• 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 previously carried out internal coating of contact tubes not only required very much manual labor and was very time consuming, but it was also unsatisfactory in regard to adhesion of the contact liquid to the surface and homogenity of the catalyst. By the simultaneous action of heat on the liquid interface in the tubes during the lowering of the liquid level as well as by a specially suited apparatus for this purpose which operates according to the principle of communicating tubes there is provided the possibility of a good adhesion to the surface as well as the formation of a homogeneous layer at very little operating expense.
    公开号:SU1066456A3
    申请号:SU813377500
    申请日:1981-09-16
    公开日:1984-01-07
    发明作者:Фойгт Карл；Клейншмит Петер；Маннер Рейнгард
    申请人:Дегусса Аг.(Фирма)；
    IPC主号:
    专利说明:

    2. A device for applying a catalytic coating on the inner surface of the pipe, including a geoBvaD for the coating material containing the catalyst, means for feeding the coating material to the treatment; a tubular tube forming vessels from the reservoir Warwam, a means for evaporating the solvent of the coating material, and a device for installing the pipe 8 to be treated are in a vertical position, which is so that, in order to increase the degree of homogeneity of the coating and to expand the technological capabilities of the device, evaporation of the solvent of the coating material is made in the form of a furnace covering the pipe being processed, and the device for installing the pipe in a vertical position is made in the form of tubular ravl to Tsikh in which an oven for vertical movement relative to the work pipe
    3, the apparatus according to claim 2, characterized in that the eye is provided with a suction device made in the form of a discharge tube installed with the possibility of lowering into the pipe being processed and placed above the furnace on the tubular guides with the possibility of vertical movement of the supporting frame at the upper end which is fixed discharge tube.
    The invention relates to catalytic coatings on the inner surface of a reactor, in particular, to a method and apparatus for applying a catalytic coating to the inner surface of a pipe used for carrying out chemical processes, in particular for producing hydrogen cyanide. A known method of applying a catalytic coating on the inner surface of a pipe concluded that the pipe equipped with a rubber stopper at one end was filled with a solution containing a catalyst, followed by closing the other end of the pipe with a rubber stopper in the middle of which the tube is missed, then the tube is rotated until the entire inner surface is wetted; the excess solution is discharged, the tube is installed in a horizontal position and slowly rotated with simultaneous heat supply to evaporate the solvent and field tea calcined coating T11. The disadvantage of this method is its multi-stage. The closest to the proposed technical essence and the achieved result is a method of coating the inner surface of a pipe, including, setting the pipe in a vertical position, filling the pipe with a liquid containing a catalyst applied to the internal surface of the pipe, lowering the liquid level in the pipe, the substance obtained product by supplying heat C21,. The method is carried out by a device for applying a catalytic coating on the inner surface of a pipe, including a reservoir for the coating material containing a catalyst, means for feeding the coating material into the pipe being worked, forming communicating vessels with the tank, means for evaporating the solvent of the cut material and installing the treated pipe in a vertical position. However, this method is characterized by an insufficient degree of homogeneity of the resulting coating and the impossibility of obtaining a coating of a different profile. The purpose of the invention is to increase the degree of homogeneity of the resulting coating and the possibility of obtaining a coating of various profiles. The goal is achieved in that according to the method of applying a catalytic coating on the inner surface of a pipe by installing the pipe in a vertical position, filling the pipe with a liquid containing a catalyst, and further reducing the level of liquid in the pipe and supplying heat, heat is applied to the interface with the liquid simultaneously with lowering the level of liquid in the pipe, the method can be used by a device including a reservoir for a coating material containing a catalyst, means for supplying the coating material to the pipe being processed, forming communicating vessels from the reservoir, means for evaporating the solvent of the coating material and a device for placing the pipe being processed in a vertical position, in which the means for evaporating the solvent of the coating material are made in the form of a furnace encompassing the pipe being processed, and device for installation, pipes in a vertical position are made in the form of tubular guides, on which a furnace is installed with the possibility of vertical movement flax treated pipe. In addition, the device is equipped with a suction device, made in the form of a discharge tube, installed with a possibility of lowering into the pipe being processed, and