CN113617304A - Gas absorption microcapsule based on microfluidic and thermal crosslinking technology and preparation method and application thereof - Google Patents
Gas absorption microcapsule based on microfluidic and thermal crosslinking technology and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a gas absorption microcapsule based on micro-fluidic and thermal crosslinking technologies and a preparation method and application thereof; the microcapsule is of a core-shell structure, the core layer is a gas absorbent formed by combining choline salt and a coordination agent, the shell layer is made of a breathable material, the monodispersity of particles is good, and the particle size form is uniform and stable; the preparation method of the microcapsule is simple, the breathable material and the eutectic solvent are used for preparing w/o/w (water/oil/water) core-shell structure microcapsules by a microfluidic technology, and the breathable shell material is solidified by thermal crosslinking to prepare the carbon dioxide gas-absorbable microcapsule which is loaded with the eutectic solvent; the specific surface area of an absorption system of the microcapsule is greatly increased, and meanwhile, after a gas absorbent, namely the eutectic solvent, is encapsulated and solidified into the microcapsule, the defect of low absorption rate caused by high viscosity of the gas absorbent is overcome, the absorption rate and the absorption capacity are greatly increased, the microcapsule is applied to absorption of carbon dioxide, and a direction is provided for industrialization of capturing the carbon dioxide by the eutectic solvent.
Description
Technical Field
The invention relates to a gas absorption microcapsule based on microfluidic and thermal crosslinking technologies, a preparation method thereof and application of the gas absorption microcapsule to carbon dioxide capture, and belongs to the field of chemical separation and purification.
Background
Approximately 30 million tons of carbon dioxide are released into the atmosphere annually by humans, thus leading to the continuous accumulation of greenhouse gases and the associated disasters caused by the greenhouse effect. An increasing number of international efforts are devoted to developing commercially viable carbon capture technologies that can be implemented on a global scale.
A variety of low cost and large scale carbon dioxide capture methods have been extensively studied, including membrane separation, organic solvent absorbents, solid absorption, and the like. As currently, the most established method for capturing carbon dioxide from flue gases is to add a flowing amine-based solution, such as Monoethanolamine (MEA), to an absorber tower, where MEA absorbs carbon dioxide quickly, is inexpensive, and is available in large quantities. In order to further increase the carbon dioxide absorption capacity of the amine-based solution, studies have been made, such as Mucunri-Yilang et al (CN107735162A), in which Diethanolamine (DEA) is used as a carbon dioxide absorbent, and an absorbent is prepared by wet-impregnating Diethanolamine (DEA) onto a clay carrier using a porous material such as clay particles as a carrier, thereby increasing the specific surface area of the absorbent and increasing the carbon dioxide absorption capacity. High absorption rate of amino solvent absorbent and high CO absorption rate2Large absorption capacity, but the disadvantages are high corrosivity, high toxicity of degradation products and CO evolution during solvent recovery2Has high energy consumption (more than 100 ℃) and is harmful to human health and environment.
At present, CO2A common method for capture is solvent absorption, in which an ionic liquid is used as a solvent to absorb CO2Has the advantage of large absorption capacity. Compared with the traditional ionic liquid, the eutectic solvent type ionic liquid has larger absorption capacity and larger absorption capacity while maintaining the advantages of the traditional ionic liquidThe key points are that the ionic liquid absorbent is nontoxic, the synthetic process steps are simple, and the price is low, so that the eutectic solvent is usually selected as the ionic liquid absorbent. But also has the defect of high ionic liquid viscosity, which causes huge corresponding gas-liquid mass transfer resistance, thereby inhibiting CO2The absorption rate and the absorption capacity are also low, and the industrial application is hindered. Although it has been shown by research that the viscosity of the eutectic solvent is greatly reduced and the absorption rate is increased by increasing a proper amount of water, the presence of water also causes CO2The decrease in the absorption capacity does not achieve both the absorption rate and the absorption capacity. And the content of water is easy to change continuously during the circulation use due to the volatilization of the water during the subsequent desorption, and the stable production is difficult to realize.
