CN113663659A - Catching agent and preparation method and application thereof - Google Patents
Catching agent and preparation method and application thereof Download PDFInfo
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- CN113663659A CN113663659A CN202111006192.3A CN202111006192A CN113663659A CN 113663659 A CN113663659 A CN 113663659A CN 202111006192 A CN202111006192 A CN 202111006192A CN 113663659 A CN113663659 A CN 113663659A
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- 238000002360 preparation method Methods 0.000 title abstract description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000002121 nanofiber Substances 0.000 claims abstract description 52
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 50
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 49
- 229920000767 polyaniline Polymers 0.000 claims abstract description 49
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000003277 amino group Chemical group 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 17
- 238000002791 soaking Methods 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 12
- 230000002378 acidificating effect Effects 0.000 claims description 11
- 239000003999 initiator Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000006247 magnetic powder Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 238000007334 copolymerization reaction Methods 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- MIOPJNTWMNEORI-GMSGAONNSA-N (S)-camphorsulfonic acid Chemical compound C1C[C@@]2(CS(O)(=O)=O)C(=O)C[C@@H]1C2(C)C MIOPJNTWMNEORI-GMSGAONNSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002516 radical scavenger Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 28
- 238000005516 engineering process Methods 0.000 abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- 231100000956 nontoxicity Toxicity 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 239000007864 aqueous solution Substances 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 13
- 238000005406 washing Methods 0.000 description 13
- 238000003756 stirring Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 238000003795 desorption Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 239000012621 metal-organic framework Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical class N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- 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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- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/28014—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 form
- B01J20/28023—Fibres or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
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Abstract
The invention discloses a trapping agent, which comprises: the magnetic polyaniline superfine nano-fiber is combined to form a cluster-shaped structure, the cluster-shaped structure has a cage-shaped structure, the diameter of the magnetic polyaniline superfine nano-fiber is less than 60nm, and active amino groups are distributed on the surface of the magnetic polyaniline superfine nano-fiber. The invention discloses a preparation method of the trapping agent. The invention also discloses application of the trapping agent in adsorbing carbon dioxide. The invention combines the trapping agent and Amine-In-Water technology, the trapping agent can replace ammonia Water, has high adsorption performance to carbon dioxide, and the carbon dioxide adsorption amount is up to 12.81 mmol/g. The invention has low economic cost, high feasibility of industrial production, no toxicity and no harm.
Description
Technical Field
The invention relates to the technical field of carbon dioxide adsorption, in particular to a trapping agent and a preparation method and application thereof.
Background
With the gradual exhaustion of energy sources in the global range, the problems of energy crisis and greenhouse effect become more and more prominent, and the data show that: CO produced by using fuel worldwide by 20102The total amount reaches 306 hundred million tons. In 2020, the pressure is broken through to 347 hundred million tons. In order to better cope with climate change, the technology of realizing carbon neutralization, efficiently capturing carbon elements and converting the carbon elements into fuel for storage is developed. The carbon capture technology is mainly divided into three steps of capture, transportation and storage. This technology is specifically a process in which carbon dioxide produced in industrial processes is separated by some means, transported to a dedicated storage site and isolated from the atmosphere for a long period of time. Wherein, the catching link can be realized by three modes: pre-combustion capture, post-combustion capture, and oxy-fuel combustion. The capture before combustion and oxygen-enriched combustion are not suitable for industrial popularization. The absorption principle after combustion is that some alkalescent substances and carbon dioxide are subjected to chemical reaction to generate salts, and then the salts are subjected to reverse reaction to release the carbon dioxide.
The existing carbon capture technology for processing carbon dioxide mainly comprises three aspects of chemistry, physics and biology. Physical methods generally use a low-temperature method and a membrane system method, mainly utilize the material characteristics of carbon dioxide, and use a low-temperature liquefaction or differential pressure principle to capture carbon, but the technologies have high cost and low carbon capture efficiency, and are easy to cause secondary pollution in storage. The Amine-In-Water technology is a process of neutralizing alkaline ammonium monohydrate and carbon dioxide to generate ammonium bicarbonate and ammonium carbonate, and then evaporating ammonium salt to obtain carbon dioxide again; the chemical method has good effect on electric field waste gas treatment, but the method for obtaining carbon dioxide by evaporating water in ammonia salt has the problems of high cost consumption, viscous solvent, difficulty in flowing, easy precipitation of solid precipitate and the like.
