公开(公告)号：US4496782A

公开(公告)日：1985-01-29

申请号：US512289

申请日：1983-07-08

Applicant: Richard V. C. Carr

Inventor： Richard V. C. Carr

IPC: C07C201/16 ,  C07C79/10

CPC classification number: C07C201/16

Abstract: A method is provided for denitrifying the aqueous spent acid of mononitration. The nitric acid in the aqueous spent acid is recovered by adiabatically reacting greater than a stoichiometric amount of a mononitroaromatic hydrocarbon with the aqueous spent acid which has been fortified to a nitric acid concentration of at least about 2 wt %. The denitrification method is useful in treating the aqueous spent acid phase from the mononitration stage of a dinitrotoluene process.

Abstract translation: 提供一种用于使单硝化的废酸水反硝化的方法。 废酸水溶液中的硝酸通过绝大多数化学计量的单硝基芳烃与已被强化至至少约2重量％的硝酸浓度的废酸水溶液绝热反应。 脱氮方法可用于从二硝基甲苯方法的单硝化阶段处理废酸水相。

公开(公告)号：US4467126A

公开(公告)日：1984-08-21

申请号：US515001

申请日：1983-07-18

Applicant: Hermann A. Zinnen

Inventor： Hermann A. Zinnen

IPC: C07C201/16 ,  C07C79/12 ,  C07C79/10

CPC classification number: C07C201/16

Abstract: An adsorptive separation process for separating the para-isomers of a di-substituted benzene from a feed mixture comprising the para-isomer and at least one other isomer. One substituted group is NO.sub.2 -- and the other group is a normal hydrocarbon having less than 6 carbon atoms per molecule, the halogens, NH.sub.2 --, NO.sub.2 -- or C.tbd.N--. The process comprises contacting the feed mixture with an adsorbent comprising crystalline silica having a silica/alumina mole ratio of at least 12, selectively adsorbing substantially all of the para-isomer to the substantial exclusion of the remaining isomers and thereafter recovering high-purity para-isomer by means of desorption with an appropriate desorbent material.

Abstract translation: 用于从包含对位异构体和至少一种其它异构体的进料混合物中分离二取代苯的对位异构体的吸附分离方法。 一个取代基是NO 2 - ，另一个基团是每分子具有小于6个碳原子的正常烃，卤素，NH 2 - ，NO 2 - 或C 3 - N - N。 该方法包括使进料混合物与包含二氧化硅/氧化铝摩尔比至少为12的结晶二氧化硅的吸附剂接触，选择性吸附基本上所有的对位异构体以基本排除其余的异构体，然后回收高纯度对 - 通过用适当的解吸材料解吸。

公开(公告)号：US4429169A

公开(公告)日：1984-01-31

申请号：US372055

申请日：1982-04-26

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/86 ,  C07C201/16 ,  C07C205/22 ,  C07C37/68

CPC classification number: C07C37/86 ,  C07C37/685 ,  C07C37/84

Abstract: A process is disclosed for separating 5-isopropyl-m-cresol from other isopropylated m-cresols by treating a mixture of the isopropylated m-cresols with a metal halide salt. The metal halide salt preferentially forms a complex with 5-isopropyl-m-cresol over other related closely-boiling isopropylated m-cresols in the mixture. The preferentially-formed complex of 5-isopropyl-m-cresol may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of, 5-isopropyl-m-cresol. The process is particularly suitable for isolating 5-isopropyl-m-cresol from closely-boiling isomers, and diisopropylated m-cresols.

Abstract translation: 公开了通过将异丙基化间甲酚与金属卤化物盐的混合物进行处理从其它异丙基化间甲酚中分离5-异丙基间甲酚的方法。 与其他相关的沸点相近的异丙基化间甲酚相比，金属卤化物盐与5-异丙基间甲酚优先形成络合物。 然后可以从混合物中分离出优先形成的5-异丙基间甲酚的复合物，并将络合物分解，得到基本上富含或完全由5-异丙基间甲酚组成的产物。 该方法特别适用于从紧密沸腾的异构体中分离出5-异丙基间甲酚和二异丙基间甲酚。

公开(公告)号：US4367347A

公开(公告)日：1983-01-04

申请号：US269137

申请日：1981-06-01

Applicant: John E. Sawicki

Inventor： John E. Sawicki

IPC: C07C67/00 ,  C07C201/00 ,  C07C201/16 ,  C07C205/06 ,  C07C79/10

CPC classification number: C07C201/16

Abstract: A method for preparing substantially pure 2,4-DNT isomer from its admixture with other DNT isomers which comprises contacting the isomer mixture with aqueous sulfuric acid at an elevated temperature, separating excess DNT isomer mixture from the sulfuric acid phase and cooling the sulfuric acid phase. Also, in a method for producing dinitrotoluenes which comprises:(a) nitrating toluene in a first nitration stage with an aqueous mixture of sulfuric and nitric acids to form an organic phase containing mononitrotoluenes and a first aqueous spent acid phase;(b) separating the organic phase from the first aqueous spent acid phase;(c) nitrating the mononitrotoluenes contained in the organic phase in a second nitration stage using a mixture of sulfuric and nitric acids to form an organic phase containing dinitrotoluenes and a second aqueous spent acid phase; and(d) separating the organic phase from the second aqueous spent acid phase for recovery of the dinitrotoluene product from the organic phase;the novel feature comprising:(e) cooling at least a portion of the first or second aqueous spent acid phase to a temperature sufficient to effect crystallization of substantially pure 2,4-DNT;(f) recovering the 2,4-DNT crystals from the cooled aqueous spent acid phase; and(g) returning the portion of the cooled spent acid phase to a nitration stage.

