CN107344092A - A kind of preparation method of high temperature resistant type calcium-based ascarite - Google Patents
A kind of preparation method of high temperature resistant type calcium-based ascarite Download PDFInfo
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- CN107344092A CN107344092A CN201710803909.4A CN201710803909A CN107344092A CN 107344092 A CN107344092 A CN 107344092A CN 201710803909 A CN201710803909 A CN 201710803909A CN 107344092 A CN107344092 A CN 107344092A
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- 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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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of high temperature resistant type calcium-based ascarite, belong to absorbent preparing technical field.The present invention prepares calcium base matrix powder by using citrate sol gel method, ionization occurs in aqueous by citric acid because citric acid belongs to Multiple Weak Acid, multiple ionization will occur in aqueous, then complex reaction occurs with molybdenum ion again, form the absorbent containing molybdenum ion, deposited again by molybdenum disulfide to absorbent powder surface, absorbent powder is coated, absorbent powder is effectively improved because the problem of hole blocks occurs under hot environment, effective solid absorbent pore passage structure, reduce the problem of duct expansion occurs because of high temperature and caves in for material, it is chemically bonded by the molybdenum ion of molybdenum disulfide and calcium-base absorbing agent material internal, improve covering property of the clad to absorbing material, so as to improve the resistance to elevated temperatures of calcium base carbon dioxide absorbing material.
Description
Technical field
The invention discloses a kind of preparation method of high temperature resistant type calcium-based ascarite, belongs to absorbent and prepares skill
Art field.
Background technology
Calcium-base absorbing agent is one of method of absorbing carbon dioxide under conventional hot environment.Utilize calcium oxide and titanium dioxide
The reaction of carbon and its back reaction, to absorb referred to as Cyclic Calcination/carbonation, by Cyclic Calcination/carbonation to two
Carbonoxide carries out cyclic absorption.Calcium-base absorbing agent is preferable with the reaction selectivity of carbon dioxide in the range of 600~700 DEG C, tool
There is higher absorptivity, and absorbent is easy to regenerate.
Calcium-base absorbing agent mainly has the advantage that：（1）The separation that directly can be realized at relatively high temperatures, reclaims what is obtained
Carbon dioxide purity is high；Absorbent is easy to regenerate, when temperature reaches 750~850 DEG C calcium carbonate can decompose to obtain calcium oxide with
Carbon dioxide, make absorbent regeneration that there is larger absorptive capacity；
（2）With preferable mechanical stability；
（3）Rich reserves, it is cheap, be easy to get, be easy to mass produce.
But calcium-base absorbing agent there is also some disadvantageously：One be in system, with the increase of cycle-index,
On the other hand it is the flue gas particularly contained for the industrial waste gas of complexity that carbonate treatment rate, which gradually reduces, calcium-base absorbing agent is present
Selective problems.And high-temperature calcination adsorbent can cause the sintering between CaO particles, cause the decline of adsorbent surface product and hole
Gap rate is drastically reduced, and the adsorbent being sintered is more difficult to be decomposed into CaO, and surface state also changes, and also results in absorption
The conversion ratio of agent declines, and influences its CO2Adsorption capacity.So the research to Ca-base adsorbent at present, it is still and seeks one kind and follow
The preferable adsorbent of ring stability, and repeat and recycle after high-temperature calcination, seek preferably to be adapted to what is recycled
Low-cost high-temperature adsorbent is that existing necessity improved to Ca-base adsorbent promotes measure.
The content of the invention
Present invention mainly solves technical problem：Adsorbent surface can be caused for existing Ca-base adsorbent high-temperature calcination
Product declines and porosity is drastically reduced, and surface state also changes, and the conversion ratio for also resulting in absorbent declines, and influences it
CO2A kind of adsorption capacity problem, there is provided preparation method of high temperature resistant type calcium-based ascarite.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Count in parts by weight, weigh 45~50 parts of deionized waters, 10~15 parts of calcium nitrate, 3~5 parts of nitric acid molybdenum stirrings respectively
Mixing, obtains mixed liquor, in mass ratio 1:5, citric acid is added in mixed liquor, simultaneously heating water bath is stirred, obtains coagulant liquid；
（2）By coagulant liquid rotary evaporated to dryness, obtain desiccant gel and be placed in Muffle furnace, after calcination processing, heating is heated and protected
Temperature calcining, standing are cooled to room temperature, ball milling sieve, obtain matrix calcium-base absorbing agent powder；
（3）Matrix calcium-base absorbing agent powder is placed in mould, compressing calcium-base absorbing agent cake, in mass ratio 1:5, will
Calcium-base absorbing agent cake is together positioned in quartz ampoule with molybdenum disulfide, and sealed silica envelope simultaneously vacuumizes；
（4）After heating heating, stopping vacuumizes and to being passed through argon gas in quartz ampoule, and insulation, which is calcined and stood, is cooled to room temperature, will
Calcined material washing, dry and stand and be cooled to room temperature, milled 1 sieve, you can be prepared into a kind of high temperature resistant type calcium base carbon dioxide
Absorbent.
