CN102774819B - Method for producing N2O4 (nitrogen tetroxide) through combining normal pressure diluted nitric acid, pressurized diluted nitric acid and concentrated nitric acid devices - Google Patents
Method for producing N2O4 (nitrogen tetroxide) through combining normal pressure diluted nitric acid, pressurized diluted nitric acid and concentrated nitric acid devices Download PDFInfo
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- CN102774819B CN102774819B CN201210106918.5A CN201210106918A CN102774819B CN 102774819 B CN102774819 B CN 102774819B CN 201210106918 A CN201210106918 A CN 201210106918A CN 102774819 B CN102774819 B CN 102774819B
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- nitric acid
- gas
- tower
- nitre
- normal pressure
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 72
- WFPZPJSADLPSON-UHFFFAOYSA-N dinitrogen tetraoxide Chemical compound [O-][N+](=O)[N+]([O-])=O WFPZPJSADLPSON-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- 239000007789 gas Substances 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 20
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 62
- 238000007254 oxidation reaction Methods 0.000 claims description 20
- 238000004061 bleaching Methods 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000003595 mist Substances 0.000 claims description 4
- PNPIRSNMYIHTPS-UHFFFAOYSA-N nitroso nitrate Chemical compound [O-][N+](=O)ON=O PNPIRSNMYIHTPS-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000002918 waste heat Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012267 brine Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N Nitrogen dioxide Chemical compound O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 abstract 3
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 abstract 1
- 238000009435 building construction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000000618 nitrogen fertilizer Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- OMBRFUXPXNIUCZ-UHFFFAOYSA-N dioxidonitrogen(1+) Chemical compound O=[N+]=O OMBRFUXPXNIUCZ-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
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- Manufacture And Refinement Of Metals (AREA)
- Fertilizers (AREA)
Abstract
The invention relates to a method for producing N2O4 (nitrogen tetroxide) through combining normal pressure diluted nitric acid, pressurized diluted nitric acid and concentrated nitric acid devices. The method comprises the following steps that the normal pressure diluted nitric acid, pressurized diluted nitric acid and concentrated nitric acid devices are combined for preparing NO2 (nitrogen dioxide) gas; liquid-stage N2O4 is prepared; and the discharged tail gas is treated. The public engineering conditions of the existing device and idle equipment can be sufficiently utilized, the investment is reduced, and the building construction period is shortened. The combination of the normal pressure diluted nitric acid, pressurized diluted nitric acid and concentrated nitric acid devices is realized, and the industrial level N2O4 is produced for reaching the goals of revitalizing the existing assets, increasing the product varieties and improving the risk-resistance capability of enterprises.
Description
Technical field
The invention belongs to N
2o
4production technical field, particularly the rare nitre of a kind of normal pressure, rare nitre and dense nitre device combination producing N pressurize
2o
4method.
Background technology
The production of current domestic nitrogen tetroxide mainly concentrates on Jilin Chemical and Huaihe River, and it is only that direct method is produced the byproduct in concentrated nitric acid process, and output is minimum, if increase the produced quantity of nitrogen tetroxide, will have a strong impact on output and the quality of finished product concentrated nitric acid.Greatly expand in daily life application with aerospace industry and organic fine chemical industry in recent years, the consumption of nitrogen tetroxide and thereupon significantly increasing, thereby in the urgent need to improving nitrogen tetroxide throughput.In addition in industrial nitric acid production, two pressurization nitric acid " four-in-one " unit accounts for dominant advantage gradually, traditional normal pressure nitric acid and Nitric Acid Device are about to be eliminated, unused nitric acid production plant is more and more, how rationally to utilize the unused device with throughput to become gradually the focus that medium and small nitrogen fertilizer factory pays close attention to.If newly-built a set of N
2o
4production equipment can not make full use of the general facilities condition of existing apparatus, also causes idle available devices not reuse, and invests highlyer, and the completion time of project is longer; And nitrogen tetroxide is only as the byproduct in industrial concentrated acid production process, and output is less, can not effectively meet the need of market, the earning rate that business capital reclaims is less, and the ability to ward off risks weakens.In addition, the exhaust gas processing device of original normal pressure nitric acid workshop section is more backward, can not meet the requirement that chemical enterprise safety and environmental protection is produced.
Summary of the invention
Object of the present invention is:
Object of the present invention is exactly the deficiency in order to overcome above-mentioned background technology, solves and provide the rare nitre of a kind of normal pressure, rare nitre and dense nitre device combination producing N pressurize
2o
4method.
