CN106669613A - Amino porous carbon dioxide adsorbent and preparation method thereof - Google Patents
Amino porous carbon dioxide adsorbent and preparation method thereof Download PDFInfo
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- CN106669613A CN106669613A CN201710035372.1A CN201710035372A CN106669613A CN 106669613 A CN106669613 A CN 106669613A CN 201710035372 A CN201710035372 A CN 201710035372A CN 106669613 A CN106669613 A CN 106669613A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
- B01J20/02—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
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2258/00—Sources of waste gases
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- B01D2258/0283—Flue gases
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Abstract
The invention relates to an amino porous carbon dioxide adsorbent and a preparation method thereof. The amino porous carbon dioxide adsorbent is an amino functional material which is obtained by impregnating and modifying synthesized ZSM-5 zeolite by using tetraethylenepentamine. The preparation method comprises the following steps: mixing and stirring tetraethoxysilane, aluminum isopropoxide, tetrapropylammonium hydroxide, sodium chloride and deionized water in proportion; putting a mixed liquid in an oven to remove alcohols; then putting the mixed liquid without alcohols in a polytetrafluoroethylene reaction kettle, and performing crystallization, washing, filtration and drying to obtain ZSM-5 zeolite; mixing and stirring the ZSM-5 zeolite with an ethanol solution of tetraethylenepentamine in a mass ratio; and finally, fully drying the mixed liquid to obtain the amino porous carbon dioxide adsorbent. According to the amino porous carbon dioxide adsorbent and the preparation method thereof, the adsorbent is high in adsorption efficiency and good in selective adsorbability in a range of 60-80 DEG C.
Description
Technical field
The present invention relates to environmental technology field, more particularly to a kind of amino porous silica carbon adsorbent and its preparation side
Method.
Background technology
Carbon dioxide is a kind of main greenhouse gases in air, with developing rapidly for World Economics, its industry row
High-volume increase year by year.In current commercial production, energy resource consumption based on fossil-fueled, especially in boiler coal burning,
Great amount of carbon dioxide is discharged in air by flue.In order to mitigation of global climate such as warms at the series of environmental problems, it is right to need
Carbon dioxide in industrial smoke is separated and captured, to reach the purpose for reducing greenhouse gas emission.
At present in industrial smoke is separated in numerous technologies of carbon dioxide, absorption and separation method and adsorption method of separation more into
It is ripe.It is to use amine-based solvents that absorption and separation method is most common, such as monoethanolamine, diethanolamine, methyl diethanolamine and diisopropyl
Hydramine, the method needs substantial amounts of energy expenditure, and the easy etching apparatus of amine-based solvents for using.Adsorption method of separation is most universal
Be that, using conventional physical absorbent, such as activated carbon and zeolite adsorption, its technology more energy-conservation, and it is rotten to effectively prevent equipment
Erosion problem.Zeolite has high affinity to polar molecule (such as carbon dioxide), therefore zeolite is considered as more suitable absorption
The solid absorbent of carbon dioxide.But for the characteristics of industrial smoke temperature is higher and carbon dioxide partial pressure is relatively low, its is intrinsic
Pore structure and the property of physical absorption can not meet the application under the industrial environment.
Therefore, need badly invention one kind can at a temperature of industrial smoke, still with stronger absorption property, and have compared with
The carbon dioxide absorber of high carbon dioxide Selective adsorption.
ZSM-5 types zeolite has thinner hole wall, more rich pore structure.Amino is introduced in ZSM-5 type zeolites can be with
Its absorption property at relatively high temperatures is improved, and improves its carbon dioxide Selective adsorption.
The content of the invention
(1) technical problem to be solved
In order to solve the problems referred to above of prior art, the present invention provides one kind can be at a temperature of industrial smoke, with height
Adsorption efficiency and the amino porous silica carbon adsorbent compared with high carbon dioxide Selective adsorption and preparation method thereof, it is existing to solve
There is the carbon dioxide absorber of technology in the low problem of this temperature range internal adsorption efficiency.
(2) technical scheme
In order to achieve the above object, the main technical schemes that the present invention is adopted include：
The present invention provides a kind of amino porous silica carbon adsorbent, and the amino porous silica carbon adsorbent is to use four
The amine of ethylene five carries out impregnating the resulting amino functional adsorbing material that is modified to the ZSM-5 types zeolite for synthesizing.
