CN112299445A - Method for preparing ultra-pure ammonia by filler rectification - Google Patents
Method for preparing ultra-pure ammonia by filler rectification Download PDFInfo
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- CN112299445A CN112299445A CN202011309150.2A CN202011309150A CN112299445A CN 112299445 A CN112299445 A CN 112299445A CN 202011309150 A CN202011309150 A CN 202011309150A CN 112299445 A CN112299445 A CN 112299445A
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- 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
Abstract
The invention provides a method for preparing ultra-pure ammonia by rectifying a filler, which comprises the following steps: removing solid particles from raw material ammonia, and then sequentially introducing the raw material ammonia into a first-stage packed tower and a second-stage packed tower for rectification to obtain 7N-stage ultra-pure ammonia; composite fillers are loaded in the first-stage packed tower and the second-stage packed tower; the composite packing comprises regular packing and small-size phi ring packing filled in the regular packing; the structured packing is obtained by overlapping and assembling a plurality of corrugated metal plates; the phi ring packing has the size of 2 x 2 mm-4 x 4mm, and the volume ratio of the regular packing to the small phi ring packing is (3-7): 1. the invention can effectively reduce the operating pressure of the rectifying tower, has higher separation efficiency than that of a regular packing, can remove water to below 10ppb without adsorption and catalysis processes in the purification process, has lower rectifying operating pressure, is beneficial to removing hydrogen, oxygen, nitrogen, argon and carbon monoxide, and can obtain 7N-level liquid ammonia by two-stage rectification.
Description
Technical Field
The invention belongs to the technical field of organic matter purification, and particularly relates to a method for preparing ultrapure ammonia by filler rectification.
Background
Field of electronic gases, ultra-high purity ammonia (NH) in semiconductor production processes3) Is an important nitrogen source for Chemical Vapor Deposition (CVD), semiconductor chip, and light emissionA large amount of ultra-high purity ammonia is required in the fabrication of diodes (LEDs) and flat panel display devices. Ammonia and Silane (SiH)4) The ammonia and the trimethylgallium act on the sapphire to form the gallium nitride light-emitting diode through vapor phase growth on MOCVD equipment, along with the rapid development of the microelectronic industry, the ultra-large scale integrated circuit and the light-emitting diode manufacturing technology are greatly leaped, even trace impurities in a deposited film can cause the reduction of the quality and the performance of the film, and finally cause the scrapping of a device, and the loss is extremely large, so the requirement of the ammonia raw material of the silicon nitride film must reach 7N-level (99.99999 percent volume fraction) ultra-high purity.
The production process of the ultra-pure ammonia is earlier developed abroad, more successful experiences are introduced into Calex, Japanese Sumitomo chemistry, Showa electrician and the like, and taking the Calex as an example, the process for obtaining 7N-grade ultra-pure ammonia from the ultra-pure ammonia through industrial ammonia mainly comprises the steps of removing oxygen through chemical water catalysis, and simultaneously assisting a getter purification method to achieve the aim of purifying. With the increasing demand of domestic ultrapure ammonia, at present, domestic ultrapure ammonia production processes are also available. Patent CN107777703A discloses a purification method for ultra-pure ammonia full-temperature range adsorption extraction deep dehydration impurity removal, which comprises the steps of obtaining 5N-grade (volume fraction of more than or equal to 99.999%) liquid ammonia by using industrial-grade liquid ammonia through a pretreatment process, entering a liquid phase adsorption process, absorbing moisture and trace impurities in raw materials, and then removing oxygen and nitrogen-dominant impurities through a rectification process to obtain 7N-grade ultra-pure liquid ammonia. Patent CN106315620A discloses an ultrapure ammonia purification device and purification method, wherein raw material liquid ammonia is gasified to form ammonia gas, and then the ammonia gas is subjected to oil removal and filtration, and enters a rectification system to remove water, oxygen and nitrogen and other impurities to obtain 7N-grade liquid ammonia.
