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    CONTINUOUS SYNTHESIS OF ISOOCTYL NITRATE IN A FLOW REACTOR
    81.
    发明申请
    CONTINUOUS SYNTHESIS OF ISOOCTYL NITRATE IN A FLOW REACTOR 有权
    在流动反应器中连续合成硝酸亚硝酯

    公开(公告)号：US20170066710A1

    公开(公告)日：2017-03-09

    申请号：US15123100

    申请日：2015-03-05

    Applicant: Corning Incorporated

    Inventor： Bing Ma ,  Wei Shen ,  Yanhua Wang ,  Mo Zhang

    IPC: C07C201/02

    CPC classification number: C07C201/02 ,  C07C203/04

    Abstract: A process for synthesizing isooctyl nitrate in a continuous flow reactor comprises flowing a H2SO4—HNO3 mixture within a flow reactor, flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4—HNO3 mixture and produce a reaction mixture stream flowing in said reactor, maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range −10° to 35° C. inclusive, and wherein the residence time of the reaction mixture stream in the flow reactor is greater than or equal to 5 seconds and less than or equal to 40 seconds, and wherein the H2SO4 of the H2SO4—HNO3 mixture is H2SO4 having a concentration of in the range of 85 to 95% inclusive, more desirably 88 to 92% inclusive, most desirably of 90%.

    Abstract translation: 在连续流动反应器中合成硝酸异辛酯的方法包括使流动反应器内的H 2 SO 4 -HNO 3混合物流动，将异辛醇流入所述流动反应器中，以将异辛醇与H 2 SO 4 -HNO 3混合物混合，并产生流动的反应混合物流 在所述反应器中，将反应混合物流保持在​​所述流动反应器中，反应温度在-10℃至35℃的范围内，其中反应混合物流在流动反应器中的停留时间大于或等于 等于5秒且小于或等于40秒，并且其中H 2 SO 4 -HNO 3混合物的H 2 SO 4为浓度为85-95％（含）范围内的H 2 SO 4，更优选为88-92％，最优选为 90％。

    Novel Method for Directly Nitration of OH-, SH-and NHR-Functions in Organic Molecules by Means of in Situ Generated Carbonic Acid Dinitrate
    83.
    发明申请
    Novel Method for Directly Nitration of OH-, SH-and NHR-Functions in Organic Molecules by Means of in Situ Generated Carbonic Acid Dinitrate 审中-公开
    通过原位生成的硝酸二苯酯在有机分子中直接硝化OH-，SH-和NHR-功能的新方法

    公开(公告)号：US20120232257A1

    公开(公告)日：2012-09-13

    申请号：US13390311

    申请日：2010-10-04

    Applicant: Nikolas Pietrzik

    Inventor： Nikolas Pietrzik

    IPC: C07C201/02 ,  C07H5/04 ,  C07H1/00 ,  C07C203/04 ,  C07D251/06 ,  C08B5/02 ,  C07H7/02

    CPC classification number: C07B43/02 ,  C07C313/36 ,  C07D251/06 ,  C07H9/04

    Abstract: The invention relates to a nitration method having the following principles: a phosgene species is converted with two equivalent silver nitrates into a double-mixed anhydride of carbonic acid and nitric acid, known here as carbonic acid dinitrate (I). Said operation is carried out in situ, and the formed dinitrate decomposes spontaneously. In addition to carbon dioxide, nitrate ions and nitronium ions are formed, said ions comprising electrophiles which are necessary for nitration. The solution which is used is acetonitrile, and is insignificant if the alcohol species is dissolved or suspended. The necessary equivalent silver nitrates are introduced into the system and optionally heated or cooled to the desired temperature. Subsequently, the acid chloride is introduced slowly, drop by drop or slowly little by little. Phosgene, diphosgene, triphosgene and chloroformic acid ester can be used as carbonic acid dichloride and monochloride, and their thiocarbonic acid analogues. A brown colouration and precipitated silver chloride display the formation of the carbonic acid reactants, said brown colouration rapidly discolouring due to an immediate reaction of the nitronium ions with the substrate with is to be nitrated. Towards the end of the addition of phosgene, the brown colouration remains for longer and longer until it no longer disappears. Then, it is stirred for another hour at room temperature. In the event of high acid-sensitive educts, non-nucleophilic nitrogen bases such as DBU can be added to the system in order to intercept the formation of nitric acid.

    Abstract translation: 本发明涉及一种具有以下原理的硝化方法：将光气物质用两当量的硝酸银转化成碳酸和硝酸的双重混合酸酐，这里称为硝酸二苯酯（I）。 所述操作在原位进行，形成的硝酸酯自发分解。 除了二氧化碳之外，还形成硝酸根离子和硝鎓离子，所述离子包含硝化所必需的亲电体。 使用的溶液是乙腈，如果醇类物质溶解或悬浮，则不重要。 将必需的相当的硝酸银引入体系中，并任选地加热或冷却至所需温度。 随后，缓慢逐滴引入酰氯，或逐渐缓缓地引入。 光气，双光气，三光气和氯甲酸酯可用作二氯化碳和一氯化碳及其硫代碳酸类似物。 棕色着色和沉淀的氯化银显示碳酸反应物的形成，棕色着色由于硝基离子与底物立即反应而迅速变色将被硝化。 在加入光气结束时，棕色着色会持续更长时间，直至不再消失。 然后在室温下再搅拌1小时。 在酸敏感性离析物高的情况下，可以向体系中加入非亲核性氮碱如DBU，以拦截硝酸的形成。

