CN113044854A - High-purity ammonia preparation method and system - Google Patents
High-purity ammonia preparation method and system Download PDFInfo
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- CN113044854A CN113044854A CN202110310612.0A CN202110310612A CN113044854A CN 113044854 A CN113044854 A CN 113044854A CN 202110310612 A CN202110310612 A CN 202110310612A CN 113044854 A CN113044854 A CN 113044854A
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- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
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- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
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- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
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Abstract
The invention discloses a method and a system for preparing high-purity ammonia, which gasifies liquid ammonia serving as a raw material, then absorbs ammonia gas by using high-purity water to obtain concentrated ammonia water, and then produces the high-purity ammonia by a two-stage rectification method, wherein the method for preparing the high-purity ammonia comprises the following steps: (1) gasifying liquid ammonia; (2) preparing ammonia water; (3) dehydrating; (4) the high-purity ammonia preparation system is used for preparing high-purity ammonia by implementing the high-purity ammonia preparation method, and comprises an absorption tower, a primary distillation tower and a rectification tower, wherein the absorption tower is used for preparing the ammonia water, the primary distillation tower is used for dehydrating strong ammonia water, and the rectification tower is used for purifying and preparing the high-purity ammonia water.
Description
Technical Field
The invention relates to the technical field of high-purity ammonia preparation, in particular to a method and a system for preparing high-purity ammonia.
Background
High-purity ammonia water belongs to an important chemical raw material, the preparation technology of the high-purity ammonia water in China is not mature at present, a mode of combining evaporation and physical filtration is common in the preparation method of the high-purity ammonia water, for example, a continuous production method of the high-purity ammonia water with the publication number of CN204454614U, the high-purity ammonia water is prepared in a mode of adsorption and physical filtration, the purity of ammonia in the operation is not ideal, and the method adopts a physical medium for filtration in the implementation so that the purity of the ammonia water cannot be guaranteed.
The purpose of the design is to provide a method and a system for preparing high-purity ammonia.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, adapt to practical requirements and provide a method and a system for preparing high-purity ammonia.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
discloses a preparation method of high-purity ammonia, which comprises the following steps:
(1) gasifying liquid ammonia;
(2) preparing ammonia water;
(3) dehydrating;
(4) rectifying and degassing to form high-purity ammonia water.
In the step (1), the raw material liquid ammonia is decompressed by a throttle expansion valve and then enters an ammonia liquid separator to absorb heat and gasify to form ammonia gas.
In the step (2), the ammonia gas is absorbed in an absorption tower through the cooled high-purity water to form ammonia water.
And (3) degassing after primary distillation in a primary distillation tower, condensing light components after primary distillation to form crude liquid ammonia, and finishing dehydration.
In the step (4), the crude liquid ammonia is rectified in a rectifying tower, and the rectified heavy components form high-purity ammonia.
The invention also discloses a high-purity ammonia preparation system, which is used for preparing high-purity ammonia by implementing the high-purity ammonia preparation method and comprises an absorption tower, a primary distillation tower and a rectification tower, wherein the absorption tower is provided with an ammonia gas inlet and a high-purity water inlet, the high-purity water inlet is positioned at the upper part of the absorption tower, the ammonia gas inlet is positioned at the lower part of the absorption tower, the ammonia gas enters through the ammonia gas inlet, the high-purity water enters through the high-purity water inlet, the bottom of the absorption tower is provided with an ammonia water outlet, and the top of the absorption tower is provided with a tail gas;
the bottom of the primary tower is provided with a primary distillation reboiler, the middle part of the primary distillation tower is provided with an ammonia water inlet, the top of the primary distillation tower is provided with a primary distillation gas discharge outlet, strong ammonia water prepared by the absorption tower enters the primary distillation tower through the ammonia water inlet, the primary distillation gas discharge outlet is connected with a primary distillation condenser, and light components formed by primary distillation form crude liquid ammonia after being condensed by the primary distillation condenser.
The bottom of the rectifying tower is provided with a rectifying reboiler, crude liquid ammonia which is primarily distilled by the primary rectifying tower enters the rectifying tower through an inlet at the upper part of the rectifying tower, the bottom of the rectifying tower is provided with a high-purity ammonia outlet, and the high-purity ammonia is discharged through the high-purity ammonia outlet.
