• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to the chemistry of aliphatic nitro compounds, in particular, to the preparation of a mixture of nitroparaffins with a predominant content of nitromethane, which is a raw material for organic synthesis. The goal is to increase the yield of nitromethane. The preparation is carried out by nitration of ethane with nitrogen dioxide in the presence of air or oxygen in a mixture with a gas inert with respect to the reaction components and the addition of nitroparaffin — ntroethane at a molar ratio of (3.8-7.92): (0.15-0.36 ): (0.15-0.31). Probes are carried out at a pressure of 10 bar. 326-353 °, contact time 6.0-6.1 s and molar ratio inert gas: ethane for the case of using an inert gas 1: (0.17-0.31). Carbon dioxide or nitrogen is used as an inert gas. 1 hp f-ly, 1 tab. about Ј (L
    公开号:SU1704629A3
    申请号:SU792843403
    申请日:1979-11-11
    公开日:1992-01-07
    发明作者:Лонор Пьер；Жакино Бернар；Кибель Жак；Мари Роже
    申请人:Сосьете Шимик Де Ля Гранд Паруас, Азот Э Продюи Шимик (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to the chemistry of aliphatic nitro compounds, in particular, to an improved method for producing a mixture of nitroparaffins with a predominant content of nitromethane, which is a raw material for the synthesis of useful products, and can be used in the chemical industry.
    The aim of the invention is to increase the yield of nitromethane.
    Ethane is nitrated with nitrogen dioxide at 326-353 C and a pressure of 10 bar in the presence of air or oxygen in a mixture with an inert gas to the reaction components and the addition of nitroethane or recycled nitro
    ethane at a molar ratio of ethane:: nitrogen dioxide: oxygen: nitroethane, equal to (3.8-7.92): 1: (0.15-0.36) :( 0.15-0.31), and the inert gas: ethane molar ratio for an inert gas use of 1: (O, 17-0.31), with a contact time of 6.0-6.1 s.
    In accordance with the proposed method, the nitration of ethane is carried out 6 in the presence of the active agent of the carrier of the easily tolerated group W or NO2 of nitroethane. The ratio of nitroethane: nitrating agent can be changed depending on the desired change in the gamma of nitroparaffins. It is advisable that the active agent
    Kj o
    N
    f
    fO
    Yu
    s
    nmvinvMM alone or in smeghe, the product of the recycling of the reaction nitron-mon.
    The quantitative ratios of the pa:) lich components of the reaction mixture, the duration of the reaction contact, the temperature and the pressure of the reaction are weighted and adjusted, depending on the paraffins required, so that the nitration takes place in a homogeneous phase.
    It is also advantageous to heat the reagents to a controlled temperature that is as much as possible equal to the nitration temperature. Such preheating should be carried out separately for the oxidizing agent and the nitrating agent and for ethane. The recirculating gases as well as the active agent can be heated either together with ethane or together with an oxidizing agent and a nitrating agent.
    i The final reaction mixture with a temperature that does not vygae than the temperature of the nitration, must be prepared especially carefully. An oxidizing agent and a nitrating agent are introduced into the ethane stream containing (optionally) inert gas. This mixture should be prepared as close as possible to the reaction zone, within which the temperature should be strictly controlled in ways that ensure good heat transfer.
    Example. Ethane is nitrated at a temperature varying between 326-353 ° C and pressure. 10 bar in the presence of air. The nitrating agent is nitrogen dioxide, the contact time is 6.0-6.1 seconds, the molar ratio of ethane nitrogen dioxide varies between 3.8-7.92. The nitration is carried out in the presence of an active agent (AA) -nitroethane recycle in the presence of an inert gas of nitrogen or carbon dioxide.
    The specific flow rate of the recirculating agent (AARC) or of the active agent introduced is equal to chitng / between the entered mass and the mass of the same kione;
    tl, selected ti.i exit from the reactor. It is expressed in kg of a circulating substance per kg of NPf nitroparaffins produced. In all the experiments where the nitration is reacted with recycling or the introduction of the active agent, only the difference between the mass of this selected compound and the mass of the same active compound fed at the entrance to the reactor is taken into account in the resulting liquids.
    The results of the experiments are presented in the table.
    Thus, in the proposed method of obtaining a mixture of nitroparaffins, the content of nitromethane is higher than in the known.
    权利要求:
    Claims (2)
    [1]
    1. A method of producing a mixture of nitro-paraffins with a predominant content of nitromethane by nitrating paraffin with nitrogen dioxide at elevated temperature and pressure in the presence of air or oxygen in a mixture with a gas inert with respect to the reaction components and adding nitroparaffin, in that to increase the yield of nitromethane, ethane is used as the initial paraffin, as nitroparaffin-nitroethane, carbon dioxide or nitrogen is used as an inert gas, and the process is carried out at a pressure of 10 bar, temperature 326-353 0, contact time, 1 s at a molar ratio of ethane: nitrogen dioxide:: oxygen: nitroethane, equal to (7.92): 1: (0.15-0.36) :( 0.15-0.31), and inert gas molar ratio :. : ethane for use with an inert gas of 1: (O, 17-0.31).
