公开(公告)号：US07928270B2

公开(公告)日：2011-04-19

申请号：US12280176

申请日：2007-03-06

Applicant: Ulrich Penzel ,  Ruediger Fritz ,  Holger Allardt ,  Johannes Adam ,  Anne-Kathrin Merten

Inventor： Ulrich Penzel ,  Ruediger Fritz ,  Holger Allardt ,  Johannes Adam ,  Anne-Kathrin Merten

IPC: C07C205/00

CPC classification number: B01D3/38 ,  C07C201/16 ,  C07C205/06

Abstract: A process is proposed for distillatively removing dinitrotoluene from process wastewater from the preparation of dinitrotoluene by nitrating toluene with nitrating acid, which comprises basifying the process wastewater to a pH of >8.5, feeding it to a stripping column in the upper region thereof and stripping it with steam in countercurrent to obtain a vapor stream laden with dinitrotoluene and a bottom stream depleted in dinitrotoluene compared to the process wastewater used.

Abstract translation: 提出了一种从硝化硝酸硝化甲苯制备二硝基甲苯中的二硝基甲苯蒸馏除去二硝基甲苯的方法，其中包括将工艺废水碱化至pH值> 8.5，将其送入其上部区域的汽提塔并将其汽提 与所用的工艺废水相比，蒸汽以逆流方式获得装载有二硝基甲苯的蒸气流和二硝基甲苯消耗的底部流。

公开(公告)号：US07030237B2

公开(公告)日：2006-04-18

申请号：US10009627

申请日：2000-12-21

Applicant: Isamu Uemasu ,  Kozo Hara ,  Hideki Takahashi

Inventor： Isamu Uemasu ,  Kozo Hara ,  Hideki Takahashi

IPC: C08B37/16

CPC classification number: C07D215/06 ,  C07B63/00 ,  C07C7/152 ,  C07C17/395 ,  C07C201/16 ,  C07C2602/42 ,  C07C25/02 ,  C07C25/10 ,  C07C205/06 ,  C07C15/08 ,  C07C15/24 ,  C07C13/21 ,  C07C13/39

Abstract: In a reaction system having at least two liquid-liquid interfaces between an organic phase of raw material containing a compound(s) to be separated and an aqueous phase of an aqueous solution of inclusion-complexing agent and between that aqueous phase and an organic phase(s) of extraction solvent(s), the compound(s) to be separated is entrapped into the aqueous phase through formation of an inclusion complex(es) of the inclusion-complexing agent with the compound(s), while the compound(s) is entrapped into the organic phase(s) of extraction solvent(s) through dissociation of said inclusion complex(es). The foregoing operation is performed using, for example, a squarish U-shaped tube or an H-shaped tube with bottom plates. Preferred examples of inclusion-complexing agent include highly water-soluble branched cyclodextrins.

公开(公告)号：US20050256343A1

公开(公告)日：2005-11-17

申请号：US10520725

申请日：2003-07-09

Applicant: Eric Fache ,  Sebastien Righini

Inventor： Eric Fache ,  Sebastien Righini

IPC: C07C201/12 ,  C07C21/12 ,  C07C201/16 ,  C07C205/22

CPC classification number: C07C201/16 ,  C07C205/22

Abstract: The invention relates to a method of preparing a high-purity nitrophenol and, more specifically, p-nitrophenol from a nitrohalobenzene. The inventive method comprises the following steps: (a) hydrolysis of a nitrohalobenzene compound by reacting said compound with a base; (b) acidification in order to produce the nitrophenol compound from the salt thereof by means of an acid treatment; (c) crystallisation of the nitrophenol compound obtained; and (d) separation of the product obtained. The invention is characterised in that it also comprises at least the following steps: (e) concentration of the reaction medium after hydrolysis (a) and before acidification (b); and (f) liquid/liquid decantation after acidification (b) and before crystallisation (c), which is intended to eliminate the water phase obtained after acidification (b).

Abstract translation: 本发明涉及一种从硝基卤苯制备高纯度硝基苯酚，更具体地说是对硝基苯酚的方法。 本发明的方法包括以下步骤：（a）通过使所述化合物与碱反应来水解硝基卤苯化合物; （b）酸化以通过酸处理从其盐生产硝基苯酚化合物; （c）获得的硝基苯酚化合物的结晶; 和（d）所得产物的分离。 本发明的特征在于其还包括至少以下步骤：（e）水解（a）和酸化（b）之前浓缩反应介质; 和（f）在酸化（b）和结晶（c）之前的液体/液体倾析，其旨在消除酸化后获得的水相（b）。

公开(公告)号：US20040262238A1

公开(公告)日：2004-12-30

申请号：US10878211

申请日：2004-06-28

Inventor： Jurgen Munnig ,  Dietmar Wastian ,  Wolfgang Lorenz ,  Berthold Keggenhoff

