CN111960436A - Ultrapure ammonia production device and production method - Google Patents
Ultrapure ammonia production device and production method Download PDFInfo
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- CN111960436A CN111960436A CN202010913925.0A CN202010913925A CN111960436A CN 111960436 A CN111960436 A CN 111960436A CN 202010913925 A CN202010913925 A CN 202010913925A CN 111960436 A CN111960436 A CN 111960436A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 236
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 98
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 49
- 238000005192 partition Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000006200 vaporizer Substances 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims description 16
- 238000003795 desorption Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 9
- 238000004891 communication Methods 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 20
- 239000003921 oil Substances 0.000 description 19
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000007788 liquid Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 10
- 239000001294 propane Substances 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000004886 process control Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- -1 moisture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides an ultrapure ammonia production device and a production method, and the ultrapure ammonia production device comprises: the evaporator group is formed by connecting at least two evaporators in series, and the two adjacent evaporators are communicated through an overflow series pipeline; the lower part of the side wall of each evaporator is provided with a liquid ammonia feed port; the bottom of each evaporator is provided with a first heavy component outlet; the top of each evaporator is provided with a first light component discharge port; a heating system for providing heat to the vaporizer to vaporize the liquid ammonia; and a partition tower communicating with the first light component discharge port of the evaporator; the top of the partition wall tower is provided with a second light component discharge port and an ultra-pure ammonia discharge port; the bottom of the dividing wall tower is provided with a second heavy component discharge port. The ultra-pure ammonia production device can obtain higher ultra-pure ammonia yield according to production requirements, can simultaneously remove light components and heavy components at one time, has lower energy consumption, and saves the production cost of ultra-pure ammonia.
Description
Technical Field
The invention belongs to the technical field of liquid ammonia purification, and particularly relates to an ultrapure ammonia production device and an ultrapure ammonia production method.
Background
The ultra-pure ammonia is an important electronic gas in the solar cell, LED and semiconductor industries, and can be used as an important nitrogen source formed by a silicon nitride film in a crystalline silicon solar cell; in the preparation of the LED, ultra-pure ammonia and trimethylgallium act on sapphire to form a gallium nitride LED through vapor phase growth; in semiconductor manufacturing processes, ultra-pure ammonia is reacted with silane to form silicon nitride films. With the development of science and technology and the increasing social demand for electronic products, novel energy-saving lighting devices and clean energy, the production enterprises have higher and higher requirements for the purity of the ultrapure ammonia.
The current preparation of the ultra-pure ammonia takes industrial liquid ammonia as a raw material, processes such as gasification, oil removal, adsorption and the like are needed, and the annual yield of the ultra-pure ammonia of each production line is not more than 2000 tons, which is mainly because a horizontal storage tank type evaporator is used at present and is limited by the preparation process of the horizontal storage tank type evaporator, and the volume of a single horizontal storage tank type evaporator is not more than 200m3So that the evaporation area of industrial ammonia is limited. On the other hand, the production of the ultra-pure ammonia at present mainly utilizes two rectifying towers to finish the purification process, wherein one rectifying tower is used for removing light components, and the other rectifying tower is used for removing heavy components. For example, chinese patent No. cn201810973945.x discloses a system and a method for producing ultrapure ammonia, including: standing and self-cleaning industrial liquid ammonia to obtain self-cleaned liquid ammonia; performing light component removal rectification on the self-purified liquid ammonia in a light component removal rectification tower to obtain ammonia saturated steam with the concentration of more than 99.99 percent; and introducing the ammonia saturated steam into a de-heavy rectifying tower for de-heavy rectification to obtain ultra-pure ammonia. The light-component removal rectifying tower and the heavy-component removal rectifying tower of the production system are additionally provided with a condenser and a reboiler, so that the energy consumption is high, and the production capacity of the ultra-pure ammonia of a single production line is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a production device and a production method of ultrapure ammonia.