The rare nitre of normal pressure involved in the present invention, rare nitre and dense nitre device combination producing N pressurize
2o
4method flow as follows:
After fast cooler, gas cooler are cooling, enter just oxidizing tower from the ammonia oxidation gas of the rare nitric acid of normal pressure unit waste heat boiler, the secondary air that the NO in gas is come by gas blower is tentatively oxidized to NO
2(oxidation ratio is up to 92%), " 55% " nitric acid simultaneously this tower being produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, produce concentrated nitric acid for a nitre.Go out the just gas of oxidizing tower and be almost all oxidized to NO by " 98% " nitric acid (from the concentrated acid storage tank of Jian Xiao workshop section) in re-oxidation tower
2, and " 75% " nitric acid being diluted (is dissolved to approximately 15% NO
2), deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO
2gas.Re-oxidation tower top NO out
2gas enters nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after water cooler is cooling, becomes containing 30% free NO
2nitrosonitric acid, then nitrosonitric acid is delivered to bleaching tower bleaching, discharge NO
2gas, concentrated nitric acid is discharged at the bottom of tower, after cooling, can recycle or deliver to a nitre finished product concentrated nitric acid storage tank for nitrosonitric acid absorber portion.Bleaching tower ejects the pure NO coming
2gas, through preliminary cooling the removing after acid mist of watercooler, enters N
2o
4condenser, is frozen salt solution (from pressurization workshop section refrigerator group) and is condensed into liquid nitrogen tetroxide, and deliver to liquid nitrogen tetroxide storage tank.Noncondensable gas is pumped to tail gas washing tower absorption NO through induced draft fan
xafter gas, enter exhaust gas processing device processing, reach discharging standards (NO
x≤ 200ppm) rear emptying.
The rare nitre of above-mentioned normal pressure, rare nitre and dense nitre device combination producing N pressurize
2o
4method comprise the following steps:
The first step: the rare nitre of normal pressure, rare nitre that pressurizes are combined preparation NO with dense nitre device
2gas;
concrete steps:
Ammonia oxidation gas from the rare nitric acid of normal pressure unit waste heat boiler, after fast cooler, gas cooler are cooling, is entered to just oxidizing tower, and the secondary air that the NO in gas is come by gas blower is tentatively oxidized to NO
2, oxidation ratio is up to 92%, and " 55% " nitric acid simultaneously this tower being produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, produce concentrated nitric acid for a nitre; Go out the just gas of oxidizing tower and almost all changed into NO by " 98% " Nitric Acid Oxidation of the concentrated acid storage tank from Jian Xiao workshop section in re-oxidation tower
2, and by " 75% " nitric acid being diluted, wherein approximately dissolve 15% NO
2, deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO
2gas; Re-oxidation tower top NO out
2gas enters nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after water cooler is cooling, becomes containing 30% free NO
2nitrosonitric acid, then nitrosonitric acid is delivered to the bleaching of the rare nitric acid plant bleaching tower of normal pressure, discharge NO
2gas, concentrated nitric acid is discharged at the bottom of tower, after cooling, can recycle or deliver to a nitre finished product concentrated nitric acid storage tank for nitrosonitric acid absorber portion;
Second step: prepare liquid N
2o
4;
concrete steps:
Rare normal pressure in the first step nitric acid plant bleaching tower is ejected to the pure NO coming
2gas, through preliminary cooling the removing after acid mist of watercooler, enters three grades of series connection N
2o
4condenser, is condensed into liquid nitrogen tetroxide from pressurization workshop section refrigerator group chilled brine, and is delivered to liquid nitrogen tetroxide tank;
The 3rd step: the tail gas of processing discharge;
concrete steps:
Noncondensable gas in second step is pumped to tail gas washing tower absorption NO through induced draft fan
xafter gas, enter exhaust gas processing device processing, reach discharging standards (NO
x≤ 200ppm) rear emptying.
The designed rare nitre of normal pressure of the present invention, rare nitre and dense nitre device combination producing N pressurize
2o
4method tool have the following advantages:
(1) the rare nitre of normal pressure of the present invention design, rare nitre and dense nitre device combination producing N pressurize
2o
4method, in conjunction with the dense nitre of direct method and the dense nitre process characteristic of a nitre method, make full use of the idle equipment of middle-size and small-size nitrogenous fertilizer enterprises and resource, reduce investment, shorten the construction period, realized the rare nitre of normal pressure, the liquid N of pressurize rare nitre and dense nitre device combination producing technical grade
2o
4be the rare nitre of normal pressure, rare nitric acid of producing of the rare nitre device production process of pressurizeing is for a nitre method concentrated nitric acid device, and its prepared concentrated nitric acid is oxidized for nitrogen tetroxide and absorbs, the re-oxidation tower nitric acid containing nitrogen peroxide is out delivered to pressurizing absorption tower hypomere or the bleaching of pressurization bleaching tower.
