CN108339522B - Amino acid @ Cu-BTC composite adsorbent and preparation method thereof - Google Patents
Amino acid @ Cu-BTC composite adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of adsorption materials, and discloses an amino acid @ Cu-BTC composite adsorbent and a preparation method thereof. Adding nano ZnO into deionized water, performing ultrasonic dispersion, and adding DMF to obtain a ZnO nano slurry solution; adding Cu (NO)3)2·3H2Dissolving O and amino acid in deionized water to obtain Cu (NO)3)2And an amino acid mixture; dissolving trimesic acid in ethanol to obtain a trimesic acid solution; adding Cu (NO)3)2Adding the amino acid and the mixed solution of the amino acid into the ZnO nano slurry solution, stirring and mixing uniformly, adding a trimesic acid solution for reaction, and performing vacuum activation on the obtained solid product to obtain the amino acid @ Cu-BTC composite adsorbent. The amino acid @ Cu-BTC composite adsorbent prepared by the invention has excellent water vapor stability and high CO2Adsorption capacity.
Description
Technical Field
The invention belongs to the technical field of adsorption materials, and particularly relates to an amino acid @ Cu-BTC composite adsorbent and a preparation method thereof.
Background
With the development of global industrialization, a large amount of CO is generated2Is discharged into the atmosphere, causes environmental problems such as greenhouse effect, global climate abnormity, sea level rise, frequent natural disasters, land desertification and the like, and has serious influence on the survival of human beings and the development of society all around the world. Thus, for CO2The effective capture and emission reduction become one of the hot topics researched by the scholars today. Currently capturing CO2The adopted technologies mainly comprise a low-temperature distillation method, a membrane separation method, a chemical absorption method, a physical adsorption method, a catalytic combustion method and the like. The physical adsorption method can be used for separation under the conditions of normal temperature and normal pressure, is more energy-saving and efficient, and is considered to be a novel separation method with the greatest industrial application prospect.
The adsorbent is critical in the adsorptive separation process and its performance will determine the efficiency and energy consumption of the separation process. Can be applied to CO at present2Trapped adsorbentThere are mainly traditional adsorbents such as zeolites and activated carbon, and emerging porous materials such as metal organic framework Materials (MOFs) and the like. Compared with the traditional adsorbent, the metal organic framework Materials (MOFs) have good application prospect in the adsorption separation of gas due to the characteristics of larger specific surface area, higher porosity, adjustable pore channels, easy surface functionalization modification and the like. Among them, Cu-BTC (also called HKUST-1) is one of MOFs material having excellent adsorption property to gas under normal temperature and pressure. Aprea et al reported that Cu-BTC was responsible for CO at 283K and 1bar2The Adsorption capacity of the adsorbent is up to 7.0mmol/g (P Aprea, D Caputo, N Gargiulo, et al]J Chem Eng Data,2010,55(9):3655-3661), is currently recognized as adsorbing CO at low pressure2One of the best performing MOF materials; in addition, Cu-BTC also has good adsorption performance for VOCs and ethylene/ethane. The adsorption performance of Cu-BTC is far higher than that of the traditional activated carbon, molecular sieve and silica gel adsorption material. However, in practical applications, water vapor is ubiquitous, and the moisture stability of Cu-BTC is very poor. Upon exposure to moisture, the Cu-O bond in Cu-BTC is broken due to attack by Water molecules, resulting in structural collapse (n.c. burtch, h.jasuja, k.s. walton, Water stability and association in metal-organic frameworks J]Chem Rev,114(2014) 10575-10612). Therefore, how to enhance the moisture stability of Cu-BTC has become one of the hot topics studied by many scholars. Sheets et al coated the surface of Cu-BTC with hydrophobic silane (W.Zhang, Y.Hu, J.Ge, H.L.Jiang, S.H.Yu, A surface and general coating to mole/water-resist metal-organic structures with interaction porosity, Journal of the American Chemical Society,136(2014) 16926) at 235 deg.C by vapor deposition technique, and the PDMS-modified material maintained good stability after 1 day contact with 55% relative humidity air, but no adsorption was reported. Al-Janabi et Al, applied post-synthesis modification method, grafting glycine onto Cu-BTC, and as a result, found that the material produced was at atmospheric pressureLower pair of CO2The adsorption capacity of the catalyst is reduced To only 2.2mmol/g, and is also lower than that of a common carbon material and molecular sieve (N.Al-Janabi, H.Deng, J.Borges, X.Liu, A.Garforth, F.R.Siperstein, X.Fan, A surface Post-synthetic modification Method To improved Hydrothermal Stability and CO2 selection of Cu metallic-Organic Framework, Industrial grade&Engineering Chemistry Research,55(2016)7941- > 7949.). The Liyujie and the like use a mechanical method to prepare a Cu-BTC @ GO composite material of Cu-BTC and graphite oxide, and the composite material still has the thickness of 1000m after being soaked in water for 10 hours2BET specific surface area/g, water stability is greatly improved (Y.Li, J.Miao, X.Sun, J.Xiao, Y.Li, H.Wang, Q.Xia, Z.Li, Michaochemical synthesis of Cu-BTC @ GO with enhanced water stability and tolumene addition [ J.]Chemical Engineering journal.2016,298: 191-7). Therefore, a method for improving the stability of water vapor and enhancing the stability to CO is developed2The adsorbing material with the adsorption performance has better application prospect in the aspect of adsorption and separation.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a preparation method of an amino acid @ Cu-BTC composite adsorbent.
