Co-production of an aromatic monoamine and an aromatic diamine directly
from benzene or a benzene derivative through controlled nitration and
reduction
    1.
    发明授权
    Co-production of an aromatic monoamine and an aromatic diamine directly from benzene or a benzene derivative through controlled nitration and reduction 失效
    通过控制硝化和还原从苯苯或苄苯衍生物直接合成芳族单胺和芳族二胺

    公开(公告)号:US5081303A

    公开(公告)日:1992-01-14

    申请号:US341743

    申请日:1989-04-21

    CPC分类号: C07C201/08 C07C209/36

    摘要: A two-stage process for the co-production of aniline and m-phenylenediamine where, in the first stage, benzene, nitric acid, and sulfuric acid are reacted in a liquid phase to produce in greater amounts nitrobenzene (approximately 70%) and m-dinitrobenzene (approximately 30%), and in lesser or trace amounts o-dinitrobenzene and p-dinitrobenzene, and water; and in the second stage the products of the first stage are reacted with hydrogen in the liquid phase to produce aniline (approximately 70%) and m-phenylenediamine (approximately 30%) in greater amounts, and o-phenylenediamine and p-phenylenediamine in lesser amounts, and water. The reaction products are separated by distillation. The first stage of a preferred embodiment of the process is characterized in that a concentrated mixture of nitric acid and sulfuric acid are fed along with mononitrobenzene to a first reactor for producing dinitrobenzene, and then the dilute acid mixture recovered from this first reactor is fed along with benzene to a second reactor for producing the mononitrobenzene used as a reactant in the first reactor. The second stage, which provides the aniline and m-phenylenediamine, is characterized in that the hydrogenation is carried out in the liquid phase with the unpurified reaction products from the first stage.Preferably, the second stage reaction is carried out utilizing a palladium-on-carbon catalyst in an amount of from 0.006 to 0.25 wt. % based on the total weight of the first stage reaction product mixture. The process is applicable to the co-production of other aromatic mono- and diamines.

    摘要翻译: 用于苯胺和间苯二胺共同生产的两阶段方法,其中在第一阶段中,苯,硝酸和硫酸在液相中反应以产生更大量的硝基苯(约70%)和m - 二硝基苯(约30%)和较少或微量的邻硝基苯和对二硝基苯和水; 并且在第二阶段中,第一阶段的产物在液相中与氢气反应以产生更大量的苯胺(约70%)和间苯二胺(约30%),邻苯二胺和对苯二胺在较小的 数量和水。 反应产物通过蒸馏分离。 该方法的优选实施方案的第一阶段的特征在于将硝酸和硫酸的浓缩混合物与一硝基苯一起加入到用于生产二硝基苯的第一反应器中,然后将从该第一反应器回收的稀酸混合物进料 用苯制备第二反应器,用于生产在第一反应器中用作反应物的单硝基苯。 提供苯胺和间苯二胺的第二阶段的特征在于氢化是在第一阶段与未纯化的反应产物在液相中进行的。 优选地,第二阶段反应使用钯 - 碳催化剂进行,其量为0.006-0.25wt。 %,基于第一阶段反应产物混合物的总重量。 该方法适用于其它芳族单胺和二胺的共生产。

    Selective recovery of a nitrophenolic by-product from nitration waste
water by precipitation
    4.
    发明授权
    Selective recovery of a nitrophenolic by-product from nitration waste water by precipitation 失效
    通过沉淀从硝化废水中选择性地回收硝基酚副产物

    公开(公告)号:US4986920A

    公开(公告)日:1991-01-22

    申请号:US377105

    申请日:1989-07-10

    IPC分类号: C07C201/16

    CPC分类号: C07C201/16 Y10S210/909

    摘要: A process of selectively recovering a nitrophenolic by-product, namely 2,4-dinitrophenol and picric acid, from nitration waste water in substantially pure form through the control of the solution pH of the nitration waste water and subsequent precipitation is provided. By adjusting the solution pH of the nitration waste water with an acid to a pH in the range of from about 4.0 to 0.5, the solubility of the selected nitrophenolic by-products is affected and the crystal formation of the individual by-products controlled.

    摘要翻译: 提供了从硝化废水以基本纯净的形式选择性地回收硝基酚副产物即2,4-二硝基苯酚和苦味酸的方法,通过控制溶液的硝化废水的pH和随后的沉淀。 通过用酸将硝酸废水的溶液pH调节至约4.0至0.5的范围内,所选择的硝基酚副产物的溶解度受到影响,并且控制了各个副产物的晶体形成。

    Method for preparation of salts of N-phosphonomethylglycine
    5.
    发明授权
    Method for preparation of salts of N-phosphonomethylglycine 失效
    N-膦酰基甲基甘氨酸盐的制备方法