Disclosure of Invention
The purpose of the invention is as follows: aiming at trapping CO by low eutectic solvent type ionic liquid in the prior art2The invention provides a gas absorption microcapsule based on micro-fluidic and thermal crosslinking technologies, which can greatly increase the absorption rate and the absorption capacity by using eutectic solvent type ionic liquid as a gas absorbent; also provides a preparation method and application of the gas absorption microcapsule.
The technical scheme is as follows: the gas absorption microcapsule based on the microfluidic and thermal crosslinking technology is of a core-shell structure, a core layer material is a gas absorbent formed by combining choline salt and a coordination agent, and a shell layer material is a breathable material.
Preferably, the gas permeable material comprises tetraethyl orthosilicate gas permeable modified by ceramics, zeolite or carbon nanoparticles, polydimethylsiloxane, polysulfone, polystyrene; further preferred is a rubber material polydimethylsiloxane.
The invention discloses a preparation method of the gas absorption microcapsule, which comprises the following steps:
(1) preparing a gas absorbent: taking choline salt and a coordination agent, drying and mixing to obtain a gas absorbent;
(2) preparing the microcapsule: and (2) taking the gas absorbent obtained in the step (1) as an internal phase, mixing a breathable material, an emulsifier A and a curing agent to obtain an intermediate phase, taking an aqueous solution of an emulsifier B as an external phase, heating the w/o/w double-layer microspheres obtained by the micro-fluidic technology, and performing thermal crosslinking to obtain the gas absorption microcapsule.
Preferably, the step (1) is to take choline salt and a complexing agent, dry the choline salt and the complexing agent in a vacuum drying oven for more than 3 days, and then transfer the choline salt and the complexing agent into an oil bath kettle at the temperature of 80-120 ℃ to mix to obtain the gas absorbent of the eutectic mixture.
Preferably, in step (1), the choline salt includes choline chloride, choline bromide; the complexing agent comprises metal salt, metal salt hydrate and hydrogen bond donor; the molar ratio of the choline salt to the complexing agent is 1: 5-1: 0.5.
Preferably, in the step (2), the mass ratio of the air-permeable material, the emulsifier A and the curing agent is 10:5: 1-10: 0.5:1, and the emulsifier A comprises Span 20-80 (Span 20-80), sucrose ester, phosphate, soybean phospholipid and degummed oil.
Preferably, in the step (2), the emulsifier B comprises poloxamer (F-127), tween 20-80 (T-20-80), polyvinyl alcohol (PVA) and polyoxyethylene ether, the water solution of the emulsifier B is a glycerol water solution, and the emulsifier B is 0.5-10 wt% of glycerol.
The invention also discloses application of the gas absorption microcapsule based on the microfluidic and thermal crosslinking technology, and the gas absorption microcapsule can be applied to absorption of greenhouse gases.
The microcapsule is prepared by a microfluidic device, PDMS is used as a substrate or a glass capillary coaxial microfluidic platform for preparing the gas absorption microcapsule with a core-shell structure, and the microfluidic platform consists of four parts: the liquid propelling injection pump, the capillary tube-in-tube microfluidic device or the PDMS are used as the substrate microfluidic device, the connecting conduit and the receiving device. The continuous phase is sheared relative to the dispersed phase by regulating and controlling the shearing force, so that the surface tension of the dispersed phase is destroyed to prepare the microcapsule encapsulating the gas absorbent.
