STUDY ON DETERMINATION OF TRACE Cu（Ⅱ） BY DDCT CHELATING RESIN PRECONCENTRATION AND THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A new method for determination of Cu（Ⅱ） by DDCT chelating resin preconcentration and thin layer resin phase spectrophotometry was developed. The method has a high sensitivity （ε455= 3.6×10^5L/mol·cm）, which is 33 times higher than that of liquid phase spectrophotometry. It has a good selectivity （most coexisting ions could not influence determination） and an ideal precision [30μg Cu（Ⅱ）, n=6, RSD= l.67%]. The content of Cu（Ⅱ） in water, high purity rare earth and its oxide was determined. The detection limit of Cu（Ⅱ） is 5.3μg/L , and the linear range is 0-7.2μg/ml. The result is satisfactory.

STUDY ON DETERMINATION OF TRACE Fe BY Fe(Ⅱ)-VA THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A new method for the determination of Fe by thin layer resin phase spectrophotometry in alkali condition was reported. The complex anion formed by Fe（Ⅱ） and VA was absorbed on the 717w resin and Fe was determined by making thin layer. This method had a high sensitivity （ε620= 3.0×10^5L/mol.cm）, which was 15 times higher than that of liquid phase spectrophotometry. It had been proved a satisfactory precision （5.01μg Fe, n=6, RSD=1.8%）. The trace Fe in natural water was determined and the recovery was 97%.

STUDY ON THE DETERMINATION OF TRACE Fe(Ⅲ) BY THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A method to determine Fe（Ⅲ） by thin layer resin phase spectrophotometry has been developed in this paper. The colored complex formed by Fe（Ⅲ） and 1,2-benzendiol is concentrated on the 717^# resin, then Fe（Ⅲ） can be determined directly by making thin layer. The method is sensitive with a apparent molar absorption of 4.8×10^4L/mol.cm, which is 16 times higher than that of liquid phase spectrophotornetry, most coexisting ions do not influence the determination. The detection limit for Fe（Ⅲ） is 1.47μg/L with the precision of 3.3% [n=6, 7μg/50mL Fe（Ⅲ）]. The calibration curve is linear in the range of 0-25μg/50mL. The preposed method was applied to the determination of Fe（Ⅲ） in water sample with satisfactory results.

PREPARATION OF WATERBORNE ULTRAFINE PARTICLES OF EPOXY RESIN BY PHASE INVERSION TECHNIQUE

Waterborne ultrafine particles of epoxy resin were prepared by phase inversion technique. The results of SEM revealed that the particles diameter was in the range of 50 to 100 nm and the effects on amount of water required at phase inversion point were also discussed.

PROGRESS IN PHASE INVERSION EMULSIFICATION FOR EPOXY RESIN WATERBORNE DISPERSIONS

In this review, our recent work in phase inversion emulsification （PIE） for polymer （especially epoxy resin） waterborne dispersions is summarized. Based on experimental results about PIE process, the physical model is proposed which can guide the synthesis of the waterborne dispersions such as polymer/nanoparticle composite dispersion. In the presence of a latent curing catalyst, PIE can give a crosslinkable epoxy resin waterborne dispersion. The dispersions can form cured transparent coatings with some unique properties such as UV shielding. They are promising in functional coatings, waterborne resin matrices for composites, and sizing for high performance fibers.

PREPARATION OF MICROGEL-EPOXY RESIN TWO-PHASE POLYMERS BY IN SITU POLYMERIZATION~*

Microgel-epoxy resin two-phase polymers were prepared by in situ copolymerization of ethylenic monomers with unsaturated polyesters. The choice of monomers and the effect of monomer concentration on microgel particle size were discussed. Agglomeration of particles played a significant role in the early stage of polymerization. The microgel dispersion in epoxy resin was stable after the finish of polymerization. Upon curing the particles remained well dispersed.

HYDRODYNAMIC AND THERMODYNAMIC EFFECTS IN PHASE INVERSION EMULSIFICATION PROCESS OF EPOXY RESIN IN WATER

The mechanism of phase inversion emulsification process （PIE） was studied for waterborne dispersion of highly viscous epoxy resin using non-ionic polymeric surfactants. Drop deformation and breakup, rheological properties, conductivity, and particle size measurements reveal the micro-structural transition amid emulsification. It is revealed that strong flow causes water drop to burst with the formation of droplets and huge interface. Phase inversion corresponds to an abrupt rheological transition from a type of viscous melt with weak elasticity to a highly elastic type of aqueous gel. This implies that the phase inversion equivalent to a curvature inversion. Based on this, a geometric model is postulated to correlate process variables to the particle size. The coverage and conformation of the surfactant plays key role for the particle size of the final emulsion. The interactions of thermodynamic and hydrodynamic effects are also discussed. It is concluded that the thermodynamics control the PIE while the hydrodynamics drives the creation of interface and involves every step of PIE.

