Abstract:A series of PF2DI surfactants were synthesized by the hydrosilylation with poly (methylhydro- siloxane) (PMHS),N-methyl-N-allyl-2-perfluoro-2ʹ-methyl-3ʹ-oxocaproamide (NF2) and N,N-dimethallylamine (DAEMA) and CH3I in the presence of the Karstedt catalyst and then by quaterisation with CH3I. The structures of the products were characterized by IR and 19FNMR. The effects of temperature, the catalyst dosage and the molar ratio of the reagents on the hydrosilylation were studied. The relative molecular mass, cationic-active matter content, solubility, surface tension and wettability were measured. The optimal process conditions of hydrosilylation were n (Si—H):n (NF2):n (DAEMA) =10:1:9, 2.5 g PMHS, 120 μL Karstedt catalyst (16.123 g Pt/L), 80℃ reacted for 6 h to give PF2DI in the yield of 58%. When n (Si—H):n (NF2):n (DAEMA) changed from 10:0.5:9.5 to 10:2:8, weight-average molar mass MW and number-average molar mass Mn , the content of cationic-active matter, the solubility in water and ethanol and the critical micelle concentration(CMC) decreased gradually; surface tension (γCMC) and the contact angle on the PMMA and paraffin surfaces first decreased and then increased. When n (Si—H):n (NF2):n (DAEMA) was 10:1:9, γCMC and the contact angles reached the minimum value and the wettabilities were the best.

Abstract:Li4Ti5O12/Li1.3Al0.3Ti1.7(PO4)3 composite was synthesized by sol-gel method. The structure, morphology and electrochemical performance of the composite were studied by X-ray diffractometry, scanning electron microscopy, galvanostatic charge-discharge test, cyclic voltammeter and electrochemical impedance spectroscopy techniques. Li4Ti5O12/Li1.3Al0.3Ti1.7(PO4)3 composite can be prepared by sol-gel technique and the particles of the composite are uniform. Compare with pure Li4Ti5O12, the Li4Ti5O12/Li1.3Al0.3Ti1.7(PO4)3 composite has lower Li insertion/extraction impedance. The specific capacity of the Li4Ti5O12/Li1.3Al0.3Ti1.7(PO4)3 composite doped with 1 wt%, 2 wt%, 3 wt%, 4 wt% and 5% wt% Li1.3Al0.3Ti1.7(PO4)3 is 6.2%, 11.8%, 15.5%, 8.0% and 2.0% higher than the pure Li4Ti5O12，respectively. The composite doped with 3 wt% Li1.3Al0.3Ti1.7(PO4)3 shows the best cycling performance of 0.022% capacity loss per cycle.

Abstract:Two Hg2+ probes (Tpy1 and Tpy2) with D-π-A structures were designed and synthesized by introducing 9-hexyl-9H-carbazole and triphenylamine units to 4'-(4-phenyl)-2,2',6',2''-terpyridine component respectively via Suzuki coupling reactions. Their structures were characterized by melting point, 1H NMR, 13C NMR, mass spectrometry and elemental analyses. Compared to other metal cations, the target probes Tpy1 and Tpy2 have good selectivity for Hg2+. The Hg2+ can be identified efficiently in solution by UV-vis absorption spectrophotometry or naked eye observation under ultraviolet lamp. DFT calculations indicate that when the probe is chelated with Hg2+, the intramolecular charge transfer (ICT) effect is significantly enhanced, and the absorption spectra are red shifted accordingly. In addition, different electron donating groups attached to the probe molecules can influence the recognition of Hg2+ significantly. The detection limits are 2.51×10-6 mol/L for Tpy1 and 4.40×10-6 mol/L for Tpy2 respectively. When the triphenylamine group was attached on the probe structure in Tpy2, the probe can not only detect Hg2+, but also exhibit response to Cu2+ cations.

