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    • 72. 发明授权
    • Polyisocyanates of the diphenyl methane series
    • 二苯甲烷系列的多异氰酸酯
    • US4613687A
    • 1986-09-23
    • US293748
    • 1981-08-17
    • Hartmut KnofelMichael Brockelt
    • Hartmut KnofelMichael Brockelt
    • C08G18/00C07C67/00C07C205/06C07C209/00C07C209/36C07C211/51C07C241/00C07C263/10C07C265/12C07C265/14C08G18/76C07C119/048
    • C07C265/12C07C205/06C07C209/36C08G18/7664
    • A polyisocyanate or mixture of polyisocyanates in which the main component(s) correspond to the formula: ##STR1## in which R.sub.1, R.sub.2, and R.sub.3 each represent hydrogen or a saturated alkyl group containing from 1 to 12 carbon atoms, provided that at least two of these radicals represent hydrogen; andm, n, o and p each represent 0 or 1, provided that when m, n, o and/or p represent 0, the free valency is taken up by a hydrogen atom and that the sum of m+n+o+p is greater than 1 on a statistical average.Such polyisocyanate or mixture of polyisocyanates may be produced by first reacting a 4-nitrobenzyl halide, a 3-nitrobenzyl halide, a benzyl halide, a benzyl alcohol or a nitrobenzyl chloride isomer mixture with nitrobenzene, an alkyl-substituted nitrobenzene, an alkyl benzene or benzene in the presence of a Friedel-Crafts or an acid catalyst. This reaction product is then nitrated, the nitro groups are converted to amino groups by reduction or hydrogenation and the amino compound(s) subsequently phosgenated to form the polyisocyanate(s). The purity of the product polyisocyanate may be improved by distilling off secondary products before and/or after the phosgenation.
    • 多异氰酸酯或多异氰酸酯的混合物,其中主要成分对应于下式:其中R 1,R 2和R 3各自表示氢或含有1至12个碳原子的饱和烷基,条件是至少 这些基团中的两个表示氢; 并且m,n,o和p各自表示0或1,条件是当m,n,o和/或p表示0时,游离的价态被氢原子吸收,并且m + n + o + 统计平均数p大于1。 这种多异氰酸酯或多异氰酸酯的混合物可以通过首先使4-硝基苄基卤,3-硝基苄基卤,苄基卤,苯甲醇或硝基苄基氯异构体混合物与硝基苯,烷基取代的硝基苯,烷基苯或 苯在Friedel-Crafts或酸催化剂存在下。 然后将该反应产物硝化,通过还原或氢化将硝基转化为氨基,随后将氨基化合物气化以形成多异氰酸酯。 产物多异氰酸酯的纯度可以通过在光气化之前和/或之后蒸馏二次产物来改善。
    • 76. 发明授权
    • Multiple-step process for the preparation of hexamethylene
diisocyanate-1,6 and/or isomeric aliphatic diisocyanates with six
carbon atoms in the alkylene residue
    • 用于制备在亚烷基残基中具有6个碳原子的六亚甲基二异氰酸酯-1,6-和/或异构脂族二异氰酸酯的多步法
    • US4596678A
    • 1986-06-24
    • US600143
    • 1984-04-13
    • Franz MergerFriedrich TowaeHans HellbachGunther IsbarnWaldemar Koehler
    • Franz MergerFriedrich TowaeHans HellbachGunther IsbarnWaldemar Koehler
    • C07C265/14C07C67/00C07C69/00C07C241/00C07C263/04C07C263/06C07C265/04
    • C07C263/04
    • Hexamethylene diisocyanate and/or isomeric alkylene diisocyanates having 6 carbon atoms in the alkylene radical, preferably 2-methylpentamethylene 1,5-diisocyanate and/or 2-ethyltetramethylene 1,4-diisocyanate are prepared without the use of phosgene in a multiple-step process by means of(a) reacting hexamethylene 1,6-diamine and/or isomeric alkylene diamines having 6 carbon atoms in the alkylene radical with urea and alcohol in the presence of dialkyl carbonate and/or carbamic acid alkyl ester as well as, in some cases, catalysts to form hexamethylene 1,6-dialkylurethane and/or isomeric alkylene dialkylurethanes having 6 carbon atoms in the alkylene radical,(b) separation and return to reaction step (a) of alcohol, dialkyl carbonate, and/or carbamic acid alkyl ester from the reaction mixture(c) evaporation of the hexamethylene 1,6-dialkylurethane and/or isomeric alkylene dialkylurethanes having 6 carbon atoms in the alkylene radical,(d) cleavage of the vaporized diurethanes into hexamethylene diisocyanate and/or isomeric alkylene diisocyanate having 6 carbon atoms in the alkylene radical and alcohol, and(e) fractional condensation of the cleavage products.
    • 在多步法中不使用光气制备在亚烷基中具有6个碳原子的六亚甲基二异氰酸酯和/或异构亚烷基二异氰酸酯,优选2-甲基五亚甲基-1,5-二异氰酸酯和/或2-乙基四亚甲基1,4-二异氰酸酯 通过(a)在碳酸二烷基酯和/或氨基甲酸烷基酯的存在下,使亚烷基中的六亚甲基1,6-二胺和/或具有6个碳原子的异构亚烷基二胺与脲和醇反应,以及在一些 情况下,在亚烷基中形成具有6个碳原子的六亚甲基1,6-二烷基氨基甲酸酯和/或异构亚烷基二烷基氨基甲酸酯的催化剂,(b)分离并返回到醇,碳酸二烷基酯和/或氨基甲酸烷基酯的反应步骤(a) (c)在亚烷基中蒸发具有6个碳原子的六亚甲基1,6-二烷基氨基甲酸酯和/或异构亚烷基二烷基氨基甲酸酯,(d)将汽化的二氨基甲酸酯裂解成h 亚烷基二异氰酸酯和/或亚烷基和醇中具有6个碳原子的异构亚烷基二异氰酸酯,和(e)裂解产物的分级缩合。