Hyperpure gases are used in various aspects of semiconductor industry. Such hyperpure gases as H2, O2, N2, Ar, He, NH3, HCl, SiH4, PH3, B2H6, AsH3, H2Se, H2Te, CF4, CO2 have been widely used in semiconductor industry. Hydrogen selenide has attracted increasing interest all over the world. Hydrogen selenide, source material for semiconductor industry, is mainly used for P-N node, protection layers and isothermal layers in semiconductor devices and is urgently needed in national defense and aerospace technology. Currently, Hydrogen selenide is either prepared throughof hyperpure H2 and selenium at 250℃-570℃with the maximized output at 570℃, or through decomposition reaction of selenium compound and water.In this paper, hydrogen selenide was prepared through a two-step method: selenium powder and aluminum powder were used to synthesize aluminum selenide, which can react with water to synthesize hydrogen selenide. Preparation protection system and tail gas treatment system were designed to ensure higher purity of hydrogen selenide and security of preparation system.Many s were applied to determine the purity of hydrogen selenide compound, including Fourier spectroscopy, pulsed discharge helium chromatography, gas chromatography/mass spectrometry（GC/MS） and trace water analysis, which laid a sound foundation for standard hydrogen selenide.Standard hydrogen selenide was prepared by weight and was analyzed by GC/MS devices. Our results showed that consistency and lineage of hydrogen selenide were satisfactory. Its stability test showed that standard hydrogen selenide remains stable within 1 year with changes less than 2% （RSD）. Standard hydrogen selenide can be allowed to declare as the national reference gas for hydrogen selenide.
Post about "synthesis"
Triphenylamine and its derivatives are important raw materials that can be producedelectric charges transport materials and electroilluminant materials. They are also used asorganic dyestuffs and pharmaceutical intermediates. Synthesis ofand , R 2;-dimethyl and 4,4′,4″-trinitrotriphenylamine enhanced by microwave wasinvestigated in this paper. The better technological conditions have been obtained via theexperiments and the products have been characterized.The better technological conditions of triphenylamine’s have been obtained,i.e. diphenylamine and bromobenzene as the raw materials, dimethyl sulfoxide as the solvent,potassium tert-butoxide as the alkali, the molar ratio of diphenylamine, bromobenzene andpotassium tert-butoxide was 1:2:2, hermetical experiments were used under microwaveirradiation, the microwave power was 125W, the reactive time was 20 min, the reactivetemperature was 136 . The molar yield of the product could reach 98.7% under thistechnological conditions.The better technological conditions of 4,4′-dimethyltriphenylamine,s havebeen obtained, i.e. 4,4′-dimethyldiphenylamine and bromobenzene as the raw materials,dimethyl sulfoxide as the solvent, potassium tert-butoxide as the alkali, the molar ratio of4,4′-dimethyldiphenylamine,bromobenzene and potassium tert-butoxide was 1:2:2, hermeticalexperiments were used under microwave irradiation, the microwave power was 100W, thereactive time was 60 min, the reactive temperature was 175 . The molar yield of the productcould reach 69.5% under this technological conditions.The better technological conditions of 4,4′,4″-trinitrotriphenylamine’s havebeen obtained, i.e. p-nitroaniline and 4-chloronitrobenzene as the raw materials, dimethylsulfoxide as the solvent, potassium tert-butoxide as the alkali, the molar ratio of p-nitroaniline,4-chloronitrobenzene and potassium tert-butoxide was 1:3:2, hermetical experiments were used under microwave irradiation, the microwave power was 125W, the reactive time was 20min, the reactive temperature was 115 . The molar yield of the product could reach 98.2%under this technological conditions. was showed that the triphenylamine’s derivatives which its phenyls connected thedonor substitutions were harder to be synthesized than the t riphenylamine and thetriphenylamine’s derivatives which its phenyls connected the acciptor substitutions wereeasier to be synthesized than the triphenylamine under mircomave irradiation by theexperimental results. was also showed that the C N cross-coupling Ullmann reaction waseasy to be processed when the halobenzen which their halogen’s radius was big as rawmaterial under mircomave irradiation by the experimental results. The laws on the microwaveare the same as the conventional conditions’.The iodobenzene which was used in the traditional methods was replaced by thebromobenzene/chlorobenzene in the synthesis of triphenylamine and 4,4′-dimethyltri-phenylamine, so the cost of raw materials was greatly reduced. At the same time, the reactivetime was greatly reduced by the advanced microwave irradiation’s method. This method alsohas many advantages, such as pure products, few catalysts, easy post processing, easyoperation, safety, little pollution and so on. There had instructional effects for theindustrialization of triphenylamine and its derivatives.
