CN1328159C - Equipment and technological process for preparing nitrogen trifluoride by using ammonia and hydrogen fluoride as raw material - Google Patents
Equipment and technological process for preparing nitrogen trifluoride by using ammonia and hydrogen fluoride as raw material Download PDFInfo
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- CN1328159C CN1328159C CNB2005100853946A CN200510085394A CN1328159C CN 1328159 C CN1328159 C CN 1328159C CN B2005100853946 A CNB2005100853946 A CN B2005100853946A CN 200510085394 A CN200510085394 A CN 200510085394A CN 1328159 C CN1328159 C CN 1328159C
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Abstract
The present invention relates to a device and a technological method for preparing nitrogen trifluoride by using ammonia and hydrogen fluoride as raw materials. Ammonia in an ammonia storage tank passes through an activated alumina absorption tower firstly to remove most of sulfide thereof and then passes through an activated carbon adsorption tower to remove most of organic substances thereof. Then the ammonia passes through a rectifying tower to remove most of dust, water and partial residual organic substances thereof and then passes through a buffer tank. Finally, ammonia gas and nitrogen with high purity and dewatering hydrogen fluoride are led to a reactor according to a scale and speed, and violent chemical reaction occurs in the reactor to generate ammonia fluoride. The substances in the reactor is the mixture of the ammonia fluoride and the hydrogen fluoride finally, thereby, an electrolyte system of NH4F-xHF is prepared, and then the mixture is input into a normal electrolytic tank to prepare the nitrogen trifluoride with the method of electrolysis. When electrolytic raw materials obtained by the method are used for producing the nitrogen trifluoride, the current density of the electrolytic tank is high. The present invention has the advantages of simple device, strong operability and safe and stable operation of the device, and especially, the cost for producing the raw materials can be reduced to 30% to 50%.
Description
(1), technical field
The invention belongs to a kind of is the equipment and the processing method of feedstock production nitrogen trifluoride with ammonia and hydrogen fluoride, and it is applicable to NH
3-xHF is the synthetic gas of nitrogen trifluoride of raw material.
(2), background technology
Nitrogen trifluoride is the gas of colourless, odorless, stable in properties at normal temperatures, and boiling point is-129 ℃, and fusing point is-208 ℃, and in addition, it still is a kind of strong oxidizer.Nitrogen trifluoride is as a kind of good plasma etch gases, when ion etching, have excellent etch-rate and selectivity, and, do not stay any residue on the etchant surface, be very good clean-out system, therefore, boundless prospect arranged at semi-conductor and microelectronic industry, in addition, it has also obtained in the superlaser field using widely.The preparation method of nitrogen trifluoride has two kinds usually: promptly to use NH
3With F
2For the feedstock production nitrogen trifluoride is the chemical synthesis of representative, and with NH
4F-xHF is raw material prepares nitrogen trifluoride by electrolyzer a electrolytic process.The advantage of electrolytic process be production run comparatively the purity and the productive rate of safety and stability, gas is all higher, therefore, this method is adopted comparatively widely by a lot of enterprises, but that its maximum shortcoming is the electrolysis raw materials cost is too high.
(3), summary of the invention:
In order to overcome the shortcoming of prior art, the invention provides a kind of is the equipment and the processing method of feedstock production nitrogen trifluoride with ammonia and hydrogen fluoride, the electrolysis raw material that obtains with this method is when producing nitrogen trifluoride, the current density height of electrolyzer, equipment is simple, workable, safe and stable equipment operation especially can be reduced to original 30%-50% with the cost of raw materials for production.
