Abstract:Using 2,2-bis(4-hydroxyphenyl)hexafluoropropane as raw materials, 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane was synthesized by nitrification reaction and reduction reaction. The factory pilot-scale study was carried out to determine the technological date after the laboratory experiment succeed. The results indicated that as for the nitrification reaction, n (ethanol)÷n (2,2-bis(4-hydroxyphenyl)hexafluoropropane) = 4, n (the dilute nitric acid)÷n (2,2-bis(4-hydroxyphenyl)hexafluoropropane) = 2.15, 60 ℃ and the reaction time (6 h), which can get the highest 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane yield (96%). As for the reduction reaction, using FeCl3/ activated carbon as catalyst and ethanol was the solvent, n (hydrazine hydrate)÷n (2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane) = 0.2, m (FeCl3/ activated carbon)÷m (2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane) = 0.05, 85 ℃ and the reaction time (10 h), which can reach the highest 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane yield (92%). The above process conditions have been studied in the factory and determined the technological date and the technological conditions.

Abstract:Because of low cost and high yield of fermentable sugars, acid-based pretreatment methods have been proven to be efficient in conversion of lignocelluloses to fuel ethanol by microbial fermentation. However, some of the byproducts including furfural and 5-hydroxymethyl furfural（5-HMF) in the acidic prehydrolysates were the inhibitors in the fermentation process. Meanwhile, large amounts of enzymatic hydrolysis lignin (EHL) residue were produced as another byproduct. To explore the application of this lignin residue for detoxification of acidic prehydrolysates, EHL was applied to decrease the concentration of furfural and 5-HMF through adsorption. The effects of contact time, lignin dose, pH on the adsorption of furfural and 5-HMF on EHL and adsorption isotherms were investigated. EHL was used to remove furfural and 5-HMF in two acidic prehydrolysates of corn stover. The results showed that the adsorption was a spontaneous exothermic process, and good fit was obtained by Freundlich model. Furfural was easier to be removed than 5-HMF through adsorption by EHL. The results indicated EHL could be the adsorbent to remove furfural and 5-HMF in acidic prehydrolysates.

Abstract:Starting from dehydroabietic acid, chiral ethyl 7-(S)-amino-dehydroabietate 6a and ethyl 7-(R)-amino-dehydroabietate 6b were synthesized by esterification, oxidation, imidization, reduction and acidification. The absolute configurations of 6a and 6b were confirmed by X-ray analysis, and the structures were characterized by 1H NMR, 13C NMR, MS and HRMS.

Abstract:Abstract:The β-cyclodextrin inclusion compound of 2-Mercaptopropionic acid was prepared by saturated water solution method,the content of 2-Mercaptopropionic acid of inclusion compound were tested by ultraviolet spectrophotometry and the synthesis process was optimized by orthogonal experimental design ,the results show that the most optimized conditions were as following:β-cyclodextrin:2- Mercaptopropionic acid =12:1 (Mass ratio); the inclusion temperature was 45 ℃; the inclusion time was 4h; the inclusion rate can reach 74.95%;then the structure of the inclusion complex was characterized by digital liquid crystal biological microscope, scanning electron microscope, ultraviolet spectrophotometry and infrared spectroscopy.

Abstract:To prepare sulfonated polyimide/ordered mesoporous carbon (SPI/CMK) hybrid membrane, the mixture, containing CMK suspension in ethanol obtained under ultrasonic condition and m-cresol solution of SPI, was casted onto the glass plates. The uniform dispersion of CMK in the hybrid membrane was confirmed via SEM. The properties of the corresponding hybrid membranes, such as water uptake, solvent uptake, size change, proton conductivity, methanol permeability, mechanical properties, and stabilities, were investigated. The results showed that, compared to the blank membrane, the anti-swelling, thermal stability, and oxidative stability of the hybrid membranes were improved by 15~30%, 20~30 oC, 1.3~1.5 times, respectively, the water stability and mechanical properties were also improved, whereas the proton conductivity of the hybrid membrane was decreased in some extent.

