CN114261992A - Application of glycerol in preparation of chemical looping combustion composite oxygen carrier and preparation method - Google Patents
Application of glycerol in preparation of chemical looping combustion composite oxygen carrier and preparation method Download PDFInfo
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- CN114261992A CN114261992A CN202111599181.0A CN202111599181A CN114261992A CN 114261992 A CN114261992 A CN 114261992A CN 202111599181 A CN202111599181 A CN 202111599181A CN 114261992 A CN114261992 A CN 114261992A
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- oxygen carrier
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- glycerol
- composite oxygen
- chemical looping
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 87
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 80
- 239000001301 oxygen Substances 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000126 substance Substances 0.000 title claims abstract description 21
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000000967 suction filtration Methods 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 235000011187 glycerol Nutrition 0.000 claims abstract 8
- 229910016516 CuFe2O4 Inorganic materials 0.000 claims description 14
- 239000000969 carrier Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- 239000003245 coal Substances 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 6
- 239000012752 auxiliary agent Substances 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of a composite oxygen carrier taking glycerol as an auxiliary agent in a coal chemical looping combustion process. Relates to the preparation of a composite oxygen carrier added with an auxiliary agent, and provides a composite oxygen carrier with higher reaction activity and sintering avoidance. The preparation method of the composite oxygen carrier comprises the following steps: mixing glycerol with deionized water, adding CuO and Fe2O3Stirring and then mechanically mixing to obtain a mixed solution; and carrying out suction filtration on the mixed solution to obtain red precipitate, drying and then calcining to obtain the composite oxygen carrier used in the coal chemical looping combustion process. A chemical looping combustion oxygen carrier which improves mechanical strength through a porous structure formed by glycerin which is an inert carrier after calcination. The invention improves the circulation stability and the reaction activity of the oxygen carrier in the chemical looping combustion process, and has simple and convenient operationSafe and reliable, high industrial value and environment-friendly.
Description
Technical Field
The invention relates to the technical field of composite oxygen carriers, in particular to application of glycerol in preparation of a chemical-looping combustion composite oxygen carrier and a preparation method thereof.
Background
Coal is the fossil fuel with the longest service life, and still remains the main energy support of China for a long time in the future. The clean and efficient utilization and energy conservation and emission reduction of coal resources have important practical significance on the sustainable development of the energy and chemical industry in China. The chemical chain combustion technology of coal has the advantages of reducing loss and realizing CO2Low consumption of trapping and suppression of generation of nitrogen oxides.
In a coal chemical looping combustion reaction system, the oxygen carrier not only has the advantages of good cycle stability, low price, wide source, environmental friendliness and the like, but also needs to have certain mechanical strength and moderate oxidation capacity and catalytic capacity, and can convert pollution elements such as sulfur, nitrogen and the like in a precursor of coal chemical looping combustion into sulfur, nitrogen and NO as far as possible2Equal pollution-free gas and reduced SO2And generation of harmful gases such as NO. At present, most oxygen carriers used at present are copper-based, iron-based, calcium-based and the like, but such a single oxygen carrier has the defects of easy sintering of the copper-based oxygen carrier, low reactivity of the iron-based oxygen carrier, harmful sulfur-containing gas release of the calcium-based oxygen carrier and the like. To overcome the above-mentioned deficiencies of single metal oxygen carriers, composite oxygen carriers have been proposed and used widely, such as CuFe2O4An oxygen carrier.
The mechanical strength and the reactivity are important indexes for evaluating the oxygen carrier, and CuFe2O4The oxygen carrier is a composite oxygen carrier which can effectively promote the combustion process of a coal chemical chain, the defect of sintering of a single copper-based oxygen carrier can be overcome in the reaction process, the reducing capability of the single iron-based oxygen carrier can be enhanced, and the cycle stability and the reaction activity are improved. However, the mechanical strength needs to be improved and improved, but few studies are reported in this respect.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide the application of glycerol in preparing the copper-iron composite oxygen carrier and a preparation method thereof. In the invention, Fe2O3Preparation of oxygen carrier from CuO, and increasing CuFe by adding glycerol2O4Reactivity and mechanical strength of the composite oxygen carrier.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, there is provided the use of glycerol in the preparation of a chemical looping combustion composite oxygen carrier.
Preferably, the chemical looping combustion composite oxygen carrier is CuFe2O4An oxygen carrier.
Preferably, the glycerol is used in an amount to prepare CuFe2O4CuO or Fe of oxygen carriers2O3Are of the same quality.
In a second aspect of the invention, a preparation method of a chemical looping combustion composite oxygen carrier is provided, which comprises the following steps:
(1) adding glycerol into deionized water, and then adding CuO and Fe2O3Stirring and then mechanically mixing to obtain a mixed solution;
(2) and carrying out suction filtration on the mixed solution to obtain red precipitate, drying, and then calcining to obtain the chemical-looping combustion composite oxygen carrier.