IPC: C02F001/68

CPC classification number: C02F1/26 ,  C02F1/66 ,  C02F9/00 ,  C02F2103/36 ,  C07C201/16 ,  C07C205/06 ,  C07C205/22 ,  C07C205/24 ,  C07C205/57

Abstract: The present invention relates to a process for working up or treating aqueous waste waters which are formed during the nitration of toluene to dinitrotoluene with nitrating acid. These aqueous waste waters containing acidic wash water and alkaline wash water from the dinitrotoluene washing step, and distillate from the sulfuric acid concentration step. The process comprises, a) combining the acidic and alkaline waste waters from the washing step and the aqueous distillate from the sulfuric acid concentration step such that the resulting mixture has a pH below 5, b) separating the aqueous and organic phases which are formed by phase separation, c) subjecting the aqueous phase from b) to an extraction step, wherein d) the organic components contained in the aqueous phase from c) are extracted with toluene, and e) introducing the toluene phase enriched with the organic components into the toluene nitration.

Abstract translation: 本发明涉及一种处理或处理在用硝酸将甲苯硝化成二硝基甲苯期间形成的废水的处理方法。 这些含有来自二硝基甲苯洗涤步骤的酸性洗涤水和碱性洗涤水的含水废水，以及来自硫酸浓缩步骤的馏出物。 该方法包括：a）将来自洗涤步骤的酸性和碱性废水与来自硫酸浓缩步骤的含水馏出物混合，使得所得混合物的pH值低于5，b）将由下式形成的水相和有机相分离： 相分离，c）使来自b）的水相进行萃取步骤，其中d）来自c）的水相中含有的有机组分用甲苯萃取，e）将富含有机组分的甲苯相引入 甲苯硝化。

公开(公告)号：US06353142B1

公开(公告)日：2002-03-05

申请号：US09704876

申请日：2000-11-02

Applicant: Eberhard Zirngiebl ,  Bernd-Michael König ,  Hans-Martin Weber ,  Thomas Linn ,  Hans-Joachim Raatz

Inventor： Eberhard Zirngiebl ,  Bernd-Michael König ,  Hans-Martin Weber ,  Thomas Linn ,  Hans-Joachim Raatz

IPC: C07C20506

CPC classification number: C07C201/12 ,  C07C201/16 ,  C07C205/12

Abstract: 1,2-Dichlorobenzene can be reacted very selectively under adiabatic reaction conditions to give 3,4-dichloronitrobenzene by intensively mixing 1,2-dichlorobenzene with nitric acid, sulphuric acid and water, simultaneously or successively, in their total amount, using a mixing energy of 1-50 watts per litre of the total reaction mixture, preferably 3-30 W/l, and maintaining a temperature of from 0 to 60° C. during mixing.

Abstract translation: 1,2-二氯苯可以在绝热反应条件下非常有选择性地反应，通过使用混合物，将1,2-二氯苯与硝酸，硫酸和水强烈混合，同时或相继地以其总量而混合，得到3,4-二氯硝基苯 能量为1-50瓦/升总反应混合物，优选3-30W / l，并​​在混合期间保持0至60℃的温度。

公开(公告)号：US06307045B1

公开(公告)日：2001-10-23

申请号：US09608217

申请日：2000-06-30

Applicant: Hiroshi Komori ,  Kazuhiko Nishioka

Inventor： Hiroshi Komori ,  Kazuhiko Nishioka

IPC: C07B3900

CPC classification number: C07D243/24 ,  C07B39/00 ,  C07B59/001 ,  C07B59/002 ,  C07C201/12 ,  C07C201/16 ,  C07C205/12

Abstract: The present invention provides a process for producing halogenated benzene compounds. In the process, an organometallic compound represented by the general formula [I]: wherein M represents an R13Sn group, an R13Si group, an R13Ge group, an (R2CO2)Hg group, a ClHg group or an (R3O)2B group wherein each R1 independently represents a C1-C8 alkyl group, R2 represents a C1-C3 alkyl group or a C1-C3 haloalkyl group, R3 represents a hydrogen atom or a C1-C3 alkyl group, n represents an integer of from 0 to 4, m represents an integer of from 0 to 1, each A independently represents a fluorine atom, a nitro group, a cyano group, a C1-C8 alkyl group, a C1-C8 alkoxy group or a C2-C8 acyloxy group, and Q represents an organic residue, is reacted in a solvent with a halide ion represented by the general formula X−, under light irradiation conditions in the presence of a semiconductor catalyst with a photocatalytic activity.

