CN111547690B - High-purity electronic grade nitric oxide production device - Google Patents
High-purity electronic grade nitric oxide production device Download PDFInfo
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- CN111547690B CN111547690B CN202010564415.7A CN202010564415A CN111547690B CN 111547690 B CN111547690 B CN 111547690B CN 202010564415 A CN202010564415 A CN 202010564415A CN 111547690 B CN111547690 B CN 111547690B
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 70
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 62
- 238000000746 purification Methods 0.000 claims abstract description 56
- 230000018044 dehydration Effects 0.000 claims abstract description 47
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 47
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 29
- 238000010521 absorption reaction Methods 0.000 claims abstract description 27
- 238000001179 sorption measurement Methods 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 18
- 239000000741 silica gel Substances 0.000 claims abstract description 18
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 18
- 239000010959 steel Substances 0.000 claims abstract description 18
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000001110 calcium chloride Substances 0.000 claims abstract description 12
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000003860 storage Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 101
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 239000000919 ceramic Substances 0.000 claims description 16
- 239000003513 alkali Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000003463 adsorbent Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 7
- 230000000149 penetrating effect Effects 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229910001868 water Inorganic materials 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012840 feeding operation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/24—Nitric oxide (NO)
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Gases By Adsorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a high-purity electronic grade nitric oxide production device, which comprises a sulfuric acid storage tank, wherein the sulfuric acid storage tank is respectively connected with a first reaction kettle and a second reaction kettle which are the same in structure through sulfuric acid pipelines, a sulfuric acid metering pump is further arranged on the sulfuric acid pipelines, stirring blades driven by a stirring motor are arranged in the first reaction kettle, a safety valve and a pressure gauge are further arranged on the first reaction kettle, the outlet ends of the first reaction kettle and the second reaction kettle are respectively connected with the inlet end of a dehydration absorption tower through reaction kettle pipelines, the outlet end of the dehydration absorption tower is connected with the inlet of a low-temperature dynamic adsorption purification device through absorption tower pipelines, the outlet end of the low-temperature dynamic adsorption purification device is sequentially connected with a calcium chloride dehydration tank and a silica gel dehydration tank through pipelines, the outlet end of the silica gel dehydration tank is respectively connected with two finished product bottle groups which are the same in structure through pipelines, and the finished product bottle groups comprise a finished product gas steel bottle and a finished product gas aluminum alloy bottle.
Description
Technical Field
The invention relates to the field of gas treatment, in particular to a high-purity electronic grade nitric oxide production device.
Background
Nitric oxide is a special gas widely applied to the fields of medicine, electronics, scientific research, environmental protection, fine chemical industry and the like, is an important gas in the electronic semiconductor industry, and is mainly used for forming, oxidizing and chemical vapor deposition of an oxide film of silicon.
With the rapid development of the electronic semiconductor industry, especially the improvement of the electronic semiconductor production technology and the improvement of the process and the technology in recent years, integrated circuits are updated for about three years; the advent of mass production and use of large-scale integrated circuits and computers, optical fiber communication, digital communication, and satellite communication technologies has made the electronic semiconductor industry a high-tech industry that has driven technological development.
The rapid development of the electronic semiconductor industry has also led to unprecedented developments in the gas industry. The improvement of the electronic semiconductor production technology and the improvement of the process and the technology greatly improve the requirements on the purity of the nitric oxide gas, the process requirements can be met only by the electronic grade nitric oxide with the purity of 99.999 percent, and the parameters of various impurities in the impurity indexes of the electronic grade nitric oxide with the purity of 99.999 percent are required to meet the following requirements: less than N 2 O/1ppm ,NO 2 /1PPM ,CO 2 /1PPM ,H 2 O/0.5ppm,N 2 /3ppm,O 2 0.5ppm. While the nitric oxide produced by the traditional nitric oxide production method and equipment cannot meet the requirementFront-end semiconductor development. There is thus a need for a method or apparatus that solves the above-mentioned problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a device which has a simple structure and a smart design and can obtain high-purity nitric oxide gas after multistage treatment.
