet under visible light. Among them, BiVO4/3MIL-100(Fe) composites displayed the highest photocatalytic activity. The results revealed that the degradation rate of 30 mg BiVO4/3MIL-100(Fe) composites for 30 mL crystal violet solution with an initial concentration of 30 mg/L was 98.7% under visible light irradiation for 80 min. The holes were main active catalytic species. Besides, BiVO4/3MIL-100(Fe) composites exhibited stronger photocatalytic degradation ability for crystal violet, rhodamine B and methylene blue under sunlight irradiation.
SHI Jun-hua , YAO Jin , LI Zhi-han , ZHU He-ping , LIU Wen-liang
2020, 37(1):0-0.
Abstract:The cellulose nanocrystals (CNC) was extracted from the shell of Camellia oleifera Abel by chemical disintegration method. The butyrated cellulose nanocrystals (BCNC) was prepared by surface modified with Butyric anhydride, and the BCNC/PLA nanocomposites were prepared by solvent casting method. Morphologies and properties of BCNC were observed, and the tensile properties, barrier properties and the transparency of BCNC/PLA nanocomposites film were studied in this paper. The strength and toughness of PLA were improved by composited with BCNC, and the tensile strength of PLA composites film was improved 30.1% by adding 5 wt% BCNC. Adding 5 wt% BCNC, the water vapor gas permeability and oxygen permeability of the film were decreased by 60.0% and 35.0%, and the composite films still maintain high transmittance. Owing to the excellent dispersion and interfacial adhesion in the matrix, the BCNC have a great influence on the tensile properties and barrier properties of PLA than CNC.
XU Fu-li , ZHANG Wei , WANG Feng-shou
2020, 37(1):0-0.
Abstract:Narrow distribution alcohol ether carboxylate (NAEC9) synthesized by oxidation was compounded with ammonium lauryl ether sulfate (ALES), hexadecyl trimethylammonium chloride (1631) and octadecyl glucoside (APG0810), the effects of different mass fractions of NAEC9 on the surface tension、foamability、wetting、emulsification and decontamination of the composite system were studied. The results show that the NAEC9/1631 mixed system was obvious synergistic effect in surface tension、foam and wettability, and the synergistic effect was strongest when the mass fraction of NAEC9 was 66.7 %, the wetting time decreased from non-wetting to 37 s, and the foam volume reached a maximum of 500 mL at 30 s. However, no obvious synergistic effect was found between NAEC9/ALES and NAEC9/APG0810 system . In terms of decontamination performance, the NAEC9/ALES mixed system has the best decontamination performance for sebum decontamination cloth and the worst decontamination ability for protein decontamination cloth. The compound of anionic surfactant NAEC9 and cationic surfactant 1631 has a good synergistic effect, and the surface activity is enhanced without precipitating.
ZHANG Bin , ZHANG Hua , WANG Gong-ying , YANG Xian-gui
2020, 37(1).
Abstract:Abstract: The experiment uses ethylene carbonate and methanol as raw materials and the LiF/CaO catalyst was prepared by impregnation method. The catalytic activity of LiF/CaO for the synthesis of dimethyl carbonate (DMC) by transesterification of ethylene carbonate (EC) with methanol was studied. The catalysts were characterized by X-ray diffraction, N2 adsorption-desorption and Hammett titration. The results indicated that new phases CaF2 and Li2O were formed when LiF/CaO was calcined. In the case of LiF loading and calcination temperature were 20%(based on mass of CaO) and 500℃, n(Methanol): n(EC) = 10:1, catalyst amount 0.1%(based on mass of EC), reaction temperature 70℃, reaction time 0.5 h. Under these conditions, EC conversion, DMC selectivity and yield were 77.98%, 99.97% and 77.96%, respectively.
YANG Hao , XIAO Zhong-liang , CHEN Tong , ZENG Yi , WANG Gong-ying
2020, 37(1).
