CN102583441B - Method for producing ammonium nitrate solid - Google Patents
Method for producing ammonium nitrate solid Download PDFInfo
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- CN102583441B CN102583441B CN 201210011710 CN201210011710A CN102583441B CN 102583441 B CN102583441 B CN 102583441B CN 201210011710 CN201210011710 CN 201210011710 CN 201210011710 A CN201210011710 A CN 201210011710A CN 102583441 B CN102583441 B CN 102583441B
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Abstract
The invention relates to a method for producing ammonium nitrate solid. Concentrated nitric acid and ammonia gas are introduced into a reaction tower of a tower reactor, with the weight flow ratio being 3.7-5.3:1, specifically, concentrated nitric acid is introduced into a spraying device arranged at the top of the reaction tower, ammonia gas is introduced to the reaction tower through an annular distributor in the middle of the reaction tower, the spraying device is adjusted to enable concentrated nitric acid to be sprayed into fine concentrated nitric acid drops at the top of the reaction tower through the spraying device, the concentrated nitric acid drops contact the ascending normal-pressure ammonia gas in the reaction tower during the falling process to react and generate ammonium nitrate solution fine droplets, the reaction temperature is controlled between 150 to 190 DEG C, moisture in the ammonium nitrate solution is vaporized through heat generated by reaction, vapor-solid separation can be achieved in the reaction tower, and the ammonium nitrate particles, namely the ammonium nitrate solid can be directly prepared. According to the method, reaction flow and reaction time can be reduced, the time of materials retaining in a system can be reduced, the energy is saved and the operating steps are simple and safe.
Description
Technical field
The present invention relates to a kind of production method of ammonium nitrate, be a kind of method of production ammonium nitrate solid, particularly single stage method nitric acid synthesis ammonium solid energy-saving production method belongs to the nitrate technical field.
Background technology
Ammonium nitrate is a kind of application Chemicals very widely, mainly as fertilizer and industrial and military explosive.And can be used for sterilant, refrigerant, nitrogen oxide absorption agent, make laughing gas, pyrotechnics etc.Its main preparation methods is that nitric acid and ammonia gas react make.Very violent chemical reaction can take place in nitric acid and ammonia, generates ammonium nitrate, emits a large amount of heats simultaneously.The temperature that reactive system raises and the concentration of nitric acid have confidential relation, and the concentration of nitric acid of use is high more, and it is strong then to react Shaoxing opera, and system's temperature rise is high more.The reaction of initial ammonium nitrate production is the normal pressure neutralisation, the heat that produces in the reaction process promptly under normal pressure, in reactor, carries out the neutralization reaction of nitric acid and ammonia, owing to can not in time be removed, so it is lower to participate in the concentration of nitric acid of reaction, be generally 45% ~ 55%, what obtain is the solution of ammonium nitrate, simultaneously, the normal pressure corrosion reaction in reaction process, produce in and vapor temperature lower, recycle to be worth, can not to be used for preparing ammonium nitrate solid, caused the loss of energy.The tubular reactor of development in recent years promptly under pressurized state, allows nitric acid and ammonia be passed in certain proportion in the less pipeline of one section diameter and reacts, and generates ammonium nitrate.Its advantage is to use the nitric acid of higher concentration (58% ~ 60%), and in can utilizing and the time part heat that produces.But the ammonium nitrate solution that remains higher concentration that obtains can't directly obtain ammonium nitrate solid.CN101633510A discloses a kind of industrial liquid ammonium nitrate and method for making and application, and described liquid ammonium nitrate is an ammonium nitrate solution, and the content of ammonium nitrate is 70～96%, and comprises per-cent greater than 10% water.This technology does not provide concrete guidance program for how production ammonium nitrate solid of the present invention.