Compared with the traditional ionic liquid, the eutectic solvent type ionic liquid has larger absorption capacity while maintaining the advantages of the traditional ionic liquid, and more importantly, the eutectic solvent type ionic liquid is nontoxic, and has simple and valuable synthesis process stepsThe price is low, and the gas absorbent is obtained by heating eutectic mixture formed by the compound containing the hydrogen bond donor and the choline salt containing the hydrogen bond acceptor through the action of the hydrogen bond; but the eutectic solvent type ionic liquid has the defect of high liquid viscosity, which causes the corresponding mass transfer resistance to be larger, thereby inhibiting CO2The absorption rate and the absorption capacity are also low. Although the prior literature reports that the specific surface area is increased by using a porous material to carry the ionic liquid, the prior literature has the problems of low carrying capacity, easy falling and unloading of the ionic liquid, poor cycle performance and the like. According to the preparation method, the eutectic solvent and the microfluidic technology are organically combined for thermal crosslinking to prepare the microcapsule, so that the purposes of high loading capacity, good cycle performance and the like are achieved. The selection of the air-permeable shell material with good compatibility is the basis of successful encapsulation of the shell material to the eutectic solvent type ionic liquid, thereby ensuring CO2The air-permeable shell material can be absorbed by the absorbent, and after the eutectic solvent type ionic liquid with high viscosity is encapsulated, the air absorption contact surface is changed into a microcapsule from high-viscosity liquid, so that the air absorption is facilitated.
The eutectic solvent and the microfluidic technology are organically combined through thermal crosslinking to prepare the microcapsule, the amount of the emulsifier of the dispersed phase and the continuous phase and the flow rate of three phases are changed through the microfluidic technology to prepare the w/o/w eutectic solvent-encapsulated microcapsule, the eutectic solvent encapsulated by the microcapsule is cured through the thermal crosslinking to form a micron microcapsule; compared with the non-thermal crosslinking microcapsule, the crosslinked microcapsule can be separated from an external phase (liquid-solid system, filtration and separation), the use process is convenient, the leakage of a eutectic solvent in the microcapsule can be prevented, and the stability of the microcapsule can be ensured in the process of repeated use of absorption and analysis. Compared with a liquid absorbent, the absorbent forming the micron-sized microcapsules has the advantages that the specific surface area is greatly increased, the contact area with gas is greatly increased, the mass transfer rate is increased, the gas absorption rate and the absorption capacity are greatly improved, and the application prospect in the aspect of absorbing gases such as greenhouse gas carbon dioxide is good.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
(1) the gas absorption microcapsule has good monodispersity, uniform and stable particle size, large specific surface area, large absorption capacity, and faster absorption rate of greenhouse gases such as carbon dioxide, and compared with the microcapsule before encapsulation, the gas absorption microcapsule with the particle size of 200 mu m has the advantages that the carbon dioxide absorption capacity is improved by 13 times, the absorption rate is improved by 26 times, and the microcapsule is environment-friendly;
(2) the gas absorption microcapsule has the advantages of cheap and easily obtained raw materials, simple preparation method, simple absorption operation process, simple analysis process and good gas absorption and recycling performance, and realizes the purpose of absorbing CO at normal pressure2The absorption capacity and the absorption rate are greatly improved, and the method is suitable for industrial production.
Drawings
FIG. 1 is a nuclear magnetic hydrogen spectrum of a eutectic solvent synthesized in example 1;
FIG. 2 is a test of the compatibility of polydimethylsiloxane with the eutectic solvent in example 2;
FIG. 3 is a graph of ATR-FITR in example 2 after cure of the polydimethylsiloxane;
FIG. 4 is a drawing of a microfluidic preparation with a diameter of 240 μm prepared by microfluidics and an optical microscope of uncured microcapsules in example 3;
FIG. 5 is SEM pictures of cured microcapsules with diameters of 240 μm and 500 μm prepared by microfluidics in examples 3 and 4 and core-shell structures;
FIG. 6 is the carbon dioxide absorption of 240 μm, 500 μm diameter microcapsules in examples 3, 4, 5 and 6;
FIG. 7 is a graph of the carbon dioxide uptake rate by 240 μm, 500 μm diameter microcapsules, DES in examples 3, 4, 5 and 6;
FIG. 8 is the cyclic absorption effect of the microcapsules of example 7 under a pressure of 240 μm microcapsules under 1 atm.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
Example 1
Synthesis of eutectic solvent
Before weighing, the choline chloride needs to be put into a vacuum drying oven to be dried for 24 hours under the vacuum condition at 50 ℃ to remove moisture (the choline chloride has strong water absorption) so as to ensure the weighing accuracy. Then openWeighing (the mol ratio of choline chloride to urea is 1:2) 46.2g of urea and 53.8g of choline chloride, putting the weighed choline chloride, urea and a magnetic stirrer rotor into a 250mL beaker, sealing the beaker by using a preservative film, melting the choline chloride, urea and the magnetic stirrer into a solution under the condition of heat collection constant temperature heating at 100 ℃, continuing heating in a water bath for 2 hours after timing, taking off the preservative film, sealing the mouth of the beaker by using tin foil paper, and putting the product into a vacuum drier to obtain the inner phase choline chloride-urea eutectic solvent mixture. Nuclear magnetic hydrogen spectrum of synthesized product (FIG. 1) ChCl-Urea (1: 2):1H NMR(400MHz,DMSO,298.15K),δ(ppm):5.52(s,8H,-NH2),3.82(s,2H,-CH2-),3.45(s,2H,-CH2-),3.14(s,9H,-CH3) The successful preparation is proved.
