CN103203159A - Method for separating nitrous oxide and carbon dioxide by using zeolite-like molecular sieve skeleton material - Google Patents
Method for separating nitrous oxide and carbon dioxide by using zeolite-like molecular sieve skeleton material Download PDFInfo
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- CN103203159A CN103203159A CN2013101186060A CN201310118606A CN103203159A CN 103203159 A CN103203159 A CN 103203159A CN 2013101186060 A CN2013101186060 A CN 2013101186060A CN 201310118606 A CN201310118606 A CN 201310118606A CN 103203159 A CN103203159 A CN 103203159A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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Abstract
The invention relates to the technical field of mixed gas separation, and particularly relates to a method for separating nitrous oxide and carbon dioxide by using a zeolite-like molecular sieve skeleton material. The method for separating nitrous oxide and carbon dioxide by using a zeolite-like molecular sieve skeleton material comprises the following steps of: weighting a zeolite-like molecular sieve skeleton material; tabletting the zeolite-like molecular sieve skeleton material under the action of pressure, and then sizing the zeolite-like molecular sieve skeleton material into a granular material as an adsorbent for adsorbing separated nitrous oxide and carbon dioxide mixed gas; filling the adsorbent into a fixed bed tubular reactor, and carrying out pretreatment on the adsorbent; preparing a feed gas; enabling the feed gas to pass through the fixed bed tubular reactor filled with the adsorbent, adjusting the partial pressure, operating temperature and pressure of each component of the feed gas; and when the adsorbent in the fixed bed tubular reactor achieves adsorption equilibrium, purging adsorbed nitrous oxide and carbon dioxide by using an inert gas, thereby achieving the purpose of separating nitrous oxide and carbon dioxide. The method disclosed by the invention has a characteristic of simple and convenient separation of nitrous oxide and carbon dioxide.
Description
Technical field
The present invention relates to the mixed gas separation technical field, particularly a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide.
Background technology
The discharging of greenhouse gases has caused global warming.According to estimates, carbon dioxide (CO
2) discharging constituted about 84% of U.S.'s greenhouse gas emission in 2000.CO
2Increase closely related with the discharge capacity of other pernicious gas pollutants with economical and industry.Common CO
2Main discharging derive from burning and the various generation CO of fossil fuel
2In the industrial process of accessory substance, as the burning of hydrocarbon, fossil fuel, the production of cement, lime, iron and steel.
Nitrous oxide (N
2O) also be a kind of important greenhouse gases.At present, the focus of people's concern is at CO
2On this greenhouse gases, but N
2The global warming potential of O (GWP) is CO
2298 times, its life-span in atmosphere reaches 114 years, this makes N
2O becomes a kind of greenhouse gases that have more threat.N
2The discharging of O is mainly by due to agricultural and the industrial processes, as, the production of the burning of nitrogen-containing compound, nitric acid and adipic acid and the processing of waste water (Javier P é rez-Ram í rez etc., Applied Catalysis B:Environmental, 2003,44,117 – 151).Though N
2O is not the main contributor of global warming, but one of six kinds of greenhouse gases that it is reduced discharging by the needs of UNFCCC defined.Therefore, in industrial processes (in the routine adipic acid industrial production), people have been devoted to reduce N
2The discharging of O.Owing to contain the N of higher concentration in the adipic acid industrial tail gas
2O gas (25-40vol.%), catalytic decomposition N
2The method of O successfully is applied, and can reduce N effectively
2The discharging of O.And in the nitric acid production industrial tail gas, because N
2O concentration is relatively low (with CO
2Deng gas coexistence), catalytic decomposition N
2O is difficult to effective application.On the other hand, N
2O can be used as a kind of reaction raw materials, can be applied to produce in other important chemical product routine N
2But O direct oxidation benzene phenol processed (Fumin Zhang etc., Catalysis Science ﹠amp; Technology, 2011,1,1250-1255).Therefore, develop a kind of effective N
2The O isolation technics both can realize N
2The reduction of discharging of O can increase N again
2The industrial utilization of O is worth.
