CN106552609A - Carbon dioxide absorber and its preparation method based on layer stephanoporate silicon dioxide block - Google Patents
Carbon dioxide absorber and its preparation method based on layer stephanoporate silicon dioxide block Download PDFInfo
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- CN106552609A CN106552609A CN201611107188.5A CN201611107188A CN106552609A CN 106552609 A CN106552609 A CN 106552609A CN 201611107188 A CN201611107188 A CN 201611107188A CN 106552609 A CN106552609 A CN 106552609A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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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- 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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention discloses a kind of preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block, comprises the following steps：Triblock copolymer P123 is dissolved in hydrochloric acid solution, then sequentially adds 1,3,5 trimethylbenzenes, methyl silicate, expoxy propane；Gained colloidal sol Jing gels, drying, be warming up to 400～800 DEG C and be incubated 5 ± 0.5h, obtain layer stephanoporate silicon dioxide block；Layer stephanoporate silicon dioxide block is put into into organic amine methanol solution, so that organic amine uniform load is in layer stephanoporate block；Gains are placed in baking oven and are dried, and obtain the carbon dioxide absorber based on layer stephanoporate silicon dioxide block.The present invention further simultaneously discloses the carbon dioxide absorber based on layer stephanoporate silicon dioxide block being prepared using said method.
Description
Technical field
The present invention relates to field of material technology, and in particular to a kind of carbon dioxide based on layer stephanoporate silicon dioxide block
Adsorbent and preparation method.
Background technology
In recent years, the increasingly increase of greenhouse gases exacerbates global warming, and brings arid, flood, sea level
A series of Climatic issues such as rising, so as to have a strong impact on the living environment of the ecological balance and human future of the earth.Dioxy
It is the predominant gas for causing greenhouse effect to change carbon, while being also a kind of potential carbon resource, therefore reduces greenhouse gases titanium dioxide
The discharge of carbon, environmental protection become one of current whole world key problem to be solved.In the capture technique of carbon dioxide, catch
Obtain the height that material directly affects capture cost.
Conventional carbon dioxide capture material mainly has lyosoption, seperation film and solid absorbent etc. at present.Using
Most capture materials is amine solvent, and the advantage of this capture material is that adsorption capacity is high, selectivity is good, but amine solvent has
Renewable high energy consumption, have the shortcomings that to equipment that corrosivity are strong and also in being only applicable to or low concentration carbon dioxide absorption.Cause
This in recent years solid absorbent receive extensive concern.
Conventional solid absorbent mainly includes that activated carbon, molecular sieve, metal-oxide, salt and amino modified are more
Porous materials etc..As disclosed in CN105797678A " compound middle temperature carbon dioxide absorber and preparation method thereof ", there is provided one
The method that magnalium type hydrotalcite composite material carrys out absorbing carbon dioxide is planted, existing middle temperature carbon dioxide absorber absorption effect is solved
The low problem of rate；" a kind of carbon dioxide absorber and preparation method based on ordered mesopore carbon " disclosed in CN105289530A,
Carbon dioxide absorber is prepared by material modification of ordered mesopore carbon, preferable adsorption effect is obtained.
But existing adsorbent be used mostly be single aperture micropore or mesoporous material, and material shape mostly is powder
End or thin film, relatively difficult using rear recycling, the stratum that the foramen magnum-mesoporous-micropore of rising in recent years is distributed simultaneously is more
Porous materials not only improve mass transfer and are conducive to absorption again, but rarely have based on layer stephanoporate block materials absorbing carbon dioxide at present
Relevant report, therefore, develop it is significant based on this Novel carbon dioxide adsorbent.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of carbon dioxide based on layer stephanoporate silicon dioxide block and inhales
Attached dose and preparation method, the method synthesize layer stephanoporate silicon dioxide block by sol-gel process, and by infusion process to which
Carry out organic amine to support.
