CN113582136B - Method for synthesizing low-moisture hydrogen bromide gas - Google Patents
Method for synthesizing low-moisture hydrogen bromide gas Download PDFInfo
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- CN113582136B CN113582136B CN202110914498.2A CN202110914498A CN113582136B CN 113582136 B CN113582136 B CN 113582136B CN 202110914498 A CN202110914498 A CN 202110914498A CN 113582136 B CN113582136 B CN 113582136B
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Abstract
The application discloses a method for synthesizing low-moisture hydrogen bromide gas, which is characterized by comprising the following steps: the method comprises the following steps: 1) Introducing bromine into a bromine electric heater, and gasifying the bromine by the bromine electric heater to obtain high-temperature bromine gas; 2) Introducing the high-temperature bromine gas obtained in the step 1) into a synthesis furnace; 3) Introducing hydrogen into the synthetic furnace after the step 2), wherein the hydrogen enters the synthetic furnace from the furnace end of the synthetic furnace; burning hydrogen in high-temperature bromine gas and synthesizing a hydrogen bromide gas semi-finished product; 4) Introducing the hydrogen bromide gas semi-finished product obtained in the step 3) into a buffer tank; 5) Removing impurities from the hydrogen bromide gas semi-finished product obtained in the step 3) to obtain a hydrogen bromide gas finished product. The method for synthesizing the low-moisture hydrogen bromide gas adopts a simple method to synthesize the hydrogen bromide gas, has simple operation, convenient observation and low operation pressure.
Description
Technical Field
The invention relates to a method for synthesizing low-moisture hydrogen bromide gas, belonging to the field of chemical production.
Background
Hydrogen bromide is used for producing various bromine compounds, and also for industries of medicine, dye, perfume, etc., and is a basic raw material for producing various inorganic bromides such as hydrobromic acid, potassium bromide, lithium bromide, calcium bromide, etc., and certain alkyl bromides such as methyl bromide, ethyl bromide, etc.
In the production of part of fine chemical products, high-purity hydrogen bromide gas is a necessary raw material for production. In the prior art, the method for synthesizing hydrogen bromide is to obtain hydrogen bromide by using hydrogen and bromine for combustion reaction through a direct combustion synthesis process.
In the method and the equipment for preparing hydrogen bromide gas in patent CN97117188.2, a hydrogen-bromine synthesizing device is prepared by adopting high-temperature resistant materials such as impregnated graphite, and the device needs to use oxidants such as air to mix with hydrogen for ignition, and then bromine steam replaces the oxidants to carry out hydrogen-bromine combustion, and the method introduces oxidants and hydrogen to be mixed and then has certain safety risk, and the materials of the device are not easy to obtain; because the device is light-tight, the burning condition is difficult to observe.
Patent CN101289167A adopts vertical combustor to synthesize hydrogen bromide method, mixes burning in heating to predetermined temperature vertical combustor with bromine steam and hydrogen according to a certain proportion, prepares hydrobromic acid, and the device needs preheat the combustor outer wall full coverage formula, and heating device is great, and is not easily controlled, and can't observe the burning situation at the combustion process.
In patent cn202110478126.X, a preparation method and a preparation device of hydrobromic acid, hydrogen is used to replace air in a combustion furnace, bromine steam delivery is firstly closed before heating ignition, and bromine steam can be continuously delivered after the heating ignition is completed. The reaction process of the combustion furnace is carried out in a hydrogen environment, the reaction process is not easy to control, and hydrogen needs to be ignited independently, the ignition process is complicated, and potential safety hazards exist.
In the method for synthesizing the low-moisture hydrogen bromide gas in the prior art, the process is complicated, the requirements on process equipment are high, the reaction process is not easy to control, and the purity of the produced bromine is low, so that the production requirements of fine chemical engineering are difficult to meet.
