Nie Changhua , CHEN Junhua , HU Jianqing , WANG Feng , TU Weiping
2019, 36(7).
Abstract:Epoxy resin has many excellent properties and is widely used in various fields. However, it is increasingly difficult for solvent-based epoxy resin to meet the requirements of environmental protection in the market. Therefore, it is quite important to seek water-based epoxy resin. In this paper, the preparation methods of water-borne epoxy resin emulsions such as mechanical method, reverse conversion method, chemical modification method and curing agent emulsification method are introduced in detail. The principle and process of various methods are systematically described, and the important factors affect of water-borne epoxy resin is analyzed and summarized. In addition, the advantages and disadvantages of different preparation methods are described in detail, and the optimization and improvement directions are prospected. The latest research progress of water-borne epoxy resins at home and abroad was reviewed. It was pointed out that the development trend of water-borne epoxy resins in the future was the selection of production formula, optimization of process flow and planned functional modification, which broadened the application of waterborne epoxy coatings.
lanxiaolin , duanzhnegkang , xujinxia , wangyongsheng , zhaoyunlu , zhaozhenzhne
2019, 36(7).
Abstract:Based on the current research situation that Cu-based catalysts are inclined to inactivate in diethanolamine dehydrogenation process because of oxidizing and agglomerating. Therefore, the dehydrogenation mechanism of diethanolamine was introduced. Moreover, the influences of supporters, different additives and microstructures on the performances of Cu-based catalysts were summarized. In the future, the development of diethanolamine dehydrogenation should seek a highly efficient catalyst, also should pay attention to continuous manufacturing. The development of continuous manufacturing at home and abroad is briefly introduced. Finally, the trend modification of Cu-based catalysts and realizing the continuous manufacturing of diethanolamine dehydrogenation were proposed.
PAN Yi , sun meng ying , yang shuang chun
2019, 36(7).
Abstract:Anionic clean fracturing fluid is a non-polymer water-based fracturing fluid based on anionic viscoelastic surfactant. It has such characteristics as simple configuration, easy flowback, no residue, low viscosity and good elasticity of gel, stable fracturing performance and so on.With the increasing of the difficulties of low pressure and low permeability oil field and the depth of oil well exploitation, the temperature resistance of Anionic Viscoelastic Surfactant Fluid (for short:AVES) has become an important aspect of the research topic.The application performance and characteristics of typical non-polymer AVES fracturing fluids and new polymer AVES fracturing fluids are reviewed, and the advantages and disadvantages of various types of AVES fracturing fluids in oilfield applications are illustrated in the list.In view of the situation that the fracturing effect of AVES fracturing fluid is not obvious at high temperature, the micellar stability is poor, and the synthesis of main agent is complex, the methods of improving the anion side chain, developing asymmetric twin anions and developing new nanoparticles are proposed, so as to simplify the system preparation and increase its temperature resistance and stability.
2019, 36(7).
Abstract:The oxidation of primary and secondary alcohols to corresponding carbonyl compounds is an important functional group conversion, which is mainly achieved by catalyst. The importance of eliminating waste production and development of green process using eco-friendly oxidants to oxidize alcohols attracts much research interests. The research progress in the catalytic oxidation of alcohols using eco-friendly ox-idants such as oxygen, hydrogen peroxide and acetone since 2000 was reviewed. At the same time, the characteristics of different methods were summarized. The development trend of green catalytic oxidation of alcohols was presented.
LIU Jin-xiang , CHEN Zi-geng , XIE Shui-bo , LIU Ying-jiu , YU Kun
2019, 36(7).
Abstract:In this experiment, oxidation-nitriding carbon nanomaterials (OCN) were successfully synthesized by a acid etching and oxidation method,and the adsorption-desorption performance of OCN on U(VI) in water was investigated.The effects of pH,temperature,OCN dosage,initial U(VI) concentration,contacting time were investigated by static batch experiments,and the adsorption mechanism was discussed.The sorption experiments indicated that OCN exhibited superior adsorption performance to U(VI),When at pH 5, the initial concentration 10 mgU(VI) L-1 ,OCN dosage 200mg/L and 30℃ ,the adsorption efficiency of OCN to U(VI) reached 98.9%.Compared with the unmodified graphite nitride carbon (g-C3N4), the adsorption performance of U(VI) was improved by about 30%,and the adsorption reaction reached the adsorption equilibrium at 10 min.The adsorption process is greatly affected by the pH of the solution and is less affected by other factors such as temperature. The pseudo-second-order kinetic equation and Langmuir model fit the adsorption process well, and the adsorption process of OCN to U(VI) is spontaneous endothermic process. The results of adsorption desorption experiments show that OCN has good reusability and a broad application prospect in the treatment of U(VI)-containing wastewater as a high-performance adsorbent.
2019, 36(7).
