CN102774819A - 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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- CN102774819A CN102774819A CN2012101069185A CN201210106918A CN102774819A CN 102774819 A CN102774819 A CN 102774819A CN 2012101069185 A CN2012101069185 A CN 2012101069185A CN 201210106918 A CN201210106918 A CN 201210106918A CN 102774819 A CN102774819 A CN 102774819A
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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, the rare nitre of particularly a kind of normal pressure, pressurization rare nitre and dense nitre device combination producing N
2O
4Method.
Background technology
The production of present domestic nitrogen tetroxide mainly concentrates on Jiization and Huaihe Riverization, and it only is that direct method is produced the sub product in the concentrated nitric acid process, and output is minimum, if the produced quantity of increase nitrogen tetroxide, with output that has a strong impact on the finished product concentrated nitric acid and quality.Greatly expand in daily life with aerospace industry and organic fine chemical industry in recent years and use, the consumption of nitrogen tetroxide and thereupon significantly increasing, thereby press for and improve nitrogen tetroxide throughput.In addition in the industrial nitric acid production; Two pressurization nitric acid " four unifications " 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 the focus that medium and small nitrogen fertilizer factory pays close attention to gradually.An if newly-built cover 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 higherly, and the completion time of project is longer; And only as the sub product in the industrial concentrated acid production process, output is less for nitrogen tetroxide, can not meet the need of market effectively, and 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 satisfy the requirement that the chemical enterprise safety and environmental protection is produced.
Summary of the invention
The object of the invention is:
The object of the invention is exactly in order to overcome the deficiency of above-mentioned background technology, to solve and provide the rare nitre of a kind of normal pressure, the rare nitre of pressurization and dense nitre device combination producing N
2O
4Method.
The rare nitre of normal pressure involved in the present invention, the rare nitre of pressurization and dense nitre device combination producing N
2O
4Method flow following:
After fast cooler, gas cooler cooling, get into oxidizing tower just from the ammonia oxidation gas of the rare nitric acid of normal pressure unit waste heat boiler, the NO in the gas tentatively is oxidized to NO by the secondary air that gas blower comes
2(oxidation ratio is up to 92%), " 55% " nitric acid that simultaneously this tower is produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, is used for a nitre and produces a concentrated nitric acid.Go out just the gas of oxidizing tower almost all is oxidized to NO by " 98% " nitric acid (from the concentrated acid storage tank of a nitre workshop section) in the re-oxidation tower
2, and diluted " 75% " nitric acid (dissolved about 15% NO
2), deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO
2Gas.The NO that the re-oxidation cat head comes out
2Gas gets into the nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after the water cooler cooling, become to contain 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 supply the nitrosonitric acid absorber portion to recycle or deliver to a nitre finished product concentrated nitric acid storage tank.Bleaching tower ejects next pure NO
2Gas gets into N after acid mist is removed in the preliminary cooling of watercooler
2O
4Condensing surface is frozen salt solution (coming the freezing unit of self-pressurization workshop section) and is condensed into liquid nitrogen tetroxide, and delivers to liquid nitrogen tetroxide storage tank.Noncondensable gas is pumped to tail gas washing tower absorption of N O through induced draft fan
XBehind the gas, get into exhaust gas processing device and handle, reach discharging standards (NO
X≤200ppm) back emptying.
The rare nitre of above-mentioned normal pressure, the rare nitre of pressurization and dense nitre device combination producing N
2O
4Method may further comprise the steps:
The first step: the rare nitre of normal pressure, the rare nitre of pressurization and dense nitre device coproduce NO
2Gas;
Concrete steps:
To from the ammonia oxidation gas of the rare nitric acid of normal pressure unit waste heat boiler after fast cooler, gas cooler cooling, get into oxidizing tower just, the NO in the gas tentatively is oxidized to NO by the secondary air that gas blower comes
2, oxidation ratio is up to 92%, and " 55% " nitric acid that simultaneously this tower is produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, is used for a nitre and produces a concentrated nitric acid; The gas that goes out first oxidizing tower is almost all become NO by " 98% " nitric acid oxidation from the concentrated acid storage tank of a nitre workshop section in the re-oxidation tower
2, and, wherein dissolve 15% NO approximately with diluted " 75% " nitric acid
2, deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO
2Gas; The NO that the re-oxidation cat head comes out
2Gas gets into the nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after the water cooler cooling, become to contain 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 supply the nitrosonitric acid absorber portion to recycle or deliver to a nitre finished product concentrated nitric acid storage tank;
Second step: prepare liquid N
2O
4
Concrete steps:
The rare nitric acid plant bleaching tower of normal pressure in the first step is ejected next pure NO
2Gas gets into three grades of series connection N after acid mist is removed in the preliminary cooling of watercooler
2O
4Condensing surface is come the freezing unit chilled brine of self-pressurization workshop section to be condensed into liquid nitrogen tetroxide, and is delivered to liquid nitrogen tetroxide jar;
The 3rd step: handle discharge tail gas;
Concrete steps:
Noncondensable gas in second step is pumped to tail gas washing tower absorption of N O through induced draft fan
XBehind the gas, get into exhaust gas processing device and handle, reach discharging standards (NO
X≤200ppm) back emptying.
