Batch Process for phenol removal using a green bed

4th year students: Omer Maarouf, Kubra Idris, , Kasar Khan Oudil, Amir Mahmood
Chemical Engineering Department , Faculty of Engineering, Soran University
Supervised by

Prof. Dr. Ibtisam Kamal

Content
Project objectives
1. Preparation of the green bed (walnut shell ash).

2. Using the green bed as adsorbent to remove phenol

from aqueous solution in batch process.

3. Studying the effect of adsorbent dose and contact time

on adsorption capacity.

4. Process Design and material balance calculations.

5. Process Control study and economical aspects.

Introduction

Phenol as contaminant

 Phenolic compounds exist in water bodies due to the discharge of polluted wastewater
from industrial, agricultural and domestic activities into water bodies.
 Phenol compounds are known to be toxic and inflict both severe and long ‐lasting
effects on both humans and animals.

 They act as carcinogens and cause damage to the red blood cells and the liver, even at
low concentrations.

 Interaction of these compounds with microorganisms, inorganic and other organic

compounds in water can produce substituted compounds or other moieties, which
may be as toxic as the original phenolic compounds.
Methods for phenol removal
Phenol removal by adsorption ( include the commercial adsorbents used)
Green adsorbents ( definition, types and advantages)
Adsorption
Adsorption is considered as one of the appropriate techniques for removal of phenolics
from water because the technique is easy to design and operate. The technique produces
no toxic wastes. Adsorption process involves the accumulation of the pollutant on the
adsorbent's surface . An appropriate adsorbent must be porous with large surface area,
possess high hydrophobicity and have the ability to selectively accumulate the pollutant
from water onto its surface. Efficiency of the adsorption process is governed by :

1.Adsorbent's properties, i.e. its functional group composition, the size of its surface area
together with the distribution of the pore size and the extent of its ash content.
2.The solution chemistry including its pH, temperature, degree of polarity, availability of
other solutes competing for the adsorbent surface area and the concentration of the
adsorbate.

3.Nature of the adsorbate. This includes its degree of solubility in water, hydrophobicity,
size and molecular weight.
Experimental part

I. Preparation of the green bed

Walnut shell was collected from household waste of Erbil Province gardens and mainly
from Erbil city. After screening the shells and separation from impurities, in order to
softening Walnut shells, walnut shells were placed for 24 hours in the urban water,
rinsed and were dried for 5 hours at 105 oC in thermostatic oven. The dry shells were
milled using electric mill and then were screened with standard laboratory sieves.
Particles with an average particle size of 0.38 mm were impregnated with acid solution.
The activated shells were carbonized in an ash furnace at 500 oC for 60 min, then used as
the green adsorbent bed in our project.

II. Preparation of standard solutions & absorbance determination

A stock solution of phenol compound was prepared by dissolving special amounts it in
water. This solution was diluted as required to obtain standard solutions containing
2,4,6,8, 10 and 12 microgram/ml. The absorbance of the solutions was determined by
UV-Visible spectrophotometer between 200 and 750nm. The standard calibration curve
is then plotted.
Characteristics of the prepared activated carbon

Parameter Value
Bulk density (kg/m3) 792
C% 52.65
O% 32.22
Si% 1.56
P% 0.97
Specific surface area (m2/g) 765
Average pore diameter (nm) 46.6
Porosity % 32.9
pH 3.3
Iodine no. (mg/g) 622
Ash content % 4.4
*The full characterization is supported by Iraqi South Oil Company, Nahran Omer Laboratories
Characterization of phenol solution by UV-Visible Spectroscopy
Exp. no. Conc. Absorbance
microgram/ml

 1 2 0.20
 2 4 0.41
 3 6 0.62
 4 8 0.74
 5 10 0.96
 6 12 1.22

Typical UV-Visible spectrum for a phenol solution

Typical calibration curve for phenol standard solution

Batch adsorption Studies
 
1. Effect of adsorbent dose
 
Batch adsorption equilibrium experiments were carried out by contacting a known amount of
walnut shell powder with 100 mL wastewater sample in a sealed glass bottle.
Set of eight samples each contain 100 ml of effluent was taken in a 300 ml beaker and
certain amount of adsorbent was added to it. The concentration of of the solutions were (0.5,
1, 1.5,2,2.5, 3,4,5, g/100ml). The samples were kept on a shaker (200rpm) at a constant
temperature for 24 h to reach equilibrium. The samples were withdrawn and filtered with
Whatman no.1 filter paper. The samples were analysed by U.V. spectrophotometer for
absorbance. The percentage removal was calculated as percentage reduction in the
absorbance. The batch studies were carried out at ambient temperature. All experiments
were carried out in duplicates and the average values were reported.
  Adsorbent dose % Removal
(g/100ml)
1 0.5 32.1
2 1 53.7
3 1.5 65.4
4 2 77.5
5 2.5 82.2
6 3 88.4
7 4 88.1
8 5 88.5
Effect of contact time
 
For carrying out batch operation, and to study the effect of contact time, set of seven
samples each contain 100 ml of effluent was taken in a 300 ml beaker and identical amount of
adsorbent was added to each sample. Each sample was kept on a shaker (200rpm) at a
constant temperature for definite time (25,50, 75, 100, 125, 150, and 200 minute). The
samples were withdrawn and filtered with Whatman no.1 filterpaper. The samples were
analysed by U.V. spectrophotometer. The percentage removal was calculated as percentage
reduction in the absorbance

  Contact time ( minute) % Removal

1 25 35.3
2 50 51.3
3 75 65.6
4 100 77.8
5 125 88.4
6 150 88.4
7 200 88.5
Mass balance: look over the following reference
 
BAYBARS ALI FIL, AND MUSTAFA KORKMAZ, GENGIZ ÖZMETIN.
AN EMPIRICAL MODEL FOR ADSORPTION THERMODYNAMICS OF
COPPER (II) FROM SOLUTIONS ONTO ILLITE CLAY-BATCH
PROCESS DESIGN. J. Chil. Chem. Soc. vol.59 no.4 Concepción dic. 2014

 http://dx.doi.org/10.4067/S0717-97072014000400012