Abstract:TiO2-GO catalysts were prepared by graphene oxide (GO) and then used to catalyze the transesterification of dimethyl carbonate with phenol to diphenyl carbonate. The characterization results of XRD, TEM, XPS and Py-TPD demonstrated that GO could remarkablely improve the dispersion of TiO2, and the electronic effect of GO could change the chemical states of Ti species and promote the formation of the active Ti(Ⅳ) and the scale of medium Lewis acid sites in GO modified catalysts increased significantly. Consquently, the amount of active sites increased in TiO2-GO which was favorable for the formation of transesterification products. The results indicated that the role of GO in the TiO2-GO catalysts was not just a support, but also an electron promoter. The TiO2-GO 50% catalyst exhibited an excellent catalytic performance for the transesterification of dimethyl carbonate with phenol to diphenyl carbonate. With the the reaction temperature 150~180℃, reaction time 9 h, the 41.8% phenol conversion and 99.9% transesterification selectivity were achieved.
DU Hong-tao , Xu Ming , ZHENG Wan-qiong , MA Fang
2020, 37(1).
Abstract:A series of deoxyvasicinone analogues were synthesized in order to produce new high efficiency deoxyvasicinone derivatives of cholinesterase (ChE) inhibitors, and their structure-activity relationships (SARs) were investigated. The compounds with six-membered rings exhibited greater ChE inhibitory activity than the compounds with other sizes of ring. C=N bonds were important for ChE inhibitory activity and selectivity for butyrylocholinoesterase (BuChE). Hydroxyl groups were able to inhibit ChE. Conversely, carbonyl groups decreased ChE inhibitory activity. Furthermore, docking studies demonstrated that proteins and ligands interacted through π-π stacking, hydrogen bonds and “water bridges”.
2020, 37(1).
Abstract:Silk/polyethylene oxide composite solid polymer electrolyte was prepared by casting polyethylene oxide (PEO) and lithium salt solution on silk and drying it into a film with natural silk as the skeleton supporting material. The structure and properties of the solid polymer electrolyte were characterized by FT-IR, tensile tester, synchronous thermal analyzer, electrochemical window test, conductivity test, etc. The battery was assembled with lithium iron phosphate as the positive electrode and lithium metal as the negative electrode to test the charging and discharging performance. The results show that the composite solid polymer has better mechanical strength (up to 10 MPa) and an excellent electrochemical window (up to 4.6 V) compared with the conventional PEO solid polymer electrolyte. The specific capacity of all-solid-state lithium batteries assembled with the electrolyte reaches 113 mAh/g at 60℃and 1C current density, and the capacity retention rate reaches 97% after 100 cycles, showing excellent cycle stability.
CAO Sheng-kui , GUN Min , CHEN Hui , SHAN Zhi-hua
2020, 37(1).
Abstract:The titanium plate is used as the cathode, the graphene is the anode, and the NaCl is the supporting electrolyte and the oxidation source for the indirect electrooxidation of the starch. The L9(34) orthogonal experiment was carried out with four factors: current density, SS mass fraction, NaCl mass fraction and electrolysis time. The results of orthogonal experiments show that the optimal SS and NaCl mass fractions are 10% and 2%, respectively. The single-current step method was used to investigate the current density and electrolysis time. The results show that the optimal current density is 20 mA/cm2. According to the transition characteristics of the potential in the image, the aldehyde group analysis of the starch oxidation process was carried out, and the optimal time of the dynamic equilibrium of the indirect oxidation experimental system was obtained as the turning point of the potential. The analysis found that the mass fraction of aldehyde-containing starch on the turning point was close to the maximum equilibrium. Auxiliary analysis of FT-IR and XRD showed that significant oxidation changes had occurred between the oxidized starch structure at the turning point and the original starch, and the optimum electrolysis time was determined to be 1200 s. Under this condition, the mass fraction of the aldehyde-containing aldehyde group was 0.432%.
