• 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:
    @ A method for conducting a chemical process in which a feed containing at least one liquid is introduced into a vessel containing a plurality of packed, vertically arranged tubes, and in which at least one liquid product and at least one gaseous product are obtained, in which the tubes and a space above them are kept flooded with liquid by controlled removal of liquid product from the lower portion ofthe vessel.
    公开号:SU1376938A3
    申请号:SU843812579
    申请日:1984-11-06
    公开日:1988-02-23
    发明作者:Галилео Алесандрини Карло (Младший)；Акос Нейди Луи
    申请人:Стауффер Кемикал Компани (Фирма)；
    IPC主号:
    专利说明:


    Si
    The invention relates to an improved process for the preparation of ethyl chlorothioformate, which finds use in the synthesis of hell) bicides.
    The purpose of the invention is to increase the conversion that is achieved by feeding the feedstock into the reactor at a point located above the upper ends of the tubes, removing the gaseous product from the upper part of the reactor above the upper end of the tubes, and waving the desired product from the lower part of the reactor by adjusting the liquid level. in the reactor so that it is supported above the upper ends of the tubes throughout the inside of the reactor.
    The drawing shows a diagram for implementing the method.
    The process is carried out in a vertical vessel 1 or a reactor. In the upper part of the vessel 1 there is a zone 2 for the separation of liquid and vapor. Inside the vessel there are many vertically mounted tubes 3, fixed in place of the upper and lower support plates 4 and 5, respectively. The tubes are tightly packed from the bottom over the ground with a crushed solid containing a catalyst — activated carbon.
    Liquid loading, which can be used as a single liquid, a mixture of different liquids or a mixture of one or more liquids with one or more gases, is introduced into the upper part of vessel 1 through line 6 above the upper support plate 4. Liquid together with other possible components of loading is injected from the top down and flows through the filled tubes 3. The liquid product, which may be a liquid supplying the feed liquid, obtained by a chemical reaction inside the tubes; 3, or a mixture of two or more such fluids is led out from the bottom of the vessel below the level of the lower support plate 5 through line 7 with vertical bend 8.
    The liquid product from line 7 is sent to section 9 downstream for further processing, which is to perform a further reaction, or to separate the liquid products. It turns out
    the final desired liquid product and output through line 10.
    The gaseous product, which may be the gas introduced into the reactor together with the liquid feed along the line
    6 (for example, a vaporized liquid dissolved in a liquid coming through line 6, a gaseous product obtained by chemical reaction in filled tubes 3, or a mixture of two or more of these gases come out of the upper part of reactor 1 through line 11 and can be directed in a similar way, if necessary, for further processing, it is necessary that the gas is vented from a point above the liquid inlet (s).
    The process in accordance with the invention is carried out continuously with a constant supply of liquid loading through line 6, a constant withdrawal of liquid product to line 7 and a permanent withdrawal of gaseous product to line 11. However, this process can also be carried out periodically.
    This process is carried out in the liquid phase by maintaining uniform filling of the filled pipes 3 with liquid and for this purpose the reactor is filled with pumped liquid, while the gaseous product (or products) or initially introduced received in the filled tubes goes up through the liquid and its excess is removed from the vessel. The liquid level in the vessel is maintained above the upper ends of the tubes in a large part of the vessel so that the tubes are filled with liquid.
    Filling the tubes with liquid is accomplished by controlling the flow of liquid from the reactor to the line.
    7 in order to provide sufficient back pressure on the fluid, forcing it to rise back up and pour over the upper ends of the tubes 5 into the space above the plate 4. This same back pressure forces the gaseous product to rise up the tubes instead of flowing down along with the liquid in the same way known method. The inlet through which the liquid is introduced through line 6 may be located all and (or) below the surface of the liquid in the upper part of the vessel 1. Dn
    For better distribution, it is desirable that the liquid from line 6 is introduced into the vessel through a plurality of inlets located in the upper part of the vessel above the upper support plate. The discharge of fluid to line 7 can be controlled by a variety of means, including bypass valves, by means of an adjustable upper elbow 8 in line 7 of the fluid drain. It is necessary that the control of the discharge of fluid into line 7 is carried out by reacting to signals from one or more sensors placed in the upper part of the vessel 1 above the upper support plate and indicating the height of the liquid level in this upper part.
