MA Feng-sen , ZHAN Hao-hui , HUANG Ying-cong , ZHANG Jie
2018, 35(4).
Abstract:The dissolving microneedles have gradually become a popular way of transdermal delivery. This paper mainly introduces all the application areas of dissolving microneedles loaded with small molecule compounds, which are divided into functional categories, treatment, diagnosis and popular cosmetology on the market nowadays.Combining with the specific microneedles preparation examples, the research progress is described by analysing of the small molecule compounds loaded in dissolving microneedle are superior to traditional pharmaceutical preparations from the properties of different compounds in various application fields. It is concluded that compounds loaded in dissolving microneedles should possess the characteristics, such as high activity , high stability, the use of traditional skin preparations can not achieve the desired effect, high additional value and combining with the characteristics of the microneedles, which provides reference for other scholars to further study the small molecule compounds loaded in dissolving microneedles. Finally, the current problems of dissolving microneedles have been put forward and the future trend of dissolving microneedles is forecasted.
ZHAO Yue , ZHAO Chun-lei , WANG Rui , GONG Hong , JIANG Heng
2018, 35(4).
Abstract:Uranium is one of the most dangerous radioactive metals, which is widely existing in waste water with uranium from nuclear fuel preparation, irradiated fuel treatment mining production activities and etc, which badly endangers aquatic ecosystems and human health. Adsorption has been found to be superior to the other techniques including simplicity, high efficiency, economical, good selectivity and so on. The adsorption materials applied for U(VI) removal and separation from water in recent three years is summarized. The typical adsorption materials of inorganic material, bio-derived material, organic material and inorganic-organic composite material were mainly introduced in terms of preparation processes, structure characteristics and adsorption properties. The research direction of adsorbent for U(VI) removal and separation in water was outlooked.
FENG Hui-xia , yangyang , liquanzhen , 李东东 , 张亚飞 , zhaodan , chennali
2018, 35(4).
Abstract:Using diatomite, chitosan and Fe3O4 as starting materials, a new low cost diatomite composite magnetic chitosan material was prepared by a simple method and studied for removal of Cr (VI) from waste water. Studied the effects of various parameters and studied adsorption kinetics, thermodynamic and isothermal model. The experimental results show that the adsorption capacity using diatomite composite magnetic chitosan material could reach 47.8mg/g at the best conditions, the situation is 15℃, pH=3, it is conducive to the adsorption at low temperature. Fitting the isothermal model, the Langmuir model provided well correlations of the experimental data, and kinetic data was well fitted by the pseudo-second-order model, the thermodynamics parameters of adsorption system indicated exothermic process. And the adsorbent can be recovered by adding NaOH solution after saturation.
guojunhong , Xu fen , Bao Xue-mei , Mu Bo , YANG Baoping , CUI Jin-feng
2018, 35(4).
Abstract:The oligophosphate (OPP) was synthesized by step-reaction polymerization using phenyl dichlorophosphate(PDCP), ethylene glycol(EG), methanol, the composites OPP/PS was prepared by polystyrene as matrix and oligophosphate (OPP). The short chain chemical structure and long-range structure of molecular chain characteristics and relative molecular mass of OPP was explored by FT-IR and gel permeation chromatography(GPC). The mechanical properties, thermal stability and flame-retardant properties of the OPP/PS was evaluated by the SEM, XPS, universal material experiment machine, TGA, limit oxygen index(LOI) and microscale combustion calorimeter. The thermal decomposition activation energy(Ea) of composites were calculated by Flynn-Wall-Ozawa(FWO) method. The results show that the heat release rate peak (PHRR) decreases, the total heat release (THR) decreases, and the LOI increases gradually and the residual carbon rate increases with the increase of OPP content in OPP/PS composites. When the w(OPP)=10%, the PHRR of the OPP/PS composites was 585.00 W/g, the THR was 14.41 kJ/g, the LOI was 24.5%, the residual carbon ratio in the nitrogen atmosphere is 11.27, the Ea decreases with the increase of thermal degradation rate α, thermal decomposition products of OPP polymetaphosphate catalytic substrate into carbon, and covered the surface of a partition the material in the layer of heat and oxygen and carbon layer, to improve the thermal stability and flame retardant properties of OPP/PS composites.
