CN114887583B - Mesoporous alumina loaded Cu 2 Preparation method of O adsorbent - Google Patents

Mesoporous alumina loaded Cu 2 Preparation method of O adsorbent Download PDF

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CN114887583B
CN114887583B CN202210454170.1A CN202210454170A CN114887583B CN 114887583 B CN114887583 B CN 114887583B CN 202210454170 A CN202210454170 A CN 202210454170A CN 114887583 B CN114887583 B CN 114887583B
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adsorbent
mesoporous alumina
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吴昊阳
王倩玉
秦明礼
李子宜
贾宝瑞
曲选辉
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University of Science and Technology Beijing USTB
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    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
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    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
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Abstract

Mesoporous alumina loaded Cu 2 A preparation method of an O adsorbent belongs to the technical field of gas purification. The adsorbent is prepared by gamma-Al 2 O 3 The physical adsorption of (C) and pi complex chemical adsorption of Cu (I) are synergistic to adsorb and purify CO, and the excellent CO adsorption capacity is shown. The invention provides a simple and extensible synthesis method for developing the CO adsorbent with large working capacity and high selectivity, and the production process is environment-friendly, pollution-free, low in operation cost and high in economic benefit, and has better industrial application prospect.

Description

Mesoporous alumina loaded Cu 2 Preparation method of O adsorbent
Technical Field
The invention belongs to the technical field of gas purification, and in particular relates to a mesoporous alumina loaded Cu 2 O adsorbent and its preparation method.
Background
Carbon monoxide (CO) is a widely distributed pollutant in the atmosphere and is easily produced due to incomplete combustion of carbonaceous materials in coal furnaces, gas water heaters, automotive engines and cigarettes. In many cases, CO is generally not noticeable due to its colorless and odorless nature, and poses many hazards to the ecological environment and human health. CO is fast combined with hemoglobin to reduce oxygen content in blood, so that tissue is anoxic and has high toxicity to human body. At least 15200 people in the united states are reported to need hospitalization for CO poisoning each year. In addition, CO is widely used in the chemical industry as a valuable raw material for the production of various chemicals such as methanol, phosgene, formic acid, acetic acid, ethylene glycol, and polyurethane foam. However, although the source of CO is broad, it is generally CO-derived 2 、H 2 O、N 2 、CH 4 And H 2 Such impurity gases exist as mixed gases, and these CO-containing gases cannot be directly used for synthesis of chemicals. Thus, from various gasesThe selective capture of CO in the mixture is critical to the impact of environmental health and economic benefits. Currently, mature technologies for separating CO rely primarily on cryogenic distillation, absorption and adsorption processes. Among them, adsorption is receiving a great deal of attention because of its efficient operation and low energy costs, but the success of adsorption technology depends on the development of efficient adsorption materials. However, the adsorption properties of widely studied CO adsorbent materials, such as Activated Carbon (AC), zeolite, molecular sieve, metal oxide and metal organic frameworks, are not ideal. Thus, developing materials with high CO selectivity, large CO working capacity, and high stability remains very challenging.
Physical adsorption is a weak adsorption process by van der Waals force, and has the main advantages of energy-saving operation and regeneration, but has limited adsorption capacity and relatively low adsorption capacity, and cannot meet the requirement of CO adsorption in practical application. Chemisorption is a strong adsorption process in which chemical reactions occur between the adsorbent and the adsorbate due to the action of chemical bonds, and the adsorption capacity of chemisorption is much higher than that of physisorption. Thus, the introduction of chemisorption into the adsorbent may further enhance the CO adsorption properties of the adsorbent material. Cu (I) on porous supports is reported to bind strongly