Example 2
Screening of shell materials
2g of polydimethylsiloxane and 0.2g of curing agent are mixed uniformly and poured into a glass bottle filled with a proper amount of choline chloride-urea eutectic solvent mixture (figure 2). The two are observed to have obvious layering, the shell material is on the upper layer, the eutectic solvent is on the lower layer, and the shell material has fluidity; after heating for a period of time, the two materials still obviously delaminate, the shell material is well solidified, and the fluidity of the shell material is lost; after standing for a period of time, the shell material and the absorbent still have obvious layering, and the shell material and the absorbent do not react with each other, namely the shell material with good compatibility with the absorbent is screened out. FIG. 3 is an ATR-FITR spectrum of the solidified shell material, and the ATR-FITR spectrum shows that each characteristic absorption peak is obvious and ranges from 1130 cm to 1000cm-1The wide polymer main chain absorption band Si-O-Si between the two is obvious, and the success of thermal crosslinking is proved.
Example 3
Preparation of 240 μm microcapsules
Taking a proper amount of polydimethylsiloxane and a curing agent as an intermediate oil phase, wherein the inner phase is a choline chloride-urea eutectic solvent mixture, and the outer phase is a 75 wt% glycerol aqueous solution (the mass of PVA is 5% of that of glycerol). The injection speed of the injection pump is controlled by the micro-fluidic technology to ensure that the flow rate of the inner phase is 0.6 mu L/min, the flow rate of the intermediate phase is 2 mu L/min and the flow rate of the outer phase is 35 mu L/min, and the microcapsule with the diameter of 240 mu m is prepared. And then thermally crosslinking for 120min at 50 ℃ to obtain the cured microcapsule. Fig. 4 is a view of microfluidic fabrication with a diameter of 240 μm using microfluidic fabrication and an optical microscope of uncured microcapsules.
Example 4
Preparation of 500 μm microcapsules
Taking a proper amount of polydimethylsiloxane and a curing agent as an intermediate oil phase, wherein the inner phase is a choline chloride-urea eutectic solvent mixture, the outer phase is a 75 wt% glycerol aqueous solution (the mass of PVA is 5% of that of glycerol), and the injection speed of a syringe pump is controlled by a micro-fluidic technology so that the flow rate of the inner phase is 0.6 mu L/min, the flow rate of the intermediate phase is 0.8 mu L/min, and the flow rate of the outer phase is 16 mu L/min to prepare microcapsules with the diameter of 500 mu m; and then thermally crosslinking for 120min at 50 ℃ to obtain the cured microcapsule. As shown in fig. 5, the SEM images showed that the prepared microcapsules had a spherical outer surface, and the SEM images taken after the microcapsules were broken showed that the prepared microcapsules had a core-shell structure.
Example 5
Absorption of carbon dioxide by microcapsules
The temperature of the absorption experiment is set to be 35 ℃, and the normal pressure absorption effect of the microcapsules with the diameter of 240 mu m, the microcapsules with the diameter of 500 mu m and the unencapsulated choline chloride-urea eutectic solvent mixture is respectively measured. The results in FIGS. 6 and 7 show that the same absorption temperature was 35 ℃ and that the absorption capacity of the 240 μm microcapsules was 40.01mgCO after equilibrium of absorption when the pressure in the tank reached 1 atmosphere2The absorption effect of the/gDES is about 3.32mgCO of the eutectic solvent (DES group) which is not encapsulated into a microcapsule213 times/gDES and 26 times the absorption rate.
