Methanol treated sludge

Isomerization processes produce sour water and caustic wastewater. The ether manufacturing process utilizes a water wash to extract methanol or ethanol from the reactor effluent stream. After the alcohol is separated, this water is recycled back to the system and is not released. In those cases where chloride catalyst activation agents are added, a caustic wash is used to neutralize any entrained hydrogen chloride. This process generates a caustic wash water that must be treated before being released. This process also produces a calcium chloride neutralization sludge that must be disposed of off-site. 

Samples of 1 gram of dried primary and dried wasted sludge were extracted in a Soxhlet extraction apparatus with 150 ml methanol for 4 hours. An aliquot of the methanol extract (20 ml out of a total volume of 200 ml) was passed over a small anion exchange column. The column was washed with 10 ml methanol before elution of the LAS with 3 ml of acidic methanol. The effluent was diluted to about 70 ml with water and the pH was adjusted to a value of 7. The solution was then brought to a value of 100 ml and an aliquot of 25 ml was passed over an octadecyl reversed phase SPE column. The sample was further treated as described above. The samples were kept in a dry state until analysis by HPLC. Prior to HPLC, the residues were dissolved in an acetonitrile/water 70/30 solvent mixture. 

Twenty grams of strychnine in 60 cc. of chloroform is shaken with oxygen (renewed daily) in the presence of a solution of 10 g. of copper sulfate in 80 cc. of water and 160 cc. of 1 Af ammonium hydroxide. On the seventh day the reaction mixture turns green and on the eleventh day a green sludge appears. The residue recovered from the chloroform layer is treated with sulfurous acid and ammonia and then taken up in chloroform. The residue from the second chloroform extract was crystallized from methanol when 9.6 g. of a solid melting at 160-165° is recovered. The undissolved resin from the crystallization, when dissolved in acid and decolorized, yields 0.7 g. of a solid (m.p. 215-245°) when precipitated with ammonia. 

Enerkem Pilot Canada Lignocellulosics, MSW, wood chips, treated wood, sludge, petroleum coke, spent plastics and wheat straw Ethanol, methanol, SNG Operational... 

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