CN102443453A - Composite oxide oxygen carrier for chemical chain combustion as well as preparation method and application thereof - Google Patents
Composite oxide oxygen carrier for chemical chain combustion as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a composite oxide oxygen carrier for chemical chain combustion as well as a preparation method and application thereof. The oxygen carrier is a composite metal oxide AB'xB1-xO3 with a perovskite structure, wherein A is rare earth lanthanum; B' is doped metal nickel; B is transition metal iron; and x is more than 0 and less than 1. During application of the oxygen carrier in a chemical chain combustion technology, the temperature in an air reactor is 500-1,000 DEG C, and the temperature in a fuel reactor is 500-1,000 DEG C. The preparation method of the oxygen carrier comprises the following steps of: preparing a solution by taking ferric nitrate, nickel nitrate and lanthanum nitrate as precursors and taking citric acid or ethylene glycol as a complexing agent, and mixing and stirring uniformly; evaporating moisture till the solution turns into sticky gel from transparent sol; drying; and baking, wherein a baked sample is a composite metal oxide with a perovskite structure. The oxygen carrier disclosed by the invention has high oxygen carrying rate, high activity and high stability.
Description
Technical field
The present invention relates to a kind of composite oxides oxygen carrier of burning chemistry chains; Specifically be the oxygen carrier of chemical chain burning technology, belong to the catalyst technology in burning chemistry chains field with the perofskite type oxide.
Background technology
At present, the whole world captures and seals up for safekeeping CO to exploitation
2Technology produced sizable interest.CO in combustion gas or the coal-fired plant flue gas
2Concentration low (generally being 3.5v%-14v%), cause separating and capture CO
2Expense and energy consumption increase, therefore exploring new combustion system is to solve CO
2An important outlet that captures.Chemical chain burning technology is a kind of combustion technology of novelty, and it has broken traditional flame notion, through the non-flaming combustion that fuel and air directly do not contact, has realized CO
2Separating, produce oxynitride hardly simultaneously, is a kind of combustion technology of efficient, cleaning, has bright development prospect.But up to the present, the research that various countries' researcher is done also is in desk study and theory stage, to oxygen carrier preparation and aspect of performance research often.Oxygen carrier circulates between two reactor drums as media, and the heat that ceaselessly generates oxygen in the air reactor and reaction is delivered to the fuel reaction device and carries out reduction reaction, so the character of oxygen carrier has directly influenced the operation of whole burning chemistry chains.At present, the oxygen carrier of main research is the metal oxygen carrier, comprises Fe, Ni, Co, Cu, Mn, Cd etc., and carrier mainly contains: Al
2O
3, TiO
2, MgO, SiO
2, YSZ etc., also have a spot of nonmetal oxide such as CaSO
4Deng.In the burning chemistry chains process, oxygen carrier is in continuous oxygen loss-De oxygen condition, so the activity of oxygen is very important in the oxygen carrier.Comparatively speaking, oxygen carrier NiO/NiAl
2O
4(CHO P etc.Fuel, 2004,83 (9)), Fe
2O
3/ Al
2O
3(MATTISSON T etc.Fuel; 2001; 80 (13)) and CoO-NiO/YSZ (JIN H Getc.Energy Fuels; 1998,12 (6)) etc. over-all properties is better, and the oxygen carrier rate is limited, circulating reaction property is lower, can't bear the not high deficiency of higher temperature of reaction, MOX dispersity in oxygen carrier but exist.
Summary of the invention
To the deficiency of prior art, the invention provides the complex metal oxides oxygen carrier that is used for chemical chain burning technology of high, the active height of a kind of oxygen carrier rate, good stability.
The complex metal oxides oxygen carrier of chemical chain burning technology of the present invention is the complex metal oxides with calcium titanium ore structure, and its general formula is AB '
xB
1-xO
3, wherein A is a rare earth lanthanum, and B ' is a doping metals nickel, and B is a transition metal iron, 0＜x＜1.