According to the present invention, dipping is carried out to the ZSM-5 types zeolite for synthesizing using the ethanol solution of TEPA modified.
According to the present invention, amino porous silica carbon adsorbent in -80 DEG C of absorption of temperature 60 C, in 100 DEG C -120 of temperature
DEG C desorption and regeneration.
The present invention provides a kind of preparation method of amino porous silica carbon adsorbent, specifically includes following steps：
S1：ZSM-5 types zeolite is mixed with the ethanol solution of TEPA by certain mass ratio, 0.5-3 hours are stirred；
S2：Mixed liquor obtained in S1 is put in baking oven, after being fully dried amino porous silica carbon adsorbent is obtained.
It is further comprising the steps of before S1 according to the present invention：
S11：Tetraethyl orthosilicate, aluminum isopropylate., TPAOH, Sodium Chloride and deionized water are fully mixed in proportion
Close, be stirred at room temperature；
S12：Mixed liquor obtained in S11 is put in baking oven to be carried out except alcohol；
S13：The mixed liquor of S12 is put in ptfe autoclave, the crystallization at 165 DEG C, then cyclic washing, mistake
Filter and obtain ZSM-5 type zeolites after being dried.
According to the present invention, the ZSM-5 types zeolite in S1 is 1 with the mass ratio of TEPA：0.3-0.9.
According to the present invention, the temperature of baking oven is 40-80 DEG C in S2.
According to the present invention, the tetraethyl orthosilicate, aluminum isopropylate., TPAOH, Sodium Chloride and deionized water in S11
Mol ratio be 25-1000：1：9：1：300-600；The time stirred in S11 is 6-24 hours.
According to the present invention, except the temperature of alcohol is 60-80 DEG C in S12, the time is 1-4 hours.
According to the present invention, the time of crystallization is 12-72 hours in S13.
(3) beneficial effect
The invention has the beneficial effects as follows：
, used as the modified material of the amino functional of ZSM-5 type zeolites, low cost, toxicity are low, titanium dioxide for TEPA
Carbon adsorption ability height, the amino of its higher density and the property of less viscosity, there is provided more reactions for being used to interact
Site.
The amino porous silica carbon adsorbent of the present invention, has given full play to the pore structure system advantage of ZSM-5 type zeolites,
Improve to the adsorption efficiency and Selective adsorption of carbon dioxide in the range of 60 DEG C -80 DEG C its amino functional is modified,
Also, the adsorbent, in 100 DEG C of -120 DEG C of desorption and regenerations, regenerative process energy consumption is little, and regenerability is good.
The preparation method of the amino porous silica carbon adsorbent of the present invention, cost of material is low, simple for process, made
The amino porous silica carbon adsorbent for obtaining is stronger to carbon dioxide adsorption ability in the range of 60 DEG C -80 DEG C, this temperature range
For the exhaust gas temperature scope of the flue gas Jing after sulfur removal technology of coal-burning boiler, therefore without the need for carry out cooling process to flue gas, reduce
The cost of decarbonation appliance transformation.
Description of the drawings
Fig. 1 is the curve of adsorption kinetics of ZT5 in the embodiment of the present invention one；
Fig. 2 is the curve of adsorption kinetics of ZT7 in the embodiment of the present invention two；
Fig. 3 is X-ray diffraction analysis (XRD) spectrogram of the ZT5 in the embodiment of the present invention and ZT7；
Fig. 4 is FTIR spectrum analysis (FT-IR) spectrogram of the ZT5 in the embodiment of the present invention and ZT7.
Specific embodiment
In order to preferably explain the present invention, in order to understand, below in conjunction with the accompanying drawings, by specific embodiment, to this
It is bright to be described in detail.