Abstract:The coated polyethylene(PE) separators were prepared (through a direct coating process) with Al2O3 as ceramic particle, acrylate emulsion as binder and deionized water as solvent. The PE separators and coated PE separators were characterized by surface tension, contact angles testing, electrolyte wettability, electrolyte uptake, thermal resistance, as well as electrochemical testing. The results showed that the surface tension of ceramic slurry decreased from 37.0 mN/m to 28.5 mN/m as 0.10 % fluoro-containing surfactant was added. Compared with PE separators, the wettability, heat resistance and electrochemical performance of coated PE separators were improved. The electrolyte uptake of the coated PE separators increased from 85 % to 165 %, and the thermal shrinkage decreased from 65 % to 3 % at 150 ℃. The capacity retention of the PE separators were only 84.7 % in 200 cycles, while that of the coated PE separators reached 90.2 % at the same condition. The capacity retention rates of the coated PE separators were slightly higher than that of the PE separators at different charge-discharge rate. The complex impedance and cyclic voltammograms of these two materials were similar.
2019, 36(7).
Abstract:The waterborne soybean oil-rosin-based hyperbranched polyester was prepared from rosin, soybean oil, maleic anhydride and glycerol and characterized by FTIR, GPC and TG. The results showed that the preferred conditions for the preparation of the polyester are as follows: the dosage of soybean oil was 50% by mass of rosin, that of maleic anhydride was 20% by mass of rosin, and the hydroxyl-carboxyl ratio of raw materials was 0.86 by adding glycerol, esterification reaction temperature was 250℃, and reaction time was 3 h. Under these conditions, the number average molecular weight (Mn) of the prepared hyperbranched polyester was 1776, the weight average molecular weight (Mw) was 5305, the acid value was 49.9 mg/g and softening point was 67℃. The yellow transparent colloid solution was obtained after 3 hours of emulsification. TG results indicated that the decomposition of polyester was mainly concentrated in the ranging from 350℃ to 450℃, indicating that it had higher thermal stability. The particle size distribution of the hyperbranched polyester colloidal solution demonstrated that the average particle size of the whole system was 22.14 nm, which revealed that the polyester had good emulsifying and dispersing properties in water.
GAO Teng , LIU Ying , ZHANG Wei-wei , WU Yan-chao
2019, 36(7).
Abstract:A series of anti-corrosion nanomaterials, AcOH-PANI, AcOH-PmAP, MOPAc-PmAP and MOPAc-PANI were synthesized by using aniline (AN) and m-aminophenol (mAP) as monomers, acetic acid (AcOH) and p-methoxyphenylacetic acid (MOPAc) as doped acids, Fenton (Fe2+/H2O2) reagent as initiator. The morphology and structure of the polymer materials were characterized by FTIR, UV-vis, XRD, SEM and particle size analyzer. The results showed that the polymer prepared by using p-methoxyphenylacetic acid as doped acid had uniform particle size distribution and good solubility. Electrochemical tests suggested that the polymer was a cathode-based mixed corrosion inhibitor, and the corrosion inhibition efficiency followed the order MOPAc-PmAP > AcOH-PmAP > MOPAc-PANI > AcOH-PANI. MOPAc-PmAP and AcOH-PmAP, in presence of Tween80, showed better anticorrosion properties. Especially when the concentration of corrosion inhibitor was 100 mg/L and that of Tween80 was 50 mg/L, the system of MOPAc-PmAP-Tween80 had the outstanding corrosion inhibition efficiency as high as 96.05%, which was higher than the system in absence of Tween80 (71.04%), indicating that there was excellent synergism between MOPAc-PmAP and Tween80.
FAN Yong-kang , Xiang Ting , Cui Xin Yu , Xia Chenn , Ye Qian Zhen , Shen Jian fu
2019, 36(7).
Abstract:Casein-pectin electrostatic complex was constructed by electrostatic adsorption, and quercetin was encapsulated in the complex to improve the stability of quercetin. Casein-pectin composites were prepared under acidic conditions. It was found that the highest transmittance was 0.81 when the concentration ratio of Casein-pectin was 1:2. Under different pH (2.0~7.0) conditions, Casein-pectin complex exhibited better stability than Casein. When the concentration of CaCl2 was 20 mg/mL, the diameter of Casein-pectin composite was the smallest, which was 346.1 nm. UV-vis curves showed that quercetin had been embedded in the Casein-pectin complex. DPPH and ABTS experiments demonstrated that quercetin showed better water-solubility and antioxidant activity (p < 0.05). The complex of Casein-quercetin-pectin showed good thermal stability (p < 0.05) when heated at 60 ℃ (pasteurization). The vitro digestion experiment indicated that Casein-quercetin-pectin had good sustained release ability.
2019, 36(7).