Using duck blood and NaNO2 as main material, theof was studied. Effects of various factors on the of the pigment were discussed, and main factors were optimized. And then the stability and rheological properties of pigment were also studied, is benefit for further research. The results showed as follows.1. The method of acetone to determine the content of can exclude the interference of impurities during response action and could reflect the amount of pigment production more accurately.2. The synthesis conditions of pigment were optimized: The concentration of , NaNO2 content, ascorbic acid content, pH, temperature and the reaction time which are affecting the synthesis were studied through the single factor experiment. Based on the single factor experiment, the response surface analysis were used to optimize the various conditions of the main factors affecting absorption, the regression equation of the NaNO2 amount （x1）, ascorbic acid content （x2） and pH （x3） on absorbance （Y） can be gotten. The optimum combination of NaNO2 content, ascorbic acid content and pH is: 0.53 ml, 272.37mg, 4.51, its response to the corresponding value for absorbance 0.91.3.Under the 450-650 nm scan, the spectrum picture of pigment extracted by 80% aqueous acetone are the same as dinitrosyl ferrohemochrome （DNFH） and reported before, which indicated that the structure of them were similar.4. The experiment of pigment stability showed that: pigment was stable in 40min, and the high temperature over 85℃caused a lot of chromoproteins deposited after 40min which illuminated that a lot of chromoproteins were lost caused by this temperature and heating processing light was a certain impact on pigment stability, but far less than the light pigment of acetone extract of the impact. There was no effect on pigment under short time ultraviolet radiation.Cu2+ and Ag+ have a greater impact on pigment solution, when the two are put into soon there have joining muddy; Zn2+ and Fe3+ have little effect on the stability of solution. Ascorbic acid was relative to the stability of pigment, but the affection was not prominent. On the other side, saccharose and glycerin boost up the stability of pigment.5. The rheological properties of pigment were studied, The results showed as follows: when temperature is 25℃, 12% of the pigment solution is the fake plastic fluid of non-Newtonian fluids, non-Newtonian index is n=0.58, consistency coefficient is K=0.63; The sticky flow activation energy of 12% of the pigment solution is 28.38 kJ/mol; when temperature is 4°C, the apparent viscosity of pigment increase as the concentration of pigment solution increased, when the concentration is higher than 9%, the viscosity increase rapidly as concentration increased. At higher concentrations, the apparent viscosity of solution decrease as shear rate increased, and performs as fake plastic flow of non-Newtonian fluid, and while the concentration is <8%, the solution is Newton.fluid.
Synthesis and Characterization of the Symmetric and Unsymmetric Molecule and Polymer Viologen and Research of Their Electrochromic Properties
Electrochromism can be defined as the phenomenon of the electrochromic material to undergo color reversible change upon oxidation or reduction, which was ensued from changing the potential applied. Electrochromic material is a kind of newly-functional material which can change people’s life style and the way of utilizing energy sources.can be widely applied to large-area display devices, smart windows and electronic paper. Owing to its plentiful colors, better optical performance, fast color change, low cost, good cycling reversibility, organic electrochromic material has become a dominant direction in the electrochromic research in recent years. Viologen is an outstanding class among them.In this paper, we synthesized thirteen target compounds, including four symmetric compounds（1-4）, six unsymmetric compounds（1b-6b）, three side chain viologen polymers（1c-3c）, which were prepared by 4,4′-bipyridine reacted with benzyl chloride, 1-bromo-n-octane, p-chloromethylstyrene, ethyl chloroacetate respectively. These compounds were characterized with FT-IR,1H NMR and were proved to be consistent with the design.We studied the optical and electric properties of the thirteen viologen compounds by ultraviolet-visible spectrophotometry and . The ultraviolet-visible absorption spectra shows that these viologen compounds have absorption from 191 to 198nm and from 256 to 263nm in near ultraviolet area. The cyclic voltammograms shows that these viologen compounds have two pairs of redox peaks. There is a one-electron redox course between -0.3V and -0.6V(V2+ （?） V·+), and there is another one-electron redox course between -0.6V and -0.9V(V·+（?）V0).We prepared the viologen s on conductive ITO glass and solved the problem of the equalization of the films by improving conditions. We prepared the transparent s based on the viologen compounds on conductive ITO glass and tested the performance of the devices. The result shows that the best charged voltage range is from 2.5V to 3.0V. The devices can change color between violet and colorless circularly. The color time is about 3 s and the fade time is less than 1s. Their electrochromic performance are excellent and they may be used to produce electronic paper.
