CN101913579A - Technology for preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorin and ammonia - Google Patents
Technology for preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorin and ammonia Download PDFInfo
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- CN101913579A CN101913579A CN 201010265714 CN201010265714A CN101913579A CN 101913579 A CN101913579 A CN 101913579A CN 201010265714 CN201010265714 CN 201010265714 CN 201010265714 A CN201010265714 A CN 201010265714A CN 101913579 A CN101913579 A CN 101913579A
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Abstract
The invention discloses technology for preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorin and ammonia. The system mainly comprises a reactor provided with a reactor heating device, a defogger provided with a defogger heating device, a catcher, a scrubber, a cold trap, a left adsorption column, a right adsorption column, a condenser, a vacuum pump and a connecting valve, which are integrated through connecting pipelines according to system functions thereof. The design is reasonable and the use is convenient, so the technology is ideal technology for preparing nitrogen trifluoride.
Description
Affiliated technical field
The present invention relates to the Technology of a kind of Chemicals-nitrogen trifluoride preparation, the technology of the preparing nitrogen trifluoride by directly fluoridizing gaseous phases of particularly a kind of fluorine and ammonia is suitable for the synthetic nitrogen trifluoride of chemical industry.
Background technology
At present, the method for making nitrogen trifluoride is that fluorine-containing feedstream and ammonium bifluoride liquid are contacted for some time in reaction zone under the condition that is enough to produce nitrogen trifluoride.In contact procedure, reduce the melt acidity value of ammonium bifluoride liquid, discharge reacting product stream.Element fluorine contacts with this body fluid of ammonium bifluoride with hydrogen fluoride mixture, makes initial melt acidity value in the reaction zone greater than the melt acidity value of this body fluid of ammonium bifluoride.The inapplicable continuous production of this method, and output capacity is relatively low.
Summary of the invention
Problem to be solved by this invention is, overcomes the deficiencies in the prior art, and the technology of the preparing nitrogen trifluoride by directly fluoridizing gaseous phases of a kind of fluorine and ammonia is provided.This technology not only technology is reasonable, and preparation is simple, and good product quality, and the nitrogen trifluoride massfraction of production is more than 95%, and has solved problem of environmental pollution.
The technical solution used in the present invention is: the reactor of reactor heating unit, the mist eliminator that the mist eliminator heating unit is installed, trap, washer, cold-trap, left adsorption column, right adsorption column, condenser, vacuum pump, connection valve are installed are assembled into one by connection line by its system function and constitute.
Chemical reaction production principle of the present invention:
Ammonia and fluorine gas enter reactor according to certain ratio, the generation nitrogen trifluoride that under certain temperature, pressure condition, reacts, and reaction equation is as follows:
NH
3+3F
2→NF
3+3HF
Technical process and main technologic parameters
The technological process of production that adopts fluorine gas and ammonia directly to carry out the synthetic nitrogen trifluoride of gas phase phase reaction is: earlier ammonium bifluoride is added in the nickel system reactor, be heated to 135 ℃ by the reactor heating unit, make its fusing, fluorine gas and the ammonia sparger in being dipped in melts is sent into reactor (fluorine gas by nitrogen dilution to volume fraction about 50%), ammonia sparger like another kind of is sent into reactor, and the ammonia amount of sending into keeps by product HF and NH in the melts
3The ratio of amount of substance be about 2.3: 1, reactor pressure is about 0.04MPa.Reaction product enters recovery system through mist eliminator, and mist eliminator is heated to more than 127 ℃ by the mist eliminator heating unit, removing the melts of carrying secretly in the gas, and makes Neutral ammonium fluoride and hydrogen fluoride reaction Generation Liquid phase fluorination hydrogen ammonium, returns in the reactor.After this reactant enters the washer that potassium hydroxide is housed through trap, remove hydrogen fluoride wherein, enter then in the cold-trap that internal temperature is about 5 ℃, thereby the part moisture in the removal air-flow, remove remaining water through left adsorption column, right adsorption column again, then gas is chilled to liquid nitrogen temperature in condenser, make almost all condensations of nitrogen trifluoride, take out remaining nitrogen with vacuum pump again, obtain massfraction at last and be the nitrogen trifluoride product more than 95%.
The invention has the beneficial effects as follows, reasonable in design, easy to use, be ideal nitrogen trifluoride fabricating technology.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is a structural representation of the present invention.
Accompanying drawing number is: 1 reactor, 2, the reactor heating unit, 3, mist eliminator, 4, the mist eliminator heating unit, 5, trap, 6, washer, 7, cold-trap, 8, left adsorption column, 9, right adsorption column, 10, condenser, 11, vacuum pump, 12, connection line, 13, connect valve, 14, add inlet.
Embodiment
With reference to Fig. 1, the reactor 1 of reactor heating unit 2, the mist eliminator 3 that mist eliminator heating unit 4 is installed, trap 5, washer 6, cold-trap 7, left adsorption column 8, right adsorption column 9, condenser 10, vacuum pump 11 are installed, connect valve 13 and be assembled into one by connection line 12 by its system function and constitute.