In order to solve the technical problems, the invention adopts the following technical scheme:
an ultrapure ammonia production plant comprising:
the evaporator group is formed by connecting at least two evaporators in series, and the two adjacent evaporators are communicated through an overflow series pipeline; a liquid ammonia feed port is formed in the lower portion of the side wall of each evaporator; a first heavy component discharge port is formed in the bottom of each evaporator; the top of each evaporator is provided with a first light component discharge port;
a heating system for providing heat to the vaporizer to vaporize liquid ammonia; and
a divided wall column communicating with the first light component discharge port of the evaporator; the top of the partition wall tower is provided with a second light component discharge port and an ultra-pure ammonia discharge port; and a second heavy component discharge port is formed at the bottom of the partition wall tower.
Preferably, the device further comprises a parallel adsorption and desorption device, and the parallel adsorption and desorption device is communicated with the second light component discharge port.
Preferably, the heating system is a reboiler in heat exchange relationship with the bottom of each of the evaporators.
Preferably, the upper part of each evaporator is provided with a filler layer, and the second heavy component discharge port is communicated with the top of each evaporator.
Preferably, each overflow series pipeline is provided with a return liquid port, and the return liquid port is communicated with the top of the evaporator at the upstream of the return liquid port.
Preferably, at least two evaporator groups are arranged, and each evaporator group is communicated with the dividing wall tower in a parallel mode.
Preferably, the bottom of each of the evaporators is of a conical bottom structure.
The invention also provides a method for producing the ultra-pure ammonia by using the ultra-pure ammonia production device, which comprises the following steps:
liquid ammonia is separated into a first light component and a first heavy component through the evaporator group, and the first heavy component is discharged through a first oil discharge pipeline;
the first light component enters the partition wall tower for secondary separation, and a second light component, ultra-pure ammonia and a second heavy component are separated; the second light component is discharged through a light discharge pipeline, and the second heavy component is discharged through a second oil discharge pipeline; part of the ultrapure ammonia is condensed and then flows back to the top of the bulkhead tower.
Preferably, the method further comprises the following steps: and the second light component is treated by the parallel adsorption and desorption device and then discharged through a light discharge pipeline.
Preferably, a portion of the second heavy component is refluxed to the top of the evaporator.
Compared with the prior art, the invention has the beneficial effects that:
according to the ultrapure ammonia production device, the evaporator group formed by connecting at least two evaporators in series is used for evaporating and purifying liquid ammonia, and the evaporation area can be controlled according to the number of the evaporators used, so that the ultrapure ammonia production device overcomes the defect of limited evaporation area in the prior art, and can obtain higher ultrapure ammonia yield according to production requirements; on the other hand, because a plurality of evaporators are connected in series through the overflow and are used for purifying the liquid ammonia, the removal rate of heavy components in the liquid ammonia can be improved, and the high-purity ammonia can be obtained. In addition, the ultra-pure ammonia production device provided by the invention uses the partition wall tower to further purify the liquid ammonia, overcomes the defect that two rectifying towers are used to respectively remove light components and heavy components in the prior art, can simultaneously remove the light components and the heavy components at one time, is lower in energy consumption, and saves the production cost of ultra-pure ammonia.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
It will be appreciated by those skilled in the art that the objects and advantages that can be achieved with the present invention are not limited to the specific details set forth above, and that these and other objects that can be achieved with the present invention will be more clearly understood from the detailed description that follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. Many aspects of the invention will be better understood with reference to the following drawings. The components in the drawings are not necessarily to scale, emphasis instead being placed upon clearly illustrating the principles of the present invention.
Fig. 1 is a schematic structural diagram of an ultrapure ammonia production apparatus provided in embodiment 1 of the present invention.
In the figure, 1, an evaporator group, 2, a heating system, 3, a partition tower, 4, an overflow serial pipeline, 5, a first oil discharge pipeline, 6, a second oil discharge pipeline, 7, a parallel adsorption and desorption device, 8, a packing layer, 9, a light component discharge pipeline, 11, an evaporator, 31, a second light component discharge port, 32, an ultra-pure ammonia discharge port, 33, a second heavy component discharge port, 111, a liquid ammonia feed inlet, 112, a first heavy component discharge port, 113 and a first light component discharge port.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the drawings, the same reference numerals denote the same or similar parts, or the same or similar steps.
