CN118059775A - Preparation and application of vermiculite/tannic acid composite aerogel with adjustable surface energy - Google Patents
Preparation and application of vermiculite/tannic acid composite aerogel with adjustable surface energy Download PDFInfo
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- CN118059775A CN118059775A CN202311744934.1A CN202311744934A CN118059775A CN 118059775 A CN118059775 A CN 118059775A CN 202311744934 A CN202311744934 A CN 202311744934A CN 118059775 A CN118059775 A CN 118059775A
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- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000001263 FEMA 3042 Substances 0.000 title claims abstract description 77
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 title claims abstract description 77
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 title claims abstract description 77
- 229940033123 tannic acid Drugs 0.000 title claims abstract description 77
- 235000015523 tannic acid Nutrition 0.000 title claims abstract description 77
- 229920002258 tannic acid Polymers 0.000 title claims abstract description 77
- 229910052902 vermiculite Inorganic materials 0.000 title claims abstract description 72
- 235000019354 vermiculite Nutrition 0.000 title claims abstract description 72
- 239000010455 vermiculite Substances 0.000 title claims abstract description 72
- 239000004964 aerogel Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 21
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims abstract description 12
- 229930182817 methionine Natural products 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- VTVVPPOHYJJIJR-UHFFFAOYSA-N carbon dioxide;hydrate Chemical compound O.O=C=O VTVVPPOHYJJIJR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006703 hydration reaction Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 29
- 239000002135 nanosheet Substances 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000000017 hydrogel Substances 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 2
- 239000002064 nanoplatelet Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 18
- 238000003860 storage Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 11
- 230000006911 nucleation Effects 0.000 abstract description 6
- 238000010899 nucleation Methods 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 5
- 239000001257 hydrogen Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 238000007789 sealing Methods 0.000 description 10
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 150000004677 hydrates Chemical class 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
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- 230000004888 barrier function Effects 0.000 description 1
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- 239000004927 clay Substances 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention belongs to the technical application field of aerogel and hydrate, and relates to preparation and application of vermiculite/tannic acid composite aerogel with adjustable surface energy. The vermiculite/tannic acid composite aerogel is used as a carrier to carry methionine solution, so that the methionine solution and carbon dioxide are promoted to form carbon dioxide hydrate under the conditions of low temperature and high pressure. The aerogel prepared by the method disclosed by the invention has the characteristics of high porosity and large specific surface area when being used as a hydrate reaction carrier, the gas-liquid contact area in the reaction process of water and carbon dioxide is obviously improved, rich nucleation sites are provided for hydration reaction, and the generation kinetics of carbon dioxide hydrate is obviously enhanced. In addition, the surface energy of the vermiculite/tannic acid composite aerogel can be regulated and controlled by controlling the dosage of tannic acid, the polar component of the surface of the material is reduced, water molecules are induced to form a proper hydrogen bond network on the surface of the aerogel, and the rate of hydrate generation and the gas storage amount are improved. The invention has the advantages of environmental protection, simple process, large gas storage capacity and the like.
Description
Technical Field
The invention belongs to the technical application field of aerogel and hydrate, and relates to preparation and application of vermiculite/tannic acid composite aerogel with adjustable surface energy.
Background
The global greenhouse effect is caused by excessive emission of greenhouse gases represented by carbon dioxide, and the environmental problems such as rising of sea level, desertification of land and the like are caused to bring about wide attention in countries around the world. The safe and efficient capture and sealing of carbon dioxide becomes a research hotspot in the front of science and the key problems to be solved urgently.
The method for capturing and sealing the carbon dioxide by using the hydrate method is a safe and environment-friendly method for capturing and sealing the carbon dioxide by using water as a medium. However, mass transfer limitations and slow formation kinetics of the reaction interface limit practical applications of the hydrate process. Hossein Dashti et al mention that RECENT ADVANCES IN GAS HYDRATE-based CO 2 capture, by introducing an accelerator into the system to achieve heterogeneous nucleation of hydrates, can significantly reduce the induction time of hydrate formation and increase the hydrate formation rate, and is a hot spot problem in recent years of research in the field of hydrates. The surface energy is a key property of a reaction interface and has important influence on the nucleation and growth processes of the hydrate. Sijia Qin et al in Can solid surface energy be a predictor of ice nucleation ability, mention that the free energy barrier in heterogeneous nucleation processes is low and that most nucleation processes in the liquid phase are triggered by interfaces. By regulating the surface energy of the material surface, water molecules are induced to form an ordered hydrogen bond network in the solid material, so that the method is an effective method for strengthening the hydrate formation kinetics.