2. a kind of preparation method of high temperature resistant type calcium-based ascarite according to claim 1, its feature
It is：Step（2）Described coagulant liquid rotating evaporation temperature is 75~80 DEG C.
3. a kind of preparation method of high temperature resistant type calcium-based ascarite according to claim 1, its feature
It is：Step（2）Described calcination processing temperature is 350~450 DEG C.
4. a kind of preparation method of high temperature resistant type calcium-based ascarite according to claim 1, its feature
It is：Step（3）Described compressing pressure is 6~8MPa.
5. a kind of preparation method of high temperature resistant type calcium-based ascarite according to claim 1, its feature
It is：Step（4）The described argon gas speed that is passed through is 25~40cm3/min。
The beneficial effects of the invention are as follows：
The present invention prepares calcium base matrix powder by using citrate Sol-Gel method, is sent out in aqueous by citric acid
Raw ionization will occur multiple ionization, be then complexed again with molybdenum ion in aqueous because citric acid belongs to Multiple Weak Acid
Reaction, forms the absorbent containing molybdenum ion, then is deposited by molybdenum disulfide to absorbent powder surface, and absorbent powder is entered
Row cladding, absorbent powder is effectively improved because the problem of hole blocks occurs under hot environment, effectively solid absorbent duct knot
Structure, the problem of duct expansion occurs because of high temperature and caves in for material is reduced, passes through molybdenum disulfide and calcium-base absorbing agent material internal
Molybdenum ion be chemically bonded, improve clad to the covering property of absorbing material, absorbed so as to improve calcium base carbon dioxide
The resistance to elevated temperatures of material.
Embodiment
Count in parts by weight, weigh 45~50 parts of deionized waters, 10~15 parts of calcium nitrate, 3~5 parts of nitric acid molybdenum stirrings respectively
Mixing, obtains mixed liquor, in mass ratio 1:5, citric acid is added in mixed liquor, is stirred and is placed in water-bath at 45~55 DEG C
Heat 15~20min, collect coagulant liquid is placed in rotary evaporated to dryness at 75~80 DEG C, collect desiccant gel and be placed in Muffle
In stove, 1~2h of calcination processing at 350~450 DEG C, 750~850 DEG C then are warming up to by 5 DEG C/min, 3~5h of insulation calcining
Afterwards, stand and be cooled to room temperature, ball milling crosses 200 mesh sieves, obtains matrix calcium-base absorbing agent powder；Matrix calcium-base absorbing agent powder is placed in
In mould, a diameter of 1.5cm is pressed under 6~8MPa, thickness is 0.2cm calcium-base absorbing agent cake；In mass ratio 1:5,
Calcium-base absorbing agent cake and molybdenum disulfide are together positioned in quartz ampoule, sealed silica envelope is simultaneously evacuated to 3~5Pa, heating
450~550 DEG C are heated to, stopping vacuumizes and to being passed through argon gas in quartz ampoule, and it is 25~40cm to control argon gas flow velocity3/ min,
After 25~30min of insulation calcining, after standing is cooled to room temperature, stopping is passed through argon gas, and modified calcium-base absorbing agent cake is used
Deionized water rinsing 3~5 times, then 6~8h is dried at 85~90 DEG C, standing is cooled to room temperature, mills and crosses 100 mesh sieves, i.e.,
A kind of high temperature resistant type calcium-based ascarite can be prepared into.