Because N
2O and CO
2Molecular weight identical, their molecular dimension is very close, as far as we know, the porous material physisorphtion of reporting in the open source literature that utilizes is difficult to realize the separation of the two.Absorption method is one of effective technology of gas separation, and its core is to select and the development high-efficiency adsorbent.Can separation of C O but do not have as yet at present
2And N
2The report of O gaseous mixture adsorbent.
Obtained class zeolite molecular sieve framework material (the Zeolitic imidazolate frameworks of extensive concern in recent years, ZIFs) be a kind of new type of metal organic framework material, formed by metal ion (mainly being zinc ion and cobalt ions) and imidazoles and the self assembly of derivative class organic ligand thereof, have high porosity, bigger serface, high thermal stability and chemical stability, the aperture is adjustable, be easy to characteristics such as finishing, thereby have a good application prospect at the gas separation field as adsorbent.ZIF-7 is wherein a kind of, each summit of its skeleton structure constituted by the metallic zinc ion and this skeleton structure in the nitrogen-atoms of each adjacent vertex by benzimidazole (the Kyo Sung Park etc. that are connected, PANS, 2006,103,10186-10191), its distinctive " effect of opening the door " (Gate-opening effects) makes it show application prospect (Johan van den Bergh etc. aspect light paraffins/alkene adsorbing separation, Chem.Eur.J.2011,17,8832-8840), but even to this day, a kind of method of class zeolite molecular sieve framework material adsorbing separation nitrous oxide and carbon dioxide of utilizing yet there are no report.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide mix gas.
Technical scheme of the present invention realizes in the following way: a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, and this utilizes the method for the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide may further comprise the steps:
⑴ take by weighing class zeolite molecular sieve framework material;
With class zeolite molecular sieve framework material under pressure behind the compressing tablet sub-sieve become graininess as the adsorbent of adsorbing separation nitrous oxide and carbon dioxide mix gas;
⑶ be filled in the adsorbent that obtains among the step ⑵ in one fixed-bed tube reactor, and adsorbent is carried out preliminary treatment;
⑷ preparation raw material gas;
⑸ the unstripped gas that prepare step ⑷ penetrates the fixed-bed tube reactor of filled with adsorbent, dividing potential drop, the operating temperature and pressure of each component of modulation unstripped gas;
⑹ after the adsorbent in the fixed-bed tube reactor reaches adsorption equilibrium, and the nitrous oxide that is adsorbed with inert gas purge and carbon dioxide reach the purpose of the inferior nitrogen of separation of oxygenated and carbon dioxide.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, described class zeolite molecular sieve framework material is ZIF-7.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑵, compressing tablet pressure is 1～10MPa, and the granular size of class zeolite molecular sieve framework material is 10～100 orders.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑶, fixed-bed tube reactor adopts stainless steel material to make.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑶, adsorbent is carried out pretreated method is: under the condition of temperature 373～573K, adopt inert gas that adsorbent is purged; Inert gas preferably adopts helium.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑷, nitrous oxide-containing and carbon dioxide in unstripped gas.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑸, each partial component pressure scope of unstripped gas is at 10～100kPa.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑸, operating temperature is 298 ± 10K.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑸, adsorptive pressure is 200 ± 10kPa.
In above-mentioned a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, in step ⑹, inert gas adopts helium.
The present invention have the inferior nitrogen of separation of oxygenated and the carbon dioxide method easy, cost is low, good effectiveness.
Description of drawings:
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of ZIF-7 sample among the embodiment 1.
Fig. 2 is the N of ZIF-7 sample under 298K among the embodiment 1
2O adsorption desorption thermoisopleth and CO
2The adsorption desorption thermoisopleth.
