CN114893792B - Remote ignition system and method for hydrogen bromide synthesis furnace - Google Patents
Remote ignition system and method for hydrogen bromide synthesis furnace Download PDFInfo
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- CN114893792B CN114893792B CN202210573283.3A CN202210573283A CN114893792B CN 114893792 B CN114893792 B CN 114893792B CN 202210573283 A CN202210573283 A CN 202210573283A CN 114893792 B CN114893792 B CN 114893792B
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- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 title claims abstract description 212
- 229910000042 hydrogen bromide Inorganic materials 0.000 title claims abstract description 106
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 71
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims description 43
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 165
- 239000001257 hydrogen Substances 0.000 claims abstract description 161
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 161
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 156
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 156
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 152
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000007789 gas Substances 0.000 claims abstract description 83
- 230000001105 regulatory effect Effects 0.000 claims abstract description 68
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 53
- 238000010926 purge Methods 0.000 claims abstract description 13
- 238000002485 combustion reaction Methods 0.000 claims description 15
- 150000002431 hydrogen Chemical class 0.000 claims description 10
- 230000001276 controlling effect Effects 0.000 claims description 7
- 238000007689 inspection Methods 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- 239000000047 product Substances 0.000 description 60
- 239000003570 air Substances 0.000 description 59
- 238000006243 chemical reaction Methods 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 239000002994 raw material Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 7
- 238000006073 displacement reaction Methods 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
- 238000004880 explosion Methods 0.000 description 5
- 238000005049 combustion synthesis Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 230000031709 bromination Effects 0.000 description 2
- 238000005893 bromination reaction Methods 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical class [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001347 alkyl bromides Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229910001503 inorganic bromide Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23Q—IGNITION; EXTINGUISHING-DEVICES
- F23Q21/00—Devices for effecting ignition from a remote location
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Hydrogen, Water And Hydrids (AREA)
Abstract
The invention discloses a remote ignition system for a hydrogen bromide synthesis furnace, which comprises a bromine vapor control unit, a compressed air control unit, a hydrogen control unit, a tail gas control unit and a hydrogen bromide product control unit; the hydrogen control unit comprises a hydrogen product pipeline and an emergency nitrogen replacement pipeline which are arranged in parallel; the tail gas emission end is provided with a tail gas control unit, the tail gas control unit comprises a tail gas switching valve and a tail gas regulating valve which are arranged in parallel, and a second hydrogen concentration on-line monitor is arranged at the outlet of the tail gas emission end; the second hydrogen concentration on-line monitor is used for setting a threshold value, when the hydrogen concentration in the synthesis furnace exceeds the set threshold value, the bromine vapor control unit, the compressed air control unit and the hydrogen control unit are closed, the tail gas switch valve and the nitrogen switch valve are opened, nitrogen purging replacement is carried out on the gas system in the hydrogen bromide synthesis furnace, and nitrogen is blown in to reduce the hydrogen concentration.
Description
Technical Field
The invention relates to the technical field of hydrogen bromide synthesis, in particular to a remote ignition system and method for a bromination synthesis furnace.
Background
The binary compounds of hydrogen bromide, also known as hydrobromic acid, HBr, are highly corrosive and can react with some active metal powders, and are basic raw materials for manufacturing various inorganic bromides and certain alkyl bromides. The high corrosiveness of the material can be used in etching processes in the semiconductor industry. In the prior art, the plasma hydrogen bromide etching technology can accurately control the etching depth and verticality, does not damage an ozone layer and generate greenhouse gas, and is a good substitute for fluorocarbon etching gas. With the development of the semiconductor industry, the electronic grade hydrogen bromide used for etching the main process of the process has raised higher requirements, and during the process, if the impurities pollute, the functions of circuits in the wafer are easily damaged, so that the integrated circuits are disabled and the formation of geometric characteristics is affected, and therefore, hydrogen bromide gas with high purity is required.
In the prior art, the synthesis method of hydrogen bromide comprises a direct combustion synthesis method of bromine and hydrogen and other methods. In a synthesis apparatus and a synthesis method of hydrogen bromide disclosed in chinese patent No. CN110523351a, hydrogen bromide is obtained by a method in which bromine reacts with ammonia gas to produce hydrogen bromide and nitrogen gas, and then the nitrogen gas is separated. The hydrogen bromide as the final product of the method contains more impurities, increases the difficulty of separation and purification, and prevents the hydrogen bromide from being utilized in the electronic grade hydrogen bromide direction.
