CN109589910A - The preparation method and application of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier - Google Patents
The preparation method and application of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier Download PDFInfo
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- 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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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0203—Preparation of oxygen from inorganic compounds
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Abstract
The invention discloses a kind of preparation method and applications of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, this method weighs barium nitrate and cobalt nitrate first, it is hybridly prepared into nitrate solution, citric acid or urea and EDTA are then sequentially added into nitrate solution;It is uniformly mixed;MO is added again2, and for heating stirring until forming glue, collection obtains colloidal sol in the water-bath that temperature is 70~85 DEG C;Colloidal sol drying is finally arrived into barium cobalt-based properties of perovskite mixed-oxide oxygen carrier with sectional combustion.Composite oxygen carrier of the invention has more excellent oxygen desorption performance, reactivity, and preparation process is simple and efficient, and is convenient for industrialized production.There is expectation to become in a very potential Novel chain type oxygen application for oxygen-enriched combusting application using oxygen carrier prepared by the invented technology.
Description
Technical field
The present invention relates to the composite perofskite metal oxygen carriers for oxygen-enriched combusting field, and in particular to a kind of barium cobalt-based calcium
The preparation method and application of titanium ore metal composite oxide oxygen carrier.
Background technique
CO with the aggravation of global warming and the variation of weather, as greenhouse gases principal element2Emission problem by
Gradually cause the concern in the whole world.
Oxygen-enriched combustion technology is an extensive reduction fire coal CO2The technology of discharge, one of critical issue of this technology
It is to reduce oxygen cost processed, improves economy.Deep Cooling Method is the large-scale method for producing oxygen through of currently the only comercial operation, but its device
Complexity, investment is big, energy consumption is high.Chain type oxygenerating technology based on perofskite type oxide has preferable economical compared with Deep Cooling Method
Property, studies have pointed out that the energy consumption of this brand-new oxygen technique is 70% or so of traditional Deep Cooling Method, cost of investment is Deep Cooling Method
50% or so, it can be effectively reduced oxygen cost processed.This CO in circulating flue gas2It is anti-with perovskite under desorption gas high temperature
O should be produced2/CO2The method that mixed gas directly feeds oxygen-enriched combusting successfully avoids perovskite film material in high temperature reducing atmospheres
Under the thermal stability that faces and a series of problems, such as chemical stability.The novel method for producing oxygen through, which becomes one, potential can answer
For in oxygen-enriched combusting and can continuously directly feed burning needed for O2/CO2Method.
In this process, the research of oxygen carrier is a critical issue;Although having there is some researchs based on perovskite
O is produced as high-temperature adsorbing agent2/CO2Mixed gas[1-5].But all there is desorption speed in these above-mentioned perovskite materials
The lower disadvantage of rate.Therefore it is necessary to find the good Ca-Ti ore type oxygen carrier of desorption performance.
[1]Yang,Z.H.,Lin,Y.S.,High-temperature oxygen sorption in a fixed bed
packed with perovskite-type ceramic sorbents.Ind.Eng.Chem.Res.,2003,42:4376-
4381.
[2]Yang,Z.H.,Lin,Y.S.,Synergetic thermal effects for oxygen sorption
and order-disorder transition on perovskite-type oxides.Solid State Ionics,
2005,176:89-96.
[3] Yin, Q.H., Lin, Y.S., Effect of doping addition on oxygen sorption
properties of La-Sr-Co-Fe-O perovskite-type oxide.Adsorption,2006,12(5-6):
329-338.
[4]Yin,Q.H.,Lin,Y.S.,The beneficial effect of order-disorder phase
transition on oxygen sorption properties of perovskite-type oxides.Solid
State Ionics,2007,178(1-2):83-89.
[5]Guntuka,S.,Banerjee,S.,Farooq,S.,Srinivasan,M.P.,A-and B-Site
substituted lanthanum cobaltite perovskite as high temperature oxygen
sorbent.Ind.Eng.Chem.Res.,2008,47:154-162.
