WO2005072859A1 - Charge de remplissage pour réaction en phase vapeur - Google Patents

Charge de remplissage pour réaction en phase vapeur Download PDF

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Publication number
WO2005072859A1
WO2005072859A1 PCT/JP2005/000938 JP2005000938W WO2005072859A1 WO 2005072859 A1 WO2005072859 A1 WO 2005072859A1 JP 2005000938 W JP2005000938 W JP 2005000938W WO 2005072859 A1 WO2005072859 A1 WO 2005072859A1
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WO
WIPO (PCT)
Prior art keywords
reaction
filler
reaction tube
jacket
gas phase
Prior art date
Application number
PCT/JP2005/000938
Other languages
English (en)
Japanese (ja)
Inventor
Yasuhiko Mori
Original Assignee
Sumitomo Chemical Company, Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Chemical Company, Limited filed Critical Sumitomo Chemical Company, Limited
Publication of WO2005072859A1 publication Critical patent/WO2005072859A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B01J8/067—Heating or cooling the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/0285—Heating or cooling the reactor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/03—Preparation from chlorides
    • C01B7/04—Preparation of chlorine from hydrogen chloride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
    • B01J2208/00176—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles outside the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
    • B01J2208/00212—Plates; Jackets; Cylinders
    • B01J2208/00221—Plates; Jackets; Cylinders comprising baffles for guiding the flow of the heat exchange medium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00654—Controlling the process by measures relating to the particulate material
    • B01J2208/00663—Concentration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/02—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles
    • B01J2208/023—Details
    • B01J2208/024—Particulate material
    • B01J2208/025—Two or more types of catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/19—Catalysts containing parts with different compositions

