CN101973535A - Technology for preparing high-purity nitrogen trifluoride by purifying nitrogen trifluoride prepared by molten-salt growth method by using rectification and absorption method - Google Patents
Technology for preparing high-purity nitrogen trifluoride by purifying nitrogen trifluoride prepared by molten-salt growth method by using rectification and absorption method Download PDFInfo
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- CN101973535A CN101973535A CN 201010265741 CN201010265741A CN101973535A CN 101973535 A CN101973535 A CN 101973535A CN 201010265741 CN201010265741 CN 201010265741 CN 201010265741 A CN201010265741 A CN 201010265741A CN 101973535 A CN101973535 A CN 101973535A
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Abstract
The invention discloses technology for preparing high-purity nitrogen trifluoride by purifying nitrogen trifluoride prepared by a molten-salt growth method by using a rectification and absorption method. In the technology, a molten-salt electrolytic tank, a defroster, a potassium hydroxide absorber, a left condenser, a molecular sieve drier, a right condenser, a filling pump and a connecting valve are mainly involved, and are assembled into a whole by a connecting pipeline according to system functions thereof. The technology is rational in design and convenient to use, and is ideal nitrogen trifluoride preparation process technology.
Description
Affiliated technical field
The present invention relates to the Technology of a kind of Chemicals-nitrogen trifluoride preparation, particularly a kind of nitrogen trifluoride with the molten-salt growth method preparation is purified with rectifying and adsorption method and is prepared the technology of high-purity nitrogen trifluoride, is suitable for the synthetic high-purity nitrogen trifluoride of chemical industry.
Background technology
At present, it is that the nitrogen trifluoride (NF3) that will comprise tetrafluoro-methane (CF4) impurity infiltrates in zeolite 3A, 4A or the 5A bed that extracting rectifying separation nitrogen trifluoride and tetrafluoro-methane prepare nitrogen trifluoride, nitrogen trifluoride optionally is adsorbed onto on the described bed, then with nitrogen trifluoride desorption from the bed, wherein said zeolite and alkaline-earth metal ions exchanged and at 150-600 ℃ time heat treated 0.5-100 hour.This method can not be comprehensive comprehensively removal impurity, time time spent is very long, it is a difficult problem in the nitrogen trifluoride purification techniques that carbon tetrafluoride foreign matter in the nitrogen trifluoride is removed, and still explores in continuous research so far.Very little (the tetrafluoro-methane molecular diameter is 4.8A because tetrafluoro-methane and nitrogen trifluoride molecular diameter differ, the nitrogen trifluoride molecular diameter is 4.5A), and tetrafluoro-methane is a non-polar molecule, thus utilize the sorbent material selective adsorption to separate tetrafluoro-methane and nitrogen trifluoride very difficult.In addition, the nitrogen trifluoride boiling point is-129 ℃, and the tetrafluoro-methane boiling point is-128 ℃, and both differ only 1 ℃, utilizes rectificating method to separate also very difficulty.
Summary of the invention
Problem to be solved by this invention is, overcomes the deficiencies in the prior art, provides a kind of nitrogen trifluoride with the molten-salt growth method preparation to purify with rectifying and adsorption method and has prepared the technology of high-purity nitrogen trifluoride.This technology not only technology is reasonable, and preparation is simple, and good product quality, and the purity of the gas of nitrogen trifluoride of production is brought up to more than 99.99% by initial about 97%, and has solved problem of environmental pollution.
The technical solution used in the present invention is: fused-salt bath, mist eliminator, potassium hydroxide resorber, left condenser, mole sieve drier, right condenser, filling pump, connection valve are assembled into one by connection line by its system function and constitute.
Mainly contain impurity such as nitrogen, oxygen, carbon monoxide, carbonic acid gas, Nitrous Oxide, difluoro hydrazine, tetrafluorohydrazine, tetrafluoro-methane, sulfur hexafluoride, silicon tetrafluoride, fluorine gas, hydrogen fluoride, water in the thick nitrogen trifluoride of the resulting anodic gas of fused salt electrolysis.In order to remove these impurity, the nitrogen trifluoride that no matter adopts which kind of synthetic method to obtain, wherein dopant species and content are similar.In order to obtain pure nitrogen trifluoride, each purification unit operation must be combined and could realize.Implementing the technology of the present invention process is:
The gas mixture that fused-salt bath produces is at first removed the entrained solid particle by a mist eliminator, secondly remove acidic impurities through the potassium hydroxide solution absorption of potassium hydroxide resorber, remove most of moisture by left condenser, right condenser again, remove micro-moisture by mole sieve drier subsequently, last condensation liquefaction nitrogen trifluoride, take out non-condensable gas, pure nitrogen trifluoride compression fills through filling pump.This flow process is because the nitrogen trifluoride synthetic technology is a molten-salt growth method, and fluorine gas has carried out in advance purifying and removed three fluorocarbonss, thereby obtains high purity product easily.
