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13 C NMR analysis of the stereoerrors and stereochemical sequence distributions (Table 8-3 and Sec 8-16) also support the polymer chain end control model [Zambelli et al, 2001] Analysis of propene ethylene copolymers of low ethylene content produced by vanadium initiators indicates that a syndiotactic block formed after an ethylene unit enters the polymer chain is just as likely to start with an S- placement as with an R-placement of the rst propene unit in that block [Bovey et al, 1974; Zambelli et al, 1971, 1978, 1979] Stereocontrol is not exerted by chiral sites as in isotactic placement, which favors only one type of placement (either S- or R-, depending on the chirality of the active site) Stereocontrol is exerted by the chain end An ethylene terminal unit has no preference for either placement, since there are no differences in repulsive interactions.

Not all syndioselective polymerizations proceed with polymer chain end control Some metallocene initiators yield syndioselective polymerization through catalyst site control (Sec 8-5) 8-4g Direction of Double-Bond Opening.

1 .o

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A syn or cis addition to the carbon carbon double bond is implied in the Ziegler Natta mechanism. The effect of the mode of addition to the double bond has no effect on the stereochemical structure of the polymers from 1-substituted ethylenes. However, the ditacticity of polymers from 1,2-disubstituted ethylenes depends not only on the mode of addition but also on whether the monomer is a cis or trans monomer. For diisoselective polymerization, syn addition to a trans monomer would give the threodiisotactic structure. This is shown in Fig. 8-14, where it is proposed that the carbon carbon bond in the monomer unit rotates after addition of the monomer to the polymer chain so as to avoid the 1,2-interactions in the fully eclipsed conformation [Goodman, 1967]. Syn addition to the cis monomer would yield the erythrodiisotactic polymer. Trans or anti addition to the two monomers would give the opposite results. Syn addition to the double bond in isotactic polymerization has been con rmed from studies with deuterium-labeled propenes [Miyazawi and Ideguchi, 1964; Natta et al., 1960; Zambelli et al., 1968]. The cis- and trans-1-d-propenes gave the erythro and threodiisotactic polymers, respectively. The syn addition mechanism described in Fig. 8-14 for isoselective polymerization is based on monomer always approaching the propagating center with the same face (either always re or always si) a reasonable assumption for a stereoselective process leading to isotactic polymerization. It is also assumed that incoming monomer is aligned with the propagating chain end so as to minimize steric repulsions between the R group of the chain end and the R groups on the carbon of the double bond that bonds to the propagating chain end; in

3-116

Many peroxides have signi cant chain-transfer constants. Dialkyl and diacyl peroxides undergo transfer by

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3-117

Figure 9.1 Two fitted curves with a 10-point data set and 1 additional outlying point of either class 0 or class 1. We can readily calculate the empirical IC for the 4 parameters under additional observation of either class. See the sub-plot for the 1Cs for an observation of class 1.

where R alkyl or acyl. The acyl peroxides have higher transfer constants than the aklyl peroxides, due to the weaker O bond of the former. The hydroperoxides are usually O

TABLE 3-5 Initiator Chain-Transfer Constantsa;b CI for Polymerization of Styrene Methyl Methacrylate Acrylamide 0.091 0.14 0.0003 0.00086 0.024 0.048 0.10 0.035 0.063 0 0 0.02 0.33 0.0028

Initiator 2,2-Azobisisobutyronitrilec t-Butyl peroxide Lauroyl peroxide (70 C) Benzoyl peroxide t-Butyl hydroperoxide Cumyl hydroperoxide Persulfate (40 C)

We add an additional point, an outlier, and refit the model from the same starting weights, to see what effect this has on the fitted model. When we add, respectively, a point from class 1 and a point from class 0, we get a very different outcome, both shown in Figure 9.1. In this instance, the asymmetric nature of the ICs leads to

Data from Brandrup et al. [1999]. All CI values are for 60 C except where otherwise noted. Ayrey and Haynes [1974]; Braks and Huang [1978].

R7, PE_header R7, R7, LSR #10 R7, R7, #1

the strongest transfer agents among the initiators. Transfer probably involves hydrogen atom abstraction

3-118

noticeably different results in the two cases . Note that the only effect that the outlier has is to change the shape of the fitted sigmoid (as shown in Figure 9.1), and that the decision boundary remains at approximately the same point and the classification accuracy remains the same. The inset plot in Figure 9.1 shows the empirical IC functions for an observation of class 1, while Figure 9.2 shows the same but with target values of 0.9 and 0.1. Note that in Figure 9.2 the shape has changed considerably and that it is now clearly discernible that the i s for 211 and 212 redescend to 0 in one direction and to a constant value in the other direction. This is described a partially redescending IC function and discussed in Section 8.7 (p. 139).

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