Therefore, in order to obtain a high-purity hydrogen bromide gas, the direct combustion synthesis method is a main method for synthesizing electronic grade hydrogen bromide. However, the reaction conditions are severe, the nozzle design of the combustion apparatus is demanding and complex, and uneven mixing of the raw materials is easily caused. The synthesis furnace of hydrogen bromide disclosed in Chinese patent No. 113501500A adopts a replacement ignition method, firstly uses oxygen and hydrogen to ignite for combustion reaction, and after the flame stabilization is achieved, uses bromine vapor to replace oxygen for hydrogen bromide synthesis reaction, so that the method reduces impurities in hydrogen bromide products, and simultaneously solves the problem of unstable flame caused by direct ignition of bromine and hydrogen. However, in the replacement ignition method adopted by the method, an operator needs to perform on-site ignition in the ignition process, the ignition operation steps are more, the replacement ignition method adopted by the method needs to be operated step by step strictly according to the operation steps, the operator is easy to misoperate in the ignition process, flame extinction is caused, the hydrogen excess seriously reaches the explosion limit, flash explosion occurs, and a control room cannot judge the flame state in the normal production process. Obviously, this field ignition method presents a significant safety risk. Therefore, the invention further improves the ignition system of the synthesis furnace based on the hydrogen bromide synthesis furnace, and improves the on-site ignition system into a remote ignition system.
Disclosure of Invention
The invention aims to provide a remote ignition system and a remote ignition method for bromination synthesis, which do not need to be ignited by an operator on site, can leave the site to carry out remote control on the ignition system only by checking whether the states of valves and equipment are in initial preparation states on the site by the operator, and can avoid the safety problem caused by artificial misoperation.
In order to achieve the above object, the present invention has the technical scheme that:
the remote ignition system for the hydrogen bromide synthesis furnace comprises a bromine vapor control unit, a compressed air control unit, a hydrogen control unit, a tail gas control unit and a hydrogen bromide product control unit, wherein the bottom of the hydrogen bromide synthesis furnace is provided with a nozzle, and the top of the hydrogen bromide synthesis furnace is provided with a tail gas discharge end and a product output end; the bromine vapor control unit, the compressed air control unit and the hydrogen control unit are respectively connected with the nozzle; the hydrogen control unit comprises a hydrogen product pipeline and an emergency nitrogen replacement pipeline which are arranged in parallel; the emergency nitrogen replacement pipeline is provided with a nitrogen switch valve and a nitrogen pipeline check valve; the product output end is provided with a hydrogen bromide product control unit; the tail gas emission end is provided with a tail gas control unit, the tail gas control unit comprises a tail gas switching valve and a tail gas regulating valve which are arranged in parallel, and a second hydrogen concentration on-line monitor is arranged at the outlet of the tail gas emission end and used for detecting the hydrogen concentration of a port; the second hydrogen concentration on-line monitor is used for setting a threshold value, when the hydrogen concentration in the synthesis furnace exceeds the set threshold value, the bromine vapor control unit, the compressed air control unit and the hydrogen control unit are closed, the tail gas switch valve and the nitrogen switch valve are opened, nitrogen purging replacement is carried out on the gas system in the hydrogen bromide synthesis furnace, and nitrogen is blown in to reduce the hydrogen concentration.
Further, the nozzle is provided with an air input port, a hydrogen input port and a bromine vapor input port; the bromine vapor control unit, the compressed air control unit and the hydrogen control unit are respectively connected with the bromine vapor input port, the air input port and the hydrogen input port.
Further, the bromine vapor control unit comprises a bromine product pipeline connected with a bromine vapor input port, and a bromine overhead tank, a bromine flowmeter, a bromine flow regulating valve, a liquid bromine switch valve, a bromine evaporator, a bromine vapor temperature control device and a bromine vapor switch valve which are sequentially arranged on the bromine product pipeline; the bromine high-level tank is arranged at the top end of the bromine product pipeline and is used for providing bromine for the hydrogen bromide synthesis furnace; the bromine flowmeter and the bromine flow regulating valve control the flow of bromine flowing into the bromine evaporator from the bromine overhead tank.
Further, the arrangement height range of the bromine overhead tank is 3-7 m, so that bromine automatically flows into the bromine evaporator by gravity; the bromine vapor temperature at the outlet of the bromine evaporator is 75-150 ℃.