Example 1
Count in parts by weight, weigh 45 parts of deionized waters, 10 parts of calcium nitrate, 3 parts of nitric acid molybdenums respectively and be stirred, obtain mixed liquor,
In mass ratio 1:5, citric acid is added in mixed liquor, is stirred and is placed in heating water bath 15min at 45 DEG C, collecting to coagulate
Glue is placed in rotary evaporated to dryness at 75 DEG C, collects desiccant gel and is placed in Muffle furnace, the calcination processing 1h at 350 DEG C,
750 DEG C, after 3h is calcined in insulation then are warming up to by 5 DEG C/min, standing is cooled to room temperature, and ball milling crosses 200 mesh sieves, obtains matrix calcium base
Absorbent powder；Matrix calcium-base absorbing agent powder is placed in mould, a diameter of 1.5cm is pressed under 6MPa, thickness is
0.2cm calcium-base absorbing agent cake；In mass ratio 1:5, calcium-base absorbing agent cake and molybdenum disulfide are together positioned over quartz ampoule
In, sealed silica envelope is simultaneously evacuated to 3Pa, and heating is heated to 450 DEG C, and stopping vacuumizes and to being passed through argon gas in quartz ampoule, controls
Argon gas flow velocity processed is 25cm3After/min, insulation calcining 25min, after standing is cooled to room temperature, stopping is passed through argon gas, will be modified
Calcium-base absorbing agent cake deionized water rinsing 3 times, then 6h is dried at 85 DEG C, standing is cooled to room temperature, mills and crosses 100
Mesh sieve, you can be prepared into a kind of high temperature resistant type calcium-based ascarite.
Example 2
Count in parts by weight, weigh 47 parts of deionized waters, 12 parts of calcium nitrate, 4 parts of nitric acid molybdenums respectively and be stirred, obtain mixed liquor,
In mass ratio 1:5, citric acid is added in mixed liquor, is stirred and is placed in heating water bath 17min at 50 DEG C, collecting to coagulate
Glue is placed in rotary evaporated to dryness at 77 DEG C, collects desiccant gel and is placed in Muffle furnace, the calcination processing 2h at 400 DEG C,
800 DEG C, after 4h is calcined in insulation then are warming up to by 5 DEG C/min, standing is cooled to room temperature, and ball milling crosses 200 mesh sieves, obtains matrix calcium base
Absorbent powder；Matrix calcium-base absorbing agent powder is placed in mould, a diameter of 1.5cm is pressed under 7MPa, thickness is
0.2cm calcium-base absorbing agent cake；In mass ratio 1:5, calcium-base absorbing agent cake and molybdenum disulfide are together positioned over quartz ampoule
In, sealed silica envelope is simultaneously evacuated to 4Pa, and heating is heated to 500 DEG C, and stopping vacuumizes and to being passed through argon gas in quartz ampoule, controls
Argon gas flow velocity processed is 32cm3After/min, insulation calcining 27min, after standing is cooled to room temperature, stopping is passed through argon gas, will be modified
Calcium-base absorbing agent cake deionized water rinsing 4 times, then 7h is dried at 87 DEG C, standing is cooled to room temperature, mills and crosses 100
Mesh sieve, you can be prepared into a kind of high temperature resistant type calcium-based ascarite.
Example 3
Count in parts by weight, weigh 50 parts of deionized waters, 15 parts of calcium nitrate, 5 parts of nitric acid molybdenums respectively and be stirred, obtain mixed liquor,
In mass ratio 1:5, citric acid is added in mixed liquor, is stirred and is placed in heating water bath 20min at 55 DEG C, collecting to coagulate
Glue is placed in rotary evaporated to dryness at 80 DEG C, collects desiccant gel and is placed in Muffle furnace, the calcination processing 2h at 450 DEG C,
850 DEG C, after 5h is calcined in insulation then are warming up to by 5 DEG C/min, standing is cooled to room temperature, and ball milling crosses 200 mesh sieves, obtains matrix calcium base
Absorbent powder；Matrix calcium-base absorbing agent powder is placed in mould, a diameter of 1.5cm is pressed under 8MPa, thickness is
0.2cm calcium-base absorbing agent cake；In mass ratio 1:5, calcium-base absorbing agent cake and molybdenum disulfide are together positioned over quartz ampoule
In, sealed silica envelope is simultaneously evacuated to 5Pa, and heating is heated to 550 DEG C, and stopping vacuumizes and to being passed through argon gas in quartz ampoule, controls
Argon gas flow velocity processed is 40cm3After/min, insulation calcining 30min, after standing is cooled to room temperature, stopping is passed through argon gas, will be modified
Calcium-base absorbing agent cake deionized water rinsing 5 times, then 8h is dried at 90 DEG C, standing is cooled to room temperature, mills and crosses 100
Mesh sieve, you can be prepared into a kind of high temperature resistant type calcium-based ascarite.