Preferably, in the step (1), the mass ratio of the glycerol to the deionized water is 1: 1.
preferably, in step (1), the glycerol, CuO and Fe2O3The mass ratio of (1): 1: 1.
preferably, in step (1), the mechanical mixing is performed by using a colloid mill at a rate of 2000r/min for 20 min.
Preferably, in the step (2), the drying temperature is 150 ℃, and the drying time is 12 h.
Preferably, in the step (2), the heating rate of the calcination is 10 ℃/min, the temperature of the calcination is 950 ℃, and the time of the calcination is 6 h.
The invention has the beneficial effects that:
1. CuFe prepared by the invention2O4The proportion of the composite oxygen carrier is that glycerol is added and the addition amount of the glycerol is adjusted to ensure that CuFe2O4The reactivity, the mechanical strength and the reaction degree with the precursor of the composite oxygen carrier are effectively improved.
2. The oxygen carrier prepared by the method has very good cyclicity and can be recycled. After a plurality of tests, the oxygen carrier is characterized, and CuFe is found2O4The composite oxygen carrier component still exists stably and the surface is not sintered, the conversion rate is still kept above 90 percent, and the addition of the glycerol is beneficial to improving the CuFe2O4The mechanical strength of the composite oxygen carrier can effectively relieve the defects of easy sintering, low reaction activity and the like of a single metal oxygen carrier.
3. The oxygen carrier prepared by the invention has better reduction capability when being doped and compounded with a single metal oxygen carrier, and can be used for mixing Fe2O3Reduction to Fe3O4And the reaction activity is improved. The unit specific surface area and the pore volume of the composite oxygen carrier are highest, and the emission of the polluted gas is controlled after the composite oxygen carrier reacts with the precursor.
4. The preparation method is simple, mild in condition and easy to control; the prepared CuFe has uniform grain diameter, high mechanical strength and better reaction activity2O4And (3) compounding an oxygen carrier.
5. The raw materials of the invention are widely available, the preparation method is simple and easy to operate, the industrial continuous production is convenient to carry out, and the invention has good market prospect. The catalyst is used for direct chemical looping combustion of coal in a fluidized bed, can improve the reaction activity of a precursor and an oxygen carrier, and controls the emission of polluted gas.
Drawings
FIG. 1: CuFe2O4XRD spectrum of (1).
FIG. 2: CuFe2O4XRD spectra before and after multiple cycles of reaction.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background section, CuFe2O4The oxygen carrier can effectively promote the chemical chain combustion of coalThe composite oxygen carrier reduces the sintering of the oxygen carrier in the reaction process and can also enhance the reduction capability of the oxygen carrier, but the mechanical property and the reaction activity of the composite oxygen carrier can not meet the chemical chain combustion of coal.
Based on the situation, the invention aims to provide the application of the glycerol in preparing the coal chemical looping combustion composite oxygen carrier and the preparation method thereof. The invention takes the glycerol as an auxiliary agent and adjusts the glycerol, the CuO and the Fe2O3And mechanically mixed and then calcined to obtain CuFe having a spinel structure2O4. Glycerol as adjuvant for CuO and Fe2O3After treatment, CuFe2O4The oxygen carrier has regular and ordered surface particles and high mechanical strength. And by adding glycerol, CuFe2O4The cycle stability of the oxygen carrier is obviously improved, the sintering of the oxygen carrier is avoided, and the oxygen carrier is a composite oxygen carrier with great potential.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Examples
(1) 50g of glycerol and 150g of deionized water were added to a 500ml beaker, followed by 50g of CuO and 50g of Fe2O3Stirring with a glass rod, slowly and uniformly adding the solution into a colloid mill, and stirring at the speed of 2000r/min for 20min to obtain a mixed solution.
(2) Transferring the mixed solution to a suction filtration device for suction filtration; drying the filtered red precipitate in a 120 ℃ oven for 12 hours; then placing the mixture in a muffle furnace, raising the temperature to 950 ℃ at the speed of 10 ℃/min, and calcining the mixture for 6 hours at constant temperature. Obtaining CuFe with spinel structure2O4An oxygen carrier.
FIG. 1 shows CuFe prepared in this example2O4XRD spectrogram of oxygen carrier, as can be seen from FIG. 1, CuFe is successfully prepared by the method2O4An oxygen carrier.After the oxygen carrier prepared in the embodiment reacts with coal, the reduced product is mainly FeO, and after the oxygen carrier reacts with steam, FeO/Fe reacts with the steam to generate Fe3O4In the presence of CuFe2O4Spinel structure of structure and 35.93 ° in XRD characterization. The phase separation of the crystal diffraction peak is changed into two separate CuO characteristic peaks and Fe2O3Characteristic peak.
Comparative example 1
The difference from the embodiment is that: glycerol, CuO and Fe2O3Is 0.5: 1: 1; the other steps are the same as the embodiment, and CuFe is prepared2O4An oxygen carrier.
