Process for the purification of MDA
    1.
    发明授权
    Process for the purification of MDA 失效
    纯化MDA的方法

    公开(公告)号:US4028361A

    公开(公告)日:1977-06-07

    申请号:US605751

    申请日:1975-08-18

    IPC分类号: C07C85/16

    CPC分类号: C07C209/78

    摘要: A process is described for the selective removal of 2,2'- and 2,4'-diaminodiphenylmethane from mixtures thereof with the corresponding 4,4'-isomer by heating the mixture of isomers in the presence of a 1,3,5-tri-arylhexahydro-1,3,5-triazine and a catalyst (aqueous mineral acid). The process is particularly useful in facilitating the isolation of substantially pure 4,4'-isomer from the aniline-formaldehyde condensation. The pure 4,4'-isomer is a valuable intermediate for polyamides as well as for the corresponding diisocyanate. The by-products of the reaction are oligomeric polymethylene polyphenyl polyamines which are also useful as curing agents and intermediates for polymethylene polyphenyl polyisocyanates and the like.

    摘要翻译: 描述了一种方法,用于通过在存在1,3,5-三氯苯的情况下加热异构体的混合物,从相应的4,4'-异构体的混合物中选择性除去2,2'-和2,4'-二氨基二苯基甲烷, 三芳基六氢-1,3,5-三嗪和催化剂(无机酸水溶液)。 该方法特别可用于促进基本上纯的4,4'-异构体与苯胺 - 甲醛缩合物的分离。 纯4,4'-异构体是聚酰胺以及相应的二异氰酸酯的有价值的中间体。 反应的副产物是低聚多亚甲基多苯基多胺,其也可用作聚亚甲基多苯基多异氰酸酯等的固化剂和中间体。

    Process for the preparation of di(amino phenyl)methanes
    2.
    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。

    Phenylcyclohexane formed by cracking dicyclohexylbenzene
    3.
    发明授权
    Phenylcyclohexane formed by cracking dicyclohexylbenzene 失效
    二环己基苯形成的苯基环己烷

    公开(公告)号:US3984490A

    公开(公告)日:1976-10-05

    申请号:US575607

    申请日:1975-05-08

    摘要: A process is described for recovering phenylcyclohexane as principal product from dicyclohexylbenzenes by heating the latter in the presence of at least an equal amount by weight of benzene and an acid clay or zeolite catalyst at a temperature of 190.degree. - 400.degree.C. The period of heating is preferably controlled so that no significant cracking of the phenylcyclohexane is caused. The process is a useful adjunct to the known methods of production of phenylcyclohexane by hydrodimerization by benzene. The latter process gives significant amounts of dicyclohexylbenzenes as by-product. The present process enables this generally undesirable by-product to be converted to phenylcyclohexane thus increasing the overall yield of phenylcyclohexane from benzene in the hydrodimerization process.

    摘要翻译: 描述了一种通过在至少相当量的苯和酸性粘土或沸石催化剂存在下在190-400℃的温度下加热后者,从二环己基苯中回收苯基环己烷作为主要产物的方法。 优选控制加热,使得不会引起苯基环己烷的显着裂化。 该方法是通过苯的氢化二聚制备苯基环己烷的已知方法的有用辅助物。 后一种方法产生大量的二环己基苯作为副产物。 本方法使得这种普遍不希望的副产物转化为苯基环己烷,从而在加氢二聚过程中从苯增加了苯基环己烷的总产率。

    Bituminous composition
    4.
    发明授权
    Bituminous composition 失效
    BITUMINOUS组合物

    公开(公告)号:US4032355A

    公开(公告)日:1977-06-28

    申请号:US631823

    申请日:1975-11-14

    IPC分类号: C08K5/17 C08K5/18 C08L95/00

    CPC分类号: C08K5/17 C08K5/18 C08K5/29

    摘要: Novel bituminous compositions are disclosed which are characterized by elevated Ring and Ball softening points ranging up to about 200.degree. C. They are prepared by the treatment of molten bitumen, in the absence of solvent, with a combination of: (a) an amine selected from the class consisting of an aliphatic amine having from 10 to 20 carbon atoms, and aromatic polyamines; and (b) an isocyanate selected from the class consisting of aliphatic isocyanates having from 10 to 20 carbon atoms, and aromatic polyisocyanates; provided that in any instance in which the amine component is aliphatic, then the isocyanate component is aromatic. The combined weight of (a) and (b) present in the bitumen, is from about 1 to about 10 weight percent based on the weight of bitumen. The bituminous compositions are useful in paving, and roofing applications, especially in countries which experience hot climates.