The low-temperature adsorbent generally refers to an adsorbent material with an adsorption temperature lower than 600 ℃, which is the focus of current research and is the future carbon adsorption material. Currently, the commonly used cryoadsorbents are: metal organic framework materials MOFs, carbon nanotubes and the like. The MOFs mainly depends on the ordered pore channel structure of the material and the chemical property which is easy to adjust, the adsorption capacity of the MOFs to carbon dioxide is improved by modifying the surface property of the MFOs, and a plurality of active metal centers are opened on the porous walls of the MFOs, so that the high carbon dioxide adsorption rate can be ensured under the low-temperature premise. The carbon nano tube respectively obtains the carbon dioxide adsorption capacity of 5.7mmol/g and 3.7mmol/g under the conditions of 0 ℃ and 25 ℃ by utilizing high surface area and high cyclicity. However, the adsorption amount of carbon dioxide by the low-temperature adsorbent is still required to be increased.
As the prior carbon capture technology of carbon dioxide has a series of problems of secondary pollution, difficult industrialization, high input cost and the like, the carbon capture process can not meet the requirement of carbon neutralization, and the cost of the technology is far higher than the value of the current carbon trading market. At present, a new technology which has low economic cost, high feasibility of industrial production, no toxicity and harm and difficulty in causing secondary pollution is urgently needed in carbon neutralization markets.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a capture agent and a preparation method and application thereof, and the invention soaks cluster-shaped magnetic polyaniline superfine nanofiber in alkaline liquor to remove acidic substances around amino groups, so that a large amount of active amino groups are exposed on the surface of the polyaniline nanofiber, and the adsorption sites of carbon dioxide are greatly improved, thereby improving the carbon dioxide adsorption performance of the invention; the invention combines the trapping agent and Amine-In-Water technology, the trapping agent can replace ammonia Water, has high adsorption performance to carbon dioxide, and the carbon dioxide adsorption amount is up to 12.81 mmol/g. The invention has low economic cost, high feasibility of industrial production, no toxicity and no harm.
The invention provides a trapping agent, which comprises: the magnetic polyaniline superfine nano-fiber is combined to form a cluster-shaped structure, the cluster-shaped structure has a cage-shaped structure, and active amino groups are distributed on the surface of the magnetic polyaniline superfine nano-fiber.
Preferably, the magnetic polyaniline nanofibers have a diameter < 60 nm.
The invention also discloses a preparation method of the trapping agent, which comprises the following steps: soaking the cluster magnetic polyaniline superfine nano-fiber in alkali liquor to obtain the trapping agent.
Preferably, the solute of the alkali liquor is an inorganic alkaline substance.
Preferably, the solute of the alkali liquor is at least one of sodium hydroxide, potassium hydroxide and ammonia monohydrate.
Preferably, the solvent of the lye is water.
Preferably, the mass fraction of the lye is 8-12 wt%.
Preferably, soaking in alkaline solution for 0.1-1 h.
The cluster-like magnetic polyaniline ultrafine nanofibers are the cluster-like magnetic polyaniline ultrafine nanofibers described in application No. 202110881122.6.
In the cluster-shaped magnetic polyaniline superfine nano-fiber, the appearance of the magnetic polyaniline superfine nano-fiber (the diameter is less than 60nm, and the length is about 2 mu m) is controllable, and the superfine nano-fiber is combined to form a cluster-shaped structure; the superfine nano fiber has larger specific surface area, and has better adsorption and constraint performance on ions/substances than a crude fiber or a shell-core structure, and in addition, the superfine nano fiber forms a cluster-shaped structure which has a cage-shaped structure and can lock organic matters and metal ions; the cluster magnetic polyaniline superfine nano-fiber has good adsorption performance through the combination of the superfine nano-fiber and the cluster structure.
Preferably, the preparation method of the cluster-shaped magnetic polyaniline ultrafine nanofiber comprises the following steps: soaking the nano magnetic powder in aniline, then uniformly mixing with the solution of acidic substances, adding an initiator, and carrying out reaction copolymerization to obtain the cluster-shaped magnetic polyaniline superfine nanofiber.
After the reaction copolymerization, solid-liquid separation is carried out, the solid is washed by warm water and ethanol in sequence, and then the cluster-shaped magnetic polyaniline ultrafine nano fiber is obtained after drying.
The nano magnetic powder is nano iron tetroxide.
Preferably, soaking in aniline for 1-8 h.
Preferably, the rate of addition of the initiator is from 1.2 to 1.6 g/min.
The above initiator may be added in the form of an aqueous solution, the concentration of the aqueous initiator solution being preferably 0.25 g/ml.
The concentration of the solution of the acidic substance is preferably 0.01 to 0.1g/ml, and the solvent of the solution of the acidic substance is preferably water.
