CN114261992B - 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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- CN114261992B CN114261992B CN202111599181.0A CN202111599181A CN114261992B CN 114261992 B CN114261992 B CN 114261992B CN 202111599181 A CN202111599181 A CN 202111599181A CN 114261992 B CN114261992 B CN 114261992B
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- oxygen carrier
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- looping combustion
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 79
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 75
- 239000001301 oxygen Substances 0.000 title claims abstract description 75
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002485 combustion reaction Methods 0.000 title abstract description 21
- 239000000126 substance Substances 0.000 title abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052596 spinel Inorganic materials 0.000 claims description 5
- 239000011029 spinel Substances 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 235000011187 glycerol Nutrition 0.000 abstract description 23
- 239000003245 coal Substances 0.000 abstract description 18
- 230000009257 reactivity Effects 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000969 carrier Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 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
- 238000002441 X-ray diffraction Methods 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
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 229910004013 NO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 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
- 230000001351 cycling effect Effects 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
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 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
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- Catalysts (AREA)
- 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 catalyst with higher reactivity and sintering avoidance. The preparation method of the composite oxygen carrier comprises the following steps: mixing glycerol with deionized water, adding CuO and Fe 2O3, stirring, and mechanically mixing to obtain a mixed solution; and (3) carrying out suction filtration on the mixed solution to obtain red precipitate, drying and calcining to obtain the composite oxygen carrier used in the coal chemical looping combustion process. The porous structure formed by the glycerin as an inert carrier after calcination improves the mechanical strength of the chemical-looping combustion oxygen carrier. The invention improves the circulation stability and the reaction activity of the oxygen carrier in the chemical looping combustion process, has simple and convenient operation, safety and reliability, higher industrial value and environmental protection.
Description
Technical Field
The invention relates to the technical field of composite oxygen carriers, in particular to application of glycerol in preparing a chemical looping combustion composite oxygen carrier and a preparation method thereof.
Background
Coal is fossil fuel with longest service time, and is still a main energy prop in China for a long time in the future. The clean and efficient utilization of coal resources, energy conservation and emission reduction have important practical significance for sustainable development of the energy chemical industry in China. The chemical-looping combustion technology of coal has the advantages of reducing loss, realizing low-consumption trapping of CO 2 and simultaneously inhibiting the generation of nitrogen oxides.
In the coal chemical looping combustion reaction system, the oxygen carrier has the advantages of good circulation stability, low price, wide sources, environmental friendliness and the like, and also is required to have certain mechanical strength, moderate oxidizing capacity and catalytic capacity, SO that the pollution elements such as sulfur, nitrogen and the like in the precursor of the coal chemical looping combustion can be converted into pollution-free gases such as sulfur, nitrogen compounds and NO 2 as much as possible, and the generation of harmful gases such as SO 2 and NO is reduced. The most used oxygen carriers at present are copper-based, iron-based, calcium-based and the like, but the single oxygen carrier has the defects that the copper-based oxygen carrier is easy to sinter, the iron-based oxygen carrier has lower reactivity, and the calcium-based oxygen carrier releases harmful sulfur-containing gas and the like. In order to overcome the above-described deficiencies of single metal oxygen carriers, composite oxygen carriers have been widely proposed and used, such as CuFe 2O4 oxygen carriers.
The mechanical strength and the reactivity are important indexes for evaluating the oxygen carrier, and the CuFe 2O4 oxygen carrier is used as a composite oxygen carrier capable of effectively promoting the coal chemical looping combustion process, so that the defect of sintering of a single copper-based oxygen carrier can be overcome in the reaction process, the reducing capacity of the single iron-based oxygen carrier can be enhanced, and the cycle stability and the reactivity can be improved. However, the mechanical strength is required 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 an application of glycerol in preparing a copper-iron composite oxygen carrier and a preparation method thereof. The invention prepares the oxygen carrier by Fe 2O3/CuO, and improves the reactivity and the mechanical strength of the CuFe 2O4 composite oxygen carrier by adding glycerol.
In order to achieve the above 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 a CuFe 2O4 oxygen carrier.
Preferably, the glycerol is used in the same amount as CuO or Fe 2O3 for preparing the CuFe 2O4 oxygen carrier.
