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    • 101. 发明授权
    • Process for the continuous production of monoisocyanates
    • 连续生产单异氰酸酯的方法
    • US4195031A
    • 1980-03-25
    • US965648
    • 1978-12-20
    • Wolfgang ReichmannKlaus KonigJohannes Koster
    • Wolfgang ReichmannKlaus KonigJohannes Koster
    • C07C265/02C07C20060101C07C67/00C07C241/00C07C263/04C07C265/04C07C118/00
    • C07C263/04
    • The instant invention relates to an improved process for the continuous production of an aliphatic monoisocyanate from the corresponding N-alkyl carbamic acid aryl ester. More particularly, the invention is directed to a process for the continuous production of monoisocyanates corresponding to the formulaR--NCOin whichR represents an aliphatic hydrocarbon radical containing 1 to 3 carbon atoms comprising thermally decomposing the corresponding N-alkylcarbamic acid aryl esters corresponding to the formulaR--NH--CO--O--R'in whichR has the meaning above andR' represents a radical of the type obtained by removing the hydroxyl group from a monophenol having a boiling point below 250.degree. C. at normal pressure, and separating the decomposition products by decomposition, further characterized in that(a) a solution of the N-alkylcarbamic acid aryl ester in an organic solvent, which solvent is inert under the reaction conditions and has a boiling point lying at least 20.degree. C. above the boiling point of the monoisocyanate to be formed, is heated to a temperature of from 160.degree. C. to 250.degree. C. at normal pressure or at slightly reduced pressure within the range of 200 to 1013 mbar, thereby resulting in the decomposition of the ester into the corresponding monoisocyanate and the corresponding phenol, as well as the evaporation of the solvent and the decomposition products, and(b) the vapors formed are fed into a distillation column with the monoisocyanate obtained at the head of the column and with the phenol and at least a major portion of the solvent obtained from a side stream or from several side streams.
    • 本发明涉及从相应的N-烷基氨基甲酸芳基酯连续制备脂族单异氰酸酯的改进方法。 更具体地说,本发明涉及连续制备相应于式R-NCO的单异氰酸酯的方法,其中R代表含有1至3个碳原子的脂族烃基,包括热分解相应的N-烷基氨基甲酸芳基酯 式R-NH-CO-OR'其中R具有上述含义,R'表示通过在常压下从沸点低于250℃的单酚除去羟基得到的类型的基团,并且分离 分解产物,其特征还在于(a)N-烷基氨基甲酸芳基酯在有机溶剂中的溶液,该溶剂在反应条件下是惰性的,并且沸点至少在20℃以上 要形成的单异氰酸酯的沸点在常压或稍微减压的范围内加热到160℃至250℃的温度 e为200至1013毫巴,从而导致酯分解成相应的单异氰酸酯和相应的苯酚,以及溶剂和分解产物的蒸发,和(b)所形成的蒸气进料到蒸馏塔 与在柱的头部和苯酚获得的单异氰酸酯以及从侧流或从多个侧流获得的至少大部分溶剂。
    • 108. 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。
    • 109. 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。
    • 110. 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)。