EP3389847A1 - Reactor for carrying out heterogeneously catalysed gas phase reactions, and use of the reactor - Google Patents
Reactor for carrying out heterogeneously catalysed gas phase reactions, and use of the reactorInfo
- Publication number
- EP3389847A1 EP3389847A1 EP16819519.6A EP16819519A EP3389847A1 EP 3389847 A1 EP3389847 A1 EP 3389847A1 EP 16819519 A EP16819519 A EP 16819519A EP 3389847 A1 EP3389847 A1 EP 3389847A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- reactor
- elements
- gas phase
- built
- heterogeneously catalyzed
- Prior art date
- Legal status (The legal status 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 status listed.)
- Pending
Links
- 238000010574 gas phase reaction Methods 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 20
- 239000000835 fiber Substances 0.000 claims description 106
- 239000000919 ceramic Substances 0.000 claims description 39
- 238000009434 installation Methods 0.000 claims description 22
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 19
- 239000011224 oxide ceramic Substances 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000002638 heterogeneous catalyst Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000002485 combustion reaction Methods 0.000 claims description 4
- 230000036961 partial effect Effects 0.000 claims description 4
- 150000002894 organic compounds Chemical class 0.000 claims description 3
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- 238000006356 dehydrogenation reaction Methods 0.000 claims description 2
- 150000002484 inorganic compounds Chemical class 0.000 claims description 2
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 8
- 229910052863 mullite Inorganic materials 0.000 description 8
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 229910001092 metal group alloy Inorganic materials 0.000 description 3
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- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 description 1
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
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- 229910003465 moissanite Inorganic materials 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/248—Reactors comprising multiple separated flow channels
- B01J19/2485—Monolithic reactors
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
-
- 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
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- 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
- B01J8/0207—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 the fluid flow within the bed being predominantly horizontal
- B01J8/0214—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 the fluid flow within the bed being predominantly horizontal in a cylindrical annular shaped bed
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- 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
- B01J8/04—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 the fluid passing successively through two or more beds
-
- 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
- B01J8/04—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 the fluid passing successively through two or more beds
- B01J8/0446—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 the fluid passing successively through two or more beds the flow within the beds being predominantly vertical
- B01J8/0449—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 the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more cylindrical beds
- B01J8/0453—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 the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more cylindrical beds the beds being superimposed one above the other
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- 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
- B01J8/04—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 the fluid passing successively through two or more beds
- B01J8/0492—Feeding reactive fluids
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- 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
- B01J8/04—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 the fluid passing successively through two or more beds
- B01J8/0496—Heating or cooling the reactor
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- 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
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00805—Details of the particulate material
- B01J2208/00814—Details of the particulate material the particulate material being provides in prefilled containers
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- 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
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00884—Means for supporting the bed of particles, e.g. grids, bars, perforated plates
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/24—Stationary reactors without moving elements inside
- B01J2219/2401—Reactors comprising multiple separate flow channels
- B01J2219/2402—Monolithic-type reactors
- B01J2219/2425—Construction materials
- B01J2219/2433—Construction materials of the monoliths
- B01J2219/2438—Ceramics
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/24—Stationary reactors without moving elements inside
- B01J2219/2401—Reactors comprising multiple separate flow channels
- B01J2219/2402—Monolithic-type reactors
- B01J2219/2441—Other constructional details
- B01J2219/2443—Assembling means of monolith modules
Definitions
- the invention relates to a reactor for carrying out heterogeneously catalyzed gas phase reactions and to a use.
- reaction temperatures In reactors for carrying out heterogeneously catalyzed gas phase reactions, the reaction temperatures often reach values in the range of about 600 to 1,500 ° C, in particular in the range of about 800 to 1, 000 ° C.
- the heterogeneous catalyst which is often in the form of a bed, is used in catalyst baskets supported by suitable bearings, brackets or brackets disposed on the reactor jacket.
- the material used for such catalyst baskets metal alloys are usually used.
- the catalyst basket expands, with the linear expansion for a typical nickel-chromium alloy, such as for the Inconel TM 600 high temperature alloy (material number 2.4816) with a linear expansion coefficient of 18-20 x 10 -6 / K, at a reaction temperature of 1 .000 ° C and a reactor diameter of 5 m is about 80 - 90 mm.
- the invention is therefore based on the technical problem of providing a reactor for carrying out heterogeneously catalyzed gas phase reactions at high reaction temperatures, which largely overcomes the disadvantages described above.
- the invention accordingly provides a reactor for carrying out heterogeneously catalyzed gas phase reactions, with one or more built-in elements in the flow direction of the gas mixture of the heterogeneously catalyzed gas phase reaction through the reactor, the built-in elements extending over the entire reactor cross section.
