Polyethylene from Ethanol/Manufacturing Instructions

Ethanol production

Ethanol can be purchased or produced on-site

Construction of fluid bed reactor

Instructions for construction of fluid bed reactor can be found on its own wikipage.

Ethanol dehydration catalyst preparation protocol

Base treated gamma aluminium oxide has been report to have 90%+ yields and 97%+ selectivity and could be a 1st generation catalyst.

Gamma aluminium oxide doped with Ti02 has been reported to have 99%+ yields and selectivity and has been shown to be superior to other metals.

"30 g g-Al2O3 powder with BET specific surface areas of 200 m2/g are diluted and mixed well with a small quantity of 0.5 mol/L Na2CO3 solution in a three-necked rounded-bottomed flask. Then, to the flask, and agitate well with a magnetic stirrer. Keep the pH of the solution at 7–8, and then the material is washed to eliminate (SO4)2 via a centrifugal machine, followed by dried at 110 8C for 8 h and calcined at 500 C for 4 h. Finally, the TiO2/g-Al2O3 catalysts with the size of 30–50 mesh are obtained after forming, crushing and sieving" Chen et al.

Protocol for preparation:

1. Combine 4 kg (approximately 1 l) g-Al2O3 with 5.0 l 0.5 mol/L Na2CO3 (264.9 g) solution in a three-necked rounded-bottomed flask.

2. Calculate 10% wt content for TiO2 and solve for titanium sulfate addition(4 kg * .1 = 400 g/79.8 g/mol TiO2 = 5.01 mol = 5.01 mol * Ti(SO4)2 240 g/mol = 1202.37 g Ti(SO4)2). Add 26.4 l 0.19 mol/L Ti(SO4)2 aqueous solution and 26.4 l 0.5 mol/L Na2CO3 solution are added simultaneously with high agitation. Maintain the solution between pH 7-8.

3. The sulfate precipitate is washed at 4000 g over to remove the sulfate solution. The solution is then dried at 110 for 8 hr and then calcined at 500 C for 4 hr.

4. The calcined catalyst is crushed and sieved through 30-50 mesh.

Prepare reagents

Dehydration reaction protocol

1. The reaction zone is filled with catalyst, sealed, and connected to the subsystems.

2. A temperature of 420 - 440 C is established by the heat jacket and a light nitrogen flow is maintained.

3. Ethanol is loaded into the vaporization chamber and heated to 200 C with a Liquid Hourly Space Velocity of 50-100 v/v/hr.

4. Gas products flow through the three temperature phase liquid condenser and liquid water is removed and gaseous ethylene stored.

Ethylene polymerization catalyst preparation

1. In a 5 liter flask combine anhydrous 41.8g (0.438 mol) MgCl2, in 2.5 l tetrahydrofuran (THF). Add 27.7 g (0.184 mol) TiCl4 in dropwise over 30 min with stir bar agitation. Add heat ~60 C for 30 min to completely dissolve TiCl4. THF 66 C boiling point

2. Dry 500 g silica at 800 C for 2 hr. Combine with 25 g TAE in 2 l THF at 60 C for 15 min. Dried activated silica at 65 C.

3. Impregnate support by combining 500 g porous silica with catalyst precursor mixture at 60 C. Dry the mixture at 60 C under N2 for 3-5 hr. Find method to control drying and ED content.

4. Prepare triethylaluminum in isopentane in 5-30% (v/v). Add to heated and loaded reactor.