Therefore, there is an urgent need to develop a kind of preparation processes simply, active good, the strong perovskite oxygen carrier of oxygen desorption performance.
Summary of the invention
The requirement of the amount of oxygen needed for the present invention is unable to satisfy supply oxygen-enriched combusting for existing perovskite oxygen carrier,
It is there are reactivity, the problems such as oxygen release amount is low, provides a kind of system of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier
Preparation Method and application;This method uses with bigger serface and has in itself the fluorite knot that transmission mechanism is spread with oxonium ion
The oxide M O of structure2It is cooperateed with perovskite as compound metallic compound oxygen carrier, realizes high activity, high performance oxygen carrier
For in oxygen-enriched combusting chain type oxygen.
To achieve the above object, a kind of preparation of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier designed by the present invention
Method, comprising the following steps:
1) barium nitrate and cobalt nitrate are weighed for 1: 1 by the molar ratio of barium ions and cobalt ions, it is molten is hybridly prepared into nitrate
Liquid, it is spare;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid or urea weighs lemon for 1: 1~1.5: 1~1.5
Lemon acid or urea, metal ion total mole number and EDTA;
3) citric acid or urea and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and MO2Molar ratio be 1: 0.3~1.5 ratio add MO2, and be 70 in temperature
For heating stirring in~85 DEG C of water-bath until forming glue, collection obtains colloidal sol;Wherein, M is Ce or Zr;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 105~110 DEG C, sectional combustion is then carried out, first
It is 350~450 DEG C in temperature and carries out 0.2~1h of calcining, then calcine 8~12h at being 850~1000 DEG C in temperature, room temperature is cooling
Grinding obtains final powdery product to get barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO is arrived afterwards3-δ/MO2,
In, M=Ce or Zr.
Further, in the step 1), the molar ratio of barium ions and cobalt ions is 1: 1.
Still further, EDTA: metal ion total mole number: the molar ratio of citric acid or urea is 1 in the step 2)
∶1∶1。
Still further, in the step 4), barium ions or cobalt ions and MO2Molar ratio be 1: 0.4.
Still further, during sectional combustion, being first 350~450 DEG C in the step 5) in temperature and being calcined
0.5h, then 10h is calcined at being 850~1000 DEG C in temperature.
The present invention also provides a kind of barium cobalt-based properties of perovskite mixed-oxide oxygen carriers of above method preparation in height
Temperature prepares pure oxygen or oxygen-enriched air or O2/CO2Mixed gas, and directly oxygen supply is to the application in oxygen-enriched combusting.
Beneficial effects of the present invention:
Composite oxygen carrier of the invention has more excellent oxygen desorption performance, which, which uses, has Large ratio surface
Product and the oxide M O for having the fluorite structure with oxonium ion diffusion transmission mechanism in itself2It cooperates with perovskite as compound
Metallic compound oxygen carrier, compared with single perovskite oxygen carrier, which has higher oxygen desorption rate, reaction
Activity, and preparation process is simple and efficient, and is convenient for industrialized production.There is expectation to become one using oxygen carrier prepared by the invented technology
In a very potential Novel chain type oxygen application for oxygen-enriched combusting application.
Detailed description of the invention
Fig. 1 is the oxygen desorption curve figure of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier prepared by embodiment 1;
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, so as to those skilled in the art understand that.