It is in molar ratio by tetraethoxysilance, aluminum isopropylate., TPAOH, Sodium Chloride and deionized water first
25-1000：1：9：1：300-600 is sufficiently mixed, and after 6-24 hours are stirred at room temperature, are put in 60 DEG C -80 DEG C of baking oven and remove
Alcohol 1-4 hours.Then the mixed liquor is put in ptfe autoclave, the crystallization 12-72 hour at 165 DEG C, then instead
After backwashing is washed, and filters and obtain after being dried pressed powder, i.e. ZSM-5 types zeolite.Again by ZSM-5 types zeolite and the second of TEPA
0.5-3 hours are stirred after alcoholic solution mixing, ZSM-5 types zeolite is 1 with the mass ratio of TEPA：0.3-0.9.Finally incite somebody to action
To mixed liquor be put in the baking oven that temperature is 40 DEG C -80 DEG C, required adsorbent is obtained after being fully dried.
Further, amino porous silica carbon adsorbent of the invention can be not only used for the absorption of carbon dioxide in gas
Separate, it is also possible to as the adsorbent of other wide range of areas, such as to pollutant such as heavy metal ion in liquid and dyestuffs
Absorption, but by contrast, it is more preferable for the adsorbing separation effect of the carbon dioxide in gas.
Further, amino porous silica carbon adsorbent of the invention can be carried out to carbon dioxide below 100 DEG C
Adsorbing separation, but present invention specifically aims in coal-burning boiler the absorption of the carbon dioxide of flue gas there is more preferable effect, fire
Exhaust gas temperature scope of the flue gas in coal burning boiler Jing after sulfur removal technology is 60 DEG C -80 DEG C or so, is drawn through experiment, of the invention
Adsorption effect of the amino porous silica carbon adsorbent when temperature is 60 DEG C -80 DEG C is best.
Further, amino porous silica carbon adsorbent of the invention desorption and regeneration, regenerative process at 100 DEG C -120 DEG C
Energy consumption is little, and regenerability is good.
Embodiment one
First by the tetraethoxysilance of 26.04g, the aluminum isopropylate. of 1.02g, 36.61g TPAOH
(25wt% aqueous solutions) and 0.29g Sodium Chloride are sufficiently mixed, and after being stirred at room temperature 12 hours, are put in 80 DEG C of baking oven and remove alcohol
2 hours.Then the mixed liquor is put in ptfe autoclave, crystallization 24 hours at 165 DEG C, then cyclic washing,
Filter and obtain ZSM-5 type zeolites after being dried.After again obtained ZSM-5 types zeolite is mixed with the ethanol solution of TEPA
Stirring 1 hour, ZSM-5 types zeolite is 1 with the mass ratio of TEPA：0.5.Finally the mixed liquor for obtaining is put into into temperature is
In 80 DEG C of baking oven, required adsorbent is obtained after being fully dried.Determine in the ratio of above-mentioned ZSM-5 types zeolite and TEPA
The entitled ZT5 of the justice adsorbent.
Embodiment two
First by the tetraethoxysilance of 104.16g, the aluminum isopropylate. of 1.02g, 36.61g TPAOH
(25wt% aqueous solutions) and 0.29g Sodium Chloride are sufficiently mixed, and after being stirred at room temperature 24 hours, are put in 60 DEG C of baking oven and remove alcohol
4 hours.Then the mixed liquor is put in ptfe autoclave, crystallization 72 hours at 165 DEG C, then cyclic washing,
Filter and obtain ZSM-5 type zeolites after being dried.1 is stirred after again ZSM-5 types zeolite is mixed with the ethanol solution of TEPA
Hour, ZSM-5 types zeolite is 1 with the mass ratio of TEPA：0.7.Finally the mixed liquor for obtaining is put into into temperature for 50 DEG C
Baking oven in, required adsorbent is obtained after being fully dried.Should in the ratio definition of above-mentioned ZSM-5 types zeolite and TEPA
The entitled ZT7 of adsorbent.
The curve of adsorption kinetics of Fig. 1 is obtained by thermogravimetric analyzer measurement.Flow is first passed through in instrument for 30ml/min
Argon, and the ZT5 obtained in embodiment one be heated to into 100 DEG C continue 1 hour to carry out pretreatment.Then ZT5 is cooled down
To certain measurement temperature, the carbon dioxide that flow is 30ml/min is passed through.As carbon dioxide is adsorbed by ZT5,
The quality of ZT5 can increase with the time.Some time inscribes, and the quality that ZT5 increases is its carbon dioxide adsorption, thus obtains Fig. 1
Curve of adsorption kinetics.