- the reactor according to the invention is characterized in that the one or more installation elements are at least partially, preferably completely, formed from a fiber composite ceramic material.
- the built-in elements are preferably built-in elements for accommodating a heterogeneous catalyst.
- the built-in elements can also comprise empty elements, which are not flowed through by the reaction gas and therefore usually also contain no catalyst material.
- These empty elements can be so-called dummy bodies which can be installed instead of catalyst-containing built-in elements, for example when the reactor is operated at reduced load.
- the dummy bodies must be designed so that a bypass of reaction gases is prevented.
- the dummy bodies are therefore formed as plates or boxes.
- the inventively provided use of built-in elements of fiber composite ceramic materials ensures that the mounting elements have a reduced thermal expansion and increased high temperature strength, so that the problems described above in the use of fittings made of metal alloys do not occur or only to a much lesser extent.
- the mounting elements in particular those which are not critical for the thermal expansion behavior, can also be formed from materials other than the fiber composite ceramic material, such as grids or networks, in particular if they are not firmly connected to the basic structure of the internals.
- the mounting elements are almost completely, particularly preferably formed completely from a fiber composite ceramic material.
- the fiber composite ceramic material is in particular formed from a ceramic matrix in which ceramic fibers are embedded.
- the fiber composite ceramic materials used according to the invention are characterized by ceramic fibers, in particular long fibers, which are embedded as a wound body or as a textile in a matrix of ceramic particles. It is spoken of fiber-reinforced ceramics, composite ceramics or simply fiber ceramics. In principle, matrix and fiber may consist of all known ceramic materials, in which context carbon is also understood as a ceramic material.
- Suitable fibers are reinforcing fibers which fall into the classes oxide, carbide, nitridic fibers or C fibers and SiBCN fibers.
- the fibers of the ceramic composite material are alumina, mullite, silicon carbide, zirconia and / or carbon fibers.
- Mullite consists of mixed crystals of alumina and silica.
- the use of fibers of oxide ceramic (Al 2 O 3, SiO 2, mullite) or of non-oxide ceramic (C, SiC) is preferred.
- the ceramic matrix and / or the ceramic fibers are formed from an oxide ceramic.
- the mounting elements consist of oxide-ceramic fibers embedded in an oxide-ceramic matrix.
- Such oxide ceramic systems are chemically very stable and durable and can therefore be used in demanding, especially corrosive reaction environments.
- Such an oxide-ceramic system may also contain mixtures of different oxide-ceramic fibers.
- creep-resistant fibers are used, d. H. Fibers, which in the creep range - in the temperature range up to 1400 ° C - show no or only a minimal temporal increase in the permanent deformation, ie the creep strain.
- 3M specifies the following limit temperatures for the NEXTEL TM fibers for 1% compression after 1000h under tensile load of 70 MPa: NEXTEL TM 440: 875 ° C, NEXTEL TM 550 and NEXTEL TM 610: 1010 ° C, NEXTEL TM 720: 1 120 ° C (Reference: Nextel TM Ceramic Textiles Technical Notebook, 3M, 2004).
- the fibers are characterized by a high creep strength to the effect that the strength is ensured in particular under atmospheric air at high operating temperatures.
- the fibers advantageously have a diameter between 10 and 12 ⁇ . They are advantageous to each other - usually with linen or satin weave - woven into textile webs, knitted into tubes or wrapped as a fiber bundle around a mold.
- the fiber bundles or fabrics are, for example, infiltrated with a slip containing the components of the later ceramic matrix, advantageously Al 2 O 3 or mullite (see, for example, Schmücker, M. (2007): “Fiber-reinforced Oxide-Ceramic Materials", Materials Science and Materials Engineering, 38 (9), 698-704).
- the ceramic fiber composite used is preferably SiC / SiC, C / C, C / SiC, Al 2 O 3 / Al 2 O 3 and / or mullite / mullite.
- the material before the slash designates the fiber type and the material after the slash designates the matrix type.
- Matrix system for the ceramic fiber composite structure can also siloxanes, Si precursors and various oxides, such as zirconium oxide, are used.
- Fiber composites based on oxide-ceramic fibers for example 3M TM NEXTEL TM 312, NEXTEL TM 440, NEXTEL TM 550, NEXTEL TM 610 or NEXTEL TM 720, are preferably used in the present invention. Particularly preferred is the use of NEXTEL 720.
- NEXTEL 720 is designed for a continuous operating temperature of 1370 ° C. The expansion coefficient is 6.0 x 10 "6 / K.
