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    • 1. 发明授权
    • Removing aqueous ammonium sulfate from oxime product
    • 从肟产物中除去硫酸铵
    • US4256668A
    • 1981-03-17
    • US50356
    • 1979-06-20
    • Chempolil T. MathewDonald Pickens
    • Chempolil T. MathewDonald Pickens
    • C07C131/00C07C131/04
    • C07C323/47C07C249/14C07C2101/14
    • An organic, substantially water-insoluble oxime product is recovered from the liquid reaction mixture of water, ammonium sulfate and the oxime product. First the reaction mixture is separated into a first liquid layer containing an aqueous ammonium sulfate solution and a second liquid layer containing an emulsion of the oxime product as the continuous phase and aqueous ammonium sulfate as the discontinuous phase. These layers are separated and the second liquid layer is contacted with solid ammonium sulfate for a time sufficient to agglomerate the discontinuous phase. The agglomerated discontinuous phase is then removed from the continuous phase. Thereafter, either a lites fraction can be distilled from the continuous phase or the oxime product can be distilled from the continuous phase, or both. The process is particularly applicable to the production of oximes such as Aldicarb oxime, cyclohexanone oxime and methylethylketoxime from aqueous reaction mixtures in which by-product ammonium sulfate is formed.
    • 从水,硫酸铵和肟产物的液体反应混合物中回收有机的,基本上不溶于水的肟产物。 首先,将反应混合物分离成含有硫酸铵水溶液的第一液体层和含有作为连续相的肟产物的乳液的第二液体层和作为不连续相的硫酸铵水溶液。 分离这些层,第二液层与固体硫酸铵接触一段足以使不连续相结块的时间。 然后从连续相中除去聚集的不连续相。 此后,可以从连续相中蒸馏出lites馏分,或者可以从连续相或两者中蒸馏出肟产物。 该方法特别适用于由其中形成副产物硫酸铵的水性反应混合物生产肟类,如涕灭威肟,环己酮肟和甲基乙基酮肟。
    • 4. 发明授权
    • Method of recovering alkali metal fluorides from organic slurry
    • 从有机浆料中回收碱金属氟化物的方法
    • US4793936A
    • 1988-12-27
    • US518882
    • 1983-08-01
    • Philip A. LefrancoisDonald Pickens
    • Philip A. LefrancoisDonald Pickens
    • C01D3/02C02F1/52
    • C01D3/02Y10S210/908Y10S210/915
    • A method for recovering organic ether solvent and alkali metal fluoride from a slurry thereof such as may be formed as a byproduct in silane manufacture. First water is added to a slurry having an organic ether liquid phase and a finely-divided solid phase comprising an alkali metal fluoride. The water is added in an amount sufficiently large to reduce adherence of organic ether to the solid phase and sufficiently small not to create a discernable separate aqueous liquid phase. The slurry with added water is maintained at a treatment temperature of at least about 50.degree. C. for a treatment period of at least one minute, typically 15-30 minutes at 90.degree.-110.degree. C. Thereafter, the treated slurry is seaparated into a crude fluoride solid and an ether liquid suitable for direct recycle or recycle after simple further treatment.
    • 从其浆料中回收有机醚溶剂和碱金属氟化物的方法,例如可以在硅烷制造中作为副产物形成。 向具有有机醚液相的浆料和包含碱金属氟化物的细分固体中加入第一水。 以足够大的量加入水以降低有机醚与固相的粘附性,并且足够小,不产生可辨别的分离的水性液相。 加入水的浆料在至少约50℃的处理温度下保持至少1分钟,在90-110℃下通常为15-30分钟的处理时间。然后将处理后的浆液分散成 简单的进一步处理后可以直接循环或再循环的氟化物固体和醚液。
    • 8. 发明授权
    • Process for halogenation of aldehydes and production of oximes therefrom
    • 醛的卤化和肟的生产方法
    • US4155933A
    • 1979-05-22
    • US894870
    • 1978-04-10
    • John H. BonfieldAndiappan K. MurthyDonald Pickens
    • John H. BonfieldAndiappan K. MurthyDonald Pickens
    • C07C45/00C07C45/63C07C47/14C07C67/00C07C313/00C07C319/20C07C323/47C07C131/00
    • C07C45/63
    • In the halogenation under reflux conditions of an unhalogenated aldehyde of the formula ##STR1## with Cl.sub.2, Br.sub.2 or I.sub.2, the aldehyde and halogen are continuously fed into a reactor at a molar ratio of halogen to unhalogenated aldehyde between about 0.8:1 and about 1.1:1 and water is continuously fed into the unhalogenated reactor at a rate of between about 1% and about 20% by weight of aldehyde. The product .alpha.-haloaldehyde is thiohydrocarbylated and then oximated to form a 2-hydrocarbylthioaldoxime of the formula ##STR2## with improved yield and quality because of the improved yield and quality of unhalogenated .alpha.-haloaldehyde. An exemplary process includes the chlorination of isobutyraldehyde (IBA) to form .alpha.-chloroisobutyraldehyde (CIBA), the thiomethylation of CIBA to form 2-methyl-2 methylthio-propionaldehyde (MTIBA) and the oximation of MTIBA to form 2-methylthio-propionaldehyde oxime (aldicarb oxime or ADO).
    • 在式Cl 1,Br 2或I 2的未卤化醛的回流条件下,将醛和卤素以约0.8:1至约1.1的卤素与非卤化醛的摩尔比连续进料到反应器中 :1和水以醛的约1重量%至约20重量%的速率连续进料到未卤化反应器中。 产物α-卤代烃被硫代烃基化,然后氧化形成式“IMAGE”的2-烃基硫代醛肟,其产率和质量得到改善,因为改善了产生和质量的非卤代α-卤代醛。 一个示例性的方法包括异丁醛(IBA)氯化以形成α-氯异丁醛(CIBA),CIBA的甲硫基化形成2-甲基-2-甲硫基 - 丙醛(MTIBA)和肟化MTIBA以形成2-甲硫基 - 丙醛肟 (涕灭威肟或ADO)。