Summary of the invention
Technical problem to be solved by this invention is, a kind of method of production ammonium nitrate solid is provided, and this method can shorten reaction process, reduces the reaction times, reduces the residence time of material in system, and is energy-conservation, and operation steps is simple and safe.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of method of production ammonium nitrate solid (or perhaps method of production solid ammonium nitrate), its technical scheme is that it is to make ammonium nitrate solid by the following method: feed concentrated nitric acid and ammonia in the reaction tower of tower reactor, the ratio of the weight rate of concentrated nitric acid and ammonia (mass rate) is 3.7 ~ 5.3:1, it specifically is the spraying plant that concentrated nitric acid is fed the top that is installed in reaction tower, simultaneously the middle part of ammonia from reaction tower fed the reaction tower by circle distributor, regulate spraying plant, make concentrated nitric acid become trickle concentrated nitric acid drop at the reaction tower top spray through spraying plant, described concentrated nitric acid drop carries out contact reacts with the normal pressure ammonia that rises in the dropping process and generates the trickle liquid pearl of ammonium nitrate solution in reaction tower, control reaction temperature is between 150 ~ 190 ℃, utilizing reaction to generate heat vaporizes the moisture in the ammonium nitrate solution, finish vapour and separate admittedly in reaction tower, directly preparing ammonium nitrate granule is ammonium nitrate solid.
In the technique scheme, the diameter of the reaction tower of described tower reactor is preferably between 3 ~ 5 meters, and the height of reaction tower is preferably between 20 ~ 25 meters.It is 80% ~ 98% concentrated nitric acid that above-mentioned concentrated nitric acid is preferably massfraction.The above-mentioned concentrated nitric acid and ammonia and control reaction temperature of feeding in the reaction tower of tower reactor preferably leans on temperature and flow linkage system to realize, the interior hygrosensor of reaction tower that described temperature and flow linkage system preferably have first solenoid electric valve, first flow determinator, second solenoid electric valve, second flow measuring instrument, the computer controller of the reaction tower outside that is installed on tower reactor and be installed on tower reactor; Above-mentioned spraying plant is equipped with the first flow determinator by pipe connection first solenoid electric valve on the pipeline between first solenoid electric valve and the spraying plant; Above-mentioned circle distributor is equipped with second flow measuring instrument by pipe connection second solenoid electric valve on the pipeline between second solenoid electric valve and the circle distributor, hygrosensor is installed between spraying plant and the circle distributor; First solenoid electric valve, first flow determinator, second solenoid electric valve, second flow measuring instrument, hygrosensor all are provided with the computer controller control linkage.Above-mentioned concentrated nitric acid is squeezed into (being delivered in other words conj.or perhaps) spraying plant through topping-up pump (force (forcing) pump), first solenoid electric valve, first flow determinator.
The present invention is that a kind of spraying plant that utilizes is sprayed into concentrated nitric acid trickle droplet, generates the method for ammonium nitrate with the normal pressure ammonia gas react in tower reactor, the heat that it utilizes reaction to generate, moisture is vaporized, drying products, reach vapour in the process that material is descended and separate admittedly in reaction tower, directly prepare ammonium nitrate granule and crystallization.The invention belongs to nitric acid synthesis ammonium solid preparation method, this method is the tower reaction nitric acid synthesis of a normal pressure ammonium, with pipe reaction nitric acid synthesis ammonium technology reduced in comparison reaction process, can reduce by reaction times of 20%, reduced the residence time of material in system.Therefore this technical superiority is embodied on the energy-saving effect, and is more energy-conservation 60 ~ 70% than traditional technology, and is synthesis under normal pressure in the production process, and safety coefficient in the production process and product quality are also corresponding to be improved.This technology does not increase investment in fixed assets, and can reduce the production run expense.Energy-saving effect of the present invention is obvious, the content of the ammonium nitrate of production 〉=99.5%, and every index all can reach the standard of premium grads among the GB2945-1989 " ammonium nitrate ".This method operation steps is simple and safe, has advantages such as the equipment input is little, economical and efficient.
Description of drawings
The structural representation that Fig. 1 is connected with the flow linkage system for tower reactor among the present invention and temperature.