Still include the aqueous ammonia cooler, the aqueous ammonia discharge port passes through aqueous ammonia circulating pump and aqueous ammonia cooler access connection, the aqueous ammonia cooler is water circulative cooling ware, two branches of aqueous ammonia cooler exit linkage, dense ammonia water jar is connected to one of them branch road, and the absorption tower is connected to the second branch road and constitutes the circulation.
Still include the first distillation liquid storage tank, the import and the first distillation condenser exit linkage of first distillation liquid storage tank, two branches of exit linkage of first distillation liquid storage tank, wherein first branch is connected with the first distillation tower top and is constituted the circulation, and the thick liquid ammonia jar is connected to the second branch.
The top of the rectifying tower is provided with a rectifying condenser, light components during rectification enter the rectifying tower again for rectification after being condensed by the rectifying condenser, and non-condensable gas is discharged through an outlet of the rectifying condenser.
The invention has the beneficial effects that:
according to the invention, the raw material liquid ammonia is gasified firstly, then the high-purity water is used for absorbing ammonia gas to obtain concentrated ammonia water, and then the concentrated ammonia water is subjected to a two-stage rectification method to produce high-purity ammonia, so that the process is simple and reliable; the purity of the finished product liquid ammonia can be effectively ensured.
Secondly, the invention can realize no three wastes discharge, various byproducts can be recycled, and the byproduct pure ammonia gas can be used as the raw material of other production devices of users to absorb tail gas NH3The content is extremely low, which meets the national emission requirement and is rich in H2And combustible gases such as CO and the like can be used as fuel of a user industrial furnace to recover heat value, and the generated dilute ammonia water, the primary distillation tail gas and the rectification tail gas can be sent to an ammonia gas absorption device of a user to produce high-concentration ammonia water.
Drawings
FIG. 1 is a schematic diagram of the absorption tower of the present invention for preparing concentrated ammonia water;
FIG. 2 is a schematic diagram of the preliminary distillation dehydration principle corresponding to the preliminary distillation tower of the present invention;
FIG. 3 is a schematic diagram of the rectification column of the present invention for preparing high purity ammonia water.
Detailed Description
The invention is further illustrated with reference to the following figures and examples:
example 1: a high purity ammonia production system, see figures 1-3.
The absorption tower is a normal-pressure packed tower, the absorption tower T001 is provided with an ammonia gas inlet and a high-purity water inlet, the high-purity water inlet is positioned at the upper part of the absorption tower, the ammonia gas inlet is positioned at the lower part of the absorption tower, the ammonia gas enters through the ammonia gas inlet, the high-purity water enters through the high-purity water inlet, the bottom of the absorption tower is provided with an ammonia water outlet, and the top of the absorption tower is provided with a tail gas ammonia gas outlet; still include aqueous ammonia cooler E001, the aqueous ammonia discharge port passes through aqueous ammonia circulating pump P001 and aqueous ammonia cooler E001 access connection, aqueous ammonia cooler E001 is the hydrologic cycle cooler and adopts the cooling water as coolant, two branches of aqueous ammonia cooler E001 exit linkage, dense ammonia water pitcher V001 is connected to one of them branch road, absorption tower T001 is connected to the second branch road and constitutes the circulation, connect dense ammonia pump P002 on the leakage fluid dram of dense ammonia water pitcher V001, the top of dense ammonia water pitcher V001 is equipped with the ammonia discharge port, this ammonia discharge port communicates the tail gas absorption tower jointly with the ammonia discharge port at absorption tower T001 top and absorbs it, the absorbent ammonia of tail gas absorption tower can form diluted aqueous ammonia and be used for preparing industry diluted aqueous ammonia.
Preliminary distillation tower T002 bottom is equipped with preliminary distillation reboiler E004, the middle part is equipped with aqueous ammonia import, the top is equipped with the initial distillation gas eduction port, and the dense ammonia water of preparation through absorption tower T001 passes through in the dense ammonia water pump back gets into preliminary distillation tower T002 by the aqueous ammonia import, and preliminary distillation gas eduction port connects preliminary distillation condenser E003, and the light component that the preliminary distillation formed forms thick liquid ammonia after the condensation of preliminary distillation condenser E003, still includes preliminary distillation liquid storage tank V002 simultaneously, the import and the exit linkage of preliminary distillation condenser E003 of preliminary distillation liquid storage tank V002, and preliminary distillation liquid storage tank V002 top is equipped with the tail gas export, and this tail gas exit linkage tail gas absorption tower, preliminary distillation condenser E003 adopt liquid ammonia as cooling medium, and liquid ammonia can form gas ammonia behind this preliminary distillation condenser E003 and use as the raw materials.