Further, the compressed air control unit comprises an air product pipeline fixedly connected with the air input port, and an air flowmeter, an air regulating valve and an air switching valve which are sequentially arranged on the air product pipeline; the air flow meter of the air product pipeline and the air flow regulating valve are used for controlling and regulating the flow of compressed air, and the flow of the compressed air is 30% -50% of the flow of bromine.
Further, the hydrogen control unit comprises a hydrogen product pipeline connected with the hydrogen input port, and a hydrogen flowmeter, a hydrogen flow regulating valve, a hydrogen product pipeline, a hydrogen switch valve and a hydrogen pipeline check valve which are sequentially arranged on the hydrogen product pipeline; the hydrogen flowmeter and the hydrogen flow regulating valve are used for controlling the flow of hydrogen, and the molar flow ratio of hydrogen to bromine is 1.05-1.15:1.
Further, the hydrogen product line is provided with a flame arrester near the hydrogen input port; the emergency nitrogen replacement pipeline is arranged between the hydrogen pipeline check valve and the flame arrester and is arranged in parallel with the hydrogen product pipeline.
Further, the hydrogen bromide product control unit comprises a hydrogen bromide product pipeline, and a hydrogen bromide regulating valve, a hydrogen bromide cooler and a first hydrogen concentration on-line monitor which are sequentially arranged on the hydrogen bromide product pipeline; the first hydrogen concentration on-line monitor is used for detecting the concentration of hydrogen at the output end of the product, when the concentration exceeds a threshold value set by the first hydrogen concentration on-line monitor, the bromine switch valve, the bromine vapor switch valve, the hydrogen switch valve and the hydrogen bromide regulating valve are automatically closed, the nitrogen switch valve and the tail gas switch valve are automatically opened, nitrogen purging replacement is carried out on a gas system in the hydrogen bromide synthetic furnace, and nitrogen is blown in to reduce the concentration of hydrogen in the furnace.
Further, the outer wall of the hydrogen bromide synthesis furnace is provided with a flame monitor and SIS interlocking in a flame height range, the flame monitor automatically detects flame combustion conditions in the hydrogen bromide synthesis furnace, when the flame detector alarms, the bromine switch valve, the bromine steam switch valve, the hydrogen switch valve and the hydrogen bromide regulating valve are automatically closed, and the nitrogen switch valve and the tail gas switch valve are opened, so that nitrogen purging replacement of the hydrogen bromide synthesis furnace is realized.
The method for igniting by adopting the remote ignition system comprises the following operation steps:
s1, confirming an initial state of an inspection system on site: the inspection liquid bromine switching valve, the bromine steam switching valve, the bromine regulating valve, the air switching valve, the nitrogen switching valve, the hydrogen bromide regulating valve and the tail gas switching valve are all in a closed state; the tail gas regulating valve is in a full-open state; the bromine evaporator is in a hot standby state; the hydrogen bromide cooler is in a cold standby state.
S2, igniting a central control room: after confirming that the initial state is correct through the site, the central control room performs one-key ignition, and the ignition step comprises the following steps:
(1) Opening the air switch valve and starting timing at the same time, wherein the time for compressed air to enter the nozzle from the air switch valve is T 1 ；
(2)T 1 Igniting the automatic igniter after the time, and monitoring the ignition condition of the automatic igniter through a flame monitor;
(3) After the flame monitor monitors that the flame state of the automatic igniter is normal, a hydrogen switch valve is opened, and hydrogen enters the hydrogen bromide synthesis furnace to perform combustion reaction;
(4) After the temperature of the hydrogen bromide synthesis furnace reaches a preset temperature, opening a liquid bromine switch valve and a bromine steam switch valve;
(5) Respectively regulating a bromine regulating valve and an air regulating valve, wherein the regulating amplitude is 5% each time, the regulating interval time is 3-10 min, and gradually replacing the oxidant in the hydrogen bromide synthesis furnace with bromine steam from air;
(6) After the replacement is completed and the flame is stabilized, the hydrogen bromide regulating valve is gradually regulated, the tail gas regulating valve is regulated down, the synthesized hydrogen bromide product is switched into the hydrogen bromide cooler, and the hydrogen bromide product is collected and stored after being cooled.
Synthesizing high-purity hydrogen bromide gas by adopting a displacement ignition method; the replacement ignition method is to mix hydrogen and compressed air and then ignite and burn to generate oxidation-reduction reaction, then gradually replace the compressed air with bromine vapor to react with the hydrogen to synthesize hydrogen bromide.
In the displacement ignition method, the gas in the synthesis furnace has two reaction gases of hydrogen and oxygen, three reaction gases of hydrogen, oxygen and bromine, and two reaction gases of hydrogen, oxygen and bromine.
