Preparation of Lignoxime and its Composition

Studies on the Sulphite Cooking. Part 4

Abstract

One hundred g of, the extraction residue of spruce wood meal (with EtOH-C_??_H₃and hot water) was refluxed with the solution, which is composed of 1000 cc EtOH, 67.7g conc. HCl, 21g NH₂OH•HCl and 60 cc water, on the water bath during 20 hours. About 40% of lignin in the wood was removed in this process. When the filtrate and washings were poured into 5l H₂O, brownish yellow flocculent amorphous substance (α) was precipitated (5.7g). After (α) was filtered off, the filtrate was neutralized to pH 3.4, concentrated in vacuo at 55° and treated continuously with ether. Ether extraction after concentration left yellow syrup (β) (1.65g). From the determinations of OCH₃ and N contents of (α) and (β), it was concluded that (α) was lignoxime, having one N (i.e. one mole carbonyl group) vs. 3.5 lignin building stones, and (β) was low-molecular lignoxime, having one N vs. one lignin building stone.