Zhang Ming-rui , MA Xing-yuan , He Ying-hua , Liu Shuai , Wu Xiao-zhen
2020, 37(1).
Abstract:The 3-isocyanatemethylene-3,5,5-trimethylcyclohexyl isocyanate (IPDI), Polytetrahydrofuran (PTMG2000), Double-tailed hydroxy silicone oil (DSE), 2,2-dihydroxymethyl propionic acid (DMPA) and 1,4-butanediol (BDO) were used as the main raw materials, comb-like organic silicon modified waterborne polyurethane (DSE-WPU) was prepared by prepolymer dispersion method, and then high-strength multifunctional nanocomposite (GO-DSE-WPU) was prepared by adding graphene oxide (GO) slurry, and the relationship between its structure and properties was studied. Mechanical properties analysis showed that the addition of GO and DSE can effectively improve the mechanical properties of GO-DSE-WPU film. Video optical contact Angle analysis shows that, with the increase of GO content, the hydrophobic performance of GO-DSE-WPU film presents a trend of first rising and then declining, and hydrophobicity has improved significantly overall. AFM spectrum analysis explained the reason of the improvement of the hydrophobicity of GO-DSE-WPU from the internal structure. It can be clearly seen from SEM cross-section line sweep energy spectrum that the enrichment rate of silicon on the film-forming surface of GO-DSE-WPU can be increased by 100%. Anti-UV analysis showed that even if a small amount of GO was added, the UV absorption rate of GO-DSE-WPU film was significantly increased and the UV transmittance was significantly reduced. The thermal performance analysis showed that the three thermal degradation temperatures of GO-DSE-WPU were improved compared with that of DSE-WPU, and the thermal performance was improved. Therefore, a multifunctional waterborne polyurethane nanocomposite with high strength can be prepared by this method, which has a wide application prospect in functional coating, surface treatment and film materials.
ZHANG Hao , LI Ya-xing , ZHANG Yi , CHENG Bo-wen , Zheng Yunfei , DING Chang-kun
2020, 37(1).
Abstract:Grafted starch ion exchange resin (GSR) was synthesized by natural starch (RS), sodium methacrylate (SMAS) and styrene (ST). The structures of products were characterized by infrared spectrum(IR), Raman spectroscopy(RAM) and 13CNMR. When the initiator concentration was 0.056 mol/L, mole ratio of n (ammonium persulfate) : n (sodium bisulfite) = 3:1, reactant input ratios was n (RS) : n (SMAS) : n (ST) = 4:2:1, reaction temperature at 65 ℃, reaction time of 3 h, the sulfonic acid group content was up to 15.65%, the methylene blue adsorption amount was 17.98mg / g, both of which increase first and then decrease with the monomer addition amount. BET test showed that GSR has increased specific surface area than native starch which is 5.078m2/g. GSR has improved stability and higher resistance to acids, bases and enzymes. It has improved adsorption to methylene blue, Safranine T and malachite green, and reduced adsorbing differentiation for dyes with different structures, moreover, it showed a good adsorption properties under different pH conditions. The decolorization rate of GSR on mixed dye waste-water has closed to 85.08%, which increases by 91.03% in comparison with RS, and better than that of zeolite and 001×7 cation- exchange resin. After four regeneration cycles, the decolorization rate is not lower than 91.12% of the first adsorption rate. The decolorization rate of GSR resin increases with the decrease of particle size. When the particle size is 150~250μm, the GSR has relatively high decolorization, and moderate particle size that similar to synthetic resin, which is convenient for the reuse and recycling, thus conducive to the continuous operations.
2020, 37(1).