placed above the furnace on tubular guides with the possibility of vertical movement of the supporting frame, on the upper end of which a discharge tube is fixed. The drawing schematically shows a device for implementing the method, a general view. The device comprises am 1, consisting of two vertical tubular guides 2, arranged parallel to one another and interconnected by means of two transverse struts 3. Frame 1 is a device for placing the treated pipe 4 in a vertical position. The device also contains means for evaporating the solvent of the coating material in the form of a furnace 5 installed on the guides 2 with the possibility of vertical movement relative to the pipe 4 being processed with the help of sliding pipes, at least one tank 6 with the coating material containing a catalyst directly or by means of at least one pipe 7 with furnace 5 and forming, together with the processed pipe 4, communicating vessels, a suction device made in the form of a discharge tube 8 installed from the possibility of lowering into the pipe being processed and placed above the furnace 5 on tubular guides 2 with the possibility of vertical movement of the supporting frame 9 On the upper end of the supporting frame 9, the outlet tube 10 with the separator 11 is fixed. The need for an suction extraction device can disappear when, for example, as a solvent for a catalyst, is. use is made of volatile components, such as, for example, low-boiling organic solvents, such as short-chain aliphatic alcohols. ethers, halogenated hydrocarbons, etc. When using these solvents, gases can be removed directly through the discharge tube 10, for example, by setting a vacuum. In cases where solvent recovery is not needed and only gases that are not harmful to the environment are formed, the device should not contain a separator. The tank 6 through pipe 12 with locking bodies 13 and 14 installed therein is connected to the pipe 4 being machined, provided with a holder 15. The separator 11 is connected via pipe 16 to a three-way valve 17 equipped with a pipe 18 and 19. The locking member 14 can be a pipe 20 through which oxygen and hydrogen can be supplied to convert the catalytic coating to the active form. To limit the upward movement of the carrier, the frame 9 on the upper end of the tubular guides 2 is fitted with an upper stopper 21. The supporting frame 9 is fixed to the tubular guides with a locking screw 22. in a way. First, the furnace 5 is moved to the upper end of the pipe being processed, 4, and it is heated to the desired temperature. After the reservoir 6 is filled with a coating material, for example, a solution, dispersion or suspension containing the substance to be applied to the inner surface of the pipe, and the closure bodies 13 and 14 are opened, the coating material flows through the conduit 12 to the inside of the pipe 4 to be leveled. After leveling the coating material, the furnace 5 at a speed depending on the type of pipe being processed, the viscosity of the coating material and its temperature is lowered until it reaches the IS holder, and the downward movement of the furnace 5 can be stopped until the holder 15 reaches the level With the lowering of the furnace 5, the level of the coating material in the treated pipe 4 decreases, and simultaneously a catalytic coating is applied to the inner surface of the processed pipe as a result of evaporation of the coating material.
    The furnace temperature is set depending on the type of coating material, the desired thickness of the applied layer and the speed of the furnaces so that a sufficient amount of the coating material evaporates, i.e. so that the catalyst contained in the dissolved form or in the form of a suspension or dispersion is firmly deposited on the inner surface of the pipe being processed. At the same time, the coating material should not boil in order to obtain a completely homogeneous coating.
    The thickness of the applied catalytic coating depends not only on the temperature of the furnace 5, but also on the lowering speed of the furnace 5, the height of the material level of the coating inside 4) of the processed pipe 4, enclosed by the furnace 5, which can be adjusted with POMS4CI tank 6, And the type and concentration of material used cover
    In this case, the higher the temperature in the pipe 4 being processed and the lower the lowering rate of the furnace 5, the thicker the applied catalytic coating for a given form and density of the coating material.
    By diluting the coating material with solvents or suspending agents, it is possible to obtain a thinner catalytic coating — at a given temperature in the treated pipe 4 and at a given lowering speed of the furnace 5.
    The effect of these parameters on the thickness of the applied coating must be determined in the corresponding preliminary experiments.
    The coating material that evaporates during application is sucked through the discharge tube 8, which, although entering the treated tube 4, but not immersed in the coating material, enters the separator 11 through the discharge tube 10.
    The phase remaining above the condensate in the separator 11 is discharged through a three-way valve 17 or through the pipeline 18 by means of a vacuum and is reused after normal recovery, or directly through the pipeline 19.