Definitions

  • the present invention relates to a filler for a gas phase reaction.
  • a gas phase reactor in which a gaseous raw material compound is reacted is usually filled with a filler in order to improve the heat conductivity of the raw material compound and to support and dilute the solid catalyst.
  • Japanese Patent Publication 4 7 4 0 7 9 2 JP page 2 ceramic Raschig rings (Rasching Ring) as a filler, i.e. silica filler (S i 0 2) composite oxide composed mainly of This filler is filled in the upper part of the gas phase reactor, and gaseous N— ( ⁇ -hydroxyethyl) -12-pyrrolidone is supplied from the upper end of the gas phase reactor. A method of heating to 50 ° C. or higher is described.
  • a Raschig ring made of inorganic glass or stainless steel is disclosed as a filler, and this filler is filled in a gas phase reactor, A method is described in which gaseous N- ( ⁇ -methoxyethyl) formamide is introduced and heated to 300 ° C or more to cause a thermal decomposition reaction.
  • Japanese Patent Application Laid-Open No. 2001-276660 discloses that a silica-alumina firing material containing at least 0.5% by weight of an alkali metal element and at least 10% by weight of silicon as an oxide is used as a filler. There is disclosed a filler obtained by carrying an alcohol compound on the resultant and then calcining the filler. The filler is charged into a gas phase reactor, and gaseous 2-ethoxyethanol is introduced into the reactor. A method is described in which a decomposition reaction is carried out by heating at a temperature of 100 ° C. or higher.
  • these conventional fillers are not always durable. For example, if they are used for a long period of time, the fillers are likely to deteriorate or lose their mass due to volatilization of components, and hydrogen chloride (HC) 1) This was particularly noticeable when acidic gas such as gas was used. Disclosure of the invention The present inventors have conducted intensive studies to develop a filler for a gas phase reactor having excellent durability. As a result, the aluminum content is about 90% by weight or more in terms of oxide, that is, in terms of aluminum oxide. The present inventors have found that a filler consisting of has little deterioration and mass change even when used for a long period of time, and can be used for a long period of time.
  • the present invention provides a filler for a gas phase reaction comprising alumina having an aluminum content of about 90% by weight or more in terms of aluminum oxide.
  • the filler of the present invention has excellent durability and can be used for a long time.
  • 1 to 3 are cross-sectional views of a gas-phase reaction reactor filled with a filler according to the present invention.
  • the filler in the present invention is made of alumina, and includes, for example, a crystalline material such as alumina and r-alumina, preferably an alumina.
  • powdered alumina (A 1 2 0 3) may be a sintered body obtained by sintering a.
  • a sintered body made of alumina is preferable because it has a small specific surface area and good thermal conductivity.
  • the alumina in the present invention contains aluminum (A 1) in an amount of about 90% by weight or more, preferably about 92% by weight or more in terms of aluminum oxide. It may contain substantially 100% by weight of aluminum oxide in terms of aluminum oxide without substantially containing metal components other than aluminum.
  • the content of metal components other than aluminum may be 0% or less as long as they are about 10% by weight or less in terms of oxides.
  • the metal component other than aluminum include silicon (S ⁇ , alkali metals such as sodium (Na) and potassium (K), and transition metals such as iron (F e) and titanium (T i). .
  • the specific surface area of the filler in the present invention are preferably lm 2 Z g or less, more preferably 0. 5 m 2 g or less, more preferably not more than 0. 2 m 2 Z g, this case, the filling of the present invention
  • the material is sufficiently durable even when a strongly acidic starting compound such as hydrogen chloride is reacted at a high temperature.
  • the filler exhibits sufficient durability especially in a strong chlorinated atmosphere such as in the presence of hydrogen chloride containing no water.
  • the specific surface area can be measured as a BET specific surface area by a nitrogen adsorption method.
  • a sintered body made of alumina is preferred because it has a small specific surface area.
  • the size of the filler in the present invention can be 0.1 mm or more and 2 cm or less, and is preferably 1 mm or more and 1 cm or less.
  • the shape of the filler varies depending on the shape of the gas phase reactor in which it is used, the reaction conditions, and the like, and is appropriately selected. For example, it may be in the form of an amorphous powder, a sphere, or a column.
  • the spherical shape is preferred because the filling into the reactor is easy, and the bulk density of the filling does not easily change depending on the filling rate.
  • Various types of spherical alumina are commercially available, for example, as a powder frame medium, a catalyst carrier, and the like, and these commercially available aluminas can be used as the filler in the present invention.
  • Examples of commercially available alumina include “HD” (trade name) and rsSA-995j (both manufactured by Nitsukato Corporation).
  • the filler in the present invention can be used by filling a reactor for introducing and reacting a gaseous raw material compound.
  • Examples of such a raw material compound include strongly acidic compounds such as hydrogen chloride (H C 1), and olefins. Since the filler in the present invention has sufficient durability against strongly acidic compounds such as hydrogen chloride, it can be suitably used for the reaction.
  • strongly acidic compounds such as hydrogen chloride (H C 1)
  • olefins since the filler in the present invention has sufficient durability against strongly acidic compounds such as hydrogen chloride, it can be suitably used for the reaction.
  • the gas phase reaction is performed in the reactor filled with the filler according to the present invention.
  • a reaction examples include an oxidation reaction in which hydrogen chloride is used as a raw material compound (A) and oxygen ( ⁇ 2 ) is reacted therewith to produce chlorine (Cl 2 ) as a reactant; Isomerization reaction to obtain an isomer of olefins as a reactant by using the olefins as a reactant; using olefins as a raw material compound, adding water and alcohols thereto, and forming a derivative of the olefins as a reactant An addition reaction to be obtained; and an oxidation reaction in which an olefin is used as a raw material compound and oxygen is reacted therewith to produce an olefin oxide as a reactant.
  • the gas-phase reaction reactor used in the present invention may be a fixed-bed reactor in which the packing material filled therein is fixed and used, or a moving-bed reactor in which the packing material is used while being moved. It may be a fluidized bed reactor which is used while being fluidized together with the raw material compound.
  • FIG. 1 to 3 are cross-sectional views of a gas-phase reactor filled with a gas-phase reaction filler (1) used in the present invention as a filler.
  • the gas phase reactor (2) fixes the filling material The fixed bed reactor used.
  • the gas-phase reactor (2) includes a reaction tube as a reactor body (20), and further includes a jacket (21) that covers the reaction tube (20).
  • a heating medium (3) flows through the jacket (21), and the reaction tube (20) is cooled or heated by the heating medium (3).
  • the heat medium (3) is taken out of the jacket (21), for example, and then temperature-controlled by a heat exchanger (not shown) or the like, and is again introduced into the jacket (21). May be circulated.
  • the type of the heat medium (3) is appropriately selected and used depending on the reaction temperature, and examples thereof include water, oil, molten salt, and ionic liquid.
  • the number of reaction tubes (20) in the gas-phase reactor (2) is not particularly limited.
  • a single-tube gas-phase reactor having only one reaction tube (20) such as a gas-phase reactor (2) shown in FIGS. 1 and 2, or FIG.
  • a multi-tube gas-phase reactor provided with two or more reaction tubes (20), and the plurality of reaction tubes (20) covered with a jacket (21). It may be.
