CN101942669A - Technique for preparing nitrogen trifluoride by electrolytic melting of ammonium bifluoride - Google Patents
Technique for preparing nitrogen trifluoride by electrolytic melting of ammonium bifluoride Download PDFInfo
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- CN101942669A CN101942669A CN 201010265731 CN201010265731A CN101942669A CN 101942669 A CN101942669 A CN 101942669A CN 201010265731 CN201010265731 CN 201010265731 CN 201010265731 A CN201010265731 A CN 201010265731A CN 101942669 A CN101942669 A CN 101942669A
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- ammonium bifluoride
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Abstract
The invention discloses a technique for preparing nitrogen trifluoride by the electrolytic melting of ammonium bifluoride, which is formed by connecting an electrolytic cell, a buffer tank, a hydrogen fluoride condensing tower, a levooxy sodium fluoride absorption tower, a dextrooxy sodium fluoride absorption tower, a defluorination tower, an alkaline tower, a molecular sieve absorption tower, an active carbon absorption tower, a sodium peroxide absorption tower, a sodium thiosulfate washing tower, a molecular sieve drying tower, a low-temperature rectifying tower, a gas holder, a compressor and a filling platform according a system function sequence by using connecting pipes to assemble a whole body. The technique is reasonable in design and convenient in use, and is an ideal nitrogen trifluoride preparation technique.
Description
Affiliated technical field
The present invention relates to the Technology of a kind of Chemicals-nitrogen trifluoride preparation, particularly a kind of electrolyzing fused ammonium bifluoride prepares the technology of nitrogen trifluoride, is suitable for the synthetic high-purity nitrogen trifluoride of chemical industry.
Background technology
At present, it is that fluorine-containing feedstream and ammonium bifluoride liquid are being enough to produce under the condition of nitrogen trifluoride in reaction zone that the melting salt legal system is equipped with nitrogen trifluoride, contact for some time.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, make initial melt acidity value in the reaction zone greater than the melt acidity value of this body fluid of ammonium bifluoride, technology is immature, and productive rate is low, complicated operation is difficult for the serialization long-time running and produces.
Summary of the invention
Problem to be solved by this invention is, overcomes the deficiencies in the prior art, provides a kind of electrolyzing fused ammonium bifluoride to prepare the technology of 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 reaches more than 98%, and has solved problem of environmental pollution.
The technical solution used in the present invention is: design and installation negative electrode, anodic electrolyzer, surge tank, hydrogen fluoride condensing tower, left Sodium Fluoride adsorption tower, right Sodium Fluoride adsorption tower, defluorinate tower, soda-wash tower, adsorbing tower with molecular sieve, activated carbon adsorber, sodium peroxide adsorption tower, Sulfothiorine washing tower, molecular sieve drying tower, low-temperature fractionating tower, gas holder, compressor in the outer hot-plate casing, fill platform and connect by connection line according to the system function order, be assembled into one and constitute.
Implementing the technology of the present invention workflow is:
Neutral ammonium fluoride and ammonium acid fluoride mol ratio 1: 1.1-1.8 are made into electrolytic solution and inject electrolyzer, the gas that comes out from anode electrolytic cell enters surge tank, hydrogen fluoride condensing tower through connection line, this surge tank plays buffering, balance and regulating effect to the gas that electrolyzer anode chamber in the system produces, to increase the stability of system's anode electrolytic cell room pressure, and, because the flow velocity of gas and temperature reduce in surge tank, therefore, can precipitate lower section solid particulate and dropping liquid at this.The gas that removed solid particulate and drop, is mainly nitrogen trifluoride enters left Sodium Fluoride adsorption tower, right Sodium Fluoride adsorption tower and defluorinate tower again to remove impurity fluorine and Sodium Fluoride, removes acidic impurities in soda-wash tower.After order enters adsorbing tower with molecular sieve, activated carbon adsorber, sodium peroxide adsorption tower, each refining plant of Sulfothiorine washing tower then, enter the molecular sieve drying tower and remove contained humidity, enter low-temperature fractionating tower and remove high-boiling-point impurity.Eject the gas nitrogen trifluoride that comes from low-temperature fractionating tower and be partially condensated as liquid, in gas holder flows back to tower,, after finished product advances the compressed machine compression of gas holder, cooling, charge into gas cylinder filling platform as phegma.
