CN108067180B - Yttrium magnesium-calcium based CO2Adsorbent and preparation method thereof - Google Patents
Yttrium magnesium-calcium based CO2Adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses yttrium magnesium-calcium based CO2Adsorbent and preparation method thereof, the yttrium magnesium-calcium based CO2The adsorbent comprises the following chemical components in percentage by mass: 40-80% of CaO and the balance of Y2O3And MgO, wherein Y2O3And the MgO content does not differ by more than 5%; and is prepared by a sol-gel method and high-temperature calcination. Yttrium magnesium-calcium based CO prepared by adopting the process2The adsorbent has large pore volume, high activity, uniform and dispersed crystal grains, and high CO content2MgO in the adsorbent has better promotion effect on physical parameters of the calcium-based adsorbent, and CO2Y in the adsorbent2O3Has better stabilizing effect on the physical structure of the calcium-based adsorbent, so the yttrium magnesium-calcium-based CO2The adsorbent has high-efficiency and stable carbon dioxide cyclic absorption/desorption capacity. Yttrium magnesium-calcium based CO2The adsorbent is suitable for a combined synergistic process of carbon dioxide capture by a calcium-based adsorbent adsorption method and enhanced hydrogen production by chemical-looping reforming, and has the characteristics of high adsorption efficiency, good cycle stability and the like.
Description
Technical Field
The invention belongs to the technical field of adsorption and separation of carbon dioxide by using a solid adsorbent, and particularly relates to a method suitable for calcium cycle CO2Cyclic stabilized yttrium magnesium-calcium based CO of capture process2An adsorbent and a preparation method thereof.
Background
According to the report of climate change organization between governments, global warming is mainly caused by CO caused by human activities2The main greenhouse gas emission is caused by the aggravation of the global warming effect. In our country's electric power production using coal as the main energy source, CO produced by burning coal2The emission being CO2The maximum point source discharge, thereby controlling and slowing the CO in the coal-electricity production of China2The emission of (A) has important significance for relieving global warming and greenhouse effect.
In recent years, carbon dioxide capture and storage technology (CCS) has been rapidly developed, and has become an important technology for alleviating greenhouse gas emissions. CCS technology, i.e. separation and capture of CO emitted during energy production2And the captured CO is removed2Storing in geological reservoirs or injecting into deep sea. Among the technical solutions for capturing carbon dioxide, solid is adoptedSeparation of CO from flue gas by bulk adsorbent2Compared with the mature amine adsorption method at the present stage, the technology has the advantage of economical efficiency and is considered as one of the important development directions in the future; the calcium-based adsorbent has wide source and low cost, and can treat CO2Has large adsorption capacity, so the method (CaL) of cyclic carbonation/calcination of calcium-based adsorbent is used for separating CO from flue gas2Are gaining increasing attention from researchers. However, CO in the captured flue gas is separated with CaL2The technology of (2) is increasingly valued by many researchers, CaO adsorbs CO2The law that the capacity of the adsorbent changes along with the increase of CaL times is widely concerned, and all research results show that natural calcium-based adsorbents adsorb CO2The conversion of (a) decreases sharply with increasing number of cycles. This problem would greatly reduce the economics and stability of the CaL technology, thereby limiting its large-scale industrial application to some extent. The problem of the rapid decrease of the conversion rate with the number of cycles has been widely studied so far, and a large number of techniques and methods for enhancing and stabilizing the adsorption capacity of the calcium-based adsorbent, such as steam activation, high-temperature pretreatment, acidification pretreatment, etc., have not yet been able to effectively solve the problem of the rapid decrease of the conversion rate with the number of cycles. Based on the current situation, the technology of metal-doped modified calcium-based adsorbent becomes a research focus and a hot spot, and the problem that the conversion rate is sharply reduced along with the cycle number can be effectively solved by reasonably applying metal doping to prepare the synthetic calcium-based adsorbent. The more used metal at present is Al2O3、MgO、SiO2、TiO2、Nd2O3、CeO2、ZrO2And the like. Y in comparison with other metal oxides2O3When the yttrium-doped calcium-based rare earth yttrium-doped rare earth element is used as a doped metal synthetic calcium-based adsorbent, the adsorption efficiency and stability of the synthetic calcium-based adsorbent can be greatly improved, but the yttrium-doped rare earth element is high in cost and is doped with a large amount of Y2O3The synthetic calcium-based adsorbents would not meet the objective of efficiently and economically adsorbing and separating carbon dioxide, thereby greatly reducing the economics of the overall CaL process.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, the present invention providesYttrium magnesium-calcium-based CO with high adsorption efficiency and high cycle stability2An adsorbent.
