• 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:
    There is proposed a process and apparatus for producing benzenecarboxylic acids or benzenedicarboxylic acid esters or mixtures of these, in which process, in particular, p-toluic acid is prepared from p-xylene and, simultaneously, monomethyl terephthalate is prepared from p-toluate, the oxidation being carried out by adding, through vortex nozzles, oxygen-containing gases and oxidant liquid, with the formation of a highly-disperse reaction phase, and the vortex nozzles open out into the oxidant fluid. …<IMAGE>…
    公开号:SU1519526A3
    申请号:SU884355159
    申请日:1988-02-12
    公开日:1989-10-30
    发明作者:Лойк Ганс；Вестерманн Ганс-Ерг
    申请人:Динамит Нобель Аг (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to reactors for the catalytic oxidation of aromatic compounds, in particular to a dp reactor for the catalytic liquid phase oxidation of xylenes and / or toloic acid esters.
    The purpose of the invention is to increase the selectivity of the process and the yield of the target product.
    FIG. 1 schematically shows the proposed reactor; in fig. 2 and 3 are a nozzle suitable for use in the proposed reactor with feeding of two components with internal mixing, cuts.
    The proposed device contains a reactor 1, the upper part of the casing of which is equipped with a pipeline 2 for supplying xylenes and / or esters

    CM
    p-tanoic acid, a catalyst feed pipe 3 and a gas phase A pipeline A, connected to condenser 5, equipped with pipe 6 for exhaust gas with an expansion valve 7 and 8 for condensate drainage. A conduit 8 is connected to a phase separator 9 provided with a conduit 10 for recycling the aromatic phase to the reactor and a conduit 11 for diverting the aqueous phase. At least one nozzle 12 is installed in the reactor vessel 1, which has a channel 13 for feeding the liquid phase 15 containing the catalyst removed from the reactor through a pipe 14 with a pump 15 installed in it and an oxidant supply channel 16 connected to pipe 17, as well as mixing zone 18. The nozzle 12 may have, for example, a nozzle 19 mounted on the mouth 20 as a diffuser. The mouth 20 of the nozzles 12 is installed in the housing 1 at a height from the bottom corresponding to U, U2-0.5 times the height.
    The lower part of the reactor vessel 1 is also provided with a pipeline 21 for discharging the oxidation product. The reactor also has a cooling device 22 made as a heat exchanger, mounted in the bypass 23 connected to the pressure side and the suction side of the pump 15.
    The reactor may have a pipeline for supplying inert liquid evaporating at the reaction temperature, which is connected to channel 13 or 16, or directly to mixing zone 18.
    Example 1. In a reactor with a diameter of 300 mm, air is oxidized with 13.5 kgf xylene (99.3 wt.% Chidtota) and 31.5 kg of a mixture containing 87 wt.% Toloyl acid methyl ester obtained by etherification with tolanoic acid methanol , in the presence of 150 ppm w / w of cobalt and 13 wt. ppm, manganese, taken in the form of acetates. Upon reaching a temperature of 130 ° C, an average of 8.0 m / h of air is supplied to the nozzle for 4.1 hours at a pressure in the reactor of 0.8 MPa and a pressure in the nozzle of 1.2 MPa.
    During the reaction, the temperature is raised to 165 ° C. Upon reaching the acid number 197, oxidation is stopped.
    5 0 5
    0
    five
    The temperature of the circulating liquid phase containing the catapisor is reduced when the heat exchanger is cooled by 4–10 ° C compared to the temperature in the reactor. The total air amount supplied is 32.7 meters. The flue gases are constantly measured, which have the following average composition 4--% by volume: carbon dioxide 1.45; 1.6; oxygen; the rest is 1.15. This selectivity is calculated at 94.1%, i.e. 1.85% more than when the oxidation is carried out in a known reactor with the same acid number, which is confirmed by the amount of the desired product. The yield per unit volume and time, defined as the ratio of the amount of air used, is, in terms of reaction volume, 180 m of air / m h. In a known reactor, this value averages 45 meters of air / h-m.