The invention reports a preparation method of vermiculite/tannic acid composite aerogel with adjustable surface energy and practical application thereof in the field of capturing and sealing carbon dioxide by a hydrate method, and the vermiculite nano sheets and tannic acid are assembled into the vermiculite/tannic acid composite aerogel with high porosity and adjustable surface energy by a material treatment method of ion crosslinking and freeze drying, so that the generation kinetics of a carbon dioxide hydrate is obviously enhanced.
Disclosure of Invention
The invention aims to overcome the defects and problems of slow generation kinetics in the existing carbon dioxide trapping and sealing process by a hydrate method, and provides a method for realizing efficient carbon dioxide trapping and sealing by the hydrate method by taking aerogel as a carrier. The vermiculite/tannic acid composite aerogel with adjustable surface energy is prepared by using cheap and easily available clay as a framework and using tannic acid to regulate the surface property of the material. The prepared sample remarkably strengthens the hydrate formation kinetics, and provides reference and guidance for the practical application of capturing and sealing carbon dioxide by a hydrate method and the design and construction of an accelerator.
The technical scheme of the invention is as follows:
a preparation method of vermiculite/tannic acid composite aerogel with adjustable surface energy comprises the following steps:
mixing vermiculite nano sheet dispersion liquid obtained by liquid phase stripping, tannic acid solution and deionized water to obtain mixed solution; dripping AlCl 3 solution to obtain vermiculite/tannic acid composite hydrogel; freeze-drying the obtained hydrogel to obtain vermiculite/tannic acid composite aerogel;
further, the concentration of the tannic acid solution is 100mg/mL, and the concentration of the vermiculite nano sheet dispersion liquid is 30mg/mL.
Further, the concentration of the vermiculite nano sheet in the mixed solution is 10mg/mL.
Further, tannic acid in the vermiculite/tannic acid composite aerogel accounts for 5-40% of the mass of the vermiculite nano sheets, and preferably 20-35%.
Further, the concentration of the AlCl 3 solution is 0.5mol/L, and the mass ratio of the amount of the substances of AlCl 3 to vermiculite is controlled to be 0.1mmol/60mg.
Further, the vermiculite/tannic acid composite aerogel is compressed, and the volume reduced after compression accounts for 25-50% of the original volume.
The application of vermiculite/tannic acid composite aerogel with adjustable surface energy comprises placing the obtained vermiculite/tannic acid composite aerogel in a high-pressure reaction kettle, dropwise adding methionine solution, sealing, and placing the high-pressure reaction kettle in a temperature-controlled water bath for cooling; after the temperature is stable, high-pressure carbon dioxide gas is injected into the high-pressure reaction kettle after the carbon dioxide gas is purged, and the hydrate generation reaction is carried out until the temperature and the pressure in the reaction kettle are stable, and the hydration reaction is completed.
Further, the initial reaction pressure during the formation of the carbon dioxide hydrate was 3.3MPa, and the initial reaction temperature was 273.15K.
Further, the concentration of the methionine solution is 3mg/mL, and the adding volume of the methionine solution is controlled to account for 25% of the total volume of the vermiculite/tannic acid composite aerogel.
The invention has the beneficial effects that: aerogel is selected as a hydrate generation carrier, so that heterogeneous nucleation of the carbon dioxide hydrate is realized, the gas-liquid contact area in the reaction process is increased, and the hydrate generation kinetics is obviously enhanced. The introduction of tannic acid can accurately regulate and control the surface energy of the material, and by reducing the polar component of the surface of the material, water molecules are induced to form an ordered hydrogen bond network on the surface of the solid material, so that the induction time of the reaction is shortened, and the gas storage capacity is improved. In addition, the pore distribution of the material can be adjusted by compressing the aerogel to a certain extent, so that the gas storage capacity is further improved, and the application potential of the material is improved.
Drawings
FIG. 1 is a graph showing the change in surface energy of vermiculite/tannic acid composite aerogel at various tannic acid contents.
FIG. 2 is a graph showing the polarity component change of vermiculite/tannic acid composite aerogel at various tannic acid contents.
FIG. 3 is a graph showing the variation of dispersion components of vermiculite/tannic acid composite aerogel at various tannic acid contents.
FIG. 4 is a graph showing the change in gas storage capacity of vermiculite/tannic acid composite aerogel at various tannic acid contents.
