CN101428773A - Purifying method for nitric oxide gas with 3N purity - Google Patents
Purifying method for nitric oxide gas with 3N purity Download PDFInfo
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- CN101428773A CN101428773A CNA2008102296033A CN200810229603A CN101428773A CN 101428773 A CN101428773 A CN 101428773A CN A2008102296033 A CNA2008102296033 A CN A2008102296033A CN 200810229603 A CN200810229603 A CN 200810229603A CN 101428773 A CN101428773 A CN 101428773A
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Abstract
The invention discloses a purification method of nitrogen oxide with 3N purity, which comprises the following steps: carrying out the decomposion of sodium nitrite with dilute sulfuric acid, alkali liquor absorption, gas and liquid separation, and drying and separating to obtain the gas, wherein the gas after being dried positively passes through a polyethylene glycol-methacrylate copolymer adsorption zone under the conditions that the temperature is minus 20 DEG C to 30 DEG C and the pressure is 0.5 MPa to 1.5 MPa; and then collecting the gas after being absorbed. By adopting a polyethylene glycol-methacrylate copolymer as an adsorbent, the disproprotionation of the nitrogen oxide and oxidation reaction can be effectively restrained, so that the impurity contents of nitrogen dioxide and nitrous oxide are reduced, and the purity of the nitrogen oxide is improved; the purity of the nitrogen oxide after being purified is larger than 99.9 percent; the content of the nitrogen dioxide is less than 20 ppm; and the content of the nitrous oxide is less than 50 ppm. Particularly, by adopting the secondary circulating adsorption process, foreign gas is positively absorbed, and simultaneously the negative decompression is performed to regenerate the absorbent. The invention has the advantages of simple operation process and low cost.
Description
Technical field:
The present invention relates to a kind of gas purification method, especially a kind of operating procedure is simple, with low cost, the purification process of the 3N that purity is high (99.9%) purity nitric oxide gas.
Background technology:
At present, nitrogen protoxide has been brought into play unique effect in every field such as medical science, electronics, chemical industry, as in PVC produces, can be used as urgent terminator, PVC monomer polymerization in the rapid termination reaction still when producing power failure or emergency episode occurring, blast to prevent that temperature in the kettle is too high, avoid the generation of Peril Incident, the liquid-type that PVC production is more in the past adopted stops auxiliary agent and has clear superiority, and it does not need N
2Do carrier gas,, speed strong in conjunction with the PVC monomer capable is fast, long quality-guarantee period.But, all contain nitrogen dioxide gas generally speaking in the nitric oxide gas, and nitrogen dioxide gas can combine formation blast huge legendary turtle compound with the PVC monomer, exist potential safety hazard, therefore the content that must strictly control nitrogen peroxide in the nitric oxide gas stream that charges in the reactor must not surpass 50ppm, and nitric oxide production purity should be not less than 3N.
The nitric oxide production method of existing production has multiple, and U.S. Pat 3663167 points out to utilize ammonia oxidation preparation in air, but required higher, the difficulty or ease realization of condition of this kind method; U.S. US5670127 points out to utilize nitric acid and sulfurous gas reaction to produce nitric oxide gas, and the shortcoming of this method is that the content of impurity (sulfurous gas) is too much, removes cumbersome; Also having a kind of is exactly to adopt Sodium Nitrite and dilute sulphuric acid reaction to produce nitrogen protoxide, and its production process is that Sodium Nitrite and dilute sulphuric acid are reacted in reaction tank, generates sodium sulfate and sodium nitrate solution and NO, H
2O also can produce as NO simultaneously
2, N
2O, N
2, SO
2, impurity such as water vapour, also can have a spot of CO sometimes
2(air admission influence) etc.; The sodium sulfate of remaining reaction solution and generation and sodium nitrate solution and a spot of CO
2, small portion SO
2, NO
2Absorb to separate from the bottom of reactor by alkali lye and remove most of NO with washing
2, N
2O, water vapor etc. flow out from reactor top with gaseous form with NO; Water vapor is absorbed in by the moisture eliminator that has or not water calcium chloride to exist at gas stream and removes, and is easy and simple to handle.
