CN108654555A - A kind of preparation method of the positive silicic acid lithium material of absorbing carbon dioxide at high temperature - Google Patents
A kind of preparation method of the positive silicic acid lithium material of absorbing carbon dioxide at high temperature Download PDFInfo
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- CN108654555A CN108654555A CN201710205799.1A CN201710205799A CN108654555A CN 108654555 A CN108654555 A CN 108654555A CN 201710205799 A CN201710205799 A CN 201710205799A CN 108654555 A CN108654555 A CN 108654555A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/106—Silica or silicates
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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
Abstract
The invention discloses a kind of positive silicic acid lithium material (Li of absorbing carbon dioxide at high temperature4SiO4) preparation method it is as follows：Using Ludox as silicon source, using lithium hydroxide as lithium source, using carbonate as precipitating reagent, precipitation reaction being carried out in ammonia spirit, is filtered after reaction or evaporates water removal, then dry, roasting obtains positive lithium metasilicate sorbing material.The preparation method of positive silicic acid lithium adsorbent provided by the invention is simple for process, is easy to large-scale production, and obtained material purity is high, crystallinity and size tunable, and performance is high, and production cost is low.
Description
Technical field
The present invention relates to a kind of preparation methods of the positive silicic acid lithium material of absorbing carbon dioxide at high temperature.The material is for electricity
A large amount of high temperature carbon dioxide gases in the discharge gas such as factory are directly absorbed, and recycle carbon resource.
Background technology
Currently, world energy sources demand 80% is all provided by carbon-based fossil fuel, and CO in its caused air2Content increases
It is subject to and climate change causes the great attentions of countries in the world.However although improving the infrastructure construction of regenerative resource,
Fossil fuel is still the main energy sources in following longer one period.Therefore it is directed to during fossil fuel energy use, it is efficiently low
It is to be badly in need of for cost carbon dioxide capture and memory technology.CO2Can by various methods, such as membrane separation process, dry method and
Wet method is detached from high-temperature flue gas and exhaust gas and is further utilized, however these methods need to consume a large amount of energy.Therefore, mesh
Preceding key is to seek a kind of economic and practical sorbent material at high temperature, for recycling high temperature carbon dioxide.
Compared with other adsorbents, positive lithium metasilicate is as a kind of novel high temperature CO2Sorbing material is in prodigious temperature model
It encloses and CO2There is preferable CO in concentration2Absorption property, because its uptake is big, absorption rate is fast, good cycling stability, make its at
Most to there is the high-efficiency adsorbent of application prospect.
The synthetic method of positive lithium metasilicate has very much, and as solid phase method is relatively simple, but required reaction temperature is higher, raw material granularity
Unevenness causes to be difficult to mix, therefore high energy consumption, obtains that positive lithium metasilicate crystallite dimension is larger and easy-sintering, it is difficult to synthesize high-purity production
Object；Combustion method is hardly obtained pure single-phase positive lithium metasilicate, and impurities are mutually more；Reaction temperature needed for sol-gal process is low,
Sample particle is smaller, but still contains impurity phase.Yu Qingni, Zhao Chengjian, Wei Wei metal oxides purify the research of CO2 absorbents
[J] aerospace medicines and engineering in medicine, 2007,20 (6)：432-435. such as Miriam J.Venegas【Venegas M J,
The dynamics and reaction mechanism of the positive lithium metasilicate absorption carbon dioxide of the such as Fregoso-Israel E, Escamilla R：Grain size is imitated
Research [J] the industry answered is studied with engineering chemistry, 2007,46 (8)：2407-2412.】Etc. compared solid phase method and collosol and gel
Silicic acid lithium material prepared by method is to CO2The influence of absorbent properties.In order to preferably study Li4SiO4The absorption mechanism of sorbing material,
Some researchers are to Li4SiO4Sorbing material has carried out dynamic (dynamical) research.Such as Masahiro K【Masahiro K,
Novel lithium-containing oxides carbon dioxide absorber [J] the international applications ceramic technology magazines of the such as Kazuaki N, Kenji E,
2005,2 (6)：467-475.】Meet biexponential model etc. the absorption for having studied positive lithium metasilicate under hot conditions；Heriberto
Pfeiffer【Positive lithium metasilicate is to CO under Rodr í guezmosqueda R, Pfeiffer H. different gas flows and grain size2Absorption
Thermodynamic analysis [J] physical chemistry magazine A, 2010,114 (13)：4535-41.】Deng utilize Li2CO3And SiO2With solid phase method
The Li of synthesis4SiO4Sorbing material, and in different CO2Gas flow has made it dynamic (dynamical) research of Static Adsorption.