With ammonia and hydrogen fluoride is that the equipment of feedstock production nitrogen trifluoride comprises the ammonia storage tank, the activated alumina adsorption tower, activated carbon adsorber, rectifying tower, surge tank, reactor, electrolyzer, the ammonia storage tank, hydrogen fluoride removes water tower, surge tank, the high pure nitrogen storage tank, it is characterized in that: the ammonia storage tank passes through pipeline, variable valve and mass flowmeter link to each other with the activated alumina adsorption tower, the activated alumina adsorption tower links to each other with activated carbon adsorber by pipeline and variable valve, activated carbon adsorber links to each other with rectifying tower by pipeline and variable valve, rectifying tower links to each other with surge tank with variable valve by pipeline, and surge tank links to each other with reactor with variable valve by pipeline; The hydrogen fluoride storage tank removes water tower by pipeline, variable valve and mass flowmeter and potassium bifluoride and links to each other, and potassium bifluoride removes water tower and links to each other with surge tank with variable valve by pipeline, and surge tank links to each other with reactor with variable valve by pipeline; The high pure nitrogen storage tank links to each other with reactor by pipeline, variable valve and mass flowmeter, reactor links to each other with electrolyzer by pipeline and variable valve, electrolyzer links to each other with follow-up equipment by pipeline and variable valve, described reactor inner core and inner all and raw material have parts in contact all to adopt the Monel metal material, and liquid ammonia storage tank must not adopt copper material to pipeline between the reactor and equipment.
With ammonia and hydrogen fluoride is that the processing method of feedstock production nitrogen trifluoride is: the present invention is with NH
3-xHF is that raw material is through the at first synthetic NH of a series of processes
4The F-yHF liquid system, and be electrolytic solution electrolytic preparation gas of nitrogen trifluoride with this liquid, it is characterized in that: NH in the reactor
3With the mole proportioning x=2.0-4 of HF, temperature of reaction is 70 ℃-180 ℃, and reaction pressure is 0.0MPa-0.6Mpa, final NH
4Y=1.3-2.0 in the F-yHF system, arrive the adsorption tower that activated alumina is housed through valve and mass flowmeter after the liquid ammonia vaporization in the ammonia storage tank, working pressure in the adsorption tower is 0.3MPa-0.7Mpa, service temperature is 0 ℃-80 ℃, in adsorption tower, most of sulfide in the ammonia is adsorbed, after ammonia flows out from adsorption tower, flow to the adsorption tower of interior dress gac through valve, the working pressure of adsorption tower is 0.3MPa-0.6Mpa, service temperature is-20 ℃-70 ℃, in adsorption tower, the most of organism in the raw material ammonia is adsorbed, and ammonia flows to rectifying tower through control valve after adsorption tower flows out, the service temperature of rectifying tower is :-30 ℃-10 ℃ of top temperature, still temperature-20 ℃-50 ℃; Ammonia flows out rectifying tower after check valve and surge tank flow to reactor, in reactor ammonia with meet from the gaseous hydrogen fluoride of hydrogen fluoride storage tank and from the high pure nitrogen of storage tank, and at the violent chemical reaction generation ammonium bifluoride of this generation, the present invention has disposed whipping appts and water-circulating cooling device on reactor, material in the reactor finally is ammonium bifluoride and hydrofluoric liquid form mixt, this mixture flows to the conventional electrolysis groove through valve, and in electrolyzer electrolytically synthesizing nitrogen trifluoride.
The electrolysis raw material that obtains with this equipment and method when producing nitrogen trifluoride, the current density height of electrolyzer, equipment is simple, and is workable, safe and stable equipment operation especially can be reduced to original 30%-50% with the cost of raw materials for production.
(4), description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Accompanying drawing is principle of the invention figure.
(5), embodiment
As shown in drawings, 1---the ammonia storage tank, 2,5,7,13,15,16,19,25,27,30---control valve, 3,26,29---mass flowmeter, 4---the activated alumina adsorption tower, 6---activated carbon adsorber, 8---rectifying tower, 9,23---check valve, 10,22---surge tank, 11---agitator motor, 12---reactor, 14---electrolyzer, 17---anode, 18---negative electrode, 21---the recirculated cooling water cover, 22---surge tank, 24---potassium bifluoride removes water tower.
