CN107744716B - The hollow compound CO of shell-type carbide slag2Absorbent and its synthetic method and application - Google Patents
The hollow compound CO of shell-type carbide slag2Absorbent and its synthetic method and application Download PDFInfo
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- CN107744716B CN107744716B CN201711130483.7A CN201711130483A CN107744716B CN 107744716 B CN107744716 B CN 107744716B CN 201711130483 A CN201711130483 A CN 201711130483A CN 107744716 B CN107744716 B CN 107744716B
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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
- B01D53/14—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 absorption
- B01D53/1456—Removing acid components
- B01D53/1475—Removing carbon dioxide
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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
- B01D53/14—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 absorption
- B01D53/1493—Selection of liquid materials for use as absorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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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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Abstract
The invention discloses a kind of hollow compound CO of shell-type carbide slag2Absorbent and its synthetic method and application, synthetic method include the following steps: that 1) carbide slag and cement are added in glucose solution, mix laggard horizontal high voltage hydro-thermal reaction；2) it by after the mixture washing drying after reaction, is pyrolyzed；3) product after pyrolysis is calcined at 400-800 DEG C, is ground after calcining up to CO2Absorbent.It can prepare that size is controllable, porous using the hydrothermal carbonization reaction of glucose in the present invention, the compound CO of carbide slag with hollow shell structure2Absorbent is conducive to CO2It is spread inside absorbent, improves the absorption CO of carbide slag2Performance.Use cement as the carrier in composite absorber, cement is reacted with carbide slag generates the Ca with high anti-sintering property12Al14O33, facilitate the stabilization of hollow shell skeleton, improve carbide slag cyclic absorption CO2Stability.
Description
Technical field
The present invention relates to a kind of hollow compound CO of shell-type carbide slag2Absorbent and its synthetic method and application, belong to dioxy
Change carbon control and emission reduction field.
Background technique
Calcium-base absorbing agent Cyclic Calcination/carbonating traps CO2Technology (also known as calcium circulating technology), because of its absorbent source
Extensively, at low cost, the extensive concern of the advantages by domestic and foreign scholars such as can couple with industries such as hydrogen manufacturing and cement.Calcium-base absorbing agent exists
Calcining and decomposing obtains CaO and CO in calcination reactor2, the CaO that calcines from calcination reactor enter carbonation reactor with
CO2Reaction, reaches and separates CO from flue gas2Purpose；React the CaCO generated3Calcining generates again in into calcination reactor
CaO is so recycled, while supplementing fresh calcium-base absorbing agent, discharge inactivation calcium-base absorbing agent and ash to calcination reactor.But
It is that calcium-base absorbing agent Cyclic Calcination/carbonating traps CO2In the process, the CO of absorbent2Performance is trapped with the increasing of cycle-index
Add and declines.Guaranteeing power plant CO2Under conditions of arresting efficiency is constant, it is necessary to screen out the absorbent of inactivation in time and supplement newly
Absorbent increases the cost loss of power plant.Therefore, it improves calcium-base absorbing agent Cyclic Calcination/carbonating and traps CO2Performance is mesh
One of preceding technology urgent problem to be solved.
Carbide slag is the industrial waste generated when producing acetylene with calcium carbide aquation method, it is difficult to carry out recycling on a large scale
It utilizes.The carbide slag of accumulation causes destruction to ecological environment around.Carbide slag can be used in Cyclic Calcination/carbonation
Middle trapping CO2, large quantities of lime stone resource can have not only been saved in this way, but also can make full use of waste.But carbide slag traps CO2Performance with
Lime stone is similar, since it is sintered during circular response, the hole of calcined product CaO is made to be collapsed and be hindered
Plug, to inhibit CO2Diffusion, hinders the carbonation reaction with CaO, leads to CO2Uptake increases performance with cycle-index
It is gradually reduced.
Summary of the invention
By the way that the study found that calcium-base absorbing agent is in carbonation, there are a critical product layer thickness, when in CaO crystalline substance
Grain surface covers the CaCO of adequate thickness3When product layer, CO2It is restricted by product layer diffusion with reacting for CaO of inside,
And as CaO crystal grain merges and grows up, intercrystalline gap becomes smaller, and carbonation reaction is further limited.Therefore, theoretical
On, the efficient CO of carbide slag can be realized using beam system for core shell structure absorbent2Remove target.