But in this field, it is not synthesis cost height to obtain positive lithium metasilicate adsorber technologies, is exactly that properties of product are poor, therefore such as
What low cost obtains high performance positive silicic acid lithium adsorbent, is the important technological problems of this field.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation of the low cost acquisition positive silicic acid lithium adsorbent of high-performance
Method.It is simple for process, be easy to large-scale production, obtained material purity is high, crystallinity and size tunable.
The positive silicic acid lithium material (Li of absorbing carbon dioxide at high temperature of the present invention4SiO4) preparation method it is as follows：It is with Ludox
Silicon source, using carbonate as precipitating reagent, precipitation reaction is carried out in ammonia spirit, was carried out after reaction using lithium hydroxide as lithium source
Filter or evaporation water removal, then dry, roasting obtain positive lithium metasilicate sorbing material.
In the method for the present invention, the Ludox with the concentration range of silica weight be 15%~35%, hydroxide
The molar ratio of lithium and Ludox is 4: 1~8: 1, and dry 8~14h of freeze-day with constant temperature at 80~120 DEG C obtains lithium metasilicate presoma,
Obtained precursor powder is roasted into 4~10h at 600~800 DEG C and synthesizes positive silicic acid lithium material.Dry atmosphere is air gas
The conditions such as atmosphere, nitrogen atmosphere, inert gas atmosphere or vacuum, calcination atmosphere are air atmosphere, nitrogen atmosphere, inert gas atmosphere
Or the conditions such as vacuum.Calcination temperature is preferably 600~700 DEG C, most preferably 620~680 DEG C, more preferably 640~660 DEG C.
In the method for the present invention, carbonate precipitating reagent derive from soluble carbonate salt, as sodium carbonate, sodium bicarbonate, potassium carbonate,
Saleratus, ammonium carbonate, ammonium hydrogen carbonate etc..
In the method for the present invention, the ammonium hydroxide of precipitation reaction system is (with NH3Meter) a concentration of 0.5~0.9mol/L.
In the method for the present invention, specific operation process is：First by LiOHH2O is dissolved in deionized water, is claimed by required proportioning
Ludox is taken, Ludox and precipitant solution are added in LiOH solution, reacted under stiring, required ammonia can be added
It in precipitant solution, can also be added in LiOH solution, reaction system can also be added during the reaction.The concentration pair of material
Reaction influences unobvious, is generally advisable with not influencing normally to stir.
Positive silicic acid lithium adsorbent prepared by the method for the present invention can be used for high temperature fluidized bed absorbing carbon dioxide technique, solve
The problem that sintering temperature existing for existing silicic acid lithium material is high and adsorption rate is low.Preparation method of the present invention is at low cost, and product uses
Performance is high, and process is simple, is easy to large-scale production, and obtained material purity is high, crystallinity and size tunable.The material is for electricity
The high temperature carbon dioxide gas for a large amount of high temperature carbon dioxides and the fossil fuel combustion process discharge discharged in factory, flue gas
It is directly absorbed, and recycles carbon resource, to play the role of alleviating greenhouse effects.Raw material of the present invention is cheap and easy to get, to go
Ionized water is medium, reduces the manufacturing cost of silicic acid lithium material；At the same time the lithium metasilicate particle synthesized is uniformly tiny, crystallization
Degree is good, phase free from foreign meter and has higher CO2Absorptivity is a kind of higher positive silicic acid lithium material of purity, is directly absorbed
CO2With energy saving, reduction CO2Discharge, to play the role of environmental protection.In the method for the present invention, in precipitation reaction system
Small molecule ammonia is introduced, keeps contact combination of the silica gel with lithium carbonate more full and uniform, is conducive to improve the purity of positive lithium metasilicate, knot
Brilliant degree and particle uniformity are conducive to the performance for improving product.