Abstract translation: 从其与其它DNT异构体的混合物制备基本上纯的2,4-DNT异构体的方法，其包括在高温下使异构体混合物与硫酸水溶液接触，从硫酸相分离过量的DNT异构体混合物并冷却硫酸相 。 此外，在制备二硝基甲苯的方法中，其包括：（a）在第一硝化阶段用硫酸和硝酸的含水混合物硝化甲苯以形成含有单硝基甲苯和第一含水废酸相的有机相; （b）将有机相与第一含水废酸相分离; （c）在第二硝化阶段使用硫酸和硝酸的混合物硝化有机相中所含的单硝基甲苯以形成含有二硝基甲苯和第二废酸水相的有机相; 和（d）将有机相与第二废酸水相分离，以从有机相中回收二硝基甲苯产物; 该新颖特征包括：（e）将至少一部分第一或第二含水废酸相冷却到足以实现基本上纯的2,4-DNT的结晶的温度; （f）从冷却的废酸水相中回收2,4-DNT晶体; 和（g）将冷却的废酸相的一部分返回到硝化阶段。

公开(公告)号：US4258224A

公开(公告)日：1981-03-24

申请号：US107194

申请日：1979-12-26

Applicant: Charles Ribaudo ,  John F. Leccacorvi ,  Everett E. Gilbert

Inventor： Charles Ribaudo ,  John F. Leccacorvi ,  Everett E. Gilbert

IPC: C07C201/16

CPC classification number: C07C201/16

Abstract: A process for recovering pure 2,4,6-trinitrotoluene (TNT) from a crude TNTixture containing unsymmetrical TNT isomers which comprises forming a homogeneous powder of the crude TNT and silica gel, introducing said powder at the top of a silica gel packed column, and resolving the TNT mixture into its component isomers by contacting said powder with a developing solvent system which is not reactive with the component isomers selected from the group consisting of polar organic solvents, non-polar organic solvents, and mixtures thereof having an energy of adsorption adequate to selectively adsorb the individual TNT isomers, such as a mixture of polar acetonitrile and non-polar trichloro trifluoroethane.

Abstract translation: 一种从含有不对称TNT异构体的粗TNT混合物中回收纯2,4,6-三硝基甲苯（TNT）的方法，包括形成粗TNT和硅胶的均匀粉末，将所述粉末引入硅胶填料柱的顶部 并且将TNT混合物分解成其组分异构体，使所述粉末与显影剂溶剂体系接触，所述显影剂溶剂体系与选自极性有机溶剂，非极性有机溶剂及其混合物的组分异构体不反应，所述极性有机溶剂， 吸附足以选择性吸附各种TNT异构体，例如极性乙腈和非极性三氯三氟乙烷的混合物。

公开(公告)号：US4230567A

公开(公告)日：1980-10-28

申请号：US28029

申请日：1979-04-06

Applicant: Wolfgang Larbig

Inventor： Wolfgang Larbig

IPC: C02F1/02 ,  C02F1/74 ,  C02F9/00 ,  C07C201/16 ,  C02C5/00

CPC classification number: C02F1/025 ,  C02F2101/34 ,  C02F2101/38

Abstract: The invention concerns a process for working up an effluent containing nitro-hydroxy-aromatic compounds which comprises heating said effluent to 150.degree. C. to 500.degree. C. with the exclusion of air and oxygen and under elevated pressure. The process results in a decrease of nitro-hydroxy-aromatic compound concentration in the effluent to below 20 ppm. and the resulting material can then be fed to a microbiological sewage plant for further working up, without the microorganisms therein being killed by the bactericidally active nitro-hydroxy-aromatic compounds.

Abstract translation: 本发明涉及一种处理含有硝基 - 羟基 - 芳族化合物的流出物的方法，其包括将所述流出物加热至150℃至500℃，排除空气和氧气并在升高的压力下。 该过程导致流出物中硝基 - 羟基 - 芳族化合物浓度降低至20ppm以下。 然后将得到的材料送入微生物污水处理厂进行进一步处理，其中的微生物不被杀菌活性的硝基 - 羟基 - 芳族化合物杀死。

公开(公告)号：US4147731A

公开(公告)日：1979-04-03

申请号：US871904

申请日：1978-01-24

Applicant: Milton B. Frankel ,  Frederick D. Raniere ,  Wallace W. Thompson ,  Edward F. Witucki ,  Dean O. Woolery, II

Inventor： Milton B. Frankel ,  Frederick D. Raniere ,  Wallace W. Thompson ,  Edward F. Witucki ,  Dean O. Woolery, II

IPC: C07C201/16 ,  C07C76/02

CPC classification number: C07C201/16

Abstract: A method of isolating nitroform from a solution of nitric acid, nitroform, and water by adding sulfuric acid and preferentially extracting the nitroform with methylene chloride. The nitroform is then extracted from the methylene chloride solution into water. It is a particular advantage of the present method that no distillations involving nitroform are required.