The rare nitre of the normal pressure that the present invention designed, the rare nitre of pressurization and dense nitre device combination producing N
2O
4Method have following advantage:
(1) the rare nitre of normal pressure of the present invention's design, the rare nitre of pressurization and dense nitre device combination producing N
2O
4Method; In conjunction with dense nitre of direct method and the dense nitre process characteristic of a nitre method, make full use of middle-size and small-size nitrogenous fertilizer enterprises idle equipment and resource, reduced investment; Shorten the construction period, realized the liquid N of the rare nitre of normal pressure, the rare nitre of pressurization and dense nitre device combination producing technical grade
2O
4Be that rare nitric acid that the rare nitre of normal pressure, the rare nitre device production process of pressurization produce is used for a nitre method concentrated nitric acid device; And the concentrated nitric acid that it is prepared is used for nitrogen tetroxide oxidation and absorption, and the nitric acid that contains nitrogen peroxide that the re-oxidation tower comes out is delivered to pressurizing absorption tower hypomere or the bleaching of pressurization bleaching tower.
(2) the rare nitre of normal pressure of the present invention's design, the rare nitre of pressurization and dense nitre device combination producing N
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 produced quantity of strict control nitrogen tetroxide, " 55% " acid and " 75% " acid guarantees the stable of mixture composition; Change nitrogen tetroxide into industrial main products, a certain amount of concentrated nitric acid of by-product has simultaneously improved the output of nitrogen tetroxide; Satisfied the market supply demand; Reasonably change the products structure composition, vitalized medium and small sized enterprises' existing assets, improved the anti-risk ability and the market competitiveness of enterprise.
(3) the rare nitre of normal pressure of the present invention's design, the rare nitre of pressurization and dense nitre device combination producing N
2O
4Method, be foundation stone with daily production management of medium and small nitrogen fertilizer factory and production technological transformation experience, 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.
Description of drawings
Fig. 1. the process flow sheet of the embodiment of the invention.
Embodiment
Further specify the present invention below in conjunction with embodiment and accompanying drawing:
Embodiment 1
Present embodiment is the concrete application of the present invention fertile Ltd of three etherealizes in Chongqing, and its step is following:
The first step: the rare nitre of normal pressure, the rare nitre of pressurization and dense nitre device coproduce NO
2Gas;
Concrete steps:
To from the ammonia oxidation gas of the rare nitric acid of normal pressure unit waste heat boiler after fast cooler, gas cooler cooling, get into oxidizing tower just, the NO in the gas tentatively is oxidized to NO by the secondary air that gas blower comes
2, oxidation ratio is up to 92%, and " 55% " nitric acid that simultaneously this tower is produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, is used for a nitre and produces a concentrated nitric acid; The gas that goes out first oxidizing tower is almost all become NO by " 98% " nitric acid oxidation from the concentrated acid storage tank of a nitre workshop section in the re-oxidation tower
2, and, wherein dissolve 15% NO approximately with diluted " 75% " nitric acid
2, deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO
2Gas; The NO that the re-oxidation cat head comes out
2Gas gets into the nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after the water cooler cooling, become to contain 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 supply the nitrosonitric acid absorber portion to recycle or deliver to a nitre finished product concentrated nitric acid storage tank;
Second step: liquid N
2O
4Preparation;
Concrete steps:
The rare nitric acid plant bleaching tower of the first step normal pressure is ejected next pure NO
2Gas gets into three grades of series connection N after acid mist is removed in the preliminary cooling of watercooler
2O
4Condensing surface is come the freezing unit chilled brine of self-pressurization workshop section to be condensed into liquid nitrogen tetroxide, and is delivered to liquid nitrogen tetroxide jar;
The 3rd step: handle discharge tail gas;
Concrete steps:
Noncondensable gas in second step is pumped to tail gas washing tower absorption of N O through induced draft fan
XBehind the gas, get into exhaust gas processing device and handle, reach discharging standards (NO
X≤200ppm) back emptying.