The technical scheme of the invention is as follows: a high purity electronic grade nitric oxide production device, characterized in that: the device comprises a sulfuric acid storage tank 1, the sulfuric acid storage tank 1 is respectively connected with a first reaction kettle 2 and a second reaction kettle 3 which are the same in structure in parallel through sulfuric acid pipelines, a sulfuric acid metering pump 4 is further arranged on the sulfuric acid pipelines, stirring blades driven by a stirring motor are arranged in the first reaction kettle 2, a safety valve and a pressure gauge are further arranged on the first reaction kettle 2, the outlet ends of the first reaction kettle 2 and the second reaction kettle 3 are respectively connected with the inlet end of a dehydration absorption tower 5 through reaction kettle pipelines, the outlet end of the dehydration absorption tower 5 is connected with the inlet of a low-temperature dynamic adsorption purification device 6 through absorption tower pipelines, the outlet end of the low-temperature dynamic adsorption purification device 6 is sequentially connected with a calcium chloride dehydration tank 7 and a silica gel dehydration tank 8 through pipelines, the outlet end of the silica gel dehydration tank 8 is respectively connected with two finished product bottle groups which are the same in structure through pipelines, each finished product bottle group comprises a finished product gas steel bottle 9 and a finished product gas aluminum alloy bottle 10, the finished product gas aluminum alloy bottle 10 is placed in a liquid nitrogen bath 11 filled with liquid nitrogen, simultaneously, the finished product bottle group further comprises a finished product gas alloy bottle 12 capable of detecting the pressure gauge 12 and the finished product gas aluminum alloy bottle 10,
the device also comprises an evacuating vacuum pipeline which is communicated with the first reaction kettle 2, the second reaction kettle 3, the dehydration absorption tower 5, the low-temperature dynamic adsorption purification device 6, the calcium chloride dehydration tank 7, the silica gel dehydration tank 8, the product gas steel bottle 9 and the product gas aluminum alloy bottle 10, the tail end of the evacuating vacuum pipeline is connected with a vacuum pipeline 15 with an evacuating pipeline 13 and a vacuum pump 14 in parallel,
the sulfuric acid pipeline, the reaction kettle pipeline, the absorption tower pipeline, the pipeline between the low-temperature dynamic adsorption purification device 6 and the calcium chloride dehydration tank 7 as well as the pipeline between the silica gel dehydration tank 8 and the finished product bottle group, the pipeline between the evacuation vacuum pipeline and each device, the evacuation pipeline 13 and the vacuum pipeline 15 are respectively provided with a pneumatic valve,
the dehydration absorption tower comprises a bracket 5-1, a tank body 5-2 is supported at the top of the bracket 5-1, a discharging pipeline 5-4 with a discharging valve 5-3 is connected at the bottom of the tank body 5-2, an air inlet pipe 5-5 with a valve is connected at the bottom of the tank body 5-2, the part of the air inlet pipe 5-5, which is positioned in the inner cavity of the tank body 5-2, is annular, a plurality of air inlets are uniformly distributed on the annular part, the direction of the air inlets is downward, an alkali liquor pipe 5-6 with a valve is connected at the middle part of the tank body 5-2, a feed inlet pipeline 5-7 is arranged at the top of the tank body 5-2, a flange blind plate 5-8 is also arranged at the tail end of the feed inlet pipeline 5-7, alkali liquor is contained in the tank body 5-2, the cavity above the alkali liquor is filled with PP multi-surface hollow balls 5-9, the top outlet of the tank 5-2 is connected with the bottom end of the extension part 5-10 through a flange structure, a screen 5-11 is arranged at the top outlet of the tank 5-2, a central pipe 5-12 is arranged at the center of the extension part 5-10, the bottom end opening of the central pipe 5-12 is communicated with the top outlet of the tank 5-2, a sleeve 5-13 with a downward opening direction is arranged outside the central pipe 5-12, the sleeve 5-13 is connected with the inner wall of the extension part 5-10 through a plurality of connecting pieces, a gap is reserved between the top end of the central pipe 5-12 and the top inner wall of the sleeve 5-13, a gap is reserved between the bottom end of the sleeve 5-13 and the bottom plate of the extension part 5-10, the top end of the extension part 5-10 is connected with an air outlet pipeline 5-15 with an air outlet valve 5-14,