Embodiment 1
The preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, comprising the following steps:
1) analytically pure Ba (NO is weighed for 1: 1 by the molar ratio of barium ions and cobalt ions3)2、Co(NO3)2·6H2O, mixing
It is configured to nitrate solution, it is spare;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid weighs EDTA for 1: 1: 1, metal ion always rubs
That number and citric acid;
3) citric acid and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and CeO2Molar ratio be 1: 0.4 ratio add CeO2, and be 75 DEG C in temperature
For heating stirring in water-bath until forming glue, collection obtains colloidal sol;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 105 DEG C, sectional combustion is then carried out, first in temperature
Calcining 0.5h is carried out for 350 DEG C, then calcines 8h at being 850 DEG C in temperature, grinding obtains final powdery product after room temperature is cooling,
Obtain barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO3-δ/CeO2。
Embodiment 2
The preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, comprising the following steps:
1) analytically pure Ba (NO is weighed for 1: 1 by the molar ratio of barium ions and cobalt ions3)2、Co(NO3)2·6H2O, mixing
It is configured to nitrate solution, it is spare;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid is that 1: 1: 1.2 to weigh EDTA, metal ion total
Molal quantity and citric acid;
3) citric acid and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and CeO2Molar ratio be 1: 1 ratio add CeO2, and the water for being 75 DEG C in temperature
For heating stirring in bath until forming glue, collection obtains colloidal sol;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 110 DEG C, sectional combustion is then carried out, first in temperature
Calcining 0.5h is carried out for 400 DEG C, then calcines 8h at being 850 DEG C in temperature, grinding obtains final powdery product after room temperature is cooling,
Obtain barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO3-δ/CeO2。
Embodiment 3
The preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, comprising the following steps:
1) analytically pure Ba (NO is weighed for 1: 1 by the molar ratio of barium ions and cobalt ions3)2、Co(NO3)2·6H2O, mixing
It is configured to nitrate solution, it is spare;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid is that 1: 1: 1.5 to weigh EDTA, metal ion total
Molal quantity and citric acid;
3) citric acid and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and CeO2Molar ratio be 1: 1.2 ratio add CeO2, and be 75 DEG C in temperature
For heating stirring in water-bath until forming glue, collection obtains colloidal sol;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 110 DEG C, sectional combustion is then carried out, first in temperature
Calcining 0.5h is carried out for 400 DEG C, then calcines 10h at being 850 DEG C in temperature, grinding obtains final powdered products after room temperature is cooling
Product to get arrive barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO3-δ/CeO2。
Embodiment 4
The preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, comprising the following steps:
1) analytically pure Ba (NO is weighed for 1: 1 by the molar ratio of barium ions and cobalt ions3)2、Co(NO3)2·6H2O, mixing
It is configured to nitrate solution, it is spare;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid is that 1: 1: 1.5 to weigh EDTA, metal ion total
Molal quantity and citric acid;
3) citric acid and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and CeO2Molar ratio be 1: 1.5 ratio add CeO2, and be 75 DEG C in temperature
For heating stirring in water-bath until forming glue, collection obtains colloidal sol;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 110 DEG C, sectional combustion is then carried out, first in temperature
It carrying out calcining 8h at calcining 0.5h is again 850 DEG C in temperature for 400 DEG C, grinding obtains final powdery product after room temperature is cooling,
Obtain barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO3-δ/CeO2。
Embodiment 5
The preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, comprising the following steps:
1) analytically pure Ba (NO is weighed for 1: 1 by the molar ratio of barium ions and cobalt ions3)2、Co(NO3)2·6H2O, mixing
It is configured to nitrate solution, it is spare;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid is that 1: 1: 1.5 to weigh EDTA, metal ion total
Molal quantity and citric acid;
3) citric acid and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and ZrO2Molar ratio be 1: 0.4 ratio add ZrO2, and be 5 DEG C in temperature
For heating stirring in water-bath until forming glue, collection obtains colloidal sol;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 110 DEG C, sectional combustion is then carried out, first in temperature
Calcining 1h is carried out for 400 DEG C, then calcines 8h at being 850 DEG C in temperature, grinding obtains final powdery product after room temperature is cooling, i.e.,
Obtain barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO3-δ/ZrO2。
Embodiment 6
The preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, comprising the following steps:
1) analytically pure Ba (NO is weighed for 1: 1 by the molar ratio of barium ions and cobalt ions3)2、Co(NO3)2·6H2O, mixing
It is configured to nitrate solution, it is spare;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid is that 1: 1: 1.2 to weigh EDTA, metal ion total
Molal quantity and citric acid;
3) citric acid and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and ZrO2Molar ratio be 1: 1 ratio add ZrO2, and the water for being 70 DEG C in temperature
For heating stirring in bath until forming glue, collection obtains colloidal sol;Wherein, M is Ce or Zr;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 110 DEG C, sectional combustion is then carried out, first in temperature
Calcining 0.5h is carried out for 400 DEG C, then calcines 12h at being 900 DEG C in temperature, grinding obtains final powdered products after room temperature is cooling
Product to get arrive barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO3-δ/ZrO2。
Metal composite oxide oxygen carrier will be prepared in above-described embodiment 1, in absorption phase, is placed on the work of oxygen processed
Make in platform, air is passed through under the conditions of temperature is 700~900 DEG C makes Ca-Ti ore type oxygen carrier adsorb the oxygen in air;
In desorption stage, with CO2As purge gass, oxygen is desorbed out of perovskite oxygen carrier and comes out and forms oxygen-enriched CO2
Air-flow;
As shown in Figure 1, under 850 DEG C of reaction temperature, CO2When as desorption gas, composite oxygen carrier of the invention
BaCoO3-δ/CeO2(when molar ratio 1: 0.4) with more excellent oxygen desorption performance compared with single perovskite oxygen carrier, oxygen is de-
Attached amount is 1.2 times of single perovskite oxygen carrier.