Description of the drawings
Fig. 1 is Li of the present invention4SiO4High temperature inhales carbon material under different calcination temperatures to CO2Adsorption-desorption cycle it is bent
Line.
Fig. 2 is the Li after 650 DEG C of roastings of the present invention4SiO4High temperature inhales isothermal adsorption of the carbon material under three different temperatures
Curve.
Specific implementation mode
The lithium metasilicate material C O that the present invention synthesizes2Absorbent properties test method is as follows：Positive silicic acid lithium material is placed in thermogravimetric
In analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample by room temperature to 800 DEG C, make adsorbent 400 DEG C~
800 DEG C of cycles carry out CO2Absorption-desorption, in addition by sample adsorption temp be 555~585 DEG C at constant temperature keep one section when
Between carry out CO2Absorbing reaction.
Below in conjunction with the accompanying drawings and the specific example substantive content that the present invention is further explained, these embodiments are merely to illustrate
The present invention rather than limit the scope of the invention.
Embodiment 1
Reaction raw materials are Ludox, lithium hydroxide and ammonium hydrogen carbonate, and positive lithium metasilicate is prepared using the precipitation method in ammonia solution
High-temperature adsorbing agent.By LiOHH2O is dissolved in deionized water, is that ammonium hydroxide is added in 0.7mol/L by ammonia density in reaction system, by n
(Li) raw material proportioning of/n (Si)=8.2: 1 weighs a certain amount of Ludox, at room temperature that Ludox and ammonium bicarbonate soln is same
When instill LiOH solution in, titration finish stirring 1h, be then evaporated, resulting material be placed in baking oven, in air atmosphere in
Freeze-day with constant temperature 12h obtains lithium metasilicate presoma at 100 DEG C, after the grinding uniformly of obtained precursor powder, is put into tube furnace, with
The heating rate of 5 DEG C/min is increased to 650 DEG C, keeps the temperature 6h, you can obtain positive silicic acid lithium material.
The silicic acid lithium material of synthesis is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample
800 DEG C are warming up to the rate of 5 DEG C/min by room temperature, then is cooled to 400 DEG C at the same rate, is then warming up to 800 DEG C again,
So cycle twice, makes adsorbent carry out CO within the scope of 400 DEG C~800 DEG C2Absorption-desorption reaction, Fig. 1, which can be seen that, to follow
CO is obtained after ring2Absorptive capacity be 18.76wt%.
Embodiment 2
Reaction raw materials are Ludox, lithium hydroxide and ammonium hydrogen carbonate, and positive lithium metasilicate is prepared using the precipitation method in ammonia solution
High-temperature adsorbing agent.By LiOHH2O is dissolved in deionized water, is that ammonium hydroxide is added in 0.5mol/L by ammonia density in reaction system, by n
(Li) raw material proportioning of/n (Si)=8.2: 1 weighs a certain amount of Ludox, at room temperature that Ludox and ammonium bicarbonate soln is same
When instill LiOH solution in, titration finish stirring 1h, be then evaporated, gained suspension be placed in baking oven, in air atmosphere
Freeze-day with constant temperature 12h obtains lithium metasilicate presoma at 100 DEG C, after the grinding uniformly of obtained precursor powder, is put into tube furnace,
700 DEG C are increased to the heating rate of 5 DEG C/min, keeps the temperature 6h, you can obtain positive silicic acid lithium material.
