CN113753868A - Purification method, purification device and production device for nitric oxide gas - Google Patents
Purification method, purification device and production device for nitric oxide gas Download PDFInfo
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- CN113753868A CN113753868A CN202111199597.3A CN202111199597A CN113753868A CN 113753868 A CN113753868 A CN 113753868A CN 202111199597 A CN202111199597 A CN 202111199597A CN 113753868 A CN113753868 A CN 113753868A
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000000746 purification Methods 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 238000010791 quenching Methods 0.000 claims abstract description 44
- 238000000926 separation method Methods 0.000 claims abstract description 39
- 230000000171 quenching effect Effects 0.000 claims abstract description 38
- 239000012535 impurity Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000003507 refrigerant Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002826 coolant Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004817 gas chromatography Methods 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 230000003993 interaction Effects 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 55
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000007710 freezing Methods 0.000 description 10
- 230000008014 freezing Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000007323 disproportionation reaction Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 3
- RBIIKVXVYVANCQ-CUWPLCDZSA-N (2s,4s,5s)-5-amino-n-(3-amino-2,2-dimethyl-3-oxopropyl)-6-[4-(2-chlorophenyl)-2,2-dimethyl-5-oxopiperazin-1-yl]-4-hydroxy-2-propan-2-ylhexanamide Chemical compound C1C(C)(C)N(C[C@H](N)[C@@H](O)C[C@@H](C(C)C)C(=O)NCC(C)(C)C(N)=O)CC(=O)N1C1=CC=CC=C1Cl RBIIKVXVYVANCQ-CUWPLCDZSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 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 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002337 glycosamines Chemical class 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 230000006903 response to temperature Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
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- 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)
-
- 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)
- C01B21/26—Preparation by catalytic or non-catalytic oxidation of ammonia
- C01B21/28—Apparatus
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Gas Separation By Absorption (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a purification method, a purification device and a production device of nitric oxide gas, wherein the purification method comprises the following steps: pretreatment: removing impurities from the feed gas containing NO and drying; separation: and (3) sending the pretreated raw material gas into a separation chamber, and sequentially passing through a plurality of quenching sections arranged in the separation chamber to obtain pure target gas, wherein the temperature limited by the quenching sections is not higher than the melting point of the target gas separated by the quenching sections. The invention has the advantages of simple and safe process, low cost, less equipment, less energy consumption and good economical efficiency.
Description
Technical Field
The present invention relates to a gas separation technology, and more particularly to a method, an apparatus and a device for purifying nitric oxide gas.
Background
Nitric oxide is currently in medicineThe stabilizer plays a unique role in various fields such as electronics, chemical engineering and the like, and is medically used for auxiliary diagnosis and treatment of clinical experiments and organic reaction; the gas-phase oxidation catalyst is used for oxidation and chemical vapor deposition processes in production in semiconductors and used as an atmosphere monitoring standard mixed gas; can be used for preparing nitric acid, silicone oxide film and carbonyl nitrosyl in the chemical field, can also be used as bleaching agent of rayon, stabilizing agent of propylene and dimethyl ether, emergency terminator in PVC production, etc., for example, the nitric oxide used as emergency terminator in PVC production can be used for quickly terminating polymerization of PVC monomer in reaction kettle when the production is stopped or emergency accident occurs, so as to prevent explosion due to overhigh temperature in kettle, and compared with existent liquid-state termination adjuvant, the NO has obvious advantage, and it does not need N2Used as carrier gas, and has strong PVC monomer combining ability, fast speed and long quality guarantee period. However, the methods for producing NO gas widely at present contain NO2Gas, NO2The gas is combined with PVC monomer to form explosion chelate, so that the potential safety hazard exists, and therefore, the NO in the NO gas must be strictly controlled during the use2Gas content (< 50ppm) and NO in NO2，N2The removal of O impurities is the main direction and the difficult point of attack of the domestic and foreign technical research.
The prior methods for producing NO have various methods, and the most widely used method at present is to prepare NO by reacting sodium nitrite with dilute sulfuric acid, wherein the production process is to react the sodium nitrite with the dilute sulfuric acid in a reaction tank to generate sodium sulfate, sodium nitrate solution, NO and H2O, and also to produce, for example, NO2、N2O、N2、SO2、H2O and the like, and a small amount of CO may be present2Etc., and the produced NO is easily reacted with O2Combined with oxidation to form NO2Meanwhile, NO can slowly generate disproportionation reaction to generate NO in the presence of alkali liquor or at high temperature2And N2O, thus, NO is removed from NO2、N2O is the main subject of technical research at home and abroad.
