Recovery of microalgae from its broth solution using kaolin based tubular ceramic

membranes prepared with different binders

Introduction of application-
Microalgae based products are useful as a feedstock for biofuels and value-added products
like protein, starch, nutraceuticals, carbohydrates, cellulose lipids, pigments and antioxidants
etc. however it has been discovered that the cost of microalgae harvesting and dewatering
along with the equipment used for same comprise of maximum cost as compared to total
biomass production cost which is main bottleneck for application of microalgae based
products on commercial scale. Hence there is need for cost-effective and efficient method for
separation of microalgae from its broth solution.
The traditional techniques which includes sedimentation, coagulation, flocculation and
centrifugation can effectively separate algae from highly concentrated broth solutions but
uses high cost in terms of energy in case of diluted broths containing < 0.5 kg/ m3 of dry
algal biomass. Additionally, these methods use additives and coagulants which in turn may
cause contamination of final product and unnecessarily increase purification step.
Generally ceramic membranes are expensive, but low-cost raw material can be used in order
to keep the membrane cost low. Also, binders play important role in altering properties of
membrane such as mechanical strength, porosity, morphology and chemical stability. Binders
used can be both organic or inorganic.
The tubular ceramic membranes were prepared using low cost clay material such as kaolin
with different types of organic binders such as gaur gum (GG), carboxymethyl cellulose
(CMC), hydroxypropyl methylcellulose (HPMC) etc by extrusion method. These tubular
ceramic membranes were used for algal separation from its broth solution. Binders are
biodegradable, biocompatible and require only low concertation.
The characteristics like porosity, average pore size, pure water permeability, mechanical
strength, chemical and thermal stability, high corrosion resistance and selectivity were
evaluated. Considering the membrane properties, fabrication ease and separation performance
the best suited tubular membrane is used for algal separation.

Process-
Kaolin based tubular ceramic membrane with 100mm length, 11.5mm OD and 5.5mm ID
was fabricated using extrusion method. The paste containing clay material, kaolin-50% wt,
quartz-25% wt, calcium carbonate-25% wt and additives (binders) 3% wt of GG, CMC,
HPMC each was made and passed through extrusion set-up to fabricate tubular shape
membrane then, the prepared kaolin based tubular membrane was kept at room temperature
for 12 hr. Thereafter, the prepared ceramic membrane was kept at 100 °C for 12 hr and then
dried at 200 °C for 12 hr in an oven. Afterwards, sintering was done in a furnace at the
temperature of 950 °C for 6 hr with a heating rate of 0.5 °C/min. Finally, the surface finishing
was done and loosened particles were removed by keeping the membrane in sonication bath
Then these membranes were dried at 100 °C and taken for further characterization
Lab-scale setup for microfiltration of algae consisted of feed tank, dampener, pump, pressure
indicator, membrane module with the tubular arrangement, rotameter and control valves. The
pressure was maintained by adjusting control volve connected at bypass. Flow rate was
manipulated by adjusting control valve located on retentate side.
The algae, Chlorella Sorokiniana with feed stream of concentration 500 mg/L was passed
through the membrane from the feed tank, and the retentate was recycled back to the feed
tank. Permeate was calculated by weighing it under a digital weighing balance. Further, after
completing filtration at a particular pressure, the membrane was cleaned for 30 min with
Millipore water followed by passing a cleansing agent (NaOCl 4% w/v solution) through the
membrane for 2 hr to remove algae cells deposited on the membrane surface. Then, Millipore
water was passed through microfiltration system for 1 hr. With this cleaning procedure, the
regenerated membrane regains its original hydraulic permeability value (within ± 2%). Then
this membrane was considered for the next run of algae separation. The microfiltration
experiment for algae separation was conducted up to 2.5 hr at different operating pressures
(69–345 kPa) with feed concentration of 500 mg/L and a constant flow rate (1.11 × 10−5
m3 /s).
The desired characteristics such as % recovery, Total protein concentration, Total
carbohydrate concentration and volume reduction factor were calculated by practicing
experiments on permeate content.
Also, the analysis for fouling mechanisms were done for microfiltration of algae. It uses four
different empirical models depending on the type of pore blocking- 1) Standard, 2) Complete
pore blocking, 3) Intermediate, 4) cake filtration model

Results and conclusion-

Membranes made with various additives have an average pore diameter in size range of
0.137–0.182 μm, water permeability of 0.92619 × 10−7 − 1.8583 × 10−7 m3 /m2 s kPa and
porosity of 36–48%.
permeate flux was increased significantly as the applied pressure increased from 69 to 276
kPa and a sharp flux was decreased at higher operating pressures (276–345 kPa)
The separation results showed that all the membranes yielded a maximum permeate flux of
1.39–1.98 × 10−5 m3 /m2 s with almost 100% recovery of algae at an applied pressure of 276
kPa.
Noting the membrane properties, ease of fabrication and separation performance, Kaolin-
HPMC membrane was best suited for microalgae recovery as it offers the greatest
combination of recovery (100%) and permeate flux (1.78 × 10−5 m3 /m2 s).
Kaolin-HPMC membrane showed best performance in terms of permeate flux and other
excellent characteristics such as mechanical strength, porosity and corrosion resistance. The
experimental data generated for investigation of flux decline mechanism was best fitted for
Cake filtration model among all four models.