Realize that the required equipment of the technology of the present invention purpose comprises: ammonia storage tank 1, activated alumina adsorption tower 4, activated carbon adsorber 6, rectifying tower 8, surge tank 10, reactor 12, electrolyzer 10, ammonia storage tank 20, potassium bifluoride remove water tower 24, surge tank 22, high pure nitrogen storage tank 23.It is characterized in that: ammonia storage tank 1 links to each other with activated alumina adsorption tower 4 by pipeline, variable valve 2 and mass flowmeter 3, activated alumina adsorption tower 4 links to each other with activated carbon adsorber 6 by pipeline and variable valve 5, activated carbon adsorber 6 links to each other with rectifying tower 8 by pipeline and variable valve, rectifying tower 8 links to each other with surge tank 10 with variable valve by pipeline, and surge tank 10 links to each other with reactor 12 with variable valve by pipeline; Hydrogen fluoride storage tank 28 removes water tower 24 by pipeline, variable valve 25, variable valve 27 and mass flowmeter 26 and potassium bifluoride and links to each other, potassium bifluoride removes water tower 24 and links to each other with surge tank 22 with variable valve by pipeline, and surge tank 22 links to each other with reactor 12 with variable valve by pipeline; High pure nitrogen storage tank 23 links to each other with reactor 12 by pipeline, variable valve 30 and mass flowmeter 29.Reactor 12 links to each other with electrolyzer 14 by pipeline and variable valve 19, and electrolyzer links to each other with follow-up equipment by pipeline and variable valve 15, variable valve 16.Described reactor 12 inner cores and inner all and raw material have parts in contact all to adopt the Monel metal material, and liquid ammonia storage tank 1 must not adopt copper material to pipeline between the reactor 12 and equipment.
The present invention is with NH
3-xHF is that raw material is through a series of process electrolytically synthesizing nitrogen trifluoride gases.Because the price of liquefied ammonia is far below the price of the ammonium bifluoride suitable with its purity, in addition, be further purified on the problem, liquefied ammonia is also wanted easily than ammonium bifluoride and is many easily, therefore, technical purpose of the present invention (reduction raw materials cost) has just obtained comparatively perfectly realizing.NH in the reactor 12
3With the mole proportioning x=2.0-4 of HF material system, temperature of reaction is 70 ℃-180 ℃, and reaction pressure is 0.0MPa-0.6Mpa, and speed of reaction is concrete much by the processing power of adsorption tower and rectifying tower and the response capacity decision of reactor.
After the vaporization of liquid ammonia in the ammonia storage tank when the adsorption tower 4 of activated alumina is housed, because activated alumina is to NH
3With sulfide goodish selectivity is being arranged aspect the absorption, therefore, the most of sulfide in the ammonia will be compared absorption up hill and dale here and fall, and the working pressure in the adsorption tower 4 is 0.3MPa-0.7Mpa, and service temperature is 20 ℃-80 ℃.
When ammonia passed through the adsorption tower 6 of interior dress gac, because gac is obvious to ammonia and organic selectivity, here, the most of organism in the ammonia was adsorbed, and the working pressure of adsorption tower 6 is 0.3MPa-0.6Mpa, and service temperature is 10 ℃-70 ℃.
Ammonia is when the rectifying tower 8, because the boiling point of ammonia and water differs greatly, therefore, ammonia can be separated herein preferably with water, and the service temperature of rectifying tower 8 is: warm-30 ℃-10 ℃ of top, still temperature-20 ℃-50 ℃.
When hydrogen fluoride removes water tower 24 through potassium bifluoride, water and potassium bifluoride reaction generate hydrogen fluoride and potassium hydroxide, thereby, the water in the hydrogen fluoride is removed comparatively completely, the working pressure that potassium bifluoride removes water tower 24 is 0.2MPa-0.6Mpa, and service temperature is 20 ℃-70 ℃.
Ammonia meets in reactor Yu from the hydrogen fluoride storage tank and through the gaseous hydrogen fluoride that potassium bifluoride dewaters after a series of processing, and at the violent chemical reaction generation ammonium bifluoride of this generation, because ammonia and hydrogen fluoride reaction are very violent, there is a large amount of reaction heat to produce simultaneously, therefore, the present invention has disposed whipping appts and water-circulating cooling device on reactor, so that temperature of reaction is further controlled.
Because we are with NH
3Be decided to be x=2.0-4 with the mole proportioning of HF material system, temperature of reaction is 70 ℃-180 ℃, reaction pressure is 0.0MPa-0.6Mpa, therefore, material in the reactor finally is liquid ammonium bifluoride and hydrofluoric mixture, and this mixture flows to the conventional electrolysis groove through valve, and in electrolyzer electrolytically synthesizing nitrogen trifluoride, the nitrogen trifluoride that electrolysis generates in electrolyzer need only simple process behind valve, just can enter follow-up workshop section with further purifying treatment.