- NEXTEL TM are in the form of textile Matt employed 720th
- the matrix has a degree of filling of fibers (volume fraction of the fibers in the composite structure) of 20 to 40%, the total solids content of the composite structure is between 50 and 80%.
- Fiber-composite ceramics based on oxide ceramic fibers are chemically resistant in oxidizing and reducing gas atmospheres (ie no change in weight after storage in air at 1200 ° C. for 15 h (reference: Nextel TM Ceramic Textiles Technical Notebook, 3M, 2004)) and thermally resistant up to more than 1300 ° C. Fiber-composite ceramics have a quasi-ductile deformation behavior. Thus, the fiber composites according to DIN EN 993-1 1 temperature change resistant and have a quasi-tough fracture behavior. Thus, the failure of a component announces itself before it breaks.
- the fiber composite material in particular the oxide ceramic fiber composite material, has the following advantageous properties:
- the fiber composite material advantageously has a porosity of 20% to 50%; it is therefore not gas-tight as defined in DIN 623-2.
- the fiber composite material advantageously has a maximum continuous use temperature of 1000 to 1500 ° C, preferably 1 100 to 1400 ° C, in particular 1200 to 1300 ° C.
- the fiber composite material advantageously has a strength of 50 to 130 [MPa], preferably 70 to 120 [MPa], in particular 80 to 100 [MPa].
- the fiber composite material advantageously has a yield strength of elastic deformation of 0.2 to 1%.
- the fiber composite material is advantageously resistant to thermal shock at the intended operating temperatures in the sense of a test according to DIN EN 993-1 1.
- the fiber composite material advantageously has a thermal coefficient of thermal expansion 3-12 x10 "-6 / K, particularly preferably 5-8 x10- 6 / K on.
- the fiber composite material advantageously has a thermal conductivity [W / m / K] of 0.5 to 30, preferably from 2 to 5, on.
- the fiber composite ceramic material can by CVI (Chemical Vapor Infiltration), pyrolysis, in particular LPI (Liquid Polymer Infiltration), by chemical reaction as LSI (Liquid Silicon Infiltration), or by the WHIPOX TM method (Wound Highly Porous Oxide Composite) are produced.
- the oxide fiber composite ceramic materials have the following advantageous for the inventive use properties: a low thermal expansion coefficient (for mullite about 4 x10 "-6 / K, of alumina about 8 x10" -6 / K, whereas for stainless steel 1 .4841 15 x10 "6 / K) - a low specific gravity (mullite about 2 g / ml compared to about 8 g / l for
- the reactor according to the invention is designed for carrying out heterogeneously catalyzed gas phase reactions at reaction temperatures between 600 and 1500 ° C., preferably also at reaction temperatures between 800 and 1 000 ° C.
- reaction temperature is understood to mean the maximum temperature which is achieved in the reactor during the implementation of the heterogeneously catalyzed gas phase reaction.
- the inventive reactor has one or more successively arranged in the flow direction of the gas mixture of the heterogeneously catalyzed gas phase reaction through the reactor built-in elements for receiving the heterogeneous catalyst, which may be present in particular as a bed or as a monolith on. These extend in each case, optionally in conjunction with dummy bodies, over the entire reactor cross-section.
- the catalyst material can be arranged in each installation element in one or more layers, for example in catalyst layers with different catalytic activity.
- the layers can optionally be separated from one another by a planar arrangement of nets.
- monoliths when monoliths are used, different monoliths can be arranged one above the other.
- the reactor is preferably a reactor for carrying out heterogeneously catalyzed gas phase reactions on an industrial scale.
- the reactor therefore preferably has a reactor cross section which is greater than 0.25 m 2 , particularly preferably greater than 1 m 2 , in the regions in which the one installation element is arranged or in which the plurality of installation elements are arranged.
- the maximum reactor cross section is preferably in the range between 5 and 50 m 2 , in particular between 10 and 30 m 2 .
- the reactor according to the invention may have any reactor cross section, for example a circular, an elliptical or a polygonal cross section.
- the reactor has a circular or approximately circular reactor cross-section, so that the reactor preferably has an overall cylindrical, for example flat-cylindrical design, ie the reactor has in this case a substantially cylindrical reactor shell, which is particularly advantageous for pressure-loaded reactor jackets ,
- the one or more in the flow direction of the gas mixture of the heterogeneously catalyzed gas phase reaction successively arranged in the reactor mounting elements are each formed as one-piece mounting elements.
- One-part in the present context means that a built-in element extends over the entire inner cross section of the reactor and is not subdivided into individual, juxtaposed installation elements.
- integrated mounting element is not limited to one-piece mounting elements, but in the context of the present invention, a “one-piece mounting element” consist of several components.
