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    Process for the recovery of nitric acid
    101.
    发明授权
    Process for the recovery of nitric acid 失效
    硝酸回收方法

    公开(公告)号：US5006325A

    公开(公告)日：1991-04-09

    申请号：US399654

    申请日：1989-08-28

    Applicant: David L. Parks, Jr. ,  Carl J. Martin

    Inventor： David L. Parks, Jr. ,  Carl J. Martin

    IPC: C01B21/46 ,  C07C201/08 ,  C07C201/16 ,  C07C205/06

    CPC classification number: C07C201/16 ,  B01D3/06 ,  B01D3/38

    Abstract: This invention relates to an improved process for the recovery and regeneration of nitric acid from spent acid obtained from the mixed acid nitration of aromatic compounds. In that process a mixed acid of sulfuric acid and nitric acid is contacted with an aromatic composition at a temperature and pressure sufficient for producing a nitroaromatic composition and a spent acid containing unreacted nitric acid, sulfuric acid and solubilized nitroaromatic compounds in said spent acid. The improvement comprises initially heating the spent acid to a temperature of from about 120.degree. to 200.degree. C. for a time sufficient to convert said nitroaromatics in said spent acid to a nitroaromatic composition having a boiling point greater than 300.degree. C. at atmospheric pressure and then flash distilling the hot spent acid containing nitroaromatics compositions at a pressure from about 5 to 15 psia and temperature of 150.degree. to 200.degree. C. Nitric acid is removed as an overhead vapor fraction in preselected concentration and sulfuric acid and nitroaromatics are obtained as a bottoms liquid stream from said flash distilling step. The nitroaromatics are then removed from the liquid stream. Sulfuric acid obtained from this process is essentially free of color and suited for concentration.

    Purification of pentachloronitrobenzene by distillation
    103.
    发明授权
    Purification of pentachloronitrobenzene by distillation 失效
    通过蒸馏纯化五氯硝基苯

    公开(公告)号：US4842696A

    公开(公告)日：1989-06-27

    申请号：US105677

    申请日：1987-10-08

    Applicant: Arturo S. Cazares

    Inventor： Arturo S. Cazares

    IPC: B01D3/34 ,  C07C201/16

    CPC classification number: C07C201/16 ,  B01D3/343 ,  Y10S203/02 ,  Y10S203/13

    Abstract: Pentachloronitrobenzene (PCNB) which initially contains in excess of 0.5% hexachlorobenzene (HCB) is purified by distilling the impure PCNB at a temperature between 100.degree.-250.degree. C. and a pressure below or at atmospheric pressure to obtain a PCNB product having a HCB content lower than 0.5%, and preferably lower than 0.1%.

    Abstract translation: 最初含有超过0.5％六氯苯（HCB）的五氯硝基苯（PCNB）通过在100-250℃和低于或大气压的压力下蒸馏不纯的PCNB来纯化，得到具有HCB的PCNB产物 含量低于0.5％，优选低于0.1％。

    Method for recovering diphenylethers from their nitrated by-products
    105.
    发明授权
    Method for recovering diphenylethers from their nitrated by-products 失效
    从其硝化副产物中回收二苯醚的方法

    公开(公告)号：US4754052A

    公开(公告)日：1988-06-28

    申请号：US928901

    申请日：1986-11-07

    Applicant: William W. Brand ,  John F. Stephen

    Inventor： William W. Brand ,  John F. Stephen

    IPC: C07C201/16 ,  C07C79/46

    CPC classification number: C07C201/16 ,  C07C303/40 ,  C07C303/44

    Abstract: A process of recycling nitrated by-products formed during the manufacture of the compound of the formula ##STR1## and salts thereof wherein J is ##STR2## and further wherein: R.sup.1 is fluorine, chlorine, bromine, or iodine or a trifluoromethyl group;R.sup.2 is a hydrogen atom, a fluorine, chlorine, bromine or iodine atom or a trifluoromethyl group;R.sup.3 is a hydrogen atom, a C.sub.1 -C.sub.4 alkyl group, a trifluoromethyl group, a cyano group or a fluorine, chlorine, bromine or iodine group; X is ##STR3## R.sup.4 is R.sup.5 or an acyl radical of the formula ##STR4## wherein Alk is a C.sub.1-6 alkyl group; R.sup.5 is a hydrogen atom or a C.sub.1-6 alkyl group optionally substituted with either one or more halogen atoms or a phenyl group;B is a C.sub.1-10 alkyl, OR.sup.7 or SR.sup.7 ;y is 1 to 4;R.sup.6 is a hydrogen atom or a C.sub.1-2 alkyl group;R.sup.7 is hydrogen, or a C.sub.1-8 alkyl group, a C.sub.3-8 cycloalkyl group, an agronomically acceptable cationic salt, or a ##STR5## wherein n is 0 to 3 and Z is selected from the group consisting of halogen, a C.sub.1-10 alkyl or alkoxy group, cyano, nitro, and trifluoromethyl; andR.sup.8 is R.sup.5 or a C.sub.1-6 alkoxy group. The process comprises 2 stages. In the first stage, the nitrated by-products are reduced. In the second stage, the reduced compounds are diazotized and the diazonium group is replaced with a hydrogen atom.