the low-temperature dynamic adsorption purification device comprises a first low-temperature tank 6-1 and a second low-temperature tank 6-2, wherein heat preservation layers 6-3 are arranged at the inner walls of the first low-temperature tank 6-1 and the second low-temperature tank 6-2, a first purification tank 6-4 is arranged in an inner cavity of the first low-temperature tank 6-1, a first air inlet pipeline 6-5 with a pneumatic valve is connected to the first low-temperature tank 6-1 in a penetrating way, a first nitrogen pipeline 6-6 with the pneumatic valve is connected to the first air inlet pipeline 6-5 in parallel, the bottom end of the first air inlet pipeline 6-5 is communicated with the bottom of the first purification tank 6-4, a ceramic adsorbent 6-7 is filled in the first purification tank 6-4, a first air outlet pipeline 6-9 with an online ceramic gas filter 6-8 is connected to the top end of the first purification tank 6-4, the pneumatic valve is also arranged on the first air outlet pipeline 6-9,
the second cryogenic tank 6-2 is connected with a second air inlet pipeline 6-10 in a penetrating way, the second air inlet pipeline 6-10 is communicated with the first air outlet pipeline 6-9 through a connecting pipeline with a pneumatic valve, the second air inlet pipeline 6-10 is also connected with a second nitrogen pipeline 6-11 with a pneumatic valve in parallel, the bottom end of the second air inlet pipeline 6-10 is communicated with the top end opening of a coil pipe 6-12 positioned in the second cryogenic tank 6-2, the bottom end outlet of the coil pipe 6-12 is positioned at the bottom of the inner cavity of the second purifying tank 6-13, the second purifying tank 6-13 is arranged in the second cryogenic tank 6-2, the second purifying tank 6-13 is also filled with a ceramic adsorbent 6-7, the top end of the second purifying tank 6-13 is connected with a second air outlet pipeline 6-14 with an on-line ceramic gas filter 6-8, the second air outlet pipeline 6-14 is also provided with a pneumatic valve, and the second air outlet pipeline 6-14 is connected with a vacuum valve with a pneumatic valve in parallel,
the device also comprises a low-temperature constant-temperature circulation unit 6-16, the low-temperature constant-temperature circulation unit 6-16 is respectively connected with the inner cavities of the first low-temperature tank 6-1 and the second low-temperature tank 6-2, mediums circulate in the low-temperature constant-temperature circulation unit 6-16, the first low-temperature tank 6-1 and the second low-temperature tank 6-2,
safety pipelines with safety valves 6-17 are arranged on the first low-temperature tank 6-1 and the second low-temperature tank 6-2,
the bottom ends of the first purification tank 6-4 and the second purification tank 6-13 are respectively connected with a drainage pipeline 6-18, a drainage valve 6-19 is arranged on the drainage pipeline 6-18, and bottom end outlets of the drainage valve 6-19 and the drainage pipeline 6-18 are respectively positioned outside the first low-temperature tank 6-1 or the second low-temperature tank 6-2.
Compared with the prior art, the invention has the following advantages:
the high-purity electronic grade nitric oxide production device in the structural form comprises two reaction kettles, so that one reaction kettle can be used for production during production, and the other reaction kettle can be used for discharging and filling materials, thereby greatly saving time; meanwhile, the device also comprises two sets of finished product bottle groups, wherein each set of finished product bottle group consists of a finished product gas steel bottle and a finished product gas aluminum alloy bottle arranged in a liquid nitrogen bath, so that when the device is filled, one set of finished product bottle groups is frozen, and the other set of finished product bottle groups can be heated and filled for continuous filling operation; the device adopts a skid-mounted design, all equipment is arranged on a base, and the device can supply goods in a modularized manner, is integrally arranged and moved, is compact in design and occupies a small area; the vacuum pump in the device can pump the vacuum degree in the reaction kettle to be less than 1Pa; meanwhile, the nitrogen monoxide gas is frozen by placing a finished gas aluminum alloy bottle in a liquid nitrogen bath, and the finished gas steel bottle is reversely filled with the special gas structure after the temperature is raised. The device does not need to be filled by a traditional molding press, avoids the pollution possibly generated by the molding press, and has relatively low cost; the generated nitric oxide gas is purified by a dehydration absorption tower with a special structure and a low-temperature dynamic adsorption purification device, and is further dehydrated by a calcium chloride dehydration tank and a silica gel dehydration tank, so that the high-purity nitric oxide gas meeting the electronic grade requirement can be finally obtained. In conclusion, the device has various advantages, is particularly suitable for popularization and application in the field, and has very broad market prospect.
Drawings
Fig. 1 is a schematic overall structure of an embodiment of the present invention.
FIG. 2 is a schematic diagram showing the structure of a dehydration absorption column section in the embodiment of the present invention.
FIG. 3 is a schematic diagram of a low temperature dynamic adsorption purification device according to an embodiment of the present invention.
