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    • 5. 发明授权
    • Uretdione diisocyanates and a process for their production
    • 脲二异氰酸酯及其制备方法
    • US5750629A
    • 1998-05-12
    • US788726
    • 1997-01-23
    • Hans-Josef LaasReinhard HalpaapJosef PedainKlaus Konig
    • Hans-Josef LaasReinhard HalpaapJosef PedainKlaus Konig
    • B01D3/28B01J31/24C07B61/00C07D229/00C08G18/79C08G18/80C09D175/00C09D175/04
    • C08G18/8016C07D229/00C08G18/798
    • The present invention relates to a process for preparing pure bis(isocyanatoalkyl)monouretdiones corresponding to formula (I) ##STR1## wherein R represents identical or different, linear or branched alkyl groups having 4 to 9 carbon atoms, by oligomerizing at least a portion of the isocyanate groups of aliphatic diisocyanates in the presence of catalysts which accelerate the dimerization of isocyanate groups, terminating the reaction at the desired degree of oligomerization, removing unreacted excess diisocyanate by extraction or thin film distillation to obtain a distillation residue, subjecting the distillation residue to thin film distillation at a temperature of 160.degree. to 220.degree. C. and a pressure of 0.01 to 1.0 mbar and obtaining bis(isocyanato-alkyl)monouretdiones corresponding to formula (I) as the distillate. The present invention also relates to the resulting bis(isocyanato-alkyl)monouretdiones corresponding to formula I and to their use for the production of polyisocyanate addition products, in particular as the isocyanate components in polyurethane coatings compositions, in which the isocyanate groups may optionally be present in blocked form.
    • 本发明涉及一种制备对应于式(I)的纯双(异氰酸根合烷基)单脲基的方法,其中R表示相同或不同的具有4至9个碳原子的直链或支链烷基,至少通过低聚 一部分脂族二异氰酸酯的异氰酸酯基团在催化剂存在下加速异氰酸酯基团的二聚反应,以期望的低聚程度终止反应,通过萃取或薄膜蒸馏除去未反应的过量二异氰酸酯,得到蒸馏残渣, 蒸馏残渣,在160〜220℃的温度和0.01〜1.0mbar的压力下进行薄膜蒸馏,得到与式(I)相应的作为馏出物的双(异氰酸基 - 烷基)单脲。 本发明还涉及所得到的对应于式I的双(异氰酸根合 - 烷基)单脲基团,以及其用于制备多异氰酸酯加成产物的用途,特别是作为聚氨酯涂料组合物中的异氰酸酯组分,其中异氰酸酯基团可任选地为 以阻塞形式存在。
    • 6. 发明授权
    • Process for the preparation of alkoxytriazolinones
    • 制备烷氧基三唑啉酮的方法
    • US5710303A
    • 1998-01-20
    • US723706
    • 1996-09-30
    • Heinz-Jurgen WroblowskyKlaus Konig
    • Heinz-Jurgen WroblowskyKlaus Konig
    • C07C281/04C07C281/16C07D249/12C07C275/70
    • C07D249/12C07C281/04
    • Alkoxytriazolinones of the formula (I), ##STR1## are obtained in good yields and in high purity by reacting iminocarbonic diesters (II) with carbazinic esters (III) ##STR2## at -20.degree. C. to +120.degree. C. (1st step) and subjecting the semicarbazide derivatives (IV) formed in this process with elimination of R.sup.2 --OH ##STR3## to a cyclizing condensation reaction in the presence of a base at 20.degree. C. to 150.degree. C. with elimination of R.sup.3 --OH, if appropriate (2nd step) and, finally, by reacting the resulting 5-alkoxytriazolinones of the formula (V) �=formula (I) where R.sup.1 =H! with an alkylating agent of the formula R.sup.1 --X (VI) at 0.degree. C. to 150.degree. C., if appropriate in the presence of a base.