PREPARATION OF BISPHENOL A EPOXY RESIN WATERBORNE DISPERSIONS BY THE PHASE INVERSION EMULSIFICATION TECHNIQUE

The phase inversion emulsification technique (PIET) is an effective physical method for preparing waterborne dispersions of polymer resins. Some results concerning the preparation of bisphenol A epoxy resin waterborne dispersions by PIET in our laboratory were summarized. Electrical properties, rheological behavior and morphological evolution during phase inversion progress were systematically characterized. The effects of the emulsifier concentration and emulsification temperature on phase inversion progress and the structural features of the waterborne particles were studied as well. The deformation and break up of water drops in a shear field were analyzed in terms of micro-theology, while the interaction and coalescence dynamics of water drops were discussed in terms of DLVO theory and Smoluchowski effective collision theory, respectively. Based on the experimental results and theoretical analysis, a physical model of phase inversion progress was suggested, by which the effects of the parameters on phase inversion progress and the structural features of the waterborne particles were interpreted and predicted.

Solid Phase Synthesis of 3,4,5-Trisubstituted-1,2,4-Triazoles Derivatives from the Resin-Bound Acylhydrazines

An extension of our methodology on solid-phase synthesis of 3,4,5-trisubstituted-1,2,4-triazoles under mild conditions has been developed. Firstly, the resin-bound acylhydrazine is reacted with orthoesters to provide resin-bound 1,3,4-oxadiazoles. Secondly, condensation of 1,3,4-oxadiazoles resin with the corresponding arylamines hydrochloride to form the the resin-bound triazoles. 3,4,5-Trisubstituted-1,2,4-triazoles derivatives were obtained from resin-bound acylhydrazines in several steps providing 78% - 87% overall yields and excellent purity. The advantages of this method include straightforward operation and high yield and purity of the products.

PHASE STRUCTURE AND PROPERTIES OF EPOXY RESIN MODIFIED BY POLYSILOXANE BEARING PENDANT AMINO GROUPS

Polysiloxane-modified epoxy resins were prepared through the reaction of epoxy resin with polydimethylsiloxanes bearing pendant N-(beta-aminoethyl)-gamma-aminopropyl groups. The morphology and properties of the cured epoxy resins modified by the polysiloxanes were investigated. It was found that the phase structure and properties of the cured epoxy resins depend mainly on the amino group content in the polydimethylsiloxane and the level of the modifier. The change of phase structure in the cured epoxy resin systems was responsible for the dramatic change in their mechanical and surface properties.

MICRO-PHASE SAEPARATION IN EPOXY RESIN WATERBORNE PARTICLES DURING CURING PROCESS

Sub-micron sized phenolic epoxy resin waterborne particles were prepared by phase inversion emulsification. Micro-phase separation occurred during the curing process at high temperature. The as-prepared samples possessed one glass transition temperature （Tg） and two exothermal processes during DSC heating scannings. After being thermally treated above the exothermal peak temperature, they possessed two glass transition temperatures with the disappearance of exothermal peaks, whilst a core/shell structure was formed. This was likely related with the outward diffusion of reactive oligomers to the outer layer of particles.

Preparation of Porous Silicone Resin Sheet with Phase Inversion in Parallel with Non Solvent Induced Phase Separation and Application to Hollow Particle Formation

We have tried to prepare the porous silicone resin sheet with the phase inversion method in parallel with the non solvent induced phase separation method. In the experiment, ethyl acetate and water were adopted as a good solvent and a poor solvent for silicone resin, respectively and ethyl alcohol as an amphiphilic solvent was used to increase the solubility of ethyl acetate in water and decrease the interfacial tension by mass transfer from water to ethyl acetate. The concentration of silicone resin in ethyl acetate and the oil soluble surfactant species were changed. Increasing the concentration of silicone resin could depress coalescence between the water droplets in the (W/O) dispersion and increase the porosity and pore number density of silicone resin sheet. Span 80 among the oil soluble surfactant species made the porosity and pore number density larger. The effect of physical proparties of liquids concerned on the porosity and pore number density was discussed on the basis of dispersing behavior of liquid droplets in the liquid-liquid dispersion. The hollow silicone resin particles could be prepared by applying the preparation method presented here.

Preparation and characterization of hexadecane microcapsule with polyurea-melamine formaldehyde resin shell materials

This paper gives a brief report of the preparation of hexadecane microcapsule with polyurea-melamine formaldehyde resin shell materials(HMPM).The sealing performance and thermal stability of HMPM was enhanced much more effectively than that of microcapsule with polyurea shell material(HPM).The results of microscopical imaging analysis system,DSC,TG,and laser particle analyzer were briefly introduced.