Abstract:Amphiphilic derivative of chitosan oligosaccharide (COS), N-linoleyl chitosan oligosaccharide (LCOS), was obtained by introducing linoleic acid into COS through acylation reaction. The chemical structure of LCOS was characterized by IR, elemental analysis and Gel permeation chromatography (GPC). The micellization behavior of LCOS in aqueous solution was studied by fluorescence spectroscopy using pyrene as a probe, and the meso-tetraphenylporphyrin-loaded LCOS micelles (TPP-LCOS) were prepared. The thermodynamical parameters of TPP-loaded process were determined by isothermal titration calorimetry (ITC). The results showed that the substitution degree of the product was about 42.1%. The critical micelle concentration of LCOS was 2.00×10-3 g/L. TPP could be efficiently loaded by LCOS into spherical nano-micelles, and the particle size of the TPP-loaded LCOS micelles was between 60 and 100 nm. In addition, the medium-strength combination between LCOS micelles and TPP (Ka=2.87×106 L/mol) would be expected to slow release of TPP and enhance the efficacy time.

Abstract:A novel fluorescent molecular probe CCo for Co2+ based on the coumarin-thiazole-hydrazone-functional structure was designed and synthesized. The molecular structure were characterized by 1HNMR and 13CNMR etc. The spectral properties, the electrochemical properties and the quantum chemical calculation of CCo were studied. CCo exhibited high selectivity to Co2+ among such metal ions as Cd2+, Co2+, Na+, Mn2+, Fe3+, Pb2+, Hg2+, Cu2+, Zn2+, Cu+, K+, Mg2+, Ag+, Ni2+, Cr3+. The addition of Co2+ led to a 60 nm red-shift in absorption spectra and 75 nm blue-shift in fluorescence spectra. To use tetrabutylammonium perchlorate as the supporting electrolyte, the CCo solution with three electrode system could recognize Hg2+. The peak value of the absorption spectra for the CCo which was verified from the theoretical calculation was consistent with the experimental value.

Abstract:By introducing a phenoxy group into the straight alkyl group of the sodium soap of ordinary fatty acids, a novel modified soap——sodium 2-(4-nonylphenoxy) acetate (SNA) was synthesized. The molecular structure of the product was identified by FT-IR and 1H-NMR, and the purity of 98% of the product was confirmed by the results of two phase titration and HPLC measurement. Performance of SNA was measured both at pH 7 and pH 10, such as Krafft point (TK), surface tension, wetting time (WT), foam ability, calcium stability, lime soap dispersing requirement and emulsifying power, which was further compared with sodium soap of oleic acid (SOA) and sodium dodecylbenzene sulfonate (LAS). The experimental results show that SNA has the excellent solubility at low temperature (TK < 0 °C); the excellent pH-independent wettability (WT = 25 s) compared to SOA (WT  15 min); and the good concentration-independent defoamability. Therefore, SNA has the potential as a novel low-foaming soap-type penetrating agent.

Abstract:The cationic polymerized fluorosurfactants, N-(perfluoroalkyl acid ethyl ester)-N-(ethyl alcohol acrylate) dimethyl bromide(PFDM), with different length of fluorocarbon chain were synthesized using perfluoroalkyl ethyl alcohols(PFEA) as raw materials. The structures of the products were identified by means of 1H NMR. The influence of the length of fluorocarbon chain on the properties of PFDM was studied by zeta potential measurement and surface tension method, and the polymerizability of the PFDM was proved. The results show that the aggregation numbers of micells and the surface activity of PFDM increase with the increasing of the length of fluorocarbon chain, the CMC of PFDM declines exponentially with the increasing of the length of fluorocarbon chain, and PFDM has good polymerizability.