    Abstract translation: 在制备式（I）化合物期间形成的硝化副产物和其盐，其中J是其中R1是氟，氯，溴或碘或三氟甲基的方法 组; R2是氢原子，氟，氯，溴或碘原子或三氟甲基; R3是氢原子，C1-C4烷基，三氟甲基，氰基或氟，氯，溴或碘基; X是R 4或R 5或其中Alk是C 1-6烷基的式“IMAGE”的酰基; R5是氢原子或任选被一个或多个卤原子或苯基取代的C 1-6烷基; B是C 1-10烷基，OR 7或SR 7; y为1〜4; R6是氢原子或C1-2烷基; R 7为氢或C 1-8烷基，C 3-8环烷基，农艺学上可接受的阳离子盐或其中n为0至3且Z选自卤素，C1- 10个烷基或烷氧基，氰基，硝基和三氟甲基; R8为R5或C1-6烷氧基。 该过程包括2个阶段。 在第一阶段，硝化副产物减少。 在第二阶段中，将还原的化合物重氮化并且重氮基团被氢原子代替。

    Process for the preparation of aromatic monocarboxylic acids from toluene and substituted toluenes
    106.
    发明授权
    Process for the preparation of aromatic monocarboxylic acids from toluene and substituted toluenes 失效
    由甲苯和取代的甲苯制备芳族单羧酸的方法

    公开(公告)号：US4603220A

    公开(公告)日：1986-07-29

    申请号：US632261

    申请日：1984-07-18

    Applicant: Marcel Feld

    Inventor： Marcel Feld

    IPC: B01J31/04 ,  C07B61/00 ,  C07C51/00 ,  C07C51/265 ,  C07C51/47 ,  C07C63/04 ,  C07C63/70 ,  C07C65/21 ,  C07C67/00 ,  C07C201/12 ,  C07C201/16 ,  C07C205/57

    CPC classification number: C07C201/12 ,  C07C201/16 ,  C07C51/265

    Abstract: In a process for preparing aromatic monocarboxylic acids by oxidation of toluene or of toluenes substituted in the nucleus, the starting substances are reacted in the liquid phase with oxygen or with a gas containing oxygen, at a temperature of 80.degree.-180.degree. C. and a pressure of 5 to 50 bar in the presence of acetic acid as diluent and a soluble cobalt and/or manganese salt in combination with a bromide, and the aromatic monocarboxylic acids are then obtained by solid-liquid separation of the cooled reaction mixture.To reduce the dimensions of the oxidation reactor, for which particularly corrosion-resistant materials are necessary, and to isolate the target products in high yield and purity, as well as to reduce the technical complexity and cost of the treatment of the amounts of solvents that are yielded, relatively small amounts of acetic acid are used as solvents or diluents, namely at a ratio by weight of the alkyl aromatic being oxidized and acetic acid of 0.5:1 to 6:1. Not until the reaction has ended is the dilution, which is necessary for the isolation of the target product by solid-liquid separation of the cooled reaction mixture, performed by the addition of dilute aqueous acetic acid or of the washing filtrate from a preceding oxidation run. A typical example is the preparation of p-tert-butylbenzoic acid from p-tert-butyltoluene by the method described.

    Abstract translation: 在通过甲苯或核中取代的甲苯的氧化制备芳族单羧酸的方法中，起始物质在液相中与氧气或含氧气体在80-180℃的温度下反应， 在乙酸作为稀释剂存在下，压力为5至50巴，与溴化物结合使用可溶性钴和/或锰盐，然后通过冷却的反应混合物的固液分离获得芳族单羧酸。 为了减小需要特别耐腐蚀材料的氧化反应器的尺寸，并以高产率和纯度分离目标产物，以及降低处理溶剂量的技术复杂性和成本， 使用相对少量的乙酸作为溶剂或稀释剂，即以氧化的烷基芳族化合物的重量比为0.5:1至6:1的乙酸。 直到反应结束为止，稀释是通过冷却的反应混合物的固液分离来分离目标产物所必需的，其通过加入稀乙酸水溶液或从先前的氧化运行中洗涤滤液进行 。 典型的实例是通过所述方法从对叔丁基甲苯制备对叔丁基苯甲酸。

    Precipitative removal of nitrocresols from dinitrotoluene waste streams
    107.
    发明授权
    Precipitative removal of nitrocresols from dinitrotoluene waste streams 失效
    从二硝基甲苯废液中沉淀除去硝基酚