to CO molecules by pi complexation, and Cu (I) is inexpensive, environmentally friendly, and stable in performance, and is considered as the preferred transition metal ion for preparing CO adsorbents. Mesoporous alumina (gamma-Al) 2 O 3 ) It is widely used as CO gas adsorbent research due to its remarkable characteristics of high specific surface area, large pore volume, abundant porosity, uniform pore size distribution, stability over a wide temperature range, durability, catalytic activity, etc. Thus, in gamma-Al 2 O 3 Cu incorporation on a Carrier 2 The O active adsorption site is a promising CO adsorption material. But of conventional Cu 2 The preparation process of the O-based adsorbent is quite complex, and CuO is reduced to Cu 2 The yield of O is far from satisfactory.
In the invention, we have developed for the first time a simple solution combustion synthesis assisted CuO self-reduction process for preparing Cu with improved pore structure, high specific surface area and high dispersion of Cu (I) in the support material 2 O@γ-Al 2 O 3 The adsorbent is then used for adsorption CO separation. Compared with the traditional method, the method has the advantages that the yield of Cu (I) is obviously improved by utilizing our strategy, and the gamma-Al can be accurately regulated according to the actual application requirement 2 O 3 Is a hole structure of (2) and Cu 2 Degree of O dispersion and Cu 2 O loading to increase CO adsorption, selective adsorption and regeneration, and its application is cost effective, wide in application and easy to scale up.
Disclosure of Invention
Aiming at the problems of low removal efficiency, unsatisfactory adsorption selectivity, unstable structure and the like of the traditional CO adsorbent, the invention designs a new thought for preparing the cuprous oxide loaded mesoporous alumina powder material by adopting a solution combustion synthesis method, and the mesoporous alumina matrix of the material has high stability, relatively higher specific surface area and pore volume and in-situ loaded Cu 2 The O particle size distribution is uniform and the bonding property with the matrix is good. The adsorbent has the characteristics of high CO removal efficiency in gas, simple preparation method, environment-friendly and pollution-free production process, simple operation, suitability for large-scale production and the like.
The invention comprises the following specific steps:
(1) The preparation process of the precursor includes the steps of taking aluminum nitrate, cupric salt and fuel as raw materials, proportioning according to a certain molar ratio, then dissolving in deionized water, magnetically stirring until the mixture is fully dissolved to form homogeneous transparent solution, heating the solution on an electric furnace at 100 ℃ to form gel, and then carrying out combustion reaction in an oxygen-enriched environment to obtain fluffy precursor powder.
(2) Placing the precursor powder prepared in the step (1) into a vacuum furnace for high-temperature calcination to obtain mesoporous alumina (CuO@gamma-Al) loaded with copper oxide grains 2 O 3 ) Intermediate products.
(3) Placing the powder prepared in the step (2) into a tube furnace for high-temperature heat treatment in an inert atmosphere to obtain cuprous oxide loaded mesoporous alumina (Cu) 2 O@γ-Al 2 O 3 ) An adsorbent.
Further, the molar ratio of the aluminum nitrate, the cupric salt and the fuel in the step (1) is 1: (2.5-12): (1.7-14.9).
Further, the cupric salt in the step (1) is at least one of cupric nitrate, cupric chloride, cupric acetate and cupric sulfate.
Further, the fuel in the step (1) is at least one of glycine, urea and oxalyl diamine.
Further, the combustion reaction temperature in the step (1) is 150 to 250 ℃.
Further, the reaction in the step (1) is carried out in a container bottle, and the bottle mouth is plugged with a rubber plug, two thin tubes are inserted into the rubber plug, one of the thin tubes is used as an air inlet for introducing oxygen, and the other of the thin tubes is used as an air outlet, so that the oxygen-enriched environment is created.
Further, the high-temperature calcination in the step (2) is carried out at a heating rate of 3-5 ℃/min, a reaction temperature of 300-600 ℃ and a heat preservation time of 0.5-2 h.
Further, the inert atmosphere in the step (3) is a stable nitrogen flow, and the flow rate of the nitrogen flow is 200-300 mL/min.