Detailed Description
Specific embodiments of the present invention will be described below with reference to the accompanying drawings. As shown in fig. 1 to 3: the high-purity electronic grade nitric oxide production device comprises a sulfuric acid storage tank 1, wherein the sulfuric acid storage tank 1 is respectively connected with a first reaction kettle 2 and a second reaction kettle 3 which are the same in structure in parallel through sulfuric acid pipelines, a sulfuric acid metering pump 4 is further arranged on the sulfuric acid pipelines, stirring blades driven by a stirring motor are arranged in the first reaction kettle 2, a safety valve and a pressure gauge are further arranged on the first reaction kettle 2, the outlet ends of the first reaction kettle 2 and the second reaction kettle 3 are respectively connected with the inlet end of a dehydration absorption tower 5 through reaction kettle pipelines, the outlet end of the dehydration absorption tower 5 is connected with the inlet of a low-temperature dynamic adsorption purification device 6 through absorption tower pipelines, the outlet end of the low-temperature dynamic adsorption purification device 6 is sequentially connected with a calcium chloride dehydration tank 7 and a silica gel dehydration tank 8 through pipelines, the outlet end of the silica gel dehydration tank 8 is respectively connected with two finished product bottle groups which are the same in structure through pipelines, the finished product bottle groups comprise a finished product gas steel bottle 9 and a finished product gas aluminum alloy bottle 10, the finished product gas aluminum alloy bottle 10 is placed in the finished product gas steel bottle group which is provided with the liquid nitrogen bath 11, and the finished product gas bottle 10 can be detected in the finished product gas bottle group which is also comprises the pressure gauge 12,
the device also comprises an evacuating vacuum pipeline which is communicated with the first reaction kettle 2, the second reaction kettle 3, the dehydration absorption tower 5, the low-temperature dynamic adsorption purification device 6, the calcium chloride dehydration tank 7, the silica gel dehydration tank 8, the product gas steel bottle 9 and the product gas aluminum alloy bottle 10, the tail end of the evacuating vacuum pipeline is connected with a vacuum pipeline 15 with an evacuating pipeline 13 and a vacuum pump 14 in parallel,
the sulfuric acid pipeline, the reaction kettle pipeline, the absorption tower pipeline, the pipeline between the low-temperature dynamic adsorption purification device 6 and the calcium chloride dehydration tank 7 as well as the pipeline between the silica gel dehydration tank 8 and the finished product bottle group, the pipeline between the evacuation vacuum pipeline and each device, the evacuation pipeline 13 and the vacuum pipeline 15 are respectively provided with a pneumatic valve,
the dehydration absorption tower comprises a bracket 5-1, a tank body 5-2 is supported at the top of the bracket 5-1, a discharging pipeline 5-4 with a discharging valve 5-3 is connected at the bottom of the tank body 5-2, an air inlet pipe 5-5 with a valve is connected at the bottom of the tank body 5-2, the part of the air inlet pipe 5-5, which is positioned in the inner cavity of the tank body 5-2, is annular, a plurality of air inlets are uniformly distributed on the annular part, the direction of the air inlets is downward, an alkali liquor pipe 5-6 with a valve is connected at the middle part of the tank body 5-2, a feed inlet pipeline 5-7 is arranged at the top of the tank body 5-2, a flange blind plate 5-8 is also arranged at the tail end of the feed inlet pipeline 5-7, alkali liquor is contained in the tank body 5-2, the cavity above the alkali liquor is filled with PP multi-surface hollow balls 5-9, the top outlet of the tank 5-2 is connected with the bottom end of the extension part 5-10 through a flange structure, a screen 5-11 is arranged at the top outlet of the tank 5-2, a central pipe 5-12 is arranged at the center of the extension part 5-10, the bottom end opening of the central pipe 5-12 is communicated with the top outlet of the tank 5-2, a sleeve 5-13 with a downward opening direction is arranged outside the central pipe 5-12, the sleeve 5-13 is connected with the inner wall of the extension part 5-10 through a plurality of connecting pieces, a gap is reserved between the top end of the central pipe 5-12 and the top inner wall of the sleeve 5-13, a gap is reserved between the bottom end of the sleeve 5-13 and the bottom plate of the extension part 5-10, the top end of the extension part 5-10 is connected with an air outlet pipeline 5-15 with an air outlet valve 5-14,
the low-temperature dynamic adsorption purification device comprises a first low-temperature tank 6-1 and a second low-temperature tank 6-2, wherein heat preservation layers 6-3 are arranged at the inner walls of the first low-temperature tank 6-1 and the second low-temperature tank 6-2, a first purification tank 6-4 is arranged in an inner cavity of the first low-temperature tank 6-1, a first air inlet pipeline 6-5 with a pneumatic valve is connected to the first low-temperature tank 6-1 in a penetrating way, a first nitrogen pipeline 6-6 with the pneumatic valve is connected to the first air inlet pipeline 6-5 in parallel, the bottom end of the first air inlet pipeline 6-5 is communicated with the bottom of the first purification tank 6-4, a ceramic adsorbent 6-7 is filled in the first purification tank 6-4, a first air outlet pipeline 6-9 with an online ceramic gas filter 6-8 is connected to the top end of the first purification tank 6-4, the pneumatic valve is also arranged on the first air outlet pipeline 6-9,
the second cryogenic tank 6-2 is connected with a second air inlet pipeline 6-10 in a penetrating way, the second air inlet pipeline 6-10 is communicated with the first air outlet pipeline 6-9 through a connecting pipeline with a pneumatic valve, the second air inlet pipeline 6-10 is also connected with a second nitrogen pipeline 6-11 with a pneumatic valve in parallel, the bottom end of the second air inlet pipeline 6-10 is communicated with the top end opening of a coil pipe 6-12 positioned in the second cryogenic tank 6-2, the bottom end outlet of the coil pipe 6-12 is positioned at the bottom of the inner cavity of the second purifying tank 6-13, the second purifying tank 6-13 is arranged in the second cryogenic tank 6-2, the second purifying tank 6-13 is also filled with a ceramic adsorbent 6-7, the top end of the second purifying tank 6-13 is connected with a second air outlet pipeline 6-14 with an on-line ceramic gas filter 6-8, the second air outlet pipeline 6-14 is also provided with a pneumatic valve, and the second air outlet pipeline 6-14 is connected with a vacuum valve with a pneumatic valve in parallel,
the device also comprises a low-temperature constant-temperature circulation unit 6-16, the low-temperature constant-temperature circulation unit 6-16 is respectively connected with the inner cavities of the first low-temperature tank 6-1 and the second low-temperature tank 6-2, mediums circulate in the low-temperature constant-temperature circulation unit 6-16, the first low-temperature tank 6-1 and the second low-temperature tank 6-2,
safety pipelines with safety valves 6-17 are arranged on the first low-temperature tank 6-1 and the second low-temperature tank 6-2,
the bottom ends of the first purification tank 6-4 and the second purification tank 6-13 are respectively connected with a drainage pipeline 6-18, a drainage valve 6-19 is arranged on the drainage pipeline 6-18, and bottom end outlets of the drainage valve 6-19 and the drainage pipeline 6-18 are respectively positioned outside the first low-temperature tank 6-1 or the second low-temperature tank 6-2.