The application of the complex metal oxides of the above-mentioned calcium titanium ore structure of the present invention in chemical chain burning technology; Wherein the temperature of complex metal oxides in air reactor is 500～1000 ℃; Temperature in the fuel reaction device is 500～1000 ℃, and reaction pressure is normal pressure.
Above-mentioned complex metal oxides oxygen carrier can be suitable shape such as sphere, bar shaped, microballoon, and particle size is generally 10 μ m-2000 μ m, and preferred particle size is 50 μ m-500 μ m.Can add other suitable inorganic refractory component during use, as aluminum oxide, titanium oxide, Natural manganese dioxide, silicon oxide etc. one or more.
The complex metal oxides of calcium titanium ore structure of the present invention adopts the citric acid complex method preparation.Detailed process is following: with iron nitrate, Lanthanum trinitrate, nickelous nitrate is presoma, and Hydrocerol A or terepthaloyl moietie are complexing agent, wiring solution-forming and mixing and stirring.Carry out moisture evaporation then, solution is transformed into the heavy-gravity gel by transparent colloidal sol, dry then, roasting, and the sample that obtains is for having the calcium titanium ore structure complex metal oxides.
In the method for preparing catalyst of the present invention, complexing agent can be Hydrocerol A or terepthaloyl moietie, and complexing agent and metals ion mol ratio are 1: 1～5: 1, are preferably 1: 1～3: 1.Preparation and stirred solution are preferably under 50～80 ℃ and carry out at 30～90 ℃.Stir speed (S.S.) is 100～500rpm, is preferably 300～400rpm.Churning time is 3～8 hours, is preferably 4～6 hours.Drying temperature is 60～200 ℃, is preferably 80～150 ℃.Be 1～36 hour time of drying, is preferably 8～24 hours.Maturing temperature is 400～1000 ℃, and roasting time is roasting 2-15 hour, is preferably 700～900 ℃ of following roastings 3～8 hours.
Chemical chain burning technology oxygen carrier of the present invention is the complex metal oxides of calcium titanium ore structure, and its general formula is AB '
xB
1-xO
3, A is a rare earth lanthanum, and B ' is a doping metals nickel, and B is a transition metal iron, and compared with prior art the present invention has following advantage:
1, behind the B position doping metals Ni of the present invention; B position metals ion electric charge, radius change, and lattice parameter changes, and form more oxygen room; Adsorb oxygen on the oxygen room is also more active; So not only improve the oxygen carrier rate of oxygen carrier, and promoted oxygen carrier to carry out oxidation-reduction process efficiently, accelerated the cycle efficiency of oxygen carrier in air reactor and combustion reactor.
2, contain a large amount of lattice oxygen in the oxygen carrier of the present invention, in combustion reactor, lattice oxygen can be replenished the adsorb oxygen of continuous consumption; After getting into air reactor, air provides oxygen to oxygen carrier again, so the present invention has the LaNi of calcium titanium ore structure
xFe
1-xO
3It is good oxygen carrier.
3, oxygen carrier of the present invention is suitable at high temperature reacting, and Heat stability is good, raw material are cheap and easy to get, and the preparation method is simple, is suitable for industrial application.
Description of drawings
Fig. 1 is the embodiment of the invention 1, example 2, example 3, example 4 prepared LaNi with calcium titanium ore structure
xFe
1-xO
3X-ray diffractogram.
Fig. 2 is the prepared TPR figure with calcium titanium ore structure catalyzer of the embodiment of the invention 1, example 2, example 3, example 4 and comparative example.
Embodiment
Further specify the process and the effect of the inventive method below in conjunction with embodiment.
Embodiment 1
Get 28.8g Fe (NO
3)
39H
2O, 2.3gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.9/0.1, adds the zero(ppm) water of 100mL, places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm, is stirred to whole dissolvings.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the mixing solutions of iron nitrate and nickelous nitrate then, stir while dripping.Get the 40g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 1.2: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 800 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.
Embodiment 2
Get 22.4g Fe (NO
3)
39H
2O, 6.9gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.7/0.3, is stirred to whole dissolvings.The zero(ppm) water that adds 100mL places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the iron nitrate solution then, stir while dripping.Get the 67g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 1.2: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 800 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.