The silicic acid lithium material of synthesis is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample
800 DEG C are warming up to the rate of 5 DEG C/min by room temperature, then is cooled to 400 DEG C at the same rate, is then warming up to 800 DEG C again,
So cycle twice, makes adsorbent carry out CO within the scope of 400 DEG C~800 DEG C2Absorption-desorption reaction, Fig. 1, which can be seen that, to follow
CO is obtained after ring2Absorptive capacity be 14.84wt%.
Embodiment 3
Reaction raw materials are Ludox, lithium hydroxide and ammonium hydrogen carbonate, and positive lithium metasilicate is prepared using the precipitation method in ammonia solution
High-temperature adsorbing agent.By LiOHH2O is dissolved in deionized water, is that ammonium hydroxide is added in 0.7mol/L by ammonia density in reaction system, by n
(Li) raw material proportioning of/n (Si)=8.2: 1 weighs a certain amount of Ludox, at room temperature that Ludox and ammonium bicarbonate soln is same
When instill LiOH solution in, titration finish stirring 1h, be then evaporated, gained suspension be placed in baking oven, in air atmosphere
Freeze-day with constant temperature 12h obtains lithium metasilicate presoma at 100 DEG C, after the grinding uniformly of obtained precursor powder, is put into tube furnace,
750 DEG C are increased to the heating rate of 5 DEG C/min, keeps the temperature 6h, you can obtain positive silicic acid lithium material.
The silicic acid lithium material of synthesis is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample
800 DEG C are warming up to the rate of 5 DEG C/min by room temperature, then is cooled to 400 DEG C at the same rate, is then warming up to 800 DEG C again,
So cycle twice, makes adsorbent carry out CO within the scope of 400 DEG C~800 DEG C2Absorption-desorption reaction, Fig. 1, which can be seen that, to follow
CO is obtained after ring2Absorptive capacity be 9.81wt%.
Embodiment 4
Reaction raw materials are Ludox, lithium hydroxide and ammonium hydrogen carbonate, and positive lithium metasilicate is prepared using the precipitation method in ammonia solution
High-temperature adsorbing agent.By LiOHH2O is dissolved in deionized water, is that ammonium hydroxide is added in 0.9mol/L by ammonia density in reaction system, by n
(Li) raw material proportioning of/n (Si)=8.2: 1 weighs a certain amount of Ludox, at room temperature that Ludox and ammonium bicarbonate soln is same
When instill LiOH solution in, titration finish stirring 1h, be then evaporated, gained suspension be placed in baking oven, in air atmosphere
Freeze-day with constant temperature 12h obtains lithium metasilicate presoma at 100 DEG C, after the grinding uniformly of obtained precursor powder, is put into tube furnace,
800 DEG C are increased to the heating rate of 5 DEG C/min, keeps the temperature 6h, you can obtain positive silicic acid lithium material.
The silicic acid lithium material of synthesis is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample
800 DEG C are warming up to the rate of 5 DEG C/min by room temperature, then is cooled to 400 DEG C at the same rate, is then warming up to 800 DEG C again,
So cycle twice, makes adsorbent carry out CO within the scope of 400 DEG C~800 DEG C2Absorption-desorption reaction, Fig. 1, which can be seen that, to follow
CO is obtained after ring2Absorptive capacity be 7.94wt%.
Embodiment 5
As described in Example 1, reaction system is added in required ammonia during the reaction, other same as Example 1.
The silicic acid lithium material of synthesis is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample
800 DEG C are warming up to the rate of 5 DEG C/min by room temperature, CO2Balance Absorption capacity be 25.17wt%.
Embodiment 6
As described in Example 1, reaction raw materials ammonium hydrogen carbonate is changed to sodium bicarbonate, and required ammonia is dissolved in sodium bicarbonate
In solution, reaction product is dry after filtration washing, roasts, other same as Example 1.
The silicic acid lithium material of synthesis is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample
800 DEG C are warming up to the rate of 5 DEG C/min by room temperature, CO2Balance Absorption capacity be 22.43wt%.
Comparative example 1
As described in Example 6, reaction process does not introduce ammonia, other same as Example 6.