Abstract:Enzymatic synthesis of S-phenyl-L-cysteine from L-serine and thiopheno catalyzed by tryptophan synthase from recombinant Escherichia coli were studied. The factors such as temperature, pH, molar ratio of L-serine to thiopheno and substrate concentration were investigated. The optimal temperature and pH value were 37 ºC and 8, respectively. The optimal molar ratio of L-serine to thiopheno was 1:1.2. The optimal substrate concentration of L-serine was 400 mmol/L. Under the optimal conditions, bioconversion rate of L-serine reached 91% after 16 h. The stable hydrogen bonds were formed between thiopheno and tryptophan synthase active site Ser235 and Gly233.

Abstract:To improve the extraction yield of polyprenols (PPs), the novel -complexing extractant that consisted of 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM]PF6) containing AgBF4 was used to extract PPs from the extracts of Ginkgo leaves. The results showed that the extraction rate of PPs reached 93.13% at 23C, while the initial concentration of PPs in n-hexane of 2g/l, silver iron concentration in the extractant of 0.02 mol/L, the volume ratio of material solution to extractant of 1:1 and extraction of 2 h. Compared with previous methanol aqueous AgNO3 extractant, [BMIM]PF6-AgBF4 extractant showed much lower silver iron concentration and significant shorter operation times. When the extractent was recycle three times, the average extraction rate was 91.21%, showing no obvious decline.

Abstract:The Selective hydrogenation of nitrobenzene(NB) to aniline(AN) is an environmental friendly synthesis route, and its core is the efficiently selective hydrogenation catalyst. Herein, the amorphous Ni-Mo-P-Expanded Graphite(EG) catalysts were prepared by impregnation-chemical reduction method. Then, their selective hydrogenation catalytic performance was researched by the probe reaction above. After that, the catalytic properties of the samples were further investigated by X-ray diffraction(XRD), thermogravimetric analysis(TG), temperature programmed reduction (TPR), test of specific surface area and pore size distribution, etc. Finally, the results show that appropriate addition of expanded graphite could increase the specific surface area and stabilize the active species of the catalyst. Meanwhile, it could also increase the thermal stability and activity of the catalyst. The optimal addition of EG is 8 wt %, with the reaction temperature of 110 ℃, hydrogen pressure of 1.8 MPa and reaction time of 90 min, the conversion of nitrobenzene and selectivity of aniline reached 99.9%, respectively.

Abstract:With beef enzymolysis liquid as raw material, the flavor essence of braised beef brisket with tomato is prepared through thermal reaction. By exploring the influence of different enzymatic hydrolysis on flavor essence through single factor and orthogonal experiments, and combining with the sensory evaluation results & degree of hydrolysis, the optimal enzymatic hydrolysis conditions are found. Flavourzyme is the best enzyme for this flavor essence, and the optimal reaction conditions are as follows: material ratio is 3∶4; enzyme dosage is 0.10%; reaction temperature is 45℃; reaction time is 3h; under the natural pH. Degree of hydrolysis is 4.45%. Moreover, in this condition braised beef brisket with tomato flavoring has strong aroma, lasting aftertaste and high similarity to the dish.

Abstract:The volatile flavor constituents of Wuxi sauce sparerib were extracted by solid phase microextraction (SPME) and simultaneous distillation extraction (SDE), and identified by the gas chromatography-mass spectrometry (GC-MS). A total of 76 compounds were identified and they were 6 hydrocarbons, 19 aldehydes, 7 ketones, 9 alcohols, 4 phenols, 2 ethers, 4 acids, 7 ester and 18 sulfur-containing compounds, nitrogen-containing compounds and heterocyclic compounds. 23 compounds were all identified by the two extraction methods, including D-limonene, hexanal, nonanal, furfural, benzaldehyde, benzeneacetaldehyde, hexadecanal, 2-heptanone, 1-hydroxy-2-propanone, 2-nonanone, linalool, 2-furanmethanol, 2-methoxy-phenol, phenylethyl alcohol, eugenol, estragole, anethole, 2-pentyl-furan, methyl-pyrazine, 2,5-dimethyl-pyrazine, 2,6-dimethyl-pyrazine, 2-furancarboxaldehyde and 1-(1h-pyrrol-2-yl)-ethanone.