Chinese patent No. 98108604.7 indicates that N is a complex of glycosamine ligand of Aminopolympin with transition metals such as Pt, Pd, Fe, Ni, Cu, Ag and Zn or their saltsThe O gas adsorbent is heated and diluted to obtain NO with the concentration of more than or equal to 95 percent, but the obtained NO has too low purity to meet the high-end requirement. US patent No. 3489515 teaches that cleaning a nitric oxide gas stream with a dilute aqueous nitric acid solution, reacting water and nitrogen dioxide to form nitric acid and nitrous acid, and cleaning with water to remove impurities, but does not adequately reduce NO2By cryogenic distillation to remove NO2The process also has a number of disadvantages, not only is the distillation equipment costly, but it also consumes NO.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a nitric oxide gas purification method, a nitric oxide gas purification device and a nitric oxide gas production device, which solve the technical problems in the prior art by adopting a method combining alkali liquor absorption, gas-liquid separation, drying and freezing, and provide a NO gas purification method, wherein the purification method has the advantages of high safety, simple equipment, less investment, less energy consumption, low cost, simple process operation, high product purity and the like, and the product with the purity of more than 99.99 percent is obtained. .
To achieve the above object, an embodiment of the present invention provides a method for purifying nitric oxide gas, including the steps of: pretreatment: removing impurities from the feed gas containing NO and drying; separation: and (3) sending the pretreated raw material gas into a separation chamber, and sequentially passing through a plurality of quenching sections arranged in the separation chamber to obtain pure target gas, wherein the temperature limited by the quenching sections is not higher than the melting point of the target gas separated by the quenching sections.
In one or more embodiments of the present invention, the pre-treatment further comprises analyzing species of composition of the feed gas to obtain the composition of the feed gas further comprises at least one or more of: NO2、N2O、SO2、CO2、H2O。
In one or more embodiments of the present invention, the analyzing of the kind of composition of the raw material gas is to determine the number of compositions N in the raw material gas by analyzing by gas chromatography.
In one or more embodiments of the invention, the separation chamber is sequentially arranged into M quench sections depending on the number of constituents in the feed gas, N, where M is no greater than N.
In one or more embodiments of the invention, the temperature defined by each quench section is sequentially raised or lowered along the feed gas inlet direction on the separation chamber.
In one or more embodiments of the invention, the cooling capacity provided by the cold medium controlling the corresponding area is also used on the separation chamber for each quench section, including: when the same kind of refrigerant is adopted, the refrigerant flow corresponding to each quenching section is controlled; or when different refrigerants are adopted, the flow rate of the refrigerant corresponding to each quenching section or the type of the adopted refrigerant is controlled. The coolant is preferably selected from liquid nitrogen, liquid ammonia, R32, R12, R134a, R407c, and the like, and the coolant exemplified here may be selected alternatively in this embodiment, or different coolant combinations may be distributed and selected for the separation target of each quenching section, that is, the separation target of the present section target and other parts, such as solid-liquid separation or liquid-gas separation, may be achieved, and the kind of coolant used in each quenching section may be selected.
In one or more embodiments of the present invention, each quenching section is further provided with a temperature monitor to obtain temperature data of the current quenching section, the temperature data is fed back to controller interaction data for controlling the refrigerant medium, and the controller controls the flow rate or the type of the refrigerant medium in the corresponding region.
In one or more embodiments of the invention, the separation chamber is further provided with a solid-liquid separator on each quench section, the solid-liquid separator comprising a screening device with screen openings.
In one or more embodiments of the present invention, a purification apparatus of the purification method of nitric oxide gas as described above is applied.
In one or more embodiments of the invention, the production plant, at least, comprises a reactor, a purification plant as described above.
Compared with the prior art, the method, the device and the production device for purifying nitric oxide gas in the embodiment of the invention adopt the method of combining alkali liquor absorption, gas-liquid separation and freezing separation to solve the technical problems in the prior art, and provide the method for purifying NO, which utilizes the characteristic that the difference between the melting points of impurities and NO is large to separate and remove NO in NO by adopting the freezing method2、N2O、SO2、CO2Etc., especially NO which is difficult to remove2、N2And O, finally obtaining the NO product with the purity of 99.99 percent, wherein the purification method has the advantages of high safety, simple equipment, less investment, less energy consumption, low cost, simple process operation, high product purity and the like.
Drawings
FIG. 1 is a schematic flow diagram according to an embodiment of the present invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
The main idea of the invention is to adopt a freezing physical method process and utilize NO and NO2、N2O、SO2、CO2、H2The gas is separated and purified according to the difference of melting points of O and other components, so that the problems of disproportionation reaction of NO and NO generated by disproportionation reaction in the prior art are solved2And N2Problem of removal of O impurities, wherein NO and NO2、N2O、SO2、CO2、H2The melting points of O are respectively: 163.6 ℃, 11 ℃, 90.8 ℃, 75.5 ℃, 78.45 ℃ and 0 ℃; in the implementation process, the problem of NO in NO is solved by adopting a freezing physical method2、N2The technical problem that O impurities are difficult to remove, and SO can be removed2、CO2、H2O these impurities are removed.
