CN113233433B - Device and method for adjusting concentration of dinitrogen pentoxide - Google Patents
Device and method for adjusting concentration of dinitrogen pentoxide Download PDFInfo
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- CN113233433B CN113233433B CN202110524640.2A CN202110524640A CN113233433B CN 113233433 B CN113233433 B CN 113233433B CN 202110524640 A CN202110524640 A CN 202110524640A CN 113233433 B CN113233433 B CN 113233433B
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/206—Nitric anhydride (N2O5)
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Abstract
The invention provides a device and a method for adjusting the concentration of dinitrogen pentoxideThe method comprises the following steps of: the first gas source is used for providing nitric oxide gas with known concentration; the second gas source is used for providing ozone gas; the nitric oxide and the ozone react in the reaction unit to generate dinitrogen pentoxide; the trapping and releasing unit is used for trapping and releasing dinitrogen pentoxide generated by the reaction; the first gas provided by the third gas source is mixed with the dinitrogen pentoxide released by the trapping and releasing unit; a temperature control unit for adjusting the temperature of the trapping and releasing unit T1 And adjusting the temperature of the mixture of the released dinitrogen pentoxide and the first gas T2 (ii) a A fourth gas source provides a dilution gas for diluting the sample with a dilution factor C And diluting the mixed gas. The invention has the advantages of automation, good stability and the like.
Description
Technical Field
The invention relates to standard gas generation, in particular to a device and a method for adjusting concentration of dinitrogen pentoxide.
Background
Free radical of nitric acid (NO) 3 ) Is an important nighttime atmospheric oxidant for ambient atmosphere. And dinitrogen pentoxide (N) as a product of the reaction of the nitric acid group with nitrogen dioxide 2 O 5 ) The production of nitrate particulates and the activation of chlorine radicals at night are affected. Research on nitrate groups and dinitrogen pentoxide and measurement of their environmental concentrations have recently become a hotspot in the field of atmospheric chemistry. Due to NO 3 And N 2 O 5 The gas is unstable and difficult to store, and no commercial calibration instrument is used for calibrating the nitric acid radical and the dinitrogen pentoxide in the market at present. But in factN prepared in laboratory 2 O 5 Solid is difficult to store (requiring storage at-80 deg.C), and N is used 2 Purging N 2 O 5 Solid to produce N 2 O 5 The gas concentration is unstable.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a device for adjusting the concentration of dinitrogen pentoxide.
The purpose of the invention is realized by the following technical scheme:
a dinitrogen pentoxide concentration adjusting device, the dinitrogen pentoxide concentration adjusting device including:
a first gas source for providing nitric oxide gas of a known concentration;
a second gas source for providing ozone gas;
a reaction unit, wherein the nitric oxide and the ozone react to generate dinitrogen pentoxide;
a trapping and releasing unit for trapping and releasing dinitrogen pentoxide generated by the reaction;
a third gas source, wherein the first gas provided by the third gas source is mixed with the dinitrogen pentoxide released by the trapping and releasing unit;
a temperature control unit for adjusting a temperature T of the trapping and releasing unit 1 And adjusting the temperature T of the mixture of the released dinitrogen pentoxide and the first gas 2 ；
A fourth gas source providing a dilution gas for diluting the mixture gas by a dilution factor C.
The invention also aims to provide a method for adjusting the concentration of dinitrogen pentoxide, which is realized by the following technical scheme:
a method for adjusting a concentration of dinitrogen pentoxide, the method comprising the steps of:
(A1) reacting nitric oxide and ozone at known concentrations in a reaction unit to produce dinitrogen pentoxide;
(A2) the dinitrogen pentoxide is trapped by a trap and release unit, and a temperature control unit adjusts the temperature T of the trap and release unit 1 Thereby regulating the release of dinitrogen pentoxide;
(A3) the released dinitrogen pentoxide is mixed with the first gas, and the mixed gas is sent to the downstream;
(A4) adjusting the temperature T of the mixture 2 Thereby adjusting the concentration of dinitrogen pentoxide;
(A5) diluting the mixed gas by a dilution factor C.