In order to solve above-mentioned technical problem, the present invention provides a kind of carbon dioxide based on layer stephanoporate silicon dioxide block
The preparation method of adsorbent, comprises the following steps：
1), weigh the hydrochloric acid solution that 5.0～9.8g triblock copolymer P123s are placed in 25～30ml (preferably 28.8ml)
In, stir under condition of ice bath to triblock copolymer P123 and be completely dissolved (mixing time about 3～6 hours)；
2), the 1，3，5-trimethyl-benzene of 2～6ml is added (be slowly added dropwise, time for adding is 30 ± 5 minutes) to step 1)
In solution, 1～3 hour under condition of ice bath, is sufficiently stirred for；
3), 10～14ml (preferably 12ml) methyl silicate is added to step 2) in solution, under condition of ice bath fully
Stirring 1～3 hour, obtains solution (clear solution)；
4), 3.2～6.4ml expoxy propane is added (be slowly added dropwise, time for adding is 30 ± 5 minutes) to step 3) obtained by
In solution, under condition of ice bath, 2～5min is sufficiently stirred for, obtains colloidal sol (vitreosol)；
5), by step 4) obtained by colloidal sol be placed in 12～48 hours in 40 ± 5 DEG C of baking ovens, obtain gel (translucent gels)；
6), by step 5) obtained by gel be placed in 60 ± 5 DEG C of baking ovens be dried 2～5 days (purpose is to make moisture evaporating completely),
Obtain block (white block)；
7), by step 6) obtained by block be warming up to 400～800 DEG C and be incubated 5 ± 0.5h, after being cooled to room temperature, obtain rank
Layer porous silica silicon bulk；
8), organic amine is added in methanol (absolute methanol), is stirred to organic amine and is completely dissolved, obtain organic amine methanol molten
Liquid；
9), by step 7) obtained by layer stephanoporate silicon dioxide block be put into step 8) obtained by organic amine methanol it is molten
Liquid, stirs 2～4h (preferably 3h) in 40 ± 5 DEG C (water-bath)；So that organic amine uniform load is in layer stephanoporate block；
Organic amine in organic amine methanol solution is 0.43～4 with the mass ratio of layer stephanoporate silicon dioxide block：1 (compared with
Good is 0.67～1.5:1)；
10), by step 9) gains be placed in 80 ± 10 DEG C of baking ovens be dried 1～2 day, obtain based on layer stephanoporate dioxy
The carbon dioxide absorber (that is, the modified layer stephanoporate silicon dioxide block of organic amine) of SiClx block.
As the improvement of the preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block of the present invention：
The step 8) in organic amine be polyethyleneimine, TEPA, at least one in pentaethylene hexamine it is (that is, a kind of or several
Kind).
Enter one as the preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block of the present invention
Step is improved：The step 1) in hydrochloric acid solution concentration be 0.001molL-1～0.1molL-1.Above-mentioned concentration is, for example,
0.001mol·L-1、0.01mol·L-1、0.1mol·L-1。
Enter one as the preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block of the present invention
Step is improved：The step 7) in, by step 6) block be put into Muffle furnace in atmosphere with 2 DEG C of min-1Speed be warming up to
400～800 DEG C, and 5 ± 0.5h is incubated, furnace cooling, obtains layer stephanoporate silicon dioxide block afterwards.
The present invention further simultaneously discloses based on layer stephanoporate silicon dioxide block two be prepared using said method
Oxidation carbon adsorbent.
The preparation method of the present invention is as shown in Figure 1.
In the present invention, triblock copolymer P123, full name are poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three
Block copolymer, its molecular formula are PEO-PPO-PEO.
The carbon dioxide absorber based on layer stephanoporate silicon dioxide block being prepared using the inventive method is (i.e.,
The carbon dioxide absorber of organic amine is supported based on layer stephanoporate silicon dioxide block), structure be foramen magnum-mesoporous-micropore simultaneously
The layer stephanoporate silicon dioxide of distribution, is shaped as blocks of solid, and which is good to carbon dioxide adsorption and circular regeneration performance, reclaims again
Raw convenient, which can be used for the carbon dioxide adsorption higher than room temperature.That is, which is good to carbon dioxide adsorption and circular regeneration performance.
The present invention has following technical advantage：Compared with same type adsorbent, it is proposed that a kind of to be based on layer stephanoporate dioxy
The preparation method of the carbon dioxide absorber of SiClx block, the development for adsorbent provide new approaches；Product has good
Heat stability, can be used for the carbon dioxide adsorption higher than room temperature；The carbon dioxide adsorption and circular regeneration performance of new adsorbent
Well, required experiment condition and experimental cost are low, preparation technology environmental protection.
