CN107384505B - 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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- CN107384505B CN107384505B CN201710812846.9A CN201710812846A CN107384505B CN 107384505 B CN107384505 B CN 107384505B CN 201710812846 A CN201710812846 A CN 201710812846A CN 107384505 B CN107384505 B CN 107384505B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 62
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 58
- 239000001301 oxygen Substances 0.000 title claims abstract description 58
- 239000010902 straw Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000005470 impregnation Methods 0.000 title claims abstract description 23
- 230000004048 modification Effects 0.000 title claims abstract description 18
- 238000012986 modification Methods 0.000 title claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 43
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000007598 dipping method Methods 0.000 claims abstract description 6
- 241000209140 Triticum Species 0.000 claims description 49
- 235000021307 Triticum Nutrition 0.000 claims description 49
- 238000012216 screening Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 8
- 239000011363 dried mixture Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 150000001340 alkali metals Chemical class 0.000 abstract description 6
- 230000009257 reactivity Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 abstract 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 230000009466 transformation Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 17
- 238000002485 combustion reaction Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 4
- 150000001342 alkaline earth metals Chemical class 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 238000004868 gas analysis Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a kind of methods for preparing iron ore oxygen carrier using wheat-straw ash wet impregnation modification.By wheat-straw ash, the iron ore particle of 0.1~1mm is impregnated in solution by dissolution filter, obtained solution in deionized water, and oxygen carrier granule is made after drying with water bath, high-temperature calcination.Basis is prepared using cheap iron ore as oxygen carrier, oxygen carrier granule is successively prepared by dipping, drying and calcination step, preparation process is simple, and the alkali metal element in wheat-straw ash is come out with ash separation, other compositions realize the resource utilization of wheat-straw ash to the adverse effect of oxygen carrier in ash when efficiently solving dry method modification.The iron ore oxygen carrier anti-sintering property of wheat-straw ash modification obtained is significantly improved with reactivity, and the total transformation efficiency of CO is higher than pure iron ore.
Description
Technical Field
The invention relates to a method for preparing an iron ore oxygen carrier by using wheat straw ash through wet impregnation modification, and belongs to the technical field of chemical-looping combustion.
Background
The global warming caused by the greenhouse effect is increasingly intensified, and CO2As a main greenhouse gas, the emission reduction technology is more and more emphasized. CO 22Is considered to be the most efficient CO capture and storage technology (CCS)2Most of the existing CCS technologies of the emission reduction technology have the problems of high carbon capture cost and large resource consumption. Chemical Looping Combustion (CLC) is a technology capable of realizing CO2The novel combustion technology of internal separation can improve the utilization efficiency of resources and reduce NOXAnd the emission is a combustion mode with great potential.
The oxygen carrier is an important factor for limiting the development of the chemical looping combustion technology, is used as a main carrier of oxygen and heat, and is circulated between a fuel reactor and an air reactor, so that the oxygen carrier has good oxygen carrying capacity, oxidation-reduction reaction activity and wear resistance, and has the characteristics of low price and environmental friendliness. Because the storage amount of the iron ore is rich and the content of the iron oxide component is high, the iron ore is considered to be an oxygen carrier with good application prospect, a great deal of research is carried out on various research institutions of the iron ore, and the feasibility of the application of the iron ore as the oxygen carrier is proved. However, the relatively low reactivity is the most limiting factor of the iron ore as the oxygen carrier, and researches show that the reactivity of the oxygen carrier can be greatly improved by modifying the oxygen carrier with alkali metal K, Na and alkaline earth metal Ca. The existing method for modifying the iron ore is generally complex in process and expensive in manufacturing cost, and is not beneficial to large-scale commercial utilization of the oxygen carrier. Meanwhile, researches find that the wheat straw ash contains a large amount of alkali metal K, Na and alkaline earth metal Ca, and if the alkali metal K, Na and the alkaline earth metal Ca can be effectively utilized, huge economic benefits can be realized.