Because nitrogen protoxide is easy to generate nitrogen peroxide with combination with oxygen generation oxidizing reaction, nitrogen protoxide self can slow generation disproportionation reaction generate nitrogen peroxide and Nitrous Oxide when alkali lye existence or high temperature simultaneously, therefore there is multinomial technical study to be intended to from nitric oxide gas stream, remove nitrogen peroxide now both at home and abroad, Nitrous Oxide, China Patent No. is 98108604.7 to point out by chitosan part and Pt, Pd, Fe, Ni, Cu, Ag, the complex compound that transition metal such as Zn or their salt generate is as the NO adsorbent, obtain the nitrogen protoxide of concentration 〉=95% again by the heating dilution, can not be used for high-end demand but nitrogen protoxide purity is too low.U.S. Pat 3489515 points out to utilize diluted nitric acid aqueous solution to clean nitric oxide gas stream, water and nitrogen peroxide reaction generate nitric acid and nitrous acid, clean with removal of contamination by water again, but this method can not fully reduce the concentration of nitrogen peroxide, and also there are many drawbacks by the method that low-temperature distillation is removed nitrogen peroxide, distillation plant cost height not only, but also can consume nitrogen protoxide.
Other has some to use sorbent material to remove the report of nitrogen peroxide impurity from nitric oxide gas stream, point out to use the ZSM5-y-type zeolite of alumina-free as patent US5417950, US5514204 points out to use silica gel and other A of no metallic cation, X, y-type zeolite, US2568396 and US41495858 point out to use activated charcoal or activated charcoal, but the total shortcoming of above these sorbent materials is easy to promote nitric oxide gas generation disproportionation reaction exactly, cause nitrogen peroxide and Nitrous Oxide foreign matter content to increase, still can not satisfy the requirement of 3N purity nitric oxide gas.
Summary of the invention:
The present invention is in order to solve the above-mentioned technical problem of existing in prior technology, provides that a kind of operating procedure is simple, cost is low, the purification process of the 3N that purity is high (99.9%) purity nitric oxide gas.
Technical solution of the present invention is: a kind of purification process of 3N purity nitric oxide gas, comprise decomposing with dilute sulphuric acid Sodium Nitrite, alkali lye absorption, gas-liquid separation, the dry separation obtaining gas, it is characterized in that: the gas of drying be that-20 ℃～30 ℃, pressure are that forward passes through polyoxyethylene glycol-alkylmethacrylate polymer adsorption zone under the condition of 0.5MPa～1.5MPa in temperature; Collection is through the gas of absorption.
Described pressure is 0.6MPa～0.8MPa preferably, carries out multiple absorption.
Described polyoxyethylene glycol-alkylmethacrylate polymer at adsorption zone with average 400～500m
2/ g surface-area gross porosity web form exists.
Described collection is freezing collection through the gas of absorption.
Adsorption zone pressure can be reduced to 0.1MPa～0.4MPa, the gas collected with part carries out purge.
The present invention adopts polyoxyethylene glycol monomethyl acrylonitrile copolymer as sorbent material, can effectively suppress nitrogen protoxide disproportionation and oxidizing reaction, reduced the content of nitrogen peroxide and Nitrous Oxide impurity, improved the purity of nitric oxide gas, nitric oxide gas purity behind the purifying is greater than 99.9%, nitrogen peroxide content is less than 20ppm, and Nitrous Oxide is less than 50ppm.Especially adopt by secondary circulation adsorption process, forward absorption foreign gas, oppositely step-down makes adsorbent reactivation simultaneously, and operating procedure is simple, with low cost.
Description of drawings:
Fig. 1 is the process flow sheet of the embodiment of the invention.
Embodiment:
Below in conjunction with description of drawings the specific embodiment of the present invention.
The same with prior art, Sodium Nitrite and dilute sulphuric acid are reacted in reaction tank, with sodium sulfate and sodium nitrate solution and a spot of CO of remaining reaction solution and generation
2, small portion SO
2, NO
2Absorb to separate from the bottom of reactor by alkali lye and remove most of NO with washing
2, N
2O, water vapor etc. flow out from reactor top with gaseous form with NO; Water vapor is absorbed in by the moisture eliminator that has or not water calcium chloride to exist at gas stream and removes.Different is with polyoxyethylene glycol-methacrylonitrile copolymers sorbent material with prior art in the present invention, absorption NO
2, N
2O impurity.Promptly as shown in Figure 1: comprise decomposing Sodium Nitrite, alkali lye absorption, gas-liquid separation, the dry separation obtaining gas that the gas of drying be that-20 ℃～30 ℃, pressure are that forward passes through gross porosity polyoxyethylene glycol-alkylmethacrylate polymer adsorption zone under the condition of 0.5MPa～1.5MPa in temperature with dilute sulphuric acid; Collection is through the gas of absorption.First class absorber regulation and control pressure is preferably in 0.8MPa, and polyoxyethylene glycol-methacrylonitrile interpolymer sorbent material is with average 450m
2/ g surface-area gross porosity web form exists, and is fixed on sorbent material device bottom by quartz layer, and second class absorber regulation and control pressure is preferably in 0.6MPa, the same layout.The gas stream forward is by the one-level second class absorber, adsorber is outer to be placed in the liquid nitrogen container by pipeline connection 1L stainless steel gas cylinder (89mm (D) * 340mm (H)), gas behind the purifying finally is collected in the gas cylinder with liquid form, by heating it is existed with gas form during use.