Abstract:The phase change microcapsule were prepared by the method of seeded micro-suspension polymerization, which was combined to the advantage of seeded emulsion polymerization and micro suspension polymerization, with styrene (St) and divinylbenzene (DVB) crosslinked polystyrene (PS) as the outer membrane and butyl stearate as core, AIBN, HPC and CaCO3 were used as initiator and compound dispersing agent, respectively. The morphological, thermal behavior and properties of microcapsules were characterized by scanning electron microscopy (SEM), differential scanning calorimeter (DSC), particle size analyzer and thermogravimetric analyzer (TG). The influence of polymerization method, crosslinking agent and dispersing agent on the morphology and properties of the microcapsules were investigated. The results indicated that the microcapsules which was prepared by seeded micro-suspension polymerization have uniformly distributed granular diameters were regularly spherical, and the latent heat and the coating rate increased by 29.4% and 15.1%, respectively. The crosslinking density of wall material, the tightness and the thermal stability were enhanced with the increasing of DVB content. When the weight ratio of HPC and CaCO3) was 2.2:1, the latent heat increased by 21.1%.

Abstract:Highly pure Ti2SC powder was synthesized by microwave hybrid heating a Ti/TiS2/C powder system in the temperature range of 200-1100 ℃. The effect of sintering temperature on the synthesis of Ti2SC was studied. For comparison, pressureless sintering (PLS) was used to synthesize Ti2SC powder from 1000 ℃ to 1400 ℃ for 15 min. By XRD, SEM, DSC and thermodynamics, the phase assembly, microstructure and reaction mechanism of samples were analyzed. The results indicate that the main phase graphite with small amount of Ti2SC was synthesized at 1400 ℃ by pressureless sintering. However, by microwave hybrid heating，at 400 ℃, Ti2SC phase was detected as a major phase and large amount of graphite existed. The peak of Ti2SC phase became strong together with weakening the peak of graphite at 800 ℃. At 1100 ℃, single-phase Ti2SC powder with the average size of 2-5 μm was achieved. In TiS2-Ti-C system, TiS2 reacted with Ti to form Ti-S compounds below 400 ℃, and Ti-S compounds reacted with Ti and graphite to produce Ti2SC at 400 ℃ and above.

Abstract:90% exposing single crystal TiO2 (001), (101) and (010) were synthesized by hydrothermal method, and noble metal Ag was loaded on TiO2 single facets through photodeposition. The crystal-facet effect for Ag-loading was studied. It was found that at the same synthesis condition, the size of Ag particles loaded on different single facet was different which was Ag/TiO2-101

Abstract:Phenyl vinyl silicone oil and phenyl hydrogen silicone oil of which the refractive index match with fumed silica are prepared, and then add fumed silica as reinforcing fillers to prepare optical transparent phenyl silicone rubber. By using tetramethyl hexamethylene diamine as a catalyst, organic polysilazane (OPSZ) coated on a silicone rubber surface achieves low-temperature curing and siliceous transition, and a dense coating having low gas permeability is obtained. Optical performance, oxygen permeation flux, and anti-sulfuration are then tested, the results show that the OPSZ coating surface is continuous, uniform, dense and free of cracks and voids, while the coating section is dense, uniform, seamless, without cracks, and have good adhesion to the silicone rubber when the coating thickness was < 32-35μm. The coatings have excellent transparency, light transmission and gas shielding properties. With a coating thickness of over 12μm, the oxygen permeation flux remains unchanged, lamps after coating have good anti-sulfuration ability, and the luminous flux maintains over 99.9%. The siliceous conversion time can be effectively shortened by increasing the heating temperature and relative humidity.

Abstract:N,N'-dimethacryloylcystine dimethyl ester was used as cross-linker, and a series of redox-responsive PMAA (Polymethacrylic acid) nano-hydrogels were prepared by distillation-precipitation polymerization method. The composition, size distribution and morphology of the nano-hydrogels were characterized by fourier transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS) and scanning electron microscope (SEM) respectively. The influences of the amount of cross linker, monomer and initiator, and the reaction time on the size and yield of the nano-hydrogels were investigated. The results demonstrated that various sizes of nano-hydrogels could be obtained by adjusting experimental conditions. Especially, the size of nano-hydrogels was significantly affected by the factors of amount of crosslinker and reaction time. Furthermore, optimum technological conditions were obtained by orthogonal experiment, in which the mole ratio of initiator, monomer and cross-linker was 1.1: 96: 2.9; the reaction time was 15 min. In addition, the PMAA nano-hydrogel showed good redox-responsive property. Under 10 mmol/L DTT condition, the PMAA nano-hydrogel could be degraded within 20 min.