Embodiment
Embodiment 1: with reference to Fig. 1, its tip position is equipped with spraying plant 9 in the reaction tower of tower reactor 2, its medium position is equipped with circle distributor 11 in the reaction tower, this circle distributor is (conveying ammonia) circulating line, and described circulating line is evenly distributed with a plurality of ventilating pits (hole that ammonia passes through) along its circumferential direction.The bottom of reaction tower has discharge hole 1, and the top of reaction tower has cat head passage 8.This tower reactor is the spray column reactor, and its structure is originally as prior art.
The present invention is (reaction formula is the face as follows) that makes ammonium nitrate solid by the following method:
In the reaction tower of tower reactor, feed concentrated nitric acid and ammonia, the ratio of the weight rate of concentrated nitric acid and ammonia is 4:1, it specifically is the spraying plant that concentrated nitric acid is fed the top that is installed in reaction tower, simultaneously the middle part of ammonia from reaction tower fed the reaction tower by circle distributor, regulate spraying plant (air-flow back-blowing device), make concentrated nitric acid become trickle concentrated nitric acid drop (fine drop) at the reaction tower top spray through spraying plant, described concentrated nitric acid drop carries out contact reacts with the normal pressure ammonia that rises in the dropping process and generates the trickle liquid pearl of ammonium nitrate solution (reaction pressure is a normal pressure) in reaction tower, control reaction temperature is between 170 ~ 190 ℃, utilizing reaction to generate heat vaporizes the moisture in the ammonium nitrate solution, finish vapour and separate admittedly in reaction tower, directly preparing ammonium nitrate granule is ammonium nitrate solid (ammonium nitrate of generation drop to the reaction tower bottom with solid form).The diameter of the reaction tower of above-mentioned tower reactor is preferably between 3 ~ 5 meters, and the height of reaction tower is preferably between 20 ~ 25 meters.Above-mentioned concentrated nitric acid is that massfraction is 80% ~ 98% concentrated nitric acid.
The above-mentioned nitric acid and ammonia and control reaction temperature of feeding in the reaction tower of tower reactor preferably leans on temperature and flow linkage system to realize, with reference to Fig. 1, the interior hygrosensor 10 of reaction tower that described temperature and flow linkage system have first solenoid electric valve 6, (long-range) first flow determinator 7, second solenoid electric valve 4, (long-range) second flow measuring instrument 3, the computer controller (programmable logic controller PLC) 5 of the reaction tower outside that is installed on tower reactor and be installed on tower reactor; Above-mentioned spraying plant 9 is by being equipped with first flow determinator 7 on the pipeline between pipe connection first solenoid electric valve, 6, the first solenoid electric valves 6 and the spraying plant 9; Above-mentioned circle distributor 11 is by being equipped with second flow measuring instrument 3 on the pipeline between pipe connection second solenoid electric valve, 4, the second solenoid electric valves 4 and the circle distributor 11, and hygrosensor 10 is installed between spraying plant 9 and the circle distributor 11; First solenoid electric valve 6, first flow determinator 7, second solenoid electric valve 4, second flow measuring instrument 3, hygrosensor 10 all with computer controller 5 control linkage settings, be that the signal output part of first flow determinator 7, the signal output part of second flow measuring instrument 3, the signal output part of hygrosensor 10 all are connected with the signal input part of computer controller 5, the signal output part of computer controller 5 is connected with the signal input part of first solenoid electric valve 6 and the signal input part of second solenoid electric valve 4 respectively.Each parts of described temperature and flow linkage system are originally as prior art.