Fig. 3 is 298K among the embodiment 2, under the 200kPa condition, and volume ratio N
2O:CO
2: the gaseous mixture of He=1:1:8 penetrates the suction/desorption breakthrough curve of the adsorbent bed gained of ZIF-7.
Fig. 4 is 298K among the embodiment 3, under the 200kPa condition, and volume ratio N
2O:CO
2: the gaseous mixture of He=1:1:2 penetrates the suction/desorption breakthrough curve of the adsorbent bed gained of ZIF-7.
Fig. 5 is 298K among the embodiment 4, under the 200kPa condition, and volume ratio N
2O:CO
2: the gaseous mixture of He=4.5:4.5:1 penetrates the suction/desorption breakthrough curve of the adsorbent bed gained of ZIF-7.
The specific embodiment
Make further below by the present invention of embodiment and to specify, but the present invention is not limited only to these embodiment.
In embodiment 1, what synthetic a certain amount of ZIF-7 sample was used for describing in detail embodiment 2 to 4 penetrates the post separating experiment.Synthetic and the architectural feature that is applicable to relevant ZIF-7 of the present invention is disclosed among the US Patent No. 2007/0202038A1.Among the present invention ZIF-7 synthetic be with reference to people such as Li (Yan-Shuo Li etc., Adv.Mater.2010,22, synthetic method 3322-3326) is revised slightly.
Embodiment 1
The zinc chloride (ZnCl) of 272.4mg is dissolved in the N of 20mL, is configured to solution A in the dinethylformamide (DMF); Benzimidazole (C with 354mg
7H
6N
2) be dissolved among the DMF of 20mL, the diethylamine (DEA) that adds 0.52mL again is configured to solution B; Solution B stirs after 30 minutes and adds solution A.The mixed liquor of A and B stirs after 30 minutes and changes in the polytetrafluoroethylene (PTFE) reactor, reacts 48 hours under the 403K in the constant temperature oven.Cooling, alcohol are washed, the pressed powder of centrifugal back gained exchanges 48 hours in methanol solution.Obtain the ZIF-7 sample after dry 24 hours under the 373K condition.
Resulting ZIF-7 sample carries out N after characterizing through X-ray powder diffraction (XRD) again
2O and CO
2Sample vacuum outgas preliminary treatment 8 hours under the 473K condition before the one-component gas absorption experiment, adsorption experiment.
The XRD collection of illustrative plates of ZIF-7 sample is presented among Fig. 1, and the collection of illustrative plates of people such as gained XRD collection of illustrative plates and Li report is consistent, shows that synthetic sample is ZIF-7.
The N of ZIF-7 sample under 298K
2O adsorption desorption thermoisopleth and CO
2The adsorption desorption thermoisopleth is seen Fig. 2.From Fig. 2, can find N
2O and CO
2The adsorption desorption thermoisopleth all has the hysteresis loop that " effect of opening the door " causes, and N
2O " pressure opens the door " (40kPa) is lower than CO
2" pressure opens the door " (60kPa).The difference of this " pressure opens the door " can be used for N effectively
2O and CO
2The separation of gaseous mixture.The present invention realizes N according to these two kinds of gases difference of " pressure opens the door " on ZIF-7 just
2O and CO
2The separation of gaseous mixture.
Embodiment 2
Penetrate column technology (Breakthrough column technique) and be used to implement the separating property of the gaseous mixture of ZIF-7.Become the particle of 30-40 order size as adsorbent the ZIF-7 sample sub-sieve behind the pressure lower sheeting of 1MPa that makes among the embodiment 1, with this adsorbent be filled in long 15cm, internal diameter is in the stainless steel fixed-bed tube reactor of 0.465cm, filling ZIF-7 adsorbent 0.8g; Under 473K, use 20mLmin
-1Helium purge 8 hours; Preliminary treatment is cooled to 298K after finishing, and the feeding volume ratio is N
2O:CO
2: the gaseous mixture of He=1:1:8, gaseous mixture overall flow rate are 5mLmin
-1, detect the variation of each gas component at reactor outlet, draw the adsorption penetration curve, shown in Fig. 3 a.After reaching adsorption equilibrium, uses by adsorbent 20mLmin instead
-1Helium purge is adsorbent bed, detects the variation of each gas component at reactor outlet, draws the desorption curve, shown in Fig. 3 b.N in the adsorption penetration curve
2O and CO
2Almost simultaneously penetrate out, separating effect is relatively poor.N in the desorption curve
2O and CO
2Desorption is complete fast simultaneously, can't realize N
2O and CO
2The separation of gaseous mixture.