  • the starting compound (A) By introducing the gaseous starting compound (A) into such a gas phase reactor (2), the starting compound (A) can be reacted.
  • the raw material compound (A) is introduced into the reaction tube (20), while the reaction tube (20) is cooled or heated by the heating medium (3).
  • the raw material mixture (A) introduced from the inlet (2a) reacts in the reaction tube, and the reactant (B) generated by the reaction is taken out from the outlet (2c).
  • the position of the filled filler (1) in the reaction tube (20) is not particularly limited.
  • the filler (1) is used by being filled near the inlet (2a) on the upstream side of the reaction region (2b) in the reaction tube (20).
  • the reaction region (2b) is a region where most of the raw material compound (A) reacts, for example, a catalyst layer filled with a solid catalyst for the reaction.
  • the filler (1) in the present invention may be used by filling it near the outlet (2c) downstream of the catalyst layer (2b).
  • the catalyst layer (2b) is supported to prevent the movement of the catalyst due to the wind pressure of the raw material mixture (A), especially the scattering from the outlet. It can be expected that the reaction product (B) after the reaction is rapidly cooled.
  • the filler (1) according to the present invention may be used by filling the catalyst layer (2b) filled with the catalyst together with the catalyst.
  • the amount of catalyst per unit volume in the catalyst layer (2b) can be reduced and adjusted, and the heat transfer from the catalyst can be adjusted. Things can be expected.
  • FIG. 2 when a single reaction tube (20) is filled with a plurality of catalyst layers (2b, 2), a layer (2d) partitioning between the catalyst layers (2b, 2b ') is formed.
  • the filler (1) in the present invention may be filled.
  • the catalyst in the catalyst layers (2b, 2b ') is prevented from moving and being mixed with the flow of the raw material compound (A) and the reactant (B).
  • the raw material compound (A) is heated in the upstream catalyst layer (2b)
  • it can be expected that the heated raw material compound is cooled and led to the downstream catalyst layer (2b ′).
  • the divided catalyst layers (2b, 2b ') may be filled with the same composition of catalytic power or may be filled with different compositions of catalytic power.
  • a jacket (2) may be provided with a partition plate (4).
  • the partition plate (4) supports the plurality of reaction tubes (20), fixes it to the jacket (21), and regulates or blocks the flow of the heat carrier (3) flowing through the jacket (21).
  • the partition plate (4) include a tube plate (41) for fixing the reaction tube (20) to the jacket (21) at the inlet (2a) of the reaction tube (20); and an outlet (2c) for the reaction tube (20).
  • Baffle plate (44) for changing the direction of flow of heat carrier (3).
  • the intermediate tube plate (43) and the baffle plate (44) may be tightly fixed to the reaction tube (20), or may have a slight gap between the reaction tube (20) and The heat medium (3) flowing in the jacket (21) may move between the sections (21, 2 ⁇ ) through the gap.
  • the baffle plate (44) changes the direction of flow of the heat medium (3) in the jacket (21) so that the heat medium (3) flows evenly in the entire jacket (21).
  • the flow of the heat medium (3) in the jacket (21) is adjusted by the partition plates (4) such as the tube sheets (41, 42), the intermediate tube sheet (43), and the baffle plate (44).
  • the inside of the jacket (21) is located near a portion where the reaction tube (20) is in contact with the partition plate (4).
  • the heat medium (3) may stay, and the cooling and heating of the reaction tube (20) may become insufficient near that portion.
  • the filler (1) in a portion of the reaction tube (20) where the heat exchange tends to be insufficient, even if the flow of the heat medium (3) is sufficient.
  • the entire reaction tube (20) can be sufficiently cooled or heated even if it is not.
  • the filler (1) used in the present invention is made of alumina having an aluminum content of 90% by weight or more, and exhibits good thermal conductivity. From the viewpoint of such good thermal conductivity, the filler (1) in the present invention preferably has a specific surface area of 1 m 2 Zg or less. Good. A sintered body made of alumina is preferred because of its small specific surface area and particularly good thermal conductivity.
  • the filler (1) in the present invention is filled near the portion where the reaction tube (20) and the partition plate (4) are in contact inside the reaction tube (20), heating is insufficient. This is preferable because it is possible to prevent a reduction in the reaction yield of the catalyst and a deterioration of the catalyst and a reaction tube due to insufficient cooling.
  • the starting compound (A) can be reacted at 600 ° C or lower, preferably 500 ° C or lower, more preferably 400 ° C or lower.
  • the filler (1) in the present invention exhibits a remarkable durability effect at 200 ° C. or higher. It is preferably used in a reaction for reacting the starting compound (A) at a temperature of at least C, more preferably at least 300 ° C.
  • spherical alumina having a particle diameter of about 3 mm and a specific surface area of 140 m 2 Zg (“NKHD-24”, manufactured by Sumitomo Chemical Co., Ltd. aluminum Niumu content (A 1 2 0 3) 99. 7 wt%, silicon content (S i 0 2) 0. 02 wt%, sodium ⁇ beam content (N a 2 0) 0. 2 7 wt%, iron content (F e 2 0 3) 0 .
  • a reaction tube similar to that of Example 1 was prepared except that a nickel thermometer sheath and a tube having an outer diameter of 6 were installed on the reaction tube so that the gas temperature in the reaction tube could be measured in the axial direction of the reaction tube.
  • the gas inlet side of the reaction tube was filled with a supported catalyst obtained by extrusion molding (1% by weight of ruthenium oxide supported on titania and alumina), and the gas outlet side was the same as that used in Example 1.
  • the same filler was filled.
  • the heat medium was introduced into the jacket covering the reaction tube with the nucleus being 3oo :, while the heat medium was introduced from the gas inlet side of the reaction tube to 300 ”, 0.00”.
  • Hydrogen chloride gas and oxygen gas were mixed and introduced at a flow rate of 300 Nm 3 Z (O: atmospheric pressure) and a flow rate of 0.014 Nm 3 (0, atmospheric pressure).
  • the gas introduced into the reaction tube reacts and generates heat when it comes into contact with the catalyst layer, and the generated reaction gas reaches 350 at the gas outlet of the catalyst layer, but then comes into contact with the filler layer.
  • the heat is removed by the heat transfer between the filler and the heating medium.
  • the temperature of the reaction gas drops to 300, the same as the heating medium.
  • the temperature power of the reaction gas 3 ⁇ 4 decreased slightly, indicating that the heat removal was good.
  • a reaction tube was prepared in the same manner as in Example 1 except that a nickel thermometer sheath and a tube having an outer diameter of 6 were installed in the reaction tube so that the gas temperature in the reaction tube could be measured in the axial direction of the reaction tube.
  • the gas inlet side of the reaction tube was filled with a supported catalyst obtained by extrusion molding (1% by weight of ruthenium oxide supported on titania and alumina), and the gas outlet side was the same as that used in Example 2.
  • the same filler was filled.
  • the temperature was set to 300, and the heat medium was introduced into a jacket covering the reaction tube.
  • Hydrogen chloride gas was introduced at a flow rate of 300 Nm 3 Z (0, converted to atmospheric pressure) and oxygen was introduced at a flow rate of 0.014 Nm 3 / min (0 ° C, converted to atmospheric pressure).
  • the gas introduced into the reaction tube reacts and generates heat when it comes into contact with the catalyst layer, and the generated reaction gas reaches 35 Ot: at the gas outlet of the catalyst layer.
  • the heat is removed by heat transfer between the filler and the heating medium, so that at a distance of 20 cm from the gas inlet side of the filler, the temperature of the reaction gas drops to 310 ° C and a temperature of 45 cm At this point, the reaction gas had decreased to 300, the same as the heat medium.
  • the rapid reduction in the temperature of the reaction gas indicated that the heat removal was good.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