Disclosure of Invention
The invention provides a method for synthesizing low-moisture hydrogen bromide gas, which adopts a simple method to synthesize the hydrogen bromide gas, and has the advantages of simple operation, convenient observation and low operation pressure.
The invention adopts the technical scheme that a method for synthesizing low-moisture hydrogen bromide gas is characterized by comprising the following steps: the method comprises the following steps:
1) Introducing bromine into a bromine electric heater, and gasifying the bromine by the bromine electric heater to obtain high-temperature bromine gas;
2) Introducing the high-temperature bromine gas obtained in the step 1) into a synthesis furnace;
3) Introducing hydrogen into the synthetic furnace after the step 2), wherein the hydrogen enters the synthetic furnace from the furnace end of the synthetic furnace; burning hydrogen in high-temperature bromine gas and synthesizing a hydrogen bromide gas semi-finished product;
4) Introducing the hydrogen bromide gas semi-finished product obtained in the step 3) into a buffer tank;
5) Removing impurities from the hydrogen bromide gas semi-finished product obtained in the step 3) to obtain a hydrogen bromide gas finished product.
Optimally, in the method for synthesizing the low-moisture hydrogen bromide gas, in the step 1), before the bromine is introduced into the electric heater, the bromine is introduced into a drying tower containing sulfuric acid through a metering pump, and the bromine is dried; bromine is preheated using a steam preheater before entering the bromine electric heater.
Preferably, in the method for synthesizing the low-moisture hydrogen bromide gas, in the step 1), bromine is dried before being preheated, so that the moisture of the bromine is reduced to below 20 ppm; in the process of preheating bromine, firstly introducing steam into a steam preheater to finish the self-preheating process of the steam preheater, wherein the temperature of the introduced steam is 140-150 ℃ and the pressure is 0.4-0.5 Mpa; after the steam preheater is self-preheated, introducing bromine into the steam preheater to preheat the bromine, wherein the steam pressure is kept unchanged in the bromine preheating process; when bromine is preheated, the bromine enters the steam preheater in a liquid state.
Preferably, in the method for synthesizing the low-moisture hydrogen bromide gas, in the step 1), when the temperature of a bromine electric heater is increased to be more than or equal to 500 ℃, bromine can be fed; the bromine electric heater heats bromine to 490-510 ℃; in step 3), the hydrogen is ignited by the high-temperature bromine gas and continuously combusted.
Preferably, in the method for synthesizing the low-moisture hydrogen bromide gas, in the step 3), the concentration of the hydrogen gas introduced into the synthesis furnace is 99.9%, and the speed of introducing the hydrogen gas into the synthesis furnace is 16m 3 The pressure in the synthetic furnace is kept between 0.02 and 0.035MPa.
Preferably, in the synthesis process of step 3), the weight ratio of hydrogen to bromine consumed by the method for synthesizing the low-moisture hydrogen bromide gas is 1:72.
preferably, in the method for synthesizing the low-moisture hydrogen bromide gas, in the step 5), the process of removing impurities from the semi-finished hydrogen bromide gas comprises the following steps: and adding red phosphorus into the sealed steel-lined tetrafluoro tower, introducing the hydrogen bromide gas semi-finished product into the sealed steel-lined tetrafluoro tower, and mixing the hydrogen bromide gas semi-finished product with the red phosphorus for reaction.
The application has the advantages that:
according to the technical scheme, bromine gas is introduced into the synthesis furnace firstly and then hydrogen is introduced into the synthesis furnace, so that the hydrogen is combusted in the bromine gas, and compared with the prior art, the combustion reaction process is easy to control, and the operation pressure during reaction is reduced.
In the prior art, hydrogen is combusted in high-temperature bromine gas to synthesize hydrogen bromide gas, but the entering bromine gas cannot immediately cause the combustion of the hydrogen, so that the hydrogen and the bromine gas form mixed gas in a hydrogen explosion range, hydrogen flash explosion is easily caused, and the pressure shock in a furnace easily causes the cracking of a synthesis furnace. Use the mode of hydrogen burning in bromine gas environment in this application, hydrogen lets in slowly, can avoid the furnace body to deposit a large amount of hydrogen in, reduces the risk that hydrogen flickers and explodes for the synthetic process is stable easy control more.