In a second aspect of the present invention, a method for preparing a chemical looping combustion composite oxygen carrier is provided, comprising the steps of:
(1) Adding glycerol into deionized water, adding CuO and Fe 2O3, stirring, and mechanically mixing to obtain a mixed solution;
(2) And (3) carrying out suction filtration on the mixed solution to obtain red precipitate, drying and 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 the step (1), the mass ratio of the glycerol to the CuO to the Fe 2O3 is 1:1:1.
Preferably, in step (1), the mechanical mixing is mechanical mixing at a rate of 2000r/min for 20min using a colloid mill.
Preferably, in the step (2), the temperature of the drying is 150 ℃ and the drying time is 12 hours.
Preferably, in the step (2), the temperature rising rate of the calcination is 10 ℃/min, the calcination temperature is 950 ℃, and the calcination time is 6h.
The invention has the beneficial effects that:
1. the CuFe 2O4 composite oxygen carrier prepared by the invention has the advantages that the reaction activity, the mechanical strength and the reaction degree with the precursor of the CuFe 2O4 composite oxygen carrier are effectively improved by adding the glycerol and adjusting the addition amount of the glycerol.
2. The oxygen carrier prepared by the invention has good circularity and can be recycled. After multiple tests, the oxygen carrier is characterized, and the defects that the CuFe 2O4 composite oxygen carrier is easy to sinter, low in reactivity and the like are effectively overcome, and the CuFe 2O4 composite oxygen carrier is stable in component and not sintered on the surface, and the conversion rate is still kept above 90%.
3. The oxygen carrier prepared by the method has better reducing capability when a single metal oxygen carrier is doped and compounded, and can reduce Fe 2O3 into Fe 3O4 to improve the reactivity. The unit specific surface area and pore volume of the composite oxygen carrier are the highest, and the emission of polluted gas after the reaction with the precursor is controlled.
4. The preparation method is simple and convenient, mild in condition and easy to control; the CuFe 2O4 composite oxygen carrier with uniform particle size, high mechanical strength and better reactivity is prepared.
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, 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 reactivity of a precursor and an oxygen carrier, and can control the discharge of polluted gas.
Drawings
Fig. 1: XRD spectra of CuFe 2O4.
Fig. 2: XRD patterns of CuFe 2O4 before and after multiple cycling reactions.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. 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, the CuFe 2O4 oxygen carrier is used as a composite oxygen carrier capable of effectively promoting the chemical looping combustion process of coal, reducing the sintering of the oxygen carrier in the reaction process and enhancing the reducing capability of the oxygen carrier, but the mechanical property and the reaction activity of the oxygen carrier cannot meet the chemical looping combustion of coal.
Based on the above, the invention aims to provide an application of glycerol in preparing a coal chemical looping combustion composite oxygen carrier and a preparation method thereof. According to the invention, the CuFe 2O4 with a spinel structure is obtained by taking the glycerol as an auxiliary agent, adjusting the mass ratio of the glycerol to CuO to Fe 2O3, and mechanically mixing the mixture and then calcining the mixture. After the CuO and the Fe 2O3 are treated by using the glycerol as an auxiliary agent, the surface particles of the CuFe 2O4 oxygen carrier are regular and ordered, and the mechanical strength is high. And by adding glycerol, the circulation stability of the CuFe 2O4 oxygen carrier is obviously improved, and the oxygen carrier is prevented from being sintered, so that the composite oxygen carrier has a very potential.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present application, the technical scheme of the present application will be described in detail with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and are commercially available.
Examples
(1) 50G of glycerin and 150g of deionized water were added to a 500ml beaker, and then 50gCuO and 50g of Fe 2O3 were added thereto, and stirred with a glass rod, and then the above solution was slowly and uniformly added to a colloid mill, and stirred at a rate of 2000r/min for 20min, to obtain a mixed solution.
(2) Transferring the mixed solution to a suction filtration device for suction filtration; placing the red precipitate after suction filtration in a baking oven at 120 ℃ for drying for 12 hours; then the mixture is put into a muffle furnace to be heated to 950 ℃ at the speed of 10 ℃/min and calcined for 6 hours at constant temperature. The CuFe 2O4 oxygen carrier with spinel structure is obtained.