FIG. 5 is a graph showing the change in gas storage capacity of vermiculite/tannic acid composite aerogel having a tannic acid content of 20% at various compression ratios.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but is not limited to the following examples.
Example 1:
The preparation and application of the vermiculite/tannic acid composite aerogel with adjustable surface energy comprise the following steps:
s1, preparing vermiculite/tannic acid composite aerogel
Mixing the vermiculite nano sheet dispersion liquid (30 mg/mL) obtained by liquid phase stripping with tannic acid solution (100 mg/mL) and deionized water, and dripping AlCl 3 solution (0.5 mol/L) to obtain the vermiculite/tannic acid composite hydrogel. Wherein, after the vermiculite nano sheet dispersion liquid is mixed with tannic acid solution and deionized water, the mass ratio of the vermiculite nano sheets is 10mg/mL, and the mass ratio of tannic acid to the vermiculite nano sheets is 0%, 5%, 10%, 20% and 40%. And freeze-drying the obtained hydrogel to obtain the vermiculite/tannic acid composite aerogel.
S2, surface energy measurement
And analyzing physical parameters such as material surface energy, polar component, nonpolar component and the like of the obtained vermiculite/tannic acid composite aerogel by using a surface energy meter.
As shown in fig. 1,2, 3, when the tannic acid content is increased from 0wt% to 40wt%, the polar component is reduced from 7.1mJ/m 2 to 4.0mJ/m 2, the dispersion component stabilizes around 41mJ/m 2, and thus the surface energy is reduced and the proportion of the polar component to the surface energy is reduced. The highly polar solid surface can disrupt the ordered arrangement of hydrogen bonds between water molecules, thereby inhibiting the formation of hydrates.
Example 2:
The preparation and application of the vermiculite/tannic acid composite aerogel with adjustable surface energy comprise the following steps:
s1, preparing vermiculite/tannic acid composite aerogel
Mixing the vermiculite nano sheet dispersion liquid (30 mg/mL) obtained by liquid phase stripping with tannic acid solution (100 mg/mL) and deionized water, and dripping AlCl 3 solution (0.5 mol/L) to obtain the vermiculite/tannic acid composite hydrogel. Wherein, after the vermiculite nano sheet dispersion liquid is mixed with tannic acid solution and deionized water, the mass ratio of the vermiculite nano sheets is 10mg/mL, and the mass ratio of tannic acid to the vermiculite nano sheets is 0%, 5%, 10%, 20% and 40%. And freeze-drying the obtained hydrogel to obtain the vermiculite/tannic acid composite aerogel.
S2, surface energy measurement
And analyzing physical parameters such as material surface energy, polar component, nonpolar component and the like of the obtained vermiculite/tannic acid composite aerogel by using a surface energy meter.
S3, generation of carbon dioxide hydrate
And (3) placing the vermiculite/tannic acid composite aerogel obtained in the step (S1) in a high-pressure reaction kettle, dropwise adding a methionine solution (3 mg/mL), sealing, and placing the reaction kettle in a temperature-controlled water bath for cooling, wherein the dosage of the methionine solution is 1.5mL of the solution/6 cm 3 of aerogel. After the temperature is stable, the high-pressure carbon dioxide gas is injected after the carbon dioxide gas is purged, and the hydrate generation reaction is carried out under the conditions of 3.3MPa and 273.15K until the temperature and the pressure in the reaction kettle are stable, and the hydration reaction is considered to be completed.
As shown in fig. 4, the presence of tannic acid in the composite aerogel can significantly increase the carbon dioxide absorption capacity. Of the samples prepared, the sample with 20% tannic acid had the highest gas storage of 130.1v/v, while the sample with 0% tannic acid had the lowest gas storage of 50.9v/v. The rich hydroxyl groups of the vermiculite nano sheets enable the surface of the vermiculite to have higher polarity, so that ordered hydrogen bond networks among water molecules are broken, and the gas storage capacity is reduced. Along with the rising of the content of tannic acid, the polarity component of the surface covered by tannic acid is obviously reduced, and the water molecules are easier to form a cage structure of the hydrate, so that the hydrate generation kinetics is obviously enhanced, and the gas storage capacity and the reaction rate are improved.
Example 3:
The preparation and application of the vermiculite/tannic acid composite aerogel with adjustable surface energy comprise the following steps:
s1, preparing vermiculite/tannic acid composite aerogel
Mixing the vermiculite nano sheet dispersion liquid (30 mg/mL) obtained by liquid phase stripping with tannic acid solution (100 mg/mL) and deionized water, and dripping AlCl 3 solution (0.5 mol/L) to obtain the vermiculite/tannic acid composite hydrogel. After the vermiculite nano sheet dispersion liquid is mixed with the tannic acid solution and the deionized water, the mass ratio of the vermiculite nano sheets is 10mg/mL, and the mass ratio of the tannic acid to the vermiculite nano sheets is 20%. And freeze-drying the obtained hydrogel to obtain the vermiculite/tannic acid composite aerogel.