The synthetic furnace can adopt a quartz glass synthetic furnace, and the reaction condition in the furnace body can be visually checked through a transparent furnace body. And a field monitoring system can be arranged at the side of the synthesis furnace, and the reaction condition can be remotely checked through monitoring so as to control the reaction condition in time.
Among the technical scheme of this application, use the bromine that the electrical heating has preheated to about 500 ℃, when hydrogen meets high temperature bromine gas, the ignition burning of hydrogen can be accomplished to the high temperature that uses bromine gas, need not solitary ignition facility and need not ignite the operation, and the synthetic process is simple and the operation degree of difficulty is low to potential safety hazard when having avoided the ignition operation. The bromine is preheated, so that the reaction process is more stable, and if the bromine is not preheated, the combustion flame is unstable during gas synthesis, so that the synthesis reaction is greatly influenced.
Among the technical scheme of this application, contain a certain amount of bromine simple substance in the hydrogen bromide semi-manufactured goods of using the scheme production of this application, the existence of bromine simple substance can influence the purity of hydrogen bromide, for improving product quality, increases in this application and carries out the step of edulcoration to hydrogen bromide gas. The impurity removal process is simple, only need use red phosphorus to fill in airtight steel lining tetrafluoro tower can, hydrogen bromide gas semi-manufactured goods mix reaction with red phosphorus in airtight steel lining tetrafluoro tower, can get rid of bromine simple substance, improve the purity of hydrogen bromide.
In the technical scheme of this application, the equipment of whole synthetic process usefulness mainly is bromine preheater, bromine electric heater, hydrogen bromide synthetic furnace, gas buffer tank closes airtight steel lining tetrafluoro tower, and for prior art, the synthetic method application apparatus of this application is few, and synthetic step is simple, and the purity of the hydrogen bromide gas of production is high, compares and has better economic benefits.
According to the technical scheme, bromine is dried in the drying tower containing sulfuric acid before being preheated, so that bromine moisture is reduced, moisture contained in the hydrogen bromide gas is reduced, and the quality of the final hydrogen bromide gas is improved.
Drawings
FIG. 1 is a flow diagram of a hydrogen bromide gas synthesis process in the present application.
Detailed Description
The technical features of the present invention will be further explained with reference to the accompanying drawings and specific embodiments.
Example 1:
as shown in the figure, the invention is a method for synthesizing low-moisture hydrogen bromide gas, which is characterized by comprising the following steps: the method comprises the following steps:
1) Introducing bromine into a bromine electric heater, and gasifying the bromine by the bromine electric heater to obtain high-temperature bromine gas; when the temperature of the bromine electric heater is raised to 500 ℃, bromine can be fed; heating bromine to 500 ℃ by a bromine electric heater;
2) Introducing the high-temperature bromine gas obtained in the step 1) into a synthesis furnace;
3) Introducing hydrogen into the synthetic furnace after the step 2), wherein the hydrogen enters the synthetic furnace from the furnace end of the synthetic furnace; the hydrogen is ignited by the high-temperature bromine gas and continuously combusted in the high-temperature bromine gas, and the hydrogen is combusted in the high-temperature bromine gas to synthesize a hydrogen bromide gas semi-finished product; the concentration of hydrogen gas fed into the synthesis furnace was 99.9%, and the velocity of hydrogen gas fed into the synthesis furnace was 16m 3 The pressure in the synthesis furnace was kept at 0.025MPa.
