公开(公告)号：US4256668A

公开(公告)日：1981-03-17

申请号：US50356

申请日：1979-06-20

Applicant: Chempolil T. Mathew ,  Donald Pickens

Inventor： Chempolil T. Mathew ,  Donald Pickens

IPC: C07C131/00 ,  C07C131/04

CPC classification number: C07C323/47 ,  C07C249/14 ,  C07C2101/14

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US4407783A

公开(公告)日：1983-10-04

申请号：US408408

申请日：1982-08-16

Applicant: Harry E. Ulmer ,  Donald Pickens ,  Forrest J. Rahl ,  Philip A. Lefrancois

Inventor： Harry E. Ulmer ,  Donald Pickens ,  Forrest J. Rahl ,  Philip A. Lefrancois

IPC: C10M101/00 ,  C01B33/04

CPC classification number: C01B33/043

Abstract: Silicon tetrafluoride is reacted with sodium hydride in a cyclic ether reaction medium such as tetrahydrofuran or 1,4-dioxane or in dimethoxyethane. Sodium aluminum hydride is dissolved in the solvent and catalyzes the reaction in amounts of 4-25%, by weight of combined sodium hydride and sodium aluminum hydride.

Abstract translation: 四氟化硅与氢化钠在环醚反应介质如四氢呋喃或1,4-二恶烷或二甲氧基乙烷中反应。 将氢化铝钠溶解在溶剂中，以4-25％（重量）的氢化钠和氢化钠铝的量催化反应。

公开(公告)号：US4096187A

公开(公告)日：1978-06-20

申请号：US821898

申请日：1977-08-04

Applicant: John Henry Bonfield ,  Andiappan Kumaresa Murthy ,  Donald Pickens

Inventor： John Henry Bonfield ,  Andiappan Kumaresa Murthy ,  Donald Pickens

IPC: C07C45/00 ,  C07C45/63 ,  C07C47/14 ,  C07C67/00 ,  C07C313/00 ,  C07C319/20 ,  C07C323/47 ,  C07C131/00

CPC classification number: C07C45/63

Abstract: In the halogenation under reflux conditions of an 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 aldehyde between about 0.8:1 and about 1.1:1 and water is continuously fed into the reactor at a rate of between about 1 and about 20% by weight of aldehyde. The product .alpha.-haloaldehyde is thioalkylated 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 .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).

Abstract translation: 在醛与Cl 2，Br 2或I 2的醛的回流条件下的卤化反应中，醛和卤素以约0.8:1至约1.1:1的卤素与醛的摩尔比连续进料到反应器中 并且以约1至约20重量％的醛的速率将水连续地进料到反应器中。 产物α-卤代烃是硫烷基化的，然后氧化形成式“IMAGE”的2-烃基硫代醛肟，具有改善的产率和质量，因为α-卤代醛的产率和质量提高。 示例性方法包括异丁醛（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）。

公开(公告)号：US4793936A

公开(公告)日：1988-12-27

申请号：US518882

申请日：1983-08-01

Applicant: Philip A. Lefrancois ,  Donald Pickens

Inventor： Philip A. Lefrancois ,  Donald Pickens

IPC: C01D3/02 ,  C02F1/52

CPC classification number: C01D3/02 ,  Y10S210/908 ,  Y10S210/915

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US5061577A

公开(公告)日：1991-10-29

申请号：US277089

申请日：1988-11-28

Applicant: Daniel F. Harnish ,  Donald Pickens ,  Richard J. Brautigam

Inventor： Daniel F. Harnish ,  Donald Pickens ,  Richard J. Brautigam

IPC: C08G59/22 ,  C08G59/30 ,  C09D5/23 ,  C09D163/00 ,  C09D171/00 ,  C09D171/02 ,  G11B5/702 ,  H01F1/00

CPC classification number: C08G59/30 ,  C08G59/22 ,  C09D163/00 ,  C09D171/02 ,  G11B5/702 ,  H01F1/0027 ,  Y10S428/90

Abstract: A class of fluorinated polyols which when added to formulated dispersions used to make a magnetic particle based coating not only improves the dispersion of the particles in the formulation during manufacture but also improves the wear characteristics of the cured coating during use. The fluorinated polyol may be prepared either by the reaction of a diglycidyl ether with a diol or by the reaction of two diols with epichlorohydrin.