Further, the step (3) is the high-temperature heat treatment, the heating rate is 6-10 ℃/min, the reaction temperature is 600-700 ℃, and the heat preservation time is 6-12 h.
Further, cu obtained in the step (3) 2 O@γ-Al 2 O 3 The adsorbent has a particle size of > 1800m 2 Total specific surface area per gram, > 3.6cm 3 The total pore volume per gram, and the cuprous oxide particle size is 4-15 nm; the adsorbent has higher CO saturated adsorption capacity, and the concentration of the adsorbent is 3.6-5.7 mmol/g at 293K.
The technology of the invention has the following advantages:
(1) The invention provides a preparation method of a high-performance CO adsorbent, which does not need to externally synthesize and introduce a mesoporous template, directly utilizes gas released in the combustion process to form a large number of holes on the surface of a material, influences the thermodynamics of reaction and the nucleation and growth of oxide by adjusting the content and the proportion of raw materials, the calcining temperature and other conditions, so as to prepare a mesoporous alumina carrier material with high specific surface area, large pore volume, regular order and uniform pore size, and provides a premise for obtaining the adsorbent with high CO adsorption capacity.
(2) The adsorbent of the invention introduces CuO into the mesoporous alumina organic framework through SCS and high-temperature calcination at 300-600 ℃, and Cu is introduced under vacuum or inert gas flow at 600-700 DEG C 2+ Self-reduction to Cu on alumina support + Is to reduce CuO to Cu 2 O, thus produce the goal adsorbent with cuprous locus, and because various reactions are carried on at lower temperature, the framework structure of mesoporous alumina remains intact, therefore the adsorbent of the invention is the well structured pi complex adsorption material, have good adsorption performance to CO.
(3) The invention synthesizes the cuprous adsorbent in the mesoporous alumina carrier by adopting in-situ reaction, improves the combination stability of the cuprous adsorbent and the mesoporous alumina carrier, and ensures Cu 2 O is not easy to fall off in the mesoporous alumina carrier, and the physical and chemical properties of the mesoporous alumina are stable, so that the obtained composite adsorbent material has stable structure and better cycle stability.
(4) The molar ratio of the aluminum nitrate to the cupric salt is controlled to be 1: (2.5-12) Cu 2 Optimization of O distribution in mesoporous alumina pore channel, no blocking of carrier pore channel structure and Cu 2 The loading of O is optimized so as to improve the adsorption capacity and separation capacity of the adsorbent to CO.
(5) Cu prepared by the invention 2 O@γ-Al 2 O 3 The surface of the adsorbent has stronger hydrophobicity, so that the competitive adsorption of water vapor and CO gas can be reduced, and the adsorption efficiency is improved; on the other hand, the problem that Cu (I) is easily oxidized into Cu (II) in humid air can be effectively solved, and the stability of adsorption performance is improved.
(6) The invention adopts the solution combustion synthesis method to prepare CuO@Al 2 O 3 The precursor powder is subjected to oxidation-reduction reaction at low temperature in an oxygen-enriched environment to achieve uniform mixing of molecular level, so that uniform loading of CuO is facilitated, the self-reduction rate of the CuO can be increased due to high dispersion of the CuO, and the yield of Cu (I) is remarkably improved.
(7) Cu prepared by the invention 2 O@γ-Al 2 O 3 The adsorbent has high overall stability, simple process, low requirements on environment and equipment and good industrial application prospect.
Detailed Description
Example 1
16.131g of aluminum nitrate, 25.972g of copper nitrate, 6.773g of glycine and 2.838g of urea were weighed into 40mL of deionized water and stirred magnetically at 200rpm to form a homogeneous, clear solution. Next, the solution was placed on a resistance furnace to heat, and evaporated with stirring at 100 ℃ to form a gel. Subsequently, heating was performed at 150℃to conduct a combustion reaction. In this process, the gel volume expands rapidly, releasing a large amount of gas, accompanied by a severe combustion reaction, while releasing a large amount of heat, to give the precursor. The precursor is put into a vacuum furnace, heated to 400 ℃ at a heating rate of 5 ℃/min and calcined for 1.5 hours at high temperature, and CuO@gamma-Al is obtained 2 O 3 Intermediate products. Finally, the prepared powder is put into a tube furnace to be subjected to high-temperature heat treatment in 200mL/min nitrogen atmosphere, the heating rate is 6 ℃/min, the reaction temperature is 670 ℃, the heat preservation time is 8 hours, and the total specific surface area is 1847.08m 2 Per gram, total pore volume of 3.96cm 3 /g、Cu 2 Cu with O particle size of 7.1nm 2 O@γ-Al 2 O 3 An adsorbent. The adsorbent has good CO adsorption performance, and the saturated adsorption capacity at 293K is 4.53mmol/g.