The invention also provides the yttrium magnesium-calcium based CO2A preparation method of the adsorbent.
The invention adopts the following technical scheme:
yttrium magnesium-calcium based CO2The adsorbent comprises the following chemical components in percentage by mass: 40-80% of CaO and the balance of Y2O3And MgO, wherein Y2O3And the content of MgO does not differ by more than 5%.
Furthermore, the invention also provides yttrium magnesium-calcium based CO2The preparation method of the adsorbent comprises the following steps:
1) respectively dripping soluble yttrium salt solution and soluble magnesium salt solution into soluble calcium salt solution, and stirring until the soluble yttrium salt solution and the soluble magnesium salt solution are uniformly mixed; wherein the soluble yttrium salt solution, soluble magnesium salt solution, soluble calcium salt solution are used in an amount according to Y in claim 1 or 22O3Determining the quality of MgO and CaO; the concentrations of the soluble yttrium salt solution, the soluble magnesium salt solution and the soluble calcium salt solution are the same and are all 2.40-2.60 mol/L;
2) dropwise adding the mixed solution obtained in the step 1) into a citric acid monohydrate solution, and stirring at the temperature of 80-90 ℃ for 5-7 hours until gel is formed; the concentration of the citric acid monohydrate solution is 4.0-6.0 mol/L; the dosage of the citric acid monohydrate solution is determined according to the molar quantity of the metal cations/the molar quantity of the citric acid monohydrate being 1.6-1.8;
3) placing the gel obtained in the step 2) in air at room temperature for 20-24 hours, then heating at 80-100 ℃ for 6-7 hours, and finally heating at 105-115 ℃ for 40-48 hours until a dry gel is formed;
4) placing the dried gel obtained in the step 3) in a muffle furnace, and calcining for 1-2 hours at 800-900 ℃ until the organic matters are fully combusted and the nitrates are completely decomposed;
5) grinding and sieving the combusted particles to obtain yttrium magnesium-calcium based CO2An adsorbent.
Further, the concentrations of the soluble yttrium salt solution, the soluble magnesium salt solution and the soluble calcium salt solution in the step 1) are all 2.50 mol/L.
Further, the concentration of the citric acid monohydrate solution in the step 2) is 5.00 mol/L.
Compared with the prior art, the invention has the following beneficial effects:
1. yttrium magnesium-calcium based CO2The adsorbent has unique formula, and is prepared by introducing Y and Mg oxide, wherein in Y2O3Can prevent adsorbent CO2The microcrystal grows and condenses, and soluble Y salt and magnesium salt can generate a large amount of gas to improve the CO adsorbent in the preparation process2Specific surface area and void volume, thereby making yttrium magnesium-calcium based CO2Specific surface area, pore volume of the adsorbent,<The mesoporous proportion of 20nm, the reaction activity and the cycling stability are greatly improved. The yttrium magnesium-calcium based CO of the invention2In the adsorbent, MgO and Y2O3As a metal doping component, wherein MgO has a better effect of improving the physical parameters of the calcium-based adsorbent, and CO2Y in the adsorbent2O3Has good stabilizing effect on the physical mechanism of the calcium-based adsorbent, stabilizes the physical structure and the pore structure in the calcium circulation process, and more efficiently adsorbs CO2(ii) a Relative to yttrium-calcium based CO2Adsorbent, yttrium magnesium-calcium based CO2The adsorbent not only greatly reduces the yttrium-calcium based CO by adding a proper amount of conventional metal2The cost of the adsorbent is greatly increased, and meanwhile, the CO is greatly increased2Chemical reaction activity, specific surface area, pore volume and pore volume of the adsorbent,<The mesoporous ratio of 20 nm. In contrast to magnesium-calcium based CO2Adsorbent, yttrium magnesium-calcium based CO2The adsorbent not only has better circulation stability, but also improves CO higher2CO of adsorbent2The adsorption capacity and the chemical reaction activity are most prominent, and the CO is greatly improved2Specific surface area, pore volume of the adsorbent,<The mesoporous ratio of 20 nm. Thus, yttrium magnesium-calcium based CO2The adsorbent has excellent chemical reaction activity and CO2Adsorption/desorption efficiency and cycle stability, and better economy.