Preferably, the acidic substance comprises: at least one of p-toluenesulfonic acid, camphorsulfonic acid, hydrochloric acid, sulfuric acid and nitric acid.
Preferably, the initiator comprises: at least one of ammonium persulfate, sodium persulfate and potassium persulfate.
Preferably, the reaction temperature is-30-60 ℃, and the reaction time is 8-12 h.
Preferably, the weight ratio of the nano magnetic powder to the aniline is 1-5: 10.
Preferably, the weight ratio of the aniline to the acidic substance to the initiator is 1-10:1-10: 1-100.
The water may be deionized water, purified water, etc.
The invention firstly soaks the nano magnetic powder in the aniline, and then selects a proper preparation process to carry out reaction copolymerization to obtain the magnetic polyaniline with a specific morphology, namely the cluster-shaped magnetic polyaniline superfine nanofiber.
The invention also provides application of the trapping agent in adsorption of carbon dioxide.
Has the advantages that:
1. in the cluster-shaped magnetic polyaniline superfine nanofiber, amino on the surface of the polyaniline nanofiber is surrounded by acidic substances, and the cluster-shaped magnetic polyaniline superfine nanofiber is soaked in alkali liquor to remove the acidic substances around the amino, so that a large number of active amino is exposed on the surface of the polyaniline nanofiber, the adsorption sites of carbon dioxide are greatly improved, and the carbon dioxide adsorption performance of the invention is improved.
2. According to the invention, the trapping agent is combined with Amine-In-Water technology, the trapping agent can replace ammonia Water, the carbon dioxide has high adsorption performance, the carbon dioxide adsorption amount is up to 12.81mmol/g, the carbon dioxide removing method is simple, and the problems of high energy consumption for removing carbon dioxide, difficulty In solvent thickening and flowing, easiness In solid precipitation and the like when ammonia Water is adopted are avoided; the trapping agent is a low-temperature adsorbent, so that the energy consumption is low, the trapping agent can be recycled, and the magnetism is convenient to recover; the invention can reduce the cost of adsorbing carbon dioxide and avoid secondary pollution; the invention has low economic cost, high feasibility of industrial production, no toxicity and no harm.
Drawings
FIG. 1 is a scanning electron micrograph of the capturing agent obtained in example 1.
FIG. 2 is a partially enlarged scanning electron micrograph of the trapping agent prepared in example 1.
FIG. 3 is a carbon dioxide desorption detection spectrum of the capturing agent in example 1.
Fig. 4 is a carbon dioxide desorption detection spectrum of the cluster-shaped magnetic polyaniline ultrafine nanofiber in example 1.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a capture agent comprises the following steps:
mixing 100ml of aniline with 10g of nano ferroferric oxide powder, uniformly stirring by magnetic force, and then soaking for 3 hours to mark as a solution A;
preparing a proper reaction container, filling 5000ml of water in the container, placing an ice bag on the periphery of the outer bottom of the container (in order to prevent the reaction from generating heat and bumping, proper temperature reduction is needed), then adding 300ml of aqueous solution containing 100g of p-toluenesulfonic acid into the container, opening an electric stirring rod, and starting stirring; then adding the solution A and mixing uniformly;
then dropwise adding 1000ml of ammonium persulfate aqueous solution with the concentration of 0.25g/ml (controlling the adding speed of the ammonium persulfate to be 1.4g/min, and finishing dropwise adding within about 3 h); keeping the temperature at 10 ℃, continuously stirring for 10h, performing suction filtration, washing the solid with warm water at 60 ℃ until the filtrate turns from dark yellow to colorless, then washing the solid with ethanol to remove p-toluenesulfonic acid, and drying in an oven at 60 ℃ to obtain cluster-shaped magnetic polyaniline ultrafine nanofibers;
adding the cluster-shaped magnetic polyaniline superfine nano-fiber into a sodium hydroxide aqueous solution with the mass fraction of 10 wt%, soaking for 0.1h, filtering, and washing a filter cake with water to obtain the trapping agent.
Example 2
The dosage of the nano ferroferric oxide powder is 20g, and the cluster magnetic polyaniline superfine nano-fiber is obtained in the same way as in the example 1;
adding the cluster-shaped magnetic polyaniline superfine nano-fiber into a sodium hydroxide aqueous solution with the mass fraction of 10 wt%, soaking for 0.2h, filtering, and washing a filter cake with water to obtain the trapping agent.