Embodiment 3
The volume ratio of gaseous mixture is N among this embodiment
2O:CO
2: He=1:1:2, gaseous mixture overall flow rate are 4mLmin
-1, other implementation condition is identical with embodiment 2.Fig. 4 a and Fig. 4 b are respectively this embodiment gained adsorption penetration curve and desorption breakthrough curve.By the adsorption penetration tracing analysis as can be known, under this embodiment condition, because the N of ZIF-7
2The O preferential adsorption, CO in the adsorption penetration air-flow
2Concentration apparently higher than N
2O has realized N
2O and CO
2The separation of gaseous mixture, separating effect are better than embodiment 2.By the desorption tracing analysis as can be known, because the N of ZIF-7
2The O preferential adsorption, N in the desorption air-flow
2The concentration of O is apparently higher than CO
2, realized N
2O and CO
2The separation of gaseous mixture, separating effect are better than embodiment 2.
Embodiment 4
The volume ratio of gaseous mixture is N among this embodiment
2O:CO
2: He=4.5:4.5:1, gaseous mixture overall flow rate are 5mLmin
-1, other implementation condition is identical with embodiment 2.Fig. 5 a and Fig. 5 b are respectively this embodiment gained adsorption penetration curve and desorption curve.By the adsorption penetration tracing analysis as can be known, under this embodiment condition, because the N of ZIF-7
2The O preferential adsorption, CO in the adsorption penetration air-flow
2Concentration apparently higher than N
2O has realized N
2O and CO
2The separation of gaseous mixture, separating effect are better than embodiment 2.By the desorption tracing analysis as can be known, because the N of ZIF-7
2The O preferential adsorption, N in the desorption air-flow
2The concentration of O is apparently higher than CO
2, realized N
2O and CO
2The separation of gaseous mixture, separating effect are better than embodiment 2.
Claims (10)
1. method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide is characterized in that this utilizes the method for the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide may further comprise the steps:
⑴ take by weighing class zeolite molecular sieve framework material;
With class zeolite molecular sieve framework material under pressure behind the compressing tablet sub-sieve become graininess as the adsorbent of adsorbing separation nitrous oxide and carbon dioxide mix gas;
⑶ be filled in the adsorbent that obtains among the step ⑵ in one fixed-bed tube reactor, and adsorbent is carried out preliminary treatment;
⑷ preparation raw material gas;
⑸ the unstripped gas that prepare step ⑷ penetrates the fixed-bed tube reactor of filled with adsorbent, dividing potential drop, the operating temperature and pressure of each component of modulation unstripped gas;
⑹ after the adsorbent in the fixed-bed tube reactor reaches adsorption equilibrium, and the nitrous oxide that is adsorbed with inert gas purge and carbon dioxide reach the purpose of the inferior nitrogen of separation of oxygenated and carbon dioxide.
2. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 is characterized in that described class zeolite molecular sieve framework material is ZIF-7.
3. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2, it is characterized in that in step ⑵, compressing tablet pressure is 1～10MPa, and the granular size of class zeolite molecular sieve framework material is 10～100 orders.
4. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2 is characterized in that in step ⑶ fixed-bed tube reactor adopts stainless steel material to make.
5. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2, it is characterized in that in step ⑶, adsorbent is carried out pretreated method is: under the condition of temperature 373～573K, adopt inert gas that adsorbent is purged; Inert gas preferably adopts helium.
6. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2 is characterized in that in step ⑷ nitrous oxide-containing and carbon dioxide in unstripped gas.
7. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2 is characterized in that in step ⑸ each partial component pressure scope of unstripped gas is at 10～100kPa.
8. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2 is characterized in that in step ⑸ operating temperature is 298 ± 10K.
9. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2 is characterized in that in step ⑸ adsorptive pressure is 200 ± 10kPa.
10. a kind of method of utilizing the inferior nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1 and 2 is characterized in that in step ⑹ inert gas adopts helium.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105879704A (en) * | 2016-03-26 | 2016-08-24 | 上海大学 | Preparation method and application of mixed matrix membrane containing zeolite imidazolate framework material |
| CN106818675A (en) * | 2017-01-20 | 2017-06-13 | 唐成康 | The application and method of modifying of zeolite molecular sieve or modified zeolite molecular sieve in mosquito is caught |
| CN107081153A (en) * | 2017-06-15 | 2017-08-22 | 青岛理工大学 | The method that one kind is based on catalyst photo catalytic reduction Cr (VI) |
| CN107179302A (en) * | 2017-04-24 | 2017-09-19 | 西北师范大学 | Applications of the Zn MOFs in 4 nitrophenols are detected |
| CN107855109A (en) * | 2017-11-03 | 2018-03-30 | 商丘师范学院 | One kind improves the oxazolyl framework material of zeolites containing zinc CO2The method of absorption property |
| CN110538634A (en) * | 2019-08-16 | 2019-12-06 | 太原理工大学 | Preparation and application of amino modified metal organic framework material with high CO2/N2O separation performance |
| CN112675811A (en) * | 2020-12-18 | 2021-04-20 | 太原理工大学 | High-efficiency separation N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereof |
| CN113389533A (en) * | 2021-07-05 | 2021-09-14 | 西南石油大学 | CO (carbon monoxide)2Integrated method for collecting, reservoir reforming and extracting crude oil |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105879704A (en) * | 2016-03-26 | 2016-08-24 | 上海大学 | Preparation method and application of mixed matrix membrane containing zeolite imidazolate framework material |
| CN106818675A (en) * | 2017-01-20 | 2017-06-13 | 唐成康 | The application and method of modifying of zeolite molecular sieve or modified zeolite molecular sieve in mosquito is caught |
| CN107179302A (en) * | 2017-04-24 | 2017-09-19 | 西北师范大学 | Applications of the Zn MOFs in 4 nitrophenols are detected |
| CN107081153A (en) * | 2017-06-15 | 2017-08-22 | 青岛理工大学 | The method that one kind is based on catalyst photo catalytic reduction Cr (VI) |
| CN107855109A (en) * | 2017-11-03 | 2018-03-30 | 商丘师范学院 | One kind improves the oxazolyl framework material of zeolites containing zinc CO2The method of absorption property |
| CN110538634A (en) * | 2019-08-16 | 2019-12-06 | 太原理工大学 | Preparation and application of amino modified metal organic framework material with high CO2/N2O separation performance |
| CN110538634B (en) * | 2019-08-16 | 2022-03-18 | 太原理工大学 | High CO2/N2Preparation and application of amino modified metal organic framework material with O separation performance |
| CN112675811A (en) * | 2020-12-18 | 2021-04-20 | 太原理工大学 | High-efficiency separation N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereof |
| CN112675811B (en) * | 2020-12-18 | 2022-06-21 | 太原理工大学 | High-efficiency separation N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereof |
| CN113389533A (en) * | 2021-07-05 | 2021-09-14 | 西南石油大学 | CO (carbon monoxide)2Integrated method for collecting, reservoir reforming and extracting crude oil |
| CN113389533B (en) * | 2021-07-05 | 2022-03-29 | 西南石油大学 | CO (carbon monoxide)2Integrated method for collecting, reservoir reforming and extracting crude oil |
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