Description of the drawings
Below in conjunction with the accompanying drawings the specific embodiment of the present invention is described in further detail.
Fig. 1 is a kind of preparation flow figure of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block.
Fig. 2 is 5000 times of stereoscan photograph of layer stephanoporate silicon dioxide of the synthesis of embodiment 1.
Fig. 3 is 50000 times of stereoscan photograph of layer stephanoporate silicon dioxide of the synthesis of embodiment 1.
Fig. 4 is the adsorption capacity change of 8 adsorption/desorption cyclic processes of adsorbent prepared by embodiment 4.
Fig. 5 is thermogravimetric analysiss (TG) result figure；
In Fig. 5, a:Embodiment 2；b:Embodiment 3；c:Embodiment 4.
Fig. 6 is the CO of embodiment 2, comparative example 1-1, comparative example 1-22Adsorption curve comparison diagram；
In Fig. 6, a:Embodiment 2；b:Comparative example 1-1；c:Comparative example 1-2.
Fig. 7 is the CO of embodiment 2, comparative example 2-1, comparative example 2-22Adsorption curve comparison diagram；
In Fig. 7, a:Embodiment 2；b:Comparative example 2-1；c:Comparative example 2-2.
Specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
Embodiment 1, a kind of preparation method of layer stephanoporate silicon dioxide block：
Weigh 7g P123 and be added to 0.01molL-1Hydrochloric acid solution 28.8ml in, under condition of ice bath, magnetic agitation 5 is little
When so that P123 is completely dissolved；The 1，3，5-trimethyl-benzene of (time for adding is 30 minutes) 4ml, ice bath bar are slowly added dropwise afterwards
3 hours are sufficiently stirred under part；Add and under 12ml methyl silicates, condition of ice bath, be sufficiently stirred for 3 hours；Then it is slowly added dropwise again
(time for adding is 30 minutes) 5.5ml expoxy propane, is sufficiently stirred for 5min under condition of ice bath, obtains colloidal sol (vitreosol)；Will
Colloidal sol is placed in 36 hours in 40 ± 5 DEG C of baking ovens, and resulting gel (translucent gels) is placed in 60 ± 5 DEG C of baking ovens and is dried 4 days
Resulting block (white block) is put into Muffle furnace in atmosphere with 2 DEG C of min by (purpose is to make moisture evaporating completely)-1
Speed be warming up to 550 DEG C, and be incubated 5h, after cooling to room temperature with the furnace afterwards, obtain layer stephanoporate silicon dioxide block.
Embodiment 2, a kind of preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block：
Weigh 5.72g PEI (polyethyleneimine) be dissolved in methanol 15ml in be configured to PEI solution, add 8.58g to implement
Layer stephanoporate silicon dioxide block obtained by example 1, stirs 3h under 40 ± 5 DEG C of water bath conditions, be placed in afterwards in baking oven be dried (80 ±
In 10 DEG C of baking ovens be dried 2 days), obtain the layer stephanoporate silicon dioxide block that PEI load capacity is 40%, i.e., as product based on
The carbon dioxide absorber of layer stephanoporate silicon dioxide block.After testing, the product has good carbon dioxide adsorption and follows
Ring performance.
Embodiment 3, a kind of preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block：
Weigh 6.54g PEI be dissolved in methanol 15ml in be configured to PEI solution, add the rank obtained by 6.54g embodiments 1
Layer porous silica silicon bulk, stirs 3h under 40 ± 5 DEG C of water bath conditions, is placed in baking oven afterwards and is dried (in 80 ± 10 DEG C of baking ovens
It is dried 2 days), the layer stephanoporate silicon dioxide block that PEI load capacity is 50% is obtained, i.e., as product based on layer stephanoporate two
The carbon dioxide absorber of silicon oxide block.After testing, product has good carbon dioxide adsorption and cycle performance.
Embodiment 4, a kind of preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block
Weigh 8.52g PEI be dissolved in methanol 15ml in be configured to PEI solution, add the stratum in 5.68g embodiments 1
Porous silica silicon bulk, stirs 3h under 40 ± 5 DEG C of water bath conditions, is placed in baking oven afterwards to be dried and (is done in 80 ± 10 DEG C of baking ovens
Dry 2 days), the layer stephanoporate silicon dioxide block that PEI load capacity is 60% is obtained, i.e., as product based on layer stephanoporate dioxy
The carbon dioxide absorber of SiClx block.After testing, product has good carbon dioxide adsorption and cycle performance.