Abstract translation: 当添加到用于制备基于磁性颗粒的涂料的配制分散体中时，一类氟化多元醇不仅改善了制造过程中颗粒在制剂中的分散性，而且改善了使用期间固化涂层的磨损特性。 氟化多元醇可以通过二缩水甘油醚与二醇的反应或两种二醇与表氯醇的反应来制备。

公开(公告)号：US5004790A

公开(公告)日：1991-04-02

申请号：US311316

申请日：1989-02-15

Applicant: Daniel F. Harnish ,  Donald Pickens ,  Andrew M. Zweig

Inventor： Daniel F. Harnish ,  Donald Pickens ,  Andrew M. Zweig

IPC: C08G59/30 ,  C08G59/40

CPC classification number: C08G59/30 ,  C08G59/4028

Abstract: A novel class of fluorinated surfactant monomers which when blended and cured with conventional non-fluorinated monomers produces resins with dramatically modified surfaces. Resins which may be thus modified include urethanes, epoxides, acrylates, polyesters and other thermosetting materials.

Abstract translation: 一种新型的氟化表面活性剂单体，当与常规非氟化单体混合和固化时，产生具有显着改性表面的树脂。 可以如此改性的树脂包括聚氨酯，环氧化物，丙烯酸酯，聚酯和其它热固性材料。

公开(公告)号：US4323706A

公开(公告)日：1982-04-06

申请号：US217938

申请日：1980-12-18

Applicant: John H. Bonfield ,  Stephen E. Belsky ,  Donald Pickens

Inventor： John H. Bonfield ,  Stephen E. Belsky ,  Donald Pickens

IPC: C07C131/00

Abstract: Acetaldehyde oxime, a commercially useful intermediate in the production of pesticides, is prepared by oximating acetaldehyde with an aqueous hydroxylamine-containing solution to form an aqueous oximation reaction mixture and recovering acetaldehyde oxime from the aqueous oximation reaction mixture by distilling a mixture of acetaldehyde oxime and water directly from the aqueous oximation reaction mixture.

Abstract translation: 乙醛肟是生产农药的商业上有用的中间体，通过用含羟胺溶液肟化乙醛以形成水性肟化反应混合物并通过蒸馏乙醛肟混合物和肟化反应混合物回收乙醛肟来制备， 水直接从水性肟化反应混合物中。

公开(公告)号：US4155933A

公开(公告)日：1979-05-22

申请号：US894870

申请日：1978-04-10

Applicant: John H. Bonfield ,  Andiappan K. Murthy ,  Donald Pickens

Inventor： John H. Bonfield ,  Andiappan K. Murthy ,  Donald Pickens

IPC: C07C45/00 ,  C07C45/63 ,  C07C47/14 ,  C07C67/00 ,  C07C313/00 ,  C07C319/20 ,  C07C323/47 ,  C07C131/00

CPC classification number: C07C45/63

Abstract: 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).

Abstract translation: 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）。

公开(公告)号：US4133834A

公开(公告)日：1979-01-09

申请号：US866421

申请日：1978-01-03

Applicant: Donald Pickens

Inventor： Donald Pickens

IPC: C07C131/00

CPC classification number: C07C251/38

Abstract: An improved process is disclosed for preparing .alpha.-and .beta.-hydroxy oximes wherein said oximes are prepared in the presence of a water soluble compound capable of contributing ferric or ferrous ions to the reaction medium. Such oximes are useful as metal complexing agents. Such complexing agents are used in processes of extracting metals from an ore solution.

Abstract translation: 公开了用于制备α-和β-羟基肟的改进方法，其中所述肟在能够向反应介质中产生三价铁或亚铁离子的水溶性化合物的存在下制备。 这种肟作为金属络合剂是有用的。 这种络合剂用于从矿石溶液中提取金属的工艺。