As shown in fig. 1, according to the method for purifying nitric oxide gas according to the preferred embodiment of the present invention, raw gas whose main component is nitric oxide generated from a reactor is separated and purified.
In one or more embodiments of the invention, NaNO is passed from the reactor2And H2SO4The reaction gas obtained from the mixed reaction contains a large amount of acidic impurity gas, water and the like, and can be treated in advance before purification, namely, most of the impurity gas in the reaction gas is removed by pretreatment means such as alkali absorption, gas-liquid separation and the like, so that purified raw material gas with only a small amount of residual impurity content is obtained.
In one or more embodiments of the present invention, the type of the impurity gas in the raw material gas may be predetermined according to a chemical principle, or the content and type of the impurity gas may be confirmed and verified by means of gas chromatography, so that the temperature setting in the separation chamber, especially the setting of different quenching sections and the temperature setting of corresponding sections when multi-section separation is required, may be conveniently and efficiently confirmed by using a physical freezing method. For example, when the raw material gas contains NO, NO2、N2O、SO2、CO2、H2In the case of the gas of the six types, if the six types of components need to be separated separately, at least 6 quenching sections should be provided in the separation chamber, and different working temperatures are sequentially set for the 6 sections according to the melting point of the target gas, so that the purpose of solid-phase separation can be satisfied, and the target gas of the corresponding section is solidified into solid and separated. Of course, for convenience of operation, the temperature setting may be set sequentially from the high temperature stage to the low temperature stage in the feed gas inlet direction, and the other high melting point is preferentially solidified and separated. Of course, the number of quench sections provided may also be less than the total number of components in the feed gas, thereby separating the more valuable fraction.
In one or more embodiments of the present invention, in order to control the temperature of the quenching section in the separation chamber, the temperature is correspondingly controlled to the melting point or the freezing point of the corresponding target gas, and the temperature can be improved and adjusted by controlling a refrigerant medium, such as the flow rate or the flow velocity of liquid nitrogen in the condenser of each section, or the refrigerant of different sections can be adjusted, so that the working temperature of the refrigerant of the current section is properly lower than the temperature of the target gas. The coolant matched with the corresponding quenching section may be selected from, but not limited to, liquid nitrogen, liquid ammonia, R32, R12, R134a, R407c, etc. according to different application targets.
In one or more embodiments of the present invention, in order to meet the requirement of accurately controlling the temperature of each quenching section, a device for sensing the current temperature state, such as a temperature sensor capable of operating at an ultra-low temperature, may be further disposed in the quenching section, and when the temperature fluctuates, the flow speed of the refrigerant in the condenser for cooling the quenching section may be adjusted, that is, the cooling capacity provided by the condenser in the current state is adjusted, for example, when the temperature of the current quenching section is higher, the flow rate of the refrigerant in the condenser is increased, the cooling capacity is increased, and the temperature is decreased to a suitable level, or vice versa. This temperature control means can be applied to one or more quench sections for regulating the overall state of the separation chamber.
In one or more embodiments of the present invention, in order to improve the accuracy and efficiency of response to temperature fluctuation of the quenching sections, a solenoid valve or other pipe valve capable of responding to a real-time control signal in real time may be provided on a refrigerant supply pipe of a condenser matched with each quenching section. The valve such as the solenoid valve and the like which respond at the time can be electrically controlled or numerically controlled, as long as the on-off state (such as 100% opening full-force supply, 50% opening limited supply or closing and the like) of the refrigerant supply pipeline can be adjusted when the temperature of the monitored quenching section fluctuates.
In one or more embodiments of the present invention, it is understood that the refrigerant supply line for supplying refrigerant to each quenching section may be a single line supply, or may be a plurality of lines in parallel, as long as the requirement is satisfied.
In one or more embodiments of the present invention, in order to meet the requirement of online automatic control, a controller such as a microcomputer or a PLC, which is linked with a pipe valve such as an electromagnetic valve and a temperature sensor, may be further provided, and the controller may control the corresponding pipe valve to react according to a preset instruction and a temperature state in each quenching section fed back by the sensor, that is, the adjustment of the working state of each quenching section in real time on line is realized.