Two branches of above-mentioned initial distillation liquid storage tank V002's bottom exit linkage, wherein first branch road is connected with initial distillation tower T002 top and is constituted the circulation, and thick liquid ammonia jar V003 is connected to the second branch road, and thick liquid ammonia jar V003 bottom is equipped with thick liquid ammonia discharge port, and thick liquid ammonia jar V003 top is equipped with the tail gas export and connects the tail gas absorption tower. The leakage fluid dram of above-mentioned preliminary distillation tower T002 bottom connects weak aqua ammonia cooler E002, and weak aqua ammonia cooler E002 can condense the weak aqua ammonia after the preliminary distillation tower reboiling, and the coolant of weak aqua ammonia cooler E002 adopts water to cool off weak aqua ammonia.
Rectifying column T003 bottom is equipped with rectification reboiler E006, and rectification reboiler E006 uses steam as the heat source, and the import that gets into the rectifying column by rectifying column T003 upper portion after the crude liquid ammonia that forms through preliminary distillation tower T002 is discharged through crude liquid ammonia tank enters the rectifying column, and the rectifying column bottom is equipped with high-purity ammonia discharge port, and high-purity ammonia is discharged through high-purity ammonia discharge port. The rectifying tower top is equipped with rectifying condenser E005, and light component during the rectification gets into rectifying tower rectification again after rectifying condenser E005 condensation, and noncondensable gas discharges through rectifying condenser export, and its rectifying condenser E005 uses liquid ammonia as condensing medium, and liquid ammonia can form gas ammonia after this rectifying condenser E005 and use as the raw materials.
Example 2, a high purity ammonia production method for carrying out and producing high purity ammonia on the high purity ammonia production system described in the above example 1, comprising the steps of:
(1) gasifying liquid ammonia; from the outside, 0.8 to 1.6MPa at-8 ℃, and impurities (H)2、N2、O2、CO、CO2、CH4、C2H6Etc.) raw material liquid ammonia with the total amount less than or equal to 1ppb (W) is decompressed by a throttle expansion valve and then enters an ammonia liquid separator for heat absorption and gasification to form ammonia gas, and H in the raw material liquid ammonia can be removed simultaneously in the step2Impurities such as O, oil stain, rust and the like, and gasified ammonia gas are carried by liquid foam removed by an ammonia liquid separator and enter the bottom of the absorption tower.
(1) Preparing ammonia water; ammonia gas (containing NH)399 (V%), -25 ℃, 0.02MPa) is absorbed in an absorption tower to form ammonia water, in the step, the high-purity water absorbs heat and is cooled by liquid ammonia when being gasified by a pure water cooler, and the high-purity water is cooled to 5 ℃ from normal temperature, and then enters the absorption tower from the top of the absorption tower. The absorption tower is a normal-pressure packed tower, ammonia gas rising from the bottom of the tower and high-purity water sprayed from the top of the tower are in countercurrent contact in a packing in the absorption tower, most of the ammonia gas is absorbed to generate concentrated ammonia water with the concentration of 21 percent, the temperature of the ammonia water is between 41 ℃ and the ammonia water is discharged from the bottom of the absorption tower, then the ammonia water is pressurized by a concentrated ammonia water pump, most of the ammonia water is cooled to 35 ℃ by circulating cooling water with the pressure of 0.2 to 0.4MPa and the temperature of less than or equal to 32 ℃ (delta t is 5 ℃), then the ammonia water returns to the absorption tower to continuously absorb the solution heat of the ammonia gas, and a. In the process, most of H in ammonia gas can be removed simultaneously2、N2、O2、CO、CO2、CH4、C2H6When the inert gas is equal, the tail gas absorbed by the tower top of the absorption tower is mainly H2、N2、O2、CO、CO2、CH4、C2H6The content of ammonia is less than or equal to 20mg/m in the presence of inert gas3And the heat value can reach the discharge requirement of GB31573-2015, can be directly discharged and can also be sent to a user industrial furnace for combustion and recovery.