Example 2
14.630g of aluminum nitrate, 34.577g of copper chloride, 13.650g of copper sulfate, 9.360g of urea and 2.061g of oxalyl diamine are weighed into 60mL of deionized water and stirred magnetically at 300rpm to form a homogeneous transparent solution. Next, the solution was placed on a resistance furnace to heat, and evaporated with stirring at 100 ℃ to form a gel. Subsequently, heating was performed at 200℃to conduct a combustion reaction. In this process, the gel volume expands rapidly, releasing a large amount of gas, accompanied by a severe combustion reaction, while releasing a large amount of heat, to give the precursor. The precursor is put into a vacuum furnace, heated to 550 ℃ at a heating rate of 3 ℃/min and calcined for 2 hours at high temperature, and CuO@gamma-Al is obtained 2 O 3 Intermediate products. Finally, the prepared powder is putHigh-temperature heat treatment is carried out in a nitrogen atmosphere with the speed of 250mL/min in a tube furnace, the temperature rising rate is 6 ℃/min, the reaction temperature is 600 ℃, the heat preservation time is 12h, and the total specific surface area is 2507.31m 2 Per gram, total pore volume of 5.16cm 3 /g、Cu 2 Cu with O particle size of 4.6nm 2 O@γ-Al 2 O 3 An adsorbent. The adsorbent has good CO adsorption performance, and the saturated adsorption capacity at 293K is 5.67mmol/g.
Example 3
21.382g of aluminum nitrate, 44.382g of copper acetate and 18.574g of oxalyl diamine were weighed out in 60mL of deionized water and stirred magnetically at 350rpm to form a homogeneous, clear solution. Next, the solution was placed on a resistance furnace to heat, and evaporated with stirring at 100 ℃ to form a gel. Subsequently, heating was performed at 200℃to conduct a combustion reaction. In this process, the gel volume expands rapidly, releasing a large amount of gas, accompanied by a severe combustion reaction, while releasing a large amount of heat, to give the precursor. The precursor is put into a vacuum furnace, heated to 600 ℃ at a heating rate of 4 ℃/min and calcined for 0.5h at high temperature, and CuO@gamma-Al is obtained 2 O 3 Intermediate products. Finally, the prepared powder is put into a tube furnace to be subjected to high-temperature heat treatment in 220mL/min nitrogen atmosphere, the heating rate is 8 ℃/min, the reaction temperature is 640 ℃, the heat preservation time is 10 hours, and the total specific surface area is 2133.80m 2 Per gram, total pore volume of 4.45cm 3 /g、Cu 2 Cu with O particle size of 13.4nm 2 O@γ-Al 2 O 3 An adsorbent. The adsorbent has good CO adsorption performance, and the saturated adsorption capacity at 293K is 4.82mmol/g.
Example 4
9.378g of aluminum nitrate, 39.375g of copper sulfate, 13.64g of copper chloride, 8.063g of glycine were weighed into 80mL of deionized water and stirred magnetically at 300rpm to form a homogeneous, clear solution. Next, the solution was placed on a resistance furnace to heat, and evaporated with stirring at 100 ℃ to form a gel. Subsequently, heating was performed at 250 ℃ to perform a combustion reaction. In the process, the gel volume expands rapidly, releasing a large amount of gas, accompanied by a severe combustion reaction, while releasing a large amount of heat,obtaining a precursor. The precursor is put into a vacuum furnace, heated to 500 ℃ at a heating rate of 5 ℃/min and calcined for 1h at high temperature, and CuO@gamma-Al is obtained 2 O 3 Intermediate products. Finally, the prepared powder is put into a tube furnace to be subjected to high-temperature heat treatment in 300mL/min nitrogen atmosphere, the heating rate is 10 ℃/min, the reaction temperature is 700 ℃, the heat preservation time is 6h, and the total specific surface area is 1987.43m 2 Per gram, total pore volume of 4.02cm 3 /g、Cu 2 Cu with O particle size of 9.7nm 2 O@γ-Al 2 O 3 An adsorbent. The adsorbent has good CO adsorption performance, and the saturated adsorption capacity at 293K is 3.77mmol/g.

