CN107715831A - One kind is used to remove CO in admixture of gas2Adsorbent and preparation method thereof - Google Patents
One kind is used to remove CO in admixture of gas2Adsorbent and preparation method thereof Download PDFInfo
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- CN107715831A CN107715831A CN201711115038.3A CN201711115038A CN107715831A CN 107715831 A CN107715831 A CN 107715831A CN 201711115038 A CN201711115038 A CN 201711115038A CN 107715831 A CN107715831 A CN 107715831A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses one kind to be used to remove in admixture of gas CO in such as waste gas2Adsorbent, the adsorbent is DD3R molecular sieves, it is by the way that the previously prepared sieve particle wet ball grindings of sigma 1 and stewing process are obtained into crystal seed, and is mixed in the Synthesis liquid containing low template, and coordinates two sections of crystallization process to prepare the DD3R molecular sieves of high-purity.
Description
Technical field
It is more particularly to a kind of to be used to remove in admixture of gas the present invention relates to a kind of preparation method of environmental-protection adsorption agent
CO2Adsorbent preparation method.
Background technology
With the increase that environmental protection and energy-saving and emission-reduction are realized, the adsorbing separation skill based on zeolite molecular sieve as adsorbent
Art is increasingly by the concern and attention of world community.Molecular sieve refers to there is uniform micropore, and its aperture and general molecule are big
Small suitable a kind of material.The application of molecular sieve is very extensive, can make efficient drying agent, selective absorbent, catalyst, from
Sub- exchanger etc., but use the cost of chemical raw material synthesis of molecular sieve very high.Conventional molecular sieve for crystalline state silicate or
Alumino-silicate, it is to be connected by silicon-oxy tetrahedron or aluminum-oxygen tetrahedron by oxygen bridge key to form the duct of molecular dimension size and sky
Cavity system, there is the ability for sieving fluid molecule of different sizes because binding molecule size and shape is different.
DD3R molecular sieves are a kind of molecular sieves of total silicon DDR configurations, have three-dimensional pore passage structure, and its duct size is
0.36*0.44nm.According to CO2Molecular diameter, there is the DDR molecular sieve of octatomic ring structure one of for preferable adsorbent.
Research in recent years can prove that DD3R molecular sieves can effectively adsorb, separate CO2.Compared to A type molecular sieve, DD3R knots
Structure is complete silicon structure, hydrophobic very capable, and preferable CO is remained in that under high temperature, aqueous environment2Adsorptive selectivity.
Although DD3R molecular sieves structure is preferable, the research paper of its application in reality and correlation, patent compared with
Other kinds of molecular sieve, such as few pitiful such as NaA, MFI, T-shaped, it is exactly that its building-up process is complex to trace it to its cause,
Such as need to be up to 25 days as long as according to traditional in-situ preparation.At present, synthesis DD3R molecular sieves use document (STATE OF more
THE ART) in dynamic synthetic method, it needs the tedious steps such as high temperature oil bath, ice bath, and it is ADA (moulds that it, which synthesizes formula of liquid,
Plate agent):SIO2（Silicon source）:EDA（Mineralizer ethylenediamine）:H2O=47:100:404:11240.Later scholar has attempted synthesizing again
Crystal seed well prepared in advance is added in liquid, generated time can be foreshortened to 2d.Some scholars attempt to prepare under fluorine-containing system
DD3R molecular sieves, the time can also be greatly shortened, but fluorine-containing system is unfavorable to environment, is not suitable for large-scale production.Also have
Scholar is attempted, as crystal seed, it can be as short as completing crystallization mistake in 9h after the Sigma-1 ball millings for belonging to DDR configurations together with DD3R
Journey.In addition, the selection for silicon source and mineralizer, also has different scholars to carry out various trials.
But change substantially less, substantially using ADA in various documents, the formula on Synthesis liquid:SiO2:EDA:H2O=
47:100:404:11240 formula, also there is a document using different formulations, but its ADA and SiO2Mol ratio keep substantially
In 0.5 or so even more high.And as the amantadine of template, its is expensive, and it significantly improves DD3R molecular screen membranes
Preparation cost, therefore, be badly in need of it is a kind of with reduce the method for amantadine dosage formula prepare DD3R molecular sieves.