In one or more embodiments of the present invention, in order to monitor the quality of the purified nitric oxide product, a detection device may be further disposed in the direction of the exhaust line of the separation chamber, and when the quality of the gas is detected to be not in accordance with the quality standard, the gas is dumped into the exhaust gas storage tank and returned to the feed gas intake position for reprocessing under appropriate conditions. And guiding qualified products into a product storage tank.
In one or more embodiments of the present invention, the production apparatus shown in FIG. 1 comprises a reaction apparatus, an alkali liquid absorption apparatus, a gas-liquid separation apparatus, a freezing separation apparatus, and in the production of nitric oxide gas, it may be performed as shown in the following procedure: NaNO2And H2SO4Mixing the mixture in a reaction tank for reaction, and mixing the rest of the reaction solution with the generated Na2SO4And NaNO3Solution and small amount of CO2、SO2And a small fraction of NO2Most of NO is removed by absorption and separation of alkali liquor2、N2Introducing O, water vapor, etc. into a dryer (containing one or more of calcium oxide, silica gel, 5A molecular sieve and 13X molecular sieve as adsorbent) with NO gas, absorbing partial water, introducing the NO gas into a freezing separation tank with liquid nitrogen coil at-15 deg.C-35 deg.C and 0.1-1 MPa, regulating the flow of liquid nitrogen to control the temperature of the separation tank at-95 deg.C-120 deg.C and 0.01-0.4 MPa, keeping NO in gas state, and introducing into the dryer2、N2O、SO2、CO2、H2O forms a solid state, namely a quenching section is arranged, the separated target gas is NO, and the temperature is keptAfter the temperature and the pressure are stable, the analysis is carried out by an on-line analytical instrument, and NO is obtained2、N2When the content of impurities such as O and the like is less than 10ppm, the gas enters a qualified product buffer tank from the separation tank, and then is collected and filled; when NO is present2、N2And when the content of impurities such as O and the like is more than 10ppm, returning to the freezing tank again for re-separation, and analyzing again until the content is qualified.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A method for purifying nitric oxide gas is characterized by comprising the following steps:
pretreatment: removing impurities from the feed gas containing NO and drying;
separation: and sending the pretreated raw material gas into a separation chamber, and sequentially passing through a plurality of quenching sections arranged in the separation chamber to obtain pure target gas, wherein the temperature of each quenching section is not higher than the melting point of the target gas separated by the quenching section.
2. The method for purifying nitric oxide gas as claimed in claim 1, wherein said pre-treating further comprises analyzing species of composition of the raw material gas to obtain composition of the raw material gas, wherein the composition of the raw material gas further comprises at least one or more of: NO2、N2O、SO2、CO2、H2O。
3. The method of purifying nitric oxide gas according to claim 2, wherein said analysis of the kind of composition of the raw material gas is performed by gas chromatography to determine the number of compositions N in the raw material gas.
4. The method of purifying nitric oxide gas as claimed in claim 3, wherein the separation chamber is sequentially provided as M quenching sections in accordance with the number N of components in the raw material gas, where M is not more than N.
5. The method for purifying nitric oxide gas according to claim 4, wherein the temperature defined in each of said quenching sections is sequentially increased or decreased along the direction of introduction of the raw material gas on said separation chamber.
6. The method for purifying nitric oxide gas as claimed in claim 5, wherein said cooling capacity provided by the cooling medium of the corresponding zone is controlled for each of said quenching sections by a cooling medium of said separation chamber, comprising:
when the same type of refrigerant is adopted, the refrigerant flow corresponding to each quenching section is controlled; or
When different refrigerants are adopted, the flow rate of the refrigerant corresponding to each quenching section or the type of the adopted refrigerant is controlled.
7. The method for purifying nitric oxide gas as claimed in claim 6, wherein each of said quenching sections is further provided with a temperature monitor to obtain temperature data of the current quenching section, said temperature data is fed back to controller interaction data for controlling the refrigerant medium, said controller controls the flow rate or kind of the refrigerant medium in the corresponding zone.
8. The method for purifying nitric oxide gas as claimed in any one of claims 1 to 7, wherein a solid-liquid separator is further provided on said separation chamber for each of said quenching sections, said solid-liquid separator including a sieving device having a sieve hole.
9. A purification apparatus applying the method for purifying nitric oxide gas according to any one of claims 1 to 8.
10. Production plant comprising at least a reactor, a purification plant according to claim 9.
Priority Applications (1)
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| CN114593560A (en) * | 2022-03-11 | 2022-06-07 | 苏州金宏气体股份有限公司 | Removal of NO from NO2、N2O purification device and purification method |
| CN117225304A (en) * | 2023-11-13 | 2023-12-15 | 河南心连心深冷能源股份有限公司 | Device and method for preparing high-purity nitric oxide |
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Application publication date: 20211207 |