Embodiment 3
Get 16g Fe (NO
3)
39H
2O, 11.5gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.5/0.5, adds the zero(ppm) water of 100mL, places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm, is stirred to whole dissolvings.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the mixing solutions of iron nitrate and nickelous nitrate then, stir while dripping.Get the 40g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 1.2: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 800 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.
Embodiment 4
Get 6.4g Fe (NO
3)
39H
2O, 18.4gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.2/0.8, adds the zero(ppm) water of 100mL, places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm, is stirred to whole dissolvings.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the mixing solutions of iron nitrate and nickelous nitrate then, stir while dripping.Get the 40g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 1.2: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 800 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.。
Embodiment 5
Get 28.8g Fe (NO
3)
39H
2O, 2.3gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.9/0.1, adds the zero(ppm) water of 100mL, places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm, is stirred to whole dissolvings.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the mixing solutions of iron nitrate and nickelous nitrate then, stir while dripping.Get the 67g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 2: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 800 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.
Embodiment 6
Get 28.8g Fe (NO
3)
39H
2O, 2.3gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.9/0.1, adds the zero(ppm) water of 100mL, places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm, is stirred to whole dissolvings.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the mixing solutions of iron nitrate and nickelous nitrate then, stir while dripping.Get the 100g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 3: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 800 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.
Embodiment 7
Get 28.8g Fe (NO
3)
39H
2O, 2.3gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.9/0.1, adds the zero(ppm) water of 100mL, places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm, is stirred to whole dissolvings.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the mixing solutions of iron nitrate and nickelous nitrate then, stir while dripping.Get the 40g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 1.2: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 900 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.
Embodiment 8
Get 28.8g Fe (NO
3)
39H
2O, 2.3gNi (NO
3)
26H
2O puts into the beaker of 500mL, and wherein the mol ratio of Fe and Ni is 0.9/0.1, adds the zero(ppm) water of 100mL, places beaker 80 ℃ water-bath then, and stirring velocity is 400rpm, is stirred to whole dissolvings.Get 34.3g La (NO
3)
36H
2O puts into the beaker of 100mL zero(ppm) water, is stirred to whole dissolvings.Be added drop-wise to lanthanum nitrate hexahydrate in the mixing solutions of iron nitrate and nickelous nitrate then, stir while dripping.Get the 40g Hydrocerol A, Hydrocerol A and metals ion total amount mol ratio are 1.2: 1, and the beaker of putting into 100mL is stirred to whole dissolvings, treat that above-mentioned mixing solutions stirred after 30 minutes, add citric acid solution slowly, stir while dripping.Stir after 5 hours, brown solution has dewatered and has become thick gel, gel is taken out in the loft drier of putting into 110 ℃ dried overnight.Take out dried uhligite precursor then, place retort furnace, rise to 400 ℃ from room temperature with the temperature rise rate of 3 ℃/min; Constant temperature calcining 2 hours; Temperature rise rate with 10 ℃/min rises to 1000 ℃ again, and constant temperature calcining 3 hours obtains the complex metal oxides oxygen carrier.
Comparative example
Adopt same procedure to prepare LaFeO
3, roasting condition, performance test condition are with embodiment 1.
Embodiment 9
Catalyst performance evaluation prepared in the foregoing description and the comparative example is carried out as follows.Evaluating catalyst test is carried out in continuous fixed bed reactor, gets catalyzer 5ml, and counts silica sand with order and mixes in 1: 1 by volume.Fuel gas is synthetic gas (30vol%H
2, 60vol%CO, 10vol%N
2), flow is 120ml/min, and temperature of reaction is 750 ℃, and reaction pressure is a normal pressure.Reduction switches to nitrogen after finishing, and simultaneous temperature is reduced to 600 ℃, keeps 20 minutes.Bubbling air then, flow is 50ml/min, temperature remains on 600 ℃.React after 10 minutes, switch to nitrogen again, simultaneous temperature rises to 750 ℃.Feed fuel gas again, reaction conditions is consistent with above-mentioned reduction reaction conditions.Adopt the on-line analysis of SP-3820 type gc, 5A molecular sieve column and Porapak Q post, TCD detects.Performance evaluation result sees table 1.