The content of the invention
The present invention proposes CO in a kind of removing admixture of gas2Adsorbent method, the adsorbent is DD3R molecules
Sieve, formed by the addition sigma-1 crystal seed hydrothermal crystallizings in Hydrothermal Synthesiss liquid, wherein described sigma-1 crystal seeds be by
Sigma-1 particles well prepared in advance carry out wet ball grinding after being mixed with water, wherein, rotational speed of ball-mill 400-600rpm, ball milling
Time is 3-4h, and ball milling program is that ball milling 10min stands 2-5min, and ball milling liquid is stood into 4h-5h, takes lower sediment thing to dry
It is dry standby；Described hydrothermal crystallization process is that sigma-1 crystal seeds are added into Synthesis liquid to be placed in synthesis reactor, and synthesis reactor is put
It is that it is gradually heating to 100-120 DEG C from room temperature and keeps 0.5-2h to enter in baking oven one, and programming rate is 0.5-2 DEG C/min, with
Synthesis reactor is transferred to afterwards to have warmed up into 180-200 DEG C of baking oven two and continues crystallization 12-24h.
Preferably, adamantane and SiO are contained in Synthesis liquid2, wherein amantadine and SIO2Mol ratio be not higher than 0.2.
Preferably, amantadine and SIO in Synthesis liquid2Mol ratio be not less than 0.05.
Preferably, mineralizer is contained in Synthesis liquid, the mineralizer is non-fluorine-containing mineralizer.
Preferably, the mineralizer is ethylenediamine.
Preferably, used ball milling ball is zirconium oxide material.
Preferably, it is described that Synthesis liquid is centrifuged in crystallization process, clean, dry and is calcined with removed template method.
Preferably, described DD3R particles are that have microwave process for synthesizing to be prepared.
The invention also provides one kind is used to remove CO in admixture of gas2Adsorbent, the adsorbent is DD3R molecules
Sieve, formed by the addition sigma-1 crystal seed hydrothermal crystallizings in Hydrothermal Synthesiss liquid, wherein described sigma-1 crystal seeds be by
Sigma-1 particles well prepared in advance carry out wet ball grinding after being mixed with water, wherein, rotational speed of ball-mill 400-600rpm, ball milling
Time is 3-4h, and ball milling program is that ball milling 10min stands 2-5min, and ball milling liquid is stood into 4h-5h, takes lower sediment thing to dry
It is dry standby；Described hydrothermal crystallization process is that sigma-1 crystal seeds are added into Synthesis liquid to be placed in synthesis reactor, and synthesis reactor is put
It is that it is gradually heating to 100-120 DEG C from room temperature and keeps 0.5-2h to enter in baking oven one, and programming rate is 0.5-2 DEG C/min, with
Synthesis reactor is transferred to afterwards to have warmed up into 180-200 DEG C of baking oven two and continues crystallization 12-24h.
Molecular sieve prepared by the present invention is applied removes CO in admixture of gas2, it is preferable that described admixture of gas
For one kind in industrial tail gas, natural gas, biogas etc..
The Integral Thought of the present invention is to be obtained in the Synthesis liquid of low concentration ADA contents by adding ball milling+standing method
Crystal seed with appropriate particle size scope and with stronger nucleus inducibility, and coordinate suitable crystallization temperature to have to obtain
The molecular sieve of even particle diameter distribution.
Technical scheme compared with prior art, has the characteristics that；
1. ADA/SiO in the Synthesis liquid of the present invention2Mol ratio be not higher than 0.2, hence it is evident that less than ratio in the prior art, and use
Ethylenediamine is mineralizer, does not use fluorine-containing mineralizer, the problems such as avoiding environmental pollution.Therefore, the method that the present invention is protected
DD3R Zeolite synthesis costs are advantageously reduced, are advantageous to its industrialized production.
2. secondly, although having in the prior art using crystal seed is used as after Sigma-1 ball millings, it equally uses Gao Mo
The Synthesis liquid of plate agent content, the present invention be made that further optimization on its basis, by ball milling parameter include rotational speed of ball-mill,
Ball-milling Time, ball milling quiescent time are broken as far as possible by complete sigma-1 molecular sieves to ensure, and coordinate follow-up standing
Infall process by ball milling into unformed devolatilization to ensure to be substantially free of unformed material in crystal seed, so as to prevent low
In the Synthesis liquid of template agent content, unformed material induction produces SGT stray crystals and coordinates two sections of follow-up crystallization process to ensure
DD3R purity.Sigma-1 particle requirements as induction crystal seed have uniform particle size, and this is due to that the particle of heterogeneity particle diameter exists
Mechanical milling process degree of crushing is difficult to ensure that homogeneous, may cause the particle that has not by ball milling, and some particles by ball milling into
Unformed shape, it is therefore necessary to ensure that the particle as crystal seed has narrow particle diameter distribution, therefore preferably use microwave hydrothermal legal system
Into sigma-1 molecular sieves, its uniform particle diameter, about 500nm, concrete operation method be by sigma-1 Synthesis liquids be placed in microwave close
Into in kettle, 180 DEG C of hydrothermal crystallizing 12h.
