CN113716526B - Combustion reactor for producing high-purity electronic grade hydrogen bromide and equipment thereof - Google Patents

Combustion reactor for producing high-purity electronic grade hydrogen bromide and equipment thereof Download PDF

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CN113716526B
CN113716526B CN202111180729.8A CN202111180729A CN113716526B CN 113716526 B CN113716526 B CN 113716526B CN 202111180729 A CN202111180729 A CN 202111180729A CN 113716526 B CN113716526 B CN 113716526B
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hydrogen bromide
electronic grade
purity electronic
grade hydrogen
combustion reactor
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CN113716526A (en
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马建修
靖宇
杜文东
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Fujian Fudou New Material Co ltd
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Fujian Fudou New Material Co ltd
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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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/165—Natural alumino-silicates, e.g. zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/261—Drying gases or vapours by adsorption
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C01B7/09—Bromine; Hydrogen bromide
    • C01B7/093—Hydrogen bromide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/106—Silica or silicates
    • B01D2253/108—Zeolites
    • B01D2253/1085—Zeolites characterized by a silicon-aluminium ratio
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/304—Linear dimensions, e.g. particle shape, diameter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/306—Surface area, e.g. BET-specific surface

Abstract

The invention provides a combustion reactor for producing high-purity electronic grade hydrogen bromide and equipment thereof, and relates to the technical field of electronic grade hydrogen bromide production. The combustion reactor for producing the high-purity electronic grade hydrogen bromide comprises a shell, a plurality of nozzle tube bundles and a coil; the upper end of the nozzle tube bundle is provided with a catalyst, the nozzle tube bundle with the volume flow ratio of introduced hydrogen to bromine gas of R comprises an inner tube and an outer tube which are sleeved with each other, hydrogen is introduced between the inner tube and the outer tube, and bromine gas is introduced into the inner tube; wherein 1 sR are woven in 1.5. The equipment for producing the high-purity electronic grade hydrogen bromide comprises a combustion reactor, a two-stage rectifying tower, a deep dehydration device, a filtering device and a filling device which are sequentially connected and used for producing the high-purity electronic grade hydrogen bromide. According to the combustion reactor and the equipment for producing the high-purity electronic grade hydrogen bromide, hydrogen gas flows through the outer pipe, bromine gas flows through the inner pipe, the volume flow ratio R of the hydrogen gas to the bromine gas is controlled to be 1-cloth R-cloth 1.5, and the problems that bromine is incompletely combusted and flames are easily extinguished are effectively solved.

Description

Combustion reactor for producing high-purity electronic grade hydrogen bromide and equipment thereof
Technical Field
The invention relates to the technical field of production of electronic grade hydrogen bromide, and particularly relates to a combustion reactor for producing high-purity electronic grade hydrogen bromide and equipment thereof.
Background
High-purity electronic grade hydrogen bromide is widely applied to etching processes of manufacturing processes in high precision fields such as ultra-large scale integrated circuits, flat panel displays, photovoltaics and the like. The high-purity hydrogen bromide can generate bromine free radicals under the action of plasma, and can etch polycrystalline silicon with high selectivity. The polysilicon etching stage in the integrated circuit is the most precise manufacturing process and is the key to realize the line width of a Critical Dimension (CD), so hydrogen bromide is a very critical electronic gas for the etching process and is an important mark for measuring the technical capability of new national chemical electronic materials. The pKa of hydrogen bromide is-9, and compared with hydrogen chloride of the same family, hydrogen bromide has stronger ionization characteristics, extremely high hygroscopicity and strong corrosion to equipment, so that the separation and purification of high-purity electronic grade hydrogen bromide faces many technical challenges, such as the removal of trace water, the dissociation of hydrogen bromide hydrate, the removal of trace metal impurities and the like. The research on the separation and purification of high-purity electronic grade hydrogen bromide is also developed in China in many cases to solve the dilemma of being restricted by people for a long time.
Although China is the third world bromine-producing country, a large amount of bromine still needs to be imported. At present, the synthesis of hydrogen bromide in China is actually derived from the early Israel hydrobromic acid synthesis process, and is also the synthesis method of hydrogen bromide disclosed in the chemical industry at present, the method is to directly burn hydrogen and bromine gas at the normal pressure of 500-600 ℃ (without catalyst) or 300-500 ℃ (with platinum catalyst) for combination reaction, then recycle the unreacted bromine gas through the activated carbon pressure swing adsorption technology, then absorb the gaseous hydrogen bromide into 42% or 62% hydrobromic acid through a water cooling absorption tower, and at the moment, gas-phase impurities such as nitrogen, oxygen and the like are separated from liquid and removed. When gaseous hydrogen bromide is desired, the hydrogen bromide is evaporated after concentration. However, these are all hydrobromic acid preparations which are very difficult to apply to anhydrous electronic grade hydrogen bromide.