2. The invention is madeThe preparation method has good manufacturability and is easy to control. Adding MgO and Y to calcium-based adsorbent2O3Then, by a sol-gel method, on the basis of a large number of creative experiments, optimal reaction conditions are obtained, and the reaction conditions are strictly controlled, so that the yttrium magnesium-calcium based CO with uniform particle size, good dispersity and good reaction activity is prepared2An adsorbent.
3. The raw materials of the invention are widely and easily available, the preparation method is simple and easy to operate, the sol-gel method can be used for preparation, the wet mixing, the equal volume impregnation and other methods can be adopted for preparation, the industrial continuous production is convenient to carry out, and the market prospect is good.
4. Calcium removal circulating CO2Outside the capture process, the yttrium magnesium-calcium based CO2The adsorbent also has good application potential in the chemical chain reforming enhanced hydrogen production process. The decomposition reaction of calcium carbonate is mainly exothermic in the process, so that the energy requirement in the chemical chain process can be reduced, and the energy consumption is reduced.
Drawings
FIG. 1 shows limestone, dolomite and yttrium magnesium-calcium based CO prepared according to example 1 of the present invention2Comparison of adsorption efficiency of adsorbents;
FIG. 2 shows a yttrium magnesium-calcium based CO prepared in example 1 of the present invention2Cycling stability profile of the adsorbent;
FIG. 3 is a yttrium magnesium-calcium based CO of the present invention2Physical structure parameter diagram of the adsorbent: FIG. 3 (a) shows three yttrium magnesium-calcium based COs prepared by three examples of the present invention2A sorbent specific surface area map; FIG. 3 (b) shows three yttrium magnesium-calcium based COs prepared by three examples of the present invention2Adsorbent pore volume graph; FIG. 3 (c) shows three yttrium magnesium-calcium based COs prepared by three examples of the present invention2Adsorbent average particle size diagram.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings, in which the starting material is analytically pure Y (NO)3)3•6H2O、Mg(NO3)2•6H2O and Ca (NO)3)3•4H2O, the product complexing agent is analytically pure citric acid monohydrate with the molecular formula of C6H8O7﹒H2O。
One, one kind of yttrium magnesium-calcium based CO2Method for preparing adsorbent
Example 1
Taking 6.40 g Mg (NO)3)2•6H2Placing the O into a 50 mL beaker, adding 10 mL deionized water, and then placing the beaker on a magnetic stirrer with a constant-temperature water bath for stirring; weighing 3.37g Y (NO)3)3•6H2Adding O into a 10 mL beaker, adding 3.5 mL deionized water and stirring; 12.64g Ca (NO) are weighed out3)3•4H2Adding O into a 100 mL beaker, adding 21.4 mL deionized water and stirring; mixing Y (NO)3)3•6H2O solution and Mg (NO)3)2•6H2Adding O solution dropwise to Ca (NO)3)3•4H2And stirring the mixture in the O solution until the mixture is uniformly mixed. Adding 10.50 g of citric acid monohydrate into a 50 mL beaker, adding 10 mL of deionized water, stirring until the citric acid monohydrate is completely dissolved, and adding Mg (NO)3)2•6H2O、Y(NO3)3•6H2O and Ca (NO)3)3•4H2And dropwise adding the mixed solution of O into the citric acid monohydrate solution, stirring the mixed solution at the temperature of 80 ℃ for 7 hours to form gel, and then placing the gel at room temperature for 22 hours to form wet gel. The wet gel was heated at 90 ℃ for 6 hours and then at 110 ℃ for 48 hours to form a xerogel. Taking out the dried gel, calcining the dried gel in a muffle furnace at 900 ℃ for 1.5 hours to completely decompose nitrate and citric acid monohydrate to finally form yttrium magnesium-calcium based CO2An adsorbent.
Yttrium magnesium-calcium based CO prepared as described in example 1 above2The adsorbent comprises the following components in parts by weight: with Y2O320 portions of stable structural components; MgO is used as an active structural component and accounts for 20 parts; the absorbent CaO accounts for 60 parts.