Abstract:Diblock copolymer P(4-ASt-b-NIPAm) with well-defined structure and narrow molecular-weight distri-bution (Mw/Mn=1.28) was synthesized by reversible addition-fragmentation transfer (RAFT) polymeriza-tion using poly(4-acetoxystyrene) P(4-ASt) and N-isopropylacrylamide (NIPAm) as monomers. The ace-tyl groups in the chain of P(4-ASt-b-NIPAm)) were selectively hydrolyzed by hydrazine hydrate to obtain diblock copolymer P(4-VPh-b-NIPAm). Copolymer P(4-VPh-b-NIPAm) was characterized by 1HNMR, FTIR and GPC. The aggregation behavior and temperature response of P(4-VPh-b-NIPAm) aqueous solu-tion were studied by fluorescence spectrum, transmittance method and DLS. The results showed that co-polymer P(VPh-b-NIPAm) could self-assemble into micelles using P(4-VPh) as core and PNIPAm as shell in aqueous solution and the critical micelle concentration (CMC) was 0.015 g/L. The average parti-cle size was about 137 nm at room temperature and the lower critical solution temperature (LCST) was 31.2℃. Horseradish peroxidase (HRP) catalyzed cross-linking of P(4-VPh) core to prepare core-crosslinked micelles with an average particle size of 119 nm. TEM showed that dry core-crosslinked micelles were spherical with particle size of 60~100 nm. The aqueous solution of core-crosslinked mi-celles had good stability and temperature response. Its phase transition temperature ranged from 32℃ to 36℃ and its LCST was about 34.9℃. The average diameter of core-crosslinked micelles decreased from 119 nm to 93 nm with increasing temperature from 25℃ to 37℃.
SHI Lei , HUANG Ling , GONG Sheng-zhao , HONG Hao-jia , XIANG Hua
2019, 36(7).
Abstract:Hypochlorite is widely used in the disinfection products for hard surface and water, and the detection of hypochlorite is very important. The ratiometric fluorescent probes have many advantages, such as high sensitivity, fast response, good selectivity and real-time monitoring, and the ratiometric probes could elim-inate the background interference well. Therefore, a ratiometric fluorescent probe ZN1 for hypochlorite was synthesized in this work. This probe possesses high speed, great sensitivity, and nice selectivity for de-tection of hypochlorite ions, and it has been successfully applied for the detection of hypochlorite in real water samples. Moreover, the sensing mechanism of the probe was studied by MS and NMR spectra.
XU Li-jie , LU Zhen-zhen , ZHOU Jian-ting
2019, 36(7):0-0.
Abstract:Transparent superhydrophobic SiO2/ silicone sealant composite coatings were prepared by spray coating method with hydrophobic nano-SiO2 and neutral silicone structural sealant, which were used as main raw materials. The molecular structure, microstructure, wettability and transmittance of the composite coatings were characterized by FTIR, SEM, contact angle measurement and UV-vis spectrophotometer. The relationship between the content of nano-SiO2 and the surface microstructure, water contact angle and transparency of the coatings was discussed. The water impact resistance and water stability of the composite coatings were also studied. The results showed that the surface of the SiO2/silicone sealant composite coatings displayed the continuous porous network structure, and aggregated SiO2 nanoparticles dispersed around the sub-micron silicone sealant which acted as the backbones, forming the micro-nano composite rough structures. When the mass ratio of nano-SiO2 was 2%, the maximum water contact angle of 169.8? and the average transmittance of 82.9% under visible range from 380 nm to 760 nm were obtained. In addition, when the mass ratio of silicone sealant was 4%, the water contact angle of the composite coatings remained above 140?after 5 h of water impact and 10 d of water immersion respectively.
Qian Fengyi , Li Rong , Ren Xuehong
2019, 36(7).
Abstract:Gemini surfactants containing two hydroxyl groups (abbreviated as 12(OH)-s-12(OH), s = 3, 4, 6, 8, 10 and 12) were synthesized using 1-Bromododecane, 2-methylaminoethanol, 1,3-Dibromopropane, 1,4-Dibromobutane, 1,6-Dibromohexane, 1,8-Dibromooctane, 1,10-Dibromodecane and 1,12-Dibromododecane. The thermal property and surface tension of Gemini surfactants in aqueous solu-tion were characterized. The results indicated that the foaming ability of the Gemini surfactants was measured. The aggregation property of Gemini surfactants in aqueous solution were simulated using dissi-pative particle dynamics (DPD). The Gemini surfactants have good thermal property and foaming property. The critical micelle concentration (CMC) of Gemini surfactants were decreased from 0.62 mmol/L(s = 3) to 0.21 mmol/L(s = 6) with the increase of spacer (s≤6), and the CMC almost keep the same when the spacer was continue increased (s >6). With the increase of Gemini surfactant concentration, the aggregate morphologies in aqueous solution were changed from spherical micelle → rod micelle → layered micelle, eventually to reverse micelle network structure. The length of spacer almost has no efficient on the micelle morphology transition in aqueous solution.
YU Ddai-bing , LI Hong-mei , YANG Juan , GAO Lu-jiao , SUN Shifan
2019, 36(7).