The invention has the beneficial effects as follows, reasonable in design, easy to use, be the high-purity nitrogen trifluoride fabricating technology of ideal.
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, fused-salt bath, 2, mist eliminator, 3, the potassium hydroxide resorber, 4, left condenser, 5, mole sieve drier, 6, right condenser, 7, filling pump, 8, connection line, 9, connect valve.
Embodiment
With reference to Fig. 1, fused-salt bath 1, mist eliminator 2, potassium hydroxide resorber 3, left condenser 4, mole sieve drier 5, right condenser 6, filling pump 7, connection valve 9 are assembled into one by connection line 8 by its system function and constitute.
Mainly contain impurity such as nitrogen, oxygen, carbon monoxide, carbonic acid gas, Nitrous Oxide, difluoro hydrazine, tetrafluorohydrazine, tetrafluoro-methane, sulfur hexafluoride, silicon tetrafluoride, fluorine gas, hydrogen fluoride, water in the thick nitrogen trifluoride of the resulting anodic gas of fused salt electrolysis.In order to remove these impurity, the nitrogen trifluoride that no matter adopts which kind of synthetic method to obtain, wherein dopant species and content are similar.In order to obtain pure nitrogen trifluoride, each purification unit operation must be combined and could realize.Implementing the technology of the present invention process is:
The gas mixture that fused-salt bath 1 produces is at first removed the entrained solid particle by a mist eliminator 2, secondly remove acidic impurities through the potassium hydroxide solution absorption of potassium hydroxide resorber 3, remove most of moisture by left condenser 4, right condenser 6 again, remove micro-moisture by mole sieve drier 5 subsequently, last condensation liquefaction nitrogen trifluoride, take out non-condensable gas, pure nitrogen trifluoride compression fills through filling pump 7.This flow process is because the nitrogen trifluoride synthetic technology is a molten-salt growth method, and fluorine gas has carried out in advance purifying and removed three fluorocarbonss, thereby obtains high purity product easily.
Not only technology is reasonable for this invention technology, and preparation is simple, and good product quality, and the purity of the gas of nitrogen trifluoride of production is brought up to more than 99.99% by initial about 97%, and has solved problem of environmental pollution.
Claims (1)
1. the nitrogen trifluoride with the molten-salt growth method preparation is purified with rectifying and adsorption method and is prepared the technology of high-purity nitrogen trifluoride, and it is characterized in that: fused-salt bath, mist eliminator, potassium hydroxide resorber, left condenser, mole sieve drier, right condenser, filling pump, connection valve are assembled into one by connection line by its system function and constitute.
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| CN 201010265741 CN101973535A (en) | 2010-08-30 | 2010-08-30 | Technology for preparing high-purity nitrogen trifluoride by purifying nitrogen trifluoride prepared by molten-salt growth method by using rectification and absorption method |
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| CN 201010265741 CN101973535A (en) | 2010-08-30 | 2010-08-30 | Technology for preparing high-purity nitrogen trifluoride by purifying nitrogen trifluoride prepared by molten-salt growth method by using rectification and absorption method |
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| CN101973535A true CN101973535A (en) | 2011-02-16 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450202A (en) * | 2003-04-30 | 2003-10-22 | 中国船舶重工集团公司第七一八研究所 | Technological method and equipment for preparing nitrogen trifluoride gas |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450202A (en) * | 2003-04-30 | 2003-10-22 | 中国船舶重工集团公司第七一八研究所 | Technological method and equipment for preparing nitrogen trifluoride gas |
Non-Patent Citations (2)
| Title |
|---|
| 《化学推进剂与高分子材料》 20021226 胡长诚 国外三氟化氮制备技术研究开发进展 1-6，9 1 , 第6期 2 * |
| 《现代化工》 20040430 宋海华等 三氟化氮纯化的新工艺 51-53 1 第24卷, 第4期 2 * |
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Open date: 20110216 |