CN105664841B - High temperature CO2Sorbing material Li4SiO4Hydration and calcinations method of modifying - Google Patents
High temperature CO2Sorbing material Li4SiO4Hydration and calcinations method of modifying Download PDFInfo
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- CN105664841B CN105664841B CN201610024991.6A CN201610024991A CN105664841B CN 105664841 B CN105664841 B CN 105664841B CN 201610024991 A CN201610024991 A CN 201610024991A CN 105664841 B CN105664841 B CN 105664841B
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- 238000001354 calcination Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 20
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052912 lithium silicate Inorganic materials 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 16
- 229910052909 inorganic silicate Inorganic materials 0.000 claims abstract description 15
- 238000006703 hydration reaction Methods 0.000 claims abstract description 11
- 230000036571 hydration Effects 0.000 claims abstract description 10
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 10
- 230000004087 circulation Effects 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 1
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 20
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003463 adsorbent Substances 0.000 abstract description 7
- AWSZRNUJNSWBRK-UHFFFAOYSA-N [Li].[Si](O)(O)(O)O Chemical compound [Li].[Si](O)(O)(O)O AWSZRNUJNSWBRK-UHFFFAOYSA-N 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004568 cement Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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 present invention relates to a kind of high temperature CO2Sorbing material Li4SiO4Hydration and calcinations method of modifying.Solid phase synthesis lithium silicate powder is modified using hydration and calcinations method, hydration temperature is 80~100 DEG C, calcining heat is 700 DEG C~900 DEG C, calcination time is 2h~6h, the adsorbent average grain diameter is less than 50 microns, absorptive capacity is more than 25%, and absorptive capacity is without obvious decay after 15 circulations.The silicic acid lithium material pore structure of the modified preparation of the present invention is more abundant, has higher carbon dioxide adsorption speed and absorptive capacity, circulation absorption functional.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of silicic acid lithium material for being used to absorb high temperature carbon dioxide
Modification method for preparing, the material can be used for absorbing the carbon dioxide discharged in the flues such as fossil fired power plant, cement kiln.
Background technology
With the fast development of modern industry, fossil energy consumption amount cumulative year after year, it discharges a large amount of during utilizing
CO2Cause serious greenhouse effects.Fossil fired power plant is CO2Primary discharge source, and the CO discharged in its high temperature furnace2
Temperature is higher, and high-temperature flue gas circularly removing method can avoid CO2Cooling processing before separation, reduces CO2Trap separation process
In energy loss, realize the demands of energy-saving and emission-reduction.Thus being capable of reversible absorption CO under synthesizing high temperature2Excellent material, to subtracting
CO in few fossil fired power plant combustion process2The discharge of gas, there is important theory significance and actual application value.Lithium metasilicate
Material is considered as to be used for high temperature adsorption CO2One of preferred materials, it has higher absorptive capacity, at high temperature with good
Good recyclability, to reduce the CO discharged from high temperature furnace2Provide new way.
Li4SiO4The preparation method of adsorbent mainly includes high-temp solid synthetic method, sol-gel process and precipitation method etc..
In recent years, various countries researcher result shows to reduce particle size, increase specific grain surface product, improves material activity, can effectively carry
High Li4SiO4The absorption property of material.Although the sample particle synthesized by sol-gel process is thinner, for solid phase method,
It prepares cost height, generated time length.
The content of the invention
It is an object of the invention to provide a kind of high temperature CO2Sorbing material Li4SiO4Hydration-calcining method of modifying, it is modified
Cost is cheap and modified to CO2Advantages of good adsorption effect.
The technical scheme is that：A kind of high temperature CO2Sorbing material Li4SiO4Hydration-calcination method method of modifying, it is right
Solid phase synthesis lithium silicate powder is modified using hydration-method for calcinating, and hydration temperature is 80~100 DEG C, and calcining heat is
700 DEG C~900 DEG C, calcination time is 2h~6h, and the sorbing material average grain diameter is less than 50 microns, and absorptive capacity is more than
25%, absorptive capacity is without obvious decay after 15 circulations.
The specific method of described Solid phase synthesis lithium silicate powder is：Lithium carbonate and silica are well mixed alcohol and ground
High-temperature calcination obtains lithium silicate powder again after mill is dry.
Described hydration-method for calcinating is specially：Solid phase synthesis lithium silicate powder is added to the water, water-bath is stirred continuously
After lower reaction fully, drying, then calcine.
In hydro-combination process, keep water constant.