Abstract:The nanorod-shaped Ag3PO4 / ZnO composites were prepared by in-situ growth method using one-dimensional rod-shaped ZnO as a carrier. The structure of the composites was characterized by XRD, SEM, TEM, XPS and UV-Vis-DRS were used to characterize the crystal phase, surface morphology and optical absorption of the nanorod Ag3PO4 / ZnO nanocomposite. The optical properties of the sample in visible light Catalytic properties. The results show that ZnO has almost no visible light activity, and the hydrothermal method changes the morphology of ZnO to increase its specific surface area, which provides more possible loading for Ag3PO4. The complex Ag3PO4 / ZnO showed a significantly higher photocatalytic activity than pure ZnO and Ag3PO4 in visible light. Finally, the photocatalytic stability of the Ag3PO4 / ZnO composite shows that the Ag3PO4 / ZnO composite forms an effective heterojunction structure and inhibits electron-hole recombination, thus greatly improving the stability of the Ag3PO4 / ZnO composite.
2020, 37(1).
Abstract:The modified activated carbon material (Mg-GAC) was prepared by reactive crystallization technique. The microstructure of the activated carbon before and after modification was analyzed by SEM and XRD. The adsorption time, pH value and temperature of GAC and Mg-GAC were studied. The effect of adsorption of copper ions in wastewater. The results show that the modified GAC greatly increases its specific surface area and increases to 738.01m2/g. When the dosage of Mg-GAC was 0.3g, the concentration of copper ion was 40mg/L, the temperature was 25 ℃, and the pH was 7 for 2 h, the adsorption amount reached 11.66mg/g. In addition, the adsorption process of copper ions conforms to the Langmuir isotherm model.
LI Xin-yang , ZHU Jia-xin , SUN Ting-ting , WANG Hai-zeng
2020, 37(1):0-0.
Abstract:The fluorine adsorbent of a magnesia based lanthanum composite was synthesized by co-precipitation method using magnesium nitrate and lanthanum nitrate as main materials. The composite powder was further molded into grains with polyvinyl alcohol (PVA) and polyvinylidene fluoride (PVDF) with a di-ameter of around 0.5cm by using extrusion molding. XRD, SEM and FTIR were used to characterize and analyze the prepared composite adsorbents. The performance of the powdered and granular composite adsorbents on the absorption of F- in aqueous solutions was tested and analyzed respectively. The results showed that the maximum adsorption of F- could reach 142.85mg/g with the powdered composite adsor-bent. The best pH for F- adsorption was found in the range of 4~10, and the adsorption equilibrium could be reached within 200min. At 25℃, the adsorption of F- with the magnesia/lanthanum composite adsor-bent was well fitted by the Langmuir isothermal adsorption model and the adsorption kinetics could be well described by the pseudo-second-order kinetic model.
Jia Jiru , Wang Tengfei , Li Xinxiang , Yin Yunjie , 贾
2020, 37(1).
Abstract:1,4-Diaminoanthraquinone (DA) as chromogen was reacted with isophorone diisocyanate (IPDI) to form a purple prepolymer, followed by interfacially polymerized with polyethylene glycol 600 to prepare amino-anthraquinone polyurethane microspheres (DAPM). The effects of emulsifier type, emulsifier dosage, emulsifying speed and chromogen dosage on the particle size of microspheres were investigated. The results showed that sodium dodecylbenzenesulphonate (SDBS) emulsifier was more suitable for the preparation of polyurethane microspheres than octaphenyl polyoxyethyiene-10 (OP-10), polyoxyethylene sorbitan monooleate (Tween80) and sorbitan monooleate (Span80). When SDBS mass fraction was 3.5% (based on the oil phase), the particle sizes of the microspheres were all around 350 nm with the narrowest particle size distribution. The average particle size decreased with the increase of emulsifying speed, when the emulsifying speed was 8000 r/min, the particle size distribution was the most concentrated. When the chromogen dosage was 1 mmol, the prepared microspheres exhibited the narrowest distribution with a particle size of 500 nm. SEM and TEM observations revealed that the as-prepared amino-anthraquinone polyurethane microspheres had a particle size of about 500 nm with smooth spherical surface and hollow internal structure. The fabric printed with DAPM had excellent color properties and color fastness.