Compared with the prior art, the invention has the beneficial effects that:
the dinitrogen pentoxide is produced by adopting an on-site reaction, and the concentration of the dinitrogen pentoxide is accurately adjusted by utilizing temperature control and dilution times, so that the method realizes the following steps:
1. the dinitrogen pentoxide gas is generated on line, and the dinitrogen pentoxide gas is not required to be stored under the condition of dry ice after being prepared in a laboratory, so that the method is simple and convenient;
2. after the dinitrogen pentoxide is released in the trapping and releasing unit, the dinitrogen pentoxide is converted into nitrogen dioxide by a nitric oxide titration method for concentration measurement, and the concentration C of the nitrogen trioxide and the dinitrogen pentoxide in the mixed gas are obtained in real time 0 The concentration can be adjusted by controlling the temperature of the trapping and releasing unit through feedback;
the concentration ratios of different nitrogen trioxide and nitrogen pentoxide are adjusted by adjusting the temperature of the mixed gas, so that different scene requirements are met;
by adjusting the temperature (the temperature of the trapping and releasing unit and the temperature of the mixed gas), the adjustment of the concentration of the dinitrogen pentoxide, that is, the adjustment of the concentration of the nitrogen trioxide is realized;
3. the calculation unit accurately calculates the concentration of dinitrogen pentoxide using a formula.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic configuration diagram of a dinitrogen pentoxide concentration adjustment apparatus according to embodiment 1 of the present invention;
FIG. 2 is a schematic view showing the structure of a dinitrogen pentoxide concentration adjusting apparatus according to embodiment 1 of the present invention.
Detailed Description
Fig. 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of explaining the technical solution of the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 is a schematic structural view of an apparatus for adjusting a concentration of dinitrogen pentoxide according to an embodiment of the present invention, and as shown in fig. 1, the apparatus for adjusting a concentration of dinitrogen pentoxide includes:
a first gas source for providing nitric oxide gas of a known concentration;
a second gas source for providing ozone gas, such as obtained by an in-situ reaction;
a reaction unit, wherein the nitric oxide and the ozone react to generate dinitrogen pentoxide;
a trapping and releasing unit, such as a cold trap, for trapping and releasing the dinitrogen pentoxide generated by the reaction;
a third gas source, wherein the first gas provided by the third gas source is mixed with the dinitrogen pentoxide released by the trapping and releasing unit;
a temperature control unit for adjusting a temperature T of the trapping and releasing unit 1 And adjusting the temperature of the mixture of the released dinitrogen pentoxide and the first gasDegree T 2 ；
A fourth gas source providing a dilution gas for diluting the mixture gas by a dilution factor C.
In order to accurately obtain the concentration of dinitrogen pentoxide, further, the dinitrogen pentoxide concentration adjustment device further includes:
a calculation unit that obtains a concentration of dinitrogen pentoxide based on the temperature and the dilution factor,
In order to obtain the coefficients a and b, the device for adjusting the concentration of dinitrogen pentoxide further comprises:
a detection unit provided downstream of the trapping and releasing unit for detecting the concentration of dinitrogen pentoxide and nitrogen trioxide in the mixed gas and C 0 ；
The computing unit is based on
Coefficients a and b are obtained.
To accurately obtain the concentration and C 0 Further, the third source of gas provides nitric oxide, the concentrations and
C 3 is the concentration of nitrogen dioxide in the nitric oxide provided by the third gas source, C 4 Is the concentration of nitrogen dioxide in the gas mixture.
To obtain the coefficient K accurately, further, the coefficient K is the equilibrium constant of the following reaction at a temperature of 298K:
in order to accurately adjust the concentration of the mixture gas to adjust the concentration of the dinitrogen pentoxide, the dinitrogen pentoxide concentration adjusting device further includes:
the conveying pipe is used for allowing the dinitrogen pentoxide released by the trapping and releasing unit to enter, and the temperature control unit is used for adjusting the temperature T of the dinitrogen pentoxide in the conveying pipe 2 (ii) a The first gas provided by the third gas source is sent into the conveying pipe.
The method for adjusting the concentration of dinitrogen pentoxide according to the embodiment of the present invention includes the steps of:
(A1) reacting nitric oxide and ozone at known concentrations in a reaction unit to produce dinitrogen pentoxide;
(A2) the dinitrogen pentoxide is trapped by a trap and release unit, and a temperature control unit adjusts the temperature T of the trap and release unit 1 Thereby regulating the release of dinitrogen pentoxide;
(A3) the released dinitrogen pentoxide is mixed with the first gas, and the mixed gas is sent to the downstream;
(A4) adjusting the temperature T of the mixture 2 Thereby adjusting the concentration of dinitrogen pentoxide;
(A5) diluting the mixed gas by a dilution factor C.
In order to accurately obtain the concentration of dinitrogen pentoxide, further, the concentration of dinitrogen pentoxide is obtained in accordance with the temperature and the dilution factor,
In order to accurately obtain the coefficients a, b and K, further, the first gas is nitric oxide, and the concentrations of dinitrogen pentoxide and nitrogen trioxide in the mixed gas and C are detected 0 ；
According to
Obtaining coefficients a and b;
the coefficient K is the equilibrium constant for the following reaction at a temperature of 298K:
to accurately obtain the concentration and C 0 Further, the concentration and
C 3 is the concentration of nitrogen dioxide in the first gas, C, in step (A3) 4 Is the concentration of nitrogen dioxide in the gas mixture.