Abstract:Abstract:NMN (nicotinamide mononucleotide) transferase and ethanol dehydrogenase were covalently immobilized with magnetic nanoparticles; to produce NADH (nicotinamide adenine dinucleotide). The conditions of co-immobilization, the properties and kinetics of co-immobilized enzyme were investigated. The optimized immobilization condition as follow : NMN transferase and alcohol dehydrogenase are 6.5 U/0.5 mg and 10.3 U/0.5 mg, respectively, and the system pH is controlled at 5.0-7.0 to immobilize the enymes for 2 h at 25℃, under which condition, NADH yield could reach 87%. After 11 reuses of the co-immobilized double enzyme, the residual enzyme activity still remains at about 61.1%, which showed a good operational stabilization. The deduction and validation of the kinetic equation of two enzymes showed that the reaction system of co-immobilized double enzymes accorded with Michaelis equation, and its kinetic reaction rate depended on the reaction rate of immobilized ethanol dehydrogenase.
ZHOU Shi-xing , SHAO Hua , WEI Cai-xia , Nigora Kuchkarova , HAN Caixia , JIN Guang-zhao
2019, 36(7).
Abstract:The chemical composition of the essential oil isolated by hydrodistillation from the flower part of Dracocephalum integrifolium Bunge was analyzed by GC/MS, and the activity of phytotoxicity was tested. Thirty three compounds were identified, representing 95.97% of total oil, which was found to be rich in monoterpene hydrocarbons (29.21%),oxygenated monoterpenes (17.27%),sesquiterpene hydrocarbons (23.84%) and oxygenated sesquiterpene (25.65%). The main constituents of the oil were eucalyptol (15.55%), α-bisabolol (10.29%), nerolidol, cis-(+) - (8.81%), β-Pinene (8.25%), (E)-β-ocimene (7.44%) and α-thujene (5.45%). The essential oil completely inhibited seed germina-tion of Amaranthus retroflexus and Poa annua at 2 μl/ml, meanwhile it exhibited weak activity on Echinochloa crusgalli. In general, the oil possessed promotive activity at low concentration and in-hibitory activity at high concentration. This is the first report on the chemical constituents as well as the phytotoxic activity of the essential oil of D. integrifolium flowers.
2019, 36(7).
Abstract:Abstract: Four Brønsted acidic ionic liquids (ILs) were synthesized using 1-methylimidazole, 1,3-propane sultone, sulfuric acid, phosphoric acid, tetrafluoroboric acid and p-toluene sulfonic acid as raw materials. Their structures were characterized and the acidity H0 was measured. These ionic liquids were applied to the synthesis of bisphenolfluorene. When the H0 was less than or equal to 1.94, the ionic liquid had cata-lytic effect, when that was less than or equal to 1.69, the ionic liquid had applicable value. A method for the determination of bisphenolfluorene by liquid chromatography was developed. The reaction products were separated and the structures of the three products were determined by NMR. The effect of reaction parameters on the condensation reaction of 9-fluorenone and phenol was investigated by univariate opti-mization. The optimal reaction conditions were obtained as follows: n(phenol): n(9-fluorenone): n(IL1)=6:1:0.125, n(IL1): n(thioglycolic acid)=5:2, reaction temperature 110℃ and reaction time 6 h. The catalytic effects of the four catalysts in the synthesis of bisphenolfluorene were investigated under the above conditions. For IL1, L IL2 and IL4 catalysts, the conversion of 9-fluorenone was 100%, and the selectivity of bisphenolfluorene was nearly 87%. In addition, the catalytic effect of ionic liquid IL1 was not significantly reduced after 5 consecutive uses.
Xiao Jun-Fei , ZHANG Yu-Yu , Sun Bao-Guo , Chen Hai-Tao , Sun Ying , Yang Xiao
2019, 36(7).
Abstract:In order to compare and analyze the content and flavor characteristics of free amino acids, organic acids and nucleotides in 4 kinds of Suancai, high performance liquid chromatography (HPLC) was used to separate and identify. The taste active value (TAV) was calculated and used to determine the contribution of each flavor component to the taste of Suancai. The results showed that the content of asparagus amino acid was the highest in four kinds of pickles, accounting for 46%~53.21% of total free amino acid content, followed by bitter arginine and sweet alanine; the lactic acid content in Suancai samples 1, 3 and 4 was the highest, accounting for 41.69%, 30.96% and 38.76% of total organic acid content, followed by acetic acid and oxalic acid; The top three organic acids were oxalic acid, lactic acid and acetic acid in sample 2. The nucleotide content in sample 1 was the highest, 0.0556 mg/g, followed by sample 2 was 0.0516 mg/g. The analysis of TAV showed that the TAV of aspartic acid, oxalic acid, formic acid, lactic acid, acetic acid, citric acid and succinic acid in 4 kinds of pickles were all more than 1, which contributed greatly to the taste of Suancai.
ZHANG Jing-lin , li juan , wang juan , sun baoguo , liu yuping , huang mingquan
2019, 36(7).