3. in addition, also the crystallization process of DD3R molecular sieves is optimized by the present invention.The present invention is by Synthesis liquid from room temperature
It is to slowly warm up to medium temperature and is kept for a period of time so that is slowly drawn into the induced particle in Synthesis liquid in Synthesis liquid
Nutritional ingredient is nucleated, and avoiding transitting directly to crystallization temperature from room temperature causes the generation of SGT stray crystals.
Brief description of the drawings
The present invention is further described in conjunction with the accompanying drawings and embodiments：
Fig. 1 is the specific preparation method of decarburization molecular sieve involved in the present invention
Fig. 2 is the XRD of the molecular sieve prepared by the present invention, and wherein A is DDR standard diagrams, and B is sample prepared by embodiment 1
Collection of illustrative plates.
Fig. 3 is sieve sample SEM photograph prepared by the embodiment of the present invention 1.
Embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings：
It is further details of explanation to the present invention presently in connection with drawings and examples.The accompanying drawing is simplified schematic diagram, only with
Illustration illustrates the essential structure of the present invention, therefore it only shows the composition relevant with the present invention.
Embodiment 1
As shown in Figure 1, it specifically includes following steps to the embodiment preparation method：
Step（1）It is prepared by crystal seed liquid
By sigma-1 particles well prepared in advance（Prepared, 180 DEG C, crystallization time 12h of crystallization temperature, put down using microwave-hydrothermal method
Equal particle diameter is 500nm）Mixed with deionized water, both mass ratioes are 5：95, agitated 20min, ultrasonic 10min are handled to ensure
It is well mixed.Mixed liquor is poured into 250ml ball grinders, and adds zirconium oxide ball milling pearl（Diameter 3mm）, set rotational speed of ball-mill as
6000rpm, Ball-milling Time 3h, ball milling program are that ball milling 10min stands 5min.After ball milling terminates, suction ball grinding fluid is in burning
In cup, 4h is stored at room temperature after sealing.Supernatant liquor is separated with lower sediment, takes lower sediment thing to be dried for standby.
Step（2）Synthesis liquid is prepared
Powdered amantadine is taken, is mixed with ethylenediamine.Through stirring repeatedly and supersound process is completely dissolved amantadine
In ethylenediamine, deionized water is added again, and stirs ultrasonic 30min, and in the state of lasting stirring ultrasound, gas is added dropwise dropwise
State silica.Mixed liquor is stirred into aging 1h at 60 DEG C after completion of dropwise addition and obtains Synthesis liquid, wherein amantadine, titanium dioxide
The mol ratio of silicon, ethylenediamine and water is 15:100:150:11240.
Step（3）Crystallization
Two standby baking ovens are taken, wherein baking oven one does not make any setting, and baking oven two is set in advance arrives 180 DEG C of crystallization temperature.Will be standby
Sigma-1 crystal seeds are added into Synthesis liquid, and both mass ratioes are 1:99, it is ultrasonically treated 10min.Mixed liquor is placed in conjunction
Into in kettle.Synthesis reactor, which is put into, to set in baking oven one makes it programming rate is 2 DEG C/min, and is kept from room temperature to 100 DEG C
2h, then synthesis reactor is transferred to have warmed up into 180 DEG C of baking oven two and continues crystallization 24h.After crystallization terminates, by Synthesis liquid from
The heart, cleaning, drying, and in 700 DEG C of Muffle kiln roasting 4h with removed template method, warming and cooling rate is 1 DEG C/min.The embodiment
Prepared sample number into spectrum is Y1.
Embodiment 2
Embodiment 2 uses method to be substantially similar to embodiment 1, and difference is that Synthesis liquid proportioning is matched using document, i.e.,
Amantadine, silica, the mol ratio of ethylenediamine and water are 47:100:404:11240, prepared sample number into spectrum is Y2.