Yang Ling-fang , Liu Zhi-rong , Wang Yun , Qiu Yang , Min Han-qing , Liu Yu-nan
2018, 35(4).
Abstract:Batch experiments were performed to study the dependence of Th(IV) absorption by insoluble humic acid (IHA) on IHA dosage, reaction time, pH、initial concentration and temperature etc. Absorption kinetics, Isotherms and thermodynamics were investigated. Absorption mechanics were also analysed with the help of Scanning Electron Microscope (SEM) and Fourier Transform Infra-Red Spectroscopy (FTIR). The experimental results of the maximum removal rate can be made to increase by 78.6% at an initial concentration of 50 mg/L,the pH value of 3.50 and in an adsorbent dose of 1. 00 g/L at 30.0 ?C till the equilibrium state is expected to arrive in approximately 6.00 hours. thermodynamic analysis suggests this reaction is endothermic and satisfies Freundlich Isotherms according to >0.900 correlation coefficient R2. Absorption kinetics agrees with pseudo-second-order kinetic plot, with R2=0.995. After carboxyl and phenolic hydroxyl reacted with Th(IV), IHA had a modified surface. From above, Th(IV) absorption by IHA can be considered as surface complex.
Yang Ya-cheng , Zhao Yong-mei , Luo Wen
2018, 35(4).
Abstract:A novel reaction-based probe (IV), 2-(4-(dimethylamino)phenyl)-4-oxo-4H-chromen-7-yl picolinate was designed and synthesized by utilizing 2-picolinate as the recognition unit. The probe was identified by 1H NMR, 13C NMR, MS and elemental analysis, and it exhibited excellent selectivity for Cu2+ among many common metal ions in HCl-Tris buffer/CH3CN (3:2, V/V) solution, its fluorescence was considerably enhanced by the addition of Cu2+ at room temperature in 5 min, and the color of the solution was changed from red to yellow which can be identified by naked eyes. A linear relationship was observed between the fluorescence intensity and the concentration of Cu2+ in the range of 0 ~ 2.0×10-5 mol·L-1. The detection limit of IV for Cu2+ is 1.67×10-8 mol/L and it can be applied in water quality detection. Mechanism study suggested that Cu2+ promoted the hydrolysis of IV via the catalytic sensing cycle, generating a highly fluorescent N,N-dimethylamine flavonoid (III).
2018, 35(4).
Abstract:VO2 was prepared by carbothermal reduction method with V2O5 and acticarbon as raw materials. Effects of reaction time and acticarbon dosage on content of various vanadium oxide were studied. The purity, phase, morphology and phase-transition temperature of product analyzed by chemical titration, XRD, DSC and SEM. The results show that the purity and conversion rate of VO2 can respectively reach 99.6% and 93.9% when n(V2O?5):n(acticarbon) is 2:1 and the reaction time is 5h. The product is M prase VO2 which has small size and uniform distribution particles, well -crystallized.
2018, 35(4).
Abstract:A modified potassium silicate solution was prepared by the reactant of potassium silicate and silica sol, moderately hydrolyzed silicone-acrylic emulsion which has been catalytic hydrolyzed with tetramethylammonium hydroxide. The water-based inorganic potassium silicate zinc-rich coatings was prepared by organic-inorganic hybridization, which was manufactured by mixing zinc powder into modified potassium silicate solution with a ratio of 1:2.6. In this paper, we investigated the influence of modulus, solid content and the addition of moderately hydrolyzed silica-acrylic emulsion on the properties of waterborne inorganic zinc-rich coatings. The mechanism of silica-acrylic emulsion on water-based inorganic zinc-rich coatings was also discussed. The results indicated that when the modulus of potassium silicate was 3.3, the addition of moderately hydrolyzed silicone-acrylic emulsion was 5% ~ 10%, the film’s hardness, flexibility and adhesion were 5H, 4mm and grade 1, respectively, there is no significant change that the film has been immersed in water and 5% sodium chloride solution over 7 days, the coatings showed the best comprehensive performance.
YE Xu , SHENG Xue-ying , LI Xian , LI Meng-ting , ZHANG Ren-yi , DENG Shuang , YANG Wang-kai , CHANG Guan-jun
2018, 35(4).
