CN106944023A - Yb1‑xMxBaCo4O7The preparation method of oxygen-enriched combusting sorbent material - Google Patents
Yb1‑xMxBaCo4O7The preparation method of oxygen-enriched combusting sorbent material Download PDFInfo
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- CN106944023A CN106944023A CN201710148369.0A CN201710148369A CN106944023A CN 106944023 A CN106944023 A CN 106944023A CN 201710148369 A CN201710148369 A CN 201710148369A CN 106944023 A CN106944023 A CN 106944023A
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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Abstract
The invention provides rare earth doped Yb1‑xMxBaCo4O7The preparation method of oxygen-enriched combusting sorbent material, employs solid state reaction and is prepared for the Yb that rare earth element is mixed1‑xMxBaCo4O7Oxygen-enriched combusting sorbent material, this method includes：Compared with prior art, the Yb that prepared by this method1‑xMxBaCo4O7Oxygen-enriched combusting sorbent material has the advantages that operating temperature is low, oxygen adsorbance is big, oxygen absorption/desorption rate is fast, cyclical stability is high.This method have the advantages that simple and easy to apply, low cost, fast and easy, prepare sample purity it is high, can large-scale production the advantages of.
Description
Technical field
The invention belongs to functional material preparing technical field, more particularly to rare earth doped Yb1-xMxBaCo4O7It is oxygen-enriched
The preparation method of burning sorbent material.
Background technology
As causing the most important greenhouse gases of global warming, carbon dioxide（CO2）Emission reduction, recovery, fixed and profit
The hot subject of global concern is had become with problem.In addition to greatly developing new energy, improving efficiency, promotion energy-conservation, solution
CO produced by certainly existing fossil fuel2Emission problem has more realistic meaning.2001, International Energy Agency proposes will be existing
There is the CO that fossil fuel is produced2Capture is got up, and is centrally stored in the counte-rplan of abandoned mine, oil field and marine bottom.Often
Contain substantial amounts of nitrogen, CO in the flue gas that rule air burning mode is discharged2Concentration is relatively low, causes CO2Capture rate is low, cost
It is higher.If it is possible to improve CO in combustion tail gas2Concentration, it will cost recovery is greatly lowered.Oxygen-enriched combusting
（Also referred to as O2/CO2Burning）It is exactly the new combustion techniques produced in this context.The technology is constituted using pure oxygen and partial tail gas
O2/CO2Gaseous mixture is instead of air as oxidant, and the primary product after fuel combustion is CO2And H2After O, water removal in tail gas
CO2At concentrations up to more than 95%, without separation can just realize CO2Trap and seal up for safekeeping.The technology can also reduce exhaust gas heat loss
Lose, improve boiler efficiency, reduce NOxAnd SO2It is an energy-efficient, environment-friendly combustion system Deng the discharge of pollutant.
Although oxygen-enriched combusting has so significant advantage, due to needing pure oxygen in its technical process, operating cost is caused to increase.Cause
This, can the production cost that reduce oxygen in oxygen-enriched burning process be to determine the key that can the technology be employed.Industry at present
On to prepare the method for oxygen on a large scale be cryogenic air separation oxygen, its major defect is that energy ezpenditure is big and cost of investment
It is high.In consideration of it, people are exploring a kind of can replace the method for producing oxygen through of cryogenic air separation method always in recent years.
Oxygen-enriched combusting O based on ceramic adsorbent2/CO2Gaseous mixture preparation technique opens one wide to ceramic adsorbent
Application prospect.Oxygen separating material widely studied at present mainly has：Ba0.95Ca0.05Co0.8Fe0.2O3-δ、
La0.2Sr0.8Co0.8Fe0.2O3-δ、SrFeCo0.5O3-δ, these oxygen separating materials have good oxygen absorption/desorption performance, still
These oxygen separating materials only have at relatively high temperatures（800-1000℃）Just there is more considerable oxygen absorption/desorption behavior.And work
Make that the too high not only energy resource consumption of temperature is excessive, while being easily destroyed the structure of material to the practical application of oxygen separating material very not
Profit.The ceramic oxygen absorbent of current research is used to prepare O2/CO2Two subject matters are faced during gaseous mixture：One is operation temperature
Height, energy consumption is larger；Two be that oxygen desorption rate is relatively slow, and production oxygen efficiency is low.If it is possible to develop oxygen adsorbance
Greatly, the ceramic oxygen adsorbent material that oxygen absorption/desorption rate is fast, operation temperature is low, cyclical stability is high, then will promote O2/
CO2Gaseous mixture produce and oxygen-enriched combustion technology fast development.Therefore, explore just has more active oxygen to inhale at a lower temperature
The new material of attached/desorption behavior is the key of Development of Novel oxygen separating material.