(can be that massfraction is 80% concentrated nitric acid with concentrated nitric acid during work, concentration is 80% concentrated nitric acid in other words conj.or perhaps) through topping-up pump (not drawing among the figure), first solenoid electric valve 6 and first flow determinator 7, squeeze into spraying plant 9 with the flow of 690kg/min, regulate spraying plant (control method is a prior art), make concentrated nitric acid through spraying plant 9(at the reaction tower top spray) form tiny concentrated nitric acid drop (the little liquid pearl of concentrated nitric acid).Simultaneously ammonia is by second solenoid electric valve 4 and second flow measuring instrument 3, enters in the reaction tower by circle distributor (promptly carrying the ammonia circulating line) 11 with the flow of 150kg/min.Described (tiny) concentrated nitric acid drop falls in reaction tower and carries out contact reacts with the normal pressure ammonia that rises in (landing) process and generate the trickle liquid pearl of ammonium nitrate solution (tiny liquid pearl), utilization is installed in the hygrosensor 10 between circle distributor 11 and the spraying plant 9, reconcile first solenoid electric valve 6 and second solenoid electric valve 4 by computer controller 5, according to the time variable control concentrated nitric acid that configures and the flow of ammonia, general dominant discharge is than being the 5.3:1(weight ratio).By reconciling flow, control reaction tower interior reaction temperature is at 180 ± 10 ℃.Specifically be to cross when low when temperature in the reaction tower, first solenoid electric valve 6 of temperature and flow linkage system and second solenoid electric valve 4 are opened and are increased, when temperature was too high in the reaction tower, first solenoid electric valve 6 and second solenoid electric valve 4 were opened and are reduced that (ratio of the weight rate of concentrated nitric acid and ammonia is 3.7 ~ 5.3:1).Reaction generates big calorimetric, and with the vaporization of the moisture in the ammonium nitrate solution (evaporation), (separating out) ammonium nitrate of generation drop to the reaction tower bottom with solid form, is emitted by discharge hole 1, obtains the ammonium nitrate finished product.Gas (steam) is discharged from cat head passage 8, after separator is isolated the entrained solid material, and after three grades of graphite falling film absorbers (graphite falling film absorption device) absorb, the tail gas high altitude discharge.
Embodiment 2: the present invention is (reaction formula is the face as follows) that makes ammonium nitrate solid by the following method: feed concentrated nitric acid and ammonia in the reaction tower of tower reactor, the ratio of the weight rate of concentrated nitric acid and ammonia is 5:1 or 5.2:1 or 4.7:1 or 3.7:1, it specifically is the spraying plant that concentrated nitric acid is fed the top that is installed in reaction tower, simultaneously the middle part of ammonia from reaction tower fed the reaction tower by circle distributor, regulate spraying plant, make concentrated nitric acid become trickle concentrated nitric acid drop at the reaction tower top spray through spraying plant, described concentrated nitric acid drop carries out contact reacts with the normal pressure ammonia that rises in the dropping process and generates the trickle liquid pearl of ammonium nitrate solution in reaction tower, control reaction temperature is between 150 ~ 160 ℃, utilizing reaction to generate heat vaporizes the moisture in the ammonium nitrate solution, finish vapour and separate admittedly in reaction tower, directly preparing ammonium nitrate granule is ammonium nitrate solid.The diameter of the reaction tower of above-mentioned tower reactor can be 4 meters, and the height of reaction tower can be 25 meters.Above-mentioned concentrated nitric acid can be 85%, 90%, 95%, 98% concentrated nitric acid for massfraction.During work with concentrated nitric acid through topping-up pump (not drawing among the figure), first solenoid electric valve 6 and first flow determinator 7, squeeze into spraying plant 9 with the flow of 600kg/min, regulate spraying plant (control method is a prior art), make concentrated nitric acid through spraying plant 9(at the reaction tower top spray) form tiny concentrated nitric acid drop (the little liquid pearl of concentrated nitric acid).Simultaneously ammonia is by second solenoid electric valve 4 and second flow measuring instrument 3, enters in the reaction tower by circle distributor (promptly carrying the ammonia circulating line) 11 with the flow of 120kg/min.The flow of above-mentioned concentrated nitric acid and its numerical value of the flow of ammonia can change, and other technical characterictic of present embodiment can be with reference to embodiment 1.
More than its content of ammonium nitrate of obtaining among each embodiment can reach the standard of GB2945-89 " ammonium nitrate " premium grads.This method technology is simple, and equipment drops into little, economical and efficient.
Above embodiment is used to further specify the present invention, but does not limit the present invention in any form.