    The discharge of fluid to line 7 can be controlled automatically by the com- puter process control (not shown) in response to such signals. Regulation of the fluid flow in this case is carried out by means of
    ten
    20 6938
    instead of going down or going out with the liquid through the outlet in line 7. This control and upward direction of the gas flow leads to both more equal mixing of the liquid and gas, and to their easier separation in vessel 1, facilitating the separate removal of liquid and gaseous products from the vessel. In addition, it provides good heat transfer throughout the tubular zone.
    The process of obtaining liquid chlorothio-15 formate using the reaction of liquid mercaptan with phosgene (which can be in the gaseous and / or liquid state) can be carried out in the following manner.
    A load including ethyl mercaptan, phosgene (preferably in the liquid state), and with a possible repeated delivery cycle of the liquid, is introduced along line 6 into the upper part of qi.
    flow regulators, bypass pumps of the 25th reactor reactor 1, containing
    thieves, valves, and so on, installed in line 7. Another way to control fluid flow is to control the upper knee at a sufficiently high level so that the value, which is the result of the product of the density of the liquid and its height in the knee 8, is equal to the density of the fluid to its height in the tubes 3. Once this balance is adjusted for a particular reaction in a steady state, monitoring the level of the fluid can be performed without the use of electrical or mechanical instruments.
    Initially, the process can be started by introducing fluid into the vessel through line 6, maintaining controlled fluid withdrawal (not participating in the process) into line 7 until the liquid level in the vessel rises above the upper support plate. At this point, you can start the reaction or another process, for example, increasing the temperature of the inside of the reactor and entering additional reagent into the load.
    The withdrawal of liquid from the reactor in a controlled manner, as described, results in not only filling the tubes with liquid, maintaining uniform flow, but also forcing the gaseous product to flow up the tubes and then along line 11
    five
    a plurality of vertically mounted tubes 3 fixed between the upper 4 and lower 5 support plates. Tubes 3 are filled with catalyst 0 with activated carbon of the appropriate size in such a way that each tube functions as a miniature filled bed reactor.
    Liquid feed through line 6 is introduced into the upper part 2 of the reactor 1 above the upper support plate through a plurality of peripheral orifices located around the reactor. Liquid is pumped from top to bottom through
    0 tube, while its level is maintained in the upper part of the reactor 1 above the upper ends of the tubes 3 and above the upper support plate 4. The mercaptan and phosgene react in filled
    5 tubes, resulting in the formation of liquid ethyl chlorothioformate and hydrochloric acid gas. In addition, part of the phosgene can evaporate BV tubes. Gaseous formed
    The Q product (or products) passes upward through the tubes 3 through the liquid / gas separation zone 2 and is withdrawn from the reactor via the upper line 11. These gaseous products then pass downward.
    g downstream FOR further processing, such as the reduction of hydrogen chloride produced during the reaction, the reduction of phosgene and for controlling the evolution of gas.5
    The liquid product consisting in the osnon of ethyl chlorothioformate along with some part of the non-overlapping starting products and small quantities of the by-product, such as diethyl disulfide, is withdrawn from the bottom of the reactor 1 to line 7, the rate of output of the liquid product to line 7 is controlled, for example, by monitoring the level of the liquid or the direction of the liquid flow in line 7 through the knee


    8, which is raised sufficiently. Reactor 1 is supplied
    juice to create a back pressure of 10.17 kg-mol / h of phosgene and
    9.26 kg-mol / h ethyl mercaptor operates at a temperature of about 15–40 ° C, the flow rate is about 50–60 ° C, and the outlet pressure is about 2.53 kg / cm.
    in the reactor to maintain the level of the liquid In the upper part of the reactor above the upper ends of almost all tubes. The liquid product is then directed downstream to downstream device 9. If the reaction in reactor 1 is not sufficiently completed and significant amounts of unreacted raw materials are contained in the liquid product in line, then device 9 can be the second reactor for further reaction of ethyl mercaptan with phosgene. The reaction products are output in line 10 and run downstream to separate the further processing. If the reaction is sufficiently completed, device 9 may be a separator: the product, ethyl chlorothiorum, is removed from other substances in a line. This and other substances consisting mainly of unreacted phosgene and / or ethyl mercaptan can be recycled to line 12 for inclusion in a liquid feed in line 6.