For above-mentioned the technical problems existing in the prior art, the object of the present invention is to provide a kind of hollow shell-type carbide slags
Compound CO2Absorbent and its synthetic method and application, this method can prepare the core-shell type knot of carbide slag and cement carbon coated template
Structure, by removal carbon template obtain hole prosperity hollow shell type structure, thus be greatly improved carbide slag Cyclic Calcination/
CO in carbonation2Absorbent properties solve carbide slag and trap CO during utilization2The lower problem of performance.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
A kind of hollow compound CO of shell-type carbide slag2The synthetic method of absorbent, includes the following steps:
1) carbide slag and cement are added in glucose solution, mix laggard horizontal high voltage hydro-thermal reaction；
2) it by after the mixture washing drying after reaction, is pyrolyzed；
3) product after pyrolysis is calcined at 400-800 DEG C, is ground after calcining up to CO2Absorbent.
The synthetic method comprises the following processes: physical mixed → dehydration hydrothermal carbonization (high pressure hydro-thermal reaction) → hole of heating up slowly
Gap reinforces (pyrolytic reaction step) → burning decarburization (high-temperature calcinations step) → high-specific surface area core-shell structure and forms (high-temperature calcination
Step) reconstruct of → chemical reaction substance, inertia loads to form (high-temperature calcinations step).
Preferably, in step 1), the concentration of the glucose solution is 0.8-1.2mol/L.
It is further preferred that the amount ratio of carbide slag and glucose solution is that every gram of carbide slag is added to 11- in step 1)
In 13mL glucose solution.
It is further preferred that the additive amount of cement makes CO in step 1)2The mass fraction of CaO reaches in absorbent
90%.
Preferably, in step 1), mix step are as follows: 60 DEG C stirred in water bath 30 minutes.
Preferably, in step 1), the temperature of high pressure hydro-thermal reaction is 160-190 DEG C, and the time is 3-12 hours, and pressure is
0.3-0.5MPa.Further preferably, the temperature of high pressure hydro-thermal reaction is 180 DEG C, and the time is 6 hours.
Preferably, it in step 2), is successively washed using distilled water and dehydrated alcohol.
Preferably, in step 2), the pyrolysis carries out under inert gas protection, and the heating rate of pyrolysis is 2.5-
3.5℃/min。
Still more preferably, in step 2), the temperature of pyrolysis is 440-460 DEG C, and the time of pyrolysis is that 1.8-2.5 is small
When.
Preferably, in step 3), the time of calcining is 0.8-1.2 hours.
Preferably, in step 3), the temperature of calcining is 600 DEG C.
The hollow compound CO of shell-type carbide slag that above-mentioned synthetic method is prepared2Absorbent, main component be CaO and
Ca12Al14O33, the content of CaO is 90%, Ca12Al14O33Content be less than 20%.
Ca12Al14O33It is that cement reacts the product generated with carbide slag, does not absorb CO2, there is the anti-burning of very strong high temperature
The performance of knot can make the compound CO of hollow shell formula carbide slag2Absorbent keeps stablizing in Cyclic Calcination-carbonic acid salification cycles.
Preferably, the hollow compound CO of shell-type carbide slag2Absorbent is hollow porous structure.
The above-mentioned hollow compound CO of shell-type carbide slag2Absorbent is in CO2Application in absorption.
The invention has the benefit that
1, method of the invention is advantageously implemented the resource utilization and CO of carbide slag2The technique road that efficient removal combines
Line.
2, it is controllable, porous to prepare size for the hydrothermal carbonization reaction in the present invention using glucose, has hollow shell knot
The compound CO of the carbide slag of structure2Absorbent is conducive to CO2It is spread inside absorbent, improves the absorption CO of carbide slag2Performance.
