CN107384505A - The method for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification - Google Patents
The method for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification Download PDFInfo
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- CN107384505A CN107384505A CN201710812846.9A CN201710812846A CN107384505A CN 107384505 A CN107384505 A CN 107384505A CN 201710812846 A CN201710812846 A CN 201710812846A CN 107384505 A CN107384505 A CN 107384505A
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- wheat
- iron ore
- oxygen carrier
- straw ash
- wet impregnation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L10/00—Use of additives to fuels or fires for particular purposes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23C—METHODS OR APPARATUS FOR COMBUSTION USING FLUID FUEL OR SOLID FUEL SUSPENDED IN A CARRIER GAS OR AIR
- F23C10/00—Fluidised bed combustion apparatus
Abstract
The present invention relates to a kind of method for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification.By wheat-straw ash dissolution filter in deionized water, obtained solution, 0.1~1mm iron ore particle is impregnated in solution, oxygen carrier granule is made after drying with water bath, high-temperature calcination.Basis is prepared by the use of cheap iron ore as oxygen carrier, oxygen carrier granule is successively prepared by dipping, drying and calcination step, preparation technology is simple, and the alkali metal in wheat-straw ash is come out with ash separation, other compositions to the adverse effect of oxygen carrier, realize the grey recycling of wheat-straw in ash when efficiently solving dry method modification.The iron ore oxygen carrier anti-sintering property of obtained wheat-straw ash modification significantly improves with reactivity, and the total transformation efficiencies of CO are higher than pure iron ore.
Description
Technical field
The present invention relates to a kind of method for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, belongs to chemistry
Chain burning technology field.
Background technology
Global warming increasingly sharpens caused by greenhouse effects, CO2As main greenhouse gases, its emission-reduction technology is by more
Carry out more attention.CO2Trapping and storing technology (carbon capture and carbon storage, CCS) be considered as
It is that can realize CO with most effective2The technology of emission reduction, current most of CCS technologies have that carbon trapping cost is high, and resource consumption is big
Problem.Chemical chain burning technology (chemical looping combustion, CLC) is that one kind can realize CO2Interior separation
New combustion technique, while the utilization ratio of resource can be improved, reduce NOXDischarge, is a kind of burning with very big potentiality
Mode.
An important factor for oxygen carrier is limitation chemical chain burning technology development, it is firing as oxygen and the main carriers of heat
Expect reciprocation cycle between reactor and air reactor, thus should possess good oxygen carrying capability, redox reaction activity,
Wear resistance, while should also have the characteristics of cheap and environment-friendly.Iron ore because rich reserves, and iron oxide into
Divide content higher, it is considered to be there is the oxygen carrier of applications well prospect, for iron ore, numerous studies have been done by each research institution,
And confirm its feasibility as oxygen carrier application.But it is iron ore as the main of oxygen carrier that reactivity is relatively low
Restrictive factor, research shows, oxygen carrier is modified using alkali metal K, Na and alkaline-earth metal Ca, can be greatly improved
The reactivity of oxygen carrier.The existing universal complex process of method modified iron ore, and cost of manufacture is expensive, it is unfavorable
Utilized in the large-scale commercial applications of oxygen carrier.Meanwhile research is found in wheat-straw ash containing substantial amounts of alkali metal K, Na and alkaline earth gold
Belong to Ca, if can effectively utilize it, huge economic benefit can be achieved.
The content of the invention
Technical problem：For above-mentioned existing technical problem and deficiency, the present invention proposes that one kind utilizes wheat-straw ash wet method
The method that dipping modification prepares iron ore oxygen carrier.The basis that the present invention is prepared using cheap iron ore as oxygen carrier, utilize
Wheat-straw ash obtained solution, then iron ore is impregnated, drying and calcination processing, finally obtain oxygen carrier by screening.Gained
The anti-caking power and reactivity of oxygen carrier greatly improve, and the preparation method can both reduce the cost of manufacture of oxygen carrier, again
Alkali metal can be extracted from wheat-straw ash, realize the recycling of wheat-straw ash.