The known hydrogen bromide synthesizing process is that hydrogen and bromine react at 300-500 deg.c in the presence of platinum catalyst to produce hydrogen bromide gas. Wherein the reaction equation is:
H 2 +Br 2 =====2HBr
the purification is realized by the combination of zeolite molecular sieve and rectification. However, practice has found that a number of problems are encountered in the production process. The following:
1. the flame of the hydrogen bromide synthesis combustion is easy to extinguish, so that the safety is difficult to ensure.
2. Unreacted bromine easily sputters to the wall and bottom of the reactor, causing severe corrosion of the equipment.
3. The product hydrogen bromide gas is mixed with a large amount of bromine and hydrogen, and the later purification pressure is large.
4. The generated hydrogen bromide has high water content and large subsequent deep dehydration pressure.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a combustion reactor for producing high-purity electronic grade hydrogen bromide, wherein the combustion reactor effectively avoids the problems that bromine is not completely combusted and flames are easily extinguished by using hydrogen to pass through an outer pipe and bromine to pass through an inner pipe and controlling the volume flow ratio R, 1-straw-R-straw-1.5 of the hydrogen and the bromine, so that the production efficiency and the conversion rate of the bromine are greatly improved, and simultaneously, the conversion rate of the bromine is improved and the corrosion of the bromine to equipment is also avoided.
The invention also aims to provide equipment for producing high-purity electronic grade hydrogen bromide, which is provided with a combustion reactor for producing the high-purity electronic grade hydrogen bromide, wherein the hydrogen gas passes through an outer pipe, the bromine gas passes through an inner pipe, and the volume flow ratio of the hydrogen gas to the bromine gas is controlled to be R, 1-R-straw-type 1.5, so that the problems of incomplete bromine combustion and easy flame extinction are effectively avoided, and the production efficiency of the whole process is greatly improved.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a combustion reactor for producing high-purity electronic grade hydrogen bromide, which comprises a shell, a plurality of nozzle tube bundles vertically arranged in the shell in an array manner, and a coil pipe arranged above the nozzle tube bundles and used for introducing air;
the upper end of the nozzle tube bundle is provided with a catalyst, the nozzle tube bundle with the volume flow ratio of introduced hydrogen to bromine gas being R comprises an inner tube and an outer tube which are mutually sleeved, hydrogen is introduced between the inner tube and the outer tube, and bromine gas is introduced into the inner tube; wherein 1 sR are woven in 1.5.
Further, in a preferred embodiment of the present invention, the outer tube is provided at an outer side thereof with an outer fin extending obliquely upward, and a graphite layer is provided on an upper surface of the outer fin.
Further, in a preferred embodiment of the present invention, the upper end of the inner tube is recessed outwardly such that the upper end of the nozzle tube bundle forms a converging section and a diverging section.
Further, in a preferred embodiment of the present invention, the diameter of the expanding section of the outer tube is reduced, and the longitudinal section of the expanding section of the outer tube is a straight line.
Further, in a preferred embodiment of the present invention, a spiral pattern is disposed inside the inner tube.
Further, in a preferred embodiment of the present invention, an inner fin is disposed inside an upper end of the inner tube, and the inner fin extends obliquely upward.
Further, in a preferred embodiment of the present invention, the combustion reactor for producing high purity electronic grade hydrogen bromide further comprises a jacket disposed outside the housing.
The invention also provides equipment for producing the high-purity electronic grade hydrogen bromide, which comprises a combustion reactor for producing the high-purity electronic grade hydrogen bromide, a two-stage rectifying tower, a deep dehydration device, a filtering device and a filling device.
Further, in the preferred embodiment of the present invention, the adsorbent of the deep dehydration device is a modified nano-sized mordenite molecular sieve, the pore diameter of the modified nano-sized mordenite molecular sieve is 5-10 angstroms, and the specific surface area is 300-500m 2 The silicon-aluminum ratio is 20-30, the particle size of the mordenite raw powder is 10-100nm, and the carrier is alumina.
Further, in a preferred embodiment of the present invention, the modified nano-sized mordenite molecular sieve is prepared by the following steps: activating the mordenite raw powder in a muffle furnace at 500 ℃ for at least 2 hours, then soaking the activated mordenite raw powder with 1-3mol/L hydrochloric acid for at least 2 hours, filtering, washing with water, drying, grinding again, crushing and granulating to obtain the modified nano-scale mordenite molecular sieve.