Electrolytic solution through the said process preparation carries out in the normal electrolytic process at conventional electrolysis groove 14, analyzes result such as table 1 from anolyte compartment's outlet sampling:
Table 1, the method for the invention are produced the composition of synthetic nitrogen trifluoride product gas
| The material title | O 2+N 2 | CF 4 | NF 3 | N xF y | CO 2 | N 2O |
| Content | 22.209％ | 0 | 73.707％ | 0.8％ | 1.2％ | 0.23％ |
Table 1 explanation: in method synthetic nitrogen trifluoride product of the present invention, O
2And N
2Concentration sum and N
2O, N
xF
yDeng concentration with compare a little less than traditional method CF with traditional method
4Be not detected NF at this
3Concentration with compare a little more than traditional method with traditional method.
Claims (4)
1, with ammonia and hydrogen fluoride is the equipment of feedstock production nitrogen trifluoride, comprise ammonia storage tank (1,20), activated alumina adsorption tower (4), activated carbon adsorber (6), rectifying tower (8), surge tank (10,22), reactor (12), electrolyzer (14), potassium bifluoride removes water tower (24), high pure nitrogen storage tank (23), it is characterized in that: ammonia storage tank (1) passes through pipeline, variable valve (2) and mass flowmeter (3) link to each other with activated alumina adsorption tower (4), activated alumina adsorption tower (4) links to each other with activated carbon adsorber (6) by pipeline and variable valve (5), activated carbon adsorber (6) links to each other with rectifying tower (8) by pipeline and variable valve, rectifying tower (8) links to each other with surge tank (10) with variable valve by pipeline, and surge tank (10) links to each other with reactor (12) with variable valve by pipeline; Hydrogen fluoride storage tank (28) removes water tower (24) by pipeline, variable valve (25,27) and mass flowmeter (26) and potassium bifluoride and links to each other, potassium bifluoride removes water tower (24) and links to each other with surge tank (22) with variable valve by pipeline, and surge tank (22) links to each other with reactor (12) with variable valve by pipeline; High pure nitrogen storage tank (23) links to each other with reactor (12) by pipeline, variable valve (30) and mass flowmeter (29), reactor (12) links to each other with electrolyzer (14) by pipeline and variable valve (19), electrolyzer links to each other with follow-up equipment by pipeline and variable valve (15,16), described reactor (12) inner core and inner all and raw material have parts in contact all to adopt the Monel metal material, and liquid ammonia storage tank (1) must not adopt copper material to pipeline and the equipment between the reactor (12).
2, according to claim 1 is the equipment of feedstock production nitrogen trifluoride with ammonia and hydrogen fluoride, it is characterized in that: potassium bifluoride removes in the water tower (24) the potassium bifluoride particle is housed.
3, use the described equipment of claim 1 to be the processing method of feedstock production nitrogen trifluoride, it is characterized in that: with NH with ammonia and hydrogen fluoride
3-xHF is that raw material is through the at first synthetic NH of a series of processes
4The F-yHF liquid system, and be electrolytic solution electrolytic preparation gas of nitrogen trifluoride with this liquid, NH in the reactor (8)
3With the mole proportioning x=2.0-4 of HF, temperature of reaction is 70 ℃-180 ℃, and reaction pressure is 0.0MPa-0.6MPa, final NH
4Y=1.3-2.0 in the F-yHF system, arrive the adsorption tower (4) that activated alumina is housed through valve (2) and mass flowmeter (3) after the liquid ammonia vaporization in the ammonia storage tank (1), working pressure in the adsorption tower (4) is 0.3MPa-0.7MPa, service temperature is 0 ℃-80 ℃, in adsorption tower (4), most of sulfide in the ammonia is adsorbed, after ammonia flows out from adsorption tower (4), flow to the adsorption tower (6) of interior dress gac through valve (5), the working pressure of adsorption tower (6) is 0.3MPa-0.6MPa, service temperature is-20 ℃-70 ℃, in adsorption tower (6), the most of organism in the raw material ammonia is adsorbed, and ammonia flows to rectifying tower (8) through control valve (7) after adsorption tower (6) flows out, the service temperature of rectifying tower (8) is :-30 ℃-10 ℃ of top temperature, still temperature-20 ℃-50 ℃; Ammonia flows out rectifying tower (8) after check valve (9) and surge tank (10) flow to reactor (12), in reactor (12) ammonia with meet from the gaseous hydrogen fluoride of hydrogen fluoride storage tank (28) and from the high pure nitrogen of storage tank (31), and at the violent chemical reaction generation ammonium bifluoride of this generation, the present invention has disposed whipping appts (11) and water-circulating cooling device (21) on reactor (12), material in the reactor finally is ammonium bifluoride and hydrofluoric liquid form mixt, this mixture flows to conventional electrolysis groove (14) through valve (19), and in electrolyzer (14) electrolytically synthesizing nitrogen trifluoride.