- the one-piece component is preferably formed as a one-piece basket with a closed vertical side wall and a perforated bottom.
- the perforations of the soil preferably have an opening ratio of 30 to 80%, preferably from 40 to 60%.
- the floor can be firmly integrated into the basket or designed as a loose floor.
- the side wall of the one-piece basket is also a cylinder jacket.
- the cylindrical closed vertical side wall is bent at its upper end to the outside to a horizontal, supporting annular disc. This allows in a simple manner the positioning of the one-piece basket on a support.
- the support is preferably designed as an annular, attached to the inner wall of the reactor shell, in particular welded to the reactor shell console.
- the support is a bearing section integrated into the reactor jacket.
- the bearing section comprises a vertical side wall and a horizontal annular nose projecting into the interior of the reactor.
- the bearing portion is formed as a rotationally symmetrical component which can be produced by turning or milling.
- the storage section the jacket is in particular weldable in the reactor jacket.
- the bearing portion may also have an integrated flange.
- the seal is formed of high temperature resistant mineral fiber materials, such as fiber cords, single or multi-layer fiber ribbons or single or multi-layer fiber mats.
- the fibers are alkaline earth silicates or aluminum silicates.
- Particular preference is given to using fiber mats or fiber swelling mats or tapes as sealing material, as described, for example, in the Applicant's international patent application WO / 2014/125023.
- Fiber swell mats are laminar deposits that expand (swell) with temperature increases.
- Fiber swell mats are usually made of silicates, z.
- silicates z.
- vermiculite As vermiculite, and an organic binder.
- Such fiber mats or fiber swell mats are sheet-like structures with a thickness in the range of about 3 to 20 mm, preferably in a range of about 5 to 10 mm.
- the width and length of the fiber source mats are due to manufacturing technology, and are each in a range of about 0.5 to 5 m.
- a typical measure of fiber source mats is 1, 20 mx 4 m.
- Fiber swell mats are usually made of silicates, preferably in fiber form, for.
- silicates preferably in fiber form, for.
- such Fiber expanding mats are sold for example by the company 3M under the brand name INTERAM® ®.
- the organic binder is in the form of organic polymer fibers, in particular in the form of organic polymer fibers having two or more melting ranges.
- Fiber swell mats containing silicate fibers, a blown mica and organic polymer fibers are particularly advantageous in that they have resilient properties, and thus an excellent seal by clamping between the components, between which cavities are to bridge, ensure:
- the organic polymer fibers begin to melt and crosslink (bond) the fibrous silicates.
- the silicate fibers thereby form a fiber skeleton with cavities in which the expanding mica is incorporated.
- the expanded mica applies tension to the fiber structure and expands it.
- the fiber swell mats are wrapped on all sides in a film made of a plastic, After the Faserquellmatte is wrapped in the plastic film, which is enclosed by the plastic film and the Faserquellmatte containing interior is vacuumed.
- the fiber swell mat expands to twice its thickness in the vacuumed state. This makes it possible, the components provided for assembly loosely, play together, without applying forces, while still ensuring that the expanding during Entvakuum Schlieren fiber source mat securely fixes the components.
- the interior space containing the fiber swelling mat can be easily vacuum-evacuated by piercing or cutting the plastic film.
- the interior space enclosed by the plastic film and containing the fiber swell mat can be vacuum-evacuated by exposing the fiber swell mat to an elevated temperature at which the plastic film burns.
- the individual, vacuum-formed fiber source mats are lined up with a rectangular stepped rebate or in rectangular tongue and groove system, so that the tightness of the connection is ensured.
- the fiber composite ceramic material for the one or more one-piece installation elements for example for the one-piece basket, is selected such that the installation element is self-supporting. Under self-supporting is to be understood that the oxide ceramic installation element in its structure can withstand the mechanical stresses (weight of the bed, own weight, force by pressure loss) under operating conditions even without auxiliary support.
- the one or more built-in elements arranged one behind the other in the flow direction of the gas mixture of the heterogeneously catalyzed gas phase reaction through the reactor are constructed in several parts.
- a "multi-part built-in element” is understood to be a built-in element which consists of a plurality of identical or similar individual built-in components which are arranged side by side in the reactor and substantially together fill the inner cross-section of the reactor.
- Each built-in part of these multi-part mounting elements can be again in one piece or consist of several components.
- the successively arranged in the flow direction of the gas mixture of the heterogeneously catalyzed gas phase reaction one or more, multi-part mounting elements may comprise a plurality, in particular three, four or more grates.
- the grates are preferably positioned loosely next to each other on carriers.
