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    • 9. 发明授权
    • Process for the production of di-trimethylolpropane
    • 二羟甲基丙烷生产工艺
    • US5324863A
    • 1994-06-28
    • US30020
    • 1993-03-24
    • Carl-Axel SjogreenGoran Axelsson
    • Carl-Axel SjogreenGoran Axelsson
    • C07B61/00C07C41/09C07C41/14C07C41/42C07C43/10C07C43/13C07C67/29C07C67/54C07C69/12C07C69/21
    • C07C41/09C07C67/08C07C67/28
    • Process for the production of di-trimethylolpropane (di-TMP), which comprises subjecting a solution containing less than 3 per cent by weight, preferably less than 1 per cent by weight of water, free trimethylolpropane (TMP) and/or partial ester between TMP and a monocarboxylic acid or its anhydride having 1-4 carbon atoms in the chain, which partial ester on average contains 1.0-2.5, preferably 1.0-2.0 ester groups per molecule to an etherification reaction by heating to 50.degree.-200.degree. C., preferably 70.degree.-190.degree. C. in the presence of an acid catalyst in solid state or in dissolved state until at most 30%, preferably at most 15% of the total content of free TMP and partial ester of TMP in the solution has been etherified to free di-TMP and partial ester of di-TMP respectively, at the same time continuously removing etherification water formed at the etherification reaction under vacuum at a pressure of 0.1-200 mm Hg, preferably 0.1-50 mm Hg or by an azeotropic distillation by means of a compound such as hexane, toluene, xylene or the like forming an azeotropic mixture, and recovering free di-TMP and di-TMP bonded as a partial ester respectively from the reaction mixture in a suitable way.
    • PCT No.PCT / SE91 / 00589。 371日期1993年3月24日 102(e)1993年3月24日PCT 1991年9月9日PCT公布。 公开号WO91 / 10633 日期:1991年7月25日。用于生产二 - 三羟甲基丙烷(二-TMP)的方法,其包括使含有少于3重量%,优选小于1重量%水的溶液,游离的三羟甲基丙烷(TMP )和/或TMP与单羧酸或其酸酐在链中具有1-4个碳原子的部分酯,该偏酯平均每分子含有1.0-2.5,优选1.0-2.0个酯基,通过加热至 50℃-200℃,优选70℃-190℃,在酸性催化剂存在下,以固态或溶解状态,直至游离TMP和部分的总含量的至多30%,优选至多15% 已经将溶液中的TMP酯醚化以分别释放di-TMP和di-TMP的部分酯,同时在0.1-200mm Hg,优选0.1的压力下,在真空下连续除去醚化反应生成的醚化水 -50 mm Hg或共沸d 通过形成共沸混合物的己烷,甲苯,二甲苯等化合物进行蒸馏,分别以合适的方式从反应混合物中回收作为偏酯结合的游离二-TMP和二-TMP。