Test one, thermogravimetric analysiss (TG) are carried out to the product obtained by 2～embodiment of embodiment 4, as a result as shown in Figure 5.
Product be can be seen that from TG curves a little mass loss near 100 DEG C, and this adsorbs in being mainly product
Caused by water volatilization, to 200 DEG C of almost no mass losses after this, the big mass loss near 200 DEG C is mainly by PEI point
Caused by solution, therefore, understand that product has good heat stability within 200 DEG C from curve.
Experiment two, carbon dioxide adsorption：
CO2Absorption property is measured by DTG (TG), is comprised the following steps that：
1st, preprocessing process：Take 10mg or so samples, all the time 50ml/min high pure nitrogen purging atmosphere in, with 5 DEG C/
The programming rate of min is increased to 110 DEG C from room temperature, then keeps constant temperature 60min, with deviate from adsorbent duct remaining water and
Air plankton；
2nd, 75 DEG C of the adsorption temp specified is cooled to the speed of 5 DEG C/min, and constant temperature 30min makes it stable；
3rd, adsorption process：High pure nitrogen is converted into into high-purity CO2, with high-purity CO of 70ml/min2Air-flow is adsorbed, and is inhaled
The attached time is 200min；
4th, desorption process：Switch to high-purity N2, flow is still 50ml/min, is warming up to 110 DEG C with the speed of 5 DEG C/min,
Constant temperature 50min is desorbed；
5th, repeat experiment 8 times, test its cycle performance；
6th, the CO in sample2Adsorption capacity is calculated according to the measurement result of TG.
The adsorption capacity of 8 adsorption/desorption cyclic processes of adsorbent prepared by embodiment 4 changes as described in Figure 4.
Comparative example 1-1, the weight of the PEI in embodiment 2 is made into 1.43g by 5.72g, i.e. organic amine and layer stephanoporate
The mass ratio of silicon dioxide block is 0.16：1；Remaining is equal to embodiment 2.
Comparative example 1-2, the weight of the PEI in embodiment 2 is made into 34.3g by 5.72g, i.e. organic amine and layer stephanoporate
The mass ratio of silicon dioxide block is 5：1；Remaining is equal to embodiment 2.
The CO of above-described embodiment 2, comparative example 1-1, comparative example 1-22Adsorption curve is contrasted as shown in fig. 6, from the curve of Fig. 6
In can look, the absorption property of embodiment 2 is best.
Comparative example 2-1, by the concentration of hydrochloric acid in embodiment 1 by " 0.01molL-1" make " 0.001molL into-1", its
Remaining same embodiment 1.With the layer stephanoporate silicon dioxide block obtained by this scheme as 2 methods described of embodiment carries out carbon dioxide
The preparation of adsorbent.
Comparative example 2-2, by the 0.01molL in embodiment 1-1Hydrochloric acid make water into, remaining is with embodiment 1.With this scheme
The layer stephanoporate silicon dioxide block of gained carries out the preparation of carbon dioxide absorber such as 2 methods described of embodiment.
The CO of above-described embodiment 2, comparative example 2-1, comparative example 2-22Adsorption curve is contrasted as shown in fig. 7, from the curve of Fig. 7
In can look, the absorption property of embodiment 2 is best.
Comparative example 3-1, make the PEI in embodiment 2 into TEPAs, weight is constant；Remaining is equal to embodiment 2.
Comparative example 3-2, make the PEI in embodiment 2 into pentaethylene hexamines, weight is constant；Remaining is equal to embodiment 2.
On the premise of adsorption time is 200min；The adsorbance of 2 products obtained therefrom of embodiment is 1.84mmol/g, is contrasted
The adsorbance of example 3-1 products obtained therefroms is 1.65mmol/g, and the adsorbance of comparative example 3-1 products obtained therefrom is 1.60mmol/g.
Finally, in addition it is also necessary to it is noted that listed above is only several specific embodiments of the invention.Obviously, this
It is bright to be not limited to above example, there can also be many deformations.One of ordinary skill in the art can be from present disclosure
The all deformations directly derived or associate, are considered as protection scope of the present invention.