    Condensate from separator 11 can be returned to the solvent collection tank and reused (not shown).
    After stopping the furnace down
    5 and returning the coating material to the closure bodies
    When it is withdrawn through the locking member 13, the locking member 14 is closed.
    Possible activation of the catalytic coating can also be carried out in the device. At the same time, the corresponding gas, such as H or Oj, is supplied to the pipe 4 to be processed through the pipework 20 and the valve 14, and the activation temperature is set by means of a raised and lowered furnace 5. In most cases, the discharge pipe 8 does not have to move. The carrier frame 9 is moved to the upper limiter 21 and secured with a locking screw 22.
    If during the coating process, combustible, explosive or corrosive gases are formed, then the discharge pipe 8, after the end of the process, is tightly closed against the treated pipe 4 with the gland 23 and the gases are diverted through the discharge pipe 10.
    Example 1. A tube made of alumina 210 cm long and 15 mm in diameter is installed in the device and filled from below with a liquid tank containing the catalyst with a platinum solution so that the liquid level is 10 cm above the lower edge of the furnace same level with the upper end of the tube. The furnace tube is adjusted to 250 s and lowered at a speed of 8 cm / m. At the same time, 0.5 g of platinum in the form of a homogeneous coating is applied to the inner surface of the pipe based on a hydrochloric hexachloroplatinum solution with a concentration of 75 g EC / l.
    After 26 minutes, the coating process is completed and the coating is activated by reduction with hydrogen at 600 ° C in the same device.
    The tube is removed from the device and used to produce hydrogen cyanide. At the same time, propane: ammonia: hydrogen 1: 3 ,, 5; 6 .. Gas is heated to 1300 ppm at 1 bar. After passing through the reaction tube, the resulting reaction mixture is cooled to between 400 and.
    The output of hydrogen cyanide is equal to 87 mol,% in terms of propane. After absorption of unreacted ammonia in sulfuric acid and hydrogen cyanide in an aqueous solution of caustic soda, the residual gas of the composition, mol%, is obtained: hydrogen 96.4; nitrogen 1,2; methane 2.4 (according to gas chromatography), which can be used as a source of hydrogen.
    Example 2. Example 1 is repeated, with the difference that instead of a platinum solution, a solution of ammonium heptamolybdenum (NHij) g 4H2O (concentration: 0, 122 g Mo / cm) is used. At the same time, 1.8 g of molybdenum compound is applied to the inner surface of the pipe in the form of a homogeneous coating. At the end of the coating process, the tube is fired in an air stream at 500 seconds for 4 hours,
    The tube is taken out of the device and used to produce hydrogen cyanide under the conditions of Example 1. The yield of hydrogen cyanide is 85 mol.% Based on propane.
    Example 3. Repeat example
    1 with the difference that the furnace is not lowered with a uniform, but different speed, starting with the speed
    8 cm / min, which is increased by
    2 cm / min every 20 cm of the furnace. In this case, a continuous coating is applied to the inner surface, in which the platinum content rises uniformly from 1.2
    up to 5.2 mg per unit area.
    The tube is used to produce hydrogen cyanide under the conditions of Example 1. The yield of hydrogen cyanide is 88.5 mol.% Based on propane.
    Example 4. Example 1 is repeated with the difference that a coating containing different catalysts in two zones is applied to the inner surface of the pipe. In this case, first cover the upper third of the pipe with a catalytic solution 1, and the furnace is lowered from top to bottom to the marked boundary. Then, an excess of the catalytic solution 1 is discharged and a further design of the residual area is carried out with a catalytic solution n.
    In this example, the catalytic solution T consists of a mixture of solution
    iridium and platinum (1 mole of iridium and 4 mole of platinum, and a catalytic solution of It from pure platinum cations. Solutions are prepared on the basis of 6-hydrate hexachloroiridium acid D8.5% iridium) and hexachloroplatinate. Homogeneous coatings are obtained.
    I
     used to obtain
    hydrogen cyanide under conditions
    of Example 1. In this case, the yield of hydrogen cyanide is 87.5 mol.% in terms of propane.
    The application of the invention simplifies the coating process and shortens its duration while maintaining the quality of the coating obtained.