It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
The embodiment of the invention provides an ultrapure ammonia production device, which is structurally shown in figure 1. An ultrapure ammonia production device comprises an evaporator group 1, a heating system 2 and a bulkhead tower 3. The evaporator group 1 is formed by connecting at least two evaporators 11 in series, and the two adjacent evaporators 11 are communicated through an overflow series pipeline 4; the lower part of the side wall of each evaporator 11 is provided with a liquid ammonia feed port 111; the bottom of each evaporator 11 is provided with a first heavy fraction discharge outlet 112; the top of each evaporator 11 is provided with a first light component discharge port 113; the heating system 2 is used for providing heat for the evaporator 11 to vaporize liquid ammonia; the partition tower 3 communicates with the first light component discharge port 113 of the evaporator 11; the top of the partition wall tower 3 is provided with a second light component discharge port 31 and an ultra-pure ammonia discharge port 32; the bottom of the divided wall column 3 is provided with a second heavy component discharge outlet 33.
When the device is used, industrial liquid ammonia (the ammonia content is 99.9%, and the balance is impurities such as moisture, oil, methane, ethane, propane and metal ions) enters the evaporator 11 from a liquid ammonia feed port 111 at the lower part of the side wall of the evaporator 11, excessive liquid ammonia enters the next evaporator 11 through an overflow series pipeline 4, a heating system 2 heats the liquid ammonia in the evaporator 11 to gasify the liquid ammonia, and a first light component (the main components comprise ammonia, methane and ethane, wherein the ammonia content is 99.99%) enters a partition tower 3 from a first light component discharge port 113 to be purified for the second time; at the same time, the first heavy component (the main components are metal ions, propane, water and the like) enters the first oil discharge pipeline 5 from the first heavy component discharge port 112 and is discharged. In the next-door tower 3, after the second purification and separation, the second light component (the main components are methane, ethane and the like) is discharged from a second light component discharge port 31, and is subjected to subsequent condensation and recovery processing, the second heavy component (the main components are metal ions such as iron, sodium and the like) enters a second oil discharge pipeline 6 from a second heavy component discharge port 33 and is discharged, and the ultrapure ammonia (the ammonia content is more than 99.99999%) obtained after purification is discharged from an ultrapure ammonia discharge port 32, and is subjected to subsequent condensation and is stored for later use. Because the evaporators 11 are connected through the overflow series pipeline 4, the first heavy component is separated and discharged at the bottom of each evaporator 11, so that the separation effect on the first heavy component is higher when the number of the evaporators 11 connected in series in the same evaporator group 1 is larger.
According to the ultrapure ammonia production device, the evaporator group 1 with at least two evaporators 11 connected in series is used for evaporating and purifying liquid ammonia, and the evaporation area can be controlled according to the number of the evaporators 11, so that the ultrapure ammonia production device overcomes the defect of limited evaporation area in the prior art, and can obtain higher ultrapure ammonia yield according to production requirements; on the other hand, because a plurality of evaporators 11 purify liquid ammonia through overflow series connection pipeline 4, can improve the clearance to heavy ends in the liquid ammonia, do benefit to and obtain high-purity ammonia of high purity. In addition, the ultra-pure ammonia production device provided by the invention uses the partition wall tower 3 to further purify the liquid ammonia, overcomes the defect that two rectifying towers are used to respectively remove light components and heavy components in the prior art, can simultaneously remove the light components and the heavy components at one time, and can save the energy consumption by more than 20% and save the production cost of ultra-pure ammonia.
Preferably, the ultrapure ammonia production device further comprises a parallel adsorption and desorption device 7, and the parallel adsorption and desorption device 7 is communicated with the second light component discharge port 31. The second light component is adsorbed and desorbed through the parallel adsorption and desorption device 7 before being condensed and recovered, so that the removal rate of non-condensable impurities in the second light component can be further improved.
Preferably, the heating system 2 is a reboiler exchanging heat with the bottom of each evaporator 11, and can exchange heat with liquid ammonia through hot water or hot steam in the reboiler, and the condensed water after heat exchange and temperature reduction returns to the reboiler to be heated again.
