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    Process for the manufacture of N,N,N',N'-tetraacetylethylenediamine
    2.
    发明授权
    Process for the manufacture of N,N,N',N'-tetraacetylethylenediamine 失效
    制备N，N，N'，N'-四乙酰基乙二胺的方法

    公开(公告)号：US4240980A

    公开(公告)日：1980-12-23

    申请号：US29258

    申请日：1979-04-11

    Applicant: Gunther Muller-Schiedmayer ,  Rudolf Aigner

    Inventor： Gunther Muller-Schiedmayer ,  Rudolf Aigner

    IPC: C07C231/00 ,  C07B20060101 ,  C07C20060101 ,  C07C67/00 ,  C07C231/08 ,  C07C233/91 ,  C07C102/00

    CPC classification number: C07C231/08 ,  Y02P20/582

    Abstract: The invention provides an improved process for the manufacture of N,N,N',N'-tetraacetylethylenediamine by acetylation of N,N'-diacetylethylenediamine with acetic anhydride, by using these two starting components in a weight ratio of from 1:1 to 1:10, stopping the acetylation before attaining the reaction equilibrium between N,N'-diacetylethylenediamine and N,N,N',N'-tetraacetylethylenediamine, preferably after having attained a conversion rate of from 20 to 70 mol % of tetraacetylethylenediamine, relative to diacetylethylenediamine, purifying the reaction mixture in order to remove the dyeing impurities, and recycling to the acetylation the purified, incompletely reacted components. Purification may be carried out by vacuum distillation or by means of an adsorbent, for example bleaching earth or active charcoal. Optionally, from 0.01 to 0.3 part by weight of ketene per part by weight of diacetylethylenediamine are added to the starting components. The process may be carried out batchwise or continuously, and it gives a practically colorless product with high yield (more than 97%).

    Abstract translation: 本发明提供了一种通过用乙酸酐乙酰化N，N'-二乙酰基乙二胺来制备N，N，N'，N'-四乙酰基乙二胺的改进方法，通过使用这两种起始组分，重量比为1:1至 1:10，在达到N，N'-二乙酰基乙二胺与N，N，N'，N'-四乙酰基乙二胺之间的反应平衡之前停止乙酰化，优选在达到四乙酰基乙二胺的20至70摩尔％的转化率之后，相对 到二乙酰基乙二胺，纯化反应混合物以除去染色杂质，并再循环到乙酰化纯化的，未完全反应的组分。 纯化可以通过真空蒸馏或通过吸附剂，例如漂白土或活性炭进行。 任选地，向起始组分中加入每重量份二乙酰基乙二胺0.01至0.3重量份的乙烯酮。 该方法可以间歇或连续进行，并且以高产率（大于97％）得到几乎无色的产品。

    Continuous process for the preparation of dimethyldiallylammonium chloride
    4.
    发明授权
    Continuous process for the preparation of dimethyldiallylammonium chloride 失效
    连续制备二甲基二烯丙基氯化铵的方法

    公开(公告)号：US4670594A

    公开(公告)日：1987-06-02

    申请号：US895182

    申请日：1986-08-11

    Applicant: Rudolf Aigner ,  Gunter Blaschke ,  Gunther Muller

    Inventor： Rudolf Aigner ,  Gunter Blaschke ,  Gunther Muller

    IPC: C07C209/00 ,  C07C67/00 ,  C07C209/12 ,  C07C211/63 ,  C07C239/12 ,  C07C85/04

    CPC classification number: C07C209/12

    Abstract: In the continuous process described for the preparation of dimethyldiallylammonium chloride by reaction, with stirring, of dimethylamine, allyl chloride and alkali metal hydroxide which is dissolved in water, the reaction is carried out in at least two stirred vessels arranged in the form of a cascade. Dimethylamine and allyl chloride in the stoichiometric amount in each case and only 60 to 95 mol % of the stoichiometrically necessary amount of alkali metal hydroxide are fed to the first stirred vessel and conducted through the vessel at a temperature of 20.degree. to 70.degree. C. with a residence time such that the product leaving the vessel and flowing to the further vessels still contains at most 10 mol % of free amine, mol percentages being related to the molar amount of dimethylamine employed; the alkali metal hydroxide lacking in the first stirred vessel compared to the stoichiometric amount is fed continuously to the further stirred vessels mentioned and in these vessels, at a temperature of 20.degree. to 70.degree. C., a residence time is set such that the product leaving the vessel still contains at most 2 mol % of free amine in each case. The desired dimethyldiallylammonium chloride is obtained from the product leaving the stirred vessel cascade.