(2) Dehydrating; the primary distillation tower is a 0.1MPa pressurized packed tower, and the upper section and the lower section are filled with materials, the upper section is a rectification section, and the lower section is a stripping section. Heating the kettle liquid of the primary distillation reboiler by using 0.2-0.4 MPa saturated steam, condensing the primary distillation condenser at the top of the tower by using liquid ammonia as a raw material, heating the strong ammonia water from the absorption tower to-78 ℃ by using the kettle liquid of the primary distillation tower through a primary distillation preheater, and then entering the primary distillation tower from the middle part of the strong ammonia water; the process of ammonia distillation and water removal is mainly carried out in the primary distillation tower, the relatively dilute ammonia water steam rising from the tower kettle and the relatively concentrated ammonia water liquid sprayed from the tower top are subjected to countercurrent mass transfer and heat transfer in a filler, the relatively concentrated ammonia water liquid is partially gasified to obtain concentrate, and the concentrate rises to the tower top; the concentration of the partial liquefied ammonia water of the thinner ammonia water vapor is reduced and the partial liquefied ammonia water is reduced to the tower kettle. When the rising strong ammonia steam reaches the top of the primary tower, H2Removing O and oil dirt, discharging from the top of the primary distillation tower, and feeding in the primary distillation condenserCooling liquid ammonia, condensing most ammonia gas into liquid ammonia with the concentration of more than 99%, and dissolving inert gas in the rest.
After the gas-liquid mixture is separated by a primary distillation liquid storage tank, the gas phase is primary distillation tail gas and comprises the following components in percentage by weight: NH (NH)390.38、N21.59、O22.42、CO1.58、CO21.56、CH41.9、C2H60.57, mixing the by-product with the rectification tail gas, and then sending the mixture to a crude liquid ammonia tank to produce concentrated ammonia water; the liquid phase is a primary distillation liquid, the liquid phase is pressurized by a primary distillation liquid pump, a small part (55 kg/h) of the liquid phase is sent to a subsequent rectification degassing system, and a large part (126 kg/h) of the liquid phase enters the top of the primary distillation tower for reflux, and the process can form multiple cycles. The dilute ammonia water dropped to the tower kettle contains 2.12 percent of ammonia, the temperature is between 116 ℃ and the flow is between 0.25m3And h, can be used as an ammonia absorption liquid and discharged into the absorption tower again.
(3) Rectifying and degassing to form high-purity ammonia water.
The rectifying tower is a 0.5MPa pressurized packed tower, and is filled with an upper section and a lower section, wherein the upper section is a rectifying section, and the lower section is a stripping section. And heating the rectifying reboiler residue by using hot water with the pressure of 0.2-0.4 MPa and the temperature of more than or equal to 70 ℃ (delta t ═ 10 ℃), condensing the rectifying condenser at the top of the tower by using raw liquid ammonia, and feeding crude concentrated liquid ammonia from the primary distillation into a rectifying tower from the middle part. The ammonia condensation and degassing process is mainly carried out in the rectifying tower, the ammonia gas rising from the tower kettle and the liquid ammonia sprayed from the tower top are subjected to countercurrent mass transfer and heat transfer in the filler, the rising ammonia gas is partially condensed, the content of dissolved gas in the condensed liquid ammonia is reduced, and the condensed liquid ammonia is dropped to the tower kettle; the descending liquid ammonia is partially gasified, and the content of dissolved gas in the gasified ammonia gas is increased and rises to the top of the tower.
The ascending ammonia gas is rich in a large amount of inert gases when reaching the top of the rectifying tower, is discharged from the top of the rectifying tower, is cooled by the gasification of liquid ammonia in a rectifying condenser at the top of the rectifying tower, most of the ammonia gas is condensed into liquid ammonia with the concentration of 97.79 percent, and the rest is dissolved inert gases. After the gas-liquid mixture is separated by a rectification liquid storage tank, the gas phase is rectification tail gas and comprises the following components in percentage by weight: NH (NH)393.18、N20.26、O20.98、CO0.37、CO22.69、CH41.13、C2H61.38 asThe by-product is mixed with the primary tail gas and then is sent out; the liquid phase is rectification liquid with the flow rate of 93kg/h, and directly enters the top of the rectification tower for reflux. The liquid ammonia dropped to the tower kettle is high-purity ammonia, the temperature is 8 ℃, the pressure is 0.5MPa, the flow is 51kg/h, and the high-purity ammonia is sent out as a product.