Claims (1)

1. Mesoporous alumina loaded Cu 2 The application of the O adsorbent is characterized in that the mesoporous alumina is loaded with Cu 2 The preparation steps of the O adsorbent are as follows:
weighing 14.630g aluminum nitrate, 34.577g copper chloride, 13.650g copper sulfate, 9.360g urea and 2.061g oxalyl diamine, dissolving in 60mL deionized water, and magnetically stirring at 300rpm to form a uniform and transparent solution; next, the solution was placed on a resistance furnace to heat, and stirred and evaporated at 100 ℃ to form a gel; subsequently, heating at 200 ℃ to perform a combustion reaction, during which the gel volume rapidly expands, releasing a large amount of gas, accompanied by a vigorous combustion reaction, while releasing a large amount of heat, to obtain a precursor;
placing the precursor into a vacuum furnace, heating to 550 ℃ at a heating rate of 3 ℃/min, and calcining at a high temperature of 2h to obtain CuO@gamma-Al 2 O 3 An intermediate product;
finally, the prepared CuO@gamma-Al 2 O 3 Placing the intermediate product powder into a tube furnace, performing high-temperature heat treatment in a nitrogen atmosphere of 250mL/min, wherein the heating rate is 6 ℃/min, the reaction temperature is 600 ℃, the heat preservation time is 12h, and the total specific surface area is 2507.31m 2 /g, total pore volume of 5.16cm 3 /g、Cu 2 Mesoporous alumina loaded Cu with O particle size of 4.6nm 2 An O adsorbent;
the mesoporous alumina negative electrodeCu-carrying 2 The O adsorbent is used for adsorbing CO.
CN202210454170.1A 2022-04-27 2022-04-27 Mesoporous alumina loaded Cu 2 Preparation method of O adsorbent Active CN114887583B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0442809A (en) * 1990-06-08 1992-02-13 Cataler Kogyo Kk Heat-resistant fibrous alumina having high surface area and its production
CN101486941A (en) * 2009-02-17 2009-07-22 华中科技大学 Process for preparing iron based oxygen carrier
CN102658080A (en) * 2012-04-13 2012-09-12 武汉理工大学 Preparation method of highly-dispersed meso pore gamma-Al2O3 base alkali (soil) metal composite adsorbent
CN109371308A (en) * 2018-12-17 2019-02-22 湘潭大学 The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end
CN110314643A (en) * 2019-07-16 2019-10-11 南京工业大学 A kind of preparation and application of the modified mesopore oxide material of high stability monovalence copper

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0442809A (en) * 1990-06-08 1992-02-13 Cataler Kogyo Kk Heat-resistant fibrous alumina having high surface area and its production
CN101486941A (en) * 2009-02-17 2009-07-22 华中科技大学 Process for preparing iron based oxygen carrier
CN102658080A (en) * 2012-04-13 2012-09-12 武汉理工大学 Preparation method of highly-dispersed meso pore gamma-Al2O3 base alkali (soil) metal composite adsorbent
CN109371308A (en) * 2018-12-17 2019-02-22 湘潭大学 The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end
CN110314643A (en) * 2019-07-16 2019-10-11 南京工业大学 A kind of preparation and application of the modified mesopore oxide material of high stability monovalence copper

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