Chemical reaction production principle of the present invention:
Ammonia and fluorine gas enter reactor according to certain ratio, the generation nitrogen trifluoride that under certain temperature, pressure condition, reacts, and reaction equation is as follows:
NH
3+3F
2→NF
3+3HF
Technical process and main technologic parameters
The technological process of production that adopts fluorine gas and ammonia directly to carry out the synthetic nitrogen trifluoride of gas phase phase reaction is: earlier ammonium bifluoride is added in the nickel system reactor 1, be heated to 135 ℃ by reactor heating unit 2, make its fusing, fluorine gas and the ammonia sparger in being dipped in melts is sent into reactor 1 (fluorine gas by nitrogen dilution to volume fraction about 50%), ammonia sparger like another kind of is sent into reactor 1, and the ammonia amount of sending into keeps by product HF and NH in the melts
3The ratio of amount of substance be about 2.3: 1, reactor pressure is about 0.04MPa.Reaction product enters recovery system through mist eliminator 3, and mist eliminator 3 is heated to more than 127 ℃ by mist eliminator heating unit 4, removing the melts of carrying secretly in the gas, and makes Neutral ammonium fluoride and hydrogen fluoride reaction Generation Liquid phase fluorination hydrogen ammonium, returns in the reactor 1.After this reactant enters the washer 6 that potassium hydroxide is housed through trap 5, remove hydrogen fluoride wherein, enter then in the cold-trap 7 that internal temperature is about 5 ℃, thereby the part moisture in the removal air-flow, remove remaining water through left adsorption column 8, right adsorption column 9 again, then gas is chilled to liquid nitrogen temperature in condenser 10, make almost all condensations of nitrogen trifluoride, take out remaining nitrogen with vacuum pump 11 again, obtain massfraction at last and be the nitrogen trifluoride product more than 95%.
Manipulating the present invention, to produce the process of nitrogen trifluoride as follows: the fluorine gas reaction mixture enters reactor 1 reacting by heating that reactor heating unit 2 is installed by adding inlet 14, after entering the mist eliminator 3 heating demists that mist eliminator heating unit 4 is installed through connection line 12, enter trap 5, washer 6, cold-trap 7, left adsorption column 8, right adsorption column 9, condenser 10 through connection line 12 again and finish generative process, take out remaining nitrogen with vacuum pump 11 again, obtain massfraction at last and be the nitrogen trifluoride product more than 95%.Not only technology is reasonable for this invention technology, and preparation is simple, and good product quality, and the nitrogen trifluoride massfraction of production is more than 95%, and has solved problem of environmental pollution.
Claims (1)
1. the technology of the preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorine and ammonia is characterized in that: the reactor of reactor heating unit, the mist eliminator that the mist eliminator heating unit is installed, trap, washer, cold-trap, left adsorption column, right adsorption column, condenser, vacuum pump, connection valve are installed are assembled into one by connection line by its system function and constitute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010265714 CN101913579A (en) | 2010-08-30 | 2010-08-30 | Technology for preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorin and ammonia |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010265714 CN101913579A (en) | 2010-08-30 | 2010-08-30 | Technology for preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorin and ammonia |
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|---|---|
| CN101913579A true CN101913579A (en) | 2010-12-15 |
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| CN 201010265714 Pending CN101913579A (en) | 2010-08-30 | 2010-08-30 | Technology for preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorin and ammonia |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110523351A (en) * | 2019-09-18 | 2019-12-03 | 苏州金宏气体股份有限公司 | A kind of synthesizer and synthetic method of hydrogen bromide |
| CN114572944A (en) * | 2021-12-23 | 2022-06-03 | 西安近代化学研究所 | Preparation method of nitrogen trifluoride and nitrogen trifluoride mixed gas |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4091081A (en) * | 1977-04-19 | 1978-05-23 | Air Products And Chemicals, Inc. | Preparation of nitrogen trifluoride |
| CN1727278A (en) * | 2005-07-27 | 2006-02-01 | 中国船舶重工集团公司第七一八研究所 | Equipment and technological process for preparing nitrogen trifluoride by using ammonia and hydrogen fluoride as raw material |
-
2010
- 2010-08-30 CN CN 201010265714 patent/CN101913579A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4091081A (en) * | 1977-04-19 | 1978-05-23 | Air Products And Chemicals, Inc. | Preparation of nitrogen trifluoride |
| CN1727278A (en) * | 2005-07-27 | 2006-02-01 | 中国船舶重工集团公司第七一八研究所 | Equipment and technological process for preparing nitrogen trifluoride by using ammonia and hydrogen fluoride as raw material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110523351A (en) * | 2019-09-18 | 2019-12-03 | 苏州金宏气体股份有限公司 | A kind of synthesizer and synthetic method of hydrogen bromide |
| CN114572944A (en) * | 2021-12-23 | 2022-06-03 | 西安近代化学研究所 | Preparation method of nitrogen trifluoride and nitrogen trifluoride mixed gas |
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Open date: 20101215 |