Abstract:Aroma is one of the important standards to evaluate extracts. Analysis flavor components will provide reference for extracts application and quality control standard. The volatile flavor components of treemoss extracts were analyzed by solid phase microextraction (SPME) and solvent-assisted flavor evaporation (SAFE) combined with gas chromatography-mass spectrometry (GC-MS) and the aroma active components were confirmed by gas chromatograph-olfactometer (GC-O) with aroma extract dilutions analysis (AEDA). It was shown that a total of 102 compounds in two treemoss extracts samples (S1 and S2) were identified. Among these, there were 27 active odorants in two treemoss extracts, and the odorants with FD > 9 were methyl β-orcinolcarboxylate, ethyl levulinate, ethyl orsellinate, ethyl hematommate, ethyl nonanoate, ethyl heptanoate and ethyl phenylacetate. Moreover, these active odorants were quantitated by internal standard method and its odor active values (OAV) were calculated; it was confirmed methyl β-orcinolcarboxylate, ethyl orsellinate and ethyl heptanoate were the key odorants of the treemoss extracts.
WANG Juan , Yi Xiang , Yang Qiang , TONG Guoqiang , HUANG Ming-quan , Liu Yuancai
2019, 36(7).
Abstract:The volatile compounds of tartary buckwheat extract was extracted by solidphase micro-extraction (SPME) and analyzed by gas chromatography-mass spectrometry (GC-MS). Then aroma-active compounds were identified by gas chromatography-olfactory (GC-O) combined with aroma extraction dilution analysis (AEDA). Finally, the key odorants of tartary buckwheat extract were confirmed by their odor activity values (OAVs). The results showed that 92 kinds of volatile compounds including 28 esters, 7 aldehydes, 9 alcohols, 7 ketones, 6 acids, 8 olefins, 20 alkanes, and 7 others were identified by SPME-GC-MS. By application of GC-O/AEDA, seventeen odor-active compounds with flavor dilution (FD) factor range from 1 to 243 were detected. Quantitation results showed that benzyl alcohol (8637.43 μg/kg), phenylacetaldehyde (3150.47 μg/kg), and D-limonene (3080 μg/kg) had a higher concentration. Finally, benzaldehyde, dimethyl trisulfide, benzyl alcohol, phenylacetaldehyde, diethyl malonate were confirmed as the key odorants of the tartary Buckwheat extract for their highest FD factors and OAVs.
WANG Shu-wei , SUI Xin-ping , LI Meng , SUN Bao-guo , CHEN Hai-tao , ZHANG Ning
2019, 36(7):0-0.
Abstract:Volatile compounds of raw and stir-fried Chinese chive were extracted by solvent-assisted flavor evaporation (SAFE) and analyzed by gas chromatography-mass spectrometry (GC-MS) with two kinds of different polarity chromatographic column. A total of 83 volaitle compounds were identified in raw Chinese chive, 127 volatile compounds were identified in stir-fried Chinese chive. Contents of esters and aldehydes were the main factors that causing the differences in the flavor profile of raw and stir-fried Chinese chive. Gas chromatography-olfactometry-mass spectrometry (GC-O-MS) combined with aroma extract dilution analysis (AEDA) was applied to identify aroma-active compounds in the two samples. Components with higher flavor dilution (FD) factors (FD≥27) were considered to have positive impact to the general flavor of samples. From this point, 17 compounds had larger contribution to the flavor profile of raw Chinese chive while 10 compounds to the stir-fried one. The identical key aroma component of the two samples was methyl allyl disulfide, which had spicy and garlicy odor. The aroma components of raw Chinese chive were mainly thioethers, which provided spicy and sour odor. Besides, the aroma substances of stir-fried Chinese chive were mainly aldehydes and heterocyclic compounds, which provided roasted and scorched odor.
ZHANG Yu-jing , LI Yun-hong , JIANG Chun-peng , YANG Shu-qi , HAN Jian-xin , ZHANG Ying
2019, 36(7).
Abstract:H-BLFnp is a novel composite nanomaterial taking high purity c-glycoside flavonoids of bamboo leaf as leading material. Based on the whitening effect evaluated by B16 melanoma cells in vitro, its skin care function was further evaluated on the human body in this paper. The indexes of biological efficacy includes skin moisture content, percutaneous moisture loss, skin gloss, brightness, melanin content and skin elasticity were tested before and after subjects using the samples. The purpose is to explore the biological efficacy of H-BLFnp on moisturizing, whitening, anti-aging, etc. Results showed that H-BLFnp significantly inhibited B16 cell proliferation, tyrosinase activity and melanin synthesis taking β-arbutin as a positive control (p<0.05), the inhibition rates achieved 45.14%, 72.55% and 54.01% respectively when the concentration of H-BLFnp was at 100 μg/mL. The H-BLFnp may exert whitening effect through inhibiting melanocyte proliferation, tyrosinase activity and melanin synthesis. Clinic test showed that H-BLFnp can significantly increase skin moisture content, skin elasticity, brightness and gloss, and reduce skin melanin content and percutaneous moisture loss.
guoliqiao , hanfangyu , libin , maoxinbiao , xuyinghua
2019, 36(7).