According to the electrolysis and the requirement of improving the quality of products, the anode of installing in the electrolyzer adopts graphite material, and the temperature of melting salt generally is controlled at 120-160 ℃, and optimum temps is controlled at 125-145 ℃, and voltage is at 6-12V.
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, electrolyzer, 2, surge tank, 3, the hydrogen fluoride condensing tower, 4, left Sodium Fluoride adsorption tower, 5, right Sodium Fluoride adsorption tower, 6, the defluorinate tower, 7, soda-wash tower, 8, adsorbing tower with molecular sieve, 9, activated carbon adsorber, 10, the sodium peroxide adsorption tower, 11, the Sulfothiorine washing tower, 12, molecular sieve drying tower, 13, low-temperature fractionating tower, 14, gas holder, 15, compressor, 16, fill platform, 17, connection line, 18, negative electrode, 19, anode, 20, outer hot-plate casing.
Embodiment
With reference to Fig. 1, electrolyzer 1, surge tank 2, hydrogen fluoride condensing tower 3, left Sodium Fluoride adsorption tower 4, right Sodium Fluoride adsorption tower 5, defluorinate tower 6, soda-wash tower 7, adsorbing tower with molecular sieve 8, activated carbon adsorber 9, sodium peroxide adsorption tower 10, Sulfothiorine washing tower 11, molecular sieve drying tower 12, low-temperature fractionating tower 13, gas holder 14, the compressor 15 of design and installation negative electrodes 18, anode 19 in the outer hot-plate casing 20, fill platform 16 and connect by connection line 17, be assembled into one and constitute according to the system function order.
Implementing the technology of the present invention workflow is:
Neutral ammonium fluoride and ammonium acid fluoride mol ratio 1: 1.1-1.8 are made into electrolytic solution and inject electrolyzer 1, the gas that comes out from electrolyzer 1 anode enters surge tank 2, hydrogen fluoride condensing tower 3 through connection line 17, this surge tank plays buffering, balance and regulating effect to the gas that electrolyzer anode chamber in the system produces, to increase the stability of system's anode electrolytic cell room pressure, and, because the flow velocity of gas and temperature reduce in surge tank 2, therefore, can precipitate lower section solid particulate and dropping liquid at this.The gas that removed solid particulate and drop, is mainly nitrogen trifluoride enters left Sodium Fluoride adsorption tower 4, right Sodium Fluoride adsorption tower 5 and defluorinate tower 6 again to remove impurity fluorine and Sodium Fluoride, removes acidic impurities in soda-wash tower 7.After order enters adsorbing tower with molecular sieve 8, activated carbon adsorber 9, sodium peroxide adsorption tower 10, Sulfothiorine washing tower 11 each refining plant then, enter molecular sieve drying tower 12 and remove contained humidity, enter low-temperature fractionating tower 13 and remove high-boiling-point impurity.Eject the gas nitrogen trifluoride that comes from low-temperature fractionating tower 13 and be partially condensated as liquid, flow back in the tower,, after finished product advances gas holder 14 compressed machines 15 compressions, cooling, charge into gas cylinder filling platform 16 as phegma through gas holder 14.
According to the electrolysis and the requirement of improving the quality of products, the anode of installing in the electrolyzer 19 adopts graphite materials, and the temperature of melting salt generally is controlled at 120-160 ℃, and optimum temps is controlled at 125-145 ℃, and voltage is at 6-12V.
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 reaches more than 98%, and has solved problem of environmental pollution.
Claims (3)
1. an electrolyzing fused ammonium bifluoride prepares the technology of nitrogen trifluoride, it is characterized in that: design and installation negative electrode, anodic electrolyzer, surge tank, hydrogen fluoride condensing tower, left Sodium Fluoride adsorption tower, right Sodium Fluoride adsorption tower, defluorinate tower, soda-wash tower, adsorbing tower with molecular sieve, activated carbon adsorber, sodium peroxide adsorption tower, Sulfothiorine washing tower, molecular sieve drying tower, low-temperature fractionating tower, gas holder, compressor in the outer hot-plate casing, fill platform and connect by connection line, be assembled into one and constitute according to the system function order.