RBaCo4O7（R represents rare earth element）It is the type oxide newly synthesized, is released with very peculiar oxygen storage with oxygen
Exoergic power.In 200-1000oC temperature range, when being heated in air or oxygen, the material in 200-400oC and
There are two quick oxygen uptakes in 600-1000oC warm areas and put oxygen process, the oxygen of 200oC absorption can discharge in 400oC；
The oxygen of 600oC absorption can discharge in 1000oC.Such material oxygen storage capacity is huge, oxygen storage capacity and storage oxygen temperature continuously adjustabe.
This characteristic has in fields such as gas separation, oxygen storage, lambda sensor, oxidation reduction catalyst, oxygen-enriched combusting sorbent materials
There is important application value, but such material is poor in cryogenic oxygen absorption/desorption performance, and researcher, which proposes, uses rare earth element
Doping method improves RBCo4O7Oxygen absorption/desorption characteristics of the low temperature of material, but such material is used as oxygen-enriched combusting adsorbent
The document of material is rarely reported.
The invention provides rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material and preparation method thereof, should
Rare earth doped Yb prepared by method1-xMxBaCo4O7Oxygen-enriched combusting sorbent material, energy consumption relatively low with operating temperature
It is smaller；Oxygen desorption rate is relatively fast simultaneously, the advantages of production oxygen efficiency is high.Rare earth doped Yb is prepared at present simultaneously1- xMxBaCo4O7The data of oxygen-enriched combusting sorbent material sample is rarely reported.
The content of the invention
The present invention proposes rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material and preparation method thereof, is solved
Existing ceramic oxygen-enriched combusting adsorbent is used to prepare O2/CO2Two subject matters are faced during gaseous mixture：One is that operation temperature is high,
Energy consumption is larger；Two be that oxygen desorption rate is relatively slow, and production oxygen efficiency is low.
Realize the technical scheme is that：A kind of rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting adsorbent material
The preparation method of material, step is as follows：
（1）By raw material BaCO3、Co3O4、Yb2O3、M2O3Ball milling, wherein M are carried out to mixed powder using ball mill2O3For Ce2O3、
Gd2O3、Tb2O3In any one；
（2）By step（1）Biased sample is placed in batch-type furnace after ball milling, with 2-10 in air atmosphereoC/min is heated to 800-
1100 °C are calcined, and are kept for 5-15 hours；
（3）By step（2）The powder of middle calcining used after ball milling, ball milling after powder compressing machine compressing tablet, compressing tablet sample in air
1000-1200 °C of section calcining is heated in atmosphere, is kept for 10-30 hours；
（4）By step（3）Middle calcining sample is down to room temperature, obtains Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material.
Step（1）Described BaCO3、Co3O4、Yb2O3、M2O3The ratio between middle Ba, Co, Yb, M amount of material is 1:4：（0.8
-0.95）：（0.05-0.2）.
Step（1）And step（2）Ball milling is carried out using ball mill, material ball ratio is 1:（1.1-1.8）, Ball-milling Time is 1-7
Hour.
Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material prepares O under cryogenic2/CO2Mixed gas.
The beneficial effects of the invention are as follows：Rare earth doped Yb is prepared using solid state reaction1-xMxBaCo4O7Oxygen-enriched combustion
Sorbent material is burnt, such material has operating temperature relatively low, and energy consumption is smaller；Oxygen desorption rate is relatively fast, produces oxygen efficiency
High the advantages of, it can be achieved to prepare O as oxygen-enriched combusting sorbent material under cryogenic conditions2/CO2Gaseous mixture, while this method has
The advantages of simple and easy to apply, low cost, fast and easy, it is produced on a large scale.