Preferably, the upper portion of each evaporator 11 is provided with a packing layer 8, and a second heavy component discharge port 33 is communicated with the top of each evaporator 11. Therefore, the countercurrent heat exchange can be carried out between the partially refluxed second heavy component and the gaseous ammonia in the evaporator 11, the packing layer 8 can improve the heat exchange area, the heat exchange effect is enhanced, and the separation effect of the liquid ammonia in the evaporator 11 is improved while the heat of the second heavy component is recycled.
Preferably, each overflow serial pipe 4 is provided with a return liquid port 41, and the return liquid port 41 is communicated with the top of the upstream evaporator 11. Each of the return liquid ports 41 in this embodiment is in communication with the first evaporator 11 of the evaporator group 1, i.e. the evaporator 11 provided with the industrial liquid ammonia feed port 111. In this way, part of the overflow liquid can be returned to the first evaporator 11, and the removal rate of the first heavy component can be increased. In order to strengthen the heat preservation effect, the outer part of the overflow series pipeline 4 is coated with a heat preservation layer.
Preferably, at least two evaporator groups 1 are provided, and each evaporator group 1 is communicated with the dividing wall tower 3 in parallel, as shown in fig. 1, and fig. 1 shows two parallel evaporator groups 1. Therefore, when the evaporator set is used, the evaporator set can be used in a standby state, namely, when one evaporator set 1 works normally, the other evaporator set 1 is in a standby state, and the maintenance or repair of equipment is facilitated under the condition that normal production is not influenced.
Preferably, the bottom of each evaporator 11 is in a conical bottom structure, and the conical bottom structure is designed to be more favorable for the first heavy component to be discharged from the bottom of the evaporator 11 after being separated.
The embodiment of the invention also provides a method for producing ultra-pure ammonia by using the ultra-pure ammonia production device, which comprises the following steps:
(1) liquid ammonia is separated into a first light component and a first heavy component through the evaporator group 1, and the first heavy component is discharged through a first oil discharge pipeline 5;
(2) the first light component enters a partition wall tower 3 for secondary separation, and a second light component, ultra-pure ammonia and a second heavy component are separated; the second light component is discharged through a light discharge pipeline 9, and the second heavy component is discharged through a second oil discharge pipeline 6; and condensing part of the ultrapure ammonia, and refluxing to the top of the dividing wall tower 3, wherein the reflux ratio is controlled to be 1: 2-1: 5.
Preferably, the method further comprises the following steps: (3) the second light component is treated by the parallel adsorption and desorption device 7 and then discharged by the light discharge pipeline 9. Before the second light component is condensed and recovered, the second light component is firstly subjected to adsorption and desorption treatment by the parallel adsorption and desorption device 7, so that the removal rate of non-condensable impurities (methane, ethane and the like) in the second light component can be further improved.
Preferably, a portion of the second heavies (about 30% of the total second heavies) is returned to the top of the evaporator 11, and another portion of the second heavies is discharged through the second oil discharge line 6. This makes it possible to improve the separation effect of liquid ammonia in the evaporator 11 while recovering the heat of the second heavy component by performing counter-current heat exchange between the partially refluxed second heavy component and gaseous ammonia in the evaporator 11.
The following is a further description with reference to specific examples.
Example 1
An ultrapure ammonia production device is shown in figure 1, and comprises two groups of evaporator groups 1 (one for one), a heating system 2, a bulkhead tower 3 and a parallel adsorption and desorption device 7 which are connected in parallel. Each evaporator group 1 is formed by connecting two evaporators 11 in series, a packing layer 8 (stainless steel wire mesh) is arranged at the upper part of each evaporator 11, the two adjacent evaporators 11 are communicated through an overflow series pipeline 4, a reflux liquid port 41 is formed in the overflow series pipeline 4, and the reflux liquid port 41 is communicated with the top of the first evaporator 11; the lower part of the side wall of each evaporator 11 is provided with a liquid ammonia feed port 111; the bottom of each evaporator 11 is provided with a first heavy fraction discharge outlet 112; the top of each evaporator 11 is provided with a first light component discharge port 113; the heating system 2 is used for providing heat for the evaporator 11 to vaporize liquid ammonia; the partition tower 3 communicates with the first light component discharge port 113 of the evaporator 11; the top of the partition wall tower 3 is provided with a second light component discharge port 31 and an ultra-pure ammonia discharge port 32, and the second light component discharge port 31 is communicated with the parallel adsorption and desorption device 7; the bottom of the divided wall column 3 is provided with a second heavy component discharge port 33, and the second heavy component discharge port 33 communicates with the top of each evaporator 11.