Fig. 1 is an XRD spectrum of the CuFe 2O4 oxygen carrier prepared in this example, and as can be seen from fig. 1, the CuFe 2O4 oxygen carrier was successfully prepared by the above method. After the oxygen carrier prepared in the example is reacted with coal, the reduced product is mainly FeO, and after the reaction with steam, feO/Fe reacts with steam to generate Fe 3O4, and a spinel structure body with a CuFe 2O4 structure exists and 35.93 degrees is represented by XRD. The phase separation of the diffraction peaks of the crystals occurs and becomes two separate CuO characteristic peaks and Fe 2O3 characteristic peaks.
Comparative example 1
The difference from the examples is that: the mass ratio of the glycerol to the CuO to the Fe 2O3 is 0.5:1:1, a step of; the rest steps are the same as those of the example, and the CuFe 2O4 oxygen carrier is prepared.
Comparative example 2
The difference from the examples is that: the mass ratio of the glycerol to the CuO to the Fe 2O3 is 2:1:1. the rest steps are the same as those of the example, and the CuFe 2O4 oxygen carrier is prepared.
Comparative example 3
The difference from the examples is that: glycerol was replaced with isopropanol. The rest steps are the same as those of the example, and the CuFe 2O4 oxygen carrier is prepared.
The conversion of C was calculated for the CuFe 2O4 oxygen carriers prepared in examples and comparative examples 1 to 3 using a self-made fluidized bed. The chemical looping combustion is carried out for 30 times by adopting Ningxia coal (the main component content of the Ningxia coal is shown in table 1) and the composite oxygen carrier prepared by the invention as fuel, and the carbon conversion rate of the oxygen carrier is shown in table 2.
TABLE 1
Note that: the contents in the table are mass fractions.
Calculation formula of carbon conversion:
Wherein phi is the volume fraction,%; m coal is the mass of the Ningxia coal sample, g; w is the mass fraction of carbon element of the Ningxia coal sample,%; q out is the total outlet gas volume flow in dry state.
TABLE 2
| Project | Carbon conversion% |
| Examples | 91.5 |
| Comparative example 1 | 90.2 |
| Comparative example 2 | 90.6 |
| Comparative example 3 | 90.4 |
As can be seen from Table 2, the oxygen carrier prepared in the examples still had a carbon conversion of greater than 91% after multiple cycles, which is much higher than that of the oxygen carrier prepared in the comparative examples. Fig. 2 is an XRD pattern of the oxygen carrier of the example before and after multiple cycles, and it can be seen that the material composition of the oxygen carrier is substantially unchanged after multiple cycles.
The oxygen carrier prepared by the method has high cycle stability and reactivity in the chemical looping combustion process, is simple and convenient to operate, is safe and reliable, has higher industrial value and is environment-friendly.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (1)
1. The application of glycerol as an auxiliary agent in improving the carbon conversion rate of the prepared composite oxygen carrier, wherein the composite oxygen carrier is a CuFe 2O4 oxygen carrier, and the crystal phase is a spinel phase; the dosage of the glycerol is the same as the mass of CuO or Fe 2O3 for preparing the CuFe 2O4 oxygen carrier;
the CuFe 2O4 oxygen carrier is prepared by the following method:
(1) Adding 50g of glycerol and 150g of deionized water into a 500mL beaker, adding 50gCuO g of Fe 2O3, stirring with a glass rod, slowly and uniformly adding the solution into a colloid mill, and stirring at a speed of 2000r/min for 20min to obtain a mixed solution;
(2) Transferring the mixed solution to a suction filtration device for suction filtration; placing the red precipitate after suction filtration in a baking oven at 120 ℃ for drying for 12 hours; then placing the mixture into a muffle furnace, heating to 950 ℃ at a speed of 10 ℃/min, and calcining for 6 hours at constant temperature to obtain the CuFe 2O4 oxygen carrier with spinel structure.
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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 |
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| 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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| Publication Number | Publication Date |
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| CN114261992A CN114261992A (en) | 2022-04-01 |
| CN114261992B true 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 |
|---|
| 基于铁基载氧体的稻秆水蒸气气化特性;廖艳芬等;华南理工大学学报（自然科学版）;20200229;第48卷(第2期);第31页 * |
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