Used polyoxyethylene glycol-methacrylonitrile copolymers adopts the imported product of going up seapeak crane chemical industry company limited, model pegzoodma-99%, and the model that perhaps adopts Hayes Separation Inc to be produced is the HayeSep.RTM. series product.
By the infrared spectrum Measurement and analysis, gas contains the nitrogen peroxide that is no more than 20ppm, is less than the Nitrous Oxide of 50ppm and is lower than the nitrogen (nitric oxide gas is used not influence) of 800ppm behind the collected purifying, and nitric oxide production purity is greater than 99.9%.
For making adsorbent reactivation, to save cost: can be to the adsorption zone step-down, pressure is less than the pressure in when absorption, be preferably in 0.1MPa～0.4MPa, make sorbent material slough institute's absorbing material, the high-purity nitric oxide gas that has made with part carries out purge then, and to reach the purification purpose, the regenerated sorbent material can be reused.
Can design the group number of adsorber in the actually operating as required, monitoring and regulator control system automatically are installed, gas adsorption purifying and adsorbent reactivation process are rationally turned round.
Claims (5)
1. the purification process of a 3N purity nitric oxide gas, comprise decomposing with dilute sulphuric acid Sodium Nitrite, alkali lye absorption, gas-liquid separation, the dry separation obtaining gas, it is characterized in that: the gas of drying be that-20 ℃～30 ℃, pressure are that forward passes through polyoxyethylene glycol-alkylmethacrylate polymer adsorption zone under the condition of 0.5MPa～1.5MPa in temperature; Collection is through the gas of absorption.
2. the purification process of 3N purity nitric oxide gas according to claim 1 is characterized in that: described pressure is 0.6MPa～0.8MPa, carries out multiple absorption.
3. the purification process of 3N purity nitric oxide gas according to claim 1 and 2 is characterized in that: described polyoxyethylene glycol-alkylmethacrylate polymer at adsorption zone with average 400～500m
2/ g surface-area gross porosity web form exists.
4. the purification process of 3N purity nitric oxide gas according to claim 3 is characterized in that: described collection is freezing collection through the gas of absorption.
5. the purification process of 3N purity nitric oxide gas according to claim 1 and 2 is characterized in that: adsorption zone pressure is reduced to 0.1MPa～0.4MPa, and the gas collected with part carries out purge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102296033A CN101428773A (en) | 2008-12-11 | 2008-12-11 | Purifying method for nitric oxide gas with 3N purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102296033A CN101428773A (en) | 2008-12-11 | 2008-12-11 | Purifying method for nitric oxide gas with 3N purity |
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| Publication Number | Publication Date |
|---|---|
| CN101428773A true CN101428773A (en) | 2009-05-13 |
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ID=40644455
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008102296033A Pending CN101428773A (en) | 2008-12-11 | 2008-12-11 | Purifying method for nitric oxide gas with 3N purity |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275882A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Preparation method of NO needed for oxalate production |
| CN102556987A (en) * | 2010-12-30 | 2012-07-11 | 佛山市华特气体有限公司 | Method for purifying nitric oxide gas |
| CN102887492A (en) * | 2012-09-28 | 2013-01-23 | 中国地质大学（武汉） | Device for converting nitrite into nitrous oxide for purification and method thereof |
| CN102897727A (en) * | 2012-11-07 | 2013-01-30 | 大连光明特种气体有限公司 | Purification method of 4N-purity nitric oxide gas |
| 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 |
-
2008
- 2008-12-11 CN CNA2008102296033A patent/CN101428773A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275882A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Preparation method of NO needed for oxalate production |
| CN102275882B (en) * | 2010-06-11 | 2013-06-05 | 中国石油化工股份有限公司 | Preparation method of NO needed for oxalate production |
| CN102556987A (en) * | 2010-12-30 | 2012-07-11 | 佛山市华特气体有限公司 | Method for purifying nitric oxide gas |
| CN102556987B (en) * | 2010-12-30 | 2014-12-10 | 佛山市华特气体有限公司 | Method for purifying nitric oxide gas |
| CN102887492A (en) * | 2012-09-28 | 2013-01-23 | 中国地质大学（武汉） | Device for converting nitrite into nitrous oxide for purification and method thereof |
| CN102897727A (en) * | 2012-11-07 | 2013-01-30 | 大连光明特种气体有限公司 | Purification method of 4N-purity nitric oxide gas |
| 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 |
| CN117225304B (en) * | 2023-11-13 | 2024-02-09 | 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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Open date: 20090513 |