CN102745649A - Bromine removing method for hydrogen bromide gas - Google Patents
Bromine removing method for hydrogen bromide gas Download PDFInfo
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- CN102745649A CN102745649A CN2012102758908A CN201210275890A CN102745649A CN 102745649 A CN102745649 A CN 102745649A CN 2012102758908 A CN2012102758908 A CN 2012102758908A CN 201210275890 A CN201210275890 A CN 201210275890A CN 102745649 A CN102745649 A CN 102745649A
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Abstract
The invention discloses a bromine removing method for a hydrogen bromide gas. The method includes the following steps of placing a bromine removing agent in a bromine removing reactor, heating to enable the internal temperature of the bromine removing reactor to reach to 100 DEG C to 115 DEG C, then enabling the hydrogen bromide gas to flow through the bromine removing reactor to subject bromine in the hydrogen bromide gas to reacting with the bromine removing agent under the temperature conditions from 100 DEG C to 115 DEG C, and enabling the mass content of free bromine in the hydrogen bromide gas flowing out of the bromine removing reactor to be maintained below a target value. The bromine removing method for the hydrogen bromide gas has the advantages that the equipment investment is small, the operation control is simple, the bromine removing efficiency is high, the industrial automation production control is easy, the industrial continuous production can be achieved, the qualities of processed hydrogen bromide gas products are high, and the purity can reach to above 99.8%.
Description
Technical field
The present invention relates to a kind of bromine method of removing of bromize hydrogen gas.
Background technology
Bromize hydrogen gas is a kind of in the halogen gas.That outward appearance shows as is colourless, pungent pungent odour is arranged, molecular weight 80.91, and fusing point-88.5 ℃, boiling point-66.8 ℃, specific density (air=1) 3.5 (0 ℃), the concentration of high-purity bromize hydrogen gas can reach more than 99.99%.Bromize hydrogen gas is soluble in water, ethanol, Glacial acetic acid min. 99.5 etc.Bromize hydrogen gas has extensive use in industry, can be used as raw material organic and that inorganic bromide is made, also can be used for making catalyst and medicine, also can be used for the etching processing of electronic circuit board etc.
Because the deep-etching effect of bromize hydrogen gas is unfavorable for large-scale industrial production, aspect storage, also has certain difficulty, therefore, the bromize hydrogen gas of a large amount of industrial applications generally is to produce use at the scene nearby.But no matter the mode of production of which kind of bromize hydrogen gas is mixed with the not bromine of complete reaction unavoidably in the bromize hydrogen gas, need remove processing to the bromine in the bromize hydrogen gas, to satisfy the industrial requirements of bromize hydrogen gas.
Summary of the invention
The purpose of this invention is to provide a kind of serialization, low cost, pollution-free, the method that can effectively remove free bromine in the bromize hydrogen gas.
The present invention adopts the treatment process that comprises following steps to reach the object of the invention: will pack into except that in the bromine reaction device except that bromide, heating makes the internal temperature except that the bromine reaction device reach 100-115 ℃; Let then bromize hydrogen gas flow through except that the bromine reaction device bromizate bromine in the hydrogen under the said temperature condition with remove bromide and react so that from remove the bromine reaction device in the effusive bromize hydrogen gas mass content of free bromine below target value; The said bromide that removes is iron powder, aluminium powder, abrasive grit, aluminum shot, iron wire, aluminium wire or its mixture.
The Intake Quantity that removes bromide is 50-80 : 1 with the mass ratio of flowing through except that the bromize hydrogen gas of bromine reaction device; The flow velocity that bromize hydrogen gas is flowed through except that the bromine reaction device is 10-20L/min.
This method comprises that also feeding nitrogen is to discharge except that the air in the bromine reaction device and the step of water vapor in removing the bromine reaction device; After the internal temperature that promptly removes the bromine reaction device reaches 100-115 ℃; Remove the bromine reaction device with the nitrogen gas stream warp so that the air and the water vapor that remove in the bromine reaction device are discharged earlier, and then the feeding bromize hydrogen gas removes bromine.Nitrogen gas stream can be controlled in 10-30 minute through the time of removing the bromine reaction device, can reach the purpose of exhausted air and water vapour.
The mass content of free bromine is low more good more in the bromize hydrogen gas; But many factors such as comprehensive treating process cost and efficient; It is suitable that the target value of the mass content of free bromine in the bromize hydrogen gas is set in 0.1%, as long as the mass content of free bromine just can satisfy request for utilization in target value below 0.1% in the bromize hydrogen gas.The particle diameter that removes iron powder in the bromide, aluminium powder among the present invention is more preferably greater than 70 orders; The particle diameter of abrasive grit, aluminum shot is preferably less than 3mm; The diameter of iron wire, aluminium wire is preferably less than 0.6mm.Removing the bromine reaction device can adopt an end to have any type of encloses container that the inlet mouth the other end has the air outlet; But consider and remove bromine efficient and effect that remove the bromine reaction device and be preferably the pipeline reactor of processing with quartz glass tube or weldless steel tube, an end of pipeline reactor is provided with the inlet mouth the other end and is provided with the air outlet; Bromize hydrogen gas gets into from inlet mouth; Flow out from the air outlet, bromize hydrogen gas is flowed through in the process of reactor drum inner chamber and is removed bromide and react, to reach the purpose except that bromine; It is that 300 millimeters, length are the quartz glass tube of 4000-8000 millimeter that quartz glass tube adopts diameter; It is that 108-219 millimeter, length are the weldless steel tube of 5000-8000 millimeter that weldless steel tube adopts diameter.Remove the mode that bromide can adopt filling in bulk, regular or load in mixture in the filling mode of removing the bromine reaction device.
