4th BIOMASS-ASIA WORKSHOP

20 22, NOVEMBER 2007

ANHYDROUS ETHANOL PRODUCTION

SU SU HLAING LECTURER DEPARTMENT OF CHEMICAL ENGINEERING MANDALAY TECHNOLOGICAL UNIVERSITY MINISTRY OF SCIENCE AND TECHNOLOGY UNION OF MYANMAR

Objectives
To prepare anhydrous ethanol with liquid phase adsorption process To investigate the adsorption of water on blue silica gel and to find the adsorption capacity of blue silica gel To determine the operating parameters for liquid phase adsorption process

What is Ethanol?
product of the fermentation of starch and sugar clear colorless liquid with a characteristic, agreeable odor completely miscible with water and organic solvents applications fuel chemical solvent cosmetics and pharmaceutical human consumption commercial alcohol 96% ethanol + 4% water anhydrous alcohol 99.5% ethanol + 0.5% water
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How is anhydrous ethanol produced?

by dehydration of commercial alcohol or industrial alcohol Technologies Extractive distillation Adsorption of water Azeotropic distillation Molecular sieve technology Pervaporation
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Adsorption Process
adsorption is essentially an attraction of adsorbate molecules to an adsorbent surface silica gel selectively adsorbs water to give anhydrous ethanol product (99.5% v/v) from commercial ethanol (96% v/v) the experimental technique is related to the various steps which must take place: preparation of blue silica gel packed column operating procedure

application of feed sample to the packed bed flow of feed sample through the packed bed
collection of separated sample (effluent sample) detection or identification of separated sample regeneration of spent silica gel (pink color)

Blue Silica Gel

Chemical molecular formula SiO2.nH2O highly active adsorption material inert and compatible with any kind of materials, except for strong alkaline substances and hydrofluoric acid turning from blue to pink after adsorping moisture an infinite life in terms of the ability to adsorb or desorb moisture silica gel can be reconditioned and reused indefinitely it is not recommended that blue silica gel be heated above 120C

Table 1. Properties of Blue Silica Gel Apparent or bulk density, g/cm3 Specific gravity Average porosity, % Specific surface, cm2/g Average pore diameter, cm Pore volume, cm3/g Commercial gas velocity, cm/min Weight adsorption of water at break point, % Weight of water at saturation, % 0.1 0.8 2.1 2.3 50 65 2x106 7x106 4x10-7 0.43 0.82 3.28 10 20 40
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Experimental Works size reduction of blue silica gel batch study (determination of isotherm) column studies (dynamic method) gravity flow separation process with one packed column gravity flow separation process with two packed column separation processes with mobile phase pumping unit
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Size Reduction of Blue Silica Gel Grinding the spherical silica gel was ground in a ball mill Screening screen analysis of the crushed particles was made with the aid of a laboratory test sieve shaker Drying the desired size of particles was preconditioned in an oven at 110C for 12 hr
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q, g of adsorbate/g of adsorbent

0.06 0.05 0.04 0.03 0.02 0.01 0 0 0.005 0.01 0.015 0.02 0.025 C, g of adsorbate/ml of fluid y = 2.6667x R = 0.9996
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Figure 1. Adsorption Isotherm Curve

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Feed Reservoir

Adsorption Column

Effluent Ethanol Sample Collector

11 Figure 2. Gravity Flow Separation Process with One Packed Column

Feed Reservoir

First Adsorption Column

Second Adsorption Column

Effluent Ethanol Sample Collector Figure 3. Gravity Flow Separation Process with Two Packed Column 12

Feed Reservoir

Pump

Adsorption Column

Effluent Ethanol Sample Collector Figure 4. Separation Process with Mobile Phase Pumping Unit by 13 using One Packed Column

Conclusions
the adsorption isotherm curve on silica gel fit with the linear isotherm Separation of water using small particle size silica gel gave better separation, however, a high pressure pump is needed. Water removal efficiency of the silica gel in this work is about 50% of the 96% ethanol is removed for one pass operation. In further work of separation with two columns in series is removed 75% on initial water present in 96% ethanol. Separation process with mobile phase pumping unit by using three column in series produces anhydrous ethanol (99.5% v/v) by removing 87.5% of initial water present in commercial ethanol.
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