The method for producing the ultra-pure ammonia by using the ultra-pure ammonia production device comprises the following steps:
(1) industrial liquid ammonia is separated into a first light component and a first heavy component through an evaporator group 1, and the first heavy component is discharged through a first oil discharge pipeline 5;
(2) the first light component enters a partition wall tower 3 for secondary separation, and a second light component, ultra-pure ammonia and a second heavy component are separated; the second light component is discharged through a light discharge pipeline 9, and the second heavy component is discharged through a second oil discharge pipeline 6; condensing part of the ultrapure ammonia, and refluxing to the top of the dividing wall tower 3, wherein the reflux ratio is controlled to be 1: 3;
(3) the second light component is treated by the parallel adsorption and desorption device 7 and then discharged by the light discharge pipeline 9. A portion of the second heavies (30% of the total second heavies) is returned to the top of the evaporator 11 and another portion of the second heavies is discharged through the second discharge line 6.
The specific process control conditions for producing ultrapure ammonia using the ultrapure ammonia production apparatus of this example were as follows:
the raw material liquid anhydrous industrial ammonia comprises the following components: 0.4% of water, 12mg/kg of oil, 1mg/kg of iron, 0.099% of methane, 0.0012% of ethane and 0.0016% of propane, wherein the content of ammonia is 99.6%; the flow rate of liquid ammonia is 250 kg/h;
an evaporator 11: the diameter D is 500mm, the height H is 800mm, the temperature in the evaporator 11 is 10-40 ℃, and the pressure is 0.1-2 kPaG; after one separation, the first light component comprises the following components: 0.66% of water, 1.8mg/kg of oil, 0.3mg/kg of iron, 0.002% of oxygen, 0.164% of methane, 0.0026% of ethane and 0.0013% of propane, wherein the content of ammonia is 99.86%;
a heating system 2, namely the temperature of hot water in a reboiler is 50-80 ℃;
the dividing wall tower 3: the height is 18m, the temperature in the next door tower 3 is-3 to 25 ℃, and the pressure is 0.1 to 0.6 MpaG; the reflux ratio is 1:3, and after the secondary separation, the ammonia content of the ultrapure ammonia is 99.99999 percent, wherein the content of hydrogen, oxygen and alkane gases is less than 0.001 percent, and the yield of the ultrapure ammonia is 150 kg/h.
Example 2
The difference from the embodiment 1 is that each evaporator group 1 is composed of 8 evaporators 11 connected in series, and other devices and the connection relationship between the devices are the same. The specific process control conditions for producing ultrapure ammonia using the ultrapure ammonia production apparatus of this example were as follows:
the raw material liquid anhydrous industrial ammonia comprises the following components: 0.1% of water, 5mg/kg of oil, 1mg/kg of iron, 0.099% of methane, 0.0005% of ethane and 0.0004% of propane, wherein the ammonia content is 99.9%; the flow rate of liquid ammonia is 347 kg/h;
an evaporator 11: the diameter D is 500mm, the height H is 800mm, the temperature in the evaporator 11 is 10-40 ℃, and the pressure is 0.1-2 kPaG; after one separation, the first light component comprises the following components: 0.16% of water, 0.3mg/kg of oil, 0.3mg/k of iron, 0.123% of methane, 0.0006% of ethane and 0.0003% of propane, wherein the ammonia content is 99.99%;
a heating system 2, namely the temperature of hot water in a reboiler is 50-80 ℃;
the dividing wall tower 3: the height is 18m, the temperature in the next door tower 3 is-3 to 25 ℃, and the pressure is 0.1 to 0.6 MpaG; after the secondary separation, the ammonia content of the ultrapure ammonia is 99.99999 percent, wherein the content of hydrogen, oxygen and alkane gases is less than 0.001 percent, and the yield of the ultrapure ammonia is 260 kg/h.
