CN103203159B - 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 PDF

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CN103203159B
CN103203159B CN201310118606.0A CN201310118606A CN103203159B CN 103203159 B CN103203159 B CN 103203159B CN 201310118606 A CN201310118606 A CN 201310118606A CN 103203159 B CN103203159 B CN 103203159B
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carbon dioxide
molecular sieve
sub
zeolite molecular
oxygenated
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CN201310118606.0A
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CN103203159A (en
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朱伟东
王宁伟
尚昊
许春慧
涂高美
傅仰河
钟依均
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浙江师范大学
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C10/00CO2 capture or storage
    • Y02C10/08Capture by adsorption
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases [GHG] other than CO2
    • Y02C20/10Capture or disposal of greenhouse gases [GHG] other than CO2 of nitrous oxide (N2O)

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

A kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide

Technical field

The present invention relates to mixed gas separation technical field, particularly a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide.

Background technology

The discharge of greenhouse gases causes global warming.According to estimates, carbon dioxide (CO 2) discharge constitute about 84% of U.S.'s greenhouse gas emission in 2000.CO 2increase closely related with the discharge capacity of other hazardous air pollutants with economical and industry.Usual CO 2primary discharge derive from the burning of fossil fuel and various generation CO 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) be also 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 (GWP) of O is CO 2298 times, its life-span in an atmosphere reaches 114 years, and this makes N 2o becomes a kind of greenhouse gases having more threat.N 2the discharge of O primarily of caused by agricultural and industrial processes, e.g., the burning of nitrogen-containing compound, nitric acid and the production of adipic acid and process (the Javier P é rez-Ram í rez etc. of waste water, AppliedCatalysis B:Environmental, 2003,44,117 – 151).Although N 2o is not the significant contributor of global warming, but it is one of six kinds of greenhouse gases of the needs reduction of discharging of united state United Nations Framework Convention on Climate Change defined.Therefore, in industrial processes (in routine adipic acid industrial production), people have been devoted to reduce N 2the discharge of O.Due to the N containing higher concentration in adipic acid industrial tail gas 2o gas (25-40vol.%), catalytic decomposition N 2the method of O is successfully applied, and effectively can reduce N 2the discharge of O.And in nitric acid production industrial tail gas, due to N 2o relative concentration is lower (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 products, routine N 2o can direct oxidation Benzene to phenol (Fumin Zhang etc., Catalysis Science & Technology, 2011,1,1250-1255).Therefore, a kind of effective N of exploitation 2o isolation technics, both can realize N 2the reduction of discharging of O can increase N again 2the industrial utility value of O.

Due to N 2o and CO 2molecular weight identical, their molecular dimension is very close, as far as we know, report in open source literature utilize porous material physisorphtion be difficult to realize both separation.Absorption method is one of effective technology of gas separaion, and its core is to select and development high-efficiency adsorbent.But not yet having at present can separation of C O 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 novel metal-organic framework materials, formed by metal ion (mainly zinc ion and cobalt ions) and the self assembly of imidazole and its derivants class organic ligand, there is high porosity, bigger serface, high thermal stability and chemical stability, aperture is adjustable, be easy to the features such as finishing, thus have a good application prospect in gas separaion field as adsorbent.ZIF-7 is wherein a kind of, each summit of its skeleton structure is made up of metallic zinc ion and in this skeleton structure, each adjacent vertex to be connected (Kyo Sung Park etc. by the nitrogen-atoms of benzimidazole, PANS, 2006, 103, 10186-10191), its distinctive " enabling effect " (Gate-openingeffects) makes it in light paraffins/olefin adsorption separation, show application prospect (Johan van den Bergh etc., 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 that utilizes have not been reported.

Summary of the invention

The object of this invention is to provide a kind of method utilizing the sub-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 utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, and this utilizes the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide to comprise the following steps:

(1) take class zeolite molecular sieve framework material;

(2) will be sub-sieved into the adsorbent of graininess as adsorbing separation nitrous oxide and carbon dioxide mix gas after class zeolite molecular sieve framework material under pressure compressing tablet;

By step (2) in obtain absorbent filling in a fixed-bed tube reactor, pretreatment is carried out to adsorbent;

(4) preparation raw material gas;

(5) the unstripped gas that (4) step is prepared is penetrated the fixed-bed tube reactor of filled with adsorbent, dividing potential drop, the operating temperature and pressure of each component of modulation unstripped gas;

(6), after the adsorbent in fixed-bed tube reactor reaches adsorption equilibrium, reached the object of the sub-nitrogen of separation of oxygenated and carbon dioxide by the nitrous oxide that adsorbs and carbon dioxide by inert gas purge.

