CN111807338A - Novel concentrated nitric acid production system by magnesium nitrate method - Google Patents

Novel concentrated nitric acid production system by magnesium nitrate method Download PDF

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Publication number
CN111807338A
CN111807338A CN202010663020.2A CN202010663020A CN111807338A CN 111807338 A CN111807338 A CN 111807338A CN 202010663020 A CN202010663020 A CN 202010663020A CN 111807338 A CN111807338 A CN 111807338A
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nitric acid
tower
magnesium nitrate
tail gas
dilute
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孙立辉
刘文利
宋云忠
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Ji'nan Double Nitrate Technology Development Co ltd
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Ji'nan Double Nitrate Technology Development Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/20Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
    • C01B21/38Nitric acid
    • C01B21/42Preparation from nitrates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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Abstract

The invention belongs to the technical field of chemical industry, and particularly relates to a novel concentrated nitric acid production system by a magnesium nitrate method, which comprises a nitric acid concentration tower and a bleaching tower; the dispersers positioned at the top of the nitric acid concentration tower and the top of the bleaching tower are both groove-type dispersers, the shower aperture of the disperser at the top of the nitric acid concentration tower is 6mm, and the shower aperture of the disperser at the top of the bleaching tower is 4 mm; the specifications of two tower sections of the nitric acid concentration tower are as follows
Figure DDA0002579327100000011
A height of 15300 mm; compared with the traditional disperser with a disc structure, the novel magnesium nitrate method concentrated nitric acid production system provided by the invention can increase the sprinkling density, avoid the generation of column flow during sprinkling, increase the gas-liquid contact area, improve the mass transfer and heat transfer between gas and liquid, and reduce the nitrate content of dilute magnesium nitrate; compared with the traditional tower section specification
Figure DDA0002579327100000012
And the height of the nitric acid concentration tower is 14900mm, the invention improvesThe rectification height of the concentrated nitric acid is improved to stabilize the concentration of the finished product acid to be more than 98.2% (w/w), and meanwhile, the denitration height is increased, and the nitrate content in the dilute magnesium nitrate is reduced.