Abstract:Electrochemical dechlorination of 2-chloro-5-trichloromethylpyridine (TCMP) to 2-chloro-5-chloromethylpyridine (CCMP) has important industrial application value in the preparation of imidacloprid. In this work, the influence of various process conditions (such as supporting electrolyte, cathode materials and their mesh number, temperature and current density) on the dechlorination, and the dechlorination potentials of TCMP and its dechlorinated products were investigated using bulk electrolysis experiments. The experimental results show that lithium acetate is the best choice among lithium acetate, lithium chloride, lithium perchlorate, ammonium chloride and tetrabutyl ammonium perchlorate. The yield of CCMP on each cathode material decreases in the following order: Cu > Pb > graphite > Ag > Zn > Ni. Under optimized process conditions (catholyte: methanol solution containing 10 φ(%) CH3COOH 5 φ(%) H2O 0.2 mol/L CH3COOLi 0.1 mol/L TCMP, cathode: 80 mesh copper, temperature: 30℃, the current density: 333 A/m2 at the early stage of reaction and 166 A/m2 at the last stage of reaction), 0.1 mol/L TCMP could be selectively dechlorinated to CCMP with the yield of 56.9%. The dechlorination po-tential of TCMP to DCMP is more positive than that of DCMP to CCMP, and the later is almost same to that of CCMP to CMP.
2019, 36(7).
Abstract:P-[(4,6-dichloro-1,3,5-triazin-2-yl)-oxy]benzene sulfonic acid sodium salt(TSP) was synthesized by condensation reaction of cyanuric chloride and p-phenolsulfonic acid in the presence of water.The molecular structure of TSP was characterized by FTIR and 1HNMR,then the analysis results showed that cyanuric chloride reacts with p-phenolsulfonic acid to form the target product.TSP was applied to delimed and bated sheep skin.Through the shrinkage temperature and physical sense of the leather,as a basis for evaluating the tanning effect,the reasonable tanning condition was obtained by single factor experiment:100% water,25% TSP(based on the weight of limed sheepskin),the tanning temperature in three stages of 25℃、40℃ and 50℃,and each temperature stage was tanned for 2 hours,the total tanning time was 6 hours and the ultimate pH was kept at 5.5~6.0 by basification.The results indicated that the shrinkage temperature of crust leather could reach 78℃ or so,and the leather had fine white grain and good touch.As a organic tanning agent,the compound has a good application prospect in leather making.
2019, 36(7).
Abstract:The CDs/ZnO/g-C3N4 composites were prepared by impregnation-thermal polymerization method, and the photodegradation efficiency of Rhodamine B was investigated. The catalyst was characterized and evaluated by means of XRD, TEM, XPS, UV-Vis DRS and FI-IR. The results show that CDs/ZnO/g-C3N4 still maintains the crystal structure of g-C3N4 in the graphite phase, and the ternary components synergistically make CDs/ZnO/g-C3N4 exhibit excellent photocatalytic properties, which degrade Rhodamine B. The effect is better than monomer g-C3N4, ZnO and ZnO/g-C3N4, and the decolorization rate can reach about 70%.
LU Jun-rui , LI Jia-dong , XIE Zhi-qiang
2019, 36(7).
Abstract:The Fe3O4 magnetic powder was prepared with simple co-precipitation oxidation method using steel pickling waste liquor as raw material. The ratio of Fe3+∶Fe2+ in the reaction solution was monitored by the change of pH during the reaction process,which provided a simple operation for the co-precipitation oxidation method. The catalytic effect of Fe3O4 with small particle size and Alfa reagent grade of 50~100 nm on the synthesis of coumarin derivatives and quinoxaline derivatives was compared. The prepared Fe3O4 samples were characterized by VSM,XRD and TEM. The structures of the compounds were con-firmed by nuclear magnetic resonance spectroscopy (NMR) and high resolution mass spectrometry (HRMS).
2019, 36(7).
Abstract:A three-dimensional iron(III)-zinc (II) porphyrin framework PCN-600(Zn) was constructed, with the 5,10,15,20-tetrakis (4-carboxyphenyl) porphyrinato]-Zn (ZnTCPP) as the ligands, and the Fe as the nodes. The resulting material was characterized by powder X-ray diffraction, scanning electron microscopy, ultraviolet-visible diffuse reflectance spectra. After that, it was used for the degradation of rhodamine B (RhB) under visible light irradiation. And we studied the effect of H2O2 concentration on the degradation efficiency of PCN-600 (Zn) as well as the main reactive species during the photocatalytic reaction. In addition, we compared the photocatalytic performance of PCN-600 (Zn) and PCN-222 (Zn), a zirconium (IV)-zinc (II) porphyrin framework. The experiment results show that the catalytic performance of PCN-600(Zn) is not very obvious for the degradation of RhB. However, it exhibits a significant performance with the synergistic effect of H2O2. And in the experimental range, with the increase of H2O2 concentration, the catalytic performance of PCN-600 (Zn) gradually improves. Experiments prove that during the catalytic process, holes (h ) are the main reactive species, and ?OH and ?O2- also make a certain contribution. More importantly, the photocatalytic performance of PCN-600 (Zn) is significantly better than that of PCN-222 (Zn).