Described Li4SiO4High temperature CO2The Li that the hydration of adsorbent-calcination method method of modifying obtains4SiO4High temperature CO2Absorption
Agent, Solid phase synthesis lithium metasilicate is modified using hydration-method for calcinating, hydration temperature is 80~100 DEG C, and calcining heat is
700 DEG C~900 DEG C, calcination time is 2h~6h, and the adsorbent average grain diameter is less than 50 microns, and absorptive capacity is more than 25%,
Absorptive capacity is without obvious decay after 15 circulation absorption desorption cycles.
Beneficial effect：
(1) adsorbent is modified using hydration, and method is simple, cheap.Need to be stirred continuously in hydro-combination process, and avoid water
Divide evaporation.
(2) modified adsorbent pores gap structure is more abundant, has higher carbon dioxide adsorption speed and larger
Adsorbance.The a large amount of high temperature carbon dioxides discharged in the tail gas flue such as cement kiln, glass factory can directly be absorbed.
(3) it is good to recycle performance, still there is preferable absorption property after 15 circulation absorption/desorption cycles.
Brief description of the drawings
In Fig. 1 embodiments 1, before modified after lithium metasilicate sample adsorption CO2Thermogravimetric curve.
In Fig. 2 embodiments 1, before modified after lithium metasilicate sample absorption/desorption cycle performance.
In Fig. 3 embodiments 1, before modified after lithium metasilicate sample Electron micrograph.
Embodiment
Embodiment 1
It is 2 by mol ratio：1 lithium carbonate and silica is well mixed, and is added suitable alcohols ground and mixed, is then carried out
Dry.At 800 DEG C by mixing after powder be put into Muffle furnace and carry out calcining and obtain lithium silicate powder in 4 hours.By obtained silicon
Sour lithium powder (1-2g) is put into the beaker that 500ml fills with water, and then beaker is placed in 80 DEG C of water-bath and is stirred continuously, 8h
After take out, dried at 105 DEG C.Powder after drying is placed again into Muffle furnace, 4h is calcined at 800 DEG C, obtains silicic acid
Lithium powder.
Lithium silicate powder after before modified is put into thermogravimetric analyzer, in 99.999%N2In atmosphere, with 10K/min's
Heating rate is warming up to 680 DEG C, then switches to 99.999%CO2In atmosphere, constant temperature 2h carries out CO at 680 DEG C2Absorb anti-
Should, gained thermogravimetric curve as shown in Figure 1, before modified after lithium metasilicate sample maximal absorptive capacity be respectively 23.8%, 30.3%.
By the lithium silicate powder after before modified in double temperature-area tubular furnaces, multiple circulation absorption test, method of testing are carried out
It is as follows：During absorption and desorption cyclic test, CO is each led into2And N2, flow is 1.0L/min, corresponding fire box temperature
It is divided into and is set as 680 DEG C, 800 DEG C.It is layered on samples weighing and uniformly in corundum Noah's ark in test process and forms thin layer, 680
After DEG C carbonating reaction in furnace 30min, weigh, subsequently into 10min is calcined in calcining furnace, experiment is so repeated.By
15 circulations, CO2Uptake it is as shown in Figure 2.Modified W-Li4SiO4, S-Li before modified4SiO4Sample absorptivity is tieed up respectively
Hold the absorptive capacity in 27%, 11% or so, sample and obvious decay do not occur.
Using SEM, the lithium silicate powder after before modified is observed, as shown in accompanying drawing 3, wherein
(a) it is modified SEM figures for (b) before modified, modified using hydration-calcining as seen from the figure, the average grain diameter of particle is by original
200 μm be reduced to 50 μm.
Embodiment 2
Reference example 1 be hydrated-and calcining prepares silicic acid lithium adsorbent, and carries out CO under the same conditions2Absorption test,
Except that hydration temperature is 100 DEG C, hydration time 4h, CO is obtained2Absorptive capacity is 29.7%.
Embodiment 3
Reference example 1 be hydrated-and calcining prepares silicic acid lithium adsorbent, and carries out CO under the same conditions2Absorption test,
Except that calcination time 2h, 6h, obtain CO2Absorptive capacity is 32.3%, 25.5%.