Abstract translation: 本发明提供了制备卤化苯化合物的方法。 在该方法中，由通式[I]表示的有机金属化合物：其中M表示R 13 Sn基团，R 13 Si基团，R 13 Ge基团，（R 2 CO 2）Hg基团，Cl Hg基团或（R 3 O） R1独立地表示C1-C8烷基，R2表示C1-C3烷基或C1-C3卤代烷基，R3表示氢原子或C1-C3烷基，n表示0〜4的整数，m 表示0〜1的整数，A各自独立地表示氟原子，硝基，氰基，C 1〜C 8烷基，C 1〜C 8烷氧基或C 2〜C 8酰氧基，Q表示 有机残余物在溶剂中与通式X-表示的卤离子在光照射条件下在具有光催化活性的半导体催化剂的存在下反应。

公开(公告)号：US06288289B1

公开(公告)日：2001-09-11

申请号：US09492851

申请日：2000-01-27

Applicant: David Anthony Boyd ,  Stuart Alan Gairns ,  Alfred Alexander Guenkel

Inventor： David Anthony Boyd ,  Stuart Alan Gairns ,  Alfred Alexander Guenkel

IPC: C07C20500

CPC classification number: A62D3/20 ,  A62D2101/26 ,  A62D2101/28 ,  C02F1/66 ,  C02F1/72 ,  C02F11/086 ,  C02F2101/36 ,  C02F2101/38 ,  C02F2103/36 ,  C02F2103/38 ,  C07C201/16 ,  Y02P20/125 ,  Y02P20/544 ,  C07C205/06 ,  C07C205/23

Abstract: An integrated process for treating alkaline wash water effluent from nitroaromatic manufacture, principally containing nitro-hydroxy-aromatic compounds is described. The integrated process concentrates the alkaline wash water to recover chemicals and water prior to treating the concentrate through supercritical water oxidation. The supercritical water oxidation step consists of treating the concentrate in the presence of an oxygen source at conditions, which are supercritical for water to cause a substantial portion of the organic component of the concentrate to oxidize. The product effluent includes a gaseous component and a clean water component, and in the event that insoluble ash is formed, an ash component. The new integrated process results in reduced chemical and water consumption compared to existing processes. In addition, the treated wash water effluent can be recycled to process or directly discharged.

Abstract translation: 描述了一种用于处理主要含有硝基 - 羟基 - 芳族化合物的硝基芳香族生产的碱性洗涤水流出物的综合方法。 在通过超临界水氧化处理浓缩物之前，一体化过程将碱性洗涤水浓缩以回收化学品和水。 超临界水氧化步骤包括在氧气源存在下处理浓缩物，该条件对于水是超临界的，导致浓缩物的大部分有机组分氧化。 产物流出物包括气态组分和清洁水组分，并且在形成不溶性灰分的情况下，含有灰分。 与现有流程相比，新的综合过程导致化学和水消耗减少。 此外，经处理的洗涤水流出物可循环使用或直接排出。

公开(公告)号：US20010005762A1

公开(公告)日：2001-06-28

申请号：US09748924

申请日：2000-12-27

Inventor： Tetsuya Shintaku ,  Masahide Tanaka ,  Nobushige Itaya

IPC: C07C205/00 ,  C07C207/00 ,  C07C051/16 ,  C07C051/235

CPC classification number: C07C201/16 ,  C07C205/51 ,  C07C205/53

Abstract: The present invention provides a method of producing easily and in a high yield a threo-2-hydroxy-3-nitrobutanoic acid compound or a mixture of a threo- and an erythro-2-hydroxy-3-nitrobutanoic acid compounds, this mixture having an erythro compound:threo compound ratio of about 1:1, which method includes reacting, in a solvent, a 2-hydroxy-3-nitrobutanoic acid compound having the formula (I) 1 wherein R is optionally substituted alkyl or optionally substituted aryl, with not less than 1 equivalent of a base to isomerize (i) the erythro compound into the threo compound, or (ii) the threo compound into the erythro compound, and a method for separating the erythro and the threo compounds easily and in a high yield. The separation method includes reacting the mixture of threo- and erythro-compounds with not more than 1 equivalent of potassium carbonate per threo compound in a solvent. According to the method of the present invention, useful pharmaceuticals can be produced easily in a high yield.

Abstract translation: 本发明提供了一种容易且高产率地制备苏-22-羟基-3-硝基丁酸化合物或苏 - 和 - 赤-2-羟基-3-硝基丁酸化合物的混合物的方法，该混合物具有 红霉素化合物：苏化合物比例为约1:1，该方法包括在溶剂中使具有式（I）的2-羟基-3-硝基丁酸化合物（其中R是任选取代的烷基或任选取代的芳基）与 不少于1当量的碱，将（i）赤式化合物异构化为苏化合物，或（ii）苏化合物进入赤式化合物，以及容易且高收率地分离赤式和苏式化合物的方法 。 分离方法包括在溶剂中使苏氨酸和赤式化合物的混合物与不多于1当量的碳酸钾/苏化合物反应。 根据本发明的方法，可以容易地以高产率制备有用的药物。