Other unspecified parts are the prior art.Although above-described embodiment is made that the present invention and retouches in detail
State, but it is only a part of the embodiment of the present invention, rather than whole embodiments, people can also according to the present embodiment without
Other embodiments are obtained under the premise of creativeness, these embodiments belong to the scope of the present invention.
Claims (6)
1. a kind of preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier, it is characterised in that: the following steps are included:
1) barium nitrate and cobalt nitrate are weighed for 1: 1 by the molar ratio of barium ions and cobalt ions, is hybridly prepared into nitrate solution, it is standby
With;
2) by EDTA: metal ion total mole number: the molar ratio of citric acid or urea weighs citric acid for 1: 1~1.5: 1~1.5
Or urea, metal ion total mole number and EDTA;
3) citric acid or urea and EDTA are sequentially added into nitrate solution;It is uniformly mixed;
4) by barium ions or cobalt ions and MO2Molar ratio be 1: 0.3~1.5 ratio add MO2, and be 70~85 in temperature
DEG C water-bath in heating stirring until being formed gluey, collection obtains colloidal sol;Wherein, M is Ce or Zr;
5) above-mentioned colloidal sol is dry in the vacuum oven that temperature is 105~110 DEG C, sectional combustion is then carried out, first in temperature
Degree carries out 0.2~1h of calcining for 350~450 DEG C, then calcines 8~12h at being 850~1000 DEG C in temperature, grinds after room temperature is cooling
Mill obtains final powdery product to get barium cobalt-based properties of perovskite mixed-oxide oxygen carrier BaCoO is arrived3-δ/MO2, wherein M
=Ce or Zr.
2. the preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier according to claim 1, it is characterised in that:
In the step 1), the molar ratio of barium ions and cobalt ions is 1: 1.
3. the preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier according to claim 1, it is characterised in that:
In the step 2), EDTA: metal ion total mole number: the molar ratio of citric acid or urea is 1: 1: 1.
4. the preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier according to claim 1, it is characterised in that:
In the step 4), BaCoO3With MO2Molar ratio be 1: 0.4.
5. the preparation method of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier according to claim 1, it is characterised in that:
In the step 5), during sectional combustion, be first 350~450 DEG C in temperature and carry out calcining 0.5h, then temperature be 850~
10h is calcined at 1000 DEG C.
6. a kind of barium cobalt-based properties of perovskite mixed-oxide oxygen carrier of claim 1 the method preparation prepares pure in high temperature
Oxygen or oxygen-enriched air or O2/CO2Mixed gas, and directly oxygen supply is to the application in oxygen-enriched combusting.
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CN113134352A (en) * | 2020-01-19 | 2021-07-20 | 天津大学 | Composite metal oxide catalyst for catalyzing direct decomposition of nitrogen oxide and preparation method thereof |
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