Description

Novel concentrated nitric acid production system by magnesium nitrate method
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a novel concentrated nitric acid production system by a magnesium nitrate method.
Background
The concentrated sulfuric acid production process by using magnesium nitrate method is a process for preparing concentrated nitric acid (its concentration is above 97.2% (w/w)) by using magnesium nitrate solution as dehydrating agent to make rectification of dilute nitric acid. However, the concentration of the concentrated nitric acid produced by the existing production process of concentrated sulfuric acid by a magnesium nitrate method fluctuates between 97.2 percent and 98.5 percent (w/w), and cannot be stabilized above 98.2 percent (w/w); the nitrate content fluctuates between 0.2 and 1.0 percent (w/w), and can not be stabilized below 0.5 percent (w/w), so that the long-term requirements of customers with the concentration above 98.2 percent (w/w) and the nitrate content below 0.5 percent (w/w) can not be met.
In the production process, the content of dilute magnesium nitrate is 0.2-0.3% (w/w), and the dilute magnesium nitrate has high content of nitrate, so that the corrosion of a magnesium nitrate heater is serious, and the magnesium nitrate heater needs to be replaced in 3-4 years, so that the production cost is increased; magnesium tail water containing 2-3% (w/w) of nitric acid generated in production is sent into a neutralization pond, 30% (w/w) of liquid sodium hydroxide is sent to a factory tail end water treatment device for retreatment after being preliminarily neutralized and qualified, and is discharged after being qualified, and some enterprises with dilute nitric acid devices are transformed to send part of the magnesium tail water to a dilute nitric acid device absorption tower as an absorbent, so that the treatment capacity of the magnesium tail water is reduced, but a large amount of magnesium tail water still needs neutralization treatment, and the neutralization treatment of the magnesium tail water not only causes environmental pollution, but also increases the production cost; the nitrogen oxide exhaust gas generated in the production and the trace nitrogen oxide gas discharged from the high altitude of each tank pollute the environment.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a novel magnesium nitrate method concentrated nitric acid production system.
In order to achieve the purpose, the invention adopts the following technical scheme:
a novel concentrated nitric acid production system by a magnesium nitrate method comprises a nitric acid concentration tower and a bleaching tower; the dispersers positioned at the top of the nitric acid concentration tower and the top of the bleaching tower are both groove-type dispersers, the shower aperture of the disperser at the top of the nitric acid concentration tower is 6mm, and the shower aperture of the disperser at the top of the bleaching tower is 4 mm;
the specifications of two tower sections of the nitric acid concentration tower are as follows
Figure BDA0002579327080000011
The height is 15300 mm.
Preferably, ceramic regular packing is arranged in the nitric acid concentration tower and the bleaching tower.
Preferably, a tetrafluoro rod is arranged in a gap between each layer of the ceramic regular packing and the tower wall of the nitric acid concentration tower and the bleaching tower for plugging.
Preferably, the novel system for producing the concentrated nitric acid by the magnesium nitrate method further comprises a dilute magnesium nitrate evaporator and an indirect condenser, a magnesium tail water rectifying tower is arranged between the dilute magnesium nitrate evaporator and the indirect condenser, the concentration of the magnesium tail water is reduced to 0.1% (w/w) from 2-3% (w/w), then the magnesium tail water is sent to an ion exchange bed to be treated to be neutral, and meanwhile, the by-product dilute nitric acid is sent to a dilute nitric acid storage tank for concentration.
Preferably, the novel magnesium nitrate method concentrated nitric acid production system further comprises a hydrogen peroxide tank and a tail gas absorption tower; the hydrogen peroxide tank is connected to the top of the tail gas absorption tower through a hydrogen peroxide pump;
the bottom of tail gas absorption tower is connected to the second dilute nitric acid tank through a pipeline, the second dilute nitric acid tank is connected to the cooler through an acid water pump, the cooler is connected to the tail gas absorption tower through a pipeline, the top of the tail gas absorption tower is connected to the tail gas ejector through a pipeline, the tail gas ejector is connected to the tail gas circulating water tank, and the tail gas circulating water tank is connected to the tail gas ejector through a tail gas circulating water pump.
Compared with the prior art, the invention has the following technical effects:
1. in the novel system for producing concentrated nitric acid by a magnesium nitrate method, dispersers positioned at the top of a nitric acid concentration tower and the top of a bleaching tower are arranged in a groove mode, the spraying aperture of the disperser at the top of the nitric acid concentration tower is 6mm, and the spraying aperture of the disperser at the top of the bleaching tower is 4 mm; compared with the traditional disc structure, the spraying density of the nitric acid concentration tower and the bleaching tower can be effectively increased, the generation of column flow during spraying is avoided, the gas-liquid contact area is increased, the mass transfer and heat transfer between gas and liquid are improved, and the nitrate content of dilute magnesium nitrate is reduced;
the specifications of two tower sections of the nitric acid concentration tower are as follows
Figure BDA0002579327080000021
A height of 15300 mm; compared with the traditional tower section specification
Figure BDA0002579327080000022
And the height of the nitric acid concentration tower is 14900mm, the technical scheme of the invention improves the rectification height of the concentrated nitric acid so as to stabilize the concentration of the finished acid to be more than 98.2% (w/w), and simultaneously increases the denitration height and reduces the nitrate content in the dilute magnesium nitrate.
2. In the novel magnesium nitrate method concentrated nitric acid production system provided by the invention, the bulk ceramic diluted ring and rectangular saddle ring packing of the nitric acid concentration tower and the bleaching tower are changed into ceramic regular packing, so that the gas-liquid contact surface area is increased, the system resistance is reduced, the nitrate content of diluted magnesium nitrate and finished acid is reduced, and the yield and quality of the finished acid are improved.
3. In the novel magnesium nitrate method concentrated nitric acid production system provided by the invention, each layer of ceramic regular packing and gaps of the nitric acid concentration tower and the bleaching tower are plugged by the tetrafluoro rod, so that the occurrence of wall flow is avoided, and the reduction of gas-liquid contact surface area is avoided, thereby improving the yield and quality of finished acid and reducing the nitrate content of dilute magnesium nitrate.
4. In the novel magnesium nitrate method concentrated nitric acid production system provided by the invention, a magnesium tail water rectifying tower is added between a dilute magnesium nitrate evaporator and an indirect condenser, the concentration of magnesium tail water is reduced from 2-3% (w/w) to 0.1% (w/w), the magnesium tail water is sent to an ion exchange bed to be treated into neutrality, and meanwhile, the by-product of 18% (w/w) dilute nitric acid is sent to a dilute nitric acid storage tank for concentration; meanwhile, magnesium tail water with 0.1 percent (w/w) of nitric acid content is treated to be neutral by adding ion exchange bed water treatment equipment and then is supplemented to a circulating water system.
5. In the novel system for producing concentrated nitric acid by a magnesium nitrate method, the tail gas absorption tower is added, hydrogen peroxide is used as an absorbent to reduce the concentration of nitrogen oxide in the tail gas to be below 30PPM for standard emission, and meanwhile, dilute nitric acid with the byproduct concentration of 20% (w/w) is sent to a dilute nitric acid storage tank for concentration.