- the multi-part built-in elements may comprise several, in particular three, four or more individual baskets, the baskets each having their own side walls and perforated trays.
- the baskets are preferably positioned loosely next to each other directly on supports or on grates located above the supports.
- the individual baskets are preferably sealed against each other and against the inner wall of the reactor shell, in particular by means of the fiber mats described above or another suitable joint filling material.
- grates are flat perforated plates or grids on which either catalyst material can be arranged directly as a bed or as monoliths or which serve as a support for baskets.
- the grates are for Gas permeable and otherwise designed so that the catalyst material or baskets are safely carried.
- Bases in the context of the present invention also have a gas-permeable bottom and can also be filled with catalyst material as a bed or as monoliths.
- baskets also have an upstanding sidewall which laterally confines the catalyst material. Also in the baskets or on the roasters can again, as described above, several catalyst layers are arranged, for example catalyst layers with different activity.
- the support arrangement on which the individual baskets and / or individual grates are arranged side by side must be able to flow through the gas mixture of the heterogeneously catalyzed gas phase reaction. This can be ensured by providing several carriers, for example rod-shaped carriers, which are arranged at a distance from one another and / or that the carriers are perforated, in particular planar carriers will preferably have perforations for the gas passage.
- the carriers and the multi-part internals are preferably made entirely or partially of fiber-ceramic composite materials.
- T-beams, double-T beams or profiled, in particular corrugated, perforated elements are used as the carrier.
- the multi-part fixtures such as grates and baskets are supported by the carriers and can be designed as complex components, for example as components with a fine lattice structure in the bottom, which causes no pressure loss during gas passage. Since the multi-part internals are supported by the stable beams, the strength of the internals can be reduced in favor of their complexity.
- both the multi-part mounting elements and the carrier are preferably formed from fiber composite ceramic materials.
- a fiber composite material for the carrier with higher strength compared to the fiber composite ceramic material is selected for the mounting elements.
- the carriers which have a simpler geometry compared to the mounting elements, to embed longer fibers in the matrix and thereby achieve a higher strength of the fiber composite ceramic material over the material for the mounting elements, whose geometry is usually more complex ,
- two, three or more built-in elements are provided, which are successively arranged in the reactor by the gas mixture of the heterogeneously catalyzed gas phase reaction.
- additional feeds as well as mixing devices for additional gas can be provided between the individual mounting elements.
- the reactor may advantageously have a conical geometry;
- this reactor geometry also has the advantage that supports on the interior reactor shell do not interfere with the replacement of individual installation elements, so that the same is easier to carry out.
- Preferred uses of the reactor of the invention include use as a furnace or combustor, such as for the complete oxidation / combustion of organic compounds, as a reactor for the partial oxidation of organic compounds, such as for the production of formaldehyde from the oxidation of methanol, as a synthesis gas synthesis reactor.
- a reactor for ammonia oxidation ie for partial oxidation in the presence of ammonia such as for the production of acrylonitrile from propylene and / or acrolein or methacrylonitrile from isobutene and or methacrolein
- a reactor for dehydrogenation in particular for the oxidative dehydrogenation of hydrocarbons, such as for the preparation of propene from propane
- a reactor for the oxidation of inorganic compounds such as for S02-Oxi or for the production of nitric acid by oxidation of ammonia
- Exhaust gas purification such as for IS O decomposition and catalytic afterburning or flue gas cleaning.
- FIG. 1 shows a schematic longitudinal section through an embodiment of a
- inventive reactor with a first variant of a one-piece
- Figure 2 is a view corresponding to Figure 1 of a second variant of a
- Figure 3 is a view corresponding to Figure 1 of a third variant of a
- FIG. 4 shows a detail of FIG. 3
- Figure 5 is a view corresponding to Figure 1 of a fourth variant of a
- Figure 6 is a view corresponding to Figure 1 of a fifth variant of a
- Figure 7 is a view corresponding to Figure 1 of a sixth variant of a one-piece mounting element
- Figure 8 is a view corresponding to Figure 1 of a seventh variant of a
- Figure 10 is a schematic longitudinal section through a preferred embodiment of a reactor with a multi-part mounting element
- Figure 1 1 is a section along the line A-A of Figure 10;
- Figure 12 is a section along the line B-B of Figure 10;
- Figure 13 is a view corresponding to Figure 10 of a second variant of a multi-part mounting element
- Figure 14 is a view corresponding to Figure 10 of a third variant of a
- Figure 15 shows a variant of a carrier for multi-part mounting elements in
- FIG. 16 shows a perspective view of the carrier of FIG. 15.