The working process of the high-purity electronic grade nitric oxide production device provided by the embodiment of the invention is as follows:
the preparation stage:
adding a sufficient amount of 30% dilute sulfuric acid into the sulfuric acid storage tank 1; a certain amount of NaNO is put into the first reaction kettle 2 and the second reaction kettle 3 2 The method comprises the steps of carrying out a first treatment on the surface of the Starting a low-temperature constant-temperature circulating unit for 6-16, and setting the temperature to be minus 50 ℃; then, each part in the device is vacuumized by a vacuum pump on a vacuum pipeline 15; the preparation is ended.
The production stage comprises the following steps:
starting a sulfuric acid metering pump 4 to pump sulfuric acid in a sulfuric acid storage tank 1 into a first reaction kettle 2, wherein the sulfuric acid and NaNO 2 The reaction is carried out in the first reaction kettle 2, nitric oxide gas is generated, the pressure of the first reaction kettle 2 is gradually increased along with the increase of the nitric oxide gas, when the pressure is observed to be more than 1Bar, a pneumatic valve on a reaction kettle pipeline connected with the first reaction kettle 2 is opened, the nitric oxide gas sequentially passes through a dehydration absorption tower 5, a low-temperature dynamic adsorption purification device 6, a calcium chloride dehydration tank 7 and a silica gel dehydration tank 8 for multistage purification, and finally enters a finished product gas aluminum alloy bottle 10 in a finished product bottle group, and the finished product is obtained byThe gas aluminum alloy bottle 10 is placed in a liquid nitrogen bath 11 containing liquid nitrogen, so that nitric oxide gas is quickly frozen into a solid state after entering the gas aluminum alloy bottle;
after the production is carried out for a certain time in the manner, a stirring motor on the first reaction kettle 2 is started to fully stir the mixed substances in the stirring motor to enable the mixed substances to uniformly react, the pressure in the first reaction kettle 2 is observed in the process, the pressure value is ensured to be 3-5Bar, and the produced nitric oxide gas is conveyed into a finished product gas aluminum alloy bottle 10 in the current finished product bottle group;
after 1.5 hours, when the pressure value in the first reaction kettle 2 is reduced to below 1Bar, indicating that the reaction is about to be finished, stopping pumping sulfuric acid into the first reaction kettle 2, opening a corresponding pneumatic valve on the second reaction kettle 3, pumping the sulfuric acid into the second reaction kettle 3, closing a bottle valve on a finished product gas aluminum alloy bottle 10 in the current finished product bottle group, opening a bottle valve on a finished product gas aluminum alloy bottle 10 in another finished product bottle group, at the moment, conveying nitric oxide gas generated in the second reaction kettle 3 into the finished product gas aluminum alloy bottle 10 in the second finished product bottle group, and also quickly freezing into a solid state, thereby completing the switching between the reaction kettle and the finished product bottle group;
in the production process of the second reaction kettle 3, the first reaction kettle 2 is subjected to unloading and feeding operation: firstly, the first reaction kettle 2 is emptied by utilizing an emptying pipeline 13, then a kettle bottom valve of the first reaction kettle 2 is opened to discharge materials in the first reaction kettle 2, and then a certain amount of NaNO is added into the first reaction kettle 2 And closing, and finally vacuumizing the first reaction kettle 2 by utilizing a vacuum pipeline 15 until the vacuum degree is less than 1Pa;
then, vacuumizing the finished gas aluminum alloy bottle 10 in the first group of finished product bottle groups until the vacuum degree is less than 1Pa, opening a valve nozzle on the finished gas steel bottle 9 in the first group of finished product bottle groups, taking the finished gas aluminum alloy bottle 10 out of the liquid nitrogen bath 11, slowly heating the finished gas aluminum alloy bottle 10 at room temperature, gradually changing solid nitric oxide into a gas state in the heating process, and conveying the solid nitric oxide into the finished gas steel bottle 9; in the process, the pressure in the finished gas aluminum alloy bottle 10 (and the finished gas steel bottle 9) is also continuously increased, when the pressure in the inner cavities of the finished gas aluminum alloy bottle 10 and the finished gas steel bottle 9 reaches 35Bar, the bottle valves of the finished gas aluminum alloy bottle 10 and the finished gas steel bottle 9 are closed, and the finished gas aluminum alloy bottle 10 and the finished gas steel bottle 9 in the first group of finished gas bottle groups are filled with high-purity nitric oxide gas, and are detached from the pipeline;
then placing the new finished product gas aluminum alloy bottle 10 in a liquid nitrogen bath 11 in the first group of finished product bottle groups, connecting the new finished product gas aluminum alloy bottle 10 with the new finished product gas steel bottle 9 through a pipeline, vacuumizing the new finished product gas aluminum alloy bottle 10 and the new finished product gas steel bottle 9 after connecting the related pipelines, and after vacuumizing, preparing the new first group of finished product bottle groups to be completed, and waiting for the next filling operation;