(2) the rare nitre of normal pressure of the present invention design, rare nitre and dense nitre device combination producing N pressurize
2o
4method, adopt three grades of liquid nitrogen tetroxide condensing workss of series connection, improved the produced quantity of nitrogen tetroxide.In actual production process, the strict produced quantity of controlling nitrogen tetroxide, " 55% " acid and " 75% " acid, guarantee the stable of mixture composition, change nitrogen tetroxide into industrial main products, simultaneously a certain amount of concentrated nitric acid of by-product, has improved the output of nitrogen tetroxide, meet market supply demand, reasonably change the product structure composition of enterprise, vitalized medium and small sized enterprises' existing assets, improved anti-risk ability and the market competitiveness of enterprise.
(3) the rare nitre of normal pressure of the present invention design, rare nitre and dense nitre device combination producing N pressurize
2o
4method, take the daily production management of medium and small nitrogen fertilizer factory and production technological transformation experience as foundation stone, be a maturation, prepare the liquid N of technical grade rationally, reliably
2o
4technological line, and adopt the most advanced exhaust gas processing device both at home and abroad, make atmospheric unit tail gas on the verge of being replaced reach discharging standards.
Accompanying drawing explanation
Fig. 1. the process flow sheet of the embodiment of the present invention.
Embodiment
Further illustrate the present invention below in conjunction with embodiment and accompanying drawing:
embodiment 1
The present embodiment is the concrete application of the present invention in the Chongqing fertile limited liability company of three etherealizes, and its step is as follows:
The first step: the rare nitre of normal pressure, rare nitre that pressurizes are combined preparation NO with dense nitre device
2gas;
concrete steps:
Ammonia oxidation gas from the rare nitric acid of normal pressure unit waste heat boiler, after fast cooler, gas cooler are cooling, is entered to just oxidizing tower, and the secondary air that the NO in gas is come by gas blower is tentatively oxidized to NO
2, oxidation ratio is up to 92%, and " 55% " nitric acid simultaneously this tower being produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, produce concentrated nitric acid for a nitre; Go out the just gas of oxidizing tower and almost all changed into NO by " 98% " Nitric Acid Oxidation of the concentrated acid storage tank from Jian Xiao workshop section in re-oxidation tower
2, and by " 75% " nitric acid being diluted, wherein approximately dissolve 15% NO
2, deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO
2gas; Re-oxidation tower top NO out
2gas enters nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after water cooler is cooling, becomes containing 30% free NO
2nitrosonitric acid, then nitrosonitric acid is delivered to the bleaching of the rare nitric acid plant bleaching tower of normal pressure, discharge NO
2gas, concentrated nitric acid is discharged at the bottom of tower, after cooling, can recycle or deliver to a nitre finished product concentrated nitric acid storage tank for nitrosonitric acid absorber portion;
Second step: liquid N
2o
4preparation;
concrete steps:
Rare the first step normal pressure nitric acid plant bleaching tower is ejected to the pure NO coming
2gas, through preliminary cooling the removing after acid mist of watercooler, enters three grades of series connection N
2o
4condenser, is condensed into liquid nitrogen tetroxide from pressurization workshop section refrigerator group chilled brine, and is delivered to liquid nitrogen tetroxide tank;
The 3rd step: the tail gas of processing discharge;
concrete steps:
Noncondensable gas in second step is pumped to tail gas washing tower absorption NO through induced draft fan
xafter gas, enter exhaust gas processing device processing, reach discharging standards (NO
x≤ 200ppm) rear emptying.
The present invention is in the application of the Chongqing fertile limited liability company of three etherealizes, in conjunction with the dense nitre of direct method and the dense nitre process characteristic of a nitre method, make full use of the idle equipment of middle-size and small-size nitrogenous fertilizer enterprises and resource, reduce investment, shorten the construction period, realized the rare nitre of normal pressure, the liquid N of pressurize rare nitre and dense nitre device combination producing technical grade
2o
4; Adopt the liquid nitrogen tetroxide condensing works of level series connection, improved the produced quantity of nitrogen tetroxide.In actual production process, the strict produced quantity of controlling nitrogen tetroxide, " 55% " acid and " 75% " acid, guarantee the stable of mixture composition, change nitrogen tetroxide into industrial main products, simultaneously a certain amount of concentrated nitric acid of by-product, has improved the output of nitrogen tetroxide, meet market supply demand, reasonably change the product structure composition of enterprise, vitalized medium and small sized enterprises' existing assets, improved anti-risk ability and the market competitiveness of enterprise; And adopt the most advanced exhaust gas processing device both at home and abroad, make atmospheric unit tail gas on the verge of being replaced reach discharging standards.