Brief description of the drawings
Fig. 1 is that the oxygen-enriched combusting sorbent material that embodiment 1,2 is prepared uses O at 340 DEG C2/CO2In handoff procedure
Oxygen absorption/desorption behavior.
Embodiment
Embodiment 1
Rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material and preparation method thereof, its step is：Using solid-state
Reaction method prepares rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material.
（1）By raw material BaCO3、Co3O4、Yb2O3、Ce2O3Ball milling is carried out to mixed powder using ball mill, material ball ratio is 1:
1.8, Ball-milling Time is 7 hours, and wherein the ratio between Ba, Co, Yb, M amount of material is 1:4：0.8：0.2.；
（2）By step（1）Biased sample is placed in batch-type furnace after ball milling, with 10 in air atmosphereoC/min is heated to 1100 °C
Calcined, kept for 15 hours；
（3）By step（2）The powder of middle calcining used after ball milling, ball milling after powder compressing machine compressing tablet, compressing tablet sample in air
1200 °C of section calcinings are heated in atmosphere, are kept for 10 hours；
（4）By step（3）Middle calcining sample is quickly down to room temperature, obtains Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material.
Fig. 1 is that the oxygen-enriched combusting sorbent material that embodiment 1,2 is prepared uses O at 340 DEG C2/CO2In handoff procedure
Oxygen absorption/desorption behavior.See from figure when oxygen-enriched combusting sorbent material is in gas O2When, sample starts oxygen uptake, works as gas
From O2Switch to CO2When, sample starts deoxidation.Result above shows under cryogenic in O2/CO2Oxygen can be realized in switching
Absorption/desorption behavior.Result above shows that such material can be used for oxygen-enriched combusting sorbent material, may be implemented in compared with cryogenic conditions
Lower preparation O2/CO2Mixed gas.
Embodiment 2
Rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material and preparation method thereof, its step is：
（1）By raw material BaCO3、Co3O4、Yb2O3、Ce2O3Ball milling is carried out to mixed powder using ball mill, material ball ratio is 1:1.1,
Ball-milling Time is 1 hour, and wherein the ratio between Ba, Co, Yb, M amount of material is 1:4：0.95：0.05.；
（2）By step（1）Biased sample is placed in batch-type furnace after ball milling, with 2 in air atmosphereoC/min is heated to 800 °C and entered
Row calcining, is kept for 15 hours；
（3）By step（2）The powder of middle calcining used after ball milling, ball milling after powder compressing machine compressing tablet, compressing tablet sample in air
1000 °C of section calcinings are heated in atmosphere, are kept for 30 hours；
（4）By step（3）Middle calcining sample is quickly down to room temperature, to avoid the oxygen uptake in cooling procedure, obtains Yb1- xMxBaCo4O7Oxygen-enriched combusting sorbent material.
Embodiment 3
Rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material and preparation method thereof, its step is：
（1）By raw material BaCO3、Co3O4、Yb2O3、Ce2O3Ball milling is carried out to mixed powder using ball mill, material ball ratio is 1:1.5,
Ball-milling Time is 4 hours, and wherein the ratio between Ba, Co, Yb, M amount of material is 1:4：0.9：0.1.；
（2）By step（1）Biased sample is placed in batch-type furnace after ball milling, with 5 in air atmosphereoC/min is heated to 900 °C and entered
Row calcining, is kept for 12 hours；
（3）By step（2）The powder of middle calcining used after ball milling, ball milling after powder compressing machine compressing tablet, compressing tablet sample in air
1100 °C of section calcinings are heated in atmosphere, are kept for 25 hours；
（4）By step（3）Middle calcining sample is quickly down to room temperature, to avoid the oxygen uptake in cooling procedure, obtains Yb1- xMxBaCo4O7Oxygen-enriched combusting sorbent material.