Because the bromine vapor and the hydrogen are directly synthesized by the combustion method, the required activation energy is high, the combustion chamber temperature is generally 800 ℃, the bromine vapor is at least preheated to more than 350 ℃ before the reaction, and more importantly, the combustion reaction of the hydrogen and the bromine gas is extremely easy to explode, and the danger coefficient is extremely high.
The method for synthesizing the hydrogen bromide by the combustion method has the advantages of good stability and strong continuity operability, so that the method adopts a replacement ignition method on the basis of the prior art, realizes remote control ignition by regulating and controlling the conditions of raw material gas and product gas at an input end and an output end, avoids direct ignition combustion of hydrogen and bromine vapor, adopts the existing method for carrying out combustion reaction on the hydrogen and the oxygen, then introducing the bromine vapor to combust with the hydrogen, gradually increases the content of the bromine vapor, reduces the content of the oxygen until the bromine vapor completely replaces the oxygen, realizes combustion synthesis of the bromine vapor and the hydrogen, generates the hydrogen bromide gas, and has easy reaction and simple operation.
In summary, the following technical effects are obtained by adopting the technical scheme:
1. by adopting the technical scheme of the invention, remote control ignition is realized by regulating and controlling the conditions of the raw material gas and the product gas at the input end and the output end, an operator only needs to check whether the states of the valves and the equipment are in the initial preparation state before reaction, and the on-site operation of the operator is not needed, so that the method is safe and reliable.
2. The bromine high-level tank is arranged at the height position of 3m or more and h or less than 7m, bromine automatically flows into the bromine evaporator by gravity, so that the transportation by a pump is avoided, and corrosion and leakage are reduced.
3. The invention adopts a remote ignition system with simple structure, can be matched with a synthesis furnace in the prior art for use, has convenient operation, saves the cost of manual operation and improves the economic benefit.
4. The remote ignition system of the invention combines the replacement ignition method in the prior art, firstly uses compressed air and hydrogen to ignite for combustion reaction, and then uses bromine vapor to replace the compressed air, thereby greatly reducing the danger coefficient of direct reaction of the bromine vapor and the hydrogen.
5. The invention is based on the replacement ignition method, adopts the synthesis furnace in the prior art to carry out remote ignition control, further improves the safety of synthesis, reduces the danger coefficient caused by misoperation of personnel and improves the accuracy of ignition operation on the basis of realizing high-purity hydrogen bromide synthesis.
6. According to the invention, the nitrogen control unit is additionally arranged, a nitrogen purging mode can be automatically started according to the monitoring of the concentration of the online hydrogen, the flame combustion condition in the synthesis path is automatically detected, SIS interlocking is arranged, when the flame detector alarms, the switching valve of each pipeline is automatically closed, and meanwhile, the nitrogen switching valve and the tail gas switching valve are opened, so that nitrogen purging replacement is carried out on the synthesis furnace, the concentration of the hydrogen in the synthesis furnace is reduced, and the risk of explosion is eliminated.
Drawings
Fig. 1 is a schematic structural diagram of embodiment 1 of the present invention.
The marks in the figure: a bromine overhead tank 1, a bromine product line 2, a bromine flowmeter 3, a bromine regulating valve 4, a liquid bromine flow switching valve 5, a bromine evaporator 6, a bromine vapor switching valve 7, a bromine vapor delivery port 8, an air product line 9, an air flow meter 10, an air regulating valve 11, an air switching valve 12, an air delivery port 13, a nitrogen switching valve 14, a hydrogen flow meter 15, a hydrogen flow regulating valve 16, a hydrogen product line 17, a hydrogen switching valve 18, a hydrogen line check valve 19, a hydrogen delivery port 20, an automatic igniter 21, a flame monitor 22, a hydrogen bromide regulating valve 23, an in-furnace pressure control device 24, an emergency nitrogen displacement line 25, an in-furnace temperature control device 26, a hydrogen bromide cooler 27, a first hydrogen concentration on-line monitor 28, a hydrogen bromide product line 29, a tail gas switching valve 30, a tail gas regulating valve 31, a second hydrogen concentration on-line monitor 32, a burst disk 33, a nozzle 34, a synthesis furnace 35, a bromine vapor temperature control device 36, a nitrogen line check valve 37, and a flame arrester 38.