    Example 2. Example 1 is repeated, but the oxidation is carried out until acid number 189 is reached. The air consumption is 33.9 meters. The exhaust gas contains on average 1.38% by volume of carbon dioxide, 3.0% by volume of oxygen and 1.12% by volume of the remaining components. The selectivity is 93.5%, i.e. 1.5% more than when oxidation is carried out in a known reactor with the same acid number.
    权利要求:
    Claims (2)
    [1]
    1. An apparatus for the catalytic liquid-phase oxidation of xylene and / or toloic acid esters, comprising a housing, the upper part of which is provided with pipelines for supplying xylene and / or esters of toloic acid, catalyst and recycled liquid and pipelines for withdrawing the gas phase, and the lower part - an oxidizer supply line, plug-in to the distributor installed in the housing, and a pipeline for discharging the oxidation product, as well as a cooling device, and a bottom that differs in that, in order to increase the selectivity of the process and the yield of the target product, the lower part of the body is equipped with a pipeline for draining the liquid phase containing the catalyst with a pump installed on it, the output is 51 3 I
    Secondly, it is connected to a distributor, made at least one at a time (5 sotds, kyuchayuschaya feed channels and a mixing chamber, the mouth of which is located 0.02-0.5 times the height of the body, and the pipeline / uta of the outlet containing the catalyst of the liquid phase is cooled by a cooling device, while the pipeline for supplying the oxidant and the outlet of the pipeline for withdrawing the catalyst-containing liquid phase are connected to the nozzle channels.
    0
    26
    [2]
    2. The device under item 1, that is, it is said that, oh, the way forward, Pneiie has a BG1G1 line of power, the switch of which is connected to the naTi (ipHiu i line, and the output to the suction line of the pump.
    3, Arrangements: to nn but nn. 1 and 2, so that it is equipped with a pipe of the day of supply of inert liquid I (L1Dr 1O1ceis liquid., Connection to the mixing chamber is reduced.
    / Y
    12
    17
    21
    Fig
    16 1
    eleven
    FIG I
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    同族专利:
    公开号 | 公开日
    CN88100904A|1988-08-24|
    EP0279288A3|1990-02-28|
    DE3704720A1|1988-08-25|
    EP0279288A2|1988-08-24|
    JPS63203647A|1988-08-23|
    PL270605A1|1988-12-08|
    BR8800636A|1988-09-27|
    YU26288A|1989-12-31|
    US4908471A|1990-03-13|
    PL153191B1|1991-03-29|
    DE3704720C2|1989-10-12|
    引用文献:
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    US4096340A|1975-06-03|1978-06-20|Teijin Hercules Chemical Co., Ltd.|Process for the preparation of dimethyl terephthalate|
    JPS5640143B2|1976-12-30|1981-09-18|
    DE2856529C2|1977-12-28|1982-09-09|Mitsui Petrochemical Industries Ltd., Tokyo|Process for the production of terephthalic acid|
    US4308241A|1980-07-11|1981-12-29|Quad Environmental Technologies Corp.|Formation of reactive droplet dispersion|
    US4342876A|1980-12-22|1982-08-03|Bechtel International Corporation|Method for oxidation of p-xylene and method for preparing dimethylterephthalate|DE4106843A1|1991-03-04|1992-09-10|Henkel Kgaa|METHOD FOR PRODUCING BENZOYLOXYBENZENE SULFONATES|
    DE19641912A1|1996-10-11|1998-04-16|Huels Chemische Werke Ag|Improved oxidation in the Witten-Hercules process for the production of dimethyl terephthalate|
    US6165435A|1998-12-24|2000-12-26|Praxair Technology, Inc.|Method and production of nitric acid|
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    US6657068B2|2002-03-22|2003-12-02|General Electric Company|Liquid phase oxidation of halogenated ortho-xylenes|
    US7541489B2|2004-06-30|2009-06-02|Sabic Innovative Plastics Ip B.V.|Method of making halophthalic acids and halophthalic anhydrides|
    US20060004223A1|2004-06-30|2006-01-05|General Electric Company|Method of making halophthalic acids and halophthalic anhydrides|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19873704720|DE3704720C2|1987-02-14|1987-02-14|
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