Claims (4)
- A kind of 1. high temperature CO2Sorbing material Li4SiO4Hydration-calcining method of modifying, it is characterised in that：To Solid phase synthesis silicon Sour lithium powder is modified using hydration-method for calcinating, and hydration temperature is 80 ~ 100 DEG C, and calcining heat is 700 DEG C ~ 900 DEG C, Calcination time is 2h ~ 6h, for the sorbing material average grain diameter less than 50 microns, absorptive capacity is more than 25%, is inhaled through 15 circulations Absorptive capacity is without obvious decay after attached desorption cycle；Described hydration-method for calcinating is specially：By Solid phase synthesis lithium metasilicate powder End is added to the water, after water-bath is stirred continuously lower reaction fully, drying, then calcine.
- 2. high temperature CO according to claim 12Sorbing material Li4SiO4Hydration-calcining method of modifying, it is characterised in that： The specific method of described Solid phase synthesis lithium silicate powder is：Lithium carbonate and silica are well mixed, and add alcohol grinding High-temperature calcination obtains lithium silicate powder again after drying.
- 3. high temperature CO according to claim 12Sorbing material Li4SiO4Hydration-calcining method of modifying, it is characterised in that： In hydro-combination process, keep water constant.
- 4. according to any described high temperature CO of claim 1 ~ 32Sorbing material Li4SiO4Hydration-calcining method of modifying obtain Li4SiO4, it is characterised in that：Solid phase synthesis lithium metasilicate is modified using hydration-method for calcinating, hydration temperature be 80 ~ 100 DEG C, calcining heat is 700 DEG C ~ 900 DEG C, calcination time 2h ~ 6h, Li4SiO4Average grain diameter is less than 50 microns, absorbs Capacity is more than 25%, and absorptive capacity is without obvious decay after 15 circulations.
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| CN106492755B (en) * | 2016-10-15 | 2019-06-14 | 王盼 | A method of preparing carbon dioxide absorber ceramics |
| CN108654555A (en) * | 2017-03-28 | 2018-10-16 | 天津工业大学 | A kind of preparation method of the positive silicic acid lithium material of absorbing carbon dioxide at high temperature |
| CN107115845B (en) * | 2017-06-21 | 2020-04-10 | 北京金隅琉水环保科技有限公司 | Carbon dioxide adsorbent, carbon dioxide adsorption tower and carbon dioxide recovery system |
| CN108217668A (en) * | 2018-01-10 | 2018-06-29 | 清华大学 | A kind of absorption CO2Positive silicic acid lithium material and preparation method thereof |
| CN108499515B (en) * | 2018-03-05 | 2021-01-05 | 昆明理工大学 | Doped CO2Preparation method of calcium-based adsorbent |
| CN108554370B (en) * | 2018-03-30 | 2020-07-10 | 华中科技大学 | Spherical lithium-based CO2Method and equipment for preparing adsorbent |
| CN108620018A (en) * | 2018-04-11 | 2018-10-09 | 昆明理工大学 | High temperature CO is prepared using dredging Sediments of Dian Chi Lake2The method of adsorbent |
| CN109926017A (en) * | 2019-04-26 | 2019-06-25 | 重庆大学 | A kind of high-performance spherical Li4SiO4Base CO2Adsorb particle and preparation method thereof |
| CN110292906B (en) * | 2019-07-30 | 2020-08-28 | 华中科技大学 | Wet grinding modified lithium silicate, preparation method thereof and application of wet grinding modified lithium silicate as adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101653718A (en) * | 2009-09-03 | 2010-02-24 | 昆明理工大学 | Method for preparing lithium silicate material for absorbing CO2 at high temperature |
| CN101696015A (en) * | 2009-10-26 | 2010-04-21 | 昆明理工大学 | Method for preparing lithium silicate serving as high-temperature CO2 absorbing material |
| CN102583415A (en) * | 2012-02-14 | 2012-07-18 | 陕西科技大学 | Method for preparing liquid phase of Li4SiO4 high-temperature carbon pick-up material |
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| WO2010054427A1 (en) * | 2008-11-11 | 2010-05-20 | The University Of Queensland | A method for producing sorbents for co2 capture under high temperatures |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101653718A (en) * | 2009-09-03 | 2010-02-24 | 昆明理工大学 | Method for preparing lithium silicate material for absorbing CO2 at high temperature |
| CN101696015A (en) * | 2009-10-26 | 2010-04-21 | 昆明理工大学 | Method for preparing lithium silicate serving as high-temperature CO2 absorbing material |
| CN102583415A (en) * | 2012-02-14 | 2012-07-18 | 陕西科技大学 | Method for preparing liquid phase of Li4SiO4 high-temperature carbon pick-up material |
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