Technical scheme：The method for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification of the present invention, the party
Method is made by wet impregnation, and described wet impregnation comprises the following steps：
1) prepared by iron ore：Original iron ore is placed in disintegrating machine and crushed, then filters out 0.1~1mm iron ore
Particle；
2) prepared by wheat-straw ash：Wheat-straw is crushed, then puts it into Muffle furnace and calcines, and screen out particle diameter and be less than
0.3mm wheat-straw ash particle；
3) prepared by solution：Wheat-straw ash particle made from step 2) is put into deionized water, stirs, is subsequently placed in
Stood in water-bath, filter obtained solution；
4) impregnation：Iron ore particle made from step 1) is put into solution made from step 3), after stirring,
Stand at room temperature, sample is made；
5) drying and calcining is handled：Sample made from step 4) is placed in air dry oven and dried, then will be dried
Mixture is put into Muffle furnace calcining, obtains finished product；
6) Screening Treatment is crushed：The finished product that step 5) is obtained crushes, and filters out that particle size range is 0.1~1mm
Grain, the iron ore oxygen carrier granule using wheat-straw ash modification is made.
Wherein,
Fe in the original iron ore2O3Mass fraction >=70%.
K in wheat-straw ash2O mass fraction >=10%.
In step 2), the grey temperature of system is set in Muffle furnace as 600~650 DEG C, calcination time is 2~3h.
In step 3), the temperature of water-bath is 20~25 DEG C, and the time of standing is 2~3h.
The time stood in step 4) is 20~21h.
In step 5), the temperature dried in air dry oven is at 100~105 DEG C, and the temperature of calcining is 900 in Muffle furnace
~950 DEG C.
Beneficial effect：The present invention relates to a kind of iron ore oxygen carrier using the modification of wheat-straw ash wet impregnation and its preparation
Method, main application fields are burning chemistry chains, can effectively reduce greenhouse gases CO2Discharge, to alleviate global warming have
Highly important meaning.
(1) it is basic by the use of the preparation of natural iron ore as the oxygen carrier of rich reserves, it is cheap, be advantageous to oxygen carrier
Extensive making, provide condition for the commercial applications of chemical chain burning technology.
(2) modified, first obtained solution, alkali metal can be separated from wheat-straw ash using wet impregnation mode
Out, other compositions are avoided in ash to the adverse effect of oxygen carrier.
(3) the problem of iron ore reactivity is relatively low is directed to, and alkali metal K, Na and alkaline-earth metal Ca can be carried significantly
The result of study of high oxygen carrier activity, is changed the preparation method directly modified using alkali metal soln oxygen carrier, proposed
Oxygen carrier is modified using wheat-straw ash, the waste of resource can be avoided to a certain extent.
(4) modification mode uses wet impregnation, and one side manufacture craft is simple and easy, can substantially reduce cost of manufacture, separately
On the one hand it can ensure that oxygen carrier fully absorbs the alkali metal in wheat-straw ash, improve the level of resources utilization.
Brief description of the drawings
Fig. 1 is the preparation method flow chart that iron ore oxygen carrier is prepared using wheat-straw ash wet impregnation modification.
Embodiment
The present invention is elaborated with reference to specific embodiment, but these examples are not intended to limit the protection model of the invention
Enclose.The raw materials used wheat-straw for after a kind of iron ore and crushing in example, deionized water is used when preparing solution.
Embodiment 1：
The method that the present invention prepares oxygen carrier using iron ore, is comprised the following steps that：
1) prepared by iron ore：Iron ore is placed in disintegrating machine and crushed, then filters out 0.1~0.3mm iron ore
Grain；
2) prepared by wheat-straw ash：Wheat-straw is crushed, then put it into Muffle furnace, sets the grey temperature of system as 600 DEG C,
Calcination time is 3h, and screens out the ash particle that particle diameter is less than 0.1mm；
3) prepared by solution：Take wheat-straw ash made from 10g steps 2) to be put into 100ml deionized waters, stir, then
It is placed in 20 DEG C of water-bath and stands 3h, filters obtained solution；
4) impregnation：Iron ore 100g made from step 1) is taken to be put into solution made from step 3), after stirring,
20h is stood at room temperature；
5) drying and calcining is handled：Sample made from step 4) is placed in air dry oven, dried at 100 DEG C, then
Dried mixture is put into Muffle furnace, 3h is calcined at 900 DEG C；
6) Screening Treatment is crushed：The sample broke that step 5) is obtained, and filter out that particle size range is 0.1-0.3mm
Grain, the iron ore oxygen carrier granule using the modification of wheat-straw ash wet impregnation is made.