Comparative example 2
The difference from the embodiment is that: glycerol, CuO and Fe2O3The mass ratio of (A) to (B) is 2: 1: 1. the other steps are the same as the embodiment, and CuFe is prepared2O4An oxygen carrier.
Comparative example 3
The difference from the embodiment is that: glycerol was replaced by isopropanol. The other steps are the same as the embodiment, and CuFe is prepared2O4An oxygen carrier.
CuFe prepared in examples and comparative examples 1-3 is subjected to self-made fluidized bed2O4And C conversion rate of the oxygen carrier is calculated. Ningxia coal (the main component content of which is shown in table 1) and the composite oxygen carrier prepared by the invention are used as fuels to carry out chemical chain combustion for 30 times, and the carbon conversion rate of the oxygen carrier is shown in table 2.
TABLE 1
Note: the contents in the table are mass fractions.
The calculation formula of the carbon conversion rate is as follows:
wherein phi i is outlet gas in a dry basis state (i is CO and CO respectively)2And CH4) Volume fraction of (d)%; mcoalg, mass of Ningxia coal sample; w is the mass fraction of Ningxia coal-like carbon element,%; q. q.soutIs the total volume flow of the outlet gas in the dry basis state.
TABLE 2
| Item | Carbon conversion% |
| Examples | 91.5 |
| Comparative example 1 | 90.2 |
| Comparative example 2 | 90.6 |
| Comparative example 3 | 90.4 |
It can be seen from table 2 that the carbon conversion of the oxygen carrier prepared in the example is still more than 91% after multiple cycles, which is much higher than that of the oxygen carrier prepared in the comparative example. Fig. 2 is an XRD pattern before and after multiple cycles of the oxygen carrier of the example, and it can be seen that there is substantially no change in the composition of the oxygen carrier after multiple cycles.
The oxygen carrier prepared by the method has high cycle stability and reaction activity in the chemical looping combustion process, is simple and convenient to operate, is safe and reliable, has high industrial value, and is environment-friendly.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (9)
1. The application of glycerol in preparing a composite oxygen carrier.
2. Use according to claim 1, wherein the composite oxygen carrier is CuFe2O4An oxygen carrier.
3. Use according to claim 2, wherein the glycerol is used in amounts and for the preparation of CuFe2O4CuO or Fe of oxygen carriers2O3Are of the same quality.
4. A preparation method of a chemical looping combustion composite oxygen carrier is characterized by comprising the following steps:
(1) adding glycerol into deionized water, and then adding CuO and Fe2O3Stirring and then mechanically mixing to obtain a mixed solution;
(2) and carrying out suction filtration on the mixed solution to obtain red precipitate, drying and then calcining to obtain the combustion composite oxygen carrier.
5. The preparation method according to claim 4, wherein in the step (1), the mass ratio of the glycerol to the deionized water is 1: 1.
6. the production method according to claim 4, wherein in the step (1), the glycerin, CuO and Fe2O3The mass ratio of (1): 1: 1.
7. the method according to claim 4, wherein in the step (1), the mechanical mixing is carried out at a rate of 2000r/min for 20min by using a colloid mill.
8. The preparation method according to claim 4, wherein in the step (2), the drying temperature is 150 ℃ and the drying time is 12 h.
9. The preparation method according to claim 4, wherein in the step (2), the temperature rise rate of the calcination is 10 ℃/min, the temperature of the calcination is 950 ℃, and the time of the calcination is 6 h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111599181.0A CN114261992B (en) | 2021-12-24 | 2021-12-24 | Application of glycerol in preparation of chemical looping combustion composite oxygen carrier and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111599181.0A CN114261992B (en) | 2021-12-24 | 2021-12-24 | Application of glycerol in preparation of chemical looping combustion composite oxygen carrier and preparation method |
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| CN114261992A true CN114261992A (en) | 2022-04-01 |
| CN114261992B CN114261992B (en) | 2024-06-25 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104164273A (en) * | 2014-08-25 | 2014-11-26 | 中国科学院青岛生物能源与过程研究所 | Method for preparing calcium-based oxygen carrier |
| CN112063431A (en) * | 2020-09-16 | 2020-12-11 | 宁夏共宣环保科技有限责任公司 | Preparation method of large-scale magnetic CuFe2O4 oxygen carrier with industrial application |
-
2021
- 2021-12-24 CN CN202111599181.0A patent/CN114261992B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104164273A (en) * | 2014-08-25 | 2014-11-26 | 中国科学院青岛生物能源与过程研究所 | Method for preparing calcium-based oxygen carrier |
| CN112063431A (en) * | 2020-09-16 | 2020-12-11 | 宁夏共宣环保科技有限责任公司 | Preparation method of large-scale magnetic CuFe2O4 oxygen carrier with industrial application |
Non-Patent Citations (1)
| Title |
|---|
| 廖艳芬等: "基于铁基载氧体的稻秆水蒸气气化特性", 华南理工大学学报（自然科学版）, vol. 48, no. 2, 29 February 2020 (2020-02-29), pages 31 * |
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