2019, 36(7):0-0.
Abstract:A novel scale inhibitor, polyethylene glycol ester / sodium vinyl sulfonate / acrylic acid (PEGMA-SVS-AA), was synthesized using polyethylene glycol ester (PEGMA) with sodium vinyl sulfonate (SVS) and acrylic acid (AA) monomer as raw materials. Synthesized target copolymer PEGMA-SVS-AA was using ammonium persulfate as initiator. The effect of polymerization process on the performance of calcium carbonate scale inhibition was investigated. The copolymer PEGMA-SVS-AA was determined by infrared. The experiment showed that when the monomer ratio n(PEG200MA) ): n(SVS): n(AA) is 1:3:5, the amount of ammonium persulfate is 6% of the total amount of monomers, the reaction time is 2.5 h, and the control reaction temperature is 80 °C, simulating the industrial production cycle cooling water conditions. The rate of calcium carbonate inhibition reached 89%. The effects of initiator dosage, time and reaction temperature on the performance of the synthesized water treatment agent were investigated. Carbonate scale was characterized using XRD and SEM, which not only altered the morphology of the calcium carbonate but also changed the crystal form.
PENG Chuan , GOU Shao-hua , FEI Yu-mei , ZHANG Hui-chao , WANG Pei-pei
2019, 36(7).
Abstract:A zwitterionic copolymer (ANND) containing twin-tail structure was synthesized using acrylamide (AM), acrylic acid (AA), N,N-dioctylmethacrylamide (DLMB) and 3-(2-methacrylamidopropyldimethylamino)propane sulfonate (MDPS) via free-radical copolymerization. The copolymer was characterized by FT-IR, 1H NMR and TG-DTG to confirm that it was prepared successfully and had favorable thermal stability. And compared with partially hydrolyzed polyacrylamide (HPAM), the thickening property, water solubility, aging resistance, shear thinning, temperature tolerance and salt resistance of the copolymer were investigated. The results showed that the copolymer had excellent water solubility and thickening property, and its apparent viscosity could reach 466.5 mPa·s at 2000 mg/L. The apparent viscosity of the copolymer could remain 60.4 mPa·s under 510 s-1 and 182.6 mPa·s at 120 oC. And the viscosity retention value of AADM could remain 94.6 mPa·s after 30 days of aging. When the copolymer was dissolved in 15000 mg/L NaCl, 2000 mg/L MgCl2 and 2000 mg/L CaCl2 solutions, the apparent viscosity of these copolymer solutions were 77.8, 72.4 and 68.6 mPa·s, respectively. Core flooding experiment further indicated that the copolymer solution could enhance oil recovery by 7.72%. The above experimental results are superior to those of HPAM under the same conditions, because the introduction of the twin-tail structure effectively enhances the hydrophobic association ability of the copolymer, and the introduction of the zwitterionic monomer weakens the sensitivity of the molecular chain to the salt.
FENG Qian , LIU Xian-jie , PENG Zhi-gang , HUO Jin-hua , LIU Huan
2019, 36(7).
Abstract:Hydrate layers are common in deep water environment with low temperature and high pressure. During surface casing cementing, hydration and heat release of cement slurry in deep water is easy to decompose natural gas hydrate and lead to formation instability, which brings great risks to deep water cementing. Based on the decomposition characteristics of natural gas hydrate at low temperature, high pressure and electrolyte, a low-hydration hot cement slurry system was successfully developed, with Portland oil well cement as the base material and the addition of self-developed micro-capsule type thermal control material (PCM-1). In the early hydration process of the cement slurry system, the temperature was continuously measured by self-developed semi-adiabatic test equipment, and the hydration heat control effect was characterized by the maximum temperature (Tm) and the maximum hydration temperature rise (Tr) of the cement slurry system. The results showed that compared with pure slurry cement system, hydration maximum temperature decreases by 21.1℃, when 15 wt% PCM-1 was added. At the same time, the maximum hydration temperature rise decreased by 23.6℃. In addition, 24 h and 48 h hydration heat respectively decreased by 7.68?104 J and 7.28?104 J. This technique can effectively control the hydration temperature rise and hydration heat of cement slurry, greatly reducing the cementing risk of hydrate layers in deep water.
2019, 36(7).
