Dispersed phases preparation

Dispersions. In phenoHc resin dispersions, the continuous phase is water or a nonpolar hydrocarbon solvent. The resin exists as droplets that have particle sizes of 1—20 p.m and are dispersed in the continuous phase. Aqueous dispersions are prepared either in situ during the preparation of the resin itself or by high shear mixing (25,35). 

The construction of calibration curves is recommended in nephelometric and turbidimetric determinations, since the relationship between the optical properties of the suspension and the concentration of the disperse phase is, at best, semi-empirical. If the cloudiness or turbidity is to be reproducible, the utmost care must be taken in its preparation. The precipitate must be very fine, so as not to settle rapidly. The intensity of the scattered light depends upon the number and the size of the particles in suspension, and provided that the average size of particles is fairly reproducible, analytical applications are possible. 

The multiple emulsion technique includes three steps 1) preparation of a primary oil-in-water emulsion in which the oil dispersed phase is constituted of CH2CI2 and the aqueous continuous phase is a mixture of 2% v/v acetic acid solution methanol (4/1, v/v) containing chitosan (1.6%) and Tween (1.6, w/v) 2) multiple emulsion formation with mineral oil (oily outer phase) containing Span 20 (2%, w/v) 3) evaporation of aqueous solvents under reduced pressure. Details can be found in various publications [208,209]. Chemical cross-linking is an option of this method enzymatic cross-linking can also be performed [210]. Physical cross-linking may take place to a certain extent if chitosan is exposed to high temperature. 

An aqueous colloidal polymeric dispersion by definition is a two-phase system comprised of a disperse phase and a dispersion medium. The disperse phase consists of spherical polymer particles, usually with an average diameter of 200-300 nm. According to their method of preparation, aqueous colloidal polymer dispersions can be divided into two categories (true) latices and pseudolatices. True latices are prepared by controlled polymerization of emulsified monomer droplets in aqueous solutions, whereas pseudolatices are prepared starting from already polymerized macromolecules using different emulsification techniques. 

Among the various branches in colloid and interface science, polymer adsorption and its effect on the colloid stability is one of the most crucial problems. Polymer molecules are increasingly used as stabilizers in many industrial preparations, where stability is needed at a high dispersed phase volume fraction, at a high electrolyte concentration, as well as under extreme temperature and flow velocity conditions. 

PVA Particles. Dispersions were prepared in order to examine stabilization for a core polymer having a glass transition temperature below the dispersion polymerization temperature. PVA particles prepared with a block copolymer having M PS) x 10000 showed a tendency to flocculate at ambient temperature during redispersion cycles to remove excess block copolymer, particularly if the dispersion polymerization had not proceeded to 100 conversion of monomer. It is well documented that on mixing solutions of polystyrene and poly(vinyl acetate) homopolymers phase separation tends to occur (10,11), and solubility studies (12) of PS in n-heptane suggest that PS blocks with Mn(PS) 10000 will be close to dissolution when dispersion polymerizations are performed at 3 +3 K. Consequently, we may postulate that for soft polymer particles the block copolymer is rejected from the particle because of an incompatibility effect and is adsorbed at the particle surface. If the block copolymer desorbs from the particle surface, then particle agglomeration will occur unless rapid adsorption of other copolymer molecules occurs from a reservoir of excess block copolymer. 

Microemulsions are a convenient medium for preparing microgels in high yields and rather uniform size distribution. The name for these special emulsions was introduced by Schulman et al. [48] for transparent systems containing oil, water and surfactants, although no precise and commonly accepted definitions exist. In general a microemulsion may be considered as a thermodynamically stable colloidal solution in which the disperse phase has diameters between about 5 to lOOnm. 

The authors concluded that using the gas-phase preparation method leads to better control of variables during preparation and to higher dispersions of the active component over the conventional liquid phase impregnation method. 