the reaction of the second reaction kettle 3 is carried out according to the operation, the generated nitric oxide gas is purified in multiple stages and then is input into a second group of finished product bottle groups, and the filling of the finished product gas aluminum alloy bottle 10 and the finished product gas steel bottle 9 is respectively completed;
that is, in the working process, when one of the two reaction kettles in the device is produced, the other one can realize the operation of unloading and filling, and in the two sets of finished bottle groups, when one set is filled, the other set can realize the operation of disassembling and assembling, thus the uninterrupted production can be realized, and the aim of improving the working efficiency is fulfilled.
Stopping production:
when the machine is required to be stopped after the last batch of gas is produced, after the production of the last batch of gas is finished, raw materials are not put into the reaction kettle, an outlet valve of the reaction kettle is closed, a pneumatic valve on a pipeline between the silica gel dewatering tank 8 and a finished product bottle group is closed, the pressure of 1-5Bar is kept in each pipeline of the device, vacuumizing operation is not required to be carried out on each pipeline of the device in the next production, and production activities can be directly carried out.
The specific working process of the dehydration absorption tower 5 in the device is as follows: firstly, removing a flange blind plate 5-8, conveying a plurality of PP multi-face hollow balls 5-9 into an inner cavity of a tank body 5-2 through a feed port pipeline 5-7, then reinstalling the flange blind plate 5-8 at a port of the feed port pipeline 5-7, pouring NaOH solution into the tank body 5-2 through an alkali liquor pipe 5-6, floating on the upper half part of the tank body 5-2 due to the fact that the PP multi-face hollow balls 5-9 are smaller than water in density, filling a plurality of PP multi-face hollow balls 5-9 into an extension part 5-10 in advance, filling the PP multi-face hollow balls into a cavity between the central pipe 5-12 and a sleeve 5-13 and between the sleeve 5-13 and the inner wall of the extension part 5-10, connecting the extension part 5-10 at the top of the tank body 5-2, ensuring that the bottom end of the central pipe 5-12 is communicated with an outlet of the tank body 5-2, and completing preparation work;
the gas to be purified is filled into the tank body 5-2 through the gas inlet pipe 5-5, the gas is discharged through the gas inlet hole on the annular part of the gas inlet pipe 5-5 and gradually rises to the upper half part of the tank body 5-2 from the bottom of the alkali liquor, and in the process, acidic substances in the gas can be neutralized by the alkali liquor, so that the aim of acid removal of the gas is fulfilled; when the gas is separated from the alkali liquor, the gas continuously rises and fully contacts with a plurality of PP multi-surface hollow spheres 5-9 in the upper half part of the tank body 5-2, and the PP multi-surface hollow spheres 5-9 can absorb the moisture in the gas so as to achieve the purpose of removing water once;
the gas subjected to acid removal and primary water removal treatment continuously rises and enters the central tube 5-12, flows downwards along the space between the central tube 5-12 and the sleeve 5-13 after being discharged from the top opening of the central tube 5-12, then flows upwards along the space between the sleeve 5-13 and the inner wall of the extension part 5-10, and finally is discharged through the air outlet pipeline 5-15, and the gas moves along a snake-shaped track in the extension part 5-10 due to the fact that the extension part 5-10 is of a slender shape, so that the flowing stroke of the gas is longer, and in the flowing process, moisture in the gas can be absorbed again by the PP multi-surface hollow ball 5-9, and the purpose of secondary water removal is achieved;
the working process of the low-temperature dynamic adsorption purification device 6 in the device is as follows:
activation of the purification device:
before use, firstly, opening two drain valves 6-19, draining water in the first purification tank 6-4 and the second purification tank 6-13, and then closing the drain valves 6-19; starting a low-temperature constant-temperature circulation unit 6-16, setting the circulation temperature to be 60 ℃, heating a first purification tank 6-4 and a second purification tank 6-13, purging the two purification tanks 6-4 by using a first nitrogen pipeline 6-6 and a second nitrogen pipeline 6-11 in the state, quickly blowing out water, nitrogen dioxide and carbon dioxide adsorbed on a ceramic adsorbent 6-7 under the purging of hot nitrogen, closing the low-temperature constant-temperature circulation unit 6-16 after continuously purging for two hours, opening a pneumatic valve on a connecting pipeline between the two purification tanks 6-13, vacuumizing the two purification tanks and related pipelines by using a vacuumizing pipeline 6-15, and closing the vacuumizing pipeline 6-15 after the vacuum degree is smaller than a certain preset value, thereby completing the activation work.