Example 3
The difference between the evaporator group 1 and the evaporator group 1 of the embodiment 1 and the embodiment 2 is that each evaporator group is composed of 12 evaporators 11 which are connected in series, and the other devices and the connection relationship between the devices are the same. The specific process control conditions for producing ultrapure ammonia using the ultrapure ammonia production apparatus of this example were as follows:
the raw material liquid anhydrous industrial ammonia comprises the following components: 0.36% of water, 14mg/kg of oil, 1.1mg/kg of iron, 0.095% of methane, 0.0011% of ethane and 0.0013% of propane, wherein the content of ammonia is 99.7%; the flow rate of liquid ammonia is 500 kg/h;
an evaporator 11: the diameter D is 500mm, the height H is 800mm, the temperature in the evaporator 11 is 10-40 ℃, and the pressure is 0.1-2 kPaG; after one separation, the first light component comprises the following components: 0.53% of water, 1.4mg/kg of oil, 0.2mg/kg of iron, 0.175% of methane, 0.0029% of ethane and 0.0011% of propane, wherein the content of ammonia is 99.91%;
a heating system 2, namely the temperature of hot water in a reboiler is 50-80 ℃;
the dividing wall tower 3: the height is 18m, the temperature in the next door tower 3 is-3 to 25 ℃, and the pressure is 0.1 to 0.6 MpaG; after the secondary separation, the ammonia content of the ultrapure ammonia is 99.99999 percent, wherein the contents of hydrogen, oxygen and alkane gases are less than 0.001 percent, the yield of the ultrapure ammonia is 400kg/h, and the annual yield reaches 3200 tons.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (10)
1. An apparatus for producing ultrapure ammonia, comprising:
the evaporator group is formed by connecting at least two evaporators in series, and the two adjacent evaporators are communicated through an overflow series pipeline; a liquid ammonia feed port is formed in the lower portion of the side wall of each evaporator; a first heavy component discharge port is formed in the bottom of each evaporator; the top of each evaporator is provided with a first light component discharge port;
a heating system for providing heat to the vaporizer to vaporize liquid ammonia; and
a divided wall column communicating with the first light component discharge port of the evaporator; the top of the partition wall tower is provided with a second light component discharge port and an ultra-pure ammonia discharge port; and a second heavy component discharge port is formed at the bottom of the partition wall tower.
2. The apparatus of claim 1, further comprising a parallel adsorption and desorption unit in communication with the second light component discharge port.
3. The apparatus of claim 1, wherein the heating system is a reboiler in heat exchange relationship with the bottom of each of the evaporators.
4. The apparatus for producing ultrapure ammonia according to claim 1, wherein a filler layer is provided in the upper part of each of said evaporators, and said second dense component discharge port is communicated with the top of each of said evaporators.
5. The apparatus of claim 4, wherein each of the overflow cascade pipes has a reflux inlet, and wherein the reflux inlet is in communication with the top of the evaporator upstream thereof.
6. The apparatus for producing ultrapure ammonia according to any one of claims 1 to 5 wherein at least two evaporator groups are provided, each evaporator group being connected in parallel to the dividing wall column.
7. The apparatus for producing ultrapure ammonia according to any one of claims 1 to 5, wherein the bottom of each of the evaporators is of a conical bottom configuration.
8. The method for producing ultrapure ammonia according to any one of claims 1 to 7, comprising the steps of:
liquid ammonia is separated into a first light component and a first heavy component through the evaporator group, and the first heavy component is discharged through a first oil discharge pipeline;
the first light component enters the partition wall tower for secondary separation, and a second light component, ultra-pure ammonia and a second heavy component are separated; the second light component is discharged through a light discharge pipeline, and the second heavy component is discharged through a second oil discharge pipeline; part of the ultrapure ammonia is condensed and then flows back to the top of the bulkhead tower.
9. The method of claim 8, further comprising the steps of: and the second light component is treated by the parallel adsorption and desorption device and then discharged through a light discharge pipeline.
10. The method of claim 9, wherein a portion of the second reformate is returned to the top of the vaporizer.
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