This document summarizes a project to salvage ethanol from a waste stream produced using the Stober process. The goal is to reduce the ammonia content to below 0.5%. Two methods are proposed: 1) distillation to remove over 99% of ammonia but with 10% ethanol loss, and 2) using a bubble bed and activated carbon to reduce ammonia to around 1% while retaining 96% of ethanol. Both methods aim to reuse over 85% of the ethanol, a major material cost. Future work includes economic analysis and accurately measuring residual ammonia levels to optimize the process.
1. Salvaging Ethanol from a Stober
Process Waste Stream
May 27th, 2016
Project Manager: Robin Ihnfeldt
Group 09:
Alan Tam
Reiko Liu
Joseph Guarnes
Melissa Nguyen
2. Project Statement
Stober Reaction: Si(OC2H5)4 + 2 H2O → SiO2 + 4 C2H5OH
90% Ethanol
<2% Water
<2% Ammonium Hydroxide
<1% TEOS &
Organics/Alcohols
GOAL: < 0.50% NH3
★ ~85% of the material cost
accounts for ethanol
3. 1.Distillation Column
< 99% NH3 removal
10% EtOH Loss
3% Water
< 0.1% NH3 left
96% EtOH
~ 3% Water
T = 31 oC
P = 1.2 atm
T = 78 oC
P = > 1 atm
EtOH 95%
Water 3%
NH3 2%
T = 25 oC
P = 1 atm
7. Cost and Material for Bubble Bed & Carbon Bed
➢Plexiglass
➢Temperature (28oC, 40oC)
➢Observe the bubble formation for
future adjustment
➢Simple Design and Construction
➢Activated Carbon $8.70/kg of C
Estimated Cost = < $10,000
9. Environmental Impact
1. Incineration 2. Repurpose
for fuel
3. Repurpose for
fertilizer
Potential
Impact
I M I x
M
I M I x
M
I M I x M
Noise 2 2 4 2 1 2 2 1 2
Odor 2 2 4 2 2 4 2 1 2
Air
pollution
4 3 12 4 3 12 4 2 8
Water
pollution
5 1 5 5 1 5 5 2 10
Land
pollution
3 0 0 3 0 0 3 1 3
Totals 25 23 25
10. Future Work & Recommendations
➢Cost & Economic Analysis
➢Find a method to accurately
determine the amount of NH3 left in
the solution
Stober silica reaction is a nanoparticle production process that creates silica nano-particles of various diameters. Since approximately 85% of the material cost accounts for ethanol, In this project, we aim to recycle the ethanol from the waste stream to lower the material cost. The main goal is to get less than 0.5% ammonia in waste stream. The waste stream has a PH value of 11 so the equilibrium reaction of the ammonium hydroxide is favo ammonia gas. The main challenge is to make lowest possible of ammonia percentage, and final cost of ethanol to be lower than cost of raw ethanol.
Hello, my name is Melissa and I will be talking about our second option to remove the ammonia from the ethanol solution. First we would send the waste stream through our bubble bed. This process would remove approximately 99% of the ammonia in the stream. The last 1% of Ammonia can then be removed by using a carbon bed. The activated carbon can remove approximately 60% of the remanding NH3. This brings our final ethanol solution with less than 0.5% of ammonia.
How does a bubble bed work? There is a feed stream of air to provide air bubbles, the column is operated at 28oC, just slightly above the boiling point of ammonium hydroxide. The bubble promotes mixing and help to carry the ammonia gas out of the system.
The carbon bed operates at 40oC because this is the best temperature for carbon to adsorb ammonia molecules.
More information on the bubble bed. Since the bubble size and the contact time of the bubble are two important parameters for the bubble bed to remove the ammonia. After doing some calculation, we chose our bubble size to be 0.5 cm, with contact time of 10s, since this would give us sufficient mass transfer of ammonia gas from the solution to the air bubble. The bubble distributor has the orifice size of 4mm, this is the distance between the orifices where the bubbles can be formed.
As we can see that the operating temperatures of the bubble bed and carbon bed are relatively low, using metals would essentially lead to heat loss of the process. Therefore, we are considering using plexiglass as the material for the columns. As the amount of ammonia gas is low, not much vapor are created and therefore pressure is not as big of a concern. The activated carbon is $8.7 per kg. The construction of the bubble bed and carbon bed can be easily machined at a low price. Our estimated cost of bubble bed and carbon bed is $10,000 which is cheaper than the distillation column.
So for safety, there isn’t too much concern.
Here’s our Piping and Instrumentation diagram. I’m not going to go through all of this but I’ll discuss our thought process.
First off, We’re working with a fairly small scale process.
The process would be contained inside a lab.
Also, we’re only dealing with temperatures ranging from room temp to 40 deg C.
As for pressures, everything is around atmospheric (p).
The main hazard would be an ammonia or ethanol leak,
so we set up multiple flow and level controllers throughout the system.
Environmental impact analysis showed that there isn’t too much of a concern.
Location: labratory in the Soriento Valley area.
Construction/operation poses nearly no impact since the process is so small.
The main impact would come from the disposal of our final waste stream.
We analyzed these three options. They all have their pros and cons
according to this chart, we estimate that it would be best to sell our process waste to a third party as a fuel.