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    Purification of pentaerythritol trinitrate by crystallization
    32.
    发明授权
    Purification of pentaerythritol trinitrate by crystallization 失效
    通过结晶纯化三硼酸三戊酯

    公开(公告)号：US3806578A

    公开(公告)日：1974-04-23

    申请号：US4010060

    申请日：1960-06-30

    Applicant: DU PONT

    Inventor： BRENNECKE H

    IPC: C07C201/02 ,  C07C77/02

    CPC classification number: C07C201/02 ,  C07C203/04

    Abstract: 1. A process for the purification of pentaerythritol trinitrate which comprises adding water to a solution of pentaerythritol trinitrate in methylene chloride, cooling, with agitation, the mixture thus formed to a temperature between about -10* and about +10*C., and separating the purified pentaerythritol trinitrate in the form of hydrate crystals from the solution, the weight ratio of said methylene chloride being between about 0.5 and about 2 parts for each part of pentaerythritol trinitrate and the weight ratio of said water being at least 1 part for each 50 parts of pentaerythritol trinitrate.

    Abstract translation: 1.一种用于纯化季戊四醇三硝酸酯的方法，其包括向季戊四醇三硝酸酯的二氯甲烷溶液中加入水，在搅拌下冷却，将混合物形成至约-10℃至约+10℃的温度， 从溶液中分离纯化的季戊四醇三水合物形式的季戊四醇三水合物，对于每份季戊四醇三硝酸酯，所述二氯甲烷的重量比为约0.5至约2份，所述水的重量比对于每种季铵盐至少为1份 50份季戊四醇三硝酸酯。

    Process for production of 1-oxo-2-nitratocycloalkanes
    36.
    发明授权
    Process for production of 1-oxo-2-nitratocycloalkanes 失效
    1-氧代-2-硝基杂环烷烃的制备方法

    公开(公告)号：US3095442A

    公开(公告)日：1963-06-25

    申请号：US15265761

    申请日：1961-11-15

    Applicant: DU PONT

    Inventor： JOHN ARTHUR WILFRED

    IPC: C07C201/02 ,  C07C203/08

    CPC classification number: C07C203/08

    Abstract: The invention comprises 1-oxo-2-nitrato-cycloalkanes, e.g., 1-oxo-2-nitratocyclohexane, which may be made by reacting a cycloalkene with nitrogen dioxide in a liquid saturated hydrocarbon reaction medium at a temperature of -15 DEG to +25 DEG C. The product is usually immiscible with the hydrocarbon reaction medium and is allowed to form a lower layer which is separated by decantation. The nitrogen dioxide may be added directly to a solution of the cycloalkene, or a solution of the cycloalkene in a hydrocarbon may be added to a solution of nitrogen dioxide in the same solvent. Preferably a solution containing 45% by volume of the cycloalkene in the hydrocarbon solvent is added to a cooled and stirred solution of 3 volumes of liquid nitrogen dioxide in 4 volumes of the solvent and a stream of air or oxygen-containing gas is bubbled through the mixture. The cycloalkenes include cyclopentene, cyclohexene, cycloheptene, methyl cyclopentenes methyl cyclohexene or methyl cycloheptene and other alkyl derivatives in which each ring contains one, two or three substituents each having 1-20 carbon atoms. Specification 974,152 is referred to.

    Abstract translation: 本发明包括1-氧代-2-硝基 - 环烷烃，例如1-氧代-2-硝基环己烷，其可以通过使环烯烃与二氧化氮在液体饱和烃反应介质中在-15℃至+ 25℃。产物通常与烃反应介质不混溶，并允许形成通过倾析分离的下层。 二氧化氮可以直接加入到环烯烃的溶液中，或者将环烯烃在烃中的溶液加入到二氧化氮在相同溶剂中的溶液中。 优选将含有45体积％的环烯烃在烃溶剂中的溶液加入到3体积的液体二氧化氮在4体积的溶剂中的冷却和搅拌的溶液中，并将空气或含氧气体流鼓泡通过 混合物。 环烯烃包括环戊烯，环己烯，环庚烯，甲基环戊烯甲基环己烯或甲基环庚烯和其中每个环含有一个，两个或三个各自具有1-20个碳原子的取代基的其它烷基衍生物。 参考规格974,152。

    Manufacture of an alkyl nitrate
    38.
    发明授权
    Manufacture of an alkyl nitrate 失效
    制备硝酸烷基酯

    公开(公告)号：US2647914A

    公开(公告)日：1953-08-04

    申请号：US23127251

    申请日：1951-06-12

    Applicant: ICI LTD

    Inventor： ALLAN WILLIAM G ,  TOBIN THOMAS J

    IPC: C07C201/02

    CPC classification number: C07C203/04 ,  C07C201/02

    Abstract: A process for the continuous production of isopropyl nitrate by the continuous distillation of a mixture of easily volatile products from a boiling reaction mixture formed from nitric acid and isopropyl alcohol and into which separate streams of nitric acid and isopropyl alcohol are introduced and in which a urea concentration effective to destroy nitrous acid is maintained is characterized in that there is passed through said boiling reaction mixture undergoing continuous distillation a stream of gas chemically indifferent to it. The indifferent gas may be, e.g., air, nitrogen, carbon dioxide or steam. The isopropyl alcohol and also the nitric acid introduced into the reaction mixture may contain urea. In an example aqueous isopropyl alcohol and nitric acid, both containing urea, are fed into a reactor containing heated aqueous nitric acid also containing urea whilst air is passed through the reaction mixture. Crude isopropyl nitrate is continuously separated from the aqueous distillate. Isopropyl alcohol may be recovered from the aqueous layer of the condensate by fractional distillation after neutralizing the nitric acid present. Specification 379,312 is referred to.

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