Detailed Description
The invention adopts a displacement ignition method to synthesize high-purity hydrogen bromide gas; the replacement ignition method is to mix hydrogen and compressed air and then ignite and burn to generate oxidation-reduction reaction, then gradually replace the compressed air with bromine vapor to react with the hydrogen to synthesize hydrogen bromide. In the displacement ignition method, the gas in the synthesis furnace has two reaction gases of hydrogen and oxygen, three reaction gases of hydrogen, oxygen and bromine, and two reaction gases of hydrogen, oxygen and bromine. Based on the replacement ignition method, the synthesis furnace in the prior art is adopted for remote ignition control, so that the safety of synthesis is further improved, the danger coefficient caused by misoperation of personnel is reduced, and the accuracy of ignition operation is improved on the basis of realizing high-purity hydrogen bromide synthesis.
The following description of the embodiments of the present invention will clearly and fully describe the technical solutions of the embodiments of the present invention in conjunction with the specific contents of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
Example 1
The hydrogen bromide synthesis furnace selected in the embodiment has the structure of the synthesis furnace disclosed in Chinese patent No. CN 113501500A.
The synthesis furnace 35 includes a nozzle 34 provided at the bottom, a tail gas discharge end provided at the top, and a product output end. The nozzle 34 is provided with a raw material feed port. The raw material gas is conveyed into the synthesis furnace 35 through the raw material conveying port for reaction, tail gas is discharged through the tail gas discharge port, and products are output through the product output port.
In this embodiment, the nozzle 34 extends into the interior of the synthesis furnace 35, and an automatic igniter 21 is provided at the furnace outlet of the nozzle 34.
The raw material delivery ports are all arranged on the nozzle 34, comprise an air input port 13, a hydrogen input port 20 and a bromine vapor input port 8, and are respectively connected with an air product pipeline 9, a hydrogen product pipeline 17 and a bromine product pipeline 2 to deliver air, hydrogen and bromine into the synthesis furnace 35 through the nozzle 34.
The synthesized hydrogen bromide is discharged via hydrogen bromide product line 29. Other tail gases pass through the tail gas discharge port
Referring to fig. 1, in the present embodiment, three control units, namely a bromine vapor control unit, a compressed air control unit and a hydrogen gas control unit, are connected to the nozzle 34.
In particular, the bromine vapor control unit comprises a bromine product line 2 connected to a bromine vapor input port 8; the bromine production line further comprises a bromine overhead tank 1, a bromine flowmeter 3, a bromine flow regulating valve 4, a liquid bromine switching valve 5, a bromine evaporator 6, a bromine steam temperature control device 36 and a bromine steam switching valve 7 which are sequentially arranged on the bromine product line 2. The bromine overhead tank 1 is arranged at the top end of the bromine product pipeline 2 and provides bromine reaction raw materials for the synthesis furnace 35.
Preferably, the arrangement height h of the bromine high-level tank 1 is required to be in a range of 3m less than or equal to h less than or equal to 7m, and the bromine raw material is arranged at a high level, so that the bromine automatically flows into the bromine evaporator 6 by gravity, thereby avoiding the transportation by a pump and reducing corrosion and leakage. And bromine flow is controlled by a bromine flow meter 3 and a bromine flow regulating valve 4.
More preferably, the heat source of the bromine evaporator 6 may use electric heating, steam or heat conducting oil, etc., and the bromine vapor temperature at the outlet of the bromine evaporator 6 is required to be in the range of 75 ℃ to 150 ℃.
The compressed air control unit comprises an air product pipeline 9 fixedly connected with an air input port 13, and further comprises an air flowmeter 10, an air regulating valve 11 and an air switching valve 12 which are sequentially arranged on the air product pipeline 9.
Preferably, the air flow meter 10 and the air flow regulating valve 11 of the air product line 9 are used to control and regulate the flow of compressed air, the compressed air flow being 30% -50% of the bromine flow.
The hydrogen control unit comprises a hydrogen product pipeline 17 fixedly connected with a hydrogen input port 20, and further comprises a hydrogen flowmeter 15, a hydrogen flow regulating valve 16, a hydrogen product pipeline 17, a hydrogen switch valve 18 and a hydrogen pipeline check valve 19 which are sequentially arranged on the hydrogen product pipeline 17.
Preferably, the hydrogen product pipeline 17 is provided with a hydrogen flowmeter 15 and a hydrogen flow regulating valve 16, which are used for controlling the flow of hydrogen, and the molar flow ratio of hydrogen to bromine is automatically regulated to be 1.05-1.15:1 through proportion control.