Oxygen carrier granule made from the present embodiment is used for during burning chemistry chains：In experimentation, first by 40g oxygen carriers
Sample is put on the air distribution plate of fluidized-bed reactor, in 5%O2/N2(2L·min-1) atmosphere under be warming up to design temperature；Treat
After temperature stabilization, gas is switched into N2Atmosphere (2Lmin-1) purging 10min；Then N is adjusted2For 1.90Lmin-1, and lead to
Enter 0.1Lmin-1CO starts reduction reaction, and the reduction reaction time is set as 20min.Gaseous product uses gas collection after cooling and dedusting
Bag is collected, and the gas collection time is 2min, and carries out flue gas analysis to the gas being collected into flue gas analyzer.As a result show, CO tires out
Product conversion ratio is 92.7%.
Embodiment 2：
The method that the present invention prepares oxygen carrier using iron ore, is comprised the following steps that：
1) prepared by iron ore：Iron ore is placed in disintegrating machine and crushed, then filters out 0.1-0.3mm iron ore
Grain；
2) prepared by wheat-straw ash：Wheat-straw is crushed, then put it into Muffle furnace, sets the grey temperature of system as 650 DEG C,
Calcination time is 3h, and screens out the ash particle that particle diameter is less than 0.1mm；
3) prepared by solution：Take wheat-straw ash made from 20g steps 2) to be put into 100ml deionized waters, stir, then
It is placed in 25 DEG C of water-bath and stands 3h, filters obtained solution；
4) impregnation：Iron ore 100g made from step 1) is taken to be put into solution made from step 3), after stirring,
20h is stood at room temperature；
5) drying and calcining is handled：Sample made from step 4) is placed in air dry oven, dried at 105 DEG C, then
Dried mixture is put into Muffle furnace, 3h is calcined at 950 DEG C；
6) Screening Treatment is crushed：The sample broke that step 5) is obtained, and filter out that particle size range is 0.1-0.3mm
Grain, the iron ore oxygen carrier granule using the modification of wheat-straw ash wet impregnation is made.
Oxygen carrier granule made from the present embodiment is used for during burning chemistry chains：In experimentation, first by 40g oxygen carriers
Sample is put on the air distribution plate of fluidized-bed reactor, in 5%O2/N2(2L·min-1) atmosphere under be warming up to design temperature；Treat
After temperature stabilization, gas is switched into N2Atmosphere (2Lmin-1) purging 10min；Then N is adjusted2For 1.90Lmin-1, and lead to
Enter 0.1Lmin-1CO starts reduction reaction, and the reduction reaction time is set as 20min.Gaseous product uses gas collection after cooling and dedusting
Bag is collected, and the gas collection time is 2min, and carries out flue gas analysis to the gas being collected into flue gas analyzer.As a result show, CO tires out
Product conversion ratio is 95.1%.
Comparative example：
The method that oxygen carrier is prepared using pure iron ore, is comprised the following steps that：
1) prepared by iron ore：Iron ore is placed in disintegrating machine and crushed, then filters out 0.1~0.3mm iron ore
Grain；
2) high-temperature calcination is handled：Iron ore particle 100g made from step 1) is taken, is put into Muffle furnace in 950 DEG C of high temperature
2~3h of lower calcining；
3) Screening Treatment is crushed：The sample broke that step 2) is obtained, and it is 0.1~0.3mm's to filter out particle size range
Particle, pure iron ore oxygen carrier granule is made.
Oxygen carrier granule made from this comparative example is used for during burning chemistry chains：In experimentation, first by 40g oxygen carriers
Sample is put on the air distribution plate of fluidized-bed reactor, in 5%O2/N2(2L·min-1) atmosphere under be warming up to design temperature；Treat
After temperature stabilization, gas is switched into N2Atmosphere (2Lmin-1) purging 10min；Then N is adjusted2For 1.90Lmin-1, and lead to
Enter 0.1Lmin-1CO starts reduction reaction, and the reduction reaction time is set as 20min.Gaseous product uses gas collection after cooling and dedusting
Bag is collected, and the gas collection time is 2min, and carries out flue gas analysis to the gas being collected into flue gas analyzer.As a result show, CO tires out
Product conversion ratio is 84.9%.
