Purification of PCNB by solvent extraction
    164.
    发明授权
    Purification of PCNB by solvent extraction 失效
    通过溶剂萃取纯化PCNB

    公开(公告)号:US5057222A

    公开(公告)日:1991-10-15

    申请号:US534895

    申请日:1990-06-08

    Applicant: Gary A. Braden

    Inventor: Gary A. Braden

    CPC classification number: B01D11/0492 C07C201/16 Y10S210/909

    Abstract: Pentachloronitrobenzene (PCNB) is purified by using a liquid-liquid extraction process with polar and nonpolar solvents to remove hexachlorobenzene (HCB). A variety of procedures, solvents and equipment may be employed to carry out the process. A process using a multiplate countercurrent liquid solvent extraction unit, and using DMF and octane as solvents for PCNB and HCB, respectively, is preferred.

    Abstract translation: 通过使用极性和非极性溶剂的液 - 液萃取方法纯化五氯硝基苯(PCNB)以除去六氯苯(HCB)。 可以使用各种程序,溶剂和设备来执行该过程。 优选使用多反向液体溶剂萃取单元,分别使用DMF和辛烷作为PCNB和HCB的溶剂的方法。

    Process for the production of dinitrotoluene
    165.
    发明授权
    Process for the production of dinitrotoluene 失效
    生产二硝基甲苯的方法

    公开(公告)号:US5001272A

    公开(公告)日:1991-03-19

    申请号:US402322

    申请日:1989-09-05

    Inventor: Robert W. Mason

    CPC classification number: C07C201/08 C07C201/16

    Abstract: Aromatic nitration reactions and, more specifically, a process for nitrating toluene to dinitrotoluene. The process involves a liquid phase nitration reaction of anhydrous nitric acid and toluene in a molar ratio of between about 5:1 and about 9:1 of nitric acid to toluene in a reactor at a reaction temperature of between about 40.degree. C. and about 70.degree. C., in the absence of sulfuric acid and in the absence of any dipolar organic solvent, to produce a mixture containing dinitrotoluene, and isolating said dinitrotoluene by contacting said mixture with a phase separating effective amount of an alkali or alkaine earth metal nitrate salt to cause phase separation of said dinitrotoluene.

    Abstract translation: 芳香硝化反应,更具体地说,是将甲苯硝化成二硝基甲苯的方法。 该方法包括在反应器中在约40℃至约约40℃的反应温度下,反应器中无水硝酸和甲苯以约5:1至约9:1的硝酸与甲苯的摩尔比进行液相硝化反应 在不存在硫酸的情况下,在不存在任何偶极有机溶剂的情况下,制备含有二硝基甲苯的混合物,并通过使所述混合物与相分离有效量的碱金属或碱土金属的硝酸盐相分离来分离所述二硝基甲苯 盐引起所述二硝基甲苯的相分离。

    Selective recovery of a nitrophenolic by-product from nitration waste
water by precipitation
    166.
    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

    CPC classification number: C07C201/16 Y10S210/909

    Abstract: 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.

    Abstract translation: 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。

    Separation of nitrobenzaldehyde isomers
    167.
    发明授权
    Separation of nitrobenzaldehyde isomers 失效
    硝基苯甲醛异构体的分离

    公开(公告)号:US4714783A

    公开(公告)日:1987-12-22

    申请号:US861792

    申请日:1986-05-12

    CPC classification number: C07C201/16

    Abstract: A process for separating ortho- or meta-nitrobenzaldehyde from a feed mixture comprising ortho-nitrobenzaldehyde or metal-nitrobenzaldehyde and at least one other isomer from which the ortho- or metal-isomer is to be separated. The feed mixture is contacted at adsorption conditions with meta-selective adsorbent comprising a type X zeolite having sodium or lithium cations at exchangeable cationic sites or with an ortho-selective adsorbent comprising a type Y zeolite having alkali metal or alkaline earth metal cations at exchangeable cationic sites or a phosphate-substituted crystalline, aluminum silicate zeolite. Preferred desorbents are lower alkyl acetates and formates, acetonitrile and benzaldehyde.

    Abstract translation: 从包含邻硝基苯甲醛或金属 - 硝基苯甲醛的进料混合物中分离出邻位或间硝基苯甲醛的方法和至少一种异构体,其中邻位或金属异构体将被分离。 进料混合物在吸附条件下与包含具有可交换阳离子位点的钠或锂阳离子的X型沸石的元选择性吸附剂接触,或者与包含具有可交换阳离子的碱金属或碱土金属阳离子的Y型沸石的邻位选择性吸附剂接触 位点或磷酸盐取代的结晶硅酸铝沸石。 优选的脱附剂是低级烷基乙酸酯和甲酸酯,乙腈和苯甲醛。

    Process for separating nitroaromatic compounds from spent nitric acid
    168.
    发明授权
    Process for separating nitroaromatic compounds from spent nitric acid 失效
    将硝基芳族化合物与废硝酸分离的方法

    公开(公告)号:US4642396A

    公开(公告)日:1987-02-10

    申请号:US638436

    申请日:1984-08-07

    CPC classification number: C07C201/16 C01B21/36

    Abstract: This invention pertains to a process for extracting a nitroaromatic composition from a nitration medium containing nitric acid, water, and nitroaromatic. The process comprises contacting the nitration medium with nitric oxide under conditions such that the nitric oxide will react with the nitric acid to form nitrogen dioxide and water. Gaseous nitrogen dioxide is removed from the reaction medium and accordingly, the dissolved nitroaromatic present in the nitration medium separates to form an organic phase which then can be removed by decantation. Typically, one mole of nitric oxide is added to the nitration medium for every two moles of nitric acid present in said medium. Reaction conditions normally are from about 0.degree. to 90.degree. C.

    Abstract translation: 本发明涉及从含硝酸,水和硝基芳族化合物的硝化介质中提取硝基芳族组合物的方法。 该方法包括使硝化介质与一氧化氮接触,使得一氧化氮将与硝酸反应形成二氧化氮和水。 从反应介质中除去气态二氧化氮,因此,硝化介质中溶解的硝基芳族化合物分离形成有机相,然后可通过倾析除去有机相。 通常,对于存在于所述介质中的每两摩尔硝酸,向硝化介质中加入1摩尔一氧化氮。 反应条件通常为约0〜90℃

    Crystal purification
    170.
    发明授权
    Crystal purification 失效
    水晶净化

    公开(公告)号:US4421937A

    公开(公告)日:1983-12-20

    申请号:US336549

    申请日:1982-01-04

    Applicant: Dan K. Lynch

    Inventor: Dan K. Lynch

    Abstract: Mixtures of crystals and a liquid, ordinarily comprising the mother liquor of the crystals are continuously separated by feeding the mixture into a screw type press having drainage apperatures, thereby subjecting the crystals with the mother liquor entrapped therein to pressures sufficient to substantially reduce the interstitial space between crystals. Reduction of the interstitial space causes the mother liquor to be forced out of the drainage aperatures thus purifying the crystals. This achieves a more effective separation of mother liquor from the crystals than can be achieved by gravity or the use of a device such as a centrifuge and eliminates the need for a foreign solvent to wash the mother liquor from the crystals.

    Abstract translation: 通常将晶体和液体的混合物连续分离,通过将混合物进料到具有排出温度的螺杆式压力机中,从而使包含在其中的母液的晶体经受足以大大降低间隙空间的压力 晶体之间。 间隙空间的减少导致母液被排出排水孔,从而净化晶体。 这实现了母液比晶体更有效的分离,可以通过重力或使用诸如离心机的装置来实现,并且不需要外来溶剂从晶体中洗涤母液。

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