Embodiment 4
Rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material and preparation method thereof, its step is：
（1）By raw material BaCO3、Co3O4、Yb2O3、Tb2O3Ball milling is carried out to mixed powder using ball mill, material ball ratio is 1:1.5,
Ball-milling Time is 4 hours, and wherein the ratio between Ba, Co, Yb, M amount of material is 1:4：0.8：0.2.；
（2）By step（1）Biased sample is placed in batch-type furnace after ball milling, with 5 in air atmosphereoC/min is heated to 1000 °C
Calcined, kept for 10 hours；
（3）By step（2）The powder of middle calcining used after ball milling, ball milling after powder compressing machine compressing tablet, compressing tablet sample in air
1200 °C of section calcinings are heated in atmosphere, are kept for 15 hours；
（4）By step（3）Middle calcining sample is quickly down to room temperature, to avoid the oxygen uptake in cooling procedure, obtains Yb1- xMxBaCo4O7Oxygen-enriched combusting sorbent material.
Embodiment 5
Rare earth doped Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material and preparation method thereof, its step is：
（1）By raw material BaCO3、Co3O4、Yb2O3、Gd2O3Ball milling is carried out to mixed powder using ball mill, material ball ratio is 1:1.5,
Ball-milling Time is 4 hours, and wherein the ratio between Ba, Co, Yb, M amount of material is 1:4：0.8：0.2.；
（2）By step（1）Biased sample is placed in batch-type furnace after ball milling, with 5 in air atmosphereoC/min is heated to 1000 °C
Calcined, kept for 10 hours；
（3）By step（2）The powder of middle calcining used after ball milling, ball milling after powder compressing machine compressing tablet, compressing tablet sample in air
1200 °C of section calcinings are heated in atmosphere, are kept for 15 hours；
（4）By step（3）Middle calcining sample is quickly down to room temperature, to avoid the oxygen uptake in cooling procedure, obtains Yb1- xMxBaCo4O7Oxygen-enriched combusting sorbent material.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, all spirit in invention
Within principle, any modifications, equivalent substitutions and improvements made etc. should be included within the scope of the present invention.
Claims (4)
1. a kind of Yb1-xMxBaCo4O7The preparation method of oxygen-enriched combusting sorbent material, it is characterised in that step is as follows：
（1）By raw material BaCO3、Co3O4、Yb2O3、M2O3Ball milling, wherein M are carried out to mixed powder using ball mill2O3For Ce2O3、
Gd2O3、Tb2O3In any one；
（2）By step（1）Biased sample is placed in batch-type furnace after ball milling, with 2-10 in air atmosphereoC/min is heated to 800-
1100 °C are calcined, and are kept for 5-15 hours；
（3）By step（2）The powder of middle calcining used after ball milling, ball milling after powder compressing machine compressing tablet, compressing tablet sample in air
1000-1200 °C of section calcining is heated in atmosphere, is kept for 10-30 hours；
（4）By step（3）Middle calcining sample is down to room temperature, obtains Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material.
2. the Yb described in claim 11-xMxBaCo4O7The preparation method of oxygen-enriched combusting sorbent material, it is characterised in that：It is described
Step（1）BaCO3、Co3O4、Yb2O3、M2O3The ratio between middle Ba, Co, Yb, M amount of material is 1:4：（1-x）：X, wherein x=
0.05-0.2。
3. the rare earth doped Yb described in claim 11-xMxBaCo4O7The preparation method of oxygen-enriched combusting sorbent material,
It is characterized in that：Step（1）And step（3）Ball milling is carried out using ball mill, material ball ratio is 1:（1.1-1.8）, Ball-milling Time is
1-7 hours.
4. Yb prepared by the preparation method described in claim any one of 1-31-xMxBaCo4O7Oxygen-enriched combusting sorbent material should
With, it is characterised in that：Yb1-xMxBaCo4O7Oxygen-enriched combusting sorbent material prepares O under cryogenic2/CO2Mixed gas.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109292830A (en) * | 2018-11-19 | 2019-02-01 | 西北师范大学 | The method of solid phase reaction preparation four oxygen seven of pure phase indium barium cobalt |
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2017
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| CN1251320A (en) * | 1998-10-20 | 2000-04-26 | 欧洲催化剂加工公司 | Process for treating catalyst or adsorbent in fluid bed |
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Application publication date: 20170714 |