The invention also aims to provide the amino acid @ Cu-BTC composite adsorbent prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an amino acid @ Cu-BTC composite adsorbent comprises the following preparation steps:
(1) adding nano ZnO into deionized water, performing ultrasonic dispersion, and adding N, N-Dimethylformamide (DMF) to obtain a ZnO nano slurry solution; adding Cu (NO)3)2·3H2Dissolving O and amino acid in deionized water to obtain Cu (NO)3)2And an amino acid mixture; dissolving trimesic acid in ethanol to obtain a trimesic acid solution;
(2) cu (NO) obtained in the step (1)3)2Adding the mixed solution of the amino acid and the ZnO nano-slurry solution into the mixed solution, and stirring the mixed solutionUniformly mixing, adding a trimesic acid solution, stirring and reacting for 5-10 min to obtain a reaction product, filtering the reaction solution, and sequentially soaking, centrifuging and drying the solid product by using methanol to obtain blue solid powder;
(3) and (3) carrying out vacuum activation on the solid powder obtained in the step (2) to obtain the amino acid @ Cu-BTC composite adsorbent.
Preferably, the ZnO and Cu (NO) in step (1)3)2·3H2The molar ratio of O is 1 (1.25-2).
Preferably, the amino acid in step (1) is glycine (Gly), β -alanine (β -Ala) or gamma-aminobutyric acid (GABA).
Preferably, the volume ratio of the total amount of the deionized water in the step (1) to the DMF to the ethanol is (1-1.1) to (1-1.2) to (1-1.3).
Preferably, the Cu (NO) in step (1)3)2·3H2The molar ratio of O to amino acid is 1 (0.2-0.5).
Preferably, the filtration in step (2) is filtration with an organic filter membrane having an average pore size of 0.45. mu.m.
Preferably, the drying in the step (2) is drying at 60-80 ℃ for 4-8 h.
Preferably, the vacuum activation in the step (3) is vacuum activation at 120-150 ℃ for 8-16 h.
An amino acid @ Cu-BTC composite adsorbent is prepared by the method.
The preparation method and the obtained product have the following advantages and beneficial effects:
(1) the preparation method is simple to operate, easy to realize and good in repeatability; the synthesis reaction can be carried out at normal temperature, the reaction time is short, the completion of the whole synthesis reaction only needs 5-10 min, and the traditional hydrothermal method for synthesizing Cu-BTC needs the reaction time of 1-2 days at 160 ℃.
(2) Compared with the existing Cu-BTC adsorption material, the amino acid @ Cu-BTC composite adsorbent prepared by the invention has excellent water vapor stability and high CO2Adsorption capacity.
Drawings
FIG. 1 shows N of Cu-BTC and the amino acid @ Cu-BTC material obtained in each example2Adsorption and desorption isotherm diagram.
FIG. 2 is an XRD spectrum of Cu-BTC and the amino acid @ Cu-BTC material obtained in each example.
FIG. 3 is an SEM image of Cu-BTC and the amino acid @ Cu-BTC material obtained in each example.
FIG. 4 shows CO of Cu-BTC and the amino acid @ Cu-BTC material obtained in each example2Adsorption isotherm plot.
Fig. 5 is an XRD pattern of Cu-BTC and Gly @ Cu-BTC obtained in example 1 after 20 days of standing at RH 50%.