In the method, the absorption and catalysis mode is adopted for impurity removal, particle pollution is easy to introduce, the treatment capacity is small, the adsorption pressure is up to 4MPa, a large ammonia leakage risk exists, and if the treatment capacity is increased, the equipment investment of the absorption and catalysis tower is high and the equipment size is large. The type of a rectifying tower or the type of a packing used for rectifying and purifying is not determined in the rectifying mode, and the rectifying pressure is higher and is usually more than 1.5 MPa; is not beneficial to the popularization of the ultra-pure ammonia process technology.
Disclosure of Invention
The invention provides a method for preparing ultrapure ammonia by filler rectification, which can effectively reduce the operating pressure of a rectification tower, can obtain 7N-grade liquid ammonia by two-stage rectification, and has the advantages of simple production process and convenient operation.
The invention provides a method for preparing ultra-pure ammonia by rectifying a filler, which comprises the following steps:
removing solid particles from raw material ammonia, and then sequentially introducing the raw material ammonia into a first-stage packed tower and a second-stage packed tower for rectification to obtain 7N-stage ultra-pure ammonia;
composite fillers are loaded in the first-stage packed tower and the second-stage packed tower;
the composite packing comprises regular packing and small-size phi ring packing filled in the regular packing;
the structured packing is obtained by overlapping and assembling a plurality of corrugated metal plates; the phi ring packing has the size of 2 x 2 mm-4 x 4mm, and the volume ratio of the regular packing to the small phi ring packing is (3-7): 1.
preferably, the corrugated metal plate has 3-5 mm holes and an aperture ratio of 90-98%.
Preferably, the holes on the corrugated metal plate are arranged in a triangular shape, and the hole pitch is 10-15 mm.
Preferably, the inclination angle of the corrugations of the surface of the corrugated metal plate is 30-45 degrees with the vertical axis direction.
Preferably, the height of the corrugated metal plate is 40-250 mm.
Preferably, the small-size phi ring packing is filled between any two corrugated metal plates.
Preferably, the rectification conditions in the first packed column are as follows:
the rectification operating pressure is 0.8-1.2 Mpa, and the tower top temperature is 18-32 ℃.
Preferably, the rectification conditions in the two-stage packed column are as follows:
the operation pressure is 0.6-1 Mpa, and the tower top temperature is 10-28 ℃.
The invention provides a method for preparing ultra-pure ammonia by rectifying a filler, which comprises the following steps: removing solid particles from raw material ammonia, and then sequentially introducing the raw material ammonia into a first-stage packed tower and a second-stage packed tower for rectification to obtain 7N-stage ultra-pure ammonia; composite fillers are loaded in the first-stage packed tower and the second-stage packed tower; the composite packing comprises regular packing and small-size phi ring packing filled in the regular packing; the structured packing is obtained by overlapping and assembling a plurality of corrugated metal plates; the phi ring packing has the size of 2 x 2 mm-4 x 4mm, and the volume ratio of the regular packing to the small phi ring packing is (3-7): 1. the invention can effectively reduce the operating pressure of the rectifying tower, has higher separation efficiency than that of a regular filler, can remove water to below 10ppb without adsorption and catalysis in the purification process, has lower rectifying operating pressure, is beneficial to removing hydrogen, oxygen, nitrogen, argon and carbon monoxide, can obtain 7N-level liquid ammonia by two-level rectification, and has simple production flow and convenient operation.
Detailed Description
The invention provides a method for preparing ultra-pure ammonia by rectifying a filler, which comprises the following steps:
removing solid particles from raw material ammonia, and then sequentially introducing the raw material ammonia into a first-stage packed tower and a second-stage packed tower for rectification to obtain 7N-stage ultra-pure ammonia;
composite fillers are loaded in the first-stage packed tower and the second-stage packed tower;
the composite packing comprises regular packing and small-size phi ring packing filled in the regular packing;
the structured packing is obtained by overlapping and assembling a plurality of corrugated metal plates; the phi ring packing has the size of 2 x 2 mm-4 x 4mm, and the volume ratio of the regular packing to the small phi ring packing is (3-7): 1.
at present, for raw material ammonia with high water content, the water content is difficult to be removed to a very low level, the invention adopts a novel packing tower, and the small-size packing is dispersedly filled in the regular packing by utilizing the characteristics of low pressure drop of the regular packing, high separation efficiency of the small-size random packing and suitability for higher pressure operation, so that the operation pressure of a rectifying tower can be effectively reduced, the packing efficiency is high, the gas-liquid distribution condition in the rectifying tower is greatly improved, the gas-liquid contact is more sufficient, the water content can be removed to be below 10ppb, the operation pressure in the rectifying process is below 1.2ppm, the removal of hydrogen, oxygen, nitrogen, argon and carbon monoxide is easier, and the purification process does not need an adsorption catalysis process.