Embodiment 3
Embodiment 3 uses method to be substantially similar to embodiment 1, and difference is that Synthesis liquid proportioning is amantadine, dioxy
The mol ratio of SiClx, ethylenediamine and water is 4:100:40:11240, prepared sample number into spectrum is Y3.
Embodiment 4
Embodiment 4 uses method to be substantially similar to embodiment 1, and difference is without ball milling adding crystal seed in Synthesis liquid
The sigma-1 particles of processing, prepared sample number into spectrum are Y4.
Embodiment 5
Embodiment 5 uses method to be substantially similar to embodiment 1, and difference is non-stewing process after sigma-1 ball millings
And direct drying and processing, prepared sample number into spectrum are Y5.
Embodiment 6
Embodiment 6 uses method to be substantially similar to embodiment 1, and difference is that crystallization process does not use baking oven one, but
Directly synthesis reactor is placed in the baking oven two for setting 180 DEG C, prepared sample number into spectrum is Y6.
Embodiment 7
Embodiment 6 uses method to be substantially similar to embodiment 1, and difference is that crystallization process is directly to be placed in synthesis reactor
Baking oven at room temperature, and 180 DEG C are to slowly warm up to, prepared sample number into spectrum is Y7.
Embodiment 8
Embodiment 8 uses method to be substantially similar to embodiment 1, and the sigma-1 used by difference is is light water
Prepared by hot method, i.e., heated using baking oven, and crystallization temperature is 180 DEG C, crystallization time 6d, and prepared sample number into spectrum is Y8.
Sample Y1-Y8 prepared by above-described embodiment carries out XRD and SEM and characterized, and its result is as shown in table 1：
Sample characterization result prepared by 1 each embodiment of table
The sample Y1 prepared using the present invention（That is embodiment 1）XRD as shown in Figure 2, its with standard diagram substantially completely
Unanimously.And SEM photograph is as shown in figure 3, its presentation brilliant, particle diameter is about 1 μm.The above results show to make using the present invention
The DD3R molecular sieves of standby high-purity.
Embodiment 2 can equally prepare the DD3R samples of high-purity, and calculate yield and the phase of embodiment 1 according to element silicon
When.The synthesis raffinate centrifuged after its crystallization analyze in invention sample and still contains a certain amount of amantadine, table
Bright template is excessive.
Embodiment 3 used the Synthesis liquid of low content template, and result is that unformed material is essentially in sample, and only zero
The DD3R molecular sieves of star.
Embodiment 4 is SGT stray crystals substantially in results sample as crystal seed using non-ball milling sigma-1 particles.
For embodiment 5 using the sigma-1 particles of the non-settlement treatment of ball milling as crystal seed, result is that DD3R and SGT coexists, this
It is due to because ball milling causes partial particulate to be entered by the not unformed material of mechanical ball mill, the material in Synthesis liquid in crystallization process
In easily induction SGT crystal.
Embodiment 6,7 uses single phase crystallization process, and more or less DOH stray crystals occurs in both of which, and this is due to this
The higher reason of invention synthesis temperature.
Embodiment 8 prepares sigma-1 crystal seeds using common hydro-thermal method, the result is that SGT stray crystals in sample be present, this be by
In the serious heterogeneity of sigma-1 grains prepared by common hydro-thermal method, cause after ball milling particle still heterogeneity, exist not by
Ball milling particle, so as to cause SGT generation.
It can apply to remove CO in admixture of gas using the molecular sieve prepared by the present invention2In, described gas mixes
Compound is one kind in industrial tail gas, natural gas, biogas etc..
Highly preferred embodiment of the present invention is the foregoing is only, is not intended to limit the invention.It is all the present invention principle and
Any modification, equivalent substitution and improvements done within spirit etc., should be included within the scope of the present invention.
