Preparation of p-nitrophenolic compounds
    71.
    发明授权
    Preparation of p-nitrophenolic compounds 失效
    对硝基酚类化合物的制备

    公开(公告)号:US5414148A

    公开(公告)日:1995-05-09

    申请号:US249200

    申请日:1994-05-26

    CPC classification number: C07C201/00 C07C201/08

    Abstract: p-Nitrophenolic compounds, e.g., p-nitrophenol itself, are selectively prepared by (a) reacting a phenolic compound with a nitrosating agent in the presence of sulfuric acid, the concentration of which H.sub.2 SO.sub.4 being at least 60%, (b) oxidizing the p-nitrosophenolic compound thus formed with nitric acid, the concentration of sulfuric acid in the medium of reaction, upon completion of oxidation, being no greater than 80%, and (c) separating the p-nitrophenolic compound which thus precipitates.

    Abstract translation: 通过(a)在硫酸存在下使酚类化合物与亚硝化剂反应,其中H 2 SO 4的浓度为至少60%,(b)将硝基酚类化合物氧化为 由硝酸形成的对亚硝基苯酚化合物,氧化后的反应介质中的硫酸浓度不大于80%,(c)分离因此析出的对硝基酚化合物。

    Process for the preparation of dinitrotoluene
    72.
    发明授权
    Process for the preparation of dinitrotoluene 失效
    制备二硝基甲苯的方法

    公开(公告)号:US5345012A

    公开(公告)日:1994-09-06

    申请号:US147654

    申请日:1993-11-03

    CPC classification number: C07C201/08

    Abstract: A continuous process for the preparation of isomeric mixtures of dinitrotoluene by a single stage nitration of toluene under adiabatic conditions. The reaction enthalpy is used for the removal by distillation of the water of reaction formed during nitration. In this process, toluene is reacted with a nitrating acid having from about 80 to about 100% by weight of an inorganic component having a specified composition and from about 0 to about 20% by weight of an organic component having a specified composition.

    Abstract translation: 在绝热条件下通过单阶段甲苯硝化甲苯制备二硝基甲苯的异构体混合物的连续方法。 反应焓用于通过蒸馏除去硝化过程中形成的反应的水。 在该方法中,甲苯与具有约80至约100重量%的具有指定组成的无机组分和约0至约20重量%的具有指定组成的有机组分的硝酸反应。

    Process for preparing dinitrotoluene
    73.
    发明授权
    Process for preparing dinitrotoluene 失效
    二硝基甲苯制备方法

    公开(公告)号:US5302763A

    公开(公告)日:1994-04-12

    申请号:US24052

    申请日:1993-03-01

    CPC classification number: C07C201/08

    Abstract: Improved process for preparing dinitrotoluene by reacting toluene with concentrated nitric acid. The process reacts toluene with a large excess of concentrated nitric acid, in the presence of a select hydrated nitrate salt which is effective in minimizing explosive hazards, to produce a product which has substantially reduced by-product content.

    Abstract translation: 通过甲苯与浓硝酸反应制备二硝基甲苯的改进方法。 在有选择的水合硝酸盐的存在下,该方法使甲苯与大量过量的浓硝酸反应,所述硝酸盐选择有效地使爆炸危险最小化,以产生具有显着降低的副产物含量的产物。

    Process for preparing dinitrotoluene with low by-product content
    74.
    发明授权
    Process for preparing dinitrotoluene with low by-product content 失效
    制备低副产物含量的二硝基甲苯的方法

    公开(公告)号:US5245092A

    公开(公告)日:1993-09-14

    申请号:US944639

    申请日:1992-09-14

    CPC classification number: C07C201/08

    Abstract: Process for preparing dinitrotoluene by reacting toluene with concentrated nitric acid. The process reacts toluene with a large excess of concentrated nitric acid at selected conditions to produce a product which has substantially reduced by-product content.

    Abstract translation: 通过甲苯与浓硝酸反应制备二硝基甲苯的方法。 该方法在选定的条件下使甲苯与大量浓缩的硝酸反应,以产生具有显着降低的副产物含量的产物。

    Regioselective nitration of diphenyl compounds
    76.
    发明授权
    Regioselective nitration of diphenyl compounds 失效
    二苯基化合物的区域选择性硝化

    公开(公告)号:US5037994A

    公开(公告)日:1991-08-06

    申请号:US477243

    申请日:1990-02-08

    CPC classification number: C07C209/36 C07C2/861 C07C201/08

    Abstract: A regioselective nitration process for diphenyl compounds which can be carried out at about ambient temperature in which each ring of the diphenyl compound is selectively nitrated in the para position to form the corresponding di(4-nitrophenyl) compound. Such compounds as diphenyl carbonate, 2,2-diphenylpropane, 2,2-diphenylhexafluoropropane, diphenyl sulfide, diphenyl ketone, diphenyl sulfone, and the like can be converted to an isomeric mixture containing an enhanced amount of the corresponding di(4-nitrophenyl) compound, which mixture may be reduced or purified and reduced to the di(4-aminophenyl) analogues for use in the manufacture of polyamides, polyimides, and polyamide-imides.

