Resins time, sulfonation

An important aspect of this procedure is the use of latent acid catalysts, such as phenyl hydrogen maleate, phenyl trifluoracetate, and butadiene sulfone. These catalysts reduce the peak exotherm from over 200°C to 130—160°C. The resin catalyst mixture has a working life of up to several days at RT. The elevated temperature of mol ding these latent catalysts generates the corresponding acids, namely, maleic, trifluoracetic, and phenolsulfonic, which cataly2e the resole reaction. Typically, a cycle time of 1—2 min is requited for a mold temperature of - 150° C. 

ButylatedPhenols and Cresols. Butylated phenols and cresols, used primarily as oxidation inhibitors and chain terrninators, are manufactured by direct alkylation of the phenol using a wide variety of conditions and acid catalysts, including sulfuric acid, -toluenesulfonic acid, and sulfonic acid ion-exchange resins (110,111). By use of a small amount of catalyst and short residence times, the first-formed, ortho-alkylated products can be made to predominate. Eor the preparation of the 2,6-substituted products, aluminum phenoxides generated in situ from the phenol being alkylated are used as catalyst. Reaction conditions are controlled to minimise formation of the thermodynamically favored 4-substituted products (see Alkylphenols). The most commonly used is -/ fZ-butylphenol [98-54-4] for manufacture of phenoHc resins. The tert-huty group leaves only two rather than three active sites for condensation with formaldehyde and thus modifies the characteristics of the resin. 

Figure 1. The measured dry weight after hydrogen peroxide scission of sulfonated PSDVB XZ% DVB cation exchange resin) is seen to decrease linearly with reaction time. The time obtained by extrapolating to zero weight corresponds to visual observation degelation indicated by the disappearance of the resin particles.

For the preparation of the foam, a solution of 1 g technical sodium diisobutyl naphthalene sulfonate in 50 ml of 3% orthophosphoric acid is prepared. 20 ml of this solution are poured into a 11 beaker and air is stirred in with a fast running mixer until the cream-like dispersion has reached a volume of 300-400 ml.Then,20 ml of the prepared urea/formaldehyde resin are mixed in, whereby the resin must be evenly distributed. After 3-4 min the introduced resin gellifies into a molded article permeated with many water/air pores under the influence of the acidic catalyst. After 24 h,the crosslinking is completed. Drying for 12 h at 40 °C in a circulating air dryer yields a brittle thermoset foam.The foamed plastic obtained is hydrophobic and has a large internal surface. It can take up about 30 times its own weight of petroleum ether. 

In a similar way, Mizota et al. grafted polymer chains functionalized with sulfonic sites over a polystyrene-type polymer. As observed above, the flexibility of the polymer chains allowed better accessibility of the catalytic sites and this solid acid catalyst was ten times more active than the conventionally used cross-linked resin in the hydrolysis of sucrose (Scheme 2) [27]. 

Development of Resist Patterns. Development was done in AZ2401 developer diluted with 2 to 5 times its volume of water AZ2401 is an aqueous solution of KOH with a surfactant. When the resist films were exposed to electron beam doses of 5 iC/cm2 at 25 keV, it usually took 1.5 to 2.0 min for complete development of the images using a diazo-naphthoquinone sensitizer with o-chloro-cresol-formaldehyde Novolak resin in (1 3) AZ2401/water developer. With poly(2-methyl-l-pentene sulfone) the chlorinated Novolak resin exposed to I juC/cm2, it took 2.0 min in (1 4) AZ2401 developer for complete image development. 

The basis of the separation of amino acids by AAA lies in the interaction between acids - present in the elution buffer - and the stationary phase. This resin is made up of small sulfonated polystyrene particles. The negative charge of the sulfonic acid residues is counterbalanced by the Li+ -cations of the elution buffer. As the whole separation process takes place at a weakly acidic pH, the carboxylic acid residues are protonated and the interaction with the stationary phase of the column is achieved by the protonated (and thus positively charged) amino group(s) of the amino acids. The more basic the amino acid is, the stronger the interaction with the stationary phase and - consequently - the longer the retention time. So it is easily understood... 

As illustrated by the examples in Table 3.9, resin-bound 4-alkoxybenzylamides often require higher concentrations of TFA and longer reaction times than carboxylic acids esterified to Wang resin. For this reason, the more acid-sensitive di- or (trialkoxy-benzyl)amines [208] are generally preferred as backbone amide linkers. The required resin-bound, secondary benzylamines can readily be prepared by reductive amination of resin-bound benzaldehydes (Section 10.1.4 and Figure 3.17 [209]) or by A-alkyla-tion of primary amines with resin-bound benzyl halides or sulfonates (Section 10.1.1.1). Sufficiently acidic amides can also be A-alkylated by resin-bound benzyl alcohols under Mitsunobu conditions (see, e.g., [210] attachment to Sasrin of Fmoc cycloserine, an O-alkyl hydroxamic acid). 

Using a surface-sulfonated ion exchange resin (refs. 11-12), optimum accessibility of the active groups which are almost exclusively located at the inner surface of the microparticles is attained. The measured reaction rate (see Table 1) is about ten times higher than that of the identically cross-linked Lewatit SPC 11B. 

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