Claims (10)
1. one kind is used to remove CO in admixture of gas2The preparation method of adsorbent, it is characterised in that the adsorbent is DD3R molecules
Sieve, formed by the addition sigma-1 crystal seed hydrothermal crystallizings in Hydrothermal Synthesiss liquid, wherein described sigma-1 crystal seeds be by
Sigma-1 particles well prepared in advance carry out wet ball grinding after being mixed with water, wherein, rotational speed of ball-mill 400-600rpm, ball milling
Time is 3-4h, and ball milling program is that ball milling 10min stands 2-5min, and ball milling liquid is stood into 4h-5h, takes lower sediment thing to dry
It is dry standby；Described hydrothermal crystallization process is that sigma-1 crystal seeds are added into Synthesis liquid to be placed in synthesis reactor, and synthesis reactor is put
It is that it is gradually heating to 100-120 DEG C from room temperature and keeps 0.5-2h to enter in baking oven one, and programming rate is 0.5-2 DEG C/min, with
Synthesis reactor is transferred to afterwards to have warmed up into 180-200 DEG C of baking oven two and continues crystallization 12-24h.
2. according to the method for claim 1, it is characterised in that contain adamantane and SiO in Synthesis liquid2, wherein amantadine
And SiO2Mol ratio be not higher than 0.2.
3. according to the method for claim 1, it is characterised in that amantadine and SiO in Synthesis liquid2Mol ratio be not less than
0.05。
4. according to the method for claim 1, it is characterised in that contain mineralizer in Synthesis liquid, the mineralizer is non-Fluoride-bearing Ore
Agent.
5. according to the method for claim 1, it is characterised in that contain mineralizer in Synthesis liquid, the mineralizer is ethylenediamine.
Ball milling ball is zirconium oxide material used by 6. according to the method for claim 1, its spy is.
7. according to the method for claim 1, it is characterised in that Synthesis liquid is centrifuged in crystallization process, cleaned, is dried and
Roasting is with removed template method.
8. according to the method for claim 1, it is characterised in that described sigma-1 particles be by microwave process for synthesizing prepare and
Into.
9. one kind is used to remove CO in admixture of gas2Adsorbent, it is characterised in that the adsorbent is DD3R molecular sieves, is passed through
Addition sigma-1 crystal seed hydrothermal crystallizings in Hydrothermal Synthesiss liquid form, wherein described sigma-1 crystal seeds are will be previously prepared
Good sigma-1 particles carry out wet ball grinding after being mixed with water, wherein, rotational speed of ball-mill 400-600rpm, Ball-milling Time 3-
4h, ball milling program is that ball milling 10min stands 2-5min, and ball milling liquid is stood into 4h-5h, takes lower sediment thing to be dried for standby；Institute
The hydrothermal crystallization process stated is that sigma-1 crystal seeds are added into Synthesis liquid to be placed in synthesis reactor, and synthesis reactor is put into baking oven one
In be that it is gradually heating to 100-120 DEG C from room temperature and keeps 0.5-2h, programming rate is 0.5-2 DEG C/min, then will synthesis
Kettle, which is transferred to have warmed up into 180-200 DEG C of baking oven two, continues crystallization 12-24h.
10. a kind of adsorbent according to claim 9 removes CO in admixture of gas2Application, it is characterised in that it is described
Admixture of gas be one kind in industrial tail gas, natural gas, biogas etc., admixture of gas is realized by the adsorbent de-
Except CO2。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603896A (en) * | 2018-12-29 | 2019-04-12 | 韩旭霞 | A kind of purifying formaldehyde material |
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| CN102786065A (en) * | 2012-08-21 | 2012-11-21 | 浙江师范大学 | Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size |
| CN104925826A (en) * | 2015-06-02 | 2015-09-23 | 中国科学院上海高等研究院 | Method for preparing DD3R molecular sieve |
| CN106621858A (en) * | 2017-02-04 | 2017-05-10 | 耿逸豪 | High-yield synthetic method for DD3R molecular sieve film |
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- 2017-11-13 CN CN201711115038.3A patent/CN107715831B/en active Active
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| CN102786065A (en) * | 2012-08-21 | 2012-11-21 | 浙江师范大学 | Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size |
| CN104925826A (en) * | 2015-06-02 | 2015-09-23 | 中国科学院上海高等研究院 | Method for preparing DD3R molecular sieve |
| CN106621858A (en) * | 2017-02-04 | 2017-05-10 | 耿逸豪 | High-yield synthetic method for DD3R molecular sieve film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109603896A (en) * | 2018-12-29 | 2019-04-12 | 韩旭霞 | A kind of purifying formaldehyde material |
| CN109603896B (en) * | 2018-12-29 | 2020-10-20 | 西安沃蓝环保科技有限公司 | Formaldehyde purification material |
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