Example 3
The dosage of the nano ferroferric oxide powder is 30g, and the cluster magnetic polyaniline superfine nano-fiber is obtained in the same way as in the example 1;
adding the cluster-shaped magnetic polyaniline superfine nano-fiber into a sodium hydroxide aqueous solution with the mass fraction of 10 wt%, soaking for 0.3h, filtering, and washing a filter cake with water to obtain the trapping agent.
Example 4
The dosage of the nano ferroferric oxide powder is 40g, and the cluster magnetic polyaniline superfine nano-fiber is obtained in the same way as in the example 1;
adding the cluster magnetic polyaniline superfine nano-fiber into a sodium hydroxide aqueous solution with the mass fraction of 10 wt%, soaking for 0.4h, filtering, and washing a filter cake with water to obtain the trapping agent.
Example 5
The dosage of the nano ferroferric oxide powder is 50g, and the cluster magnetic polyaniline superfine nano-fiber is obtained in the same way as the example 1;
adding the cluster-shaped magnetic polyaniline superfine nano-fiber into a sodium hydroxide aqueous solution with the mass fraction of 10 wt%, soaking for 0.5h, filtering, and washing a filter cake with water to obtain the trapping agent.
Example 6
A method for preparing cluster-shaped magnetic polyaniline superfine nano-fiber comprises the following steps:
mixing 100ml of aniline with 30g of nano ferroferric oxide powder, uniformly stirring by magnetic force, and then soaking for 1 hour to mark as a solution A;
preparing a proper reaction container, filling 5000ml of water in the container, placing an ice bag on the periphery of the outer bottom of the container (in order to prevent the reaction from generating explosive boiling due to heat release, proper temperature reduction is needed), adding 300ml of an aqueous solution containing 100g of camphorsulfonic acid into the container, opening an electric stirring rod, and starting stirring; then adding the solution A and mixing uniformly;
then 1000ml of sodium persulfate aqueous solution with the concentration of 1g/ml is dripped (the addition speed of the sodium persulfate is controlled to be 1.2 g/min); keeping the temperature at minus 30 ℃, continuously stirring for 12h, carrying out suction filtration, washing the solid with warm water at 60 ℃ until the filtrate turns from dark yellow to colorless, then washing the solid with ethanol to remove p-toluenesulfonic acid, and drying in an oven at 60 ℃ to obtain the cluster-shaped magnetic polyaniline ultrafine nanofiber;
adding the cluster-shaped magnetic polyaniline superfine nano-fiber into a sodium hydroxide aqueous solution with the mass fraction of 8 wt%, soaking for 0.2h, filtering, and washing a filter cake with water to obtain the trapping agent.
Example 7
A method for preparing cluster-shaped magnetic polyaniline superfine nano-fiber comprises the following steps:
mixing 100ml of aniline with 20g of nano ferroferric oxide powder, uniformly stirring by magnetic force, and then soaking for 8 hours to mark as a solution A;
preparing a proper reaction container, filling 5000ml of water in the container, placing an ice bag (which needs to be properly cooled in order to prevent the reaction from generating heat and bumping) at the periphery of the outer bottom of the container, adding 300ml of aqueous solution containing 100g of hydrochloric acid (the mass fraction of HCl in the hydrochloric acid is 5 wt%) into the container, opening an electric stirring rod, and starting stirring; then adding the solution A and mixing uniformly;
then 1000ml of potassium persulfate aqueous solution with the concentration of 0.1g/ml is dripped (the addition speed of the potassium persulfate is controlled to be 1.6 g/min); keeping the temperature at 60 ℃, continuously stirring for 8h, performing suction filtration, washing the solid with warm water at 60 ℃ until the filtrate turns from dark yellow to colorless, then washing the solid with ethanol to remove p-toluenesulfonic acid, and drying in an oven at 60 ℃ to obtain the cluster-shaped magnetic polyaniline ultrafine nanofiber;
adding the cluster-shaped magnetic polyaniline superfine nano-fiber into a sodium hydroxide aqueous solution with the mass fraction of 12 wt%, soaking for 0.3h, filtering, and washing a filter cake with water to obtain the trapping agent.
Experiment 1
The detection results of the capturing agent obtained in example 1 are shown in FIG. 1-2.
FIG. 1 is a scanning electron micrograph of a trapping agent prepared in example 1; FIG. 2 is a partially enlarged scanning electron micrograph of the trapping agent prepared in example 1.
As can be seen from the figures 1-2, in the trapping agent prepared by the invention, the magnetic polyaniline ultrafine nano-fibers are combined to form a cluster structure, the cluster structure has a cage structure, the diameter of the magnetic polyaniline ultrafine nano-fibers is less than 60nm, and the fibers are very thin.