    Novel polyisocyanate trimerization catalyst
    5.
    发明授权
    Novel polyisocyanate trimerization catalyst 失效
    新型聚异氰酸酯三聚催化剂

    公开(公告)号:US3986991A

    公开(公告)日:1976-10-19

    申请号:US584743

    申请日:1975-06-09

    IPC分类号: C08G18/09 C08G18/18

    摘要: A novel catalyst combination for the trimerization of polyisocyanates to polyisocyanurates is disclosed. The catalyst combination comprises (i) a tertiary amine trimerization catalyst containing a dimethylamino moiety, (ii) an alkali metal salt of an N-(2-hydroxyphenyl)methyl glycine, and (iii) a monomeric epoxide. The use of these catalysts in the preparation of polyisocyanurate foams results in facile machine preparation of bun stock foam without incurring the processing problems that arise from the prior art method. The polyisocyanurate foams produced using the novel catalyst combination of the invention are characterized by a reduced level of smoke generated on combustion.

    Process for preparing di(aminophenyl)methanes
    6.
    发明授权
    Process for preparing di(aminophenyl)methanes 失效
    制备二(氨基苯基)甲烷的方法

    公开(公告)号:US4039580A

    公开(公告)日:1977-08-02

    申请号:US598794

    申请日:1975-07-24

    CPC分类号: C08G18/7664

    摘要: A process is described for the preparation of polymethylene polyphenyl polyamines containing from 40 to 60 percent by weight of diamine and also containing markedly less high molecular weight polyamines than products hitherto available. Phosgenation of the polyamines gives the corresponding mixture of polymethylene polyphenyl polyisocyanates of markedly lower viscosity and lighter color than products hitherto available, and yielding polymer foams which are substantially white in color.The process comprises condensing aniline and formaldehyde (molar ratio 4-10:1) in the absence of catalyst, separating water from the resulting aminal mixture, contacting the aminals at 20.degree. C to 60.degree. C with a solid catalyst (diatomaceous earths, clays, zeolites) until formation of benzylamines is substantially complete, distilling aniline from the resulting benzylamines under reduced pressure and below 150.degree. C until the aniline content is 3 to 22 percent by weight, and contacting the resulting product with a solid catalyst (diatomaceous earths, clays, zeolites) at 100.degree. C to 190.degree. C until conversion to polymethylene polyphenyl polyamines is complete.

    摘要翻译: 描述了一种制备含有40至60重量%二胺的聚亚甲基多苯基多胺的方法,并且与目前可获得的产品相比,含有显着较少的高分子量多胺。 多胺的光气化产生与目前可获得的产品相比显着低粘度和较浅颜色的聚亚甲基多苯基多异氰酸酯的相应混合物,并产生基本上为白色的聚合物泡沫。

    Cellular isocyanurate polymer
    7.
    发明授权
    Cellular isocyanurate polymer 失效
    蜂窝状异氰脲酸酯聚合物

    公开(公告)号:US4039487A

    公开(公告)日:1977-08-02

    申请号:US650453

    申请日:1976-01-19

    摘要: Polyisocyanurate foams are disclosed which are characterized by low Flame Spread Ratings and low smoke generation values, as determined by the Underwriter's Laboratory Tunnel Test in accordance with the ASTM E-84 test procedure. The smoke and flame resistant properties are achieved, not through the use of flame retardants or additives, but rather by the use of a minor amount of a hydroxyl terminated aromatic polyester having a hydroxyl equivalent weight from about 150 to about 500 and which is the product of the reaction of an excess of a polyethyleneglycol having an equivalent weight from about 75 to about 225, with an aromatic polycarboxylic compound.