    Abstract translation: 在用于通过在搅拌下反应制备二甲基二烯丙基氯化铵的连续方法中溶解在水中的二甲胺，烯丙基氯和碱金属氢氧化物，反应在至少两个以级联形式排列的搅拌容器中进行 。 在每种情况下，化学计量量的二甲胺和烯丙基氯以及化学计量必需量的碱金属氢氧化物仅为60〜95摩尔％，进料到第一搅拌釜中，并在20〜70℃的温度下通过容器。 停留时间使得离开容器并流向另外的容器的产物仍含有至多10摩尔％的游离胺，摩尔百分数与所用二甲胺的摩尔量有关; 在第一搅拌釜中与化学计量量相比，不饱和的碱金属氢氧化物连续地供给到所述的另外的搅拌容器和这些容器中，在20℃至70℃的温度下，将停留时间设定为使产物 在每种情况下，容器仍含有至多2摩尔％的游离胺。 所需的二甲基二烯丙基氯化铵从离开搅拌釜级联的产物中获得。

    Method for producing arylpoly(oxalkyl)-benzyldimethyl-ammonium derivatives
    8.
    发明授权
    Method for producing arylpoly(oxalkyl)-benzyldimethyl-ammonium derivatives 失效
    芳基聚（氧烷基） - 苄基二甲基铵衍生物的制备方法

    公开(公告)号：US06794543B2

    公开(公告)日：2004-09-21

    申请号：US10276210

    申请日：2002-11-14

    Applicant: Klaus Raab ,  Gerhard Crass ,  Rudolf Aigner

    Inventor： Klaus Raab ,  Gerhard Crass ,  Rudolf Aigner

    IPC: C07C21300

    CPC classification number: C07C213/02 ,  C07C217/08

    Abstract: The invention provides a process for preparing arylpoly(oxalkyl)benzyl-dimethylammonium derivatives of the formula (1) which comprises reacting compounds of the formulae (2) and (3) where X=Br, Cl, R—SO3 with R=alkyl, alkylaryl R1=H, C1- to C16-alkyl or O—C1- to O—C16-alkyl in the ortho, meta or para position, R2=H, C1- to C4-alkyl or O—C1- to O—C4-alkyl, R3=H, C1- to C16-alkyl or O—C1- to O—C16-alkyl in the ortho, meta or para position, and n=1, 2, 3 or 4, at temperatures of from 60 to 160° C. in a solvent under the autogenous pressure.

    Abstract translation: 本发明提供一种制备式（1）的芳基聚（氧烷基）苄基 - 二甲基铵衍生物的方法，其包括使式（2）和（3）的化合物与其中X = Br，Cl，R-SO 3与R =烷基，烷芳基R1 在邻位，间位或对位是H，C 1至C 16 - 烷基或O-C 1至O-C 1-6 - 烷基，R 2 = H，C 1至C 4 - 烷基或O-C 1至O-C 4 - 烷基 在邻位，间位或对位，R 3 = H，C 1至C 16 - 烷基或O-C 1至O-C 1-6 - 烷基，并且n = 1,2,3或4，温度为60至160℃ 在自生压力下在溶剂中。

    Low-melting ester quats
    9.
    发明授权
    Low-melting ester quats 失效
    低熔点季铵盐

    公开(公告)号：US6072063A

    公开(公告)日：2000-06-06

    申请号：US807868

    申请日：1997-02-26

    Applicant: Oliver Eyrisch ,  Rudolf Aigner

    Inventor： Oliver Eyrisch ,  Rudolf Aigner

    IPC: C11D1/62 ,  A01N37/12 ,  A61K8/44 ,  A61Q19/00 ,  B01F17/00 ,  B01F17/18 ,  C07C213/02 ,  C07C213/06 ,  C07C213/08 ,  C07C219/06 ,  D06M13/463 ,  C07C101/00