Example 2:
an example of application of the device and method for adjusting the concentration of dinitrogen pentoxide according to embodiment 1 of the present invention.
In this example, as shown in FIG. 2, the first gas source is a cylinder that provides a known concentration of nitric oxide and contains a concentration of nitrogen dioxide C 3 (ii) a The second gas source employs an ozone production unit, such as CN 200910154006.3; the third gas source and the first gas source are shared to provide nitric oxide; a fourth gas source provides synthetic air, provides gas for the second gas source to prepare ozone, and provides purge gas for the trapping and releasing unit, and also serves as dilution gas; the trapping and releasing unit adopts a cold trap, so that dinitrogen pentoxide is enriched at a low temperature and released after heating; the released dinitrogen pentoxide is mixed with nitric oxide provided by a third gas source, and part of the mixed gas enters the conveying pipe and is sent to the detection unit; the detection unit adopts a spectrophotometer and is used for detecting the concentration of the nitrogen dioxide in the mixed gas.
The method for adjusting the concentration of the dinitrogen pentoxide comprises the following steps of:
(A1) the synthetic air provided by the fourth air source enters the second air source and generates ozone under the irradiation of ultraviolet rays (such as a mercury lamp);
the nitric oxide of known concentration provided by the first gas source and the excess ozone provided by the second gas source react in the reaction unit to generate dinitrogen pentoxide by, in particular,
NO+O 3 →NO 2 ，
NO 2 +O 3 →NO 3 ，
NO 2 +NO 3 ←→N 2 O 5 the equilibrium constant of the reaction at a temperature of 298K is the coefficient K;
(A2) the dinitrogen pentoxide is trapped by a trapping and releasing unit, such as a cold trap at-80 ℃; after the trapping is finished, gas is switched, gas provided by a fourth gas source enters the trapping and releasing unit for purging, and the temperature control unit adjusts the temperature T of the trapping and releasing unit 1 Thereby regulating the release of dinitrogen pentoxide;
(A3) mixing the released dinitrogen pentoxide with nitric oxide provided by a third gas source, and conveying part of the mixed gas to a conveying pipe and conveying part of the mixed gas to a detection unit;
the spectrophotometer detects the absorbance of the mixed gas at 485nm (absorption spectrum line of nitrogen dioxide), and the concentration C of the nitrogen dioxide in the mixed gas is obtained by utilizing the spectral analysis technology 4 Thereby obtaining the concentration sum of the nitrogen trioxide and the dinitrogen pentoxide in the mixed gas
A computing unit is based on
Fitting coefficients a and b;
(A4) adjusting the temperature T of the mixed gas in the conveying pipe by using the temperature control unit 2 Thereby adjusting the concentration ratio of the dinitrogen pentoxide and the nitrogen trioxide, namely adjusting the concentration of the dinitrogen pentoxide; such as, for example,
when the temperature in the conveying pipe is 0 ℃, the dinitrogen pentoxide accounts for 94%, and when the temperature in the conveying pipe is 80 ℃, the dinitrogen pentoxide accounts for 1.7%;
(A5) the fourth gas source provides gas, so that the mixed gas discharged out of the conveying pipe is diluted by the dilution multiple C to obtain the concentration of the dinitrogen pentoxide in the diluted gas,
Claims (10)
1. A dinitrogen pentoxide concentration adjustment device, characterized in that the dinitrogen pentoxide concentration adjustment device includes:
a first gas source for providing nitric oxide gas of a known concentration;
a second gas source for providing ozone gas;
a reaction unit, wherein the nitric oxide and the ozone react to generate dinitrogen pentoxide;
a trapping and releasing unit for trapping and releasing dinitrogen pentoxide generated by the reaction;
a third gas source providing a first gas to be mixed with the dinitrogen pentoxide released by the trapping and releasing unit, wherein the first gas is nitric oxide;
a temperature control unit for adjusting a temperature T of the trapping and releasing unit 1 And adjusting the temperature T of the mixture of the released dinitrogen pentoxide and the first gas 2 ；
A fourth gas source providing a dilution gas for diluting the mixture gas by a dilution factor C.
