Dissolution Kinetic And Solvent Extraction Of Aluminium From Kaolin

CHAPTER TWO

2.0 EXPERIENTIAL METHODS

2.1 Materials

2.1.1 sample collection

The sample (kaolin) was collected from a porter at Okelele, Ilorin East Local government, Ilorin, Kwara Nigeria.

2.1.2 Reagents

The reagents uses for these study sources of chemistry department, Kwara State Polytechnic, Ilorin Kwara State include hydrochloric acid (HCL), distill water, Dithizone, potassium hydroxide.

2.1.3 Apparatus

All these apparatus used for this study are sourced from the department. These apparatus include Beaker, conical flask, pipette, crucible, ceramic pestle and mortar, thermometer, filter paper, funnel, spatula, bottle, weighing balance, stove, separating funnel, measuring cylinder, stirring rod, wire gaze, 250ml standard flask.

2.2 MATERIAL AND METHODS

2.2.1 Sample preparation

2.2.2 Grinding

Ceramic pistil and mortal was use to grind the sample into powder form.

 2.2.1.2 pulverization/particle sizing

The sample (kaolin) was been sieve into different particles sizes after grinding, this was done at the geological laboratory, university of Ilorin, Kwara State. The size ranges from 0.09µm, 0.3µm and 0.4µm.

2.3 CHARACTERISTICS OF THE SAMPLE 

2.3.1 Aqueous metal analysis 

              The aqueous metal, analysis of the sample was carried out at the agronomy department faculty of Agriculture, University of Ibadan, Ibadan Nigeria.

2.4 Physio-analysis

2.4.1 MOISTURE CONTENT

The moisture content of the sample was carried out at the geological department, University of Ilorin, Ilorin Kwara State. 2g of the sample was weighted in triplicate in the Crucible, these was later dried in the oven for 6 hrs at temperature 55Ëšc. The sample was withdrawn from the oven and was quickly transferred into the desiccator in other to prevent further moisture absorption from the atmosphere. The moisture content was the determined using:

Moisture content (%) =                                X                 (8)

Where W1 = weight of the sample crucible before drying.

W2 = weight of the sample of crucible after drying.

2.4.2 Ash content

The oven dried kaolin sample was put inside furnace and waster at high temperature about 500-600Ëšc for 2 hours after wasting the sample was then withdraw at the furnace and allows to cool for about an hour and then was determined was then recovered. The ash contact was determined using.

Ash content (%) =                                   X                                       (9)

Where: W1 = Weight of a sample + cruscible before drying

   W2 = Weight of the sample + cruscible after drying

2.5 Dissolution and solvent extraction studies

2.5.1 Leaching procedure

Leaching experiments were performed in the chemistry laboratory, chemistry department, Kwara State Polytechnic, Ilorin Kwara State. The experiments were performed by adding and mixing 1gram of the sample (kaolin) into 50ml of the leachant (0.1m, 0.5m, 1m and 4molar ) was heated to the desired temperature for 10, 20 30 and 60 minutes. Some selected residual products obtained after leaching in appropriate leachant concentration was analyzed using atomic absorption spectrometer to get the total metal concentration.

2.5.2 Solvent extraction procedure

Liquid- Liquid extraction was carried out using leachante from the leaching of 5grams of kaolin or in 0.4m HCL for 60mins for which the highest dissolution efficiency was recorded. Batch experiments were accordingly carried out at room temperature (25 ± 20C) by equilibrating 0.1m of Dithizone was use with 25ml of the leachate and shaking the mixture of both. After equilibration and phase separation, the concentration of aluminium left in the aqueous phase was analyzed using atomic absorption spectrometer (AAS).

2.6 TOTAL ALUMINIUM ANALYSIS

 2.6.1 Total iron precipitation

Iron oxidation was carried out by drop wise addition of potassium hydroxide and stirred for a period of time, when the mixture shows or form precipitate or slurry. It was then filtered using filter paper.  The titrate was residue solution later taken for AAS and the pure solution of aluminium obtained was subsequently use for the solvent extraction studies.

2.6.2 Extraction of aluminium

Diyhizone was used for the quantitative solvent extraction studies. Batch experiment was carried out by equilibrating equal volumes aluminium solution (25ml each), the mixture shaken for 40 minutes. After equilibration and phase separation using separating funnel. The percent of total aluminium extraction was quantitatively calculated.

2.6.3 Stripping process

The validity of the procedure was checked by complete stripping of several aluminium loaded in organic phase using dilute hydrochloric acid (0.5m) solution and analyzing the aluminium concentration in the striped phase.

 2.6.4 Aluminium salt production

Aluminium and its compounds such as oxides are products with wide applications in chemical and other apllied industries. The extracted stripped and pure solution of aluminium obtained after utilization of process operation such as (solvent extracting, precipitation and stripping for the enrichment of aluminium and obtains aluminum salt.