    • 通过使亚氨基碳酸二酯(II)与咔嗪酸酯(III)在-20℃至+ 120℃下反应,以良好的产率和高纯度获得式(I),(IMAGE)(I)的烷氧基​​三唑啉酮 (第1步),在20℃〜150℃下,在碱的存在下,将在该工序中形成的氨基脲衍生物(Ⅳ)与R2-OH的反应进行环化缩合反应, (Ⅴ)[=式(I)其中R1 = H)与式R1-X(Ⅵ)的烷基化剂反应得到的5-烷氧基三唑啉酮 )在0℃至150℃,如果合适,在碱的存在下。
    • 7. 发明授权
    • Polyamine crosslinking agent formulation and its preparation
    • 多胺交联剂配方及其制备
    • US5705594A
    • 1998-01-06
    • US767564
    • 1996-12-16
    • Klaus KonigOtto NeunerWerner Rasshofer
    • Klaus KonigOtto NeunerWerner Rasshofer
    • C07D251/34C08G59/50C08J3/24C08K5/3492C08L63/00C08L73/02C08L79/02C08G18/08C08G18/10
    • C08G59/5086C07D251/34
    • Liquid polyamine crosslinking agent formulations based on trimerized toluylene 2,4- and/or 2,6-diisocyanate, with formation of an isocyanurate structure and hydrolysis of the isocyanate groups to amine groups, are described. The novel crosslinking agent formulations have a content of 40 to 80% of the total weight of the solids content of the crosslinking agent formulation of 1,3,5-tris-(3-amino-4-methyl-phenyl,2-methyl-3-aminophenyl) isocyanurate (I) which is not further condensed, and a content of not more than 1.0% of the total weight of the crosslinking agent formulations of toluylene-2,4- and/or -2,6-diamine (III). For the preparation, toluylene diisocyanate is trimerized, to form the isocyanurate structure, until 10 to 25% of the NCO groups have been reacted. The toluylene diisocyanate which has not undergone condensation is then distilled off, the bottom product formed by this operation is taken up directly in a solvent A and the 30 to 70% strength by weight solution formed by this procedure is metered into a hydrolysis in water/N,N-dialkyl-carboxylic acid amide in the presence of a catalytic amount of a basic catalyst. After the hydrolysis, the crosslinking agent formulations are brought to a solids content of 35 to 60% of the total weight of the formulation by distilling off a portion of the solvents and adding a solvent B.
    • 描述了基于三聚甲苯2,4-和/或2,6-二异氰酸酯的液态多胺交联剂制剂,其形成异氰脲酸酯结构和将异氰酸酯基团水解为胺基。 新型交联剂配方的含量为交联剂配方的1,3,5-三(3-氨基-4-甲基 - 苯基,2-甲基 - 苯基) - 苯胺的固体含量的总重量的40-80% 3-氨基苯基)异氰脲酸酯(I),其不再进一步缩合,并且不大于甲苯-2,4-和/或-2,6-二胺(III)的交联剂配方的总重量的1.0重量% )。 为了制备,将甲苯二异氰酸酯进行三聚,形成异氰脲酸酯结构,直到10〜25%的NCO基团都已反应。 然后蒸馏除去未进行冷凝的甲苯二异氰酸酯,将通过该操作形成的底部产物直接溶于溶剂A中,并将通过该方法形成的30-70重量%的重量浓度的溶液计量加入水/ N,N-二烷基 - 羧酸酰胺在催化量的碱性催化剂存在下反应。 水解后,通过蒸馏掉一部分溶剂并加入溶剂B使交联剂配方的固体含量达到制剂总重量的35至60%。
    • 8. 发明授权
    • Process for the preparation of alkoxytriazolinones
    • 制备烷氧基三唑啉酮的方法
    • US5594147A
    • 1997-01-14
    • US528584
    • 1995-09-15
    • Heinz-Jurgen WroblowskyKlaus Konig
    • Heinz-Jurgen WroblowskyKlaus Konig
    • C07C281/06C07D249/12
    • C07D249/12C07C281/06
    • Alkoxytriazolinones of the general formula (I), ##STR1## in which R.sup.1 represents hydrogen, or represents in each case optionally substituted alkyl, alkenyl, alkinyl, cycloalkyl, cycloalkylalkyl, aryl or arylalkyl, andR.sup.2 represents in each case optionally substituted alkyl, alkenyl, alkinyl, cycloalkyl, cycloalkylalkyl, aryl or arylalkyl,(which can be used as intermediates for the preparation of herbicidal active compounds) are obtained in very good yields and in high purity by reacting imino(thio)carbonic esters (II) with alkoxyethyl carbazinates (III) ##STR2## in which Q represents O or S, R.sup.3 represents (for example) alkyl, aryl or aralkyl and R.sup.4 represents (for example) alkyl,at -20.degree. C. to +150.degree. C. (1st step) and subjecting the new semicarbazide derivatives (IV) ##STR3## which are formed with elimination of R.sup.3 --QH, if appropriate after intermediate isolation, to a cyclizing condensation reaction at 0.degree. C. to 200.degree. C., without the addition of a base, advantageously under reduced pressure, with the elimination of alkoxyethanols (2nd step).
    • 通式(I)的烷氧基​​三唑啉酮,其中R 1表示氢,或在每种情况下表示任选取代的烷基,烯基,炔基,环烷基,环烷基烷基,芳基或芳基烷基,和R 2表示在各种情况下任选取代的 烷基,烯基,炔基,环烷基,环烷基烷基,芳基或芳基烷基(可用作制备除草活性化合物的中间体)以非常好的产率和高纯度通过使亚氨基(硫代)碳酸酯(II) 其中Q代表O或S,R3代表(例如)烷基,芳基或芳烷基,R4代表(例如)烷基,在-20℃至+ 150℃(第1步),在0℃〜200℃进行环化缩合反应,在中间分离后,如果合适,将R3-QH所形成的新的氨基脲衍生物(IV) 没有添加基础,优势 我们在减压下,消除烷氧基乙醇(第二步)。