Abstract:Polymethyl acrylate (PMA) was synthesized using methyl acrylate (MA) as raw materials, and polyacryloyl hydrazide (PAH) was prepared by means of the aminolysis of PMA with hydrazine hydrate. Hyaluronic acid (HA) was partially oxidized by sodium periodate to obtain oxidized hyaluronic acid (oxi-HA), and a series of oxidized hyaluronic acid/polyacryloyl hydrazide (oxi-HA/PAH) hydrogels were prepared via Schiff base reaction of oxi-HA and PAH. The structures of PMA, PAH, and oxi-HA were characterized utilizing 1H NMR and FTIR, the molecular weight of PMA was determined using multi-angle laser light scattering system (MALLS). The gelling time, microtopography, swelling ratio, degradation behavior, rheological properties and in vitro drug release performance of hydrogels were investigated via the vial inversion method, SEM, weighing method, rhelogy, and Bradford method, respectively. The results showed that the gelling time of the series of oxi-HA/PAH hydrogels ranged from 8 s to 205 s, and the hydrogels with continuous three-dimensional network structure exhibited suitable viscoelasticity and mechanical strength. In phosphate buffer solution (PBS, pH 7.4) at 37 ℃, the swelling ratio of hydrogels ranged from 12 to 22 after 7 hours, the degradation percentage of oxi-HA60/PAH30 hydrogel was about 66% after 20 days, and the cumulative release percentage of bovine serum albumin (BSA) as model protein drug from drug-loaded oxi-HA60/PAH30 hydrogel was about 86% after 10 days.
CUI lei , DONG Jing , Yang Li-Juan
2018, 35(4).
Abstract:Flower-like ZnS microspheres are synthesized by a simple one-step solvothermal method using zinc acetate and thiourea as raw materials, and then oxidized at high-temperature 550℃,600℃ and 650℃, respectively. The crystal structures, morphologies, compositions, specific surface areas and optical properties of the samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), automatic surface area analyzer, Raman spectrometer (Raman) and UV-Vis absorption spectrum. Moreover, photocatalytic activities are evaluated by degradation of RhB solution. The results show that the samples synthesized in situ are ZnS microspheres with cubic phase. After 1 hour high-temperature oxidation of the samples at 550℃, a small amount of ZnO is observed due to the penetration of oxygen atoms and type-II ZnS/ZnO heterostructures are formed after one hour oxidation at a high temperature of 600℃.When oxidation at the highest temperature of 650 ℃ for 1 hour, the samples nearly become the ZnO component. With the increasing of oxidation temperature, the energy gap decreases in overall. Finally, the photocatalytic activity presented that fabricated ZnS/ZnO heterostructures showed best photcatalytic performance.The degradation rate of RhB reached 98.5% after 40 minutes of UV irradiation.
2018, 35(4):0-0.
Abstract:A series of branched waterborne polyurethane associative thickener (BHEUR) were prepared, polyethylene glycol (PEG) and isophorone diisocyanate(IPDI) as raw materials, and homemade branched type nuclear was introduced. The molecular structure of the obtained BHEUR was characterized by means of FTIR and GPC. The thickening property and the rheological property of BHEUR solution were studied by viscometer and rotational rheometer,considering the influences of different structures on the thickening effect of BHEUR. The results showed that when the molecular weight of PEG was 4000, the BHEUR-4 formed presented good self-thickening ability and thickening effect on PU emulsion. The viscosity of PU emulsion can be 50112mPa.s when the mass fraction of BHEUR-4 added was 1.6%. The test of rheological property showed that the four kinds of samples exhibited different degrees of shear-thinning behaviors with the increase of shear rates and such phenomenon of BHEUR-4 could occur under the lower shear rates, proving that it has formed a perfect associative network structure. The effect of BHEUR solution on the particle size of PU emulsion displayed that the synthetic BHEUR had good thixotropy.
XIN Lu-lu , ZHANG Yu , LIU Bao-chuan , ZHANG Bao-hua
2018, 35(4):0-0.
