CN105664841A - Hydration-calcination modification method of high-temperature CO2 adsorption material Li4SiO4 - Google Patents
Hydration-calcination modification method of high-temperature CO2 adsorption material Li4SiO4 Download PDFInfo
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- CN105664841A CN105664841A CN201610024991.6A CN201610024991A CN105664841A CN 105664841 A CN105664841 A CN 105664841A CN 201610024991 A CN201610024991 A CN 201610024991A CN 105664841 A CN105664841 A CN 105664841A
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- 238000001354 calcination Methods 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000001179 sorption measurement Methods 0.000 title abstract description 8
- 238000002715 modification method Methods 0.000 title abstract description 3
- 238000000034 method Methods 0.000 claims abstract description 29
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052912 lithium silicate Inorganic materials 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 claims abstract description 13
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 10
- 230000036571 hydration Effects 0.000 claims abstract description 9
- 238000006703 hydration reaction Methods 0.000 claims abstract description 9
- 230000004087 circulation Effects 0.000 claims abstract description 5
- 229910052909 inorganic silicate Inorganic materials 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001035 drying 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
- 239000000203 mixture Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003463 adsorbent Substances 0.000 abstract description 8
- 239000001569 carbon dioxide Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 125000004122 cyclic group Chemical group 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 230000002238 attenuated effect Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 6
- 230000000694 effects Effects 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
- 238000002360 preparation method Methods 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
- 238000002835 absorbance Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 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
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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
-
- 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
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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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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a hydration-calcination modification method of a high-temperature CO2 adsorption material Li4SiO4. Lithium silicate powder synthesized by a solid phase method is modified by a hydration-calcination method. Hydration temperature is 80-100 DEG C, calcination temperature is 700-900 DEG C, and calcination time is 2-6 h. Average particle size of an adsorbent is less than 50 micrometers, absorption capacity is greater than 25%, and absorptive capacity is not obviously attenuated after 15 times of circulations. Pore structure of the lithium silicate material prepared after modification is more abundant, and the material has high carbon dioxide adsorption rate and absorptive capacity and has good cyclic adsorption performance.
Description
Technical field
The invention belongs to field of material technology, be specifically related to the modification method for preparing of a kind of Lithium metasilicate material for absorbing high temperature carbon dioxide, this material can be used for absorbing the carbon dioxide of discharge in the flue such as fossil fired power plant, cement kiln.
Background technology
Along with the fast development of modern industry, fossil energy consumption cumulative year after year, it utilizes a large amount of CO of discharge in process2Cause serious greenhouse effect. Fossil fired power plant is CO2Primary discharge source, and in its high temperature furnace discharge CO2Temperature is higher, and high-temperature flue gas circularly removing method can avoid CO2Cooling before separation processes, and reduces CO2Energy loss in trapping separation process, it is achieved the demand of energy-saving and emission-reduction. Thus can reversible absorption CO under synthesizing high temperature2Excellent material, to reducing CO in fossil fired power plant combustion process2The discharge of gas, has important theory significance and actual application value. Lithium metasilicate material is considered as high temperature adsorption CO2One of preferred materials, it has higher absorptive capacity, at high temperature has good recyclability, for reducing the CO of discharge from high temperature furnace2Provide new way.
Li4SiO4The preparation method of adsorbent mainly includes high-temp solid synthetic method, sol-gel process and the sedimentation method etc. In recent years, various countries' researcher result shows to reduce particle size, increase specific grain surface is long-pending, improve material activity, can be effectively improved Li4SiO4The absorption property of material. Although the sample particle synthesized by sol-gel process is relatively thin, compared to solid phase method, its preparation cost is high, and generated time is long.
Summary of the invention
It is an object of the invention to provide a kind of high temperature CO2Adsorbing material Li4SiO4Hydration-calcining method of modifying, modified with low cost and modified to CO2Advantages of good adsorption effect.
The technical scheme is that a kind of high temperature CO2Adsorbing material Li4SiO4Hydration-calcination method method of modifying, hydration-method for calcinating is adopted to be modified Solid phase synthesis lithium silicate powder, hydration temperature is 80～100 DEG C, calcining heat is 700 DEG C～900 DEG C, calcination time is 2h～6h, described adsorbing material mean diameter is less than 50 microns, and absorptive capacity is more than 25%, and after 15 times circulate, absorptive capacity is without obvious decay.