3, use cement as the carrier in composite absorber, cement is reacted with carbide slag to be generated with high anti-agglutinatting property
The Ca of energy12Al14O33, facilitate the stabilization of hollow shell skeleton, improve carbide slag cyclic absorption CO2Stability.
4, entire technique is easily achieved, the hollow compound CO of shell-type carbide slag2Absorbent is in severe calcination condition (high temperature and height
Concentration C O2) under still have higher CO2Absorbability and reactivity stabilization, have good prospects for commercial application.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the hollow compound CO of shell-type carbide slag of the invention2Absorbent preparation flow schematic diagram.
Fig. 2 is the hollow compound CO of shell-type carbide slag of the invention2X-ray diffraction (XRD) map of absorbent.
Fig. 3 is the hollow compound CO of shell-type carbide slag of the invention2Electronic scanner microscope (SEM) figure of absorbent: (a)
After hydrothermal carbonization；(b) after calcining.
Fig. 4 is the hollow compound CO of shell-type carbide slag of the invention2The circulation CO of absorbent2(absorbent prepares item to uptake
Part: 5g carbide slag+0.15g cement+10.81g glucose+60mL distilled water (CaO content=90wt.%), hydrothermal carbonization temperature
180 DEG C, the hydrothermal carbonization time 6 hours, 450 DEG C of pyrolysis temperature, pyrolysis time 2 hours, calcination temperature was 600 DEG C, calcination time
It is 1 hour；Cyclic Calcination/carbonating experiment condition: carbonation time 20 minutes, 700 DEG C of carbonation temperature, carbonizing atmosphere
15%CO2/ 85%N2(volume fraction), calcination time 10 minutes, experiment carried out on double-fixed bed reactor).
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Embodiment 1
The hollow compound CO of shell-type carbide slag2The synthetic method of absorbent, includes the following steps:
(1) then room temperature lower-weighing 10.81g glucose is added in 60mL distilled water；
(2) 5g carbide slag and 0.15g cement are added in above-mentioned glucose solution, 60 DEG C of stirred in water bath 30 of constant temperature are divided
Clock obtains mixed liquor；
(3) above-mentioned gained mixed liquor pours into the high-pressure hydrothermal reaction kettle that volume is 100mL, the hydrothermal synthesis 6 at 180 DEG C
Hour；
(4) high-pressure hydrothermal reaction kettle after hydro-thermal reaction is cooled to room temperature, then by the mixture distilled water of taking-up
It is successively washed with dehydrated alcohol 3 times, it is dry；
(5) by dried sample in pure N2Heating (heating rate is 3 DEG C/min) under atmosphere, and 2 are pyrolyzed at 450 DEG C
Hour；
(6) sample being pyrolyzed is calcined 1 hour at 600 DEG C；
(7) calcined sample is ground into fine crushing, the as hollow compound CO of shell-type carbide slag2Absorbent.
Preparation process route such as Fig. 1 of the present invention, is briefly described as follows its principle: physical mixed → dehydration hydro-thermal carbon
Changing → slow heating hole is reinforced →, decarburization of burning → high-specific surface area core-shell structure formation → chemical reaction substance reconstruct, inertia are negative
It carries and is formed.As shown in Fig. 2, XRD analysis the result shows that, the hollow compound CO of shell-type carbide slag2The main component of absorbent be CaO and
Ca12Al14O33(diffraction maximum is stronger) has a small amount of Ca2Al2SiO7(diffraction maximum is weaker), Ca12Al14O33It is cement and carbide slag
The product generated is reacted, wherein Ca12Al14O33Do not absorb CO2, there is very strong high temperature anti-sintering property, in Cyclic Calcination/carbon
It keeps stablizing in salification cycles.Morphology analysis shows to become after the sample after hydration carbonization is calcined for solid bowl structure
For porous hollow shell type structure, effectively removing for internal carbon template is realized, as shown in Figure 3.