To sum up, the iron ore oxygen carrier of the present invention modified using wheat-straw ash wet impregnation, wheat-straw ash are drawn
Enter the reactivity for greatly enhancing oxygen carrier, significantly improve the transformation efficiency of fuel.
Special instruction, the above is elaborated to the embodiment of the present invention, but the present invention is not limited to
Embodiment is stated, in those of ordinary skill in the art's possessed knowledge, present inventive concept can also not departed from
Under the premise of to concrete operation step, various changes can be made and various reactants and reaction condition are modified replacement, therefore directly
Or it is both contained in indirectly with the present invention in other association areas in the range of of the invention contain.
Claims (7)
- A kind of 1. method for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, it is characterised in that this method is led to Cross wet impregnation to be made, described wet impregnation comprises the following steps：1) prepared by iron ore：Original iron ore is placed in disintegrating machine and crushed, then filters out 0.1~1mm iron ore particle；2) prepared by wheat-straw ash：Wheat-straw is crushed, then puts it into Muffle furnace and calcines, and screen out particle diameter and be less than 0.3mm wheat-straw ash particle；3) prepared by solution：Wheat-straw ash particle made from step 2) is put into deionized water, stirs, is subsequently placed in water-bath Middle standing, filter obtained solution；4) impregnation：Iron ore particle made from step 1) is put into solution made from step 3), after stirring, room temperature Lower standing, sample is made；5) drying and calcining is handled：Sample made from step 4) is placed in air dry oven and dried, then by dried mixing Thing is put into Muffle furnace calcining, obtains finished product；6) Screening Treatment is crushed：The finished product that step 5) is obtained crushes, and filters out the particle that particle size range is 0.1~1mm, system The iron ore oxygen carrier granule of wheat-straw ash modification must be utilized.
- 2. the method according to claim 1 for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, it is special Sign is, Fe in the original iron ore2O3Mass fraction >=70%.
- 3. the method according to claim 1 for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, it is special Sign is, K in wheat-straw ash2O mass fraction >=10%.
- 4. the method according to claim 1 for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, it is special Sign is in step 2), the grey temperature of system is set in Muffle furnace as 600~650 DEG C, calcination time is 2~3h.
- 5. the method according to claim 1 for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, it is special Sign is in step 3) that the temperature of water-bath is 20~25 DEG C, and the time of standing is 2~3h.
- 6. the method according to claim 1 for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, it is special The time that sign is to stand in step 4) is 20~21h.
- 7. the method according to claim 1 for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification, it is special Sign is in step 5), and the temperature dried in air dry oven is at 100~105 DEG C, in Muffle furnace the temperature of calcining for 900~ 950℃。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142491A (en) * | 2020-09-18 | 2020-12-29 | 西安交通大学 | Integrated oxygen carrier for chemical looping hydrogen production, preparation method, hydrogen production system and method |
| CN113337325A (en) * | 2021-04-27 | 2021-09-03 | 东南大学 | Rapid screening method of high-performance oxygen carrier material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367157A (en) * | 2016-11-07 | 2017-02-01 | 东南大学 | Method for preparing chemical looping combustion oxygen carrier and modifying iron ore through oilseed rape straw ash |
| CN106867624A (en) * | 2017-03-07 | 2017-06-20 | 东南大学 | A kind of CuO and quasi- east coal ash modify oxygen carrier of iron ore and preparation method thereof jointly |
-
2017
- 2017-09-11 CN CN201710812846.9A patent/CN107384505B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367157A (en) * | 2016-11-07 | 2017-02-01 | 东南大学 | Method for preparing chemical looping combustion oxygen carrier and modifying iron ore through oilseed rape straw ash |
| CN106867624A (en) * | 2017-03-07 | 2017-06-20 | 东南大学 | A kind of CuO and quasi- east coal ash modify oxygen carrier of iron ore and preparation method thereof jointly |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142491A (en) * | 2020-09-18 | 2020-12-29 | 西安交通大学 | Integrated oxygen carrier for chemical looping hydrogen production, preparation method, hydrogen production system and method |
| CN112142491B (en) * | 2020-09-18 | 2022-02-22 | 西安交通大学 | Integrated oxygen carrier for chemical looping hydrogen production, preparation method, hydrogen production system and method |
| CN113337325A (en) * | 2021-04-27 | 2021-09-03 | 东南大学 | Rapid screening method of high-performance oxygen carrier material |
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