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    • 1. 发明授权
    • Process for the isolation of crystalline 1,3-cylohexanedione
    • 分离结晶1,3-环己二酮的方法
    • US4487971A
    • 1984-12-11
    • US537648
    • 1983-09-30
    • Heinz LittererHelmut Meidert
    • Heinz LittererHelmut Meidert
    • C07C45/45C07C45/81C07C45/83C07D309/32C07D315/00
    • C07D315/00C07C45/455C07C45/81C07C45/83C07D309/32
    • The invention provides a process for the isolation of crystalline 1,3-cyclohexanedione from the crude product formed in the catalytic gaseous phase cyclization of 5-oxohexanoic acid. Before or directly after condensation an auxiliary component consisting of at least one compound selected from the group consisting of cyclic hydrocarbons, chlorinated aliphatic hydrocarbons and monoethers is added to the crude product, subsequently the mixture of crude product and auxiliary component is distilled under normal or reduced pressure until the reaction water is removed and the residual content of auxiliary component in the remaining concentrate has attained a defined value, and the precipitated crystalline 1,3-cyclohexanedione is filtered off. Alternatively, the auxiliary component added may be distilled off substantially completely. In this case, either the same or another of the compounds or compound mixtures indicated as auxiliary component must be added subsequently to the remaining concentrate interspersed with crystals in order to obtain a substantially complete precipitation of the 1,3-cyclohexanedione in the form of crystals and formation of a filterable crystal pulp.Alternatively, the crude product may be heated after condensation and the crude crystallized product obtained optionally after cooling be mixed with the auxiliary component. The further work-up is as described above.
    • 本发明提供了从在5-氧代己酸的催化气相环化中形成的粗产物中分离结晶1,3-环己二酮的方法。 在冷凝前或直接冷凝后,将由至少一种选自环状烃,氯化脂肪烃和单醚的化合物组成的辅助成分加入到粗产物中,随后将粗产物和辅助成分的混合物在正常或还原 直到反应水被除去并且剩余浓缩物中的辅助组分的残余含量达到规定值,并且滤出沉淀的结晶1,3-环己二酮。 或者,可以基本上完​​全蒸馏除去所添加的辅助成分。 在这种情况下,作为辅助成分指示的相同或另一种化合物或化合物混合物必须随后添加到散布有晶体的剩余浓缩物中,以获得晶体形式的1,3-环己二酮的基本上完全的沉淀 并形成可过滤的水晶纸浆。 或者,粗产物可以在冷凝后加热,并且任选地在冷却后获得的粗结晶产物与辅助组分混合。 进一步的后处理如上所述。
    • 7. 发明授权
    • Process for preparing p-chlorotoluene and/or m-chlorotoluene
    • 制备对氯甲苯和/或间氯甲苯的方法
    • US4650915A
    • 1987-03-17
    • US764511
    • 1985-08-09
    • Hans-Jurgen ArpeHeinz LittererNorbert Mayer
    • Hans-Jurgen ArpeHeinz LittererNorbert Mayer
    • B01J20/18B01J23/00B01J29/08B01J29/18B01J29/40B01J29/70C07B61/00C07C17/00C07C17/12C07C17/358C07C17/38C07C17/389C07C17/395C07C25/02C07C67/00
    • C07C25/02C07C17/358C07C17/389
    • The invention relates to a process for preparing p-chlorotoluene and/or m-chlorotoluene by ring-chlorination of toluene by using the following two pages (a) and (b) when further processing the toluene chlorination product composed of mixed isomers:(a) Isolation of p-chlorotoluene from a mixture of o-, m- and p-chlorotoluene by selective adsorption of p-chlorotoluene onto a mesoporous or macroporous zeolite and subsequent desorption of p-chlorotoluene(b) Treatment of an o-chlorotoluene-rich mixture of isomers with an isomerization catalyst.For the exclusive preparation of p-chlorotoluene first p-chlorotoluene is isolated and removed from the toluene chlorination product in stage (a). The remaining mixed isomers are then treated in stage (b) to increase their content of m- and p-isomers and then returned into stage (a).For the preparation of m-chlorotoluene and, if appropriate, additionally of p-chlorotoluene first the toluene chlorination product is treated in stage (b) to increase its content of m- and, if appropriate, p-isomer. p-Chlorotoluene is then isolated in stage (a) and returned to stage (b), or, if appropriate, removed. The remaining mixture essentially comprising o- and m-isomers is separated by distillation or adsorption and o-chlorotoluene is then returned into stage (b) and m-chlorotoluene is removed.
    • 本发明涉及通过使用以下两页(a)和(b)进一步处理由混合异构体组成的甲苯氯化产物时,通过甲苯的环氯化来制备对氯甲苯和/或间氯甲苯的方法:(a )通过将对氯甲苯选择性吸附到介孔或大孔沸石上并随后对对氯甲苯的解吸,从邻 - ,间 - 和对 - 氯甲苯的混合物中分离对氯甲苯(b)处理富含邻氯甲苯 异构体与异构化催化剂的混合物。 对于专门制备对氯甲苯,首先在阶段(a)中从甲苯氯化产物中分离并除去对氯甲苯。 然后在阶段(b)中处理剩余的混合异构体以增加它们的m-和p-异构体的含量,然后返回到阶段(a)。 为了制备间氯甲苯,并且如果合适,另外还加入对氯甲苯,在步骤(b)中处理甲苯氯化产物,以增加其含量,如果合适,增加对异构体。 然后在阶段(a)中分离出对 - 氯甲苯并返回到阶段(b),或者如果合适的话除去。 通过蒸馏或吸附分离基本上含有O-和m-异构体的剩余混合物,然后将邻氯甲苯回到步骤(b)中,并除去间氯甲苯。