Example 2
3.20 g of Mg (NO) was taken3)2•6H2Placing the O into a 20 mL beaker, adding 5 mL deionized water, and then placing the beaker on a magnetic stirrer with a constant-temperature water bath for stirring; weighing 1.69g Y (NO)3)3•6H2Adding O into a 5 mL beaker, adding 1.76mL of deionized water and stirring; 16.85g Ca (NO) are weighed out3)3•4H2Adding O into a 50 mL beaker, adding 28.6 mL deionized water and stirring; mixing Y (NO)3)3•6H2O solution and Mg (NO)3)2•6H2Adding O solution dropwise to Ca (NO)3)3•4H2And stirring the mixture in the O solution until the mixture is uniformly mixed. 10.52 g of citric acid monohydrate was added to a 50 mL beaker, 10 mL of deionized water was added and stirred until the citric acid monohydrate was completely dissolved, and Mg (NO) was added3)2•6H2O、Y(NO3)3•6H2O and Ca (NO)3)3•4H2And dropwise adding the mixed solution of O into the citric acid monohydrate solution, stirring the mixed solution at the temperature of 80 ℃ for 7 hours to form gel, and then placing the gel at room temperature for 22 hours to form wet gel. The wet gel was heated at 90 ℃ for 6 hours and then at 110 ℃ for 48 hours to form a xerogel. Taking out the dried gel, calcining the dried gel in a muffle furnace at 900 ℃ for 1.5 hours to completely decompose nitrate and citric acid monohydrate to finally form yttrium magnesium-calcium based CO2An adsorbent.
Yttrium magnesium-calcium based CO prepared as described in example 2 above2The adsorbent comprises the following components in parts by weight: with Y2O310 portions of stable structural components; MgO is used as an active structural component and accounts for 10 parts; the absorbent CaO accounts for 80 parts.
Example 3
Collecting 9.60 g Mg (NO)3)2•6H2Placing the O into a 20 mL beaker, adding 15 mL deionized water, and then placing the beaker on a magnetic stirrer with a constant-temperature water bath for stirring; weighing 5.07g Y (NO)3)3•6H2Adding O into a 10 mL beaker, adding 5.3mL deionized water and stirring; 8.43g Ca (NO) was weighed3)3•4H2O is added toAdding 14.3 mL of deionized water into a 50 mL beaker, and stirring; mixing Y (NO)3)3•6H2O solution and Mg (NO)3)2•6H2Adding O solution dropwise to Ca (NO)3)3•4H2And stirring the mixture in the O solution until the mixture is uniformly mixed. 10.38 g of citric acid monohydrate was added to a 50 mL beaker, 10 mL of deionized water was added and stirred until the citric acid monohydrate was completely dissolved, and Mg (NO) was added3)2•6H2O、Y(NO3)3•6H2O and Ca (NO)3)3•4H2And dropwise adding the mixed solution of O into the citric acid monohydrate solution, stirring the mixed solution at the temperature of 80 ℃ for 7 hours to form gel, and then placing the gel at room temperature for 22 hours to form wet gel. The wet gel was heated at 90 ℃ for 6 hours and then at 110 ℃ for 48 hours to form a xerogel. Taking out the dried gel, calcining the dried gel in a muffle furnace at 900 ℃ for 1.5 hours to completely decompose nitrate and citric acid monohydrate to finally form yttrium magnesium-calcium based CO2An adsorbent.
Yttrium magnesium-calcium based CO prepared as described in example 3 above2The adsorbent comprises the following components in parts by weight: with Y2O330 portions of stable structure components; MgO is used as an active structural component and accounts for 30 parts; 40 parts of absorbent CaO.
Di, Y magnesium-calcium based CO2Characterization and Performance testing of adsorbents
1. Yttrium magnesium-calcium based CO2Characterization of the adsorbents
Yttrium magnesium-calcium based CO prepared as described above2The adsorbent was subjected to specific surface area, pore volume and particle size distribution tests, and the results are shown in fig. 3. FIG. 3 (a) shows three yttrium magnesium-calcium based COs2The specific surface area of the adsorbent is shown, and the yttrium magnesium-calcium based CO obtained by the preparation method of the invention can be seen from the specific surface area2The specific surface areas of the adsorbents are all 23m3More than g; FIG. 3 (b) shows three yttrium magnesium-calcium based COs2Pore volume diagram of adsorbent, from which it can be seen that yttrium magnesium-calcium based CO obtained by the preparation method of the present invention2The pore volumes of the adsorbents are all 0.08cm3More than g; FIG. 3 (c) shows three yttrium magnesium-calcium based CO2The average particle size of the adsorbent is shown in the figure, and the yttrium magnesium-calcium based CO obtained by the preparation method of the invention can be seen from the figure2Average particle diameter of adsorbent<20 nm. The numbers 1, 2 and 3 on the abscissa of the figure correspond to the adsorbents prepared in examples 1 to 3.