A kind ofly to utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, described class zeolite molecular sieve framework material is ZIF-7.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (2) in, tableting pressure is 1 ~ 10MPa, and the granular size of class zeolite molecular sieve framework material is 10 ~ 100 orders.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (3) in, fixed-bed tube reactor adopts stainless steel material to make.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (3) in, carrying out pretreated method to adsorbent is: under the condition of temperature 373 ~ 573K, adopts inert gas to purge adsorbent; Inert gas preferably adopts helium.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (4) in, nitrous oxide-containing and carbon dioxide in unstripped gas.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (5) in, each partial component pressure scope of unstripped gas is at 10 ~ 100kPa.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (5) in, operating temperature is 298 ± 10K.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (5) in, adsorptive pressure is 200 ± 10kPa.

A kind ofly utilize in the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide above-mentioned, step (6) in, inert gas adopts helium.

The present invention there is the sub-nitrogen of separation of oxygenated and carbon dioxide process easy, cost is low, effective feature.

Accompanying drawing illustrates:

Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of ZIF-7 sample in embodiment 1.

Fig. 2 is the N of ZIF-7 sample under 298K in embodiment 1 2o Adsorption and desorption isotherms and CO 2adsorption and desorption isotherms.

Fig. 3 is in embodiment 2 under 298K, 200kPa condition, 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 in embodiment 3 under 298K, 200kPa condition, 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 in embodiment 4 under 298K, 200kPa condition, 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.

Detailed description of the invention

Below by embodiment the present invention made and further illustrating, but the present invention is not limited only to these embodiments.

In embodiment 1, synthesize a certain amount of ZIF-7 sample and penetrate post separating experiment for describing in detail in embodiment 2 to 4.The synthesis and structure feature being applicable to relevant ZIF-7 of the present invention is disclosed in US Patent No. 2007/0202038A1.In the present invention, the synthesis of ZIF-7 is the synthetic method with reference to people (Yan-Shuo Li etc., Adv.Mater.2010,22,3322-3326) such as Li, slightly revises.

Embodiment 1

The zinc chloride (ZnCl) of 272.4mg is dissolved in the DMF (DMF) of 20mL and is configured to solution A; By the benzimidazole (C of 354mg 7h 6n 2) be dissolved in the DMF of 20mL, then the diethylamine (DEA) adding 0.52mL is configured to solution B; Solution B adds solution A after stirring 30 minutes.Proceed in polytetrafluoroethylene (PTFE) reactor after the mixed liquor of A and B stirs 30 minutes, react 48 hours under 403K in constant temperature oven.The pressed powder of cooling, alcohol wash, centrifugal rear gained exchanges 48 hours in methanol solution.ZIF-7 sample is obtained after dry 24 hours under 373K condition.

The ZIF-7 sample obtained after X-ray powder diffraction (XRD) characterizes, then carries out N 2o and CO 2one-component gas absorption is tested, sample vacuum outgas pretreatment 8 hours under 473K condition before adsorption experiment.

In FIG, the collection of illustrative plates that the people such as gained XRD collection of illustrative plates and Li report is consistent in the XRD collection of illustrative plates display of ZIF-7 sample, shows that the sample of synthesis is ZIF-7.

The N of ZIF-7 sample under 298K 2o Adsorption and desorption isotherms and CO 2adsorption and desorption isotherms is shown in Fig. 2.Can find from Fig. 2, N 2o and CO 2the hysteresis loop that Adsorption and desorption isotherms all has " enabling effect " causes, and N 2" enabling pressure " (40kPa) of O is lower than CO 2" enabling pressure " (60kPa).The difference of this " enabling pressure " can effectively for N 2o and CO 2the separation of gaseous mixture.The present invention just according to these two kinds of gases on ZIF-7 " enabling pressure " difference and realize N 2o and CO 2the separation of gaseous mixture.

Embodiment 2

Penetrate column technology (Breakthrough column technique) to be used to implement ZIF-7 to the separating property of gaseous mixture.ZIF-7 sample obtained in embodiment 1 is sub-sieved into the particle of 30-40 order size as adsorbent after the tableting under pressure of 1MPa, be in the stainless steel fixed-bed tube reactor of 0.465cm by this absorbent filling at long 15cm, internal diameter, filling ZIF-7 adsorbent 0.8g; Under 473K, use 20mLmin -1helium purge 8 hours; Be cooled to 298K after pretreatment terminates, passing into volume ratio is N 2o:CO 2: the gaseous mixture of He=1:1:8, gaseous mixture overall flow rate is 5mLmin -1, detect the change of each gas component at reactor outlet, draw adsorption breakthrough curve, as shown in Figure 3 a.20mLmin is used instead after adsorbent reaches adsorption equilibrium -1helium purge is adsorbent bed, detects the change of each gas component at reactor outlet, draws desorption curve, as shown in Figure 3 b.N in adsorption breakthrough curve 2o and CO 2almost penetrate out, separating effect is poor simultaneously.N in desorption curve 2o and CO 2desorption is complete fast simultaneously, cannot realize N 2o and CO 2the separation of gaseous mixture.