Performance test
On double-fixed bed reactor (including calcining furnace and carbonating furnace) to certain untreated carbide slag of acetylene gas factory and
The CO of carbide slag (preparation of embodiment 1) after processing2Absorbent properties are determined.It is laid in the 500mg carbide slag sample of porcelain boat
(two kinds of calcination conditions: (1) 850 DEG C of temperature, the pure N of atmosphere are calcined first in calcining furnace2, (mildly calcined item within the time 10 minutes
Part)；(2) 920 DEG C of temperature, atmosphere 70%CO2/ 30%N2, the 10 minutes time (severe calcination condition)), the sample after the completion of calcining
Into carbonating furnace, carbonation reaction is carried out in carbonating furnace, temperature is 700 DEG C, carbonizing atmosphere 15%CO2/ 85%
N2, the time 20 minutes.The porcelain boat of sample is filled in calcining furnace and carbonates reciprocation cycle in furnace, completes Cyclic Calcination/carbonating
Absorb CO2Experiment.Reaction gas high pressure gas cylinder provides, and high pressure gas cylinder exit gas is entered through pressure reducing valve by flowmeter control anti-
It answers in device.Quality after the calcining of carbide slag sample and carbonating uses electronic balance (precision 0.1mg) to weigh, and passes through carbonating
The CO of reaction front and back mass change unit of account absorbent2Uptake, as shown in formula (1).
In formula, CNFor the CO of unit mass absorption agent2Uptake, g/g；N is circular response number；m0It is initial for absorbent
Weight, g；mNFor absorbent quality after n-th circular response, g；mCal,NFor the calcined quality of n-th absorbent, g.
As shown in figure 4, experimental data shows compared with carbide slag, the hollow compound CO of shell-type carbide slag2The initial rank of absorbent
Section CO2Uptake is relatively low, C under mild calcination condition1For 0.44g/g, and carbide slag is then 0.58g/g.But hollow shell-type calcium carbide
The compound CO of slag2Absorbent cyclical stability is substantially better than carbide slag, after the 10th time recycles, the hollow compound CO of shell-type carbide slag2It inhales
Receive agent CO2Uptake substantially remains in 0.4g/g；The CO of carbide slag2Uptake increases decaying rapidly, 20 circulations with cycle-index
CO afterwards2Uptake drops to 0.24g/g.The hollow compound CO of shell-type carbide slag2Absorbent for carbide slag superiority severe
It is become apparent under calcination condition, C20It is 2 times of carbide slag under the same terms.Electricity.To the hollow compound CO of shell-type carbide slag2It inhales
It receives agent and calcining carbide slag carries out N2Adsorption analysis obtains their specific surface area and specific pore volume data, as a result such as 1 institute of table
Show.The hollow compound CO of shell-type carbide slag2Absorbent has hole abundant, and specific surface area and specific pore volume integral are not carbide slags
2.6 and 3.6 times.Therefore, the hollow compound CO of shell-type carbide slag2Why absorbent keeps higher CO2Absorbent properties and preferably circulation
Stability, be mainly attributed to its porous hollow shell structure, flourishing pore structure, high specific surface area and specific pore volume and
Ca12Al14O33The anti-sintering property of absorbent is improved as inert carrier.
The hollow compound CO of shell-type carbide slag of table 12The specific surface area and specific pore volume product of absorbent and calcining carbide slag
Embodiment 2
The hollow compound CO of shell-type carbide slag2The synthetic method of absorbent, includes the following steps:
(1) then room temperature lower-weighing 10g glucose is added in 60mL distilled water；
(2) 4.8g carbide slag and 0.15g cement are added in above-mentioned glucose solution, 60 DEG C of stirred in water bath 30 of constant temperature are divided
Clock obtains mixed liquor；
(3) above-mentioned gained mixed liquor pours into the high-pressure hydrothermal reaction kettle that volume is 100mL, the hydrothermal synthesis 6 at 170 DEG C
Hour；
(4) high-pressure hydrothermal reaction kettle after hydro-thermal reaction is cooled to room temperature, then by the mixture distilled water of taking-up
It is successively washed with dehydrated alcohol 3 times, it is dry；
(5) by dried sample in pure N2Heating (heating rate is 3 DEG C/min) under atmosphere, and 2 are pyrolyzed at 450 DEG C
Hour；
(6) sample being pyrolyzed is calcined 1 hour at 700 DEG C；
(7) calcined sample is ground into fine crushing, the as hollow compound CO of shell-type carbide slag2Absorbent.