In the invention, the structured packing is preferably formed by overlapping and assembling a plurality of corrugated metal plates, and the height of each corrugated metal plate is preferably 40-250 mm, more preferably 50-200 mm, and most preferably 100-150 mm; a plurality of through holes with the thickness of 3-5 mm are distributed on the corrugated metal plate, the through holes are arranged in a triangular mode, and the hole pitch of the through holes is preferably 10-15 mm, and more preferably 12-14 mm; the aperture ratio of the corrugated metal plate is preferably 90 to 98%, and more preferably 92 to 96%.
In the present invention, the corrugations of the corrugated metal plate have an inclination angle of 30 to 45 degrees, preferably 35 to 40 degrees, with respect to the axial direction.
When a plurality of corrugated metal plates with the structure are superposed and assembled, small-size phi ring wire mesh packing is filled between any two corrugated metal plates, the corrugated metal plates are sequentially assembled, the small-size wire mesh packing is tightly pressed and compacted by using a special tool, and finally, a steel belt is used for fastening in the circumferential direction, so that the composite material is obtained.
In the present invention, the size of the phi-ring packing is preferably 2 × 2mm to 4 × 4mm, more preferably 2 × 2mm to 3 × 3 mm; the volume ratio of the regular packing to the small-size phi ring packing is (3-7): 1, more preferably (4-6): 1, most preferably 5: 1.
After the composite filler is assembled, the surface of the assembled composite filler is degreased and cleaned for later use.
The treated regular packing is placed in a first-stage packing tower and a second-stage packing tower according to the packing placing and cleaning standards, and is filled in sections, and each disc of packing is placed in a 90-degree staggered mode and cleaned.
Then introducing the industrial ammonia raw material without the solid particles into a first-stage packed tower and a second-stage packed tower in sequence, and performing first-stage rectification and second-stage rectification in sequence.
In the invention, the operation pressure of the primary rectification is preferably 0.8-1.2 MPa, more preferably 0.9-1.1 MPa, and most preferably 1.0MPa, and the tower top temperature is preferably 18-32 ℃, preferably 20-30 ℃, and most preferably 25-28 ℃; light component impurities such as oxygen, nitrogen, carbon monoxide and the like are removed from the top of the primary rectifying tower; removing water and metal ion impurities at the bottom of the tower.
Feeding the material at the bottom of the primary rectifying tower into a secondary rectifying tower, wherein the operating pressure of the secondary rectifying tower is preferably 0.6-1 MPa, more preferably 0.7-0.9 MPa, and most preferably 0.8 MPa; the tower top temperature is preferably 10-28 ℃, more preferably 12-25 ℃, and most preferably 15-20 ℃; and removing water, metal ions and high-boiling-point substances at the bottom of the secondary rectifying tower, condensing tower top material flow through a secondary condenser, then feeding the tower top material flow into a reflux tank, feeding a part of outlet of the reflux tank into the top of the secondary rectifying tower as reflux liquid, and extracting a part of outlet of the reflux tank to obtain a 7N-level liquid ammonia product.
The invention provides a method for preparing ultra-pure ammonia by rectifying a filler, which comprises the following steps: removing solid particles from raw material ammonia, and then sequentially introducing the raw material ammonia into a first-stage packed tower and a second-stage packed tower for rectification to obtain 7N-stage ultra-pure ammonia; composite fillers are loaded in the first-stage packed tower and the second-stage packed tower; the composite packing comprises regular packing and small-size phi ring packing filled in the regular packing; the structured packing is obtained by overlapping and assembling a plurality of corrugated metal plates; the phi ring packing has the size of 2 x 2 mm-4 x 4mm, and the volume ratio of the regular packing to the small phi ring packing is (3-7): 1. the invention can effectively reduce the operating pressure of the rectifying tower, has higher separation efficiency than that of a regular filler, can remove water to below 10ppb without adsorption and catalysis in the purification process, has lower rectifying operating pressure, is beneficial to removing hydrogen, oxygen, nitrogen, argon and carbon monoxide, can obtain 7N-level liquid ammonia by two-level rectification, and has simple production flow and convenient operation.