Claims (4)
1. method of producing ammonium nitrate solid, it is characterized in that it is to make ammonium nitrate solid by the following method: in the reaction tower of tower reactor, feed concentrated nitric acid and ammonia, the ratio of the weight rate of concentrated nitric acid and ammonia is 3.7 ~ 5.3:1, above-mentioned concentrated nitric acid is that massfraction is 80% ~ 98% concentrated nitric acid, it specifically is the spraying plant that concentrated nitric acid is fed the top that is installed in reaction tower, simultaneously the middle part of ammonia from reaction tower fed the reaction tower by circle distributor, regulate spraying plant, make concentrated nitric acid become trickle concentrated nitric acid drop at the reaction tower top spray through spraying plant, described concentrated nitric acid drop carries out contact reacts with the normal pressure ammonia that rises in the dropping process and generates the trickle liquid pearl of ammonium nitrate solution in reaction tower, control reaction temperature is between 150 ~ 190 ℃, utilizing reaction to generate heat vaporizes the moisture in the ammonium nitrate solution, finish vapour and separate admittedly in reaction tower, directly preparing ammonium nitrate granule is ammonium nitrate solid.
2. the method for production ammonium nitrate solid according to claim 1, the diameter of reaction tower that it is characterized in that above-mentioned tower reactor is between 3 ~ 5 meters, and the height of reaction tower is between 20 ~ 25 meters.
3. the method for production ammonium nitrate solid according to claim 1, it is characterized in that the above-mentioned concentrated nitric acid and ammonia and control reaction temperature of in the reaction tower of tower reactor, feeding by temperature and the realization of flow linkage system, the interior hygrosensor (10) of reaction tower that described temperature and flow linkage system have first solenoid electric valve (6), first flow determinator (7), second solenoid electric valve (4), second flow measuring instrument (3), the computer controller (5) of the reaction tower outside that is installed on tower reactor and be installed on tower reactor; Above-mentioned spraying plant (9) is equipped with first flow determinator (7) by pipe connection first solenoid electric valve (6) on the pipeline between first solenoid electric valve (6) and the spraying plant (9); Above-mentioned circle distributor (11) is by pipe connection second solenoid electric valve (4), on the pipeline between second solenoid electric valve (4) and the circle distributor (11) second flow measuring instrument (3) is installed, hygrosensor (10) is installed between spraying plant (9) and the circle distributor (11); First solenoid electric valve (6), first flow determinator (7), second solenoid electric valve (4), second flow measuring instrument (3), hygrosensor (10) all with computer controller (5) control linkage setting.
4. the method for production ammonium nitrate solid according to claim 3 is characterized in that above-mentioned concentrated nitric acid is through topping-up pump, first solenoid electric valve (6), first flow determinator (7) and squeeze into spraying plant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201210011710 CN102583441B (en) | 2012-01-16 | 2012-01-16 | Method for producing ammonium nitrate solid |
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| CN 201210011710 CN102583441B (en) | 2012-01-16 | 2012-01-16 | Method for producing ammonium nitrate solid |
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| CN102583441B true CN102583441B (en) | 2013-07-24 |
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| CN110845053B (en) * | 2019-10-28 | 2021-06-01 | 宿州伊维特新材料有限公司 | Method for recycling nitrous oxide pre-washing water |
| CN112661185A (en) * | 2021-01-13 | 2021-04-16 | 安徽理工大学环境友好材料与职业健康研究院(芜湖) | Preparation method of niobate nanotube with one-dimensional tubular structure |
| CN114315491B (en) * | 2022-01-18 | 2022-09-09 | 湖北东神天神实业有限公司 | Method for preparing powdery ammonium nitrate fuel oil explosive and product thereof |
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| US4221770A (en) * | 1978-08-21 | 1980-09-09 | Gulf Oil Corporation | Ammonium nitrate particulate abatement process |
| CN100360407C (en) * | 2006-07-03 | 2008-01-09 | 化学工业第二设计院 | Method for producing ammonium nitrate |
| CN1907856A (en) * | 2006-07-12 | 2007-02-07 | 太原海力丰科技发展有限公司 | Method for preparing concentration liquid of ammonium nitrate |
| CN101531381B (en) * | 2009-04-23 | 2010-11-03 | 四川金圣赛瑞化工有限责任公司 | Method for producing ammonium nitrate by ammonium-containing waste gas |
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