Embodiment 3
The hollow compound CO of shell-type carbide slag2The synthetic method of absorbent, includes the following steps:
(1) then room temperature lower-weighing 11.35g glucose is added in 70mL distilled water；
(2) 5.5g carbide slag and 0.17g cement are added in above-mentioned glucose solution, 60 DEG C of stirred in water bath 30 of constant temperature are divided
Clock obtains mixed liquor；
(3) above-mentioned gained mixed liquor pours into the high-pressure hydrothermal reaction kettle that volume is 100mL, the hydrothermal synthesis 5 at 170 DEG C
Hour；
(4) high-pressure hydrothermal reaction kettle after hydro-thermal reaction is cooled to room temperature, then by the mixture distilled water of taking-up
It is successively washed with dehydrated alcohol 3 times, it is dry；
(5) by dried sample in pure N2Heating (heating rate is 3 DEG C/min) under atmosphere, and 2 are pyrolyzed at 460 DEG C
Hour；
(6) sample being pyrolyzed is calcined 1 hour at 700 DEG C；
(7) calcined sample is ground into fine crushing, the as hollow compound CO of shell-type carbide slag2Absorbent.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (11)
1. a kind of hollow compound CO of shell-type carbide slag2The synthetic method of absorbent, characterized by the following steps:
1) carbide slag and cement are added in glucose solution, mix laggard horizontal high voltage hydro-thermal reaction；
2) it by after the mixture washing drying after reaction, is pyrolyzed；
3) product after pyrolysis is calcined at 400-800 DEG C, is ground after calcining up to CO2Absorbent.
2. synthetic method according to claim 1, it is characterised in that: in step 1), the concentration of the glucose solution is
0.8-1.2mol/L；
The amount ratio of carbide slag and glucose solution is that every gram of carbide slag is added in 11-13mL glucose solution；
The additive amount of cement makes CO2The mass fraction of CaO reaches 90% in absorbent.
3. synthetic method according to claim 1, it is characterised in that: in step 1), mix step are as follows: in 60 DEG C of water-baths
Stirring 30 minutes.
4. synthetic method according to claim 1, it is characterised in that: in step 1), the temperature of high pressure hydro-thermal reaction is
160-190 DEG C, the time is 3-12 hours, pressure 0.3-0.5MPa.
5. synthetic method according to claim 4, it is characterised in that: in step 1), the temperature of high pressure hydro-thermal reaction is 180
DEG C, the time is 6 hours.
6. synthetic method according to claim 1, it is characterised in that: in step 2), using distilled water and dehydrated alcohol according to
Secondary washing.
7. synthetic method according to claim 1, it is characterised in that: in step 2), the pyrolysis is protected in inert gas
The lower progress of shield, the heating rate of pyrolysis is 2.5-3.5 DEG C/min；
The temperature of pyrolysis is 440-460 DEG C, and the time of pyrolysis is 1.8-2.5 hours.
8. synthetic method according to claim 1, it is characterised in that: in step 3), the time of calcining is that 0.8-1.2 is small
When, the temperature of calcining is 600 DEG C.
9. the hollow compound CO of shell-type carbide slag that any synthetic method of claim 1-8 is prepared2Absorbent, feature
Be: its main component is CaO and Ca12Al14O33, the content of CaO is 90%, Ca12Al14O33Content less than 20%.
10. the hollow compound CO of shell-type carbide slag according to claim 92Absorbent, it is characterised in that: it is hollow porous knot
Structure.
11. the hollow compound CO of shell-type carbide slag described in claim 102Absorbent is in CO2Application in absorption.
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| CN103936543A (en) * | 2014-04-08 | 2014-07-23 | 昆明理工大学 | Method for synchronously obtaining carbon dioxide absorbent along with production of acetylene |
| CN104759203A (en) * | 2015-03-17 | 2015-07-08 | 华能国际电力股份有限公司 | Fluidized bed technology and fluidized bed system for directly capturing CO2 in mineralized flue gas |
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