Disclosure of Invention
The technical problem is as follows: aiming at the existing technical problems and defects, the invention provides a method for preparing an iron ore oxygen carrier by using wheat straw ash through wet impregnation modification. The method takes cheap iron ore as the basis of oxygen carrier preparation, utilizes wheat straw ash to prepare solution, then carries out dipping, drying and calcining treatment on the iron ore, and finally screens to prepare the oxygen carrier. The sintering resistance and the reaction activity of the obtained oxygen carrier are greatly improved, the preparation method can reduce the manufacturing cost of the oxygen carrier, and can extract alkali metal elements from wheat straw ash, thereby realizing the resource utilization of the wheat straw ash.
The technical scheme is as follows: the invention relates to a method for preparing an iron ore oxygen carrier by utilizing wheat straw ash through wet impregnation modification, which is prepared through wet impregnation and comprises the following steps:
1) preparing iron ore: placing original iron ore into a crusher to be crushed, and then screening out iron ore particles with the particle size of 0.1-1 mm;
2) preparing wheat straw ash: crushing wheat straws, then putting the wheat straws into a muffle furnace for calcining, and screening wheat straw ash particles with the particle size of less than 0.3 mm;
3) solution preparation: putting the wheat straw ash particles prepared in the step 2) into deionized water, uniformly stirring, then placing in a water bath for standing, and filtering to obtain a solution;
4) dipping treatment: putting the iron ore particles prepared in the step 1) into the solution prepared in the step 3), uniformly stirring, and standing at room temperature to prepare a sample;
5) drying and calcining treatment: drying the sample prepared in the step 4) in an air-blast drying oven, and then putting the dried mixture into a muffle furnace for calcining to obtain a finished product;
6) crushing and screening treatment: crushing the finished product obtained in the step 5), and screening out particles with the particle size range of 0.1-1 mm to obtain the iron ore oxygen carrier particles modified by the wheat straw ash.
Wherein,
fe in the original iron ore2O3The mass fraction is more than or equal to 70 percent.
K in wheat straw ash2The mass fraction of O is more than or equal to 10 percent.
In the step 2), the temperature of the prepared ash in the muffle furnace is 600-650 ℃, and the calcining time is 2-3 h.
In the step 3), the temperature of the water bath is 20-25 ℃, and the standing time is 2-3 h.
The standing time in the step 4) is 20-21 h.
In the step 5), the drying temperature in the blast drying oven is 100-105 ℃, and the calcining temperature in the muffle furnace is 900-950 ℃.
Has the advantages that: the invention relates to an iron ore oxygen carrier modified by wheat straw ash wet impregnation and a preparation method thereof, and mainly belongs to the field of chemical looping combustion, and the oxygen carrier can effectively reduce greenhouse gas CO2The emission of (2) has very important significance for relieving global warming.
(1) The natural iron ore with rich reserves is used as the preparation basis of the oxygen carrier, the price is low, the large-scale preparation of the oxygen carrier is facilitated, and the condition is provided for the commercial application of the chemical-looping combustion technology.
(2) The modification is carried out by a wet impregnation method, and the solution is prepared firstly, so that alkali metal elements can be separated from wheat straw ash, and the adverse effect of other components in the ash on the oxygen carrier is avoided.
(3) Aiming at the problem of low reactivity of iron ore and the research result that the alkali metal K, Na and the alkaline earth metal Ca can obviously improve the activity of the oxygen carrier, the preparation method that the oxygen carrier is modified by directly using the alkali metal solution is changed, the wheat straw ash is used for modifying the oxygen carrier, and the waste of resources can be avoided to a certain extent.
(4) The modification mode adopts wet impregnation, on one hand, the manufacturing process is simple and easy to implement, the manufacturing cost can be greatly reduced, on the other hand, the oxygen carrier can be ensured to fully absorb the alkali metal elements in the wheat straw ash, and the resource utilization efficiency is improved.
Drawings
FIG. 1 is a flow chart of a manufacturing method for preparing an iron ore oxygen carrier by using wet impregnation modification of wheat straw ash.
Detailed Description
The present invention is described in detail below with reference to specific examples, which are not intended to limit the scope of the invention. In the example, the raw material used was iron ore and pulverized wheat straw, and deionized water was used for the solution preparation.