Effect and benefit that hydrogen bromide provided by the present invention removes the bromine method are: 1. through simple treatment facility and treatment process; Bromine removes in the realization bromize hydrogen gas; Facility investment is little, controls simply, and it is high to remove bromine efficient; Be easy to the industrial automation production control, can realize industrial continuity production.2. the bromize hydrogen gas quality product after handling is high, and purity can reach more than 99.8%, can satisfy the specification of quality of industrial bromize hydrogen gas.
Embodiment
Below further specify the bromine method of removing of bromize hydrogen gas of the present invention through embodiment, these embodiment only are used to the present invention is described and to not restriction of the present invention.
Embodiment 1
To with diameter be 300 millimeters, length be 4000 millimeters quartz glass tube make remove to fill in the bromine reaction device and remove the i.e. 50 kilograms of iron powders of bromide; Heat by the heating tape that is wrapped on the quartz glass tube then, make except that 100 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 10 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 285.7 liters of bromize hydrogen gas by the glass flow rate meter with the 10L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.1% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.881%.
Embodiment 2
To with diameter be 300 millimeters, length be 5000 millimeters quartz glass tube make remove to fill in the bromine reaction device and remove the i.e. 60 kilograms of aluminium powders of bromide; Heat by the heating tape that is wrapped on the quartz glass tube then, make except that 103 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 15 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 300 liters of bromize hydrogen gas by the glass flow rate meter with the 12L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.08% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.913%.
Embodiment 3
To being that 108 millimeters, length are that removing of making of 5000 millimeters seamless steel pipe fills in the bromine reaction device that to remove bromide be that mass ratio is 60 kilograms in the mixture of iron powder and the aluminium powder of 1:1 with diameter; Heat by the heating tape that is wrapped on the seamless steel pipe then, make except that 105 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 18 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 320 liters of bromize hydrogen gas by the glass flow rate meter with the 14L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.09% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.907%.
Embodiment 4
To being that 159 millimeters, length are that removing of making of 6500 millimeters seamless steel pipe fills in the bromine reaction device that to remove bromide be that diameter is 65 kilograms of the abrasive grits of 3mm with diameter; Heat by the heating tape that is wrapped on the seamless steel pipe then, make except that 110 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 23 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 350 liters of bromize hydrogen gas by the glass flow rate meter with the 16L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.03% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.869%.
Embodiment 5
To being that 219 millimeters, length are that removing of making of 8000 millimeters seamless steel pipe fills in the bromine reaction device that to remove bromide be that diameter is 72 kilograms of the aluminum shots of 3mm with diameter; Heat by the heating tape that is wrapped on the seamless steel pipe then, make except that 113 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 25 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 400 liters of bromize hydrogen gas by the glass flow rate meter with the 18L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.1% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.869%.
Embodiment 6
To being that 300 millimeters, length are that removing of making of 7000 millimeters quartz glass tube fills in the bromine reaction device that to remove bromide be that mass ratio is 76 kilograms in the mixture of wire netting and the iron powder of 2:1 with diameter; Heat by the heating tape that is wrapped on the quartz glass tube then, make except that 112 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 28 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 450 liters of bromize hydrogen gas by the glass flow rate meter with the 18L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.09% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.907%.
Embodiment 7
To being that 300 millimeters, length are that removing of making of 8000 millimeters quartz glass tube fills in the bromine reaction device that to remove bromide be that mass ratio is 80 kilograms in the mixture of wire netting and the aluminium net of 1:1 with diameter; Heat by the heating tape that is wrapped on the quartz glass tube then, make except that 115 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 30 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 480 liters of bromize hydrogen gas by the glass flow rate meter with the 20L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.03% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.968%.
Embodiment 8
To being that 300 millimeters, length are that removing of making of 6000 millimeters quartz glass tube fills in the bromine reaction device that to remove bromide be that mass ratio is 70 kilograms in the mixture of wire netting and the aluminium powder of 3:1 with diameter; Heat by the heating tape that is wrapped on the quartz glass tube then, make except that 113 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 28 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 420 liters of bromize hydrogen gas by the glass flow rate meter with the 16L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.06% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.937%.