    CPC classification number: A61Q19/00 ,  A61K8/416 ,  A61K8/44 ,  B01F17/0042 ,  C07C219/06

    Abstract: Ester quats of the formula (1) below are described: ##STR1## where RCO is an aliphatic acyl radical having 6 to 22 carbon atoms, R.sup.1 is a methyl radical, R.sup.2 is a C.sub.1 -C.sub.6 -alkyl radical, R.sup.3 is a C.sub.3 -C.sub.6 -alkyl radical and X.sup.- is a halogen anion. They are prepared by quaternizing the corresponding carboxylic acid ethanolamine ester compound with a methyl halide in the absence or presence of solvents. The ester quats of the invention have a low melting point. Furthermore, even in high concentration they are highly water soluble and, on account of their preparation, are obtained in high purity and free from toxic contents. These ester quats can be used in many ways and are suitable, for example, for preparing solid or aqueous formulations having a high surfactant effect.

    Abstract translation: 其中，RCO为碳原子数为6〜22的脂肪族酰基，R1为甲基，R2为C1-C6烷基，R3为C3-C6烷基， 自由基和X-是卤素阴离子。 它们通过在不存在或不存在溶剂的情况下用甲基卤化物将相应的羧酸乙醇胺酯化合物季铵化来制备。 本发明的酯季度具有低熔点。 此外，即使在高浓度下，它们是高度水溶性的，并且由于其制备，获得高纯度且没有有毒物质。 这些酯季铵盐可以以许多方式使用，并且适用于例如制备具有高表面活性剂效果的固体或水性制剂。

    Process for the preparation of aqueous betaine solutions
    10.
    发明授权
    Process for the preparation of aqueous betaine solutions 失效
    制备甜菜碱水溶液的方法

    公开(公告)号：US5292942A

    公开(公告)日：1994-03-08

    申请号：US42115

    申请日：1993-04-02

    Applicant: Rudolf Aigner ,  Guillermo Maier ,  Rainer Muller ,  Hubert Seitz

    Inventor： Rudolf Aigner ,  Guillermo Maier ,  Rainer Muller ,  Hubert Seitz

    IPC: C07C227/08 ,  C07C229/12 ,  C07C229/16 ,  C07C231/12 ,  C07C233/36 ,  C11D1/90 ,  C07C229/00

    CPC classification number: A61K8/44 ,  C07C227/08 ,  C07C231/12 ,  A61Q19/10

    Abstract: A process is described for the preparation of aqueous solutions of betaines of the formula ##STR1## in which: R.sup.1 is an alkyl radical having 6 to 22 carbon atoms or is a radical of the formula R'CONH(CH.sub.2).sub.z --, in which R' has the meaning of R.sup.1 and z is 2, 3 or 4, R.sup.2 is an alkyl radical having 1 to 4 carbon atoms or is a radical of the formula --(CH.sub.2).sub.m --OH, in which m is 1, 2 or 3, R.sup.3 is an alkyl radical having 1 to 4 carbon atoms or is a radical of said formula --(CH.sub.2).sub.m --OH and y is 1, 2 or 3. The aqueous betaine solutions are prepared by quaternization of the corresponding tertiary amines with an .omega.-halocarboxylic acid and with an alkali metal hydroxide in the aqueous phase. The quaternization is carried out continuously in two or three stirred tanks arranged in a cascade, defined process characteristics being maintained in each tank. Using the novel process, aqueous betaine solutions are obtained in high yield and purity in a simple manner.

    Abstract translation: 描述了制备式“β”的甜菜碱水溶液的方法，其中：R 1是具有6至22个碳原子的烷基，或者是式R'CONH（CH 2）z - 的基团，其中 R'具有R 1的含义，z是2,3或4，R 2是具有1至4个碳原子的烷基，或者是式 - （CH 2）m -OH的基团，其中m是1,2或 3，R 3是具有1至4个碳原子的烷基或是所述式 - （CH 2）m -OH的基团，y是1,2或3.通过季铵化相应的叔胺与 ω-卤代羧酸和碱金属氢氧化物在水相中。 季铵化在连续排列的两个或三个搅拌槽中连续进行，在每个罐中保持定义的工艺特性。 使用该新方法，以简单的方式以高产率和纯度获得甜菜碱水溶液。

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