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1.发明授权
公开(公告)号：US3969465A
公开(公告)日：1976-07-13
申请号：US524492
申请日：1974-11-18
摘要： Waste salt solution from cyclohexanone manufacture is acidulated in a neutralizer, after which the organic phase is separated and subjected to a counter-current extraction with a saturated aqueous solution of mostly monocarboxylic acids separated from a later stage of the process. The watery extract carries off sodium sulphate that would otherwise interfere with further refining and this extract is then returned to the neutralizing vessel where the waste salt solutions are being acidulated, thereby reducing the need for externally supplied water to keep sodium sulphate from precipitating in the neutralizer and also enabling the dissolved monocarboxylic acids to be recovered. The organic phase leaving the counter-current extractor then goes to a flash evaporator in a condition now free of sodium sulphate, so that the evaporator may continuously remove water and monocarboxylic acids, which are then condensed and separated, with the water phase going back to the extractor as previously mentioned. The outputs are a mixture of monocarboxylic acids from the last separator and a mixture of dicarboxylic acids and hydroxy acids from the liquid coming out of the evaporator.
摘要翻译： 将环己酮制造的废盐溶液在中和剂中酸化，然后分离有机相，并用大部分单羧酸的饱和水溶液与该方法的后期分离进行逆流萃取。 水性提取物会运送硫酸钠，否则会干扰进一步的澄清，然后将该提取物返回到中和容器中，其中废盐溶液被酸化，从而减少外部供应水的需要，以保持硫酸钠不会在中和剂中沉淀 并且还能够回收溶解的一元羧酸。 离开逆流萃取器的有机相然后以现在不含硫酸钠的状态进入闪蒸器，使得蒸发器可以连续地除去水和一元羧酸，然后水和一元羧酸被冷凝和分离，水相回到 提取器如前所述。 输出是来自最后一个分离器的单羧酸和来自蒸发器出来的液体的二羧酸和羟基酸的混合物的混合物。
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2.发明授权
公开(公告)号：US4052441A
公开(公告)日：1977-10-04
申请号：US620306
申请日：1975-10-07
CPC分类号： C07C51/43 , C07C51/493
摘要： After acidification and separation of a concentrated aqueous solution of sodium sulfate, the water-containing organic phase that remains is first distilled to remove mainly water, then chilled to crystallize out the bulk of the dicarboxy acids, then esterified and distilled again to obtain monocarboxy acid esters in distillate fractions, after which the residue is further esterified to facilitate obtaining the remaining dicarboxy acids in usable form.
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3.发明授权Water-compatible solvents for film-forming resins and resin solutions made therewith 失效用于成膜树脂的水相溶剂和由其制成的树脂溶液
公开(公告)号：US4005051A
公开(公告)日：1977-01-25
申请号：US520901
申请日：1974-11-04
CPC分类号： C09D7/001
摘要： The dimethyl ethers of succinic, glutaric and adipic acids show a great increase in their water miscibility when they are mixed with either 6-hydroxycaproic acid methyl ester, one or more of the glycol ethers, diglycol ethers and glycol ether acetates, or both 6-hydroxycaproic acid methyl ester and one or more of the glycol ethers, diglycol ethers and glycol ether acetates. These dimethyl esters are, accordingly, substituents for the glycol ether derivatives in water-miscible solvents for film-forming resins. They may provide up to 80% by weight of the non-water components of the solvent. They may be produced at the same time as the methyl ester of 6-hydroxycaproic acid in a single esterification step by esterifying a fraction of acids derived from the waste salt solutions of cyclohexanone manufacture, as described in a related application, Ser. No. 372,021, now U.S. Pat. No. 3,859,335.
摘要翻译： 当琥珀酸，戊二酸和己二酸的二甲醚与6-羟基己酸甲酯，一种或多种二醇醚，二甘醇醚和二醇醚乙酸酯混合时，它们的水混溶性显着增加， 羟基己酸甲酯和一种或多种二醇醚，二甘醇醚和乙二醇醚乙酸酯。 因此，这些二甲基酯是用于成膜树脂的水混溶性溶剂中的二醇醚衍生物的取代基。 它们可以提供高达80重量％的非水组分的溶剂。 它们可以在单一酯化步骤中与6-羟基己酸的甲酯同时生产，通过酯化源自环己酮制造的废盐溶液的一部分酸，如相关申请中所述。 现在的美国专利号为372,021。 3,859,335。
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4.发明授权
公开(公告)号：US3993691A
公开(公告)日：1976-11-23
申请号：US516658
申请日：1974-10-21
IPC分类号： C07C69/00 , C07C51/00 , C07C53/00 , C07C55/02 , C07C59/01 , C07C67/00 , C07C67/08 , C07C59/04
摘要： In a process for producing esters of carboxylic acids from the waste salt solutions derived from the manufacture of cyclohexanone, the mixture of organic acids obtained by acidulation with a strong acid and separation of an inorganic salt solution is refined to separate the monocarboxylic acids from the hydroxycarboxylic and dicarboxylic acids by a three-stage distillation at a temperature lower than 120.degree. C. The first stage is performed at a moderate vacuum, the second stage at a higher vacuum and the third stage is a steam distillation stage at a moderate vacuum, with the steam requirements reduced by returning to the evaporator an aqueous phase that is readily separated from the distillate. The use of steam in this manner only in the third stage reduces the steam requirements to economic proportions. More than 99% of the monocarboxylic acids may be separated from the other carboxylic acids in this fashion.
摘要翻译： 在由制备环己酮得到的废盐溶液中生产羧酸酯的方法中，将通过酸强酸和无机盐溶液分离而获得的有机酸的混合物被精制以将一元羧酸与羟基羧酸分离 和二羧酸通过在低于120℃的温度下进行三级蒸馏。第一阶段在中等真空下进行，第二阶段在较高真空下进行，第三阶段是在中等真空下的蒸汽蒸馏阶段， 通过使蒸发器返回到容易与馏出物分离的水相，蒸汽需求降低。 以这种方式仅在第三阶段使用蒸汽将蒸汽需求降低到经济比例。 可以以这种方式将99％以上的单羧酸与其它羧酸分离。
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