Abstract:Avermectin microspheres were prepared with sodium alginate and chitosan as wall material using dropping method. The effects of the concentration of sodium alginate, chitosan, calcium chloride and the ration of the core-wall on the microsphere morphology, particle size, embedding rate were investigated. The properties of microspheres were characterized by SEM and FTIR, and the release properties and mechanism in soil were studied. The experiment results showed that the optimized preparation conditions are as follows: the concentration of sodium alginate, chitosan and calcium chloride were 3%, 0.6% and 5%, respectively. The ration of core-wall was 1:2. The prepared microspheres had good spherical shape and its average diameter is about 0.7 mm, the drug content and the encapsulation efficiency were 31.65% and 83.81%, respectively. FT-IR analysis displayed there was no chemical interaction between the core and wall material in addition to the hydrogen bonding. The avermectin release characteristics of microspheres was in accord with the Riger-Peppas model, and the release mechanism was Fick diffusion.
2018, 35(4):0-0.
Abstract:The effect of molecular structure and temperature change on the viscosity of anionic gemini surfactant solution was investigated by rheometer. The microstructure of the solution was studied by scanning electron microscopy . On the mechanism of solution viscosity,the results show that the influence of the hydrophilic head type on the viscosity of the gemini surfactant solution show the same pattern (the carboxylate salt>sulfonate>sulfuric acid) .The number of carbon atoms in the interval group is2 and the number of carbon atoms in the hydrophobic chain increased;the viscosity of the carboxylate gemini surfactant solution and sulfonate gemini surfactant solution increased simulataneously . At the same time, the number of carbon atoms in the interval group increased, while the viscosity of the sulfonate gemini surfactant solution increased firstly and then decreased, and the viscosity of the carboxylate gemini surfactant solution decreased, Which DS18-3-18 and DC16-2-16 thickening effect is better. With the temperature increases,the viscosity of DS18-3-18 and DC16-2-16 solution decreased, but the viscosity of DS18-3-18 solution (13.25mPa.s) was still higher than that of DC16-2-16 at 90 ℃. Microstructures show that the number of carbon atoms in the interval group increases (s = 2, 3, 4), and the micelles of DS18-s-18 solution are changed from spherical to flaky to spherical. The number of lamellar micelles or bulk density in the DS18-3-18 solution decreases and there is still a well-connected sheet micelle in the solution and at 90 ℃.So the DS18-3-18 has better temperature and viscosity.
SHENG Zun-lai , ZHAO Jia-hong , YAN Xin , WANG Bi-ying , ZHAO Shan-shan , ZHANG Ying
2018, 35(4).
Abstract:The performance and separation capabilities of six resins (NKA-9、AB-8、D-101、HPD-300、HPD-826 and HPD-400) were evaluated to enrich gallic acid in Chebulae Fructus. NKA-9 resin with strong polarity displayed the best performance in these resins due to its good adsorption and desorption capabilities. Subsequently, the static and dynamic adsorption tests of NKA-9 resin for gallic acid in Chebulae Fructus were systematically tested. The optimal parameters were obtained as followed: Adsorption: concentrations of gallic acid in sample solution 0.152 mg/mL; pH 3.0; sample loading amount 3 BV; flow rate 3 BV/h; temperature 25 ?C. Desorption: Distilled water 5 BV, flow rate 3 BV/h, then 30% ethanol 7 BV, flow rate 2 BV/h. The purity of gallic acid in Chebulae Fructus extract increased from 4.7% to 25.3%, and the recovery was as high as 82.6% under above conditions.
lixiaocui , ruanxuehua , houyong , yanxiaoming , liaoxuhang , liushichao , hegaohong
2018, 35(4).
Abstract:Polymerized ionic liquids(PILs) are novel membrane materials with good CO2/N2 perm-selectivity. However, the industrial application of PILs is restricted by infrequent and expensive polymerizable ionic liquids. In this work, imidazolium-functionalized polysulfones (PSf-g-[MIm][Cl]) were synthesized by simple and controllable chloromethylation-Menshutkin two-step method. The effects of degree of Imidazolium (DIm), test temperature and pressure on the performance of the membrane were investigated. The results show that the membrane has a better pressure stability and the content of MIm is a critical factor on CO2 separation performance. As the content of MIm increases, CO2 permeability and CO2/N2 perm-selectivity improve obviously, attributing to the formation of continuous channel. Moreover, PSf-g-[MIm][Cl] shows excellent film forming ability even with a degree of imidazolium up to 172%, at 25 ℃, 0.4 MPa and humid conditions, the membrane shows good CO2 permeability of 66.4 barrer and CO2/N2 perm-selectivity of 118.4.