- Figure 1 shows a longitudinal section through a portion of a reactor 10, in which a one-piece mounting element 1 1 is arranged.
- the one-piece component 1 1 is formed as a basket 12 which is bounded laterally by a vertical side wall 13 and at the bottom of a perforated bottom 14.
- the vertical side wall 13 of the basket 12 merges in the top in an outwardly horizontally angled annular disc 15 which rests on a support 16 which is connected to the wall 17 of the reactor 10, for example by welding.
- the annular disc 15 of the basket 12 is sealed against the support by means of a seal 18.
- catalyst material 19 which may be formed for example as a bed of catalyst particles or as a monolithic catalyst.
- the basket 12 may be covered on its upper side with a precious metal net 20.
- the arrow 21 illustrates the flow direction of the gas flow of the heterogeneously catalyzed gas phase reaction through the reactor 10.
- a weighting element 22 for example one or more covering blocks or a circumferential covering ring, is additionally provided above the horizontally angled annular disk 15 in order to ensure the secure positioning of the noble metal network and the catalyst bed.
- the support 16 is located in a thermally stressed region of the reactor 10, since in this area, the heterogeneously catalyzed gas phase reaction takes place. Therefore, the reliable attachment of the support 16 on the inner wall of the reactor shell 17 is technologically demanding.
- this problem is solved in that the Reactor casing 17 is formed in several parts and has a bearing portion 23, softer inserted at the level of the mounting element 1 1 in the reactor shell 17 and connected to the rest of the reactor shell via welded joints 24.
- the bearing portion 23 of the reactor shell 17 has a side wall 25 and an integrally formed with the side wall 25, inwardly projecting, annular nose 26, which forms the support for the mounting element.
- the side wall 25 extends vertically above and below the annular nose 26 and thus forms part of the reactor shell.
- the bearing portion 23 with its inwardly projecting nose 26 may be formed as a turned or milled workpiece.
- the workpiece section forming the bearing section 23 is again shown in isolation in FIG. Since the welds 24 are now located at a greater distance from the thermally stressed area in the vicinity of the basket 12, high temperature problems in mounting the support in the embodiment shown in Figure 3 can be more easily avoided.
- FIG. 5 shows a fourth variant of a reactor with a one-piece built-in element.
- the mounting element 1 1 is again designed as a basket 12, in contrast to the variants of Figures 1 -3, the vertical side wall 13 is not bent at its upper end horizontally to an annular disc to mount the basket 12 on the support 16, but the Basket 12 is seated in total, again via a sealing ring 18 arranged therebetween, on the support 16.
- FIG. 6 shows a further preferred embodiment of a basket 12 formed as a one-piece mounting element 1 1, wherein between the side wall 13 of the basket 12 and the support 16, an insulating member 27 is provided from high-temperature ceramic, the wall of the reactor shell 17, in particular the side wall 25 of the bearing section 23, thermally protects.
- the support 16 is shown as part of a rotated bearing portion 23, as described in connection with Figure 3 in more detail.
- Figure 7 shows a longitudinal section through a further preferred embodiment with one-piece mounting element 1 1, wherein the jacket 17 of the reactor 10 is again formed in several parts.
- the reactor shell is made of inexpensive mild steel.
- the reactor shell 17 consists of an intermediate ring 30 made of high temperature steel.
- the upper and lower shell sections 28, 29 have connecting flanges 31, 32, between which the intermediate ring is pressed in via sealing elements 33. In these areas, the reactor 10 can also be easily disassembled for maintenance purposes.
- FIG. 9 shows a longitudinal section through a further preferred embodiment of a reactor 10 according to the invention.
- three one-piece installation elements 1 1 arranged one behind the other in the flow direction and formed as baskets 12 are arranged in the reactor 10, as they are also in connection with the variant 1 have already been described in more detail.
- the reactor shell 17 tapers from top to bottom, so that the individual baskets 12 can be easily removed despite a fixedly connected to the reactor shell 17 support 16 by a (not shown) upper mounting opening of the reactor 10.
- devices not shown in FIG. 9, for injecting intermediate gas, withdrawal means or mixing devices can be provided.
- FIG. 10 shows a longitudinal section through a further preferred embodiment of the reactor 10 according to the invention with a built-in element.
- the installation element is designed as a multipart installation element 35.
- the individual parts of the multipart mounting element 35 are formed by grids 36, which are arranged on ceramic supports 37, 38, which in turn rest on the support 16.
- catalyst material 19 is applied, for example as a bed, as shown in Figure 10.
- the catalyst material can also be applied to the grates 36 in monolithic form, for example.