    Process and reaction vessel for production of alkyl nitrite
    86.
    发明授权
    Process and reaction vessel for production of alkyl nitrite 失效
    用于生产亚硝酸烷基酯的方法和反应容器

    公开(公告)号：US4908466A

    公开(公告)日：1990-03-13

    申请号：US102367

    申请日：1987-09-29

    Applicant: James R. Nelson

    Inventor： James R. Nelson

    IPC: C07C201/02 ,  B01D3/00 ,  C07C67/00 ,  C07C201/00 ,  C07C201/04 ,  C07C203/00 ,  C07C203/02 ,  C07C203/04

    CPC classification number: B01D3/009 ,  C07C201/04 ,  Y02P20/127

    Abstract: A process and reaction vessel for producing alkyl nitrite is disclosed the process comprising (a) contacting nitric oxide, lower alcohol and oxygen in a reaction zone such that alkyl nitrite is formed, said reaction zone comprising a reactor section and a rectification section, (b) supplying a liquid scrubbing agent to an upper portion of the rectification section, (c) withdrawing a gaseous alkyl nitrite product stream from the upper portion of the rectification section, and (d) withdrawing a liquid stream from a lower portion of the reactor section. The reactor section provides intimate vapor-liquid contact sufficient to enhance the conversion of nitric oxide to alkyl nitrite and the rectification section provides sufficient vapor residence time to enhance conversion of oxygen, as well as sufficient rectification capabilities to reduce the amounts of water and nitric acid in the gaseous alkyl nitrite product stream.

    Continuous closed loop nitration of polyhydric alcohols
    88.
    发明授权
    Continuous closed loop nitration of polyhydric alcohols 失效
    多元醇的连续闭环硝化

    公开(公告)号：US4251455A

    公开(公告)日：1981-02-17

    申请号：US35754

    申请日：1979-05-03

    Applicant: Hans-Jurgen Gebauer

    Inventor： Hans-Jurgen Gebauer

    IPC: C07C201/02 ,  C07C77/02

    CPC classification number: C07C201/02

    Abstract: A process for the continuous manufacture of a nitric acid ester of a polyhydric alcohol by reacting the polyhydric alcohol with nitrating acid, comprising circulating a stream of waste nitrating acid through a closed loop, injecting nitrosulphuric acid into said circulating stream, cooling the stream downstream of the injection, feeding the alcohol via a mixer into the cooled stream, cooling the stream to remove heat produced by reaction, and separating nitrated polyhydric alcohol from the loop, along with sufficient waste acid to keep the volume in the loop substantially constant, circulation being carried out at a rate such that the average residence time of waste acid in the loop is less than about 15 minutes, preferably about 2 to 5 minutes. This avoids the prolonged storage of large quantities of waste acid which is inherently dangerous. When the system is to be shut down all the circulating waste acid can be replaced by fresh nitrosulphuric acid, relatively small in volume.

    Abstract translation: 一种通过使多元醇与硝酸反应来连续制造多元醇硝酸酯的方法，其包括使废硝酸酸流循环通过闭环，将亚硝基硫酸注入所述循环流中，冷却流 注射，通过混合器将醇进料到冷却的流中，冷却流以除去由反应产生的热量，并将硝化的多元醇与环分离，以及足够的废酸以保持循环中的体积基本上恒定，循环为 以使得循环中废酸的平均停留时间小于约15分钟，优选约2至5分钟的速率进行。 这避免了长期储存大量本来危险的废酸。 当系统关闭时，所有的循环废酸可以用新鲜的亚硫酸替代，体积相对较小。

    Process for preparation of pentolite
    89.
    发明授权
    Process for preparation of pentolite 失效
    制备PENTOLITE的方法

    公开(公告)号：US3580754A

    公开(公告)日：1971-05-25

    申请号：US3580754D

    申请日：1969-05-01

    Applicant: DU PONT

    Inventor： BARNHARD PHILIP

    IPC: C06B21/00 ,  C06B25/32 ,  C07C201/02 ,  C06B3/00

    CPC classification number: C06B25/32 ,  C06B21/0008 ,  C07C201/02 ,  C07C203/04

    Abstract: PROCESS FOR THE PREPARATION OF STABLE PENTOLITE FROM CRUDE PENTAERYTHRITOL TETRANITRATE COMPRISING AGITATING IN WATER A MIXTURE OF MOLTEN TRINITROPOTOLUENE AND CRUDE PENTAERYTHRITOL TETRANITRATE AT A TEMPERATURE ABOVE THE MELTING POINT OF THE TRINITROTOLUENE AND BELOW THE MELTING POINT OF THE PENTAERYTHRITOL TETRANITRATE, WHILE MAINTAINING THE PH OF THE WATER IN THE RANGE FROM 7 TO ABOUT 10, FOLLOWED BY SEPARATING THE PENTOLITE FROM THE AQUEOUS PHASE.

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