The chemical composihons of the zeolites such as Si/Al ratio and the type of cation can significantly affect the performance of the zeolite/polymer mixed-matrix membranes. MiUer and coworkers discovered that low silica-to-alumina molar ratio non-zeolitic smaU-pore molecular sieves could be properly dispersed within a continuous polymer phase to form a mixed-matrix membrane without defects. The resulting mixed-matrix membranes exhibited more than 10% increase in selectivity relative to the corresponding pure polymer membranes for CO2/CH4, O2/N2 and CO2/N2 separations [48]. Recently, Li and coworkers proposed a new ion exchange treatment approach to change the physical and chemical adsorption properties of the penetrants in the zeolites that are used as the dispersed phase in the mixed-matrix membranes [56]. It was demonstrated that mixed-matrix membranes prepared from the AgA or CuA zeolite and polyethersulfone showed increased CO2/CH4 selectivity compared to the neat polyethersulfone membrane. They proposed that the selectivity enhancement is due to the reversible reaction between CO2 and the noble metal ions in zeolite A and the formation of a 7i-bonded complex. 

In this chapter we report on the gas-phase preparation of metal-supported catalysts, that is on the deposition of dispersed metallic nanoparhcles onto a surface. Taking most of the examples from the thoroughly studied chemistry of the [Mo(CO)is]/oxide support system, we successively consider (i) surface organometallic chemistry issues, (ii) the methods used to avoid chemical contaminahon of the deposit and (iii) the competition between nucleation and growth. 

As mentioned earlier, ordinary emulsions as prepared by mixing oil, water, and emulsifier are thermodynamically unstable. That is, such an emulsion may be stable over a length of time, but it will finally separate into two phases (the oil phase and the aqueous phase). They can also be separated by centrifugation. These emulsions are opaque, which means that the dispersed phase (oil or water) is present in the form of large droplets (more than a micrometer and thus visible to the naked eye). 

So far, we have prepared and tested many kinds of colloids, mainly in nonaqueous suspensions with combinations of metals or alloys as a dispersed phase and organic liquids as the dispersion media, without the use of any dispersing agents these are listed in Table 9.4.1. We next give some examples of transmission electron micrographs of nanoparticles produced by an aerosol method. A sample for TEM measurement was obtained by dropping colloidal suspension onto a Cu mesh coated with an evaporated carbon film of 10 nm thickness. Many colloids were so unstable... 

By far the most studied PolyHIPE system is the styrene/divinylbenzene (DVB) material. This was the main subject of Barby and Haq s patent to Unilever in 1982 [128], HIPEs of an aqueous phase in a mixture of styrene, DVB and nonionic surfactant were prepared. Both water-soluble (e.g. potassium persulphate) and oil-soluble (2,2 -azo-bis-isobutyronitrile, AIBN) initiators were employed, and polymerisation was carried out by heating the emulsion in a sealed plastic container, typically for 24 hours at 50°C. This yielded a solid, crosslinked, monolithic polymer material, with the aqueous dispersed phase retained inside the porous microstructure. On exhaustive extraction of the material in a Soxhlet with a lower alcohol, followed by drying in vacuo, a low-density polystyrene foam was produced, with a permanent, macroporous, open-cellular structure of very high porosity (Fig. 11). 

The dispersed phase of high internal phase emulsions may also be used to prepare polymeric materials in this case, conversion of monomer dispersed droplets to polymer results in latexes or particulates. 

Copolymer particles can also be prepared from HIPEs [159]. Thus, a HIPE dispersed phase consisting of styrene and methacrylic acid was polymerised to give copolymers. The surface concentration of carboxylic acid groups increased linearly with concentration of methacrylic acid in the feed. The small amount of water present in the concentrated emulsion, relative to conventional emulsion polymerisation, reduces the loss of methacrylic acid, which is highly water-soluble. 

Dispersed phase polymerisation of HIPEs has also been used to prepare polymer-supported quaternary onium phase transfer catalysts [162]. One strategy involved the polymerisation of a concentrated emulsion of vinyl benzyl chloride (VBC) in water and subsequent quaternisation of the polymer resin with tertiary amines and phosphines (Fig. 22). 

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