Protein fractionation by means of microfiltration (MF) is significantly affected by fouling, especially when spiral-wound membranes (SWMs) are used. We investigated the influence of the mode of transmembrane pressure (Δp_TM) increase to target level and the deposit layer pressure history on the filtration performance during skim milk MF at temperatures of 10 °C and 50 °C. Two filtration protocols were established: No. 1: Δp_TM was set directly to various target values. No. 2: Starting from a low Δp_TM, we increased and subsequently decreased Δp_TM stepwise. The comparison of both protocols tested the effect of the mode of Δp_TM increase to target level. The latter protocol alone tested the effect of the deposit layer history with regard to the Δp_TM. As expected, flux and protein permeation were both found to be functions of the Δp_TM. Further, both measures were independent of the filtration protocol as long as Δp_TM was held at a constant level or, as part of protocol No. 2, Δp_TM was increased. Thus, we can state that the mode of Δp_TM increase to target level does not affect filtration performance in SWM. We found that after completion of a full cycle of stepping Δp_TM up from 0.5 bar to 3.0 bar and back down, flux and deposit layer resistance were not affected by the deposit layer history at 10 °C, but they were at 50 °C. Protein permeation, however, was lower for both 10 °C and 50 °C, when the Δp_TM cycle was completed. The processing history had a significant impact on filtration performance due to remaining structural compression effects in the deposited layer, which occur most notably at higher temperatures. Furthermore, temperatures of 50 °C lead to deposit layer aging, which is probably due to an enhanced crosslinking of particles in the deposit layer. Apart from that, we could show that fouling resistance does not directly correlate with protein permeation during skim milk MF using SWM.

Micellar casein and casein monomers in milk serum are in a dynamic equilibrium. At temperature below 15–20 °C a considerable amount of casein monomers, β-casein in particular, is released from the casein micelle into the aqueous serum phase. This study investigates the effects of added calcium and related variations of pH on this peculiar equilibrium in order to minimize the amount of caseins in the serum and to better understand the casein permeation during microfiltration. The pH was varied in the range of 6.3 to 7.3 and the content of calcium was increased up to 7.5 mM by adding CaCl₂. Upon equilibration, the milk was separated by ultracentrifugation and the amounts of protein in the supernatant were analyzed. It was shown that the addition of low amounts of calcium shifts the equilibrium towards the micellar casein phase and can, thus, lower the serum casein content induced at low temperatures. Relative to that, the adjustment of pH separately from the CaCl₂ addition had a minor effect on casein concentration and composition in the serum.

This study determined the maximum possible filtration time per filtration cycle and the cumulated number of operational hours per year as a function of the processing temperature during milk protein fractionation by 0.1 µm microfiltration (MF) of pasteurized skim milk. The main stopping criteria were the microbial count (max. 10⁵ cfu/mL) and the slope of the pH change as a function of filtration time. A membrane system in a feed and bleed configuration with partial recirculation of the retentate was installed, resembling an industrial plants’ operational mode. Filtration temperatures of 10, 14, 16, 20, and 55 °C were investigated to determine the flux, pH, and bacterial count. While the processing time was limited to 420 min at a 55 °C filtration temperature, it could exceed 1440 min at 10 °C. These data can help to minimize the use of cleaning agents or mixing phase losses by reducing the frequency of cleaning cycles, thus maximizing the active production time and reducing the environmental impact.

Existing works on the influence of spatial effects on flux and permeation of proteins in microfiltration (MF) have focused on ceramic membranes. There is little information on spiral-wound membranes (SWMs). Since the inner core of a SWM is practically inaccessible by non-destructive techniques, three different prototypes were constructed in this study to optimize suitability for the investigation of spatial effects on filtration performance. To measure the pressure drop, shortened SWMs 0.25, 0.50, and 0.75 times the length of a standard industrial SWM (0.96 m) were designed. Second, a sectioned membrane (0.96 m) with separated compartments on the permeate side was constructed to analyze spatial effects on flux and protein permeation along the flow path of a SWM. Three different features characterized this sectioned module: sectioned permeate pockets, a sectioned permeate collection tube, and sectioned permeate drain and measurement systems. Crossflow filtration experiments showed that these modifications did not alter the filtration performance compared to an unmodified control SWM. Thus, it can be applied to assess spatially-resolved filtration performance in SWMs. The third prototype designed was a test cell with accessible flat sheet membranes and spacer material, as in SWMs. The flow path in this test cell was designed to match the characteristics of the channels between the membrane sheets in a standard SWM as closely as possible. The flow path length and the combination of membrane material and spacer architecture were the same as in the control SWM. This test cell was designed to assess the effects of length and processing conditions on the formation of a deposit layer. The combined results of these test modules can yield new insights into the spatial distribution of flux, permeation of target components, and deposit formation.

During skim milk microfiltration (nominal pore size of 0.1 µm) at 10 °C, the whey protein purity in the permeate is reduced by an enhanced serum casein permeation, primarily of β-casein. To decrease casein permeation, the possibility of a pre-heating step under pasteurization conditions before the filtration step was investigated, so as to shift the equilibrium from soluble serum casein monomers to impermeable micellar casein. Immediately after the pre-heating step, low temperature microfiltration at 10 °C was conducted before the casein monomers could diffuse into the serum. The hypothesis was that the dissociation of β-casein into the serum as a result of a decreasing temperature takes more time than the duration of the microfiltration process. It was found that pre-heating reduced the β-casein permeation during microfiltration without significantly affecting the flux and whey protein permeation, compared with a microfiltration at 10 °C without the pre-heating step. Furthermore, the addition of calcium (5 and 10 mM) not only reduced the casein permeation and thus increased the permeate purity, defined as a high whey protein-to-casein (g L⁻¹/g L⁻¹) ratio, but also decreased the filtration performance, possibly due to the structural alteration of the deposited casein micelle layer, rendering the deposit more compact and more retentive. Therefore, the possible combination of the addition of calcium and pre-heating prior to microfiltration was also investigated in order to evidence the potential increase of whey protein (WP) purity in the permeate in the case of Ca²⁺ addition prior to microfiltration. This study shows that pre-heating very close to low temperature microfiltration results in an increased purity of the whey protein fraction obtained in the permeate.