Example 6
Absorption of carbon dioxide by microcapsules
The temperature of the absorption experiment is set to 35 ℃, the normal pressure absorption effects of the microcapsules with the diameter of 240 mu m, the microcapsules with the diameter of 500 mu m and the unencapsulated choline chloride-urea eutectic solvent mixture are respectively measured, the results of the figure 6 and the figure 7 show that the same absorption temperature is 35 ℃, when the pressure in the kettle reaches 1 atmosphere, the absorption effect of the microcapsules with the diameter of 500 mu m is 35.24mgCO after the absorption is balanced2The absorption effect of the/gDES is about 3.32mgCO of the eutectic solvent (DES group) which is not encapsulated into a microcapsule 210 times the/gDES and 10 times the absorption rate.
Example 7
Cyclic absorption experiment of microcapsules
Putting a proper amount of 240 μm microcapsule into an absorption kettle, absorbing at 35 deg.C for 120min under 1atm, heating to 50 deg.C and maintaining for 120min to completely desorb the microcapsule; the temperature was set at 35 ℃ again, and the above absorption and desorption processes were carried out for 3 cycles. Fig. 8 shows the absorption effect in sequence: 40.01mgCO2/gDES、38.55mgCO2/g DES、33.46mgCO2/g DES、32.56mgCO2the/gDES shows that the prepared microcapsule has good circulation effect and is suitable for industrial application.
Claims (9)
1. A gas absorption microcapsule based on microfluidic and thermal crosslinking technologies is characterized in that the microcapsule is of a core-shell structure, a core layer material is a gas absorbent formed by combining choline salt and a coordination agent, and a shell layer material is a breathable material.
2. Gas-absorbing microcapsules according to claim 1, characterized in that the gas-permeable material comprises tetraethylorthosilicate, polydimethylsiloxane, polysulfone or polystyrene gas-permeable modified with ceramic, zeolite or carbon nanoparticles.
3. A process for the preparation of gas-absorbing microcapsules based on microfluidic and thermal crosslinking techniques according to claim 1, characterized in that it comprises the following steps:
(1) preparing a gas absorbent: taking choline salt and a coordination agent, drying and mixing to obtain a gas absorbent;
(2) preparing the microcapsule: taking the gas absorbent obtained in the step (1) as an internal phase, mixing a breathable material, an emulsifier A and a curing agent to obtain an intermediate phase, taking an emulsifier B aqueous solution as an external phase, obtaining w/o/w double-layer microspheres by a microfluidic technology, and then heating for thermal crosslinking to obtain the gas absorption microcapsule.
4. A method of making gas-absorbing microcapsules according to claim 3 wherein in step (1) the choline salt comprises choline chloride, choline bromide; the complexing agent comprises metal salt, metal salt hydrate and hydrogen bond donor.
5. The method for producing a gas-absorbing microcapsule according to claim 3, wherein in step (1), the molar ratio of the choline salt to the complexing agent is 1:5 to 1: 0.5.
6. The method for producing gas-absorbing microcapsules of claim 3, wherein in the step (2), the mass ratio of the gas-permeable material, the emulsifier A and the curing agent is 10:5:1 to 10:0.5: 1.
7. The method for producing gas-absorbing microcapsules according to claim 3, wherein in the step (2), the emulsifier A comprises Span 20-80 (Span 20-80), sucrose ester, phosphate, soybean phospholipid, and deglycosa.
8. The method for preparing a gas-absorbing microcapsule according to claim 3, wherein in step (2), the emulsifier B comprises Palo-Sam (F-127), Tween 20-80 (T-20-80), polyvinyl alcohol (PVA), polyoxyethylene ether.
9. Use of gas-absorbing microcapsules based on microfluidic and thermal cross-linking technologies according to claim 1, characterized in that they are applicable to the absorption of greenhouse gases.
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