In general, the novel magnesium nitrate method concentrated nitric acid production system provided by the invention can ensure that the concentration of finished acid is stabilized above 98.2% (w/w) and the content of nitrate is lower than 0.5% (w/w), so that the content of nitrate in dilute magnesium nitrate is reduced to be lower than 0.1% (w/w), the corrosion rate of a dilute magnesium nitrate heater is reduced, and the service life of the dilute magnesium nitrate heater can be prolonged to be more than 8 years from 4-5 years; in addition, the invention can realize zero discharge of the acidic wastewater, save energy, reduce consumption and protect environment; and the invention can realize the organized standard emission of the tail gas and protect the environment.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
Fig. 1 is a schematic diagram of a novel magnesium nitrate method concentrated nitric acid production system according to an embodiment of the invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified by combining the specific drawings.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Aiming at the technical problems in the traditional process for producing concentrated nitric acid by a magnesium nitrate method, the invention provides a novel system for producing concentrated nitric acid by a magnesium nitrate method, which comprises a nitric acid concentration tower and a bleaching towerWhite tower; the dispersers positioned at the top of the nitric acid concentration tower and the top of the bleaching tower are both groove-type dispersers, the shower aperture of the disperser at the top of the nitric acid concentration tower is 6mm, and the shower aperture of the disperser at the top of the bleaching tower is 4 mm; the specifications of two tower sections of the nitric acid concentration tower are as follows
Figure BDA0002579327080000041
The height is 15300 mm.
Furthermore, ceramic regular packing is arranged in the nitric acid concentration tower and the bleaching tower.
And a tetrafluoro rod is arranged in a gap between each layer of ceramic regular packing and the tower wall of the nitric acid concentration tower and the bleaching tower for plugging.
Furthermore, the system for producing the concentrated nitric acid by the magnesium nitrate method further comprises a dilute magnesium nitrate evaporator and an indirect condenser, a magnesium tail water rectifying tower is arranged between the dilute magnesium nitrate evaporator and the indirect condenser, the concentration of the magnesium tail water is reduced from 2-3% (w/w) to 0.1% (w/w), then the magnesium tail water is sent to an ion exchange bed to be treated to be neutral, and meanwhile, the by-product dilute nitric acid is sent to a dilute nitric acid storage tank for concentration.
Further, the system for producing the concentrated nitric acid by the magnesium nitrate method also comprises a hydrogen peroxide tank and a tail gas absorption tower; the hydrogen peroxide tank is connected to the top of the tail gas absorption tower through a hydrogen peroxide pump;
the bottom of tail gas absorption tower is connected to the second dilute nitric acid tank through a pipeline, the second dilute nitric acid tank is connected to the cooler through an acid water pump, the cooler is connected to the tail gas absorption tower through a pipeline, the top of the tail gas absorption tower is connected to the tail gas ejector through a pipeline, the tail gas ejector is connected to the tail gas circulating water tank, and the tail gas circulating water tank is connected to the tail gas ejector through a tail gas circulating water pump.
The following describes the production system of concentrated nitric acid by a magnesium nitrate method provided by the invention with reference to fig. 1. The production system comprises a concentrated magnesium nitrate storage tank, a first dilute nitric acid tank, a dilute magnesium nitrate storage tank, a concentrated magnesium nitrate head tank, a dilute nitric acid head tank, a mixing distributor, a magnesium nitrate heater, a nitric acid concentration tower, a bleaching tower, a finished product acid cooler, a concentrated nitric acid condenser, a gas-liquid separator, a tower tail ejector, a tower tail water circulating tank, a magnesium tail ejector, a magnesium tail water circulating tank, a magnesium nitrate evaporator, a magnesium tail water rectifying tower, an indirect condenser, a tail gas absorption tower, a hydrogen peroxide tank, a second dilute nitric acid tank, an acid cooler, a tail gas ejector, a tail water circulating tank, an ion exchange bed and a desalination water tank;
a concentrated magnesium nitrate pump is arranged between the concentrated magnesium nitrate storage tank and the concentrated magnesium nitrate head tank and used for pumping concentrated magnesium nitrate into the concentrated magnesium nitrate head tank, and a dilute nitric acid pump is arranged between the first dilute nitric acid tank and the dilute nitric acid head tank and used for pumping dilute nitric acid into the dilute nitric acid head tank;
the concentrated magnesium nitrate head tank and the dilute nitric acid head tank are communicated to a mixing distributor through pipelines, the mixing distributor is connected with a nitric acid concentration tower,
the top of the nitric acid concentration tower is connected to the bottom of the bleaching tower, the bottom of the nitric acid concentration tower is connected to a magnesium nitrate heater, and the magnesium nitrate heater is connected to a dilute magnesium nitrate storage tank through a pipeline;
the tower top of the bleaching tower is connected to a concentrated nitric acid condenser, and the tower bottom is also connected to a finished product acid cooler through a bleaching tower bottom acid seal;
the concentrated nitric acid condenser is connected to a gas-liquid separator, the gas-liquid separator is connected to a tower tail ejector, the tower tail ejector is connected to a tower tail water circulation tank, and the tower tail water circulation tank is connected to the first dilute nitric acid tank through a magnesium tail water circulation pump;
the dilute magnesium nitrate storage tank is connected to a magnesium nitrate evaporator through a dilute magnesium nitrate pump, the concentrated magnesium nitrate obtained through evaporation treatment enters the concentrated magnesium nitrate storage tank, the magnesium nitrate evaporator is further connected to a magnesium tail water rectifying tower through a pipeline, the dilute nitric acid obtained through rectification is led into a first dilute nitric acid tank through a pipeline, the magnesium nitrate evaporator is further connected to an indirect condenser through a pipeline, the indirect condenser is connected to a magnesium tail ejector and a magnesium tail water circulating tank through a pipeline,
the dilute magnesium nitrate storage tank, the concentrated magnesium nitrate storage tank, the tower tail water circulation tank and the magnesium tail water circulation tank are respectively connected to the tail gas absorption tower through pipelines; the hydrogen peroxide tank is connected to the top of the tail gas absorption tower through a hydrogen peroxide pump,
the bottom of the tail gas absorption tower is connected to a second dilute nitric acid tank through a pipeline, the second dilute nitric acid tank is connected to a cooler through an acid water pump, the cooler is connected to the tail gas absorption tower through a pipeline,
the top of the tail gas absorption tower is connected to a tail gas ejector through a pipeline, the tail gas ejector is connected to a tail gas circulating water tank, and the tail gas circulating water tank is connected to the tail gas ejector through a tail gas circulating water pump;
the magnesium tail water circulating tank is connected to the ion exchange bed through a magnesium tail water circulating pump, the ion exchange bed is connected to a desalination water tank through a pipeline, and the desalination water tank is guided to circulating cooling return water through a desalination water pump;
the foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (5)