Abstract:The single epoxy-terminated polydimethylsiloxane (SEPDMS) was prepared with hydrogen-terminated polydimethylsiloxane (HTPDMS) and allyl glycidyl ether (AGE) by hydrosilylation reaction. Subsequently the epoxy functional polysiloxane was grafted to the generation 1 dendritic polyamide-amine (G1 PAMAM). FT-IR, 1H-NMR and nano particle size analyzer were utilized to characterize the structure of the product and the particle size of the emulsion. Finally, the dendritic-linear polymer (G1 PAMAM-Si) was applied to the fatliquoring progress. The structure and performance of fatliquored leather were investigated by SEM and other analysis methods. It was shown that the fatliquored leather with G1 PAMAM-Si exhibits the increasement of collagen fiber distance and improvement of softness and mechanical properties.

Abstract:Chitosan quaternary ammonium salt(HACC) was synthesized by reaction of chitosan(CTS) with 2,3-trimethyl ammonium chloride(GTA) via inverse emulsion polymerization. The structure of HACC was characterized by Fourier transform infrared spectrum(FTIR), nuclear magnetic resonance hydrogen spectrum((1HNMR), environmental scanning electron microscope(ESEM) and X-ray diffraction(XRD). In addition, the effect of HLB, volume ratio of oil to water, the amount of initiator, reaction time, temperature and m(GTA):m(CTS) on degree of substitution(DS) and yield(P) were investigated. The results indicated that the optimal processing for the preparation of HACC were as follows: HLB=6.0, volume ratio of oil to water is 1:1, amount of initiator is 1.5%, reaction time is 5h, temperature is 60℃, m(GTA):m(CTS)=3.0. The products has highest DS and P, DS=1.331, P=81.16%. Moreover, flocculation experiment employed kaolin suspension as synthetic wastewater and the cationic polyacrylamide(CPAM), CTS and HACC as flocculant, the effects of flocculant dosage and pH of wastewater on result were investigated, respectively. It was indicated that CPAM, CTS and HACC has good flocculation effect on kaolin suspension. The appropriate flocculation of HACC were as follows: the optimum flocculation pH=6, best dosage of flocculant dosage is 1 mg/L. And under the same conditions, HACC possessed better flocculating performances than CTS and CPAM.

Abstract:In anhydrous ethanol system, with methyltriethoxysilane (MTES) as raw material and sodium hydroxide as catalyst, through the reactions of hydrolysis and condensation, the hydrophobic polymethylsesquisiloxane nano-powders(PMQS) were synthetized.The chemical structure and surface morphology of PMQS were characterized by means of FTIR and SEM.The non-ionic surfactant was used to emulsify PMQS and ASO in order to obtain a translucent of PMQS /ASO microemulsion.Then the particle size of the emulsion micelles was measured by nano-particle surface potential analyzer.The application performance of ASO and PMQS/ASO emulsion was investigated.And the membrane surface morphology of cotton were studied through SEM.The results show that the property such as softness,slide and water proofing of cotton was much better when the quality ratio of PMQS:ASO was 3:7,.and with the particle size of the emulsion is about 150nm.While, the contact angle of cotton fabric is about 135 o.

Abstract:A series of waterborne polyurethane containing maleimide group emulsion were successfully synthesized by the reaction of poly-caprolactone diol(PCL1000), isophorone diamine(IPDI), 1,4-butanediol(BDO), dimethylol propionic acid(DMPA), trimethylol propane(TMP) and N-(4-hydroxyphenyl) maleimide (4-HPM) as main raw materials. The surface sizing properties of the polyurethane emulsion were studied, and the synthetic conditions were optimized. The results show that the emulsion owns excellent sizing property when R is 1.4, w(COOH) is 1.4%, w(4-HPM) is 1.0%, and with 2% polymer emulsion addition. The papers' sizing value can reach 64s, tensile strength approaches 57 N?m /g and folding endurance 82 times.