Purifying gas:
starting a low-temperature constant-temperature circulation unit 6-16, setting the circulation temperature to be minus 60 ℃, cooling the first purification tank 6-4 and the second purification tank 6-13, opening a pneumatic valve on the first air inlet pipeline 6-5 after the temperature is stabilized at minus 60 ℃ for 5 minutes, enabling nitric oxide gas to enter the first purification tank 6-4, quickly freezing water, nitrogen dioxide and carbon dioxide in the nitric oxide gas into solid state at the low temperature of minus 60 ℃, and adsorbing the solid state on the ceramic adsorbent 6-7, wherein the first purification tank 6-4 plays a role in primary absorption;
then opening a pneumatic valve on the connecting pipeline to enable the initially absorbed nitric oxide gas to enter a coil pipe 6-12, wherein the coil pipe 6-12 can prolong the flowing time of the nitric oxide gas, and residual water, nitrogen dioxide and carbon dioxide are adsorbed on a ceramic adsorbent 6-7 after the gas enters a second purification tank 6-13, wherein the second purification tank 6-13 plays a role in efficient absorption;
finally, a pneumatic valve on the second exhaust pipeline 6-14 is opened, and the purified nitric oxide gas enters subsequent equipment such as separation, refining, compression and the like, so that the purification process is completed.
It should be noted that after a certain period of operation of the device, the ceramic adsorbent 6-7 tends to saturate and the purification effect is reduced, and at this time, the device needs to be activated again, and the specific activation step is the same as described above.
Claims (1)
1. A high purity electronic grade nitric oxide production device, characterized in that: the device comprises a sulfuric acid storage tank (1), the sulfuric acid storage tank (1) is respectively connected with a first reaction kettle (2) and a second reaction kettle (3) which are the same in structure in parallel through sulfuric acid pipelines, a sulfuric acid metering pump (4) is further arranged on the sulfuric acid pipelines, stirring blades driven by a stirring motor are arranged in the first reaction kettle (2), a safety valve and a pressure gauge are further arranged on the first reaction kettle (2), the outlet ends of the first reaction kettle (2) and the second reaction kettle (3) are respectively connected with the inlet ends of a dehydration absorption tower (5) through reaction kettle pipelines, the outlet ends of the dehydration absorption tower (5) are connected with the inlet of a low-temperature dynamic adsorption purification device (6) through absorption tower pipelines, the outlet ends of the low-temperature dynamic adsorption purification device (6) are sequentially connected with a calcium chloride dehydration tank (7) and a silica gel dehydration tank (8) through pipelines, the outlet ends of the silica gel dehydration tank (8) are respectively connected with two finished product bottle groups which are the same in structure through pipelines, the finished product bottle groups comprise a finished product gas (9) and a finished product gas (10) and a liquid nitrogen bottle (10) which can be simultaneously placed in a finished product gas bottle (10) and a liquid nitrogen bottle (10) and a finished product gas bottle (10) which can be simultaneously placed in the finished product gas bottle (10) and a liquid nitrogen bottle (11),
the device also comprises an evacuating vacuum pipeline which is communicated with the first reaction kettle (2), the second reaction kettle (3), the dehydration absorption tower (5), the low-temperature dynamic adsorption purification device (6), the calcium chloride dehydration tank (7), the silica gel dehydration tank (8), the finished gas steel cylinder (9) and the finished gas aluminum alloy cylinder (10), the tail end of the evacuating vacuum pipeline is connected with a vacuum pipeline (15) with an evacuating pipeline (13) and a vacuum pump (14) in parallel,
the sulfuric acid pipeline, the reaction kettle pipeline, the absorption tower pipeline, the pipeline between the low-temperature dynamic adsorption purification device (6) and the calcium chloride dehydration tank (7) as well as the silica gel dehydration tank (8), the pipeline between the silica gel dehydration tank (8) and the finished product bottle group, the pipeline between the evacuation vacuum pipeline and each device, the evacuation pipeline (13) and the vacuum pipeline (15) are respectively provided with a pneumatic valve,
