日本農芸化学会誌
Online ISSN : 1883-6844
Print ISSN : 0002-1407
ISSN-L : 0002-1407
前スルフォン化エゾ松木粉のヒドロキシルアミン共存エタノリシス反應及びリグノオキシムスルフォン酸に就て
サルファイト蒸解の研究(第5報)
軒原 栄三
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ジャーナル フリー

1953 年 27 巻 1 号 p. 41-46

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Each 20g of presulphonated spruce wood meal (solid lignosulphonic acid; Klason lignin and sulphur content are 25.2% and 0.9%, respectively) was treated with 200 cc of 3% ethanolic HCl and 4.2g NH3OH•HCl in boiling water bath during 1.5_??_28 hrs. After 10_??_28 hrs., about 60% of lignin was dissolved. When ethanolic filtrates were introduced in 5l H2O, light yellow flocculent precipitates (α) were formed. By the continuous extractions of aqueous filtrates with ether and evaporation of ether, brown syrups (β) were obtained. Average -OCH3, nitrogen and sulphur contents of α (β) are 15.86, 1.82 and 1.66%respect-ively (13.85, 7.25 and 0.92%). Therefore, their mole ratio in a (β) is 5.1:1.3:0.5 (4.5:5.2:0.3).
From the results of the colorimetric determination of free NH2OH and oxime by Navak-Wilson's method [J. Bacteriology, 55, 517 (1948)], and of the potentiometric titrations of α, it is confirmed that nitrogen of α is oxime-form, and α is amphorite [HO3S-L(OCH3)7•(OC2H5)•(=NOH)2, isoelectric point: pH 4.5], having acidic (-SO3H) and basic groups (=NOH). Therefore, α (β) was designated, by the author, as α (β)-lignoximesulphonic acid. From results above mentioned, it is assumed that lignin molecule in presulphonated wood meal (solid lignosulphonic acid) has. carbonyl group and may be connecting with each other or with carbohydrate by means of acetal-linkage.
It is supposed that β is similar in reference to these charaters.

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