    公开(公告)号：US4597875A

    公开(公告)日：1986-07-01

    申请号：US731424

    申请日：1985-05-07

    Applicant: Richard V. C. Carr ,  John E. Sawicki ,  Bernard A. Toseland

    Inventor： Richard V. C. Carr ,  John E. Sawicki ,  Bernard A. Toseland

    IPC: C02F9/00 ,  C07C201/16 ,  C02F1/52 ,  C02F1/66

    CPC classification number: C02F1/66 ,  C07C201/16 ,  C02F2101/345 ,  C02F2101/38 ,  Y10S210/909

    Abstract: This invention relates to a process for removing nitrocresols and picric acid contaminants from a wastewater stream generated in the production of nitroaromatics, particularly dinitrotoluene, by the mixed acid technique. The process involves contacting the crude dinitrotoluene generated by the mixed acid technique with an alkaline medium to generate an alkaline wash water containing water soluble nitrocresols and picric acid therein. This wastewater is separated from the organic component and recycled for contact with further quantities of crude dinitrotoluene product from the reactor. When the concentration of the water soluble salts of nitrocresols and picric acid is of sufficient concentration the wash water is treated with aqueous acid in sufficient proportion to convert the water soluble salts to water insoluble organics. After treatment with acid, the organic material is separated from the wastewater and the organics incinerated.

    Abstract translation: 本发明涉及通过混合酸技术从硝基芳族化合物，特别是二硝基甲苯生产中产生的废水流中除去硝基甲酚和苦味酸污染物的方法。 该方法包括将由混合酸技术产生的粗二硝基甲苯与碱性介质接触，以产生含有水溶性硝基甲酚和苦味酸的碱性洗涤水。 该废水与有机组分分离并再循环用于与来自反应器的另外量的粗二硝基甲苯产物接触。 当硝基甲酚和苦味酸的水溶性盐的浓度足够浓度时，洗涤水用足够比例的酸水溶液处理，以将水溶性盐转化为水不溶性有机物。 用酸处理后，有机物与废水分离，有机物被焚烧。

    Isolation of m,m'-dinitrobenzophenone
    109.
    发明授权
    Isolation of m,m'-dinitrobenzophenone 失效
    分离m，m'-二硝基二苯甲酮

    公开(公告)号：US4560800A

    公开(公告)日：1985-12-24

    申请号：US650881

    申请日：1984-09-17

    Applicant: Kiran R. Bakshi ,  Adrian D'Souza ,  Edward T. Sabourin

    Inventor： Kiran R. Bakshi ,  Adrian D'Souza ,  Edward T. Sabourin

    IPC: C07C201/16 ,  C07C45/61

    CPC classification number: C07C201/16 ,  C07C201/08

    Abstract: A process for the preparation and recovery of m,m'-dinitrobenzophenone and which comprises reacting benzophenone with nitric acid in oleum; adjusting the reaction product to a water content from 12 to 30 weight percent; and extracting the m,m'-dinitrobenzophenone with a chlorinated hydrocarbon solvent.

    Abstract translation: 一种制备和回收m，m'-二硝基二苯甲酮的方法，其包括使二苯甲酮与硝酸在发烟硫酸中反应; 将反应产物调节至12至30重量％的水含量; 并用氯化烃溶剂萃取m，m'-二硝基二苯甲酮。

    Complex formed to separate nitrated phenolic compounds from other phenolic compounds
    110.
    发明授权
    Complex formed to separate nitrated phenolic compounds from other phenolic compounds 失效
    形成复合物以将硝化酚类化合物与其他酚类化合物分离

    公开(公告)号：US4479019A

    公开(公告)日：1984-10-23

    申请号：US582083

    申请日：1984-02-21

    Applicant: Gerd Leston

    Inventor： Gerd Leston

    IPC: C07C201/16 ,  C07C205/22 ,  C07C79/32

    CPC classification number: C07C201/16 ,  C07C205/22

    Abstract: A process is disclosed for separating nitrated phenolic compounds from other nitrated and unnitrated phenolics by treating a mixture of the phenolics with a metal halide salt. The metal halide salt preferentially forms a complex with one of the phenolics over other related phenolics in the mixture. The preferentially-formed complex of one of the phenolics may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of, one phenolic. The process is particularly suitable for resolving a mixture comprising phenol or cresol from their ortho-nitrated derivatives, or a mixture of two isomeric nitrated phenols or cresols or a mixture of mono-and dinitrated phenols or cresols.

    Abstract translation: 公开了通过将酚类与金属卤化物盐的混合物进行处理来分离硝化酚类化合物与其它硝化和未硝化酚醛树脂的方法。 与混合物中的其它相关酚类物质相比，金属卤化物盐优先与酚类之一形成络合物。 然后可以从混合物中分离一种酚类的优先形成的络合物，并且复合物被分解以提供基本上富含或完全由一种酚类组成的产物。 该方法特别适用于从其邻硝化衍生物或两种异构硝化酚或甲酚的混合物或单硝酸盐和二硝基苯酚或甲酚的混合物中分离出包含苯酚或甲酚的混合物。

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