The curve of adsorption kinetics of Fig. 2 is obtained by thermogravimetric analyzer measurement.Flow is first passed through in instrument for 30ml/min
Argon, and the ZT7 obtained in embodiment two be heated to into 100 DEG C continue 1 hour to carry out pretreatment.Then ZT7 is cooled down
To certain measurement temperature, the carbon dioxide that flow is 30ml/min is passed through.As carbon dioxide is adsorbed by ZT7,
The quality of ZT7 can increase with the time.Some time inscribes, and the quality that ZT7 increases is its carbon dioxide adsorption, thus obtains Fig. 2
Curve of adsorption kinetics.
With reference to Fig. 1, Fig. 2, it is mutually synthermal under conditions of, the carbon dioxide adsorption of ZT7 is bigger than ZT5；For same reality
Apply carbon dioxide absorber obtained in example, the absorption of the adsorbance of higher temperature carbon dioxide than lower temperature carbon dioxide
Amount is big；ZT5 and ZT7 be all when the time being about 0min-5min, the growth rate of carbon dioxide adsorption quickly, afterwards two
Carbonoxide adsorbance increasess slowly.
With reference to Fig. 3, wherein, abscissa 2-Theta-Scale refers to the angle of diffraction, and vertical coordinate intensity refers to diffraction maximum
Intensity.By Fig. 3 findings, 2 θ=7.9,8.9,23.3,24.0,4.5 is the characteristic peak of ZSM-5 type zeolites, illustrates the zeolite quilt
The modified still crystal structure with ZSM-5 type zeolites of dipping.
With reference to Fig. 4, wherein, abscissa wavenumber refers to wave number, represents the position of absworption peak, vertical coordinate
Transmission refers to transmitance, represents absorption intensity.By Fig. 4 findings, wave number is 2933cm-1, 2814cm-1, 1563cm-1
And 1470cm-1Vibrations peak be modified by TEPA with obtained carbon dioxide absorber it is relevant.Wherein wave number is 2933cm-1And 2814cm-1The flexible vibrations peak at place is due to there is CH2CH2CH2-NH2C-H in group2, and be 1563cm in wave number-1
And 1470cm-1The vibrations peak at place be due to primary amine group (RNH2) in N-H2It is related.
To sum up, amino porous silica carbon adsorbent of the invention, has given full play to the pore structure system of ZSM-5 type zeolites
Advantage, inhales in the modified adsorption efficiency that improve in the range of 60 DEG C -80 DEG C to carbon dioxide of its amino functional and selection
Attached property, also, the adsorbent, in 100 DEG C of -120 DEG C of desorption and regenerations, regenerative process energy consumption is little, and regenerability is good；The ammonia of the present invention
The preparation method of Quito hole carbon dioxide absorber, cost of material is low, simple for process, obtained amino porous silica
Carbon adsorbent is stronger to carbon dioxide adsorption ability in the range of 60 DEG C -80 DEG C, and this temperature range is the flue gas Jing of coal-burning boiler
Exhaust gas temperature scope after sulfur removal technology, therefore without the need for carrying out cooling process to flue gas, reduce the cost of decarbonation appliance transformation.
It is to be appreciated that the description for carrying out to the specific embodiment of the present invention above is simply to illustrate that the skill of the present invention
Art route and feature, its object is to allow those skilled in the art will appreciate that present disclosure and implement according to this, but
The present invention is not limited to above-mentioned particular implementation.Every various change made within the scope of the claims is repaiied
Decorations, all should cover within the scope of the present invention.
Claims (10)
1. a kind of amino porous silica carbon adsorbent, it is characterised in that：
The amino porous silica carbon adsorbent is to carry out dipping to the ZSM-5 types zeolite for synthesizing using TEPA to be modified
Resulting amino functional adsorbing material.
2. amino porous silica carbon adsorbent as claimed in claim 1, it is characterised in that：
Dipping is carried out to the ZSM-5 types zeolite of the synthesis using the ethanol solution of the TEPA modified.
3. amino porous silica carbon adsorbent as claimed in claim 1, it is characterised in that：
The amino porous silica carbon adsorbent adsorbs for -80 DEG C in temperature 60 C, in 100 DEG C of -120 DEG C of desorption and regenerations of temperature.