Further, the hydrogen product line 17 is provided with a flame arrestor 38 near the hydrogen input port 20 to prevent flame flashback and explosion.
In this embodiment, an emergency nitrogen replacement line 25 is provided between the hydrogen line check valve 19 and the flame arrester 38, and is used for performing nitrogen purge replacement on the system in the whole synthesis furnace under the conditions of failed ignition, flame extinction and shutdown of the synthesis furnace 35, so as to prevent explosion.
Preferably, the nitrogen product line 25 is connected in parallel with the hydrogen product line 17 and fixedly connected to the hydrogen input port 20, and the nitrogen product line 25 is provided with a nitrogen on-off valve 14 and a nitrogen line check valve 37.
Further, a hydrogen bromide product control unit and a tail gas control unit are respectively arranged at the tail gas discharge end and the product output end at the top end of the synthesis furnace 35.
The hydrogen bromide product control unit comprises a hydrogen bromide product pipeline 29, and a hydrogen bromide regulating valve 23, a hydrogen bromide cooler 27 and a first hydrogen concentration on-line monitor 28 which are sequentially arranged on the hydrogen bromide product pipeline 29. The first hydrogen concentration on-line monitor 28 is used to detect the concentration of hydrogen at the product end.
The hydrogen bromide cooler 27 is used to cool down the hydrogen bromide product. Meanwhile, the first hydrogen concentration on-line monitor 28 is used for on-line monitoring the hydrogen concentration of the hydrogen bromide product pipeline 29, when the detection value of the first hydrogen concentration on-line monitor 28 exceeds a set value, the bromine switch valve 5, the bromine vapor switch valve 7, the hydrogen switch valve 18 and the hydrogen bromide regulating valve 23 are automatically closed, the nitrogen switch valve 13 and the tail gas switch valve 30 are automatically opened, and nitrogen purging replacement is carried out on a gas system in the synthesis furnace 35.
The tail gas control unit comprises a tail gas switch valve 30, a tail gas regulating valve 31 and a rupture disk 33 which are arranged in parallel, and a second hydrogen concentration on-line monitor 32 is arranged at the tail gas discharge end and is used for detecting the hydrogen concentration of a port; the rupture disk 33 serves to prevent overpressure rupture of the synthesis furnace 35.
Specifically, the second hydrogen concentration on-line monitor 32 is configured to monitor the concentration of hydrogen in the synthesis furnace 35 in the ignition state, and once the hydrogen concentration exceeds a set threshold value, the air switch valve 12 and the hydrogen switch valve 18 are automatically closed, the nitrogen switch valve 13 and the tail gas switch valve 30 are automatically opened, the nitrogen purge replacement is performed on the gas system in the synthesis furnace 35, the nitrogen is blown in to reduce the hydrogen concentration, and when the second hydrogen concentration on-line monitor 32 shows that the hydrogen concentration in the synthesis furnace 35 is lower than the required concentration, the re-ignition is allowed, otherwise, the switch valves are in a locked state and cannot be operated.
Preferably, the synthetic furnace 35 is made of transparent quartz glass, so that the internal flame combustion hydrogen can be conveniently monitored, a flame monitor 22 is arranged on the outer wall of the synthetic furnace 35 within the flame height range, the flame combustion condition in the synthetic furnace 35 can be automatically detected, SIS interlocking is arranged, when the flame detector 22 alarms, the bromine switch valve 5, the bromine steam switch valve 7, the hydrogen switch valve 18 and the hydrogen bromide regulating valve 23 are automatically closed, and the nitrogen switch valve 13 and the tail gas switch valve 30 are opened, so that the nitrogen purging replacement of the synthetic furnace 35 is realized.
The SIS interlock is a safety instrument system (safty instruments system abbreviated as SIS), which is one type of interlock system and generally implements safety protection control of process equipment of a factory, and sometimes includes unit safety protection control. Can be realized by adopting the prior art.
Preferably, the outer wall of the synthesis furnace 35 is provided with an outer jacket, and circulating cooling water is introduced into the jacket for removing heat generated in the reaction process, so as to prevent heat accumulation in the synthesis furnace and overtemperature.
Further, in the synthesis furnace 35, an in-furnace pressure control device 24 and an in-furnace temperature control device 26 are provided, respectively, for monitoring the temperature and pressure of the synthesis furnace. Preferably, the pressure control device 24 is a pressure transmission, and when the pressure in the synthesis furnace exceeds a set value, the tail gas switching valve 36 is automatically opened, so that the overpressure of the synthesis furnace is prevented, and the replacement of rupture discs is reduced.