The carbon dioxide adsorption experiment was performed on the cluster-shaped magnetic polyaniline ultrafine nanofibers and the capture agent in example 1, and the amount of carbon dioxide adsorbed was measured.
The carbon dioxide adsorption experiment comprises the following specific steps: adding 10g of material to be detected into 100ml of water, mixing uniformly, introducing carbon dioxide gas at 25 ℃ for 30min, taking out the adsorption material, and using CO2TPD (manufacturer France DAS, model 7000) detects the amount of carbon dioxide adsorbed in each adsorption material. The results are shown in Table 1 and FIGS. 3-4.
FIG. 3 is a carbon dioxide desorption detection spectrum of the capturing agent in example 1; fig. 4 is a carbon dioxide desorption detection spectrum of the cluster-shaped magnetic polyaniline ultrafine nanofiber in example 1.
In fig. 3, peak fitting is performed on the carbon dioxide desorption curve B to obtain a peak fitting curve 1-5 and an accumulated peak value fitting curve, wherein the peak fitting curve 1 is a carbon dioxide desorption peak, and the desorption temperature is less than 600 ℃; peak fitting 3-5 is the decomposition peak of the trapping agent, because the trapping agent will decompose at high temperature after being soaked in alkali liquor, and the table in FIG. 3 is the equation fitted to each peak.
In fig. 4, peak fitting is performed on the carbon dioxide desorption curve B to obtain peak fitting 1 to 4 and an accumulated peak value fitting curve, where the peak fitting 1 is a carbon dioxide desorption peak, and the table in fig. 4 is an equation fitted to each peak.
TABLE 1 carbon dioxide adsorption results
As can be seen from table 1 and fig. 3-4: the catching agent of the invention has good adsorbability to carbon dioxide, and the adsorbability is 563.64mg/g when the adsorbability is up to 12.81 mmol/g.
Compared with the existing metal oxides, carbon materials, molecular sieves and MOFs materials regulated and controlled by organic amine, the carbon dioxide adsorption performance comparison result is shown in Table 2.
TABLE 2 carbon dioxide adsorption Performance results for various materials
As can be seen from Table 2, the carbon dioxide adsorption capacity of the capturing agent of the present invention is much higher than that of the existing adsorbent.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A capture agent, comprising: the magnetic polyaniline superfine nano-fiber is combined to form a cluster-shaped structure, the cluster-shaped structure has a cage-shaped structure, and active amino groups are distributed on the surface of the magnetic polyaniline superfine nano-fiber.
2. A method for preparing the scavenger according to claim 1, comprising the steps of: soaking the cluster magnetic polyaniline superfine nano-fiber in alkali liquor to obtain the trapping agent.
3. The method for preparing a trapping agent according to claim 2, wherein the solute of the alkali solution is an inorganic alkaline substance; preferably, the solute of the alkali liquor is at least one of sodium hydroxide, potassium hydroxide and ammonia monohydrate; preferably, the solvent of the lye is water; preferably, the mass fraction of the alkali liquor is 8-12 wt%; preferably, soaking in alkaline solution for 0.1-1 h.
4. The method for preparing the capture agent according to claim 2 or 3, wherein the method for preparing the cluster-like magnetic polyaniline ultrafine nanofiber comprises the following steps: soaking the nano magnetic powder in aniline, then uniformly mixing with the solution of acidic substances, adding an initiator, and carrying out reaction copolymerization to obtain the cluster-shaped magnetic polyaniline superfine nanofiber.
5. The method for preparing the capture agent according to claim 4, wherein the capture agent is soaked in aniline for 1-8 h; preferably, the rate of addition of the initiator is from 1.2 to 1.6 g/min.
6. The method for producing a capturing agent according to claim 4 or 5, wherein the acidic substance comprises: at least one of p-toluenesulfonic acid, camphorsulfonic acid, hydrochloric acid, sulfuric acid and nitric acid; preferably, the initiator comprises: at least one of ammonium persulfate, sodium persulfate and potassium persulfate.
7. The method for preparing the capture agent according to any one of claims 4 to 6, wherein the reaction temperature is-30 to 60 ℃ and the reaction time is 8 to 12 hours.
8. The method for preparing the capture agent according to any one of claims 4 to 7, wherein the weight ratio of the nano magnetic powder to the aniline is 1-5: 10.
9. The method for producing the trapping agent according to any one of claims 4 to 8, wherein the weight ratio of the aniline, the acidic substance, and the initiator is 1-10:1-10: 1-100.
10. Use of the capture agent of claim 1 for adsorbing carbon dioxide.
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