S2, surface energy measurement
And analyzing physical parameters such as material surface energy, polar component, nonpolar component and the like of the obtained vermiculite/tannic acid composite aerogel by using a surface energy meter.
S3, aerogel compression
The prepared aerogel was compressed with a compression ratio of 25% and 50%.
S4, generation of carbon dioxide hydrate
And (3) placing the vermiculite/tannic acid composite aerogel obtained in the step (S1) in a high-pressure reaction kettle, dropwise adding a methionine solution (3 mg/mL), sealing, and placing the reaction kettle in a temperature-controlled water bath for cooling, wherein the dosage of the methionine solution is 1.5mL of the solution/6 cm 3 of aerogel. After the temperature is stable, the high-pressure carbon dioxide gas is injected after the carbon dioxide gas is purged, and the hydrate generation reaction is carried out under the conditions of 3.3MPa and 273.15K until the temperature and the pressure in the reaction kettle are stable, and the hydration reaction is considered to be completed.
As shown in fig. 5, when the compression ratio is increased from 25% to 50%, the gas storage amount is first increased from 136.9v/v to 146.8v/v and then decreased. The pore diameter of the compressed aerogel is reduced, but the damage to the original structure is limited. The reduced pore size slightly reduces the rate of carbon dioxide absorption, the reduced pores prevent rapid formation of carbon dioxide hydrates, and the blockage of carbon dioxide mass transfer is avoided, thereby increasing the gas storage capacity.
Claims (9)
1. The preparation method of the vermiculite/tannic acid composite aerogel with adjustable surface energy is characterized by comprising the following steps:
Mixing vermiculite nano sheet dispersion liquid obtained by liquid phase stripping, tannic acid solution and deionized water to obtain mixed solution; dripping AlCl 3 solution to obtain vermiculite/tannic acid composite hydrogel; and freeze-drying the obtained hydrogel to obtain the vermiculite/tannic acid composite aerogel.
2. The method of claim 1, wherein the concentration of the tannic acid solution is 100mg/mL and the concentration of the vermiculite nanosheet dispersion is 30mg/mL.
3. The method of claim 1, wherein the concentration of the vermiculite nanoplatelets in the mixed solution is 10mg/mL.
4. The method of claim 1, wherein the tannic acid in the vermiculite/tannic acid composite aerogel is 5% -40% of the mass of the vermiculite nano sheets.
5. The preparation method according to claim 1, wherein the concentration of the AlCl 3 solution is 0.5mol/L, and the mass ratio of the amount of AlCl 3 substance to vermiculite is controlled to be 0.1mmol/60mg.
6. The method of claim 1, wherein the vermiculite/tannic acid composite aerogel is compressed to reduce the volume of the compressed aerogel by 25% to 50% of the original volume.
7. The application of the vermiculite/tannic acid composite aerogel with adjustable surface energy is characterized in that the obtained vermiculite/tannic acid composite aerogel is placed in a high-pressure reaction kettle, methionine solution is added dropwise, then the high-pressure reaction kettle is sealed, and the high-pressure reaction kettle is placed in a temperature-controlled water bath for cooling; after the temperature is stable, high-pressure carbon dioxide gas is injected into the high-pressure reaction kettle after the carbon dioxide gas is purged, and the hydrate generation reaction is carried out until the temperature and the pressure in the reaction kettle are stable, and the hydration reaction is completed.
8. The use according to claim 7, wherein the initial reaction pressure during the formation of the carbon dioxide hydrate is 3.3MPa and the initial reaction temperature is 273.15K.
9. The use according to claim 7, wherein the methionine solution has a concentration of 3mg/mL, and the added volume of methionine solution is controlled to be 25% of the total volume of the vermiculite/tannic acid composite aerogel.
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| CN202311744934.1A CN118059775A (en) | 2023-12-18 | 2023-12-18 | Preparation and application of vermiculite/tannic acid composite aerogel with adjustable surface energy |
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| CN202311744934.1A CN118059775A (en) | 2023-12-18 | 2023-12-18 | Preparation and application of vermiculite/tannic acid composite aerogel with adjustable surface energy |
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