2. The device for adjusting the concentration of dinitrogen pentoxide according to claim 1, wherein the device for adjusting the concentration of dinitrogen pentoxide further comprises:
a calculation unit that obtains a concentration of dinitrogen pentoxide based on the temperature and the dilution factor,
3. The device for adjusting the concentration of dinitrogen pentoxide according to claim 2, wherein the device for adjusting the concentration of dinitrogen pentoxide further comprises:
a detection unit provided downstream of the trapping and releasing unit for detecting the concentration of dinitrogen pentoxide and nitrogen trioxide in the mixed gas and C 0 ；
The computing unit is based on
The coefficients a and b are obtained.
4. Device for adjusting the concentration of dinitrogen pentoxide according to claim 3, wherein said third gas source supplies nitric oxide, said sum of concentrations
，C 3 Is the concentration of nitrogen dioxide in the nitric oxide provided by the third gas source, C 4 Is the concentration of nitrogen dioxide in the gas mixture.
5. Device for adjusting the concentration of dinitrogen pentoxide according to claim 2, characterized in that the coefficient K is the equilibrium constant of the following reaction at a temperature of 298K:
6. the device for adjusting the concentration of dinitrogen pentoxide according to claim 1, wherein the device for adjusting the concentration of dinitrogen pentoxide further comprises:
the conveying pipe is used for allowing the dinitrogen pentoxide released by the trapping and releasing unit to enter, and the temperature control unit is used for adjusting the temperature T of the dinitrogen pentoxide in the conveying pipe 2 (ii) a The first gas provided by the third gas source is sent into the conveying pipe.
7. A method for adjusting a concentration of dinitrogen pentoxide, the method comprising the steps of:
(A1) reacting nitric oxide and ozone at known concentrations in a reaction unit to produce dinitrogen pentoxide;
(A2) the dinitrogen pentoxide is trapped by a trap and release unit, and a temperature control unit adjusts the temperature T of the trap and release unit 1 Thereby regulating the release of dinitrogen pentoxide;
(A3) the released dinitrogen pentoxide is mixed with the first gas, and the mixed gas is sent to the downstream;
(A4) adjusting the temperature T of the mixture 2 Thereby adjusting the concentration of dinitrogen pentoxide;
(A5) diluting the mixed gas by a dilution factor C.
8. The method for adjusting the concentration of dinitrogen pentoxide according to claim 7, wherein the concentration of dinitrogen pentoxide is obtained in accordance with a temperature and a dilution factor,
9. The method according to claim 8, wherein the first gas is nitric oxide, and the concentration of dinitrogen pentoxide or nitrogen trioxide in the mixed gas and C are detected 0 ；
According to
Obtaining coefficients a and b;
the coefficient K is the equilibrium constant for the following reaction at a temperature of 298K:
10. the method of adjusting the concentration of dinitrogen pentoxide according to claim 9, wherein the sum of the concentrations
，C 3 Is the concentration of nitrogen dioxide in the first gas, C, in step (A3) 4 Is the concentration of nitrogen dioxide in the gas mixture.
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| SU1089047A1 (en) * | 1982-05-26 | 1984-04-30 | Казанский Ордена Ленина И Ордена Трудового Красного Знамени Государственный Университет Им.В.И.Ульянова-Ленина | Method for preparing nitrogen pentoxide |
| GB9017135D0 (en) * | 1990-08-04 | 1990-09-19 | Secr Defence | Method of extracting dinitrogen pentoxide from its mixture with nitric acid |
| GB9017134D0 (en) * | 1990-08-04 | 1990-09-19 | Secr Defence | Process of and apparatus for preparing dinitrogen pentoxide |
| DE19840018A1 (en) * | 1998-09-02 | 2000-03-09 | Fraunhofer Ges Forschung | Process and device for producing nitrous oxide |
| EP1630133A1 (en) * | 2004-08-27 | 2006-03-01 | Innovative Ozone Services Inc. | Method and arrangement for producing nitrogen oxides |
| US8784762B2 (en) * | 2011-02-15 | 2014-07-22 | Ati Properties, Inc. | Treatment of NOx-containing gas streams |
| KR101443342B1 (en) * | 2012-06-28 | 2014-09-19 | 현대제철 주식회사 | APPARATUS OF REMOVING NOx |
| CN106187870A (en) * | 2016-07-28 | 2016-12-07 | 南京红太阳生物化学有限责任公司 | A kind of 4 picoline location nitrations are the method for 3 nitro 4 picolines |
| CN106430130B (en) * | 2016-10-13 | 2018-06-12 | 中国科学院化学研究所 | A kind of online preparation of dinitrogen pentoxide and standard generating system and preparation method |
| CN112090253A (en) * | 2020-09-14 | 2020-12-18 | 浙江大学 | Method and device for simultaneously desulfurizing and denitrifying flue gas by combining step-by-step catalytic oxidation with wet absorption |
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