    [2]
    2. A method of pop 1, characterized in that recycled nitroethane is used as nitro-paraffin
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    同族专利:
    公开号 | 公开日
    JPS6337778B2|1988-07-27|
    BR7907346A|1980-07-15|
    ES485432A1|1980-05-16|
    FR2442828A1|1980-06-27|
    AT553T|1982-01-15|
    RO77527A|1982-02-26|
    US4313010A|1982-01-26|
    EP0011553A1|1980-05-28|
    DD146946A5|1981-03-11|
    DE2961833D1|1982-02-25|
    EP0011553B1|1982-01-13|
    TR20583A|1982-02-08|
    PL123569B1|1982-10-30|
    JPS5566543A|1980-05-20|
    FR2442828B1|1981-07-24|
    PL219489A1|1980-07-14|
    CA1121386A|1982-04-06|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE1069133B|1959-11-19|E. I. Du Pont De Nemours And Company, Wilmington, Del. |Process for the preparation of nitro compounds of alkalis, cycloalkanes and aryl-substituted alkanes|
    US2071122A|1937-02-16|Process of nitrating ethane |
    US2609401A|1952-09-02|Nitration of saturated aliphatic |
    US2332491A|1940-05-01|1943-10-19|Commercial Solvents Corp|Catalytic process for nitration of hydrocarbons|
    US2512587A|1949-06-08|1950-06-20|Commercial Solvents Corp|Method of temperature control in nitration of hydrocarbons|
    US2883433A|1957-04-16|1959-04-21|Du Pont|Process for the preparation of nitro derivatives|
    US2883434A|1957-04-16|1959-04-21|Du Pont|Liquid phase process for the preparation of nitro derivatives|
    US2883432A|1957-04-16|1959-04-21|Du Pont|Process for the production of saturated aliphatic nitro compounds|
    FR1439414A|1964-06-22|1966-05-20|Commercial Solvents Corp|Process for the production of nitrated hydrocarbons|
    US3378596A|1964-06-22|1968-04-16|Commercial Solvents Corp|Process for producing nitrohydrocarbons|
    US3272874A|1964-11-18|1966-09-13|Commercial Solvents Corp|Production of nitroalkanes|
    FR2158681A5|1971-10-28|1973-06-15|Azote & Prod Chim|Nitro paraffins prepn - by reaction of propane with nitrogen peroxide|
    BE790694A|1971-10-29|1973-04-27|Azote & Prod Chim|NITROPARAFFINS MANUFACTURING PROCESS|
    FR2199753A6|1972-09-21|1974-04-12|Azote & Prod Chim|Nitroparaffins by nitration of hydrocarbon gas - with nitrogen peroxide and preheated air at selected temp and pressure|
    FR2421867B1|1978-04-04|1980-09-05|Azote & Prod Chim|FR2452315B1|1979-03-28|1985-07-05|Azote & Prod Chim|NITRATION REACTOR FOR HYDROCARBONS IN GAS PHASE UNDER PRESSURE|
    FR2453846A1|1979-04-10|1980-11-07|Azote & Prod Chim|PROCESS AND PLANT FOR MANUFACTURING NITROPARAFFINS BY NITRATION OF HYDROCARBONS IN THE GASEOUS PHASE|
    US4458094A|1982-01-22|1984-07-03|W. R. Grace & Co.|Process for forming nitroparaffin|
    US4517392A|1983-07-05|1985-05-14|W. R. Grace & Co.|Preparation of nitro compounds by vapor phase nitration of organic alcohols|
    US4476336A|1983-07-05|1984-10-09|W. R. Grace & Co.|Process for forming nitroparaffin|
    US4517393A|1983-07-05|1985-05-14|W. R. Grace & Co.|Preparation of nitro compounds by vapor phase nitration of ketones|
    US4524226A|1983-07-05|1985-06-18|W. R. Grace & Co.|Preparation of nitro compounds by vapor phase nitration of aldehydes|
    US4517394A|1983-07-05|1985-05-14|W. R. Grace & Co.|Preparation of nitro compounds by vapor phase nitration of carboxylic acids|
    FR2558827B1|1984-01-27|1986-06-27|Azote & Prod Chim|PROCESS FOR THE MANUFACTURE OF NITROMETHANE AND INSTALLATION|
    US4766257A|1984-09-12|1988-08-23|W. R. Grace & Co.|Preparation of nitro compounds by vapor phase nitration of olefins|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7832118A|FR2442828B1|1978-11-14|1978-11-14|
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