The combustion reactor and the equipment for producing the high-purity electronic grade hydrogen bromide have the advantages that:
(1) The combustion reactor for producing high-purity electronic-grade hydrogen bromide is characterized in that the outer pipe is arranged through hydrogen, bromine gas is arranged through the inner pipe, the volume flow ratio R of the hydrogen to the bromine gas is controlled to be 1, 1-layer-R-layer-1.5, the problems that bromine is incompletely combusted and flame is easily extinguished are effectively solved, the production efficiency and the conversion rate of bromine are greatly improved, meanwhile, the conversion rate of the bromine is improved, and the corrosion of the bromine to equipment is also avoided.
(2) The equipment for producing the high-purity electronic grade hydrogen bromide modifies the adsorbent of the deep dehydration device, greatly improves the adsorption capacity of the adsorbent and improves the purity of the prepared hydrogen bromide.
(3) The hydrogen bromide is directly purified after being prepared by combustion reaction of equipment for producing high-purity electronic grade hydrogen bromide, so that the problem of high dehydration pressure when the hydrogen bromide is concentrated and evaporated from hydrobromic acid is solved.
(4) The outer tube of the nozzle tube bundle is provided with the outer fins, so that the bromine is effectively prevented from corroding equipment.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic diagram of a first configuration of a combustion reactor for producing high purity electronic grade hydrogen bromide in accordance with an embodiment of the present invention;
FIG. 2 is a schematic diagram of a second configuration of a combustion reactor for producing high purity electronic grade hydrogen bromide in accordance with an embodiment of the present invention;
FIG. 3 is an enlarged schematic view at A in FIG. 1;
FIG. 4 is another schematic view of a nozzle bundle according to an embodiment of the present invention;
FIG. 5 is a schematic top view of a nozzle bundle according to an embodiment of the present invention;
FIG. 6 is a schematic top view of a nozzle bundle according to an embodiment of the present invention;
figure 7 is a schematic diagram of the apparatus for producing high purity electronic grade hydrogen bromide in accordance with an embodiment of the present invention.
In the figure: 100-producing a combustion reactor for high purity electronic grade hydrogen bromide; 110-a housing; 120-a nozzle bundle; 130-coil pipe; 111-jacket; 121-inner tube; 122-an outer tube; 123-catalyst; 124-a contraction section; 125-an expansion section; 126-inner fins; 127-outer fins; 200-equipment for producing high-purity electronic grade hydrogen bromide; 210-a two-stage rectification column; 220-deep dehydration device; 230-a filtration device; 240-filling means.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "upper", "lower", "vertical", "inside", "outside", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships conventionally put in use of products of the present invention, and are only for convenience of description and simplicity of description, but do not indicate or imply that the devices or elements referred to must have specific orientations, be constructed in specific orientations, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, the term "vertical" or the like does not imply that the components are required to be absolutely horizontal or overhanging, but rather may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed" and "connected" are to be interpreted broadly, e.g., as being either fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
Referring to fig. 1-2, the present embodiment provides a combustion reactor 100 for producing high purity electronic grade hydrogen bromide, which includes a shell 110, a plurality of nozzle tube bundles 120, and a coil 130. A plurality of nozzle tube bundles 120 are disposed in a vertical array within the shell 110. The coil 130 is disposed above the nozzle bundle 120 and is internally ventilated for dissipating heat from the entire nozzle bundle 120. The outside of the case 110 is provided with a jacket 111 for heat exchange.
Referring to fig. 1-4, the nozzle bundle 120 includes an inner tube 121 and an outer tube 122 sleeved with each other. The upper end of the nozzle bundle 120 is provided with a catalyst 123. Hydrogen is introduced between the inner tube 121 and the outer tube 122, and bromine is introduced into the inner tube 121. The volume flow ratio of the hydrogen gas to the bromine gas is R, wherein 1 is formed by the layers R and 1.5. The excessive hydrogen can push bromine to burn to the front edge of the flame, so that the bromine is fully burned, and the flame is stable. The problem that effective flame is easy to extinguish greatly improves the production efficiency and the conversion rate of bromine, and simultaneously improves the conversion rate of bromine and avoids the corrosion of bromine to equipment. When R =1.4, the effect is optimal.