In order to further illustrate the present invention, the method for preparing ultra-pure ammonia by rectifying a filler provided by the present invention is described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
Selecting a disc with the height of 50mm, punching small holes with the diameter of 4mm on a metal corrugated plate sheet with a proper size, wherein the small holes are arranged in a triangular shape, the hole interval is 10mm, the hole opening rate is 92%, and rolling fine lines to remove burrs;
corrugating the corrugations to form 35 degree inclination angles with the axial direction;
when the regular packing is assembled, small-sized wire mesh packing is filled between two metal plate corrugations
Is/are as follows
Ring packing, structured packing and
the volume ratio of the ring packing is 4:1, the ring packing is assembled in sequence, a small-size silk screen packing is tightly pressed and compacted by using a special tool, finally, the small-size silk screen packing is pricked by using a steel belt in the circumferential direction, the regular packing filled with the small-size silk screen packing is manufactured, and the surface of the regular packing is degreased and cleaned;
the treated regular packing is placed in a packing tower according to the packing placement and treatment cleaning standards and is filled in sections, and each disc of packing is placed in a 90-degree staggered mode and cleaned;
removing solid particles from raw material industrial ammonia from a raw material storage tank through a filter by using a metering pump, and then sending the raw material industrial ammonia into a primary rectifying tower, wherein the rectifying operation pressure is 0.8Mpa, the tower top temperature is 18 ℃, and light component impurities such as oxygen, nitrogen, carbon monoxide and the like are removed from the tower top; removing water and metal ion impurities at the bottom of the tower;
the material at the bottom of the primary rectifying tower enters a secondary rectifying tower, the operating pressure of the secondary rectifying tower is 0.6Mpa, the temperature at the top of the tower is 10 ℃, water, metal ions and high-boiling-point substances are removed from the bottom of the secondary rectifying tower, the material flow at the top of the tower is condensed by a secondary condenser and then enters a reflux tank, one part of the outlet of the reflux tank enters the top of the secondary rectifying tower as reflux liquid, and the other part of the outlet of the reflux tank is extracted to obtain a 7N-level liquid ammonia product;
7N liquid ammonia product is at final entering steel bottle filling after the cold ware cooling, according to the dress weight of filling that sets for, reaches the regulation weight after, fills the automatic shutoff of valve, opens another and waits to fill the steel bottle. The product analysis results are shown in Table 1.
Example 2
Selecting the disc height of 120mm, punching small holes of 4mm on a metal corrugated plate sheet with a proper size, wherein the small holes are arranged in a triangular mode, the hole interval is 12mm, the opening rate is 94%, and rolling fine lines to remove burrs;
corrugating the corrugations to form 40 degree inclination angles with the axial direction;
when the regular packing is assembled, small-sized wire mesh packing is filled between two metal plate corrugations
Is/are as follows
Ring packing, structured packing and
the volume ratio of the ring packing is 5:1, the ring packing is assembled in sequence, a special tool is used for tightly pressing and compacting the small-size silk screen packing, finally, a steel belt is used for pricking in the circumferential direction, the regular packing filled with the small-size silk screen packing is manufactured, and the surface is degreased and cleaned;
the treated regular packing is placed in a packing tower according to the packing placement and treatment cleaning standards and is filled in sections, and each disc of packing is placed in a 90-degree staggered mode and cleaned;
removing solid particles from raw material industrial ammonia from a raw material storage tank through a filter by using a metering pump, and then sending the raw material industrial ammonia into a primary rectifying tower, wherein the rectifying operation pressure is 1.0Mpa, the tower top temperature is 25 ℃, and light component impurities such as oxygen, nitrogen, carbon monoxide and the like are removed from the tower top; removing water and metal ion impurities at the bottom of the tower;
the material at the bottom of the primary rectifying tower enters a secondary rectifying tower, the operating pressure of the secondary rectifying tower is 0.8Mpa, the temperature at the top of the tower is 18 ℃, water, metal ions and high-boiling-point substances are removed from the bottom of the secondary rectifying tower, the material flow at the top of the tower is condensed by a secondary condenser and then enters a reflux tank, one part of the outlet of the reflux tank enters the top of the secondary rectifying tower as reflux liquid, and the other part of the outlet of the reflux tank is extracted to obtain a 7N-level liquid ammonia product;
7N liquid ammonia product is at final entering steel bottle filling after the cold ware cooling, according to the dress weight of filling that sets for, reaches the regulation weight after, fills the automatic shutoff of valve, opens another and waits to fill the steel bottle. The product analysis results are shown in Table 1.
