Process for the preparation of polyamines
    47.
    发明授权
    Process for the preparation of polyamines 失效
    制备多胺的方法

    公开(公告)号:US4147724A

    公开(公告)日:1979-04-03

    申请号:US751625

    申请日:1976-12-17

    摘要: This invention relates to a new and improved process for the preparation of polyamines based on diphenylmethane by acid condensation of aromatic amines with formaldehyde followed by processing of the condensation mixture. Compared with similar processes known in the art, the process according to the invention combines the advantage of requiring less distillation for processing the reaction mixture with the advantage of a wide scope for variation of the composition of the product finally obtained, particularly with regard to its concentration of 2,4'-isomers and greatly reduced concentration of 2,2'-isomers. More particularly, the instant invention is directed to a process for the preparation of multinuclear aromatic polyamines by condensation of aromatic amines with formaldehyde in the presence of aqueous acid catalysts in a condensation reaction carried out in at least two stages, followed by neutralization of the catalyst and recovery of aromatic polyamines characterized in that free amine is removed from the condensation reaction mixture by means of a hydrophobic solvent after the first condensation stage and before the final condensation stage, and the amine thus removed is returned to the aqueous, catalyst-containing phase by returning the resulting amine-containing solvent phase to said aqueous phase before the first condensation stage.

    摘要翻译: 本发明涉及通过芳族胺与甲醛的酸缩合,然后加工缩合混合物制备基于二苯基甲烷的多胺的新的和改进的方法。 与本领域已知的类似方法相比,根据本发明的方法结合了需要较少蒸馏以处理反应混合物的优点,其优点在于最终获得的产物组成变化的范围广泛,特别是关于其 浓度为2,4'-异构体并大大降低了2,2'-异构体的浓度。 更具体地说,本发明涉及一种制备多核芳族多胺的方法,该方法是在含水酸性催化剂的存在下,在至少两个阶段进行的缩合反应中,将芳族胺与甲醛缩合,然后中和催化剂 芳族多胺的回收,其特征在于在第一缩合阶段之后和最后的冷凝阶段之前借助于疏水性溶剂从缩合反应混合物中除去游离胺,并且将这样除去的胺返回到含水催化剂的相 通过在第一冷凝阶段之前将所得含胺溶剂相返回所述水相。

    Process for the preparation of di(amino phenyl)methanes
    48.
    发明授权
    Process for the preparation of di(amino phenyl)methanes 失效
    制备二(氨基苯基)甲烷的方法

    公开(公告)号:US4039581A

    公开(公告)日:1977-08-02

    申请号:US590801

    申请日:1975-06-27

    摘要: Aniline and formaldehyde are condensed (2-10 moles aniline per mole of formaldehyde) at ambient temperature in the absence of acid catalysts to give a mixture of aminals (anilinoacetals) and aniline from which the water is removed. The anhydrous aminals are contacted with a solid catalyst (clays, zeolites, diatomaceous earth) using either batch or continuous operation initially at 20.degree. C to 55.degree. C until benzylamine formation is substantially complete, then at 50.degree. C to 65.degree. C until benzylamine conversion to methylene polyphenyl polyamines is 75 - 90% complete and finally at 80.degree. C to 100.degree. C. A polyamine mixture is obtained in which diaminodiphenylmethane is the major (order of 90 percent by weight or higher) component, the bulk of the higher oligomeric polyamines being triamine. The diaminodiphenylmethane component contains of the order of 85 percent of 4,4'-isomer, the rest being 2,4'-isomer except for very small amounts (order of 2 percent or less) of 2,2'-isomer.Advantages of the process include high yield of diaminodiphenylmethane with relatively high 4,4'-isomer content, low oligomeric polyamine content, low temperature operation (energy consumption lower), no acidic reactants to cause corrosion of equipment, and rapid rates of conversion.

    摘要翻译: 在不存在酸催化剂的情况下,在环境温度下,苯胺和甲醛缩合(每摩尔甲醛为2-10摩尔苯胺),得到除去水的胺(苯胺基缩醛)和苯胺的混合物。 使用间歇或连续操作,在20℃至55℃下使无水胺与固体催化剂(粘土,沸石,硅藻土)接触,直到苄胺形成基本完成,然后在50℃至65℃下直至苄胺 转化为亚甲基多苯基多胺的组合物为75-90%,最后在80℃至100℃。得到多胺混合物,其中二氨基二苯基甲烷为主要成分(90%重量或更高) 低聚多胺是三胺。 二氨基二苯基甲烷组分含有约为85%的4,4'-异构体,其余为2,4'-异构体,只是非常少量(2%或更低的量级)的2,2'-异构体。

    Polyamine curing agents for use in preparing polyurethane elastomers and foams
    49.
    发明授权
    Polyamine curing agents for use in preparing polyurethane elastomers and foams 失效
    聚氨酯固化剂用于制备聚氨酯弹性体和助磨剂

    公开(公告)号:US3563906A

    公开(公告)日:1971-02-16

    申请号:US3563906D

    申请日:1968-12-04

    申请人: DU PONT

    摘要: AMINE CURING AGENTS FOR LIQUID ISOCYANATO-TERMINATED POLYURETHANES OBTAINED BY CONDENSING A MONOAMINE COMPOSITION WITH FORMALDEHYDE IN THE PRESENCE OF A MINERAL ACID. THE MONOAMINE CAN BE 2-CHLOROANILINE OR MIXTURES OF 2-CHLOROANILINE WITH ANILINE AND/OR O-TOLUIDINE. THE PROPORTIONS OF REACTANTS ARE SELECTED TO PRODUCE CURING AGENTS WHICH HAVE MODERATE REACTIVITIES AND EXHIBIT A LIMITED TENDENCY TO CRYSTALLIZED UNDER NORMAL OPERATION CONDITIONS. THE AMINE COMPOSITIONS ARE PARTICULARLY USEFUL AS CURING AGENTS IN THE PREPARATION OF POLYURETHANE FOAMS. THE NEW COMPOUNDS, 3-CHLORO-4,4''-DIAMINODIPHENYLMETHANE AND 3-CHLORO-3''-METHYL-4,4''-DIAMINODIPHENYLMETHANE CAN BE OBTAINED FROM APPROPRIATE REACTION PRODUCTS.

    摘要翻译: 通过在无机酸存在下将单胺组合物与甲醛缩合而获得的聚氨酯泡沫和弹性体的胺固化剂。 单胺可以是2-氯苯胺或2-氯苯胺与苯胺和/或邻甲苯胺的混合物。 选择反应物的比例以产生具有中等反应性的固化剂,并且在正常操作条件下表现出有限的结晶倾向。 胺组合物在制备聚氨酯泡沫时特别可用作固化剂。 新化合物3-氯-4,4'-二氨基二苯基甲烷和3-氯-3'-甲基-4,4'-二氨基二苯基甲烷可以从合适的反应产物中获得。