Detection method：Static Adsorption detects
（1）Weigh the quality of cupel, record data m0；
（2）Unmodified calcium based raw material is in cupel after weighing 0.5g 1#, 2#, 3# sample and calcining, record data m1；
（3）Cupel equipped with sample is put into tube furnace, opens carbon dioxide gas bottle valve, adjusts rotor stream
Gauge, adjust to 50mL/min, gas flow is in stable state；
（4）Tube furnace power supply is opened, setting heating schedule is：15 DEG C/min, 700 DEG C of constant temperature 40min；
（5）Tube furnace power supply is closed, is cooled to 200 DEG C, taking-up is put into drier and is cooled to room temperature, weighs the quality of cupel, remembers
Record data are m2。
Example 1,2,3 and control group prepared by the present invention（The matrix absorbent powder of uncoated modification）Contrasted,
Performance comparison is as shown in table 1
The performance table of comparisons of table 1
As seen from the above table, the carbon dioxide absorber for preparing of the present invention can high temperature resistant be recycled for multiple times, and adsorption rate substantially carries
It is high.
Claims (5)
1. a kind of preparation method of high temperature resistant type calcium-based ascarite, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, weigh 45~50 parts of deionized waters, 10~15 parts of calcium nitrate, 3~5 parts of nitric acid molybdenum stirrings respectively
Mixing, obtains mixed liquor, in mass ratio 1:5, citric acid is added in mixed liquor, simultaneously heating water bath is stirred, obtains coagulant liquid；
（2）By coagulant liquid rotary evaporated to dryness, obtain desiccant gel and be placed in Muffle furnace, after calcination processing, heating is heated and protected
Temperature calcining, standing are cooled to room temperature, ball milling sieve, obtain matrix calcium-base absorbing agent powder；
（3）Matrix calcium-base absorbing agent powder is placed in mould, compressing calcium-base absorbing agent cake, in mass ratio 1:5, will
Calcium-base absorbing agent cake is together positioned in quartz ampoule with molybdenum disulfide, and sealed silica envelope simultaneously vacuumizes；
（4）After heating heating, stopping vacuumizes and to being passed through argon gas in quartz ampoule, and insulation, which is calcined and stood, is cooled to room temperature, will
Calcined material washing, dry and stand and be cooled to room temperature, milled 1 sieve, you can be prepared into a kind of high temperature resistant type calcium base carbon dioxide
Absorbent.
A kind of 2. preparation method of high temperature resistant type calcium-based ascarite according to claim 1, it is characterised in that：
Step（2）Described coagulant liquid rotating evaporation temperature is 75~80 DEG C.
A kind of 3. preparation method of high temperature resistant type calcium-based ascarite according to claim 1, it is characterised in that：
Step（2）Described calcination processing temperature is 350~450 DEG C.
A kind of 4. preparation method of high temperature resistant type calcium-based ascarite according to claim 1, it is characterised in that：
Step（3）Described compressing pressure is 6~8MPa.
A kind of 5. preparation method of high temperature resistant type calcium-based ascarite according to claim 1, it is characterised in that：
Step（4）The described argon gas speed that is passed through is 25~40cm3/min。
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Cited By (4)
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| CN108607512A (en) * | 2018-04-04 | 2018-10-02 | 大连理工大学 | The method of the sulfide modified MOF materials of molybdenum base |
| CN108704627A (en) * | 2018-05-07 | 2018-10-26 | 湖南城市学院 | A kind of CO absorption2Solid material TSCD-Zr preparation and method of modifying |
| CN109179372A (en) * | 2018-10-26 | 2019-01-11 | 华南理工大学 | A kind of high-performance biology cellulose carbon aerogels and its preparation method and application |
| CN110124644A (en) * | 2019-04-12 | 2019-08-16 | 华中科技大学 | A kind of multicomponent collaboration enhanced Ca-base adsorbent and preparation method thereof |
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| CN109179372A (en) * | 2018-10-26 | 2019-01-11 | 华南理工大学 | A kind of high-performance biology cellulose carbon aerogels and its preparation method and application |
| CN109179372B (en) * | 2018-10-26 | 2020-07-28 | 华南理工大学 | High-performance biological cellulose carbon aerogel and preparation method and application thereof |
| CN110124644A (en) * | 2019-04-12 | 2019-08-16 | 华中科技大学 | A kind of multicomponent collaboration enhanced Ca-base adsorbent and preparation method thereof |
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Application publication date: 20171114 |