2. electrolyzing fused ammonium bifluoride according to claim 1 prepares the technology of nitrogen trifluoride, it is characterized in that: the anode of installing in the electrolyzer adopts graphite material.
3. electrolyzing fused ammonium bifluoride according to claim 1 and 2 prepares the technology of nitrogen trifluoride, it is characterized in that: electrolyzing fused optimum temps is controlled at 125-145 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010265731 CN101942669A (en) | 2010-08-30 | 2010-08-30 | Technique for preparing nitrogen trifluoride by electrolytic melting of ammonium bifluoride |
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| CN 201010265731 CN101942669A (en) | 2010-08-30 | 2010-08-30 | Technique for preparing nitrogen trifluoride by electrolytic melting of ammonium bifluoride |
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| CN101942669A true CN101942669A (en) | 2011-01-12 |
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| CN 201010265731 Pending CN101942669A (en) | 2010-08-30 | 2010-08-30 | Technique for preparing nitrogen trifluoride by electrolytic melting of ammonium bifluoride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112569625A (en) * | 2020-12-30 | 2021-03-30 | 中船重工（邯郸）派瑞特种气体有限公司 | Rectification and purification device for nitrogen trifluoride crude product |
| CN112742158A (en) * | 2020-12-30 | 2021-05-04 | 中船重工（邯郸）派瑞特种气体有限公司 | Hydrogen fluoride waste gas treatment system and method in nitrogen trifluoride electrolysis preparation process |
| CN113247870A (en) * | 2021-04-03 | 2021-08-13 | 中船重工（邯郸）派瑞特种气体有限公司 | Method and device for preparing high-purity nitrogen trifluoride gas |
| WO2024138943A1 (en) * | 2022-12-30 | 2024-07-04 | 福建德尔科技股份有限公司 | Preparation method for nitrogen trifluoride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11335105A (en) * | 1998-05-22 | 1999-12-07 | Mitsui Chem Inc | Production of nitrogen trifluoride gas |
| US6010605A (en) * | 1995-10-17 | 2000-01-04 | Florida Scientific Laboratories Inc. | Nitrogen trifluoride production apparatus |
| CN1450203A (en) * | 2003-04-30 | 2003-10-22 | 中国船舶重工集团公司第七一八研究所 | Fine preparation process for high-purity nitrogen trifluoride gas |
-
2010
- 2010-08-30 CN CN 201010265731 patent/CN101942669A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6010605A (en) * | 1995-10-17 | 2000-01-04 | Florida Scientific Laboratories Inc. | Nitrogen trifluoride production apparatus |
| JPH11335105A (en) * | 1998-05-22 | 1999-12-07 | Mitsui Chem Inc | Production of nitrogen trifluoride gas |
| CN1450203A (en) * | 2003-04-30 | 2003-10-22 | 中国船舶重工集团公司第七一八研究所 | Fine preparation process for high-purity nitrogen trifluoride gas |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112569625A (en) * | 2020-12-30 | 2021-03-30 | 中船重工（邯郸）派瑞特种气体有限公司 | Rectification and purification device for nitrogen trifluoride crude product |
| CN112742158A (en) * | 2020-12-30 | 2021-05-04 | 中船重工（邯郸）派瑞特种气体有限公司 | Hydrogen fluoride waste gas treatment system and method in nitrogen trifluoride electrolysis preparation process |
| CN113247870A (en) * | 2021-04-03 | 2021-08-13 | 中船重工（邯郸）派瑞特种气体有限公司 | Method and device for preparing high-purity nitrogen trifluoride gas |
| WO2024138943A1 (en) * | 2022-12-30 | 2024-07-04 | 福建德尔科技股份有限公司 | Preparation method for nitrogen trifluoride |
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Open date: 20110112 |