2. Yttrium magnesium-calcium based CO2Performance testing of the adsorbents
To verify the yttrium magnesium-calcium based CO obtained by the preparation method of the present invention2Adsorbent pair CO2Has higher adsorption and cycling stability, and the results of the reaction activity and stability tests are shown in figure 1 and figure 2. FIG. 1 shows the combination of limestone, dolomite and Yttrium magnesium-calcium based CO prepared in example 12FIG. 1 shows the adsorption efficiency of the adsorbent, and the yttrium magnesium-calcium based CO prepared by the present invention is compared with limestone and dolomite2Adsorbent pair CO2The adsorption efficiency is higher; FIG. 2 is a yttrium magnesium-calcium based CO prepared in example 12The cycle stability chart of the adsorbent can be seen, and the yttrium magnesium-calcium based CO prepared by the invention2The adsorbent has good cycle stability.
In conclusion, the yttrium magnesium-calcium based CO prepared by the invention2Adsorbent, mainly composed of Y2O3MgO and CaO. In the synthetic adsorbent, MgO has better promotion effect on the physical parameters of the calcium-based adsorbent, and Y2O3Has better stabilizing effect on the physical mechanism of the calcium-based adsorbent, thereby obtaining the specific surface area, the pore volume,<20nm of yttrium magnesium-calcium based CO with good mesoporous proportion, good reaction activity and good cycling stability2An adsorbent.
In particular, the above cases are only preferred embodiments of the present invention, and the present invention can also replace the specific operation steps and various reactants in the above-mentioned methods. Therefore, all equivalent changes, which can be made by using the description and drawings of the present invention and directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (3)
1. Yttrium magnesium-calcium based CO2An adsorbent characterized by comprising the following massThe chemical components in percentage by weight are as follows: CaO 60%, Y2O320% of MgO and 20% of MgO;
the preparation method comprises the following steps:
1) respectively dripping soluble yttrium salt solution and soluble magnesium salt solution into soluble calcium salt solution, and stirring until the soluble yttrium salt solution and the soluble magnesium salt solution are uniformly mixed; wherein the dosage of the soluble yttrium salt solution, the soluble magnesium salt solution and the soluble calcium salt solution is Y2O3Determining the quality of MgO and CaO; the concentrations of the soluble yttrium salt solution, the soluble magnesium salt solution and the soluble calcium salt solution are the same and are all 2.50 mol/L;
2) dropwise adding the mixed solution obtained in the step 1) into a citric acid monohydrate solution, and stirring at the temperature of 80-90 ℃ for 5-7 hours until gel is formed; the concentration of the citric acid monohydrate solution is 4.0-6.0 mol/L; the dosage of the citric acid monohydrate solution is determined according to the molar quantity of the metal cations/the molar quantity of the citric acid monohydrate being 1.6-1.8;
3) placing the gel obtained in the step 2) in air at room temperature for 20-24 hours, then heating at 80-100 ℃ for 6-7 hours, and finally heating at 105-115 ℃ for 40-48 hours until a dry gel is formed;
4) placing the dried gel obtained in the step 3) in a muffle furnace, and calcining for 1-2 hours at 800-900 ℃ until the organic matters are fully combusted and the nitrates are completely decomposed;
5) grinding and sieving the combusted particles to obtain yttrium magnesium-calcium based CO2An adsorbent.
2. Yttrium magnesium-calcium based CO according to claim 12Adsorbent, characterized in that the concentration of the citric acid monohydrate solution in step 2) is 5.00 mol/L.
3. Yttrium magnesium-calcium based CO as claimed in claim 1 or 22The application of the adsorbent is characterized in that the adsorbent adsorbs carbon dioxide generated in a chemical-looping reforming enhanced hydrogen production process.
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| CN102416315A (en) * | 2010-09-28 | 2012-04-18 | 北京有色金属研究总院 | Magnesium-containing rare earth oxygen storage material and preparation method thereof |
| CN102784630A (en) * | 2012-07-25 | 2012-11-21 | 华中科技大学 | Preparation method for calcium-based CO2 sorbent |
| CN103785347A (en) * | 2012-10-30 | 2014-05-14 | 北京低碳清洁能源研究所 | Composite oxide adsorbent for adsorption of medium/high temperature CO2 |
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| CN102416315A (en) * | 2010-09-28 | 2012-04-18 | 北京有色金属研究总院 | Magnesium-containing rare earth oxygen storage material and preparation method thereof |
| CN102784630A (en) * | 2012-07-25 | 2012-11-21 | 华中科技大学 | Preparation method for calcium-based CO2 sorbent |
| CN103785347A (en) * | 2012-10-30 | 2014-05-14 | 北京低碳清洁能源研究所 | Composite oxide adsorbent for adsorption of medium/high temperature CO2 |
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