    公开(公告)号:US4578224A

    公开(公告)日:1986-03-25

    申请号:US622427

    申请日:1984-06-20

    摘要: Disclosed is a method for the preparation of salts of N-phosphonomethylglycine which comprises the steps of (a) reacting hydantoin or a 3-substituted hydantoin, a compound of the formula ##STR1## wherein R is selected from the group consisting of hydrogen, alkyl having from 1 to 10 carbon atoms, aryl having from 6 to 12 carbon atoms, alkylcarbonyl wherein the alkyl group has from 1 to 10 carbon atoms, and arylcarbonyl wherein the aryl group has from 6 to 12 carbon atoms, with paraformaldehyde in the presence of a low molecular weight carboxylic acid at a temperature and for a sufficient period of time to produce a mixture of intermediate products, including the 1-hydroxymethyl derivative of the starting hydantoin; (b) converting said 1-hydroxymethyl derivative to the 1-phosphonomethyl derivative by thereafter adding to the reaction mixture either (i) a substituted phosphorus compound selected from the group consisting of phosphorus trichloride, and phosphorus tribromide; or (ii) adding to the reaction mixture phosphorous acid and a anhydride selected from the group consisting acetic anhydride, propionic anhydride, butyric anhydride, or mixture thereof, and continuing said reaction at a temperature and for a sufficient period of time to cause completion of the reaction to form the 1-phosphonomethyl derivative; and (c) hydrolyzing the 1-phosphonomethylhydantoin product thus formed with a base selected from the group consisting of alkali metal or alkaline earth hydroxide, to produce a salt of N-phosphonomethylglycine.

    摘要翻译: 公开了一种制备N-膦酰基甲基甘氨酸盐的方法,该方法包括以下步骤:(a)使乙内酰脲或3-取代的乙内酰脲,式IMA化合物,其中R选自氢,烷基 具有1至10个碳原子,具有6至12个碳原子的芳基,其中烷基具有1至10个碳原子的烷基羰基和其中芳基具有6至12个碳原子的芳基羰基,在多聚甲醛存在下, 低温分子量羧酸在一段温度和足够的时间内产生包括起始乙内酰脲的1-羟甲基衍生物的中间产物的混合物; (b)将所述1-羟甲基衍生物转化为1-膦酰基甲基衍生物,然后向反应混合物中加入(i)选自三氯化磷和三溴化磷的取代的磷化合物; 或者(ii)向反应混合物中加入亚磷酸和选自乙酸酐,丙酸酐,丁酸酐或其混合物的酸酐,并在一段温度和足够的时间内继续进行该反应,从而完成 形成1-膦酰基甲基衍生物的反应; 和(c)用选自碱金属或碱土金属氢氧化物的碱选择如此形成的1-膦酰基乙内酰脲产物,以产生N-膦酰基甲基甘氨酸的盐。

    Method of curing unsaturated polyester resins at low temperatures
    8.
    发明授权
    Method of curing unsaturated polyester resins at low temperatures 失效
    在低温下固化不饱和聚酯树脂的方法

    公开(公告)号:US4666978A

    公开(公告)日:1987-05-19

    申请号:US802312

    申请日:1985-11-27

    IPC分类号: C08F299/04 C08G63/76

    CPC分类号: C08F299/045

    摘要: Method of promoting the cure of unsaturated polyester resins with a peroxide initiator at room or below room temperatures (low temperatures) by including as a promoter N,N-dimethyl-p-toluidine (DMPT) or a blend of DMPT and N,N-dimethyl-m-toluidine (DMMT) and to the polyester composition containing such promoter. The use of the DMPT or blend of DMPT and DMMT as a promoter provides a fast cure at low temperatures without loss of physical properties of the cured resins.

    摘要翻译: 通过包括助催化剂N,N-二甲基对甲苯胺(DMPT)或DMPT和N,N-二甲基对甲苯胺的共混物,在室温或低于室温(低温)下,用过氧化物引发剂促进不饱和聚酯树脂的固化方法, 二甲基 - 间甲苯胺(DMMT)和含有该促进剂的聚酯组合物。 使用DMPT或DMPT和DMMT的共混物作为助催化剂可以在低温下快速固化,而不损失固化树脂的物理性能。

    Preparation of arylphosphinic acids
    10.
    发明授权
    Preparation of arylphosphinic acids 失效
    芳基次膦酸的制备

    公开(公告)号:US4359431A

    公开(公告)日:1982-11-16

    申请号:US259880

    申请日:1981-05-04

    IPC分类号: C07F9/30 C07F9/48

    CPC分类号: C07F9/304

    摘要: Arylphosphinic acids are prepared by reacting an aromatic compound with phosphorus trichloride in the presence of aluminum chloride to form an aluminum/phosphorus complex and then hydrolyzing the complex with aqueous phosphoric acid to form the arylphosphinic acid as an insoluble phase and a soluble aluminum salt. The arylphosphinic acid and aluminum salt are then easily separated.

    摘要翻译: 芳基次膦酸通过在氯化铝存在下使芳族化合物与三氯化磷反应以形成铝/磷络合物,然后用磷酸水溶液水解络合物以形成作为不溶相的芳基次膦酸和可溶性铝盐来制备。 芳基次膦酸和铝盐容易分离。