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.

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

In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-] in a strong acidic environments. This anion complex can also exchanges with a weaker anions on the surface active site of anion exchange resin, so that a [R+] [BiI4-] solid phase binary associational system is produced. Owing to the solid system is a great many dispersive particulates, it can be pressed to a thin-layer by press tools of the so called 搕hin-layer resin phase?or 搑esin phase? and using this solid association system spectrophotometry for the determination of trace metals. So it can increase the analytical sensitivity. This association system exhibits maximum absorbance at 460nm, and obeys Beer抯 law over the concentration range 0.01ug/ml^1.20ug/ml of bismuthous(III). It has a molar absorptivity of 7.1×105 [L/mol穋m]. It indicated the resin phase spectrophotometry is a sensitive analytical method for trace bismuthous. It is 18 times higher than routine aqueous spectrophotometry. The relative standard deviations is 1.82% (n=6) for the measurements of 0.5ug/ml Bi(III). The detection limit of Bismuthous(III) is 1.4×10-8mol/L. The method has applied to the analysis Bi(III) in environmental water samples.

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 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.

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.

Determination of Trace Amount of Yttrium with Bromopyrogallol Red by solid-phase Spectrophotometry

A simple and sensitive method for the determination of trace amount of yttrium by solid-phase spectrophotometry has been studied. Yttrium can form a 1 : 1 complex with bromopyrogallol red (BPR) on resin, which was determined directly at 605 nm, pH=6.5. It has a highly sensitivity (epsilon = 6.3 x 10(6)) which is 300-fold higher than the corresponding spectrophotometry in solution. The method was applied to the determination of yttrium in churchite.

Study on New Sensitive Method of Determination of Phosphorus by Solid Phase Spectrophotometry

The use of solid phase spectrophotometry for the determination of trace phosphorus in the system of phosphomolybdate-fructose is described. The adsorption of the system on anion-exchange resin is reported.

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.

Two Organic Phase Suspension Polymerization for Novel Hypercrosslinked Resin Bead by Polycondensation of CMB

The suspension polymerization with two organic phases was adopted to prepare spherical hyper- crosslinked resin by self-polycondensation of 4,4＇-bis-（chloromethyl）- 1, 1＇-biphenyl （CMB）. The chemical structure,morphology and pore characteristics of the novel spherical resin were characterized with Fourier transform infrared spectroscopy （FTIR）, micrograph and Brunauer-Emmett-Teller （BET）. It is found that the suspension system and stirring speed impose a great influence upon the regularity and size distribution of hypercrosslinked beads. To prepare CMB resin beads with diameter of about 300 μm, the optimal condition is as follows： stirring speed 300 r·min^-1, and the volume ratio of the two organic phases （nitrobenzene/dimethyl silicon oil） 1 ： 5. After the self-polycondensation and sqccedent post-crosslinking of CMB monomer, the spherical adsorbent presents high spec^al surface area （1190 m^2· g^-1） and abundant pore^volume （0.714 cm^3· g^-1）, and could be potentially applied qn the adsorption of various organic molecules and synthesis of porous ion exchanger.

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.

Comparison between Spectrophotometry and Gas Phase Molecular Absorption Spectrometry for Determination of Nitrite Nitrogen in Flue Gas

Spectrophotometry and gas phase molecular absorption spectrometry for determination of nitrite nitrogen in flue gas were compared.KOH absorption solution was used to absorb nitrite nitrogen in flue gas,and the concentration of nitrite nitrogen in the absorption solution was determined by spectrophotometry and gas phase molecular absorption spectrometry to obtain the concentration of nitrite nitrogen in flue gas.The experiments show that both methods are accurate and reliable.

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.

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.

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.

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。

萃余水相中酸和铀的连续测量方法

萃余水相中的酸浓度、铀浓度一般需分开检测,操作步骤繁琐,工作量大。本研究建立了连续测量萃余水相中酸浓度和铀浓度的新方法:先以强碱为滴定剂,通过指示剂的变色指示滴定终点,检测酸浓度;再加入硫酸和偶氮胂Ⅲ溶液,使溶液显色,在650 nm处测量显色溶液的吸光度。结果显示,酸浓度测量的精密度为1.53%,示值误差为1.69%;铀质量浓度测量精密度为1.13%,示值误差为1.52%。在实际水样测量中,本方法和实验室现行方法测量数据基本一致,酸浓度测量的加标回收率为97.0%~102.5%,铀质量浓度测量的加标回收率为97.0%~102.0%,本方法可准确、快速、连续监测萃余水相中的酸浓度和铀浓度。

生物基树脂改性沥青流变特性评价及体系融合行为

受石油资源储量和供应的限制,将生物质材料引入石油沥青已经成为一个热门话题。本研究以麦草秸秆液化产物为原材料合成三种生物基树脂(BPF、BPU和BPF-PU),并将其用于生物沥青的制备,旨在探究生物基树脂对沥青流变特性的影响及二者之间的交互作用。首先,通过频率扫描和多重应力蠕变恢复试验分析了树脂对沥青胶结料黏弹特性和高温抗车辙性能的影响;其次,借助流变学理论对树脂-沥青体系的相态结构进行了分析;最后,从荧光显微结构和官能团分布特征的角度探究了二者之间的融合行为。结果表明,BPF和BPF-PU能够增加沥青中的弹性成分,提升其高温抗车辙性能,而BPU则会强化沥青的黏性响应;三种树脂能够较为均匀地分散到基质沥青中,并与其形成稳定的相态结构,这可能是因为树脂与基质沥青之间形成了醚键(C-O-C)。本研究有助于为农作物秸秆的增值转化和生物沥青的开发提供新的思路,但在生物沥青性能的全面评价方面需要进一步研究。