Example 3
Selecting a disc with the height of 200mm, punching small holes with the diameter of 4mm on a metal corrugated plate sheet with a proper size, wherein the small holes are arranged in a triangular mode, the hole interval is 15mm, the hole opening rate is 96%, and rolling fine lines to remove burrs;
corrugating the corrugations to form 40 degree inclination angles with the axial direction;
when the regular packing is assembled, small-sized wire mesh packing is filled between two metal plate corrugations
Is/are as follows
Ring packing, structured packing and
the volume ratio of the ring packing is 5:1, the ring packing is assembled in sequence, a special tool is used for tightly pressing and compacting the small-size silk screen packing, finally, a steel belt is used for pricking in the circumferential direction, the regular packing filled with the small-size silk screen packing is manufactured, and the surface is degreased and cleaned;
the treated regular packing is placed in a packing tower according to the packing placement and treatment cleaning standards and is filled in sections, and each disc of packing is placed in a 90-degree staggered mode and cleaned;
removing solid particles from raw material industrial ammonia from a raw material storage tank through a filter by using a metering pump, and then sending the raw material industrial ammonia into a primary rectifying tower, wherein the rectifying operation pressure is 1.2Mpa, the tower top temperature is 28 ℃, and light component impurities such as oxygen, nitrogen, carbon monoxide and the like are removed from the tower top; removing water and metal ion impurities at the bottom of the tower;
the material at the bottom of the primary rectifying tower enters a secondary rectifying tower, the operating pressure of the secondary rectifying tower is 1Mpa, the temperature at the top of the tower is 20 ℃, water, metal ions and high-boiling-point substances are removed from the bottom of the secondary rectifying tower, the material flow at the top of the tower is condensed by a secondary condenser and then enters a reflux tank, one part of the material at the outlet of the reflux tank enters the top of the secondary rectifying tower as reflux liquid, and the other part of the material at the outlet of the reflux tank is extracted to obtain a 7;
7N liquid ammonia product is at final entering steel bottle filling after the cold ware cooling, according to the dress weight of filling that sets for, reaches the regulation weight after, fills the automatic shutoff of valve, opens another and waits to fill the steel bottle. The product analysis results are shown in Table 1.
Comparative example 1
Selecting the disc height of 120mm, punching small holes of 4mm on a metal corrugated plate sheet with a proper size, wherein the small holes are arranged in a triangular mode, the hole interval is 12mm, the opening rate is 94%, and rolling fine lines to remove burrs;
pressing the corrugations to enable the corrugations and the axial direction to form an inclination angle of 40 degrees, and assembling the regular packing;
the treated regular packing is placed in a packing tower according to the packing placement and treatment cleaning standards and is filled in sections, and each disc of packing is placed in a 90-degree staggered mode and cleaned;
removing solid particles from raw material industrial ammonia from a raw material storage tank through a filter by using a metering pump, and then sending the raw material industrial ammonia into a primary rectifying tower, wherein the rectifying operation pressure is 1.0Mpa, the tower top temperature is 25 ℃, and light component impurities such as oxygen, nitrogen, carbon monoxide and the like are removed from the tower top; removing water and metal ion impurities at the bottom of the tower;
the material at the bottom of the primary rectifying tower enters a secondary rectifying tower, the operating pressure of the secondary rectifying tower is 0.8Mpa, the temperature at the top of the tower is 18 ℃, water, metal ions and high-boiling-point substances are removed from the bottom of the secondary rectifying tower, the material flow at the top of the tower is condensed by a secondary condenser and then enters a reflux tank, one part of the outlet of the reflux tank enters the top of the secondary rectifying tower as reflux liquid, and the other part of the outlet of the reflux tank is extracted to obtain a 7N-level liquid ammonia product;
7N liquid ammonia product is at final entering steel bottle filling after the cold ware cooling, according to the dress weight of filling that sets for, reaches the regulation weight after, fills the automatic shutoff of valve, opens another and waits to fill the steel bottle. The product analysis results are shown in Table 1.