ZHU Hong-ling , Fu Jiajia , Xu Bo , Zhao Xiaoman , Wang Qiang , Artur CavacoPaulo , Su Jing
2018, 35(4).
Abstract:Enzymatic polymerization of 4-aminophenol was conducted using laccase enzyme from Trametes hirsute. The polymerization reaction was carried out in acetate buffer solution ( pH 5.0) at 40℃. After 10h, black solid power was obtained. The molecular weight of the product was determined by MALDI-TOF MS. UV-Vis, FT-IR, DSC and TGA were employed to investigate the structure and thermal behavior of produced poly(4-aminophenol). The possible structure of polymer was speculated. The molecular weight of poly(aminophenol)ranges from 300Da to 1500Da, the degree of polymerization are from 3 to 14. Thermal analysis showed that the decomposition temperature of polymer was 223℃,indicating that the polymer have excellent heat resistance.
JIA Pengfei , WANG Juan , CHANG Yongfang , ZHANG Weiliang , DONG Xutong , ZHOU Danyi , YANG Mengxin , ZHANG Xingchen
2018, 35(4).
Abstract:An acidic ionic liquid [N4H4(CH2)].4HSO4 was prepared with the raw materials of hexamethylenetetramine and concentrated sulfuric acid, and it was applied to the synthesis of ethyl chloroacetate. The technological parameters involved in esterification reation were optimized. Structures of the title compound and the catalyst were confirmed by 1HNMR. The results showed that n(chloroacetic acid):n(ethanol)=1:1.8, the amount of ionic liquid was 30% of the total mass of chloroacetic acid, the reaction temperature was 100℃, the reaction time was 3.5h and the yield of ethyl chloroacetate was 93.27%.When the acidic ionic liquid was repeated 6 times, the yield of ethyl chloroacetate was 90.16%. The product was easy to separate and the acidic ionic liquid overcomed the defects of inorganic acid catalyst.
ZHOU Chen-liang , WANG Ya-xiong
2018, 35(4).
Abstract:Effects of K and Zr promoter on precipitated iron-based catalyst for CO hydrogenation were investigated. The bulk structure, surface morphology, bonded state of surface elements, and chemical properties of the catalysts were characterized by means of X-ray diffraction(XRD), scanning electron microscopy(SEM), Raman spectroscopy, H2/CO-temperature-programmed reduction and catalytic activity tests for the selective formation of light olefins. Results showed that K was benefit to format 100~150nm solid particles of α-Fe2O3, and Zr contributed to the dispersion of α-Fe2O3 to the particles with 10~50 nm diameter, while the cooperation of K and Zr could helpful to generate spherical particles with diameter of 20~30 nm. K and Zr could improve the low H2 reduction temperature of 85℃ and 14℃ respectively, meanwhile improve the low CO reduction/carbonization temperature of 68℃ and 12℃. K in reaction process could generate active Fe5C2 phase, improve the CO conversion rate from 42.3% to 67.0%, lower the content of CH4 by 10.37% and increased the O/P by 2.24, but Zr exhibited no such function. The catalyst promoted by K and Zr show a remarkable synergic effect which leaded to the reduction of Fe3O4 crystal from 26.4nm of fresh catalyst to 21.2nm after it was used, tending to amorphous type. Meanwhile, the synergic effect of K and Zr increased CO conversion to above 90%, C2=~C4= distribution to 30.51mol%, O/P to 3.59 and the yield of C2=~C4= got about 28.65%.
Li Meng-tian , Jiang Ping-ping
2018, 35(4).
Abstract:Abstract: The hydrothermal method was applied to prepare carbon based solid acid catalyst which was named by glucose-sodium bisulfate monohydrate-X(Glu-SBM-X). The mass ratio of glucose and sodium bisulfate monohydrate was varied to obtain catalysts with different acid concentrations. The catalysts were identified by X-ray diffraction (XRD), fourier transform infrared (FT-IR), scanning electron microscopy(SEM), thermogravimetic analysis (TGA), which proved that the carbonaceous material possesses -SO3H groups. And the neat spherical structure was obtained. The catalytic performances of carbon based solid acid catalysts were carried out in the esterification of oleic acid with methanol. Meanwhile, the effects of the mass ratio of glucose and sodium bisulfate monohydrate, reaction temperatures, reaction time, the molar ratio of methanol and oleic acid on the conversion rate of the oleic acid were performed. The results showed that when the mass ratio of glucose and sodium bisulfate monohydrate was 1:4 and the the molar ratio of methanol and oleic acid was 10:1, the conversion rate of the oleic acid reached 95.20% after conducting the esterification reaction at 70 ℃ for 5 h . The catalyst showed excellent reusability because the conversion rate of the oleic acid remained above 92.6% after reusing for four cycles.