Abstract:Thermoplastic polyurethane (TPU)/leucine (Leu) anticorrosion strippable films TPU/Leu-1、TPU/Leu-2、TPU/Leu-3 before and after compatibilization modified were prepared. The anticorrosion resistance performance of films were investigated by salt water test, tafel polarization curve and electrochemical impedance spectroscopy(EIS). Proceed from the inhibition corrosion of films on the diffusion of corrosive particles to carbon steel surface, the diffusion behavior of corrosive particles and the anticorrosion action of three kinds of TPU/Leu anticorrosive strippable films were studied by molecular dynamics simulation method. The results showed that the χ of TPU and Leu was less than χc and the δ and CED increased after adding compatibilizer KH-560 and E44. RDF results showed that the interaction force between components of strippable films and compatibilizers mainly included hydrogen bonding and electrostatic adsorption. It indicated that KH-560 and E44 can play an important role in improving compatibility of TPU/Leu strippable films. The corrosion potential of TPU/Leu-1 was -0.430V, while corrosion potential values of TPU/Leu-2 and TPU/Leu-3 increased to -0.320V and -0.348V. It illustrated that the corrosion resistance of strippable films were improved after modification. The diffusion of MD simulation results showed that self diffusion performance and D declined adding compatibilizer. Meanwhile, FFVH2O(TPU/Leu-2)<FFVH2O(TPU/Leu-3)<FFVH2O(TPU/Leu-1), FFVCl-(TPU/Leu-2)<FFVCl-(TPU/Leu-3)<FFVCl-(TPU/Leu-1). The result showed description of strippable films inhibit the diffusion behavior, in which the inhibition effect of KH-560 modified TPU/Leu-2 was the most obvious.
WANG Na , GAO Hui-ying , ZHANG Jing , LI Long
2019, 36(7).
Abstract:The SBA-15 molecular sieve was grafted onto the graphene to prepare the functional filler. Which was applied in water-based epoxy resin. The filler was characterized by fourier transform infrared spectroscopy, nitrogen adsorption–desorption isotherms and transmission electron microscopy. The corrosion resistance and mechanical properties of the coating with different amount of filler were characterized by electrochemical impedance spectroscopy (EIS), salt spray test and adhesion test. The experimental results showed that when adding 1.0% functional filler, the coating had the best electrochemical performance, salt spray resistance and adhesion performance. The anticorrosive property of the composite coating was superior to that of pure epoxy coating, due to the pore/sheet synergistic of the functional filler added. The time of corrosion particles to the surface of the metal substrate was delayed effectively.
2019, 36(7).
Abstract:The continuous flow process of liquid phase oxidation to glyoxylic acid was studied in a microchannel reactor using glyoxal and hydrogen peroxide as raw materials.The effects of material ratio, catalyst dosage, hydrogen peroxide concentration, residence time and temperature on the reaction were investigated.The optimized reaction conditions are: n(glyoxal)∶n(H2O2)∶n(FeSO4)= 1∶1∶0.13, the hydrogen peroxide concentration 1.67 mol/L, residence time 10 min, and reaction temperature 30℃. Under the above-mentioned reaction conditions, glyoxal conversion rate reaches94.7%and the glyoxylic acid selectivity reaches 85.4%.This process takes full advantage of the excellent mass and heat transfer characteristics of the microchannel continuous flow reactor, greatly shortens the reaction time, increases the reaction rate, expands the selection range of the process conditions, realizes the effective control of the oxidation reaction process, and increases the safety factor.
2019, 36(7).
Abstract:The reactive behavior on hydrogenation of p-nitroaniline in water catalyzed by supported nickel catalyst was studied. The laboratory test and pilot-plant test were conducted. The effects of reaction temperature, pressure, holding time, p-nitroaniline mass concentration and wastewater recycle on the hydrogenation reaction were investigated. The results showed that the product p-phenylenediamine has high mass fraction, and catalyst and water can be recycled. The optimal reaction parameters are that temperature 110℃, reaction time 2~3 h, pressure 2.0 MPa, stirring speed 800 r/min, dosage of initial catalyst 10% (based on the mass of p-nitroaniline, similarly hereinafter), catalyst loss 0.2% (based on the additive mass of initial catalyst). Under these optimal reaction conditions, the conversion of p-nitroaniline was 100%, and the yield of p-phenylenediamine was over 99.5%. The amount of wastewater discharged after wastewater recycle was small and had no effect on catalytic activity and product quality.
ZHU Yun-ying , BAI Song , WU Qin
2019, 36(7).
Abstract:Nine chiral malonate derivatives containing 1,3,4-thiadiazole moiety (Ⅳa~i) were synthesized by one-pot asymmetric Mannich reaction using cinchona alkaloid squaramide catalyst. High yields (70%~89%) and excellent enantioselectivities [up to>99%, enantiomeric excess (e.e.)] were obtained in toluene in the presence of 10 mol% catalyst Ⅴe at 60 ℃ which were the optimum reaction conditions . The bioassay results showed that these derivatives possessed good activities against tobacco mosaic virus (TMV). Especially, chiral compound (-)-Ⅳf exhibited high curative and protective activities against TMV in vivo (50.8% and 42.6%, respectively), equivalent to that of commercially available antiviral agent riba-virin.