The system device is used for remote ignition, and comprises the following operation steps:
1. on-site validation checking initial state of system: the inspection liquid bromine switch valve 5, the bromine steam switch valve 7, the bromine regulating valve 4, the air regulating valve 11, the air switch valve 12, the nitrogen switch valve 13, the hydrogen switch valve 18, the hydrogen bromide regulating valve 23 and the tail gas switch valve 30 are all in a closed state; the exhaust gas regulating valve 31 is in a fully open state; the bromine evaporator 6 is in a hot standby state; the hydrogen bromide cooler 27 is in a cold standby state.
2. Ignition of a central control room: after confirming that the initial state is correct on site, the central control room performs one-key ignition, and the specific steps of ignition include:
(1) Opening the air switching valve 12 and simultaneously starting the timing, the compressed air enters the nozzle 34 from the air switching valve 12 for a time T 1 。
(2)T 1 After the ignition time, the automatic igniter 21 ignites, the ignition condition is monitored through the flame monitor 22, and whether the flame state is normal is continuously monitored after the ignition is successful.
(3) The hydrogen switch valve 18 is opened, and hydrogen enters the nozzle 34 from the hydrogen switch valve 18 to perform combustion reaction with oxygen
(4) After the temperature of the synthesis furnace thermometer reaches the preset temperature, the liquid bromine switch valve 5 and the bromine steam switch valve 7 are opened.
(5) Gradually increasing the opening of the bromine regulating valve 4, reducing the opening of the air regulating valve 11, regulating the amplitude 5% each time, and regulating the interval time to 3-10 min, so as to gradually replace the oxidant in the synthesis furnace 35 by bromine steam from air.
(6) After the replacement is completed and the flame is stabilized, the hydrogen bromide regulating valve 23 is gradually increased, the opening of the tail gas regulating valve 31 is reduced, the synthesized hydrogen bromide product is switched to be placed in the hydrogen bromide cooler 27, and the hydrogen bromide product is collected and stored after being cooled.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. A method of remote ignition for a remote ignition system of a hydrogen bromide synthesis furnace, comprising the steps of:
s1, confirming an initial state of an inspection system on site: the inspection liquid bromine switch valve, bromine vapor switch valve, bromine regulating valve, air switch valve, nitrogen switch valve, hydrogen bromide regulating valve and tail gas switch valve are all in a closed state; the tail gas regulating valve is in a full-open state; the bromine evaporator is in a hot standby state; the hydrogen bromide cooler is in a cold standby state;
s2, igniting a central control room: after confirming that the initial state is correct through the site, the central control room performs one-key ignition, and the ignition step comprises the following steps:
(1) Opening the air switch valve and starting timing at the same time, wherein the time for compressed air to enter the nozzle from the air switch valve is T 1 ；
（2）T 1 Igniting the automatic igniter after the time, and monitoring the ignition condition of the automatic igniter through a flame monitor;
(3) After the flame monitor monitors that the flame state of the automatic igniter is normal, a hydrogen switch valve is opened, and hydrogen enters the hydrogen bromide synthesis furnace to perform combustion reaction;
(4) After the temperature of the hydrogen bromide synthesis furnace reaches a preset temperature, opening a liquid bromine switch valve and a bromine vapor switch valve;
(5) Respectively adjusting a bromine adjusting valve and an air adjusting valve, wherein the adjusting amplitude is 5% each time, the adjusting interval time is 3-10 min, and gradually replacing the oxidant in the hydrogen bromide synthesis furnace with bromine vapor from air;
(6) After the replacement is finished and the flame is stabilized, gradually adjusting a hydrogen bromide regulating valve, adjusting a tail gas regulating valve, switching the synthesized hydrogen bromide product into a hydrogen bromide cooler, cooling and collecting and storing;
the device is characterized in that the remote ignition system comprises a bromine vapor control unit, a compressed air control unit, a hydrogen control unit, a tail gas control unit and a hydrogen bromide product control unit;
the bromine vapor control unit, the compressed air control unit and the hydrogen control unit are respectively connected with the nozzle;
the hydrogen control unit comprises a hydrogen product pipeline and an emergency nitrogen replacement pipeline which are arranged in parallel; the emergency nitrogen replacement pipeline is provided with a nitrogen switch valve and a nitrogen pipeline check valve;
the product output end is provided with a hydrogen bromide product control unit;