Example 1:
the method for preparing the oxygen carrier by using the iron ore comprises the following specific steps:
1) preparing iron ore: placing the iron ore into a crusher for crushing, and then screening iron ore particles with the particle size of 0.1-0.3 mm;
2) preparing wheat straw ash: crushing wheat straws, putting the wheat straws into a muffle furnace, setting the ash temperature to be 600 ℃, calcining for 3 hours, and screening ash particles with the particle size of less than 0.1 mm;
3) solution preparation: taking 10g of wheat straw ash prepared in the step 2), putting the wheat straw ash into 100ml of deionized water, uniformly stirring, then placing the mixture in a water bath at the temperature of 20 ℃, standing for 3 hours, and filtering to obtain a solution;
4) dipping treatment: putting 100g of the iron ore prepared in the step 1) into the solution prepared in the step 3), uniformly stirring, and standing for 20 hours at room temperature;
5) drying and calcining treatment: putting the sample prepared in the step 4) into an air drying oven, drying at 100 ℃, then putting the dried mixture into a muffle furnace, and calcining for 3 hours at 900 ℃;
6) crushing and screening treatment: crushing the sample obtained in the step 5), and screening out particles with the particle size range of 0.1-0.3mm to prepare the iron ore oxygen carrier particles modified by the wheat straw ash wet impregnation.
The oxygen carrier particles prepared in this example were used in a chemical looping combustion process: in the experimental process, 40g of oxygen carrier sample is firstly put on a grid plate of a fluidized bed reactor and is in 5 percent O2/N2(2L·min-1) Heating to a set temperature in the atmosphere of (3); after the temperature is stabilized, the gas is switched to N2Atmosphere (2 L.min)-1) Purging for 10 min; then adjust N2Is 1.90 L.min-1And introducing 0.1 L.min-1The CO started reduction reaction, and the reduction reaction time was set to 20 min. And cooling and dedusting the gas product, collecting the gas product by using a gas collection bag, wherein the gas collection time is 2min, and performing flue gas analysis on the collected gas by using a flue gas analyzer. The results showed a cumulative CO conversion of 92.7%.
Example 2:
the method for preparing the oxygen carrier by using the iron ore comprises the following specific steps:
1) preparing iron ore: placing the iron ore into a crusher for crushing, and then screening out iron ore particles with the particle size of 0.1-0.3 mm;
2) preparing wheat straw ash: crushing wheat straws, then putting the wheat straws into a muffle furnace, setting the ash making temperature to be 650 ℃, calcining for 3 hours, and screening ash particles with the particle size of less than 0.1 mm;
3) solution preparation: taking 20g of wheat straw ash prepared in the step 2), putting the wheat straw ash into 100ml of deionized water, uniformly stirring, then placing the mixture in a water bath at 25 ℃ for standing for 3 hours, and filtering to obtain a solution;
4) dipping treatment: putting 100g of the iron ore prepared in the step 1) into the solution prepared in the step 3), uniformly stirring, and standing for 20 hours at room temperature;
5) drying and calcining treatment: putting the sample prepared in the step 4) into a forced air drying oven, drying at 105 ℃, then putting the dried mixture into a muffle furnace, and calcining for 3 hours at 950 ℃;
6) crushing and screening treatment: crushing the sample obtained in the step 5), and screening out particles with the particle size range of 0.1-0.3mm to prepare the iron ore oxygen carrier particles modified by the wheat straw ash wet impregnation.
The oxygen carrier particles prepared in this example were used in a chemical looping combustion process: in the experimental process, 40g of oxygen carrier sample is firstly put on a grid plate of a fluidized bed reactor and is in 5 percent O2/N2(2L·min-1) Heating to a set temperature in the atmosphere of (3); after the temperature is stabilized, the gas is switched to N2Atmosphere (2 L.min)-1) Purging for 10 min; then adjust N2Is 1.90 L.min-1And introducing 0.1 L.min-1The CO started reduction reaction, and the reduction reaction time was set to 20 min. Cooling and dedusting the gas product, collecting with gas collecting bag for 2min, and analyzing the collected gas with flue gas analyzerThe gas is subjected to flue gas analysis. The results showed a cumulative CO conversion of 95.1%.