2018, 35(4):0-0.
Abstract:La modified Cu-Fe/SiO2was prepared by ultrasound assisted impregnation. The effect of rare earth La additional on the catalytic performance of Cu-Fe/SiO2 was investigated. The catalysts were systematically characterized by techniques of X-ray diffraction (XRD), N2 adsorption isotherm, temperature-programmed desorption of CO (CO-TPD), and temperature-programmed reduction of H2 (H2-TPR), meanwhile the catalytic performance for CO hydrogenation to higher alcohols was also evaluated. The experimental results showed that with the modification of La, promoted the dispersion of active sites, the specific surface area was increased notably, enhanced adsorption capacity of CO and decreased reducibility of active sites. Therefore, the modified catalyst obviously improved the higher selectivity to C2 alcohols, and the content of methanol in reaction product was reduced significantly.
SONG Dao-jun , Xu Yong-jun , Tu Wei-ping , Liao Jun-xu
2018, 35(4):0-0.
Abstract:In the process of production of levulinic acid by acid catalytic hydrolysis of cane molasses,taking the yield of levulinic acid as the main indicator, single factor and combined effects of reaction time, the concentration of molasses, molasses-catalyst mass ratio , temperature were evaluated based on single-factor experiments. Box-Benhnken center combination experimental principle and response surface methodology(RSM) were adopted to optimize the preparation conditions of levulinic acid. A quadratic polynomial regression model was established to predict the LA yield. The results showed that the regression of this model was significant while the lack of fit was not significant, which indicated the model fitted well with experimental data. Each factor alone could significantly influence the yield of LA, and the order was molasses-catalyst mass ratio > temperature >effects of reaction time>the concentration of molasses. The highest LA yield was obtained under the optimal condition of 40 wt % molasses, 23.40:1 molasses - H2SO4 mass ratio at 151℃ for 5 h. The average yield of LA reached 30.11 wt% under the optimum conditions for three times. Compared with the predicted value of 30.96 wt%, the relative deviation was only 0.85 wt% , which proved the model was reasonable and feasible.
LIU Jian-bing , Xu Wang-jin , Chen Kai-yi , Du Yan-lin , Cao Lei , Zhang Xue-peng
2018, 35(4).
Abstract:Using the basic skeleton of commercialized benzoyl urea as leading compound, thirteen compounds were designed and synthesized by introducing 5-aminothiazole moiety into benzoylurea. The literature synthetic method of 2,4-disubstituted-5-aminothiazole derivatives based on the Ugi four-component reaction by Thompson has been optimized, their structures of all these compounds have been comfirmed by 1H NMR, 13C NMR, IR and MS. Their results of bioassay showed that most of the title compounds exhibited excellent insecticidal activities. Among them, compounds 5f, 5g, 5h, 5j and 5m showed 100% insecticidal activity against mosquito larvae at a concentration of 10 ppm, furthermore, when the concentration decreased to 5 ppm and 2 ppm, compound 5j still showed 100% activity which was higher than that of positive control; Compounds 5d and 5j showed 100% insecticidal activity against cotton bollworm and corn borer at a concentration of 600 ppm.
2018, 35(4).
Abstract:The precursor was synthesized by microwave method with six cobalt nitrate (Co(NO3)2?(6H2O) and benzoyl acetone (C10H10O2) as raw materials. The precursor is calcined at 500 ℃ in air are obtained under the conditions of amorphous Co3O4 flower.The microstructure and surface morphology of the amorphous Co3O4 flower were studied by XRD、SEM and TEM.The electrochemical test results show that the initial charge specific capacity of the amorphous Co3O4 flower anode material is 816mAh / g at a current density of 100mA / g. After 100 cycles of circulation, the capacity retention rate is 89.2%, with high specific capacity and good cycle performance and a wide range of application prospects.
2018, 35(4).