4) Introducing the hydrogen bromide gas semi-finished product obtained in the step 3) into a buffer tank;
5) Removing impurities from the hydrogen bromide gas semi-finished product obtained in the step 3) to obtain a hydrogen bromide gas finished product. The impurity removal process of the hydrogen bromide gas semi-finished product comprises the following steps: and adding red phosphorus into the sealed steel-lined tetrafluoro tower, introducing the hydrogen bromide gas semi-finished product into the sealed steel-lined tetrafluoro tower, and mixing the hydrogen bromide gas semi-finished product with the red phosphorus for reaction.
In the step 1), before bromine is introduced into an electric heater, introducing the bromine into a drying tower containing sulfuric acid through a metering pump, and drying the bromine. And the bromine enters a drying tower containing sulfuric acid for drying, so that the moisture of the bromine is reduced, and the moisture contained in the hydrogen bromide gas is reduced.
In the step 1), drying is carried out before preheating the bromine, and then the moisture of the bromine is reduced to 19.5ppm.
Bromine is preheated using a steam preheater before entering the bromine electric heater. In the process of preheating bromine, firstly introducing steam into a steam preheater to finish the self-preheating process of the steam preheater, wherein the temperature of the introduced steam is 145 ℃, and the pressure is 0.45Mpa; after the steam preheater is self-preheated, introducing bromine into the steam preheater to preheat the bromine, wherein the steam pressure is kept unchanged in the bromine preheating process; when bromine is preheated, bromine enters the steam preheater in a liquid state.
In the synthesis process of the step 3), the weight ratio of hydrogen to bromine is 1:72.
the reaction data in the embodiment is the optimal reaction data of the application, the production of the hydrogen bromide finished product is carried out under the condition, the lower production loss and production energy consumption can be ensured under the condition of ensuring the quality of the hydrogen bromide finished product, and the comprehensive economic benefit is higher than that of other embodiments.
Example 2
This example differs from example 1 in that: in the step 1), drying is carried out before preheating the bromine, and then the moisture of the bromine is reduced to 18.5ppm.
In the step 1), feeding bromine when the temperature of a bromine electric heater is raised to 505 ℃; heating bromine to 490 ℃ by a bromine electric heater; in the step 3), the pressure in the synthetic furnace is kept between 0.02 MPa.
Bromine is preheated using a steam preheater before entering the bromine electric heater. In the process of preheating bromine, when steam is introduced into a steam preheater for self-preheating, the temperature of the introduced steam is 140 ℃ and the pressure is 0.4Mpa; after the steam preheater is self-preheated, introducing bromine into the steam preheater to preheat the bromine, wherein the steam pressure is kept unchanged in the bromine preheating process; when bromine is preheated, bromine enters the steam preheater in a liquid state.
Example 3
This example differs from examples 1 and 2 in that: in the step 1), drying is carried out before preheating the bromine, and then the moisture of the bromine is reduced to 17ppm.
In the step 1), feeding bromine when the temperature of a bromine electric heater is raised to 510 ℃; heating bromine to 510 ℃ by a bromine electric heater; the pressure in the synthesis furnace in the step 3) is kept at 0.035Mpa.
When steam is introduced into the steam preheater for self-preheating, the temperature of the introduced steam is 150 ℃ and the pressure is 0.5Mpa; after the steam preheater is self-preheated, introducing bromine into the steam preheater to preheat the bromine, wherein the steam pressure is kept unchanged in the bromine preheating process; when bromine is preheated, the bromine enters the steam preheater in a liquid state.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
Claims (6)
1. A method for synthesizing low-moisture hydrogen bromide gas is characterized in that: the method comprises the following steps:
1) Introducing bromine into a bromine electric heater, and gasifying the bromine by the bromine electric heater to obtain high-temperature bromine gas;
2) Introducing the high-temperature bromine gas obtained in the step 1) into a synthesis furnace;
3) Introducing hydrogen into the synthetic furnace after the step 2), wherein the hydrogen enters the synthetic furnace from the furnace end of the synthetic furnace; burning hydrogen in high-temperature bromine gas and synthesizing a hydrogen bromide gas semi-finished product;
4) Introducing the hydrogen bromide gas semi-finished product obtained in the step 3) into a buffer tank;
5) Removing impurities from the hydrogen bromide gas semi-finished product obtained in the step 3) to obtain a hydrogen bromide gas finished product;
in the step 1), feeding bromine when the temperature of the bromine electric heater is increased to be more than or equal to 500 ℃; bromine is heated to 490-510 ℃ by a bromine electric heater; in step 3), the hydrogen is ignited by the high-temperature bromine gas and continuously combusted.