4, according to claim 2 is the processing method of feedstock production nitrogen trifluoride with ammonia and hydrogen fluoride, and it is characterized in that: the reactant in the described reactor (12) is NH
3With HF.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100853946A CN1328159C (en) | 2005-07-27 | 2005-07-27 | Equipment and technological process for preparing nitrogen trifluoride by using ammonia and hydrogen fluoride as raw material |
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| CNB2005100853946A CN1328159C (en) | 2005-07-27 | 2005-07-27 | Equipment and technological process for preparing nitrogen trifluoride by using ammonia and hydrogen fluoride as raw material |
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| CN1328159C true CN1328159C (en) | 2007-07-25 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913579A (en) * | 2010-08-30 | 2010-12-15 | 天津市泰源工业气体有限公司 | Technology for preparing nitrogen trifluoride by directly fluoridizing gaseous phases of fluorin and ammonia |
| CN104947135B (en) * | 2015-06-09 | 2017-10-13 | 中国船舶重工集团公司第七一八研究所 | A kind of device for preparing gas of nitrogen trifluoride and application |
| CN108557785A (en) * | 2018-05-09 | 2018-09-21 | 刘成霞 | A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material |
| CN111039267B (en) * | 2019-12-29 | 2023-09-08 | 中船(邯郸)派瑞特种气体股份有限公司 | Device and method for prepurifying electrolytic prepared nitrogen trifluoride crude product |
| CN112626548A (en) * | 2020-12-22 | 2021-04-09 | 中船重工（邯郸）派瑞特种气体有限公司 | Charging system and method for nitrogen trifluoride electrolytic cell |
| CN115487522B (en) * | 2022-09-06 | 2023-06-23 | 内蒙古东岳金峰氟化工有限公司 | Hydrogen fluoride purification system and process |
| CN115490215B (en) * | 2022-09-20 | 2024-01-30 | 洛阳森蓝化工材料科技有限公司 | Device and method for preparing nitrogen trifluoride |
Citations (4)
| 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 |
| 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 |
| US20040096387A1 (en) * | 2002-11-19 | 2004-05-20 | Syvret Robert George | Method for nitrogen trifluoride production |
| US20040120877A1 (en) * | 2002-12-23 | 2004-06-24 | Satchell Donald P. | NF3 production reactor |
-
2005
- 2005-07-27 CN CNB2005100853946A patent/CN1328159C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040096387A1 (en) * | 2002-11-19 | 2004-05-20 | Syvret Robert George | Method for nitrogen trifluoride production |
| US20040120877A1 (en) * | 2002-12-23 | 2004-06-24 | Satchell Donald P. | NF3 production reactor |
| 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 |
| 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 |
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Effective date of registration: 20190708 Address after: 057550 No. 1 Weiwu Road, Chemical Industry Agglomeration Area, Feixiang County, Handan City, Hebei Province Patentee after: CSIC (Handan) Perry Special Gas Co. Ltd Address before: 056027 Yuan Xiaoyan, 17 Exhibition Road, Handan City, Hebei Province Patentee before: No.718 Inst., China Shipping Heavy Industry Group Co. |
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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Patentee after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Patentee before: PERIC SPECIAL GASES Co.,Ltd. |
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