公开(公告)号：US5910604A

公开(公告)日：1999-06-08

申请号：US816930

申请日：1997-03-13

Applicant: Stephen Martin Brown ,  Brian David Gott ,  Thomas Gray ,  Seyed Mehdi Tavana

Inventor： Stephen Martin Brown ,  Brian David Gott ,  Thomas Gray ,  Seyed Mehdi Tavana

IPC: C07C201/16 ,  C07C205/59 ,  C07C303/36 ,  C07C303/44 ,  C07C311/51

CPC classification number: C07C303/44 ,  C07C201/16

Abstract: A process for the purification of a compound of general formula I: ##STR1## wherein R.sup.1 is hydrogen or C.sub.1 -C.sub.6 alkyl, C.sub.2 -C.sub.6 alkenyl or C.sub.2 -C.sub.6 alkynyl, any of which may optionally be substituted with one or more substituents selected from halogen and hydroxy; or COOR.sup.4, COR.sup.6, CONR.sup.4 R.sup.5 or CONHSO.sub.2 R.sup.4 ;R.sup.4 and R.sup.5 independently represent hydrogen or C.sub.1 -C.sub.4 alkyl optionally substituted with one or more halogen atoms;R.sup.6 is a halogen atom or a group R.sup.4 ;R.sup.2 is hydrogen or halo; andR.sup.3 is C.sub.1 -C.sub.4 alkyl, C.sub.2 -C.sub.4 alkenyl or C.sub.2 -C.sub.4 alkynyl, any of which may optionally be substituted with one or more halogen atoms; or halo; or, where appropriate, a salt thereof;from a mixture containing the compound of general formula I together with one or more isomers or di-nitrated analogs thereof; the process comprising dissolving the mixture in a suitable crystallization solvent and recrystallizing the product from the resulting crystallization solution wherein the crystallization solution contains not more than 25% loading of the compound of general formula I, loading being defined as: ##EQU1## and wherein the temperature to which the solution is cooled for crystallization is not greater than about 30.degree. C.; wherein, after the addition of the crystallizing solvent but before recrystallization, the crystallization solution is subjected to at least one wash with an aqueous solution having an acid pH. The process is particularly useful for purifying acifluorfen produced via a route starting with m-cresol.

Abstract translation: 一种用于纯化通式I化合物的方法：其中R 1是氢或C 1 -C 6烷基，C 2 -C 6烯基或C 2 -C 6炔基，其中任何一个可任选被一个或多个选自卤素和羟基的取代基取代 ; 或COOR4，COR6，CONR4R5或CONHSO2R4; R4和R5独立地表示氢或任选被一个或多个卤素原子取代的C 1 -C 4烷基; R6是卤素原子或基团R4; R2是氢或卤素; 并且R 3是C 1 -C 4烷基，C 2 -C 4烯基或C 2 -C 4炔基，其中任何一个可任选地被一个或多个卤素原子取代; 或卤素; 或者在适当情况下为其盐; 由含有通式I化合物的混合物与一种或多种异构体或其二硝化类似物一起混合; 该方法包括将混合物溶解在合适的结晶溶剂中并从所得结晶溶液中重结晶产物，其中结晶溶液含有不超过25％的通式I化合物的负载，负载定义为：并且其中温度为 该溶液冷却结晶不超过约30℃。 其中，在加入结晶溶剂之后但重结晶之前，用酸性pH值的水溶液对结晶溶液进行至少一次洗涤。 该方法特别可用于纯化通过以间甲酚开始的途径产生的三氟果霜。

公开(公告)号：US5847240A

公开(公告)日：1998-12-08

申请号：US824654

申请日：1997-03-24

Applicant: Allen B. Quakenbush ,  Buford T. Pennington

Inventor： Allen B. Quakenbush ,  Buford T. Pennington

IPC: C06B21/00 ,  C06B25/04 ,  C07C201/16 ,  C07C205/00

CPC classification number: C06B21/0091 ,  C06B25/04 ,  C07C201/16

Abstract: A process is disclosed for removing a light organic compound from a liquid composition comprising said light organic compound in admixture with a nitroaromatic compound, said light organic compound having a partial vapor pressure in said composition that is greater than the partial vapor pressure of said nitroaromatic compound in said composition, said process comprising contacting said composition with steam or a gas to cause at least a portion of said light organic compound to pass out of said composition and into admixture with said steam or gas.

Abstract translation: 公开了一种从包含所述轻质有机化合物的液体组合物与硝基芳族化合物混合物中除去轻质有机化合物的方法，所述轻质有机化合物在所述组合物中的部分蒸汽压大于所述硝基芳族化合物的部分蒸汽压 在所述组合物中，所述方法包括使所述组合物与蒸汽或气体接触以使所述轻质有机化合物的至少一部分从所述组合物中排出并与所述蒸汽或气体混合。