    摘要翻译: 公开了聚异氰脲酸酯泡沫,其特征在于根据ASTM E-84测试程序,由Underwriter's Laboratory Tunnel Test确定的低火焰蔓延等级和低烟雾产生值。 烟气和阻燃性能不是通过使用阻燃剂或添加剂而是通过使用少量羟基当量重量为约150至约500的羟基封端的芳族聚酯而得到的,并且是产物 过量的当量为约75至约225的聚乙二醇与芳族多元羧酸化合物的反应。

    Polymethylene polyphenyl polyisocyanate
    9.
    发明授权
    Polymethylene polyphenyl polyisocyanate 失效
    聚亚甲基多苯基多异氰酸酯

    公开(公告)号:US4092343A

    公开(公告)日:1978-05-30

    申请号:US797545

    申请日:1977-05-16

    CPC分类号: C08G18/7664

    摘要: A process is described for the preparation of polymethylene polyphenyl polyamines containing from 40 to 60 percent by weight of diamine and also containing markedly less high molecular weight polyamines than products hitherto available. Phosgenation of the polyamines gives the corresponding mixture of polymethylene polyphenyl polyisocyanates of markedly lower viscosity and lighter color than products hitherto available, and yielding polymer foams which are substantially white in color.The process comprises condensing aniline and formaldehyde (molar ratio 4-10:1) in the absence of catalyst, separating water from the resulting aminal mixture, contacting the aminals at 20.degree. C to 60.degree. C with a solid catalyst (diatomaceous earths, clays, zeolites) until formation of benzylamines is substantially complete, distilling aniline from the resulting benzylamines under reduced pressure and below 150.degree. C until the aniline content is 3 to 22 percent by weight, and contacting the resulting product with a solid catalyst (diatomaceous earths, clays, zeolites) at 100.degree. C to 190.degree. C until conversion to polymethylene polyphenyl polyamines is complete.

    摘要翻译: 描述了一种制备含有40至60重量%二胺的聚亚甲基多苯基多胺的方法,并且与目前可获得的产品相比,含有显着较少的高分子量多胺。 多胺的光气化产生与目前可获得的产品相比显着低粘度和较浅颜色的聚亚甲基多苯基多异氰酸酯的相应混合物,并产生基本上为白色的聚合物泡沫。

    Purification process for MDA
    10.
    发明授权
    Purification process for MDA 失效
    MDA的净化过程

    公开(公告)号:US4029705A

    公开(公告)日:1977-06-14

    申请号:US605753

    申请日:1975-08-18

    IPC分类号: C07C85/16

    CPC分类号: C07C209/78

    摘要: A process is described for the selective removal of 2,2'- and 2,4'-diaminodiphenylmethanes from mixtures containing 2,2'-, 2,4'- and 4,4'-diaminodiphenylmethanes and polyamines by heating these mixtures in the presence of aqueous hydrochloric acid (55 to 95 percent by equivalents based on the total amine in the starting material) and formaldehyde. The process is particularly useful to facilitate the isolation of substantially pure 4,4'-isomer from aniline-formaldehyde condensation products. The pure 4,4'-isomer is a valuable intermediate for polyamides as well as for the corresponding diisocyanate. The by-products of the reaction are oligomeric polymethylene polyphenyl polyamines which are also useful as curing agents and intermediates for polymethylene polyphenyl polyisocyanates and the like.

    摘要翻译: 描述了从含有2,2'-,2,4'-和4,4'-二氨基二苯基甲烷和多胺的混合物中选择性除去2,2'-和2,4'-二氨基二苯基甲烷的方法,通过加热这些混合物 存在盐酸水溶液(相对于原料中的总胺为55〜95%当量)和甲醛。 该方法特别有助于从苯胺 - 甲醛缩合产物中分离基本上纯的4,4'-异构体。 纯4,4'-异构体是聚酰胺以及相应的二异氰酸酯的有价值的中间体。 反应的副产物是低聚多亚甲基多苯基多胺,其也可用作聚亚甲基多苯基多异氰酸酯等的固化剂和中间体。