1. A novel concentrated nitric acid production system by a magnesium nitrate method comprises a nitric acid concentration tower and a bleaching tower; the method is characterized in that dispersers positioned at the top of a nitric acid concentration tower and the top of a bleaching tower are both groove-type dispersers, the shower aperture of the disperser at the top of the nitric acid concentration tower is 6mm, and the shower aperture of the disperser at the top of the bleaching tower is 4 mm;
the specifications of two tower sections of the nitric acid concentration tower are as follows
Figure FDA0002579327070000011
The height is 15300 mm.
2. The system for producing concentrated nitric acid by a magnesium nitrate method according to claim 1, wherein the nitric acid concentration tower and the bleaching tower are internally provided with ceramic structured packing.
3. The system for producing concentrated nitric acid by a magnesium nitrate method according to claim 2, wherein a tetrafluoro rod is arranged in a gap between each layer of the ceramic structured packing and the tower wall of the nitric acid concentration tower and the bleaching tower for plugging.
4. The system for producing concentrated nitric acid by a novel magnesium nitrate method according to claim 1, further comprising a dilute magnesium nitrate evaporator and an indirect condenser, wherein a magnesium tail water rectifying tower is arranged between the dilute magnesium nitrate evaporator and the indirect condenser, the concentration of the magnesium tail water is reduced from 2-3% (w/w) to 0.1% (w/w), then the magnesium tail water is sent to an ion exchange bed to be treated to be neutral, and meanwhile, the by-product dilute nitric acid is sent to a dilute nitric acid storage tank for concentration.
5. The system for producing concentrated nitric acid by a magnesium nitrate method according to claim 1, further comprising a hydrogen peroxide tank and a tail gas absorption tower; the hydrogen peroxide tank is connected to the top of the tail gas absorption tower through a hydrogen peroxide pump;
the bottom of tail gas absorption tower is connected to the second dilute nitric acid tank through a pipeline, the second dilute nitric acid tank is connected to the cooler through an acid water pump, the cooler is connected to the tail gas absorption tower through a pipeline, the top of the tail gas absorption tower is connected to the tail gas ejector through a pipeline, the tail gas ejector is connected to the tail gas circulating water tank, and the tail gas circulating water tank is connected to the tail gas ejector through a tail gas circulating water pump.
CN202010663020.2A 2020-07-10 2020-07-10 Novel concentrated nitric acid production system by magnesium nitrate method Pending CN111807338A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113304496A (en) * 2021-06-17 2021-08-27 河南晋开化工投资控股集团有限责任公司 Device and process for producing dilute nitric acid by magnesium nitrate method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113304496A (en) * 2021-06-17 2021-08-27 河南晋开化工投资控股集团有限责任公司 Device and process for producing dilute nitric acid by magnesium nitrate method

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Application publication date: 20201023