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    SAFE METHOD FOR PRODUCING ALKYL NITRATE
    53.
    发明申请
    SAFE METHOD FOR PRODUCING ALKYL NITRATE 有权
    生产硝酸亚烷基酯的安全方法

    公开(公告)号：US20150031909A1

    公开(公告)日：2015-01-29

    申请号：US14374031

    申请日：2012-12-21

    Applicant: SHANDONG LIBAODE CHEMICAL CO., LTD.

    Inventor： Deliang Xu ,  Hengtao Mao

    IPC: C07C201/02

    CPC classification number: C07C201/02 ,  C07C203/04

    Abstract: The present invention provides a method for producing alkyl nitrate. The centrifugal extraction equipment acts as the esterification separator; a mixed acid solution containing sulfuric acid and nitric acid enters from the heavy phase inlet of the centrifugal extraction equipment; alkyl alcohol enters from the light phase inlet of the centrifugal extraction equipment; the feeding molar ratio of alkyl alcohol and nitric acid equals to 1:1.0-3.0; esterification reaction occurs with the mixed acid and alkyl alcohol at a temperature of 10˜60° C. under the rotating speed of 800-2000 r/min; under the action of centrifugal force, the generated coarse ester as a light phase and the spent acid as a heavy phase are separated; coarse ester as a light phase is discharged through the light-phase outlet of the centrifugal extractor; the spent acid as a heavy phase is discharged through the heavy-phase outlet of the centrifugal extractor; after alkali washing and water washing conventionally, coarse ester is dehydrated for drying and purified, then the refining products of alkyl nitrate is obtained. In the method of the present invention, esterification reaction, the separation of reaction products and the spent acid are finished in the same reactor simultaneously, which reduces the contact time of reaction products with the spent acid greatly, avoids the side reaction effectively, and ensures the safety of esterification process.

    Abstract translation: 本发明提供硝酸烷基酯的制造方法。 离心萃取设备作为酯化分离器; 含有硫酸和硝酸的混合酸溶液从离心萃取设备的重相入口进入; 烷基醇从离心萃取设备的轻相进口进入; 烷基醇和硝酸的进料摩尔比等于1：1.0-3.0; 在混合酸和烷基醇的温度为10〜60℃，以800〜2000r / min的转速进行酯化反应; 在离心力作用下，生成的粗酯为轻质相，废酸为重相分离; 粗酯作为轻相通过离心萃取器的光相出口排出; 作为重相的废酸通过离心萃取器的重相出口排出; 在碱洗和水洗常规之后，将粗酯脱水干燥和纯化，得到硝酸烷基酯的精制产物。 在本发明的方法中，酯化反应，反应产物和废酸的分离同时在同一反应器中完成，这大大降低了反应产物与废酸的接触时间，有效避免了副反应，确保了 酯化过程的安全性。

    Process For Preparing Halogenoalkylnitrates
    57.
    发明申请
    Process For Preparing Halogenoalkylnitrates 失效
    制备卤代烷基硝酸盐的方法

    公开(公告)号：US20080004463A1

    公开(公告)日：2008-01-03

    申请号：US11667970

    申请日：2005-11-09

    Applicant: Romano Rivolta ,  Peter Finlander

    Inventor： Romano Rivolta ,  Peter Finlander

    IPC: C07C203/04 ,  C07C201/02

    CPC classification number: C07C203/04

    Abstract: A process for preparing a compound of formula (I) X-(CH2)n-ONO2  (I)wherein: X is a halogen atom selected from Cl, Br, I; n is an integer from 3 to 6; said process comprising the slow addition of a compound of formula (II) X-(CH2)n-OH  (II) wherein X and n are as defined above to a nitrating agent selected from the group consisting of concentrated nitric acid/concentrated sulfuric acid (sulfonitric mixture), nitric acid alone, NaNO2 in trifluoroacetic acid, nitronium salts such as NO2BF4 and an organic solvent selected from the group consisting of CH2Cl2, CHCl3, CCl4, perfluorohexane, perfluoroheptane. The invention refers also to solutions containing: a compound of general formula (I) and a solvent selected from the group consisting of CH2Cl2, CHCl3, CCl4, perfluorohexane, perfluoroheptane, characterized in that the compound of formula (I) is present in a concentration not higher than 20% by weight.

    Abstract translation: 制备式（I）化合物的方法<？in-line-formula description =“In-line Formulas”end =“lead”？> X-（CH 2 N 2）n （I）<？in-line-formula description =“In-line Formulas”end =“tail”？>其中：X是选自Cl， Br，I n为3〜6的整数， 所述方法包括缓慢加入式（II）化合物<？in-line-formula description =“In-line Formulas”end =“lead”→> X-（CH 2/2） 其中X和n如上所定义，选自组中的硝化剂，其中X和n如上所定义， 由浓硝酸/浓硫酸（磺化混合物），硝酸单独，三氟乙酸中的NaNO 2，硝酸盐如NO 2 BF 4， / SUB>和选自CH 2/2 Cl 2，CHCl 3，CCl 4，/ SO 3的有机溶剂 >，全氟己烷，全氟庚烷。 本发明还涉及包含通式（I）的化合物和选自CH 2 2 Cl 2，CHCl 3， 全氟己烷，全氟庚烷，其特征在于式（I）化合物的浓度不高于20重量％。

    Nitration of organic compounds and organic nitrogen compounds produced
    58.
    发明授权
    Nitration of organic compounds and organic nitrogen compounds produced 失效
    生成有机化合物和有机氮化合物的硝化

    公开(公告)号：US4496783A

    公开(公告)日：1985-01-29

    申请号：US489467

    申请日：1983-04-28

    Applicant: Ian M. Campbell ,  Donald L. Baulch ,  Gary J. Audley

    Inventor： Ian M. Campbell ,  Donald L. Baulch ,  Gary J. Audley

    IPC: C07B43/00 ,  C07B31/00 ,  C07C67/00 ,  C07C201/00 ,  C07C201/02 ,  C07C201/04 ,  C07C201/08 ,  C07C203/00 ,  C07C203/02 ,  C07C205/02 ,  C07C79/02

    CPC classification number: C07C201/08 ,  C07C201/02 ,  C07C201/04

    Abstract: Nitration of organic compounds and organic nitrogen compounds produced.Organic nitrogen compounds are formed in the vapor phase by organic radical formation by reaction of an organic compound with hydroxyl radicals derived from the reaction between hydrogen peroxide and nitrogen dioxide and the nitration of the organic radicals, suitably with nitrogen dioxide. The process may be conducted as a single stage process using an excess of nitrogen dioxide over that required for hydroxyl radical formation. The production of hydroxyl radicals is maximized by the use of a catalytic solid surface such as a solid acid or an acidic oxide or mixed oxide. The product may be a mixture of some or all of the nitrite, nitrate and nitro-derivative which may be used as such, e.g. as a fuel additive, as a source of the individual compounds or as a feedstock for a further synthesis.

    Abstract translation: 生成有机化合物和有机氮化合物的硝化。 通过有机化合物与过氧化氢和二氧化氮之间的反应衍生的羟基自由基反应形成有机氮化合物，并适当地用二氧化氮硝化有机氮化合物。 该方法可以作为使用过量二氧化氮超过羟基自由基形成所需的二氧化氮的单阶段方法进行。 通过使用催化固体表面如固体酸或酸性氧化物或混合氧化物，使羟基自由基的产生最大化。 产物可以是一些或全部亚硝酸根，硝酸根和硝基衍生物的混合物，可以如此使用。 作为燃料添加剂，作为单独化合物的来源或作为进一步合成的原料。

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