Thermal Stability,Thermal Decomposition and Mechanism Analysis of Cycloaliphatic Epoxy/4,4'-dihydroxydiphenylsulfone/Aluminum Complexes Latent Resin Systems

The thermal stability of latent resin systems, cycloaliphatic epoxy/4,4＇- dihydroxydiphenylsulfone/aluminum complexes, was investigated by dynamic differential scanning calorimetry （DSC） analysis. Experiments were conducted under non-isothermal condition in a nitrogen atmosphere at the heating rate of 10, 20, 30 and 40 ℃/min, respectively. TG curves showed that, in the temperature range of 25 to 600 ℃, the stability of the resin systems could be enhanced by increasing the length of the aliphatic chain in the initiator. Both the Kissinger method and the Ozawa-Flyrm-Wall method were employed to calculate activation energies of the decomposition reaction, and the values obtained from the two methods were compared. Moreover, the corresponding reaction mechanism was identified by the Achar differential method and the Coats- Redfem integral method. The experimental results showed that these four methods were reliable and effective to study the kinetics of the thermal decomposition reaction; and the most probable thermal decomposition mechanism of the resin systems we proposed was found to comply with Mampel power law （m=1）.

Polymer-support Selenium-induced Electrophilic Cyclization:Solid-phase Synthesis of Flavonoids

The Lewis acid mediated polystyrene supported selenium cyclization of chalcones and oxidative cleavage of selenium resins flavonoids in good yields and purities have been reported. induced intramolecular gave the corresponding

A Facile Solid-phase Synthesis of 3-Carboxycoumarins

Carboxycoumsrins were synthesized via the solid phase synthesis conviently. The resin bound cyclic malonic ester reacted with o-methoxy or o-hydroxybenzaldehydes. Then cyclization was processed under H2SO4 to afford the products in excellent purities and yields.

Cure reaction and phase behavior of liquid crystalline epoxides-anhydride systems

A series of novel liquid crystalline epoxides with lateral substituents were cured with anhydrides and the cure kinetics was investigated by non-isothermal DSC technique. The results showed that the lengths of lateral substituents have great effect on the value of Ea. The curing reaction became less active, when the liquid crystalline epoxides have long lateral substituents and were controlled by diffusion at the late stage of cure. A nematic structure was observed by POM and XRD.

Convenient Solid-phase Synthesis of Benzothiazole Derivatives

Resin-bound cyclic malonic ester l reacted with aryl isothiocynate, then was treated with bromine, followed by cleavage from the resin under perchloric acid to give benzothiazoles 4.

IPDI改性水性醇酸乳液的制备及性能研究

水性醇酸涂料漆膜的硬度、光泽与耐水性较油性醇酸涂料差,改进这些性能对水性醇酸涂料的推广应用有重要意义。本研究以大豆油、季戊四醇及苯酐为原料,采用醇解法合成醇酸预聚体,并引入异佛尔酮二异氰酸酯(IPDI)改性,通过相反转法制成IPDI改性水性醇酸乳液。研究了IPDI用量、中和剂AMP-95用量、乳化工艺对水性醇酸乳液性能的影响。结果表明:当IPDI用量(以苯酐的质量计)为50%,AMP-95用量(以树脂的质量计)为0.6%,乳化剂用量(以树脂的质量计)为5%,搅拌速度为4000 r/min时,所制得的水性醇酸乳液漆膜硬度达2H,光泽为90.87,表干2 h,耐水性24 h无异常,漆膜综合性能表现良好。

SYNTHESIS AND PROPERTIES OF TRANSPARENT THIODIGLYCOL DIMETHACRYLATE COPOLYMER RESINS

The title compound, thiodiglycol dimethacrylate (TDGDMA), was synthesized from thiodiglycol and methacryloyl chloride by phase transfer catalysis reaction, and its structure was confirmed by FTIR and 1H-NMR analyses. TDGDMA possesses good polymerizability to produce a homopolymer resin with excellent transparency (T%, 90), moderate refractivity (nd20, 1.55), lower dispersivity (Abbe's number, 50.6) and higher glass transition temperature (Tg, 119°C). Through copolymerization with styrene (St) or styrene-4,4'-bismethacryloyloxydiphenylsulfone (BPSDMA), many properties of the copolymer such as refractive index, Abbe's number, strength, onset wavelength in the UV region and density were significantly modified. A copolymer resin with balanced properties between refractive index and dispersion was produced at the weight ratio of TDGDMA:St:BPSDMA (25:50:25), where nd20 and Abbe's number are 1.5815 and 36.5, respectively.