    Abstract translation: 二苯基化合物的区域选择性硝化方法,其可以在约环境温度下进行,其中每个环的二苯基化合物在对位选择性硝化以形成相应的二(4-硝基苯基)化合物。 作为碳酸二苯酯,2,2-二苯基丙烷,2,2-二苯基六氟丙烷,二苯基硫醚,二苯基酮,二苯基砜等的化合物,可以转化成含有相应的二(4-硝基苯基) 化合物,该混合物可以被还原或纯化并还原成二(4-氨基苯基)类似物,用于制造聚酰胺,聚酰亚胺和聚酰胺 - 酰亚胺。

    Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from
3,5-dichloranisole
    77.
    发明授权
    Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from 3,5-dichloranisole 失效
    由3,5-二氯苯甲醚制备1,3,5-三氨基-2,4,6-三硝基苯

    公开(公告)号:US4952733A

    公开(公告)日:1990-08-28

    申请号:US289653

    申请日:1988-12-21

    CPC classification number: C07C201/12 C07C201/08 C07C209/10

    Abstract: Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB.

    Abstract translation: 由3,5-二氯苯甲醚制备1,3,5-三氨基-2,4,6-三硝基苯(TATB)。 在相对温和的条件下硝化3,5-二氯苯甲醚,得到3,5-二氯-2,4,6-三硝基苯甲醚,产率高,纯度高。 该后一种化合物的溶解得到所需的TATB。 通过用亚硫酰氯和二甲基甲酰胺处理3,5-二氯-2,4,6-三硝基苯甲醚,得到1,3,5-三氯-2,4,6-三硝基苯,通过TATB的另一条路线。 该产品的解淀粉生成TATB。

    Laser-induced nitration
    79.
    发明授权
    Laser-induced nitration 失效
    激光诱导硝化

    公开(公告)号:US4908110A

    公开(公告)日:1990-03-13

    申请号:US340815

    申请日:1989-04-17

    CPC classification number: B01J19/121 C07C201/08 C07C205/02

    Abstract: Infrared laser-induced production of nitrated products is achieved by irradiating compounds selected from propane, n-butane, isobutane, n-pentane, and cyclopropane in the gas phase while in a stainless steel cell 5.times.5.times.10 cm equipped with zinc selenide windows to admit the infrared laser radiation in the range of 10.4 or 9.4 micrometers provided by a continuous wave CO.sub.2 laser. KC1 windows on the short path are to monitor infrared spectra of reactants and products. Nitrogen dioxide or nitric acid is present as the second reactant and the nitrating agent. The infrared laser-induced method far exceeds the yield of nitrated products found in the argon-ion laser-induced nitration of isobutane reported in the literature. Applicants' method at least equals the yield from thermally activated systems with a minimum formation of undesirable side products. A representative sample, 220 torr of gaseous butane, and 20 torr NO.sub.2 is irradiated in one experiment for 30 seconds with 75 W/cm.sup.2 at a frequency of 956 cm.sup.-1. About 40% of the NO.sup.2 is converted to nitrocompounds. Identified as nitro-products are nitromethane, nitroethane, 1-nitropropane, 1-nitrobutane and 2-nitrobutane. More than 60% of the nitro-products are in the long chain forms, 1-nitrobutane and 2-nitrobutane. Pressure of the NO.sub.2 reactant range from about 20 to 30 torr while the hydrocarbon reactant pressure range from about 200 to about 500 torr. Irradiation times ranges from about 30 to about 60 seconds. Laser powers range from 75 watts/cm.sup.2 to about 82 watts/cm.sup.2.

    Abstract translation: 通过在气相中照射选自丙烷,正丁烷,异丁烷,正戊烷和环丙烷的化合物来实现硝化产物的红外激光诱导产生,同时在5×5×10cm的装有硒化锌窗口的不锈钢电池中容纳红外线 激光辐射范围为10.4或9.4微米,由连续波CO2激光器提供。 短路上的KC1窗口是监测反应物和产物的红外光谱。 存在二氧化氮或硝酸作为第二反应物和硝化剂。 红外激光诱导的方法远远超过文献报道的氩离子激光诱导的异丁烷硝化中发现的硝化产物的产率。 申请人的方法至少等于热活化系统的产量,最少形成不希望的副产品。 一个代表性的样品,220托的气态丁烷和20托的NO 2在一个实验中以75W / cm 2的频率在956cm -1处照射30秒。 约40%的NO2转化为硝基化合物。 硝基甲烷,硝基乙烷,1-硝基丙烷,1-硝基丁烷,2-硝基丁烷等。 硝基产物超过60%是长链形式,1-硝基丁烷和2-硝基丁烷。 NO 2反应物的压力范围为约20至30托,而烃反应物压力范围为约200至约500托。 照射时间范围为约30至约60秒。 激光功率范围为75瓦特/平方厘米至约82瓦特/平方厘米。

    Nitration processes
    80.
    再颁专利
    Nitration processes 失效
    硝化过程

    公开(公告)号:USRE33168E

    公开(公告)日:1990-02-20

    申请号:US214932

    申请日:1988-07-05

    CPC classification number: C07C209/76 C07C201/08

    Abstract: The present invention relates to improvements in processes of preparing dinitrated .[.aromatic compounds, particularly dinitrated aniline and dinitrated substituted aniline compounds, employing relatively dilute and then more concentrated nitric acid as the nitrating agent.]. .Iadd.aniline and substituted phenol compounds in a two-step process, employing, in the first or mononitration step the spent nitric acid from the second of dinitration step. .Iaddend.

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