Autoclave processes

The original process for high pressure polyethylene was based on use of a high pressure autoclave and used air to introduce free radicals sufficient to initiate polymerization of ethylene. Principal features of the autoclave process are summarized in Table 7.2. 

Use of air has been largely supplanted by organic peroxides (see section 2.3). Organic peroxides are injected at several points in the autoclave and initiates free radical polymerization by chemistry discussed in Chapter 2. Reactor residence 

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The sweet water from continuous and batch autoclave processes for splitting fats contains tittle or no mineral acids and salts and requires very tittle in the way of purification, as compared to spent lye from kettle soapmaking (9). The sweet water should be processed promptly after splitting to avoid degradation and loss of glycerol by fermentation. Any fatty acids that rise to the top of the sweet water are skimmed. A small amount of alkali is added to precipitate the dissolved fatty acids and neutralize the liquor. The alkaline liquor is then filtered and evaporated to an 88% cmde glycerol. Sweet water from modem noncatalytic, continuous hydrolysis may be evaporated to ca 88% without chemical treatment. 

Polymer Production. Three processes are used to produce nylon-6,6. Two of these start with nylon-6,6 salt, a combination of adipic acid and hexamethylenediamine in water they are the batch or autoclave process and the continuous polymerisation process. The third, the soHd-phase polymerisation process, starts with low molecular weight pellets usually made via the autoclave process, and continues to build the molecular weight of the polymer in a heated inert gas, the temperature of which never reaches the melting point of the polymer. 

Atlanta, Ga., 26th-30th April 1998, p. 1842-9. 012 PRODUCT AND PROCESS DEVELOPMENTS IN THE NITROGEN AUTOCLAVE PROCESS FOR POLYOLEFIN FOAM MANUFACTURE Eaves D E Witten N Zotefoams pic (SPE)... 

A review is presented of the nitrogen autoclave process for the manufacture of crosslinked polyolefin foams. Process and product developments over the last few years are summarised and future possibilities are described. Process developments include use of higher temperatures and pressures to produce foams having densities as low as 10 kg/cub.m. Product developments include foams based on HDPE/LDPE blends, propylene copolymers and metallocene-catalysed ethylene copolymers. The structure and properties of these foams are compared with those of foams produced by alternative processes. 5 refs. 

In this section a specialized set of equations governing transport of mass, momentum, and energy in resin transfer molding, injected pultrusion, and autoclave processing are obtained from the general balance equations presented in Section 5.3. This involves eliminating unimportant terms in the general balance equations based on the specific nature of the process. 

Autoclave processing is a process in which individual prepreg plies are laid up in a prescribed orientation to form a laminate (Fig. 5.9). The process involves consolidation of the laminate, which generally results in a three-dimensional flow field. Similar to the IP process the fiber bed is not stationary in the AP process hence, its movement has to be specifically considered when the appropriate conservation equation for this process are developed. If it is assumed that the resin has a relatively constant density (i.e., the excess resin is squeezed out before the gel point is reached) then the appropriate conservation of mass equation for this consolidating system is Equation 5.12. 

The stability, growth, and transport of voids during composite processing is reviewed. As a framework for this model, the autoclave process was selected, but the concepts and equations may be applied equally effectively in a variety of processes, including resin transfer molding, compression molding, and filament winding. In addition, the problem of resin transport and its intimate connection with void suppression are analyzed. 

Before presenting the general model formulation and some results, it will be helpful to briefly examine the autoclave process details and some of the evidence for voids. 

Figure 6.2 Curing cycle temperature-time profile for typical graphite-epoxy composite in a vacuum bag autoclave process. Autoclave pressure is applied during the 135°C (275°F) hold...

The real question in light of Figure 6.10 is what exactly is the resin pressure throughout the product part Is it equal to the gas pressure above the bag in the autoclave process, or the entry resin pressure in the RTM process If not, how can the actual resin pressure be reliably predicted ... 

Once the elastic residual moment from Equation 8.30 or the viscoelastic residual moment history from Equation 8.39 have been determined, the final value may be applied elastically as platens open (hot pressing) or as the applied pressure is released (autoclave processing) to find the resulting cross-ply curvature. This curvature can then be correlated to experimental data. 

Figure 10.1 AV-8B wing skin preparing for autoclave processing...

Several viscosity and kinetic models, and experimental procedures for developing these models, are available for a number of commercially available resin systems [1-5]. These models allow insight into autoclave process decisions based on changes in resin viscosity and kinetic behavior and can be used to determine hold temperatures and durations that allow sufficient resin flow and cross-linking to avoid over bleeding, exotherms, and void formation. 

High pressures are commonly used during autoclave processing to provide ply compaction and suppress void formation. Autoclave gas pressure is transferred to the laminate due to the pressure differential between the autoclave environment and the vacuum bag interior. Translation of the autoclave pressure to the resin depends on several factors, including the fiber content, laminate configuration, and the amount of bleeder used. 

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