The embodiments of the present invention are disclosed as the preferred embodiments, but not limited thereto, and those skilled in the art can easily understand the spirit of the present invention and make various extensions and changes without departing from the spirit of the present invention.
Claims (9)
1. The preparation method of high-purity ammonia is characterized by comprising the following steps:
(1) gasifying liquid ammonia;
(2) preparing ammonia water;
(3) dehydrating;
(4) rectifying and degassing to form high-purity ammonia water.
2. The process for producing high purity ammonia according to claim 1, characterized in that: in the step (1), the raw material liquid ammonia is decompressed by a throttle expansion valve and then enters an ammonia liquid separator to absorb heat and gasify to form ammonia gas.
3. The process for producing high purity ammonia according to claim 1, characterized in that: in the step (2), the ammonia gas is absorbed in an absorption tower through the cooled high-purity water to form ammonia water.
4. The process for producing high purity ammonia according to claim 1, characterized in that: and (3) degassing after primary distillation in a primary distillation tower, condensing light components after primary distillation to form crude liquid ammonia, and finishing dehydration.
5. The process for producing high purity ammonia according to claim 1, characterized in that: in the step (4), the crude liquid ammonia is rectified in a rectifying tower, and the rectified heavy components form high-purity ammonia.
6. A high purity ammonia production system for producing high purity ammonia by carrying out the high purity ammonia production method according to any one of claims 1 to 4, characterized by comprising an absorption column, a preliminary distillation column and a rectification column, wherein the absorption column has an ammonia gas inlet and a high purity water inlet, the high purity water inlet is located at an upper portion of the absorption column, the ammonia gas inlet is located at a lower portion of the absorption column, the ammonia gas is introduced through the ammonia gas inlet, the high purity water is introduced through the high purity water inlet, an ammonia water discharge port is provided at a bottom portion of the absorption column, and a tail gas ammonia gas discharge port is provided at a top portion of the absorption column;
the bottom of the primary distillation tower is provided with a primary distillation reboiler, the middle part of the primary distillation tower is provided with an ammonia water inlet, the top of the primary distillation tower is provided with a primary distillation gas discharge port, the strong ammonia water prepared by the absorption tower enters the primary distillation tower through the ammonia water inlet, the primary distillation gas discharge port is connected with a primary distillation condenser, and light components formed by primary distillation are condensed by the primary distillation condenser to form crude liquid ammonia;
the bottom of the rectifying tower is provided with a rectifying reboiler, crude liquid ammonia which is primarily distilled by the primary rectifying tower enters the rectifying tower through an inlet at the upper part of the rectifying tower, the bottom of the rectifying tower is provided with a high-purity ammonia outlet, and the high-purity ammonia is discharged through the high-purity ammonia outlet.
7. The system for producing high purity ammonia according to claim 6, wherein: still include the aqueous ammonia cooler, the aqueous ammonia discharge port passes through aqueous ammonia circulating pump and aqueous ammonia cooler access connection, the aqueous ammonia cooler is water circulative cooling ware, two branches of aqueous ammonia cooler exit linkage, dense ammonia water jar is connected to one of them branch road, and the absorption tower is connected to the second branch road and constitutes the circulation.
8. The system for producing high purity ammonia according to claim 6, wherein: still include the first distillation liquid storage tank, the import and the first distillation condenser exit linkage of first distillation liquid storage tank, two branches of exit linkage of first distillation liquid storage tank, wherein first branch is connected with the first distillation tower top and is constituted the circulation, and the thick liquid ammonia jar is connected to the second branch.
9. The system for producing high purity ammonia according to claim 6, wherein: the top of the rectifying tower is provided with a rectifying condenser, light components during rectification enter the rectifying tower again for rectification after being condensed by the rectifying condenser, and non-condensable gas is discharged through an outlet of the rectifying condenser.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114618269A (en) * | 2022-02-16 | 2022-06-14 | 苏州市兴鲁空分设备科技发展有限公司 | Ammonia-containing tail gas purifying device |
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