LI Chaoming , ZHOU Jing , GUO Qiaoxia , REN Shenyong , SHEN Baojian
2020, 37(1).
Abstract:3,6-Di-tert-butylcarbazole was synthesized under anhydrous and anaerobic condition by using 2-chloro-2-methylpropane as alkylation reagent and AlCl3 as catalyst with an isolated yield of 53%. The structure of the product was characterized by 1HNMR and 13CNMR. 3,6-Di-tert-butylcarbazole was used as an antioxidant agent of lubricating oil, and then it was compounded with an organic molybdenum addi-tive, organic molybdate (MoE) which was synthesized by our research group. Subsequently, 0.8% mass fraction of this compound was added into lube base oil II. The antioxidant performance of lube base oil II was evaluated by differential scanning calorimetry (DSC) dynamic method and rotary pressure vessel ox-idation test (RPVOT). DSC results showed that 3,6-di-tert-butylcarbazole effectively improved the oxida-tion stability and thermal stability of lube base oil II. The initial oxidation temperature of the sample by adding 3,6-di-tert-butylcarbazole was increased by 50.9℃, while that of lube base oil II by adding the compound of 3,6-di-tert-butylcarbazole and MoE was increased by 66.3℃. RPVOT results revealed that 3,6-di-tert-butylcarbazole could increase the oxidation induction period of lube base oil II to 2 times, the compound of it and MoE could increase the oxidation induction period to 2.5 times. The oil solubility test displayed that the introduction of tert-butyl groups on the carbazole benzene ring increased the solubility of carbazole in lube base oil II.
2020, 37(1).
Abstract:Amphiphilic polymer ZW-12 was synthesized by aqueous solution polymerization of acrylamide(AM), acryloxyethyl trimethylammonium chloride (DAC), 2-acrylamide-2methyl propanesulfonic acid (AMPS) and dodecyl dimethyl allyl ammonium chloride. Using octadecyl dihydroxyethyl betaine as associating crosslinking agent M-1. The effect of different concentration of M-1 on the rheological properties of ZW-12 solution was studied by RS6000 rheometer with hydrophobic associating polymer ZW-12 and surfactant M-1andthe microstructure of the fluid was observed by sem. The results showed that both the thixotropic and creep properties of the composite system changed significantly after the concentration of M-1 reached 0.30%. The thixotropic experiment showed the generation of stress overwash and the large increase of the area of thixotropic ring. Burger model was used to fit the creep experiment, and it was also found that when the concentration of M-1 was greater than 0.30%, the Maxwell spring modulus G0 increased significantly. Scanning electron microscopy verified the inference that the fluid structure changed before and after 0.30% concentration. Cross equation and Jeffery model were used to fit the viscosity and shear curves of the fluid at different concentrations of M-1, and it was determined that the combined influence of M-1 on the viscosity and modulus of the fluid resulted in the change of its non-newtonian behavior.
CHENG Hang-hang , shenyiding , maguoyan , yagnkai , houxuming
2020, 37(1):0-0.
Abstract:The phosphorylated styrene-acrylic rust preventive emulsion (PM-2-SP) with core-shell structure was synthesized by semi-continuous seeded emulsion polymerization using methacrylic acid (MAA), hydroxypropyl methacrylate (HPMA) as a crosslinking monomer, styrene (St) and methyl methacrylate (MMA) as hard monomer, butyl acrylate (BA) as Soft monomer, 2-hydroxyethyl methacrylate phosphate (PM-2) as a functional monomer and dodecanethiol as a segment regulator. The effects of the amount of PM-2 on the stability of PM-2-SP emulsion, the water resistance of the PM-2-SP film and the anti-rust properties of the film were studied. Also, the size and morphology of the PM-2-SP emulsion particles were characterized by DLS and TEM. The surface of the film was observed by atomic force microscopy (AFM). The corrosion resistance of the paint film was tested using a salt spray tester. Consequently, the results show that the emulsification of the system and anti-rust performance of the paint film were optimal when the content of PM-2 is 4wt%. The particle size of PM-2-SP emulsion with core-shell structure was 135.7nm and the PDI was as low as 0.150. The film had the smooth and compact surface as well as excellent resistance to water. In addition,The corrosion potential and corrosion current of the film was -0.391V and 1.95E-7(A?cm2), respectively. What's more, compared with pure styrene-acrylic, the rising rate of corrosion potential and reduction rate of corrosion current of the film was 74.16% and 94.76%, respectively. The salt spray resistance time of the film had extended to 144h.