Abstract translation: 一种通过加入硫酸从硝酸，硝基和水溶液中分离硝基的方法，并用二氯甲烷优先萃取硝基。 然后将硝基形式从二氯甲烷溶液中提取到水中。 本方法的特别优点是不需要涉及硝基的蒸馏。

公开(公告)号：US3980717A

公开(公告)日：1976-09-14

申请号：US158594

申请日：1971-06-30

Applicant: Lee A. Subluskey

Inventor： Lee A. Subluskey

IPC: C07C201/16 ,  C07C79/26

CPC classification number: C07C201/16 ,  C07C201/08

Abstract: Process for the manufacture of para-nitro-meta-cresol in high yield from directly available and inexpensive meta/para-cresol mixtures, without need heretofore for first resolving the cresol mixture to provide a separate meta-cresol reactant.The process comprises subjecting the cresol mixture to nitration, whereby para-nitro-meta-cresol is formed, and then separating the para-nitro-meta-cresol from the resulting nitration reaction mixture.In one embodiment, the cresol mixture is introduced into reaction with an aqueous acid mixture containing HNO.sub.3 and HNO.sub.2 as the only acid ingredients, under defined critical conditions of feed flow rate, temperature, acid concentrations, and reactant proportions to provide the cresol nitration reaction product mixture.

Abstract translation: 从直接可利用的和便宜的间/对甲酚混合物中高产率地制备对硝基间甲酚的方法，而无需首先拆分甲酚混合物以提供单独的间甲酚反应物。

公开(公告)号：US3959395A

公开(公告)日：1976-05-25

申请号：US536271

申请日：1974-12-26

Applicant: Thomas D. Higgins, Jr. ,  Raymond A. Newsom

Inventor： Thomas D. Higgins, Jr. ,  Raymond A. Newsom

IPC: C07C7/04 ,  C07C1/00 ,  C07C7/20 ,  C07C15/44 ,  C07C15/46 ,  C07C67/00 ,  C07C201/00 ,  C07C201/16 ,  C07C205/22 ,  C07C205/23 ,  C07C79/24 ,  C07C37/28

CPC classification number: C07C201/16 ,  C07C7/20

Abstract: A process is provided for recovery and re-use of dinitrophenols employed as inhibitors of polymerization in the distillation and purification of styrene. The styrene still residues commonly referred to as tar or tars are treated with an aqueous hydroxide at a controlled pH, the phases are separated, the aqueous phase is treated with an acid and an organic solvent at a controlled pH and the resulting organic phase is recycled to a suitable point in the styrene purification system. The recycled solution is a more effective inhibitor than the dinitrophenol originally employed.

Abstract translation: 提供了一种在苯乙烯的蒸馏和纯化中用作聚合抑制剂的二硝基苯酚的回收和再利用方法。 通常被称为焦油或焦油的苯乙烯残留物在受控的pH下用氢氧化物水溶液处理，分离各相，水相在受控的pH下用酸和有机溶剂处理，并将所得的有机相回收 到苯乙烯净化系统中的合适点。 回收的溶液比起初使用的二硝基苯酚更有效。

公开(公告)号：US3880942A

公开(公告)日：1975-04-29

申请号：US36800573

申请日：1973-06-07

Applicant: MONSANTO CO

Inventor： HUG DELMAR O ,  GARABEDIAN TANIEL A

IPC: B01D9/00 ,  C07C201/16 ,  C07C79/12

CPC classification number: C07C201/16 ,  B01D9/0013 ,  C07C205/12

Abstract: Improved purity is achieved in a process for separating the isomers of nitro- and halo-substituted aromatic compounds in a mixture of liquid isomers by fractional, surface crystallization from the melt, wherein the isomeric mixture is cooled until crystals form on a cooling surface. The improvement comprises conducting the fractional, surface crystallization on a polymeric, e.g., polytetrafluoroethylene, cooling surface. The process is particularly beneficial for separating paranitrochlorobenzene from a liquid isomeric liquid of ortho-, metaand para-nitrochlorobenzenes.

Abstract translation: 在通过从熔体中分级表面结晶分离液体异构体的混合物中的硝基和卤素取代的芳族化合物的异构体的方法中实现了提高的纯度，其中将异构体混合物冷却直到在冷却表面上形成晶体。 改进包括在聚合物例如聚四氟乙烯冷却表面上进行分数表面结晶。 该方法特别有利于从对 - ，间 - 和对 - 硝基氯苯的液体异构体液体中分离对硝基氯苯。