Described Solid phase synthesis lithium silicate powder method particularly includes: lithium carbonate and after silicon dioxide mix homogeneously ethanol mill-drying, high-temperature calcination obtains lithium silicate powder again.
Described hydration-method for calcinating is particularly as follows: be added to the water Solid phase synthesis lithium silicate powder, after water-bath is stirred continuously lower reaction fully, dries, then calcines.
In hydro-combination process, keep the water yield constant.
Described Li4SiO4High temperature CO2The Li that the hydration of adsorbent-calcination method method of modifying obtains4SiO4High temperature CO2Adsorbent, hydration-method for calcinating is adopted to be modified Solid phase synthesis Lithium metasilicate, hydration temperature is 80～100 DEG C, calcining heat is 700 DEG C～900 DEG C, calcination time is 2h～6h, described adsorbent mean diameter is less than 50 microns, and absorptive capacity is more than 25%, and after 15 circulation absorption desorption cycle, absorptive capacity is without obvious decay.
Beneficial effect:
(1) adsorbent adopts hydration to modifiy, and method is simple, cheap. Hydro-combination process needs be stirred continuously, and avoid moisture to evaporate.
(2) modified adsorbent pores gap structure is abundanter, has higher carbon dioxide adsorption speed and bigger adsorbance. Can to cement kiln, in the tail gas flue such as glass factory, a large amount of high temperature carbon dioxides of discharge directly absorb.
(3) recycle performance good, still there is good absorption property after 15 circulation absorption/desorption cycle.
Accompanying drawing explanation
Fig. 1. in embodiment 1, Lithium metasilicate sample adsorption CO after before modified2Thermogravimetric curve.
Fig. 2. in embodiment 1, Lithium metasilicate sample absorption/desorption cycle performance after before modified.
Fig. 3. the Lithium metasilicate sample Electron microgram in embodiment 1, after before modified.
Detailed description of the invention
Embodiment 1
By lithium carbonate that mol ratio is 2:1 and silicon dioxide mix homogeneously, add suitable alcohols ground and mixed, be then dried. At 800 DEG C by mixing after powder put into Muffle furnace carries out calcining within 4 hours, obtain lithium silicate powder. Prepared lithium silicate powder (1-2g) is put in the 500ml beaker filling with water, then beaker is placed in the water-bath of 80 DEG C and is stirred continuously, take out after 8h, dry at 105 DEG C. Powder after drying is placed again in Muffle furnace, calcines 4h at 800 DEG C, obtain lithium silicate powder.
Lithium silicate powder after before modified is put into thermogravimetric analyzer, at 99.999%N2In atmosphere, it is warming up to 680 DEG C with the heating rate of 10K/min, then switches to 99.999%CO2In atmosphere, at 680 DEG C, constant temperature 2h carries out CO2Absorption reaction, gained thermogravimetric curve as shown in Figure 1, the Lithium metasilicate sample maximal absorptive capacity after before modified respectively 23.8%, 30.3%.
By the lithium silicate powder after before modified in double; two temperature-area tubular furnaces, carrying out repeatedly circulation absorption test, method of testing is as follows: in absorption and desorption cyclic test process, each lead into CO2And N2, flow is 1.0L/min, and corresponding fire box temperature is divided into and is set as 680 DEG C, 800 DEG C. Samples weighing uniform spreading are formed thin layer by test process in corundum Noah's ark, after 680 DEG C of carbonating reaction in furnace 30min, weighs, subsequently into calcining 10min in calcining furnace, be so repeatedly performed test. Circulate through 15 times, CO2Absorbtivity as shown in Figure 2. Modified W-Li4SiO4, S-Li before modified4SiO4Sample absorbance is respectively maintained at 27%, about 11%, and obvious decay does not occur in the absorptive capacity in sample.
Adopt scanning electron microscope, lithium silicate powder after before modified is observed, as shown in Figure 3, wherein (a) schemes for modified SEM for (b) before modified, adopting hydration-calcine modified as seen from the figure, the mean diameter of granule is reduced to 50 μm by original 200 μm.
Embodiment 2
Reference example 1 carries out hydration-calcining and prepares Lithium metasilicate adsorbent, and carries out CO under the same conditions2Absorption test, institute the difference is that, hydration temperature is 100 DEG C, and hydration time is 4h, obtains CO2Absorptive capacity is 29.7%.