2020, 37(1).
Abstract:The hindered amine light stabilizer 625 was synthesized by methylation reaction from hindered amine light stabilizer 360 and paraformaldehyde in toluene, and the structure was elucidated by 1HNMR. Via the single factor experiments and the orthogonal experiments,the suitable methylation conditions were obtained as follows, n(360):n(formaldehyde)=1:4.6, the reaction temperature was 85℃, and the reaction time was 6h. Under these conditions, the methylation rate was 97.4%. Compared with the formalde-hyde/formic acid method, formic acid wasn’t required inthe reaction. The method avoided the problem of salt-forming agglomeration of the light stabilizer 360 with formic acid and of the cumbersome workup, simplified the operation, reduced the cost. It has the advantages of higher methylation rate and lighter product color.
2020, 37(1).
Abstract:This paper describes an novel synthesis of D5-cypermethrin with D6-phenol (98% atom D) as the labeled precursor. D6-phenol was dehydrated by potassium deuterium oxide in anhydrous toluene, and then reacted with 3-bromobenzaldehyde to obtain the key labeled intermediate D5-3-phenoxy-benzaldehyde through Ullmann Condensation Reaction. Finally, D5-cypermethrin was obtained by “phase transfer catalysis cyanohydrins reaction” with sodium cyanide and 3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarbonyl chloride by one-step method. The yield based on the amount of substance of deuterium-substituted phenol was 20%. As-synthesized product was con-firmed by MS, NMR and HPLC to be target compound. Its chemical purity is higher than 98%, and isotopic abundance is higher than 98% (atom D). This method could also be used to synthesize other labeled pyrethroids.
FENG Bai-cheng , GE Ping-yu , HOU Xi-chao , JIN Yan
2020, 37(1).
Abstract:Abstract: α-acylation reactions of a series of β-dicarbonyl compounds were carried out in a deep eutectic solvent (DES) using benzoyl chloride derivatives and β-dicarbonyl compounds as raw materials, the catalytic mechanism for the reaction was investigated. The effects of reaction temperature, time, types and the amounts of DES on the product yields were investigated. The best yield can be obtained by reacting at 120℃ for 4 h in 10% mol deep eutectic solvent composed of choline chloride and Zinc chloride, the yield can reach 86%-94%. DES still maintained high catalytic activity after reused 4 times. The reaction conditions of the process were green and mild.
2020, 37(1).
Abstract:A continuous flow micro-channel reactor was used to selectively remove methyldichlorosilane from trichlorosilane by photochlorination reaction. The effect of various factors on the removal rate of methyldichlorosilane was investigated. The results show that increasing the chlorine gas and light intensity, increasing the reaction temperature, reducing the wavelength of the light source, and prolonging the reaction time are beneficial to the removal of methyldichlorosilane. Under the optimal conditions, the methyldichlorosilane content in the product is less than 0.05ppm, the removal rate reached to 99.6%. A small amount of silicon tetrachloride is found in the reaction products, which is formed by chlorination of polychlorosilane and trichlorosilane. With the improved trichlorosilane as the raw material, the carbon content of the polycrystalline silicon prepared by the evaluating furnace is less than 3?1015atoms/cm3,which meets the requirements of the first-grade electronic products.