The application of the present invention fertile Ltd of three etherealizes in Chongqing; In conjunction with dense nitre of direct method and the dense nitre process characteristic of a nitre method; Make full use of middle-size and small-size nitrogenous fertilizer enterprises idle equipment and resource; Reduce investment, shortened the construction period, realized the liquid N of the rare nitre of normal pressure, the rare nitre of pressurization and dense nitre device combination producing technical grade
2O
4Adopt the liquid nitrogen tetroxide condensing works of level series connection, improved the produced quantity of nitrogen tetroxide.In actual production process, the produced quantity of strict control nitrogen tetroxide, " 55% " acid and " 75% " acid guarantees the stable of mixture composition; Change nitrogen tetroxide into industrial main products, a certain amount of concentrated nitric acid of by-product has simultaneously improved the output of nitrogen tetroxide; Satisfied the market supply demand; Reasonably change the products structure composition, vitalized medium and small sized enterprises' existing assets, improved the 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)
1. the rare nitre of normal pressure, the rare nitre of pressurization and dense nitre device combination producing N
2O
4Method, it is characterized in that step is following:
The first step: the rare nitre of normal pressure, the rare nitre of pressurization and dense nitre device coproduce NO
2Gas:
Concrete steps:
To from the ammonia oxidation gas of the rare nitric acid of normal pressure unit waste heat boiler after fast cooler, gas cooler cooling, get into oxidizing tower just, the NO in the gas tentatively is oxidized to NO by the secondary air that gas blower comes
2, oxidation ratio is up to 92%, and " 55% " nitric acid that simultaneously this tower is produced is delivered to the diluted acid storage tank of pressurization nitric acid workshop section with force (forcing) pump, is used for a nitre and produces a concentrated nitric acid; The gas that goes out first oxidizing tower is almost all become NO by " 98% " nitric acid oxidation from the concentrated acid storage tank of a nitre workshop section in the re-oxidation tower
2, and, wherein dissolve 15% NO approximately with diluted " 75% " nitric acid
2, deliver to the rare nitric acid plant bleaching tower hypomere of pressurization and reclaim NO
2Gas; The NO that the re-oxidation cat head comes out
2Gas gets into the nitrosonitric acid absorption tower and is absorbed by " 98% " nitric acid after the water cooler cooling, become to contain 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 supply the nitrosonitric acid absorber portion to recycle or deliver to a nitre finished product concentrated nitric acid storage tank;
Second step: prepare liquid N
2O
4:
Concrete steps:
The rare nitric acid plant bleaching tower of normal pressure in the first step is ejected next pure NO
2Gas gets into three grades of series connection N after acid mist is removed in the preliminary cooling of watercooler
2O
4Condensing surface is come the freezing unit chilled brine of self-pressurization workshop section to be condensed into liquid nitrogen tetroxide, and is delivered to liquid nitrogen tetroxide jar;
The 3rd step: handle discharge tail gas:
Concrete steps:
Noncondensable gas in second step is pumped to tail gas washing tower absorption of N O through induced draft fan
XBehind the gas, get into exhaust gas processing device and handle, reach discharging standards (NO
X≤200ppm) back emptying.
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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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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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CN102774819A true CN102774819A (en) | 2012-11-14 |
CN102774819B CN102774819B (en) | 2014-05-28 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN103708431A (en) * | 2013-12-27 | 2014-04-09 | 安徽淮化股份有限公司 | Device for preparing nitrogen tetroxide by employing sulfuric acid method |
CN103877838A (en) * | 2014-01-16 | 2014-06-25 | 湖北益泰药业有限公司 | Method for improving recovery rate of nitric acid in glucurolactone production |
RU2547752C2 (en) * | 2012-12-18 | 2015-04-10 | Федеральное государственное унитарное предприятие "Научно-исследовательский институт машиностроения" (ФГУП "НИИМаш") | Manufacture of dinitrogen tetroxide |
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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 generating high concentration NO2 using the generating system |
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2012
- 2012-04-13 CN CN201210106918.5A patent/CN102774819B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102341344A (en) * | 2009-03-03 | 2012-02-01 | 株式会社赛安 | high concentration NO2 generating system and method for generating 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 |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN103708431A (en) * | 2013-12-27 | 2014-04-09 | 安徽淮化股份有限公司 | Device for preparing nitrogen tetroxide by employing sulfuric acid method |
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 |
CN103877838A (en) * | 2014-01-16 | 2014-06-25 | 湖北益泰药业有限公司 | Method for improving recovery rate of nitric acid in glucurolactone production |
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 |
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