The reactivity worth of table 1 catalyzer
Claims (6)
1. the composite oxides oxygen carrier of a burning chemistry chains, it is characterized in that: oxygen carrier is the complex metal oxides AB ' with calcium titanium ore structure
xB
1-xO
3, wherein A is a rare earth lanthanum, and B ' is a doping metals nickel, and B is a transition metal iron, wherein 0＜x＜1.
2. according to the described oxygen carrier of claim 1, it is characterized in that: the complex metal oxides oxygen carrier with calcium titanium ore structure is sphere, bar shaped, microballoon, and particle size is 10 μ m-2000 μ m.
3. claim 1 or 2 application of described oxygen carrier in chemical chain burning technology; Wherein the temperature of complex metal oxides oxygen carrier in air reactor of calcium titanium ore structure is 500～1000 ℃; The temperature of burning back in the fuel reaction device is 500～1000 ℃, and reaction pressure is normal pressure.
4. the preparation method of the oxygen carrier of the said burning chemistry chains of claim 1; With iron nitrate, nickelous nitrate, Lanthanum trinitrate is presoma, is complexing agent with Hydrocerol A or terepthaloyl moietie, wiring solution-forming and mixing and stirring; Carry out moisture evaporation then; Solution is transformed into the heavy-gravity gel by transparent colloidal sol, dry then, roasting, and the sample after the roasting is the calcium titanium ore structure complex metal oxides.
5. according to the described method of claim 4; It is characterized in that: complexing agent and metals ion mol ratio are 1: 1～5: 1, and preparation and stirred solution carry out under 30～90 ℃, and churning time is 3～8 hours; Drying temperature is 60～200 ℃; Be 1～36 hour time of drying, and maturing temperature is 400～1000 ℃, and roasting time is 2-15 hour.
6. according to the described method of claim 5; It is characterized in that: complexing agent and metals ion mol ratio are 1: 1～3: 1, and preparation and stirred solution carry out under 50～80 ℃, and churning time is 4～6 hours; Drying temperature is 80～150 ℃; Be 8～24 hours time of drying, and maturing temperature is 600～900 ℃, and roasting time is 3～8 hours.
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| CN103785391A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | High-activity Fischer-Tropsch synthesis catalyst, and preparation method and application thereof |
| CN104549339A (en) * | 2013-10-23 | 2015-04-29 | 中国石油化工股份有限公司 | Methane selective oxidation catalyst, as well as preparation method and application thereof |
| CN107537503A (en) * | 2016-06-23 | 2018-01-05 | 中国石油化工股份有限公司 | A kind of oxygen carrier of biomass preparing synthetic gas, its preparation method and application |
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| CN109395571A (en) * | 2018-12-06 | 2019-03-01 | 浙江工业大学 | A method of resistance to carbonating calcium-base absorbing agent is prepared using sol-gal process |
| CN111266113A (en) * | 2020-02-27 | 2020-06-12 | 西北大学 | A kind of oxygen carrier for chemical chain combustion and cracking, preparation method and application thereof |
| CN112295565A (en) * | 2020-10-30 | 2021-02-02 | 中国矿业大学 | Multi-metal-doped perovskite catalyst, preparation method thereof and application of catalyst in catalytic pyrolysis of coal tar |
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| CN103785391A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | High-activity Fischer-Tropsch synthesis catalyst, and preparation method and application thereof |
| CN103785391B (en) * | 2012-11-01 | 2016-08-03 | 中国石油化工股份有限公司 | A kind of high activity fischer-tropsch synthetic catalyst and its preparation method and application |
| CN104549339A (en) * | 2013-10-23 | 2015-04-29 | 中国石油化工股份有限公司 | Methane selective oxidation catalyst, as well as preparation method and application thereof |
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| CN116983996B (en) * | 2023-06-20 | 2024-03-29 | 华南农业大学 | A method for preparing light olefins and co-producing high-purity carbon monoxide by chemical chain reforming of landfill gas |
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Application publication date: 20120509 |