Abstract:Volatile flavor components in Sinkiang Naan package of meat were extracted by simultaneous distillation extraction (SDE)or solid-phase micro extraction (SPME) and analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 69 volatile compounds were identified in Sinkiang Naan package of meat, including 15 hydrocarbons, 18 aldehydes, 9 alcohols, 5 ketones, 4 acids, 7 esters, 11 heterocyclic and other compounds. Different results were obtained using the different extraction methods.The major compounds in the SDE extract were hydrocarbons (19.68%) and aldehydes (23.7%), while the major compounds extracted by SPME were alkanes (14.48%) and alcohols (11.34%).

Abstract:Febuxostat was synthesized from 4-hydroxybenzonitrile via alkylation，bromination，thioformylation，cyclization，cyanation，and hydrolysis. In the improved process，a LiCl-promoted thioformylation needed less time as well as avoided the use of strong acidic conditions. With the catalysis of trace Pd(OAc)2，a cyano group was smoothly installed in the presence of K4[Fe(CN)6] without anhydrous anaerobic operation. Non-toxic K4[Fe(CN)6] was used advantageously compared to toxic cyanide sources. The total yield was as high as 64.3 %．The structure was confirmed by melting point，1H NMR，13C NMR and ESI-MS.

Abstract:With the CM-β-CD as a chiral selector to separation of chiral drugs by capillary electrophoresis, but which exist the problem of low separation selectivity, the asymmetry of the peaks, the adsorption of the sample molecules, and the instability baseline. A cyclodextrin derivatives similar with ionic liqid was prepared by the cation exchange reaction of CM-β-CD with 1-butyl-3-methy-limidazolium bromine ionic liquid. And study the application in capillary electrophoresis, that is as a chiral selector to separation of chiral drugs. Compared with CM-β-CD, the results showed that the separation selectivity remarkably increase, improve the peak shape and the baseline basically stable, obtained the ideal separation effect.

Abstract:Cardanol acetate (CA) was synthesized with bio-based cardanol reacted with acetic anhydride catalyzed by toluene sulfonic. The second step, that is, cardanol acetate (CA) was epoxidized by hydrogen peroxide as a clean oxidant and formic acid was deployed as catalyst. Herein, the influences of several related factors on the epoxy value of product, such as the concentration of hydrogen peroxide (H2O2), the amounts of formic acid and hydrogen peroxide, reaction temperature, and reaction time were discussed. Based on aforementioned rules, the optimum condition was concluded as follows: 70 % H2O2, n (formic acid) : n (H2O2) : n (the amount of double bond in CA)=0.2 : 1.5 : 1, the reaction temperature was 65 oC and the reaction time was 6 h. Furthermore, the epoxy value of the final product under present condition was 6.8 % and a yellow transparent oily liquid was obtained. Simultaneously, the acid value, heat weight loss, viscosity and TG curves of the product were also investigated, respectively. As a result, ECA can satisfy the requirements of plasticizer.

Abstract:A CO2-triggered viscosity-sensitive copolymer P(AM-DMAEMA) was synthesized by N, N-dimethylaminoethyl methacrylate and acrylamide with different monomer ratio. The optimal conditions were that: monomer concentration 20%, initiator concentration 0.2%, polymerization temperature 40℃, polymerization time 4.0h. Molecular structure of polymer was characterized by 1H-NMR.Conductivity, Zeta-potential, effective diameter and viscosity experiments were employed to investigate their CO2-triggered viscosity properties and the mechanism of viscosity variation has been found. The results showed that the copolymer presented diversely viscosity variation properties and good CO2 absorb stability．