Embodiment 3

In this embodiment, the volume ratio of gaseous mixture is N 2o:CO 2: He=1:1:2, gaseous mixture overall flow rate is 4mLmin -1, other implementation condition is identical with embodiment 2.Fig. 4 a and Fig. 4 b is respectively this embodiment gained adsorption breakthrough curve and desorption breakthrough curve.Analyzed from adsorption breakthrough curve, under this embodiment condition, because ZIF-7 is to N 2o Preferential adsorption, CO in adsorption penetration air-flow 2concentration apparently higher than N 2o, achieves N 2o and CO 2the separation of gaseous mixture, separating effect is better than embodiment 2.Analyzed from desorption curve, because ZIF-7 is to N 2o Preferential adsorption, N in desorption air-flow 2the concentration of O is apparently higher than CO 2, achieve N 2o and CO 2the separation of gaseous mixture, separating effect is better than embodiment 2.

Embodiment 4

In this embodiment, the volume ratio of gaseous mixture is N 2o:CO 2: He=4.5:4.5:1, gaseous mixture overall flow rate is 5mLmin -1, other implementation condition is identical with embodiment 2.Fig. 5 a and Fig. 5 b is respectively this embodiment gained adsorption breakthrough curve and desorption curve.Analyzed from adsorption breakthrough curve, under this embodiment condition, because ZIF-7 is to N 2o Preferential adsorption, CO in adsorption penetration air-flow 2concentration apparently higher than N 2o, achieves N 2o and CO 2the separation of gaseous mixture, separating effect is better than embodiment 2.Analyzed from desorption curve, because ZIF-7 is to N 2o Preferential adsorption, N in desorption air-flow 2the concentration of O is apparently higher than CO 2, achieve N 2o and CO 2the separation of gaseous mixture, separating effect is better than embodiment 2.

Claims (10)

1. utilize a method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide, it is characterized in that this utilizes the method for the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide to comprise the following steps:
(1) take class zeolite molecular sieve framework material ZIF-7;
(2) will be sub-sieved into the adsorbent of graininess as adsorbing separation nitrous oxide and carbon dioxide mix gas after class zeolite molecular sieve framework material under pressure compressing tablet;
By step (2) in obtain absorbent filling in a fixed-bed tube reactor, pretreatment is carried out to adsorbent;
(4) preparation raw material gas;
(5) the unstripped gas that (4) step is prepared is penetrated the fixed-bed tube reactor of filled with adsorbent, dividing potential drop, the operating temperature and pressure of each component of modulation unstripped gas;
(6), after the adsorbent in fixed-bed tube reactor reaches adsorption equilibrium, reached the object of the sub-nitrogen of separation of oxygenated and carbon dioxide by the nitrous oxide that adsorbs and carbon dioxide by inert gas purge.
2. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (2) in, tableting pressure is 1 ~ 10MPa, and the granular size of class zeolite molecular sieve framework material is 10 ~ 100 orders.
3. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (3) in, fixed-bed tube reactor adopts stainless steel material to make.
4. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (3) in, carrying out pretreated method to adsorbent is: under the condition of temperature 373 ~ 573K, adopts inert gas to purge adsorbent.
5. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 4, is characterized in that described inert gas adopts helium.
6. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (4) in, nitrous oxide-containing and carbon dioxide in unstripped gas.
7. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (5) in, each partial component pressure scope of unstripped gas is at 10 ~ 100kPa.
8. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (5) in, operating temperature is 298 ± 10K.
9. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (5) in, adsorptive pressure is 200 ± 10kPa.
10. a kind of method utilizing the sub-nitrogen of class zeolite molecular sieve framework material separation of oxygenated and carbon dioxide according to claim 1, it is characterized in that step (6) in, inert gas adopts helium.
CN201310118606.0A 2013-04-08 2013-04-08 Method for separating nitrous oxide and carbon dioxide by using zeolite-like molecular sieve skeleton material CN103203159B (en)

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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
CN107081153B (en) * 2017-06-15 2020-02-18 青岛理工大学 Method for reducing Cr (VI) based on catalyst photocatalysis
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

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CN102006921A (en) * 2008-02-21 2011-04-06 埃克森美孚研究工程公司 Separation of carbon dioxide from methane utilizing zeolitic imidazolate framework materials
CN102015065A (en) * 2008-02-21 2011-04-13 埃克森美孚研究工程公司 Separation of carbon dioxide from nitrogen utilizing zeolitic imidazolate framework materials

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