2. The method of synthesizing low moisture hydrogen bromide gas according to claim 1, wherein: in the step 1), before bromine is introduced into an electric heater, introducing the bromine into a drying tower containing sulfuric acid through a metering pump, and drying the bromine; bromine is preheated using a steam preheater before entering the bromine electric heater.
3. The method of synthesizing low moisture hydrogen bromide gas as claimed in claim 2, wherein: in the step 1), drying bromine before preheating to reduce the moisture of the bromine to below 20 ppm; in the process of preheating bromine, firstly introducing steam into a steam preheater to finish the self-preheating process of the steam preheater, wherein the temperature of the introduced steam is 140-150 ℃ and the pressure is 0.4-0.5 Mpa; after the steam preheater is self-preheated, introducing bromine into the steam preheater to preheat the bromine, wherein the steam pressure is kept unchanged in the bromine preheating process; when bromine is preheated, the bromine enters the steam preheater in a liquid state.
4. The method of synthesizing low moisture hydrogen bromide gas according to claim 1, wherein: in step 3), the concentration of hydrogen gas fed into the synthesis furnace was 99.9%, and the velocity of hydrogen gas fed into the synthesis furnace was 16m 3 The pressure in the synthetic furnace is kept between 0.02 and 0.035MPa.
5. The method of synthesizing low moisture hydrogen bromide gas according to claim 1, wherein: in the synthesis process of the step 3), the weight ratio of hydrogen to bromine is 1:72.
6. the method of synthesizing low moisture hydrogen bromide gas according to claim 1, wherein: in the step 5), the impurity removal process of the hydrogen bromide gas semi-finished product comprises the following steps: and (3) adding red phosphorus into the sealed steel-lined tetrafluoro tower, introducing the hydrogen bromide gas semi-finished product into the sealed steel-lined tetrafluoro tower, and mixing the hydrogen bromide gas semi-finished product with the red phosphorus for reaction.
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| US6425265B1 (en) * | 2001-09-26 | 2002-07-30 | Praxair Technology, Inc. | Process and apparatus for purifying hydrogen bromide |
| KR100978806B1 (en) * | 2008-07-11 | 2010-08-30 | (주)이노메이트 | Manufacturing apparatus and method for high purity hydrogen bromide |
| CN201325873Y (en) * | 2008-12-18 | 2009-10-14 | 山东默锐化学有限公司 | Hydrogen bromide easy preparation device |
| CN102001627B (en) * | 2010-11-18 | 2012-05-02 | 中国地质大学（武汉） | Preparation method of bromine hydride gas and generating device thereof |
| US9835325B2 (en) * | 2012-04-26 | 2017-12-05 | Showa Denko K.K. | Evaporative gas generating device, method for producing evaporative gas, hydrogen bromide production device, and method for producing hydrogen bromide |
| CN205258000U (en) * | 2015-12-07 | 2016-05-25 | 潍坊玉成化工有限公司 | Can high -efficient device of preparing hydrogen bromide solution |
| CN212942228U (en) * | 2020-04-10 | 2021-04-13 | 潍坊欣泽希化工有限公司 | Hydrogen bromide gas purifying tower |
| CN112938900B (en) * | 2021-04-30 | 2023-02-17 | 山东新和成维生素有限公司 | Preparation method and preparation device of hydrobromic acid |
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