Comparative example 2
The treated small-sized silk screen filler is placed according to the filler placement and treatment cleaning standard
Is/are as follows
The ring packing is placed in a packing tower and filled in sections, and each section of packing is placed in a 90-degree staggered mode and cleaned;
removing solid particles from raw material industrial ammonia from a raw material storage tank through a filter by using a metering pump, and then sending the raw material industrial ammonia into a primary rectifying tower, wherein the rectifying operation pressure is 1.0Mpa, the tower top temperature is 25 ℃, and light component impurities such as oxygen, nitrogen, carbon monoxide and the like are removed from the tower top; removing water and metal ion impurities at the bottom of the tower;
the material at the bottom of the primary rectifying tower enters a secondary rectifying tower, the operating pressure of the secondary rectifying tower is 0.8Mpa, the temperature at the top of the tower is 18 ℃, water, metal ions and high-boiling-point substances are removed from the bottom of the secondary rectifying tower, the material flow at the top of the tower is condensed by a secondary condenser and then enters a reflux tank, one part of the outlet of the reflux tank enters the top of the secondary rectifying tower as reflux liquid, and the other part of the outlet of the reflux tank is extracted to obtain a 7N-level liquid ammonia product;
7N liquid ammonia product is at final entering steel bottle filling after the cold ware cooling, according to the dress weight of filling that sets for, reaches the regulation weight after, fills the automatic shutoff of valve, opens another and waits to fill the steel bottle. The product analysis results are shown in Table 1.
TABLE 1 ultra pure Ammonia product component content in the inventive examples
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method for preparing ultra-pure ammonia by rectifying filler comprises the following steps:
removing solid particles from raw material ammonia, and then sequentially introducing the raw material ammonia into a first-stage packed tower and a second-stage packed tower for rectification to obtain 7N-stage ultra-pure ammonia;
composite fillers are loaded in the first-stage packed tower and the second-stage packed tower;
the composite packing comprises regular packing and small-size phi ring packing filled in the regular packing;
the structured packing is obtained by overlapping and assembling a plurality of corrugated metal plates; the phi ring packing has the size of 2 x 2 mm-4 x 4mm, and the volume ratio of the regular packing to the small phi ring packing is (3-7): 1.
2. the method according to claim 1, wherein the corrugated metal sheet has 3 to 5mm holes with an open porosity of 90 to 98%.
3. The method according to claim 1, wherein the holes of the corrugated metal sheet are arranged in a triangular pattern with a pitch of 10 to 15 mm.
4. The method of claim 1, wherein the corrugations of the corrugated metal sheet surface are inclined at an angle of 30 to 45 ° to the vertical axis.
5. The method according to claim 1, wherein the height of the corrugated metal sheet is 40 to 250 mm.
6. The method of claim 1 wherein said small size phi hoop filler is filled between any two of said corrugated metal sheets.
7. The method of claim 1, wherein the rectification conditions within the first packed column are as follows:
the rectification operating pressure is 0.8-1.2 Mpa, and the tower top temperature is 18-32 ℃.
8. The method of claim 1, wherein the rectification conditions within the two-stage packed column are as follows:
the operation pressure is 0.6-1 Mpa, and the tower top temperature is 10-28 ℃.
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| JPH09286613A (en) * | 1996-04-19 | 1997-11-04 | Nippon Steel Chem Co Ltd | Production of high purity alumina and mullite for electronic material |
| JP2002316816A (en) * | 2001-04-19 | 2002-10-31 | Mitsui Chemicals Inc | Method for separating ammonia by distillation |
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