Abstract:The cationic polymer flotation agent PADS was synthesized by inverse emulsion polymerization with acrylamide, two methyl chloride and acrylic acid as functional material. The chemical structure of the polymer was identified by IR spectrum. In the preferred scheme, the optimal conditions were: m(AM):m(DMDAAC)=5:5, initiator dosage V-50 being 0.6%,polymerization temperature being 45 ℃，and reaction time being 4 hours. The optimization experiment of flotation agent’s dosage was conducted with luminousness as a target at 45℃.The experimental results showed that luminousness of sewage reached 92.7% when the dosage of flotation agent is 40 mg/L, which had a good flotation performance .

Abstract:A micro-size eggshell Ni-based catalyst supported in fluid catalytic cracking catalyst residue (SFC3R) was synthesized by impregnation. The structure, morphology and reducibility of the catalyst were characterized by FIB-EDX、XRD、H2-TPR and TEM. The eggshell Ni/SFC3R catalyst was used for C5 petroleum resin hydrogenation，and the effects of temperature，pressure and reaction time were investigated. The properties and structure of hydrogenated C5 petroleum resin were analyzed by the method of Gardner color number， softening point， GPC， FT-IR and 1H-NMR. Results show that SFC3R contains zeolite structure and the Ni active component is mainly distributed in the outer layer of the SFC3R to form the eggshell distribution. The crystallite size of NiO of eggshell Ni/SFC3R catalyst is 21.5 nm, which exhibit good dispersion. The optimum conditions of C5 petroleum resin hydrogenation were found as temperature 280 ℃，H2 pressure 8.0 MPa and reaction time 4 h. The Gardner color of hydrogenated C5 petroleum resin is below 1# and the color is water white. The sulfur content and bromine number of hydrogenated C5 petroleum resin is <10mg/kg and 0.45 gBr/100g， respectively. And the unsaturated bond of C5 petroleum resin reaches saturation basically.

Abstract:Abstract: In order to improve the water resistance and other properties of the waterborne polyurethane, polyurethane prepolymer(PPU) was synthesized in which isophorone diisocyanate (IPDI), polytetramethylene ether glycol (PTMG), 2,2-bis(hydroxymethyl) butyric acid (DMPA) and 1,4-butanediol(BDO) were as raw materials, dibutyltin dilaurate (DBTDL) was used as catalyst. And then the hydroxyl terminated dendrimer (PAMAM-OH) was as core to synthesize dendritic waterborne polyurethane（HWPU）by graft copolymerization. The optimum synthesis conditions of PPU were optimized through single-factor experiment. The reaction time was 2h, the reaction temperature was 80℃ and n (—NCO): n (—OH) was 6:1. The performance of HWPU was characterized by Fourier transform infrared spectra (FTIR), X-ray diffraction (XRD) and nano particle surface potential analyzer ,as well as the water resistance, the surface roughness and the mechanical properties of films were tested. The results show that the reaction is carried out as the expected route, the particle size is 43.56 nm, the crystallinity of the film is 1.59%, the water absorption of the film is 4.8% after 24 h, the tensile strength is 39.2 MPa and the elongation at break is 376.4% as well as the surface roughness of the film is reduced. Compared with the waterborne polyurethane in which there is no PAMAM-OH, the water absorption of HWPU decreases by 67.15. Its water resistance and tensile strength both are improved.