Embodiment 3
Reference example 1 carries out hydration-calcining and prepares Lithium metasilicate adsorbent, and carries out CO under the same conditions2Absorption test, institute the difference is that, calcination time is 2h, 6h, obtains CO2Absorptive capacity is 32.3%, 25.5%.
Claims (5)
1. a high temperature CO2Adsorbing material Li4SiO4Hydration-calcining method of modifying, it is characterised in that: to Solid phase synthesis lithium silicate powder adopt hydration-method for calcinating be modified, hydration temperature is 80 ~ 100 DEG C, and calcining heat is 700 DEG C ~ 900 DEG C, and calcination time is 2h~6h, described adsorbing material mean diameter is less than 50 microns, and absorptive capacity is more than 25%, and after 15 circulation absorption desorption cycle, absorptive capacity is without obvious decay.
2. high temperature CO according to claim 12Adsorbing material Li4SiO4Hydration-calcining method of modifying, it is characterised in that: described Solid phase synthesis lithium silicate powder method particularly includes: lithium carbonate and after silicon dioxide mix homogeneously ethanol mill-drying, high-temperature calcination obtains lithium silicate powder again.
3. high temperature CO according to claim 12Adsorbing material Li4SiO4Hydration-calcining method of modifying, it is characterised in that: described hydration-method for calcinating is particularly as follows: be added to the water Solid phase synthesis lithium silicate powder, after water-bath is stirred continuously lower reaction fully, dries, then calcines.
4. high temperature CO according to claim 12Adsorbing material Li4SiO4Hydration-calcining method of modifying, it is characterised in that: in hydro-combination process, keep the water yield constant.
5. according to the arbitrary described high temperature CO of claim 1 ~ 42Adsorbing material Li4SiO4The Li that obtains of hydration-calcining method of modifying4SiO4, it is characterised in that: adopting hydration-method for calcinating to be modified Solid phase synthesis Lithium metasilicate, hydration temperature is 80 ~ 100 DEG C, and calcining heat is 700 DEG C ~ 900 DEG C, and calcination time is 2h~6h, Li4SiO4Mean diameter is less than 50 microns, and absorptive capacity is more than 25%, and after 15 times circulate, absorptive capacity is without obvious decay.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106492755A (en) * | 2016-10-15 | 2017-03-15 | 成都育芽科技有限公司 | A kind of new method for preparing carbon dioxide absorber pottery |
| CN107115845A (en) * | 2017-06-21 | 2017-09-01 | 北京金隅琉水环保科技有限公司 | Carbon dioxide absorber, carbon dioxide adsorption tower and carbon dioxide recovery system, in accordance |
| 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 |
| CN108499515A (en) * | 2018-03-05 | 2018-09-07 | 昆明理工大学 | A kind of doping type CO2The preparation method of Ca-base adsorbent |
| CN108554370A (en) * | 2018-03-30 | 2018-09-21 | 华中科技大学 | A kind of spherical lithium base CO2The preparation method and equipment of 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 |
| 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 |
| 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 |
| CN110292906A (en) * | 2019-07-30 | 2019-10-01 | 华中科技大学 | Modified lithium metasilicate of wet grinding and preparation method thereof and the application as adsorbent |
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Cited By (14)
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| CN106492755A (en) * | 2016-10-15 | 2017-03-15 | 成都育芽科技有限公司 | A kind of new method for preparing carbon dioxide absorber pottery |
| 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 |
| CN107115845A (en) * | 2017-06-21 | 2017-09-01 | 北京金隅琉水环保科技有限公司 | Carbon dioxide absorber, carbon dioxide adsorption tower and carbon dioxide recovery system, in accordance |
| 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 |
| CN108499515A (en) * | 2018-03-05 | 2018-09-07 | 昆明理工大学 | A kind of doping type CO2The preparation method of Ca-base adsorbent |
| CN108499515B (en) * | 2018-03-05 | 2021-01-05 | 昆明理工大学 | Doped CO2Preparation method of calcium-based adsorbent |
| CN108554370A (en) * | 2018-03-30 | 2018-09-21 | 华中科技大学 | A kind of spherical lithium base CO2The preparation method and equipment of 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 |
| CN110292906A (en) * | 2019-07-30 | 2019-10-01 | 华中科技大学 | Modified lithium metasilicate of wet grinding and preparation method thereof and the application as adsorbent |
| 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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| CN105664841B (en) | 2018-01-19 |
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