- the grates 36 have one latticed or otherwise perforated structure, which ensures that on the one hand the gas flow can happen, but on the other hand, the catalyst material is retained on the grates.
- the grates 36 are preferably arranged with a certain distance from each other, so that the thermally induced changes in dimensions could be compensated.
- the ceramic carriers 37 in the example shown have a cross-section with a double-T geometry.
- the carrier 37 are formed in the example shown as a straight carrier.
- the peripheral supports 38 may, for example, have a U-shaped cross-section, the base of the U resting against the inner wall of the reactor shell 17.
- the edge-side carrier 38 may also be formed as a carrier with double-T geometry. In the schematic drawing of Figure 12, both variants are shown.
- the peripheral supports 38 are preferably formed as segments and are adapted to the inner wall of the reactor shell 17 over a corresponding length.
- FIG. 14 shows a longitudinal section through a further preferred embodiment of the reactor 10 according to the invention with a multipart installation element 35.
- the multipart installation element consists of baskets 39 which lie directly on the linear supports 37 in double-T geometry and the peripheral supports 38 ,
- the ceramic baskets 39 are filled with catalyst material 19 in the form of catalyst beds or monolith catalysts.
- the baskets 39 of the multi-part mounting element have a perforated bottom 40 and optionally a precious metal net 41 on top of the baskets 39.
- the precious metal network 41 is not provided.
- a particular preferred application of the precious metal network is, for example, the nitric acid oxidation, where the network itself already serves as a catalyst and cause the catalysts in the baskets, so to speak, the purification of the reaction gas.
- the baskets 39 are also designed in number and shape so as to completely fill the inner cross-section of the reactor with the corresponding clearance between the baskets. Since catalyst material 19 is only in the baskets 39, the gaps between the baskets 39 must be filled with a joint filling material 43, for example in the form of a high-temperature fiber mat, in order to prevent a bypass of the gas flow. Also, the edge-side gap between the baskets and the inner wall of the Raktormatels 17 is filled with a filling material 43, preferably with an insulating material.
- the multi-part mounting element consists of both ceramic baskets 39, which are filled with catalyst material in the form of catalyst beds or monolith catalysts, as well as ceramic grids 36.
- the baskets 39 rest on the grates 36, while the grates 36th , as in the variant of Figures 10 - 12 are supported by ceramic support 37, 38. In the gaps between the baskets 39, a high-temperature-resistant joint filling material 43 in the form of high-temperature fiber mats is again introduced.
- the base area of the baskets 39 corresponds to the base area of the grates 36, but the respective base area can also be selected independently of one another, so that, for example, a basket 39 can extend over a plurality of grates 36.
- the oxide ceramic carrier or carrier elements can have a wide variety of shapes. While in the previously described embodiments carriers 37 have been shown in double T-shape or carrier 38 in U-shape, FIGS. 15 and 16 show ceramic carriers 44 having a wavy profiled perforated structure. FIG. 15 shows a cross-sectional view with a grate 36 arranged on the carriers 44 and FIG. 16 a perspective view of the carrier 44 without a grate. In the illustrated example, each carrier 44 consists of a single shaft. By joining several carriers 44 at their longitudinal edges 45, the illustrated periodic structure is formed. In this way, large-area support structures for reactors on an industrial scale can be made easier. However, it is also possible to produce individual carriers 44, which consist of several wave trains.
- the carriers 44 have openings 46 through which the gas of the gas phase reaction can flow.
- An ammonia-air mixture (12.5% by volume of NH3, 87.5% by volume of air) is fed to the ammonia combustion furnace, in which, as shown in Figure 1, a one-piece mounting element is installed.
- the basket has a clear diameter of 3.52 m.
- the reactor is operated with an ammonia / air mixture throughput of 3650 Nm 3 / h and per m 2 of catalyst net area.
- the inlet temperature of the ammonia-air mixture in the reactor is 28.4 ° C and the pressure before the platinum catalyst network in the reactor 1089 mbar (abs.).
- the ammonia burns at temperatures of about 880 ° C. to the reaction product, which is then passed through the catalytically active charge contained in the basket and contains nitrogen monoxide as the main component and small amounts of nitrous oxide N 2 O ("nitrous oxide") 1000 ppm downstream of the platinum catalyst net, ie even before impacting the catalytically active filling in the basket.
- the basket is followed by the basket, which contains a 150 mm high layer of unsupported catalyst strands, these strand rods having a star-shaped cross-section, 6 mm in diameter and 5 to 30 mm in length, consisting of a mixture of CuO, ZnO and Al 2 O 3.
- the basket has a lateral boundary which is approximately 250 mm high.