Claims (1)
- The rare nitre of normal pressure, rare nitre and dense nitre device combination producing N pressurize 2o 4method, it is characterized in that step is as follows:The first step: the rare nitre of normal pressure, rare nitre that pressurizes are combined preparation NO with dense nitre device 2gas:concrete steps:Ammonia oxidation gas from the rare nitric acid of normal pressure unit waste heat boiler, after fast cooler, gas cooler are cooling, is entered to just oxidizing tower, and the secondary air that the NO in gas is come by gas blower is tentatively oxidized to NO 2, oxidation ratio is up to 92%, and " 55% " nitric acid simultaneously this tower being produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, produce concentrated nitric acid for a nitre; Go out the just gas of oxidizing tower and almost all changed into NO by " 98% " Nitric Acid Oxidation of the concentrated acid storage tank from Jian Xiao workshop section in re-oxidation tower 2, and by " 75% " nitric acid being diluted, wherein approximately dissolve 15% NO 2, deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO 2gas; Re-oxidation tower top NO out 2gas enters nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after water cooler is cooling, becomes containing 30% free NO 2nitrosonitric acid, then nitrosonitric acid is delivered to the bleaching of the rare nitric acid plant bleaching tower of normal pressure, discharge NO 2gas, concentrated nitric acid is discharged at the bottom of tower, after cooling, can recycle or deliver to a nitre finished product concentrated nitric acid storage tank for nitrosonitric acid absorber portion;Second step: prepare liquid N 2o 4:concrete steps:Rare normal pressure in the first step nitric acid plant bleaching tower is ejected to the pure NO coming 2gas, through preliminary cooling the removing after acid mist of watercooler, enters three grades of series connection N 2o 4condenser, is condensed into liquid nitrogen tetroxide from pressurization workshop section refrigerator group chilled brine, and is delivered to liquid nitrogen tetroxide tank;The 3rd step: the tail gas of processing discharge:concrete steps:Noncondensable gas in second step is pumped to tail gas washing tower absorption NO through induced draft fan xafter gas, enter exhaust gas processing device processing, reaching discharging standards is NO xemptying after≤200ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210106918.5A CN102774819B (en) | 2012-04-13 | 2012-04-13 | Method for producing N2O4 (nitrogen tetroxide) through combining normal pressure diluted nitric acid, pressurized diluted nitric acid and concentrated nitric acid devices |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210106918.5A CN102774819B (en) | 2012-04-13 | 2012-04-13 | Method for producing N2O4 (nitrogen tetroxide) through combining normal pressure diluted nitric acid, pressurized diluted nitric acid and concentrated nitric acid devices |
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| Publication Number | Publication Date |
|---|---|
| CN102774819A CN102774819A (en) | 2012-11-14 |
| CN102774819B true CN102774819B (en) | 2014-05-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2547752C2 (en) * | 2012-12-18 | 2015-04-10 | Федеральное государственное унитарное предприятие "Научно-исследовательский институт машиностроения" (ФГУП "НИИМаш") | Manufacture of dinitrogen tetroxide |
| CN103496680A (en) * | 2013-10-10 | 2014-01-08 | 中国海洋石油总公司 | Preparation method of NOx gas with ultrahigh concentration and method for producing concentrated nitric acid by using NOx gas with ultrahigh concentration |
| CN103708431B (en) * | 2013-12-27 | 2015-06-10 | 安徽淮化股份有限公司 | Device for preparing nitrogen tetroxide by employing sulfuric acid method |
| CN103877838B (en) * | 2014-01-16 | 2017-08-15 | 湖北益泰药业有限公司 | A kind of method for improving the nitric acid rate of recovery in Glucurolactone production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202072473U (en) * | 2011-05-25 | 2011-12-14 | 山西阳煤丰喜肥业(集团)有限责任公司 | Device for preparing NO2 through reaction between dilute nitric acid and sodium nitrite |
| CN102341344A (en) * | 2009-03-03 | 2012-02-01 | 株式会社赛安 | High-concentration NO2 generating system and method for producing high-concentration NO2 using the generating system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102341344A (en) * | 2009-03-03 | 2012-02-01 | 株式会社赛安 | High-concentration NO2 generating system and method for producing high-concentration NO2 using the generating system |
| CN202072473U (en) * | 2011-05-25 | 2011-12-14 | 山西阳煤丰喜肥业(集团)有限责任公司 | Device for preparing NO2 through reaction between dilute nitric acid and sodium nitrite |
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