Abstract:Using tetrabutyl titanate as the main agent, polyhydric alcohol as the complexing agent, a type of acid organic-titanium cross-linking agent was synthesized. HPAM is used as a thickener. The study has examined the effects of the content of butyl titanate, the ratio of complexing agent and the pH value on the delayed gelling and the viscosity.The performance of the organic titanium/ HPAM fracturing fluid shows that: the delayed time is 300s, the viscosity of the system was still higher than 50 mPa?s after shearing for 90 min at the temperature of 95℃ and the shearing rate of 170s-1, so the fracturing fluid possessed good temperature tolerance and shearing resistance. By the result of the dynamic frequency scanning, G’>G”, so it is a typical viscoelastic fluid. When the sand ratio was 30% in volume, settling velocity was 0.025mm/s. It is less harmful to reservoir because the viscosity of the gel breaking liquid is lower than5.0mPa?s and the residue content is low after gel breaking.

Abstract:A series of acrylic acid -sodium allyl sulfonate copolymers were synthesized via free radical polymerization. Acrylic acid and sodium allyl sulfonate were used as monomers, ammonium persulfate and sodium hypophosphite were chosen as complex initiation system. The change of slurry viscosity was studied under the different amount of ammonium persulfate, sodium hypophosphite and monomers. It was confirmed that 80℃ was the optimum reaction temperature. The adding amount of ammonium persulfate preferably was 0.9% by mass of monomer, and that of sodium hypophosphite was 3%. The ratio of monomer and initiator preferably was 24:1. The copolymers were characterized by Fourier Transform Infrared Spectroscopy (FTIR). The influences of polymers to viscosity, body strength and dispersion of clay slurry were measured. It was discovered that 0.25% AA-CLS brought the lowest slurry viscosity on 695mPa•s, which reduced from 1988mPa•s. The body strength was raised by 38%. And the best dispersion of the slurry was also obtained.

Abstract:With methacrylate (MA) and glycidyl methacrylate (GMA) as monomers, ethylene glycol dimethacrylate (EGDMA) as crosslinker, and sodium dodecylsulfate (SDS) as emulsifier, varying the feed ratio of n(GMA)/n(MA), five epoxy-containing organic nanopolymers (ONPs) were synthesized by emulsion polymerization method. The cationized organic nanopolymers (CONPs) were prepared by reacting ONPs with trimethylamine hydrochloride. FT-IR, particle size measurement, charge density determination, and TGA were used to characterize the structures of ONPs and CONPs. The antimicrobial properties of CONPs against E. coli and S. aureus were investigated by biological microscope and flask-shaking method. The results show that CONPs are particles with positive charges. ONPs and CONPs have good thermal stability. The mean diameters and antimicrobial activities of CONPs increase with increasing the amount of GMA in recipes.

Abstract:The synthesis of 1,3-propylene glycol monoallyl ether was investigated with 1,3-propylene glycol, solid potassium hydroxide and allyl chloride as raw materials, 1,3-propylene glycol as the reaction medium and tetrabutylammonium bromide as phase transfer catalyst. The effects of materials mole ratio, alkali dosage, the mount of catalyst, reaction temperature and time on yield of product were studied. The reaction conditions were optimized by using response surface methodology with three factors and five levels. The optimum conditions were as follows: m(tetrabutylammonium bromide):m(allyl chloride)=5%, n(1,3- propylene glycol):n(potassium hydroxide):n(allyl chloride) =6.3:1.2:1, at 72℃ for 3h. The yield could reach 82.48%. The recovery and reuse of 1,3-propylene glycol could reduce the economic costs. This process has the advantages of low toxicity, low content of by-products, short reaction time and high yield.