4. a kind of preparation method of amino porous silica carbon adsorbent, it is characterised in that specifically include following steps：
S1：ZSM-5 types zeolite is mixed with the ethanol solution of TEPA by certain mass ratio, 0.5-3 hours are stirred；
S2：Mixed liquor obtained in the S1 is put in baking oven, after being fully dried the amino porous silica carbon adsorption is obtained
Agent.
5. the preparation method of amino porous silica carbon adsorbent as claimed in claim 4, it is characterised in that the S1 it
Before, it is further comprising the steps of：
S11：Tetraethyl orthosilicate, aluminum isopropylate., TPAOH, Sodium Chloride and deionized water are sufficiently mixed in proportion,
It is stirred at room temperature；
S12：Mixed liquor obtained in the S11 is put in baking oven to be carried out except alcohol；
S13：The mixed liquor of the S12 is put in ptfe autoclave, the crystallization at 165 DEG C, then cyclic washing, mistake
Filter and obtain ZSM-5 type zeolites after being dried.
6. the preparation method of amino porous silica carbon adsorbent as claimed in claim 4, it is characterised in that：
ZSM-5 types zeolite in the S1 is 1 with the mass ratio of TEPA：0.3-0.9.
7. the preparation method of amino porous silica carbon adsorbent as claimed in claim 4, it is characterised in that：
Oven temperature in the S2 is 40-80 DEG C.
8. the preparation method of amino porous silica carbon adsorbent as claimed in claim 5, it is characterised in that：
The mol ratio of tetraethyl orthosilicate, aluminum isopropylate., TPAOH, Sodium Chloride and deionized water in the S11 is
25-1000：1：9：1：300-600；
The time stirred in the S11 is 6-24 hours.
9. the preparation method of amino porous silica carbon adsorbent as claimed in claim 5, it is characterised in that：
Except the temperature of alcohol is 60-80 DEG C in the S12, the time is 1-4 hours.
10. the preparation method of amino porous silica carbon adsorbent as claimed in claim 5, it is characterised in that：
The time of crystallization is 12-72 hours in the S13.
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Cited By (5)
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| CN109046258A (en) * | 2018-09-05 | 2018-12-21 | 陕西凯蓝环保科技有限公司 | A kind of molecular screen material and preparation method thereof of efficient absorption ambient carbon dioxide |
| CN111808678A (en) * | 2020-08-04 | 2020-10-23 | 大连工业大学 | Method for separating monoglyceride and diglyceride in edible oil based on mesoporous adsorbent |
| CN113198422A (en) * | 2021-04-19 | 2021-08-03 | 长安大学 | Amino-functionalized halloysite porous microsphere-based gas adsorption material, and preparation method and application thereof |
| CN113426410A (en) * | 2021-06-16 | 2021-09-24 | 珠海格力电器股份有限公司 | Porous carbon material and preparation method thereof |
| CN113731353A (en) * | 2021-08-03 | 2021-12-03 | 哈尔滨工业大学（深圳） | Carbon absorption material and synthesis method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046258A (en) * | 2018-09-05 | 2018-12-21 | 陕西凯蓝环保科技有限公司 | A kind of molecular screen material and preparation method thereof of efficient absorption ambient carbon dioxide |
| CN111808678A (en) * | 2020-08-04 | 2020-10-23 | 大连工业大学 | Method for separating monoglyceride and diglyceride in edible oil based on mesoporous adsorbent |
| CN111808678B (en) * | 2020-08-04 | 2022-06-24 | 大连工业大学 | Method for separating monoglyceride and diglyceride in edible oil based on mesoporous adsorbent |
| CN113198422A (en) * | 2021-04-19 | 2021-08-03 | 长安大学 | Amino-functionalized halloysite porous microsphere-based gas adsorption material, and preparation method and application thereof |
| CN113426410A (en) * | 2021-06-16 | 2021-09-24 | 珠海格力电器股份有限公司 | Porous carbon material and preparation method thereof |
| CN113731353A (en) * | 2021-08-03 | 2021-12-03 | 哈尔滨工业大学（深圳） | Carbon absorption material and synthesis method thereof |
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