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    • 5. 发明申请
    • IMPROVED OXIDATION PROCESS
    • 改进氧化工艺
    • WO1996038402A1
    • 1996-12-05
    • PCT/US1996009173
    • 1996-05-31
    • KIELY, DonaldCARTER, AndySHROUT, David
    • C07C51/16
    • C07C51/316C07C59/105
    • Rapid temperature rises which characterize carbohydrate - nitric acid oxidation reactions used to form carbohydrate-derived acids may be moderated and temperature control readily maintained by blowing a gas such as air, oxygen, nitrogen or the like into the reaction mixture as needed to control the temperature of the reaction. The more moderate reaction conditions afford higher yield of the desired product with a concomitant reduction of by-products which may be difficult to remove and usually are unwanted as well. Upon completion the oxidation mixture is made basic (e.g. with an alkali metal base hydroxide or carbonate, ammonia or an amine) to a pH at which the carboxyl group or groups of the product carbohydrate-derived acid are entirely in the salt form. The aqueous solution is then passed through an ion retardation resin column to recover the carbohydrate-derived salt, using water as the eluent. If desired, the carbohydrate-derived acid salt may then be recovered easily by removal of solvent water or by precipitation by addition of a water-miscible organic compound such as methanol, ethanol acetone, isopropanol, etc.
    • 表征用于形成碳水化合物衍生的酸的碳水化合物 - 硝酸氧化反应的快速温度升高可以是缓和的,并且根据需要通过将气体如空气,氧气,氮气等吹入反应混合物来容易地维持温度控制,以控制温度 的反应。 更温和的反应条件提供了所需产物的较高产率,同时还原副产物,这可能难以除去并且通常也是不希望的。 完成后,将氧化混合物制成碱性(例如用碱金属碱性氢氧化物或碳酸盐,氨或胺)至产物碳水化合物衍生的酸的羧基或基团完全为盐形式的pH。 然后将水溶液通过离子延迟树脂柱,以水作为洗脱液回收碳水化合物衍生的盐。 如果需要,可以通过除去溶剂水或通过加入水混溶性有机化合物如甲醇,乙醇丙酮,异丙醇等容易地回收碳水化合物衍生的酸盐。