Abstract:We utilized the silane coupling agent to transform and decorate the chemical property of the Nano-SiO2 on its surface. By this means, we can acquire BC-27, an organic boron Nano-crosslinker. At the same time, we test the structural features and properties of BC-27 and its fracturing fluid by adopting FTIR、SEM、High temperature rheometer、High temperature and high pressure filtration apparatus. Meanwhile, we prospected the content of the modified Nano-SiO2, the weight percent of HPG, cross-linking rate and the pH value influence on the cross-linking property of BC-27. We also assessed these properties of the hydroxypropyl guar fracturing fluids formed by BC-27, such as the ability of heat resistance and shear resistance, filter loss, breaking viscosity, the flowing back and the detriment of core. The study shows :When w(The modified Nano-SiO2) = 0.18%,the property of the Nano-crosslinker BC-27 is the best. When w(HPG) = 0.35% , the cross-linking rate is 100:0.3 and the pH rate is about 11, the properties of the fracturing fluid is the best :the highest anti-temperature value is 130℃,and the cross-linking time is adjustable between 89s to 225s. What’s more, the viscosity of the fracturing fluid with organic boron Nano-crosslinker BC-27 is at least 440mPa·s ,which shear a duration of 120min at 130℃. While the viscosity of fracturing fluid with the common organic boron crosslinker OS-150, just keeps the value about 280mPa·s. Besides, the ratio of core injury is 23.08% by the fracturing fluid with OS-150, and the ratio of core detriment can slump to 19.47% by the fracturing fluid with BC-27. The characteristics of Nano-crosslinker was wonderful, its own favorable delay performance, and could efficiently reduce the doses of hydroxypropyl guar.
MA Guo-yan , SHEN Yi-ding , Li Xiao-rui , LIU Jin , WANG Xiao-rong , GUO Xing
2018, 35(4).
Abstract:Steady rheological behavior of HAP aqueous solution was investigated by using dynamic rheometer. Effect of surfactant on HAP aqueous solution was also investigated. The results showed the apparent viscosity of HAP aqueous solution decreased and then kept constant with the increment of shear rate. A hydrophobic associating polymer fracturing fluid (HAP-M) were prepared by HAP and sodium dodecyl sulfate (SDS). Heat and shear resistance, viscoelasticity, thixotropy, proppant-carrying capacity and gel breaking property of HAP-M fracturing fluid were evaluated. HAP-M fracturing fluid has a good heat and shear resistance. Its viscosity can remain above 50 mPa•s after shearing at the rate of 170 s-1 for 90 min at the temperature of 90℃. According to the viscoelasticity results of HAP-M fracturing fluid, both of the storage modulus (G') and loss modulus (G″) do not change with the stress changing, and G' is larger than G″, which indicates that HAP-M fracturing fluid is of viscoelasticity and mainly elastic behavior. Furthermore, the thixotropy of HAP-M fracturing fluid is better than that of hydroxypropyl guar gum (HPG) fracturing fluid. The sedimentation rate is 1.18 mm/s on the condition of 40% sand ratio,which indicates that the fracturing fluid has a good proppant-carrying capacity. The gel breaker of ammonium persulfate can make the fracturing fluid gel break in 1 h at 80℃.The viscosity of gel breaking liquid is less than 5 mPa•s and the surface tension and interfacial tension of that are 25.14 mN/m and 0.56 mN/m, respectively.
2018, 35(4).
Abstract:A collagen based adhesive was prepared by using polyurethane prepolymer as the cross-linking agent, and collagen hydrolyzate derived from tanned leather wastes as the raw material. Five different wood adhesive formulations were obtained through controlling the molar rate of the amino group and the isocyanate group. The properties and structure were measured by solid content, water resistance and modern instrument characterization. The relative molecular mass of modified adhesives was obviously increased, the crystallinity was obviously reduced and the thermal stability is improved significantly after modification. The results indicated that the water resistance was the best when the molar rate was 1:1 and the wet shear strength could reach to 1.08MPa(≥0.7MPa), which met the requirement of GB/T9846.3-2004. The solid content (38.16%) and the stability of Formulation 2 adhesive were also the optimal.
2018, 35(4).