the dehydration absorption tower comprises a bracket (5-1), a tank body (5-2) is supported at the top of the bracket (5-1), a discharging pipeline (5-4) with a discharging valve (5-3) is connected at the bottom of the tank body (5-2), an air inlet pipe (5-5) with a valve is connected at the bottom of the tank body (5-2), the part of the air inlet pipe (5-5) positioned in the inner cavity of the tank body (5-2) is annular, a plurality of air inlets are uniformly distributed on the annular part, the direction of the air inlets is downward, an alkali liquor pipe (5-6) with a valve is connected at the middle part of the tank body (5-2), a feeding port pipeline (5-7) is arranged at the top of the tank body (5-2), a flange blind plate (5-8) is also arranged at the tail end of the feeding port pipeline (5-7), a cavity above the alkali liquor is filled with PP hollow balls (5-9), an outlet (5-2) is connected with a central part (10) of the tank body (5-2) through a flange (5-10) at the central part of the top of the tank body (5-2), the bottom end opening of the central tube (5-12) is communicated with the top outlet of the tank body (5-2), a sleeve (5-13) with a downward opening direction is arranged outside the central tube (5-12), the sleeve (5-13) is connected with the inner wall of the extension part (5-10) through a plurality of connecting pieces, a gap is reserved between the top end of the central tube (5-12) and the top inner wall of the sleeve (5-13), a gap is reserved between the bottom end of the sleeve (5-13) and the bottom plate of the extension part (5-10), the top end of the extension part (5-10) is connected with an air outlet pipeline (5-15) with an air outlet valve (5-14),
the low-temperature dynamic adsorption purification device comprises a first low-temperature tank (6-1) and a second low-temperature tank (6-2), wherein heat preservation layers (6-3) are arranged at the inner walls of the first low-temperature tank (6-1) and the second low-temperature tank (6-2), a first purification tank (6-4) is arranged in an inner cavity of the first low-temperature tank (6-1), a first air inlet pipeline (6-5) with a pneumatic valve is connected to the first low-temperature tank (6-1) in a penetrating way, a first nitrogen pipeline (6-6) with the pneumatic valve is connected to the first air inlet pipeline (6-5) in parallel, the bottom end of the first air inlet pipeline (6-5) is communicated with the bottom of the first purification tank (6-4), a ceramic adsorbent (6-7) is filled in the first purification tank (6-4), a first air outlet pipeline (6-9) with an online ceramic gas filter (6-8) is connected to the top end of the first purification tank (6-4), the first air inlet pipeline (6-9) is provided with the pneumatic valve,
the second cryogenic tank (6-2) is connected with a second air inlet pipeline (6-10) in a penetrating way, the second air inlet pipeline (6-10) is communicated with a first air outlet pipeline (6-9) through a connecting pipeline with a pneumatic valve, the second air inlet pipeline (6-10) is also connected with a second nitrogen pipeline (6-11) with a pneumatic valve in parallel, the bottom end of the second air inlet pipeline (6-10) is communicated with the top end opening of a coil pipe (6-12) positioned in the second cryogenic tank (6-2), the bottom end outlet of the coil pipe (6-12) is positioned at the bottom of an inner cavity of a second purifying tank (6-13), the second purifying tank (6-13) is arranged in the second cryogenic tank (6-2), a ceramic adsorbent (6-7) is also filled in the second purifying tank (6-13), the top end of the second purifying tank (6-13) is connected with a second air outlet pipeline (6-14) with a ceramic air filter (6-8), the bottom end outlet of the coil pipe (6-12) is positioned in parallel with the second air outlet pipeline (6-14) is arranged in parallel with the pneumatic valve (6-14),
the device also comprises a low-temperature constant-temperature circulation unit (6-16), the low-temperature constant-temperature circulation unit (6-16) is respectively connected with the inner cavities of the first low-temperature tank (6-1) and the second low-temperature tank (6-2), mediums circulate in the low-temperature constant-temperature circulation unit (6-16), the first low-temperature tank (6-1) and the second low-temperature tank (6-2),
safety pipelines with safety valves (6-17) are arranged on the first low-temperature tank (6-1) and the second low-temperature tank (6-2),
the bottom ends of the first purification tank (6-4) and the second purification tank (6-13) are both connected with a drainage pipeline (6-18), a drainage valve (6-19) is arranged on the drainage pipeline (6-18), and bottom end outlets of the drainage valve (6-19) and the drainage pipeline (6-18) are both positioned outside the first low-temperature tank (6-1) or the second low-temperature tank (6-2).
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