Claims (5)
1. based on layer stephanoporate silicon dioxide block carbon dioxide absorber preparation method, it is characterised in that：Including following
Step：
1) 5.0～9.8g triblock copolymer P123s, are weighed to be placed in the hydrochloric acid solution of 25～30ml, is stirred under condition of ice bath
It is completely dissolved to triblock copolymer P123；
2), the 1，3，5-trimethyl-benzene of 2～6ml is added to step 1) in solution, under condition of ice bath, it is sufficiently stirred for 1～3 hour；
3), 10～14ml methyl silicates are added to step 2) in solution, it is sufficiently stirred under condition of ice bath 1～3 hour, obtains
Solution；
4), 3.2～6.4ml expoxy propane is added to step 3) in resulting solution, under condition of ice bath, 2～5min is sufficiently stirred for,
Obtain colloidal sol；
5), by step 4) obtained by colloidal sol be placed in 12～48 hours in 40 ± 5 DEG C of baking ovens, obtain gel；
6), by step 5) obtained by gel be placed in 60 ± 5 DEG C of baking ovens be dried 2～5 days, obtain block；
7), by step 6) obtained by block be warming up to 400～800 DEG C and be incubated 5 ± 0.5h, after being cooled to room temperature, obtain stratum many
Hole silicon dioxide block；
8), organic amine is added in methanol, is stirred to organic amine and is completely dissolved, obtain organic amine methanol solution；
9), by step 7) obtained by layer stephanoporate silicon dioxide block be put into step 8) obtained by organic amine methanol solution, in
40 ± 5 DEG C of 2～4h of stirring；So that organic amine uniform load is in layer stephanoporate block；
Organic amine in organic amine methanol solution is 0.43～4 with the mass ratio of layer stephanoporate silicon dioxide block：1；
10), by step 9) gains be placed in 80 ± 10 DEG C of baking ovens be dried 1～2 day, obtain based on layer stephanoporate silicon dioxide
The carbon dioxide absorber of block.
2. the preparation method of the carbon dioxide absorber based on layer stephanoporate silicon dioxide block according to claim 1,
It is characterized in that：The step 8) in organic amine be polyethyleneimine, TEPA, at least one in pentaethylene hexamine.
3. according to claim 2 based on layer stephanoporate silicon dioxide block carbon dioxide absorber preparation method, its
It is characterised by：The step 1) in hydrochloric acid solution concentration be 0.001molL-1～0.1molL-1。
4. according to Claims 2 or 3 based on layer stephanoporate silicon dioxide block carbon dioxide absorber preparation method,
It is characterized in that：
The step 7) in, by step 6) block be put into Muffle furnace in atmosphere with 2 DEG C of min-1Speed be warming up to 400～
800 DEG C, and 5 ± 0.5h is incubated, furnace cooling, obtains layer stephanoporate silicon dioxide block afterwards.
5. the dioxy based on layer stephanoporate silicon dioxide block being prepared using such as the arbitrary methods described of Claims 1 to 4
Change carbon adsorbent.
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| CN109569517A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | A kind of preparation method of solid amine absorber |
| CN110075812A (en) * | 2019-05-17 | 2019-08-02 | 上海大学 | A kind of preparation method and application of amination silica dioxide granule adsorbent |
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| CN110591609A (en) * | 2019-09-29 | 2019-12-20 | 陈炳均 | Preparation method of washable coating adhesive |
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| CN107827116A (en) * | 2017-12-15 | 2018-03-23 | 江苏泛亚微透科技股份有限公司 | A kind of preparation method of porous silica silicon bulk aeroge |
| CN110075812A (en) * | 2019-05-17 | 2019-08-02 | 上海大学 | A kind of preparation method and application of amination silica dioxide granule adsorbent |
| CN110075812B (en) * | 2019-05-17 | 2022-02-25 | 上海大学 | Preparation method and application of silicon dioxide particle adsorbent |
| CN110548495A (en) * | 2019-08-29 | 2019-12-10 | 宁波诺丁汉新材料研究院有限公司 | Preparation method of adsorbent for capturing post-combustion carbon and adsorbent |
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