In the first part of the system outlined in the following:and its derivatives possess antitumour activity and some of them, such as Etoposide (VP-16) and Teniposide (VM-26), have been used as anticancer drugs for clinical chemotherapy. The C-4 configuration, which is of crucial importance for biological activity. Otherwise ,the challenge of a stereoselective is embedded in the formation of the four contiguous stereocenters and the presence of a base sensitive translactone moiety. There are some approaches known from previous literature for :Diels-Alder reaction, Tandem conjugate addition reaction etal.Papers in the experimental part of our literature considered on the basis of the experimental exploration, and podophyllotoxin s with the structural characteristics of a simple pepper aldehyde as the starting material, a,β-unsaturated carbonyl compounds are selective reduction lithium aluminum hydrogen reduction reaction as the key steps to have the Knoevenagel condensation, peracetic acid epoxy between chlorine and alkaline hydrogen peroxide epoxy, DCC condensation esterification reaction of the podophyllotoxin s.
The present dissertation comprehensively reports the systematical studies on the improvement of alkaline manganese batteries.The thesis has taken nano-Pb（OH）2 and AgCuO2 as main object of study and have carried out comparatively systematic research in two facets.Firstly,the discharge capability and circular characteristic of Pb（OH）2 doped EMD electrode has been studied.We have established a new method to synthesize Pb（OH）2.The best condition of this process is also discussed.XRD test,FSEM test,TG-DSC test and FT-IR test show that the prepared Pb（OH）2 is nano-Pb（OH）2.In order to study the influence of doping,nano-Pb（OH）2 is doped to EMD electrode.The discharge tests and the CV tests show that the discharge capability of Pb（OH）2 doped MnO2 electrode is improved. When the impure quantity reached to 2.5%,the discharge capability of nano-Pb（OH）2 doped EMD electrode increased 15.3%.The best ratio of Pb（OH）2 to total anode active material is 5%,9M KOH is used as electrolyte and graphite is used as electric conductor material.Secondly,we have synthesized AgCuO2 using the deoxidation mechanism.The best condition of this process is also discussed.XRD test,SEM test show that the AgCuO2 has been prepared successfully.We also studied theof AgCuO2 electrode.The charge and discharge capability under a unchangeable high current tests and the CV tests show that the of the electrode is very good.Under the high current density of 5A·g-1,the discharge capability of the electrode is 480mAh·g-1.The 100 circulation cycles discharg capability declined unconspicuous.The capability of AgCuO2 is very stabilized. is one kind of very good battery positive pole materials.