Comparative example:
the method for preparing the oxygen carrier by using the pure iron ore comprises the following specific steps:
1) preparing iron ore: placing the iron ore into a crusher for crushing, and then screening iron ore particles with the particle size of 0.1-0.3 mm;
2) high-temperature calcination treatment: taking 100g of the iron ore particles prepared in the step 1), and calcining the iron ore particles in a muffle furnace at a high temperature of 950 ℃ for 2-3 h;
3) crushing and screening treatment: crushing the sample obtained in the step 2), and screening out particles with the particle size range of 0.1-0.3mm to obtain the pure iron ore oxygen carrier particles.
The oxygen carrier particles prepared in this comparative example were used in a chemical looping combustion process: in the experimental process, 40g of oxygen carrier sample is firstly put on a grid plate of a fluidized bed reactor and is in 5 percent O2/N2(2L·min-1) Heating to a set temperature in the atmosphere of (3); after the temperature is stabilized, the gas is switched to N2Atmosphere (2 L.min)-1) Purging for 10 min; then adjust N2Is 1.90 L.min-1And introducing 0.1 L.min-1The CO started reduction reaction, and the reduction reaction time was set to 20 min. And cooling and dedusting the gas product, collecting the gas product by using a gas collection bag, wherein the gas collection time is 2min, and performing flue gas analysis on the collected gas by using a flue gas analyzer. The results showed a cumulative CO conversion of 84.9%.
In conclusion, the iron ore oxygen carrier modified by the wheat straw ash through wet impregnation has the advantages that the reaction activity of the oxygen carrier is greatly enhanced due to the introduction of the wheat straw ash, and the conversion efficiency of fuel is remarkably improved.
While specific embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and various changes in the specific procedures and changes in the reactants and reaction conditions may be made without departing from the spirit of the present invention.
Claims (7)
1. A method for preparing an iron ore oxygen carrier by utilizing wheat straw ash wet impregnation modification is characterized in that the method is prepared by wet impregnation, and the wet impregnation comprises the following steps:
1) preparing iron ore: placing original iron ore into a crusher to be crushed, and then screening out iron ore particles with the particle size of 0.1-1 mm;
2) preparing wheat straw ash: crushing wheat straws, then putting the wheat straws into a muffle furnace for calcining, and screening wheat straw ash particles with the particle size of less than 0.3 mm;
3) solution preparation: putting the wheat straw ash particles prepared in the step 2) into deionized water, uniformly stirring, then placing in a water bath for standing, and filtering to obtain a solution;
4) dipping treatment: putting the iron ore particles prepared in the step 1) into the solution prepared in the step 3), uniformly stirring, and standing at room temperature to prepare a sample;
5) drying and calcining treatment: drying the sample prepared in the step 4) in an air-blast drying oven, and then putting the dried mixture into a muffle furnace for calcining to obtain a finished product;
6) crushing and screening treatment: crushing the finished product obtained in the step 5), and screening out particles with the particle size range of 0.1-1 mm to obtain the iron ore oxygen carrier particles modified by the wheat straw ash.
2. The method for preparing the iron ore oxygen carrier by using the wheat straw ash wet impregnation modification according to claim 1, wherein Fe in the original iron ore2O3The mass fraction is more than or equal to 70 percent.
3. The method for preparing the iron ore oxygen carrier by using the wheat straw ash through wet impregnation modification according to claim 1, wherein K in the wheat straw ash is2The mass fraction of O is more than or equal to 10 percent.
4. The method for preparing the iron ore oxygen carrier by using the wheat straw ash through wet impregnation modification according to claim 1, wherein in the step 2), the temperature of the prepared ash in the muffle furnace is 600-650 ℃, and the calcination time is 2-3 h.
5. The method for preparing the iron ore oxygen carrier by using the wheat straw ash through wet impregnation modification according to claim 1, wherein in the step 3), the temperature of a water bath is 20-25 ℃, and the standing time is 2-3 h.
6. The method for preparing the iron ore oxygen carrier by using the wheat straw ash through wet impregnation modification according to claim 1, wherein the standing time in the step 4) is 20-21 h.
7. The method for preparing the iron ore oxygen carrier by using the wheat straw ash through wet impregnation modification according to the claim 1, wherein in the step 5), the drying temperature in the blast drying oven is 100-105 ℃, and the calcining temperature in the muffle furnace is 900-950 ℃.
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