Est décrite une charge de remplissage pour des réactions en phase vapeur qui est constituée d’une alumine ayant une teneur en aluminium d’environ 90 % en poids ou plus en termes d’oxyde d’aluminium. Cette charge de remplissage peut être utilisée en continu pendant une longue période dans la mesure où elle subit peu de changements de propriétés ou de masse même après une longue utilisation.
PCT/JP2005/000938 2004-01-29 2005-01-19 Charge de remplissage pour réaction en phase vapeur WO2005072859A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004-021004 2004-01-29
JP2004021004 2004-01-29

Publications (1)

Publication Number Publication Date
WO2005072859A1 true WO2005072859A1 (fr) 2005-08-11

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2005/000938 WO2005072859A1 (fr) 2004-01-29 2005-01-19 Charge de remplissage pour réaction en phase vapeur

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WO (1) WO2005072859A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5432408A (en) * 1977-08-13 1979-03-09 Mitsubishi Petrochem Co Ltd Preparation of ethylene oxide and its reaction vessel
JP2001137689A (ja) * 1999-08-31 2001-05-22 Nippon Shokubai Co Ltd 接触気相酸化反応器
JP2001199710A (ja) * 2000-01-13 2001-07-24 Sumitomo Chem Co Ltd 塩素の製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5432408A (en) * 1977-08-13 1979-03-09 Mitsubishi Petrochem Co Ltd Preparation of ethylene oxide and its reaction vessel
JP2001137689A (ja) * 1999-08-31 2001-05-22 Nippon Shokubai Co Ltd 接触気相酸化反応器
JP2001199710A (ja) * 2000-01-13 2001-07-24 Sumitomo Chem Co Ltd 塩素の製造方法

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