the tail gas emission end is provided with a tail gas control unit, the tail gas control unit comprises a tail gas switching valve, a tail gas regulating valve and a rupture disk which are arranged in parallel, and a second hydrogen concentration on-line monitor is arranged at the outlet of the tail gas emission end and used for detecting the hydrogen concentration of a port;
the second hydrogen concentration on-line monitor is used for performing nitrogen purging replacement on a gas system in the hydrogen bromide synthesis furnace when the hydrogen concentration in the synthesis furnace exceeds the set threshold value, a bromine vapor control unit, a compressed air control unit and a hydrogen control unit are closed, a tail gas switching valve and a nitrogen switching valve are opened, and nitrogen is blown in to reduce the hydrogen concentration;
the nozzle is provided with an air input port, a hydrogen input port and a bromine vapor input port; the bromine vapor control unit, the compressed air control unit and the hydrogen control unit are respectively connected with the bromine vapor input port, the air input port and the hydrogen input port;
the bromine vapor control unit comprises a bromine product pipeline connected with a bromine vapor input port, and a bromine overhead tank, a bromine flowmeter, a bromine flow regulating valve, a bromine switching valve, a bromine evaporator, a bromine vapor temperature control device and a bromine vapor switching valve which are sequentially arranged on the bromine product pipeline; the bromine high-level tank is arranged at the top end of the bromine product pipeline and is used for providing bromine for the hydrogen bromide synthesis furnace; the bromine flowmeter and the bromine flow regulating valve control the flow of bromine flowing into the bromine evaporator from the bromine overhead tank;
the arrangement height range of the bromine overhead tank is 3-7 m, so that bromine automatically flows into the bromine evaporator by gravity; the temperature of bromine vapor at the outlet of the bromine evaporator is 75-150 ℃;
the hydrogen control unit comprises a hydrogen product pipeline connected with the hydrogen input port, and a hydrogen flowmeter, a hydrogen flow regulating valve, a hydrogen switching valve and a hydrogen pipeline check valve which are sequentially arranged on the hydrogen product pipeline; the hydrogen flowmeter and the hydrogen flow regulating valve are used for controlling the flow of hydrogen, and the molar flow ratio of hydrogen to bromine is 1.05-1.15:1;
the hydrogen bromide product control unit comprises a hydrogen bromide product pipeline, and a hydrogen bromide regulating valve, a hydrogen bromide cooler and a first hydrogen concentration on-line monitor which are sequentially arranged on the hydrogen bromide product pipeline; the first hydrogen concentration on-line monitor is used for detecting the concentration of hydrogen at the output end of the product, when the concentration exceeds a threshold value set by the first hydrogen concentration on-line monitor, the bromine switch valve, the bromine vapor switch valve, the hydrogen switch valve and the hydrogen bromide regulating valve are automatically closed, the nitrogen switch valve and the tail gas switch valve are automatically opened, nitrogen purging replacement is carried out on a gas system in the hydrogen bromide synthetic furnace, and nitrogen is blown in to reduce the concentration of hydrogen in the furnace.
2. The method of claim 1, wherein the compressed air control unit comprises an air product line fixedly connected to the air input port, and an air flow meter, an air regulating valve, and an air switching valve sequentially provided on the air product line; the air flow meter of the air product pipeline and the air regulating valve are used for controlling and regulating the flow of compressed air, and the flow of the compressed air is 30% -50% of the flow of bromine.
3. The method of claim 1, wherein the hydrogen product line is provided with a flame arrestor proximate the hydrogen input port; the emergency nitrogen replacement pipeline is arranged between the hydrogen pipeline check valve and the flame arrester and is arranged in parallel with the hydrogen product pipeline.
4. The method of claim 1, wherein the outer wall of the hydrogen bromide synthesis furnace is provided with a flame monitor and SIS interlocking in a flame height range, the flame monitor automatically detects flame combustion conditions in the hydrogen bromide synthesis furnace, when the flame monitor alarms, the bromine switch valve, the bromine vapor switch valve, the hydrogen switch valve and the hydrogen bromide regulating valve are automatically closed, the nitrogen switch valve and the tail gas switch valve are opened, and nitrogen purging replacement of the hydrogen bromide synthesis furnace is realized.
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| CN113754165B (en) * | 2021-09-08 | 2023-04-25 | 山东瑞纳特化工有限公司 | Initiator waste acid recycling device system and method |
| CN115120994A (en) * | 2022-08-16 | 2022-09-30 | 苏州金宏气体股份有限公司 | Bromine evaporator and bromine evaporation system |
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