Abstract:In order to cure hydroxyl-terminated polybutadiene (HTPB) at room temperature, tetramethyl-terephthalobisnitrile oxide (TTNO) was synthesized from 1,2,4,5-tetramethylbenzene with four steps by bromomethylation, oxidation, condensation and dehydrogenation reactions with a total yield of 50%. Their structures were characterized by FT-IR 1H NMR and 13C NMR. Define R value equals molar ratio of –CNO and C=C. We chose 0.03, 0.04, 0.05, 0.06 and 0.07 as R value to prepare the dumbbell-shaped cross-linked polymers. The FT-IR, tensile strength, DSC, TG and contact angle of the cross-linked polymers were tested and analyzed. With the increasing of R value, tensile strength of cross-linked polymer increase from 0.201MPa to 0.512 MPa, Tg from -73.08℃ to -66.70℃ and the contact angle decrease from 98.80° to 73.54°. The results shows that tetramethyl-terephthalobisnitrile oxide can curing HTPB at 25℃, the cross-linked polymers are expected to be used in the composite solid propellant.
ZHENG Yan-qing , WU Jin-tian , LIN Qi
2018, 35(4).
Abstract:The water-based ultra-thin intumescent fire-retardant coating special emulsion was prepared by using thermosetting epoxy resin modified thermoplastic acrylic emulsion as film forming matter. By using FT-IR, DSC, TGA, SEM, the emulsion properties and the effect of emulsion on fireproof coatings were studied. The results show that:the decomposition temperature and glass transition temperature of emulsion membrane were enhanced by epoxy modified,so that it can be match with expansion system. Using epoxy resin modified acrylic ester emulsion as film forming material ,the coating can form a dense, uniform honeycomb bubble hole after thermal expansion, and it achieve good fireproof performance .
GAO Li-ya , HAN Shuang-fu , MA Rui-hui , CHEN Yun-ting , ZHANG Fu-qiang
2018, 35(4).
Abstract:Raw kaolinite was first intercalated with dimethyl sulfoxide (DMSO) under ultrasonic field, and then composited to modify coal tar pitch through melt process. The interlayer spacing, interlayer interaction, dispersion morphology and thermal stability of modified coal tar pitch were characterized by X-ray diffraction, FTIR spectrum, electron microscope and thermal analysis. The results show that the hydrogen bonds between aluminum hydroxyl and silicon oxygen bond are weakened because of DMSO intercalation, the interlayer space of kaolinite expands from 0.716 nm to 1.124 nm and the intercalation rate reaches 98.57%. After melt composition, the (001) diffraction peak disappears which means the kaolinite is delaminated by coal tar pitch molecules and the kaolinite layers are dispersed in the form of thin layers in coal tar pitch. At the maximum weight-loss-rate temperature of 650 ℃for intercalated kaolinite modified coal tar pitch, the weight loss is 78.04%, while raw coal tar pitch (RCTP) is high as 85.41%. For RCTP, the accumulative weight loss value of 50% appears at 490 ℃, whereas modified pitch rises to 550 ℃. Compared to RCTP, the softening point of modified pitch with 6 wt% intercalated kaolinite improves from 42.3 ℃ to 45.4 ℃, but the increasing extent of softening point decreases with more kaolinite dosage. Therefore, these dispersed layers improve the thermal stability of coal tar pitch obviously, which may be caused by ways of delaying air transmission.
2018, 35(4).
Abstract:The solid acid catalyst (HClO4/SBA-15) was prepared by using a molecular sieve SBA-15 supported perchloric acid, and characterized by infrared spectroscopy. A method for the synthesis of ornidazole with solid acid HClO4/SBA-15 as catalyst, 2-methyl-5-nitroimidazole and epichlorohydrin was developed. The influences of different catalytic dosage, reaction time, reaction temperature and different solvents on the conversion were investigated. The optimum conditions showed that when the amount of 2-methyl-5-nitroimidazole: HClO4 / SBA-15 was equal to 5:3, and the reaction was carried out at 0°C for 8h with the reaction of isopropanol as the solvent, the conversion of 2-methyl-5-nitroimidazole could reach to 76.3%, Purity of 99.8%. The product was identified by nuclear magnetic resonance spectroscopy and mass spectrometer. The results showed that the quality of ornidazole was consistent with the quality standard of pharmacopoeia. The catalyst can be reused and the conversion rate is still 65.8% for the third use.