The silicic acid lithium material of synthesis is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios, by sample
800 DEG C are warming up to the rate of 5 DEG C/min by room temperature, CO2Balance Absorption capacity be 10.51wt%.
Embodiment 7
Positive silicic acid lithium material it can be seen from above example and Fig. 1 after 650 DEG C of roastings is to CO2With stronger suction
Attached property, therefore made further parsing to this using dynamic analysis under this calcination temperature.
The silicic acid lithium material that embodiment 1 synthesizes is placed in thermogravimetric analyzer, in CO2∶N2In the atmosphere of=1: 7 molar ratios,
555 DEG C are increased to from room temperature with the heating rate of 5 DEG C/min, and constant temperature is kept for a period of time at this temperature, detects it to two
The adsorption capacity of carbonoxide, Fig. 2 can be seen that reach absorption equilibrium after its absorptive capacity be 21.45wt%.
Embodiment 8
The silicic acid lithium material that embodiment 1 is synthesized is placed in thermogravimetric analyzer, in CO2∶N2The atmosphere of=1: 7 molar ratios
In, 565 DEG C are increased to from room temperature with the heating rate of 5 DEG C/min, and constant temperature is kept for a period of time at this temperature, and it is right to detect its
The adsorption capacity of carbon dioxide, Fig. 2 can be seen that reach absorption equilibrium after its absorptive capacity be 23.32wt%.
Embodiment 9
The silicic acid lithium material that embodiment 1 is synthesized is placed in thermogravimetric analyzer, in CO2∶N2The atmosphere of=1: 7 molar ratios
In, 585 DEG C are increased to from room temperature with the heating rate of 5 DEG C/min, and constant temperature is kept for a period of time at this temperature, and it is right to detect its
The adsorption capacity of carbon dioxide, Fig. 2 can be seen that reach absorption equilibrium after its absorptive capacity be 24.11wt%.
Claims (10)
1. a kind of preparation method of the positive silicic acid lithium material of absorbing carbon dioxide at high temperature, it is characterised in that：Using Ludox as silicon source,
Using lithium hydroxide as lithium source, using carbonate as precipitating reagent, precipitation reaction is carried out in ammonia spirit, is filtered or steams after reaction
Hair water removal, then dry, roasting obtain positive lithium metasilicate sorbing material.
2. preparation method according to claim 1, it is characterised in that：The Ludox is with the concentration of silica weight
Ranging from 15%~35%.
3. preparation method according to claim 1, it is characterised in that：The molar ratio of lithium hydroxide and Ludox is 4: 1~8
∶1。
4. preparation method according to claim 1, it is characterised in that：Dry 8~14h dry at 80~120 DEG C is obtained
Lithium metasilicate presoma.
5. preparation method according to claim 1, it is characterised in that：Roasting process is the precursor powder that will be dried to obtain
4~10h is roasted at 600~800 DEG C synthesizes positive silicic acid lithium material.
6. preparation method according to claim 1, it is characterised in that：Carbonate precipitating reagent derives from soluble carbonate salt.
7. preparation method according to claim 1, it is characterised in that：Carbonate precipitating reagent is from sodium carbonate, bicarbonate
Sodium, potassium carbonate, saleratus, ammonium carbonate or ammonium hydrogen carbonate.
8. preparation method according to claim 1, it is characterised in that：Precipitation reaction system is with NH3The ammonia concn of meter is
0.5~0.9mol/L.
9. preparation method according to claim 1, it is characterised in that：Precipitation reaction specific operation process is：First will
LiOH·H2O is dissolved in deionized water, weighs Ludox by required proportioning, LiOH solution is added in Ludox and precipitant solution
In, it is reacted under stiring.
10. preparation method according to claim 9, it is characterised in that：Ammonia needed for reaction is added in precipitant solution, or
It is added in LiOH solution, or reaction system is added during the reaction.
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