Embodiment 9
To being that 300 millimeters, length are that removing of making of 8000 millimeters quartz glass tube fills in the bromine reaction device that to remove bromide be that mass ratio is 80 kilograms in the mixture of aluminium net and the aluminium powder of 2:1 with diameter; Heat by the heating tape that is wrapped on the quartz glass tube then, make except that 110 ℃ of the arrival of the temperature in the bromine reaction device; In removing the bromine reaction device, charge into nitrogen then, nitrogen is flowed through except that bromine reaction device 30 minutes, the circulation by nitrogen will remove air in the bromine reaction device and steam discharge; Then use chlorine gas pump, with 480 liters of bromize hydrogen gas by the glass flow rate meter with the 18L/min flow velocity continuously by removing the bromine reaction device, bromize hydrogen gas is flowed through in the process except that bromide, bromine wherein with remove bromide and react and be removed; After testing, the mass content of free bromine is 0.02% in the bromize hydrogen gas that from remove the bromine reaction device, flows out, and the mass content of HBr is 99.988%.
The content of free bromine quantitatively absorbs back employing silver nitrate titration method mensuration through water in the bromize hydrogen gas; The main content of bromize hydrogen gas quantitatively absorbs the back through water and adopts the alkali-titration method to measure.In the foregoing description, the particle diameter of used iron powder, aluminium powder is greater than 70 orders; The particle diameter of abrasive grit, aluminum shot is less than 3mm; The diameter of iron wire, aluminium wire is less than 0.6mm.
Claims (5)
1. the bromine method of removing of a bromize hydrogen gas, it is characterized in that: this method may further comprise the steps:
To pack into except that in the bromine reaction device except that bromide, heating makes the internal temperature except that the bromine reaction device reach 100-115 ℃; Let then bromize hydrogen gas flow through except that the bromine reaction device bromizate bromine in the hydrogen under the said temperature condition with remove bromide and react so that from remove the bromine reaction device in the effusive bromize hydrogen gas mass content of free bromine below target value; The said bromide that removes is iron powder, aluminium powder, abrasive grit, aluminum shot, iron wire, aluminium wire or its mixture.
2. the bromine method of removing of bromize hydrogen gas as claimed in claim 1 is characterized in that: the Intake Quantity that removes bromide is 50-80 : 1 with the mass ratio of flowing through except that the bromize hydrogen gas of bromine reaction device; The flow velocity that bromize hydrogen gas is flowed through except that the bromine reaction device is 10-20L/min.
3. according to claim 1 or claim 2 the bromine method of removing of bromize hydrogen gas; It is characterized in that: this method comprises that also feeding nitrogen is to discharge except that the air in the bromine reaction device and the step of water vapor in removing the bromine reaction device; After the internal temperature that promptly removes the bromine reaction device reaches 100-115 ℃; Remove the bromine reaction device with the nitrogen gas stream warp so that the air and the water vapor that remove in the bromine reaction device are discharged earlier, and then the feeding bromize hydrogen gas removes bromine.
4. the bromine method of removing of bromize hydrogen gas as claimed in claim 1, it is characterized in that: the particle diameter of said iron powder, aluminium powder is greater than 70 orders; The particle diameter of abrasive grit, aluminum shot is less than 3mm; The diameter of iron wire, aluminium wire is less than 0.6mm.
5. the bromine method of removing of bromize hydrogen gas as claimed in claim 1 is characterized in that: the said pipeline reactor of bromine reaction device for processing with quartz glass tube or weldless steel tube that remove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102758908A CN102745649A (en) | 2012-08-06 | 2012-08-06 | Bromine removing method for hydrogen bromide gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102758908A CN102745649A (en) | 2012-08-06 | 2012-08-06 | Bromine removing method for hydrogen bromide gas |
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| CN102745649A true CN102745649A (en) | 2012-10-24 |
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| CN2012102758908A Pending CN102745649A (en) | 2012-08-06 | 2012-08-06 | Bromine removing method for hydrogen bromide gas |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955189A (en) * | 2009-07-13 | 2011-01-26 | 北京有色金属研究总院 | Method and device for preparing high-purity boron tribromide |
| CN102001627A (en) * | 2010-11-18 | 2011-04-06 | 中国地质大学（武汉） | Preparation method of bromine hydride gas and generating device thereof |
| US20120053381A1 (en) * | 2009-05-13 | 2012-03-01 | Wayne Errol Evans | Integrated process to produce c4+ hydrocarbons with removal of brominated organic impurities |
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2012
- 2012-08-06 CN CN2012102758908A patent/CN102745649A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120053381A1 (en) * | 2009-05-13 | 2012-03-01 | Wayne Errol Evans | Integrated process to produce c4+ hydrocarbons with removal of brominated organic impurities |
| CN101955189A (en) * | 2009-07-13 | 2011-01-26 | 北京有色金属研究总院 | Method and device for preparing high-purity boron tribromide |
| CN102001627A (en) * | 2010-11-18 | 2011-04-06 | 中国地质大学（武汉） | Preparation method of bromine hydride gas and generating device thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李迎堂 等: "二溴甲烷产品合成工艺改进研究", 《盐业与化工》 * |
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Application publication date: 20121024 |