    Example 1 (known). A reactor system with a capacity of about 16,783 kg per day of ethyl chlorothioformate is used. A tubular reactor with upward flow, with tubes filled with a catalyst — activated carbon, is used as the reactor.
    1.17 kg-mol / h of osgen and 9.26 kg-mol / h of ethyl mercapgan are fed to the reactor. The reactor operates with an inlet temperature of about 15-40 ° C, with an outlet temperature of about 50-65 ° C and an outlet overpressure of about 2.11-2.53 kg / cm. The conversion of ethyl mercaptan to chlorothioformate is about 60%. Product Reac
    After removal of unreacted products, diy contains 98% of the basic substance, 0.5-1% diethyl sulfide and about 1% diethyldithiocarbonate.
    Example 2. The proposed reactor is similar to the reactor of Example 1. However, the capacity of this reactor is about 25,878 kg per day of ethyl chlorothioformate. This reactor operates in a downward flow mode with tubes filled with a catalyst — activated carbon.
    Reactor 1 is supplied
    10.17 kg-mol / h of phosgene and
    9.26 kg-mol / h of ethyl mercaptan. The reactor operates at an inlet temperature of about 15–40 ° C, the inlet temperature is about 50–60 ° C, and an overpressure at the outlet is about 2.11– 2.53 kg / cm.
    The conversion of ethyl mercaptan to chlorothioformate is about 90%. After removal of unreacted raw materials, the net content of the main product is 98%, about 0.5% is diethyl sulfide, and less than 1% is diethyldithiocarbonate.
    Example 3. A dual reactor system with a proikh yield of 77,634 kg per day of ethyl chlorothioformate is used. The first reactor is a tubular, filled with a liquid with a falling flow, the tubes are filled with a catalyst — activated carbon. The second reactor, the reactor of the confluent type, with a filler containing a coal catalyst bed, operates in the upstream mode. In the first reactor 1, 30.5 kg-mol / h of phosgene and 27.78 kg-mol / h of ethyl mercaptan are supplied.
    The reactor operates at an inlet temperature of about 15-40 ° C, the temperature at about 50-65 ° C and an overpressure of 2.11-2.53 kg / cm. The reaction products from the first reactor are fed to the bottom of the second reactor 9 together with a recycled stream containing 14.57 kg-mol / h of phosgene and 6.40 kg-mol / h of ethyl chlorothioformate. The second reactor operates at an inlet temperature of about 18–26 ° C, an exit temperature of about 33–49 ° C, and an overpressure on the inlet of about 1.69–1.97 kg / cm.
    The conversion of ethyl mercaptan to chlorothioformate is 94%.
    The output of the main product is 98%, about 9.5% is diethyl sulfide and less than 1% is dithiocarbonate.
    Thus, the proposed method allows to increase the conversion of ethyl mercaptan from 60 to 90%.
    权利要求:
    Claims (1)
    [1]
    Claims of Invention A method for producing ethyl chlorothioformate by the interaction of liquid ethyl-β-mercaptan and phosgene in a reactor containing vertically positioned tubes filled with activated carbon at a temperature of 15-40 ° C at the reactor inlet and 50-60 ° C at the reactor outlet and an overpressure of 2, 11- 2.53 kg / cm at the outlet of the reactor with poI.
    five
    the subsequent separation of the gaseous reaction containing hydrogen chloride and the injected phosgene, and the separation of the liquid target product, characterized in that, in order to increase the conversion, the starting products are fed to the reactor at a point located above the upper ends of the tubes from the upper part of the reactor above the upper ends of the tubes, and the target product is distributed from the lower part of the reactor by adjusting the level of | liquid in the reactor so that it is supported iral- with the upper ends of the tubes all over the inside of the reactor.
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    引用文献:
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    US1631162A|1924-04-25|1927-06-07|Griscomrussell Company|Vertical film-type evaporator|
    US2165490A|1936-12-10|1939-07-11|Nat Aniline & Chem Co Inc|Gas absorption|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US06/549,150|US4551325A|1983-11-07|1983-11-07|Method for conducting a chemical process in a packed multi-tubular reactor|
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