    权利要求:
    Claims (3)
    [1]
    The method of applying a catalytic coating on the inner surface of the pipe by installing the pipe in an upright position, filling the pipe with liquid containing the catalyst, and then lowering the liquid level in the pipe and supplying heat, so that , in order to increase the degree of homogeneity of the coating and. the possibility of obtaining coatings of various profiles, the supply of heat is carried out to the interface with the liquid simultaneously with lowering the liquid level in the pipe.
    SU „1066456>
    [2]
    2. A device for applying a catalytic coating to the inner surface of the pipe, including rezewo for the coating material containing the catalyst, means for supplying the coating material to the processed pipe, forming communicating vessels with the reservoir f means for evaporating the solvent of the coating material and a device for installing the processed pipe in a vertical position, characterized in that, in order to increase the degree of homogeneity of the coating and expand the technological capabilities of the device, means d I 'evaporation of the solvent of the coating material is in the form ne chi embracing treatment tube, and means for setting the tube in the vertical position made in the form of tubular guides on which the furnace is mounted with the possibility of vertical movement relative to the processed pipe.
    [3]
    3. The device pop. 2, characterized in that it is equipped with a suction device made in the form of a discharge tube installed with the possibility of lowering into the pipe being processed, and placed above the furnace on tubular guides with the possibility of vertical movement of the carrier frame, on the upper end of which a discharge tube is fixed.
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    同族专利:
    公开号 | 公开日
    ZA816404B|1982-09-29|
    DE3034957A1|1982-04-01|
    BE890365A|1982-03-15|
    CH651481A5|1985-09-30|
    US4471712A|1984-09-18|
    US4415485A|1983-11-15|
    JPS5781837A|1982-05-22|
    JPH0212621B2|1990-03-22|
    DE3034957C2|1983-01-13|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2488450C2|2010-04-27|2013-07-27|Борис Владимирович Скворцов|Application of coat onto pipe inner surface|
    RU2503506C2|2011-12-29|2014-01-10|Общество с ограниченной ответственностью "Аналитические приборы и системы"|System of automatic control over application of insulating coat on cylindrical article inner surface|DE562136C|1931-10-11|1932-10-21|Ver Stahlwerke Akt Ges|Method for lining hollow bodies, for example pipes|
    FR1007617A|1949-01-10|1952-05-08|Method and device for internal sealing of pipes|
    US2768876A|1950-07-26|1956-10-30|Degussa|Process for the production of hcn from volatile hydrocarbons and ammonia|
    US3112215A|1959-10-09|1963-11-26|Lonza Ag|Preparation of catalytically active coatings|
    US3074808A|1959-10-19|1963-01-22|Phillips Petroleum Co|Method and apparatus for coating the interior of a pipe|
    US3107146A|1960-01-28|1963-10-15|Toyo Koatsu Ind Inc|Method of producing hydrogen cyanide|
    US3842799A|1972-03-10|1974-10-22|E Podkletnov|Apparatus for the application of liquid corrosion-preventive compound to the inner surface of pipes|GB2211179B|1987-10-15|1992-08-12|Hoechst Ceram Tec Ag|Aluminium oxide shaped articles and process for their manufacture|
    DE3915685C1|1989-05-13|1990-12-06|Degussa Ag, 6000 Frankfurt, De|
    DE4040150C2|1990-02-28|1992-02-06|Degussa Ag, 6000 Frankfurt, De|
    DE4128202A1|1991-08-26|1993-03-04|Hoechst Ceram Tec Ag|Sintered alumina reaction tube - with internal spiral rib, esp. for high temp. hydrogen cyanide synthesis|
    DE4128201A1|1991-08-26|1993-03-04|Hoechst Ceram Tec Ag|Sintered alumina reaction tube - contg. spiral insert, esp. for high temp. hydrogen cyanide synthesis|
    IN195165B|1996-06-21|2005-01-28|Engelhard Corp|
    DE19909029A1|1999-03-02|2000-09-21|Degussa|Production of a catalytically active layer on a monolithic support comprises filling flow paths in the support with coating dispersion or impregnated solution, drying and calcining|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3034957A|DE3034957C2|1980-09-17|1980-09-17|Method and device for the internal coating of contact tubes|
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