- sampling point 1 Directly after the platinum catalyst network (sampling point 1) and in the middle of the reactor downstream directly below the bottom of the basket (sampling point 2) and at the periphery of the reactor downstream directly below the outer edge region of the bottom of the basket (sampling point 3) samples of the Reaction product are removed and analyzed for nitrous oxide concentration by GC / MS method.
- Another extraction point 4 is installed downstream of the basket and a downstream waste heat exchanger unit.
- an ammonia-air mixture is reacted as described above, wherein a metallic basket of Inconel 600 (material number 2.4816) is used.
- the catalytically active filling has a funnel-shaped depression in the form of a trench of 96 mm depth.
- the height of the existing bed in the edge area above the ground is only 54 mm (before the beginning of the test it was 150 mm).
- the measured nitrous oxide concentration at the sampling point 3 practically below the funnel-shaped depression is 676 ppm nitrous oxide
- the measured nitrous oxide concentration is 186 ppm so that the average measured nitrous oxide concentration downstream of the metallic basket and the downstream downstream heat exchanger unit at the sampling point 4 is 227 ppm ,
- the basket was made by infiltrating a Nextel TM 610 oxide ceramic fabric with a slip containing Al 2 O 3 and laminating it to a shape appropriate to the desired basket geometry. After drying at 100 ° C, the dried material was demolded and fired at 1250 ° C.
- the edge region in the ceramic basket has only a small funnel-shaped depression in the form of a trench of 37 mm depth in the catalytically active filling whose height in the edge region of the ceramic basket is still 1 13 mm (before the start of the experiment 150 mm).
- the measured nitrous oxide concentration at the sampling point 3 practically below the funnel-shaped depression is 316 ppm nitrous oxide, at the sampling point 2 the measured nitrous oxide concentration is 190 ppm so that the average measured nitrous oxide concentration downstream of the oxide ceramic basket and the downstream downstream heat exchanger unit at the sampling point 4 is 199 ppm ,
- edge-sided ceramic support preferably U-profile, wall-adapted
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Abstract
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PCT/EP2016/081571 WO2017103199A1 (en) | 2015-12-16 | 2016-12-16 | Reactor for carrying out heterogeneously catalysed gas phase reactions, and use of the reactor |
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WO2021213747A1 (en) * | 2020-04-20 | 2021-10-28 | Haldor Topsøe A/S | Reactor for a catalytic process |
CN112871122B (en) * | 2020-12-31 | 2022-11-29 | 哈尔滨工业大学 | Reaction kettle for preparing nano silicon modified steel fibers in large batch and preparation method |
WO2023232853A1 (en) * | 2022-06-02 | 2023-12-07 | Casale Sa | Catalyst support system for ammonia oxidation burners |
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CN103341674B (en) * | 2013-06-26 | 2015-05-27 | 哈尔滨工业大学 | Graphene auxiliary brazing method for ceramic matrix composite material and metal material |
PL3033302T3 (en) | 2013-08-16 | 2018-04-30 | Basf Se | Basket-like device with wall insulation |
WO2015048505A1 (en) * | 2013-09-30 | 2015-04-02 | Kimberly-Clark Worldwide, Inc. | Thermoplastic article with active agent |
FR3018526B1 (en) | 2014-03-14 | 2021-06-11 | Herakles | CVI DENSIFICATION INSTALLATION INCLUDING A HIGH-CAPACITY PREHEATING ZONE |
FR3024053B1 (en) * | 2014-07-28 | 2020-07-24 | Total Raffinage Chimie | GAS INJECTION ELEMENT IN A REGENERATOR OF A FLUID CATALYTIC CRACKING UNIT |
WO2016055453A1 (en) | 2014-10-07 | 2016-04-14 | Basf Se | Reactor for carrying out gas-phase reactions using a heterogeneous catalytic converter |
WO2016055452A1 (en) | 2014-10-07 | 2016-04-14 | Basf Se | Reactor for carrying out gas phase reactions using a heterogeneous catalytic converter |
HUE060103T2 (en) | 2015-11-27 | 2023-01-28 | Basf Se | Modular catalyst monoliths |
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2016
- 2016-12-16 WO PCT/EP2016/081571 patent/WO2017103199A1/en active Application Filing
- 2016-12-16 RU RU2018125955A patent/RU2727172C2/en active
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US10576449B2 (en) | 2020-03-03 |
RU2727172C2 (en) | 2020-07-21 |
CN108602042B (en) | 2021-03-16 |
WO2017103199A1 (en) | 2017-06-22 |
RU2018125955A3 (en) | 2020-05-14 |
CN108602042A (en) | 2018-09-28 |
US20180369780A1 (en) | 2018-12-27 |
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