Cleavable surfactants contain a weak bond which is cleavable under certain conditions （such as acid, alkaline, heat, UV irradiation, and so on）. So they are more friendly to environment than common surfactants. At the same time, Cleavable surfactants can avoid troublesome problems such as foaming or unwanted emulsion formation after completing its application. Their products after cleavage possess some new functions that can be used in some special fields （such as biological pharmacy）. Many scientists are very interested in further exploiting more properties of these products at home and abroad. Nowadays, exploiting newand studying their have become a hot topic in surfactant field.Four new cleavable s-triazine fatty sulfonate surfactants [2-fatty amino-4-（2-sulfonic ethyl） amino-6-chloro-1,3,5-s-triazine] with different length of alkyl chains were synthesized from cyanuric chloride, fatty amine and （The abbreviations were OSEAT, DSEAT, TSEAT, HSEAT, respectively）. And their yields were all higher than 85%.Structures of OSEAT, DSEAT, TSEAT, HSEAT were characterized by elemental analysis, 1HNMR, IR and UV. And their was studied. The results indicate that this series of surfactants possess following characters:These surfactants exhibit high surface activity. Their critical micellar concentration are 6.19×10-3, 1.77×10-4, 3.58×10-5, 7.67×10-5mol/L. Their surface tensions under critical micellar concentration are 39.21, 38.48, 32.53, 38.15mN/m. Their efficiency to reduce surface tension of water （pC20） are 2.81, 4.37, 5.01, 4.57 at 25℃, respectively.These surfactants exhibit better foaming ability and foam stability. The foaming power of DSEAT is biggest, and the height of foam reachs to peak value of 185mm. The foaming power of HSEAT increased with raising temperature, and the peak value is 144mm at 55℃. The anti-calcium ability of OSEAT is best, and its foaming power and foam stability were hardly influenced by calcium ion concentration.DSEAT and TSEAT exhibit obvious wetting property and emulsifying power. Their wetting time are 79.5s and 295.2s, and their emulsifying time are 107.5s and 93.5s, respectively.Compared with sodium dodecyl benzene sulfanate C12-LAS, the efficiency of this series of surfactants to reduce surface tension of water is higher, their stability in hard water is better, and the foaming power is strong. The wetting property and emulsification ability are excellent.
(2β,16β-bis-(4-dimethyl piperazino)-3α,17β-diacetoxy-5α-androstane dibromide)is a long-acting nondepolarizing neuromuscular blocking agent,which was developed by Gedeon Richter Ltd.of Hungary.The processes of have not been reported at home,and there are only few literatures overseas.At present,the demand of pipecuronium bromide at home mostly depends on importation.Therefor developing a new process which can adapt to plant-scale production has a great deal of profits.2β,16β-bis-(4-methyl piperazino)- 3α,17β- diacetoxy -5α-androstane(7),the intermediate of the ,was synthesized via seven steps from easily obtained starting material such as 5α- epiandrosterone(21).We changed 5α-epiandrosterone by steps of esterification and elimination into 5α-androst-2-ene-17- one(2),with 85.3%overall yield.2β,16β-bis-(4-methyl piperazino)-3α-hydroxy-17-oxo-5α-androstane(5)was prepared by two different processes with compound 5α-androst-2-ene-17-one as the starting material(2). Starting with compound(2),one process is through three steps,including esterification of isopropenyl acetate,epoxidation of m-chloroperoxybenzoic acid and ring – opening addition of N-methylpiperazine,with 28.0%overall yield;the other process is through three steps, including bromination of cupric bromide,epoxidation of m-chloroperoxybenzoic acid and ring – opening addition by N-methylpiperazine of cupric bromide substituted by N-methylpiperazine,with 17.3%overall yield.Starting with compound(5),compound(7)is finally synthesized by the reduction of sodium borohydride and esterification of acetic acid and acetic anhydride with 63.8%overall yield.Compared with the two methods,the yield of the first is higher.Moreover,its comprehensive conditions are better.N-methylpiperazine can be replaced by Piperidine, which is also an important method to the intermediate of vecuronium and pancuroniurn.However,there are several disadvantages.For instances,synthesis of 17β-acetoxy-5α-androsta-2,6-diene(3)has a lower yield than method one,and the crystallization time of the product can not be easily hold.The second routine surmounts the difficulties,however,the yield is lower.The experimental conditions should be improved.The intermediates and the final product(7)that synthesized in the thesis are characterized by using FTIR,H~1-NMR and Mass Spectrometry(MS).