Referring to fig. 3 and 4, the upper ends of the inner tubes 121 are outwardly recessed such that the upper ends of the nozzle bundles 120 form a converging section 124 and a diverging section 125. The contraction section 124 and the expansion section 125 of the nozzle tube bundle 120 form a structure similar to a laval passage, so that the flow speed of hydrogen can be greatly improved, flame can be effectively pushed upwards, flame extinguishment is effectively avoided, and the reaction stability is improved. In this embodiment, the longitudinal cross sections of the contracting section 124 and the expanding section 125 of the inner tube 121 are two straight lines (fig. 3) with different lines, and in other embodiments, the longitudinal cross sections of the contracting section 124 and the expanding section 125 of the inner tube 121 may also be one continuous curve (fig. 4), so long as the present embodiment can improve the flow speed of hydrogen, can effectively push up flame, effectively avoid flame extinction, and improve the technical effect of reaction stability, all within the protection scope of the present embodiment. In this embodiment, a spiral pattern (not shown) is further provided inside the inner tube 121. The spiral pattern increases the turbulence of bromine, so that the flow of bromine on the inner tube 121 side can be accelerated, and the phenomenon that the bromine is attached to the inner tube 121 to cause blockage is avoided. Referring to fig. 5 and 6, the inner side of the upper end of the inner tube 121 is provided with an inner fin 126 pointing to the center line of the inner tube 121, the inner fin 126 extends obliquely upward, and the inner fin 126 can increase the turbulence degree of the bromine inside, so that the hydrogen and the bromine on the outer side are fully mixed, the movement of the front edge of the bromine flame towards the flame direction can be promoted, the flame is effectively stabilized, and the incomplete penetration of the bromine on the side of the inner tube 121 can be avoided. It should be noted that, in the present embodiment, the inner fins 126 point to the center line of the inner tube 121 (fig. 5), in other embodiments, the inner fins 126 may be distributed spirally (fig. 6) in sequence, and do not point to the center line of the inner tube 121, so that the technical effect of effectively stabilizing the flame in the present embodiment can be achieved, and the present embodiment is also within the protection scope of the present embodiment.
Referring to fig. 1-4, the diameter of the expanding section 125 of the outer tube 122 is reduced, and the longitudinal section of the expanding section 125 of the outer tube 122 is a straight line. Above-mentioned structure sets up for at the in-process of reaction, hydrogen flows towards whole nozzle tube bundle 120's central authorities along the expansion section 125 of outer tube 122, can effectively avoid the sputtering of bromine, has improved the security, can help nozzle tube bundle 120 heat dissipation simultaneously. It is to be understood that in the present invention, the diameter of the expanding section 125 of the outer tube 122 becomes smaller, and the longitudinal section of the expanding section 125 of the outer tube 122 is a straight line. In other embodiments, the diameter of the expanding section 125 of the outer tube 122 may be unchanged, or the diameter of the expanding section 125 of the outer tube 122 is reduced, but the longitudinal section of the expanding section 125 of the outer tube 122 is a curve, which also can achieve the effect of increasing the flow speed of hydrogen in this embodiment, and can effectively push the flame upwards, thereby effectively avoiding the flame from being extinguished, and improving the technical effect of reaction stability, and is also within the protection scope of this embodiment. The outer side of the outer tube 122 is provided with an outer fin 127 extending obliquely upwards, and the upper surface of the outer fin 127 is provided with a graphite layer, so that corrosion caused by bromine sputtering when flame combustion is insufficient can be effectively avoided, and the outer tube 122 is prevented from being corroded due to overflow, and safety accidents occur. Meanwhile, the outer fins 127 can help heat dissipation to some extent. It should be noted that, in this embodiment, the outer tube 122 is provided with the outer fin 127, and the upper surface of the outer fin 127 is provided with the graphite layer, in other embodiments, the graphite layer may not be provided, and even the outer fin 127 is not provided, the technical effect of preparing the high-purity electronic grade hydrogen bromide can be achieved, and it is within the scope of the present embodiment.
Example 2
Referring to fig. 7, the present embodiment further provides an apparatus 200 for producing high purity electronic grade hydrogen bromide, which comprises a combustion reactor 100 for producing high purity electronic grade hydrogen bromide, a two-stage rectifying tower 210, a deep dehydration device 220, a filtering device 230 and a filling device 240, which are connected in sequence.
The adsorbent of the deep dehydration device 220 is a modified nano-grade mordenite molecular sieve. The modified nanometer mordenite molecular sieve has a pore diameter of 5-10 angstroms and a specific surface area of 300-500m 2 The silicon-aluminum ratio is 20-30, the particle size of the mordenite raw powder is 10-100nm, and the carrier is alumina.