Abstract:An important organic intermediate 2-bromophenol can be prepared by the tert butyl transfer reaction of toluene with 2-bromo-4-tert-butyl phenol. The effect of catalyst and the reaction condition on the tert butyl transfer reaction of 2-bromo-4-tert-butyl phenol were investigated. The results show that aluminum tri-chloride and its complex salt with tertiary amine and hydrogen chloride are active in the reaction. The analysis of 27Al NMR shows that the real catalytic species may be chloroaluminate, which formed by the reaction of aluminum trichloride with hydrogen chloride from the hydrolysis of aluminum trichloride. Further, the hydrogen chloride and hydrogen bromide are proved to be the aluminum trichloride activator, and the dosage of aluminum trichloride can be reduced. The optimized process condition is as followed : 4-tert butyl phenol reacted with bromine at 0℃in dichloromethane selectively forming 2-bromo-4-tert butyl phenol, then,2-bromophenol can be prepared through “one pot reaction” by adding aluminum tri-chloride and toluene in molar percentage of 30 and 600 at 30℃. The conversion and selectivity of 2-bromo-4-tert butyl phenol are of 96.5% and 99.6%, respectively.

Abstract:Ga2O3/palygorskite composite catalyst was prepared by an impregnation method with palygorskite loading gallium oxide(Ga2O3), the structure of catalyst was characterized by means of IR, XRD, BET and TEM. The preparation conditions and catalytic activity of catalyst were investigated. The results indicated that the suitable preparation conditions of catalyst were Ga2O3 loading at 10 %, and calcination temperature 450 ℃. The average esterification rate was 95.0 % under the following conditions for synthesis of cyclohexyl cinanmate: n(cinnamic aicd):n(cyclohexanol)=1:4.5(cinnamic aicd was 0.02 mol), catalyst amount was 0.5 g, heat at 130 ℃ for 70 min. It could reach to 81.5 % while used for 5 times. It's a second-order reaction, the apparent activation energy was 90.78 kJ/mol, and the reaction rate constant was 1.03×10-2 L/(mol•min) in 130 ℃.

Abstract:In order to simplify the process, nitroguanidine(NQ) was synthesized from crystallization mother liquor with the nitrate method by controlling crystallization, the average grain size, acidity and purity of the product met the military requirements according to experimental results. The optimum process conditions were obtained as follows: the stirring rate: 350r/min; the dropping speed of dilution solution: 2mL/min; the crystallization temperature: 271K; the time for crystal growing:90 minutes. The results show that NQ with average grain size between 3μm to 6μm, acidity below 0.05% and purity exceed 99.2% could be produced in the optimum conditions. The crystal morphology of controlling crystallize product was compared with the crude NQ after recrystal, according to SEM images, the process of NQ product preparation using nitrate method by controlling crystallization is effective.

Abstract:Hexahydropyrrolo[3,4-b]-7-azaindole derivatives were synthesized from 3-nitroazaindoles and 1,3-dipole which was generated in situ through [3+2] dipolar cycloaddition. The synthetic conditions of hexahydropyrrolo[3,4-b]-7-azaindole derivatives were optimized, using methylene chloride as solvent, and with the reaction taking place at room temperature for 1 h. The yield under such conditions was 85%～95% and the diastereoselectivity was over 99:1. The structures of these compounds were characterized by 1H-NMR, 13C-NMR and high resolution mass spectrometry analysis. The results showed that target structures products were obtained. Furthermore, X-ray diffraction was used to analysis the structures of compound (S,S)-6-benzyl-4b-nitro-8-tosyl-4b,5,6,7,7a,8-hexahydropyrrolo[3',4':4,5]pyrrolo[2,3-b]pyridine (Ⅲa). The result showed that the relative configuration of chiral center was (S,S) or (R,R).

Abstract:Herein, we reported an efficient method to manufacture 2'-Deoxycytidine. This process, which is using α-D-2-Deoxyribose and Uracil as economical starting material, went through 6 linear steps, including methyl-glycosidation, protection, chlorination, nucleophilic substitution, amination and deprotection reactions. The final product is obtained as 44% overall yield and 99% purity after recrystallization. This process has several advantages, such as mild reaction conditions, relative safe operation and straightforward purification for final product and intermediates. Up to now, kg-scale manufacture of 2-Deoxycytidine is completed in the chemical factory.