In this paper, MCM-22 zeolite was synthesized bymethod, using hexamethyleneimine (HMI) as a structure-directing agent. The influences of different parameters, such as silica source, crystallization time, the reactant ratio, and procedure in the of MCM-22 zeolite were investigated in detail. And characterization of MCM-22 was carried out by power X-ray diffraction (XRD), scaning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), Temperature-Programmed Desorption of NH3 (NH3-TPD) and so on. On the basis of successful synthesis of MCM-22 zeolite under the static hydrothermal condition, the synthesis of MCM-22 zeolite with activated carbon was also investigated. Furthermore, the catalytic performance in the dimethyl ether (DME) aromatization reaction over MCM-22 zeolite was studied. The results were summarized as follows:1. Under static synthesis conditions, a pure MCM-22 could be obtained at proper synthesis reaction composition using silicic acid, silica sol and silica gel as silica source. However, their aggregate morphologies and particle sizes were different. Not MCM-22 but ANA zeolite was obtained using sodium silicate as a silica source. The silica source and the alkalinity in the synthesis gel had great influence on the quality and purity of the products, while the amount of HMI and H2O had little influence on the synthesis of MCM-22 zeolite. The optimal synthesis conditions were: n(SiO2)/n(Al2O3)=30-60, n(OH-)/n(SiO2)=0.15-0.25, n(HMI)/n(SiO2) =0.35-0.6, n(H2O)/n(SiO2)=20-45. The crystallization time could be shorted markedly by adding seeds, while the synthesis procedure did not show significant influence on the synthesis of MCM-22. The long aging-time favored the nucleus formation of the MCM-22 zeolites.2. Under optimized synthesis conditions, high-quality MCM-22 zeolite was synthesized and characterized by XRD, SEM, FT-IR, N2 adsorption-desorption and NH3-TPD. was demonstrated that the MCM-22 zeolite obtained was high-quality without other impure phases.The existence of mesoporous was evidenced by the N2 adsorption-desoroption isotherms. And NH3-TPD profile showed MCM-22 had two kinds of acid site, stronger acidic centers and weaker acid sites on the framework. 3. When m(C): m(SiO2) ratio was 0.5-0.8, MCM-22 zeolite could be obtained with activated carbon under static hydrothermal conditions. And the amount of activated carbon was too high or too low, MCM-22 was hard to form or easily transform to ZSM-35. The results of XRD and SEM showed that MCM-22 obtained was pure without other impure phases, and activated carbon in the gel had little influence on the nucleation stage and crystal growing stage of MCM-22.4. In the reaction of DME aromatization, the selectivity of aromatics over H-MCM-22 decreased gradually with increasing n(SiO2)/n(Al2O3). As temperature increased, the conversion of DME and selectivity of aromatics over H-MCM-22 and H-C-MCM-22 both increased coorespondingly. The selectivity of aromatics over H-MCM-22 increased, but decreased over H-C-MCM-22 with increasing space velocity.
The development of traditional chemical pesticides has been limited because of traditional chemical pesticides having been some harm to human、environment and non-target organism,so the creative direction of present new pesticide creative direction has been becoming to look for the new high performance、lower toxicity、good selectivity and higher safety fungicide。Triazole compounds attracted people’s more concern because of broad-spectrum of biological activity、lower toxicity、lower resistance and the diversity of chemical structural。3,3-dimethyl-1-(-1,2,4-1-trizole-1-yl)-butanone is an important intermed- iate which synthesize triazole fungicide,and most of their prepared derivatives have good fungicidal activity。At present, many products have been developed and applied such as fungicides, insecticides,plant growth regulator and drugs。Triazole compound of different structures has different biological activity, so the new structures of triazole compound’s research and development becomes a hotspot。The paper researched the bio pathway of Ergosterol、the key enzymes of bio of ergosterol、the action mechanism of active group and structure-activity relationship。Eight novel triazole compounds which target enzyme were squalene epoxidase and isomerase/reductase and which raw material was 3,3-dimethyl-1-(-1,2,4-1-trizole-1-yl) – butanone was synthesized by aldehyde-ketone condensation、Michael addition reaction and reduction reaction。The structure of compounds was identified by IR、1H NMR、13CNMR and MS spectral methods.The antifungal activity of compounds were performed。The results showed that at the concentration of 100 mg/L,all of compounds showed different activity against four plant pathogenic fungi。The inhibition rate of compound 2 to four plant pathogenic fungi is higher than other compounds and more than 70%,especially to Cotton Fusarium Wilt。The inhibition rate of compound 3 to four plant pathogenic fungi is lower than other compounds,especially to Fusarium graminearum and Fusarium oxysporium,6.08% and 4.41% respectively。The inhibition rate of the compounds expect for compounds 3 to Cotton Fusarium Wilt is higher than other plant pathogenic fungi。The inhibition rate of compound 3 to Fusarium oxysporium which is 71.57% is higher than to other plant pathogenic fungi。