The modified nano-grade mordenite molecular sieve is prepared by the following method: activating the mordenite raw powder in a muffle furnace at 500 ℃ for at least 2 hours, then soaking the activated mordenite raw powder with 1-3mol/L hydrochloric acid for at least 2 hours, filtering, washing with water, drying, grinding again, crushing and granulating to obtain the modified nano-scale mordenite molecular sieve.
In conclusion, the combustion reactor for producing high-purity electronic-grade hydrogen bromide and the equipment thereof provided by the invention have the advantages that the combustion reactor for producing high-purity electronic-grade hydrogen bromide passes through the hydrogen to pass through the outer pipe, the bromine to pass through the inner pipe, and the volume flow ratio R of the hydrogen to the bromine is controlled, wherein the number of the hydrogen to the bromine is 1-less and R-less is 1.5, so that the problems that bromine is not completely combusted and flames are easily extinguished are effectively avoided, the production efficiency and the conversion rate of bromine are greatly improved, meanwhile, the conversion rate of the bromine is improved, and the corrosion of the bromine to the equipment is also avoided. The equipment for producing the high-purity electronic grade hydrogen bromide modifies the adsorbent of the deep dehydration device, greatly improves the adsorption capacity of the adsorbent and improves the purity of the prepared hydrogen bromide. The hydrogen bromide is directly purified after being prepared by combustion reaction of equipment for producing high-purity electronic grade hydrogen bromide, so that the problem of high dehydration pressure when the hydrogen bromide is concentrated and evaporated from hydrobromic acid is solved. The outer tube of the nozzle tube bundle is provided with the outer fins, so that the bromine is effectively prevented from corroding equipment.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (9)

1. A combustion reactor for producing high-purity electronic grade hydrogen bromide is characterized by comprising a shell, a plurality of nozzle tube bundles vertically arranged in the shell in an array manner, and a coil pipe which is arranged above the nozzle tube bundles and is communicated with air;
the upper end of the nozzle tube bundle is provided with a catalyst, the nozzle tube bundle with the volume flow ratio of introduced hydrogen to bromine gas being R comprises an inner tube and an outer tube which are sleeved with each other, the hydrogen is introduced between the inner tube and the outer tube, and the bromine gas is introduced into the inner tube; wherein, 1 is composed of the layers of R-cloth 1.5; the outer side of the outer tube is provided with an outer fin extending upwards in an inclined mode, and the upper surface of the outer fin is provided with a graphite layer.
2. A combustion reactor for producing high purity electronic grade hydrogen bromide according to claim 1, wherein the upper end of said inner tube is outwardly concave such that the upper end of said nozzle tube bundle forms a converging section and a diverging section.
3. A combustion reactor for producing high purity electronic grade hydrogen bromide according to claim 2 wherein said flared section of said outer tube is of reduced diameter and said flared section of said outer tube is of straight longitudinal cross-section.
4. A combustion reactor for the production of high purity electronic grade hydrogen bromide according to claim 1, wherein the inside of said inner tube is provided with a helical pattern.
5. A combustion reactor for the production of high purity electronic grade hydrogen bromide according to claim 1, wherein said inner tube is provided with internal fins on the inside of its upper end, said internal fins extending obliquely upward.
6. A combustion reactor for producing high purity electronic grade hydrogen bromide according to claim 1 further comprising a jacket disposed outside of said housing.
7. An apparatus for producing high purity electronic grade hydrogen bromide, which comprises the combustion reactor for producing high purity electronic grade hydrogen bromide according to claim 1, a two-stage rectifying tower, a deep dehydration device, a filtering device and a filling device which are connected in sequence.
8. The apparatus for producing high purity electronic grade hydrogen bromide according to claim 7, wherein the adsorbent of said deep dehydration device is modified nano-grade mordenite molecular sieve, the pore diameter of said modified nano-grade mordenite molecular sieve is 5-10 angstroms, and the specific surface area is 300-500m 2 The silicon-aluminum ratio is 20-30, the particle size of the mordenite raw powder is 10-100nm, and the carrier is alumina.
9. The apparatus for producing high purity electronic grade hydrogen bromide according to claim 8, wherein said modified nano-sized mordenite molecular sieve is prepared by a method comprising: activating the mordenite raw powder in a muffle furnace at 500 ℃ for at least 2 hours, then soaking the activated mordenite raw powder with 1-3mol/L hydrochloric acid for at least 2 hours, filtering, washing with water, drying, grinding again, crushing and granulating to obtain the modified nano-scale mordenite molecular sieve.
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