Abstract:Ethylene glycol monoethyl ether acetate was synthesized from ethylene glycol monoethyl ether and acetic acid，high activity of titanium sulfate selected as catalyst.Through single factor experiment,got the proper conditiongs for the synthesis: Based on 0. 2 mol ethylene glycol monoethylether , titanium sulfate/ Ethylene glycol monoethyl ether mass ratio of 0.055:1, acetic acid / ethylene glycol monoethyl ether molar ratio of 1. 5:1, mount of cyclohexane of 15ml, reaction temperature of 130 ℃, and reaction time of 3 h.Under this condition, give the highest yield of ethylene glycol monoethyl ether acetate is above 99%,selecticiy of 100%, Its structure was confirmed by IR, 1HNMR,catalyst reused five times still have high activity , titanium sulfate were characterized by XRD and TPD.

Abstract:In this study, phthalic anhydride was reduced by sodium borohydrid,then condensed with ethyl chloroformate on the effect of KHMDS, the product of the condensation was then hydrolysesed to give the phthalide-3-carboxylic acid which was the final target compounds. The effects of reducing agent proportion and reaction time on the yield of the reduction were studied,and also the effects of reagent mole ratio,reaction temperature and reaction time on the yield of the condensation were studied.After 3 steps,the total yield could reach up to 64.2%, the reaction condition was mild, and sodium cyanide which was the violent in toxicity was avoided to use,the structure of the targer compound was confirmed by means of ESI-MS and 1HNMR.

Abstract:Ni/SiO2 catalysts modified by Al, Cr, Cu and Zn were prepared by precipitation and applied in fixed-bed gas-phase catalytic cyclization of ethanediamine (EDA) with glycerol to 2-methylpyrazine (2-MP) in the present work. And at the same time, the effects of calcination and reaction temperature, GHSV and water content on the catalytic properties of Ni-Zn/SiO2 in cyclization were also investigated. The results indicated that the presence of ZnO led to the simultaneous production of acidic and alkali sites over Ni-Zn/SiO2, which was helpful to the activation of EDA and glycerol molecules and 2-MP formation through cyclization was improved. It was also found that the calcination temperature was an important factor on affecting the catalytic property of catalysts in cyclization. And Ni-Zn/SiO2 calcined at 500 oC exhibited the highest 2-MP yield of 66.4% along with complete conversion towards glycerol and EDA was obtained over Ni-Zn/SiO2 catalyst under the optimum reaction conditions: reaction conditions 380 oC, GHSV of carrier N2 150 h−1, water content in fed reaction liquid 70%.

Abstract:The N, N-dimethyltrimethylsilylamine (DMATMS) was synthesized by reacting trimethylchlorosilane （TMCS） with dimethylamine catalyzed by timethylmethoxysilane in the solvent 1, 2, 4-trimethylbenzene（TMB）. Effects of molar ratio of TMCS to TMB，reaction temperature, amount of catalyst, reaction time on the yield of DMATMS were investigated, and the target compound was characterized by means of FTIR, 1H NMR and GC. The results indicated that the highest yield of DMATMS was 90.77% when the molar ratio of TMCS to TMB was 1: 2, the reaction temperature was 30 ℃, amount of catalyst is 0.3 mL, feeding time of TMCS is 20 min, and reaction time was 60 min. After purification, the purity of DMATMS reaches 97.31%.

Abstract:This article presents an efficient method for the synthesis of 3,5-dinitrosalicyl hydrazide-15N2, with salicylic acid as the common substrate. Nitration of salicylic acid with KNO3-15N provided 3,5-dinitrosalicylic acid-15N2 and then we got 3,5-dinitrosalicyl hydrazide-15N2 by the esterification and hydrazinolysis reaction. The yield of 3,5-dinitrosalicyl hydrazide-15N2 was 55.5% based on K15NO3. The product was confirmed by NMR and LC-MS to be the target compound. Its chemical purity was 97.3% and isotopic enrichment of 15N was 99. 2 atom%15N. It could be used as internal standard in the field of food safety testing．