FIG. 6 shows CO measured at 298K and 1bar for Cu-BTC and Gly @ Cu-BTC obtained in example 1 in an environment of RH 50% for different days2Adsorption amount change chart.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) Nano ZnO (3.6mmol, n)1) Dissolved in deionized water (8ml, n)2) Adding DMF (16ml, n) after ultrasonic dispersion for 10min3) Obtaining ZnO nano-slurry solution; adding Cu (NO)3)2·3H2O(7.2mmol,n4) And Gly (2.16mmol, n)5) Dissolved in deionized water (8ml, n)6) Obtaining Cu (NO)3)2And a Gly mixture; trimesic acid (3.2mmol, n)7) Dissolved in ethanol (16ml, n)8) Obtaining a trimesic acid solution; wherein the dosage ratio of each substance is (n)2+n6):n3:n8＝1:1:1；n1:n4＝1:2。
(2) Cu (NO) obtained in the step (1)3)2Adding the mixed solution of the organic acid and the Gly into a ZnO nano slurry solution, stirring and mixing uniformly, adding a trimesic acid solution, stirring and reacting for 5-10 min to obtain a blue solution containing a reaction product, filtering the solution by using an organic filter membrane with the average pore diameter of 0.45 mu m, and sequentially soaking solid products in methanolCentrifugation and drying gave a blue solid powder.
(3) And (3) placing the solid powder obtained in the step (2) at 120 ℃ for vacuum activation for 12h to obtain glycine @ Cu-BTC solid powder which is marked as Gly @ Cu-BTC material.
Example 2
(1) Nano ZnO (5.76mmol, n)1) Dissolved in deionized water (8ml, n)2) Adding DMF (19ml, n) after ultrasonic dispersion for 10min3) Obtaining ZnO nano-slurry solution; adding Cu (NO)3)2·3H2O(7.2mmol,n4) And β -Ala (2.88mmol, n)5) Dissolved in deionized water (8ml. n)6) Obtaining Cu (NO)3)2Mixing with β -Ala, adding 3.2mmol of trimesic acid7) Dissolved in ethanol (16ml, n)8) Obtaining a trimesic acid solution; wherein the dosage ratio of each substance is (n)2+n6):n3:n8＝1:1.2:1；n1:n4＝1:1.25。
(2) Cu (NO) obtained in the step (1)3)2And β -Ala mixed solution is added into the ZnO nano-slurry solution, the mixture is stirred and mixed evenly, the trimesic acid solution is added, the mixture is stirred and reacts for 5-10 min to obtain blue solution containing reaction products, the solution is filtered by an organic filter membrane with the average aperture of 0.45 mu m, and the solid products are sequentially soaked in methanol, centrifuged and dried to obtain blue solid powder.
(3) And (3) placing the solid powder obtained in the step (2) at 120 ℃ for vacuum activation for 16h to obtain β -alanine @ Cu-BTC solid powder which is marked as Ala @ Cu-BTC material.
Example 3
Nano ZnO (3.6mmol, n)1) Dissolved in deionized water (8ml, n)2) Adding DMF (16ml, n) after ultrasonic dispersion for 10min3) Obtaining ZnO nano-slurry solution; adding Cu (NO)3)2·3H2O(7.2mmol,n4) And GABA (2.88mmol, n)5) Dissolved in deionized water (8ml, n)6) Obtaining Cu (NO)3)2And a GABA mixture; trimesic acid (3.2mmol, n)7) Dissolved in ethanol (21ml, n)8) Obtaining a trimesic acid solution; wherein each one ofThe dosage ratio of the substances is (n)2+n6):n3:n8＝1:1:1.3；n1:n4＝1:2。
(2) Cu (NO) obtained in the step (1)3)2And adding the GABA mixed solution into the nano-slurry ZnO solution, stirring and mixing uniformly, adding a trimesic acid solution, stirring and reacting for 5-10 min to obtain a blue solution containing a reaction product, filtering the solution by using an organic filter membrane with the average pore diameter of 0.45 mu m, and sequentially soaking, centrifuging and drying the solid product by using methanol to obtain blue solid powder.
(3) And (3) placing the solid powder obtained in the step (2) at 150 ℃ for vacuum activation for 8h to obtain gamma-aminobutyric acid @ Cu-BTC solid powder which is marked as GABA @ Cu-BTC material.
The pore structure of the amino acid @ Cu-BTC material prepared in the above example was characterized using an ASAP2460 specific surface pore size distributor, manufactured by Micromeritics, USA. FIG. 1 shows the materials prepared in all examples and the N of Cu-BTC at 77K2And (3) an adsorption and desorption isotherm, wherein information such as the specific surface area, the pore volume and the like of the material can be calculated according to the isotherm, and the obtained structural information is listed in table 1. As can be seen from the results shown in FIG. 1 and Table 1, the BET specific surface area of the amino acid @ Cu-BTC material prepared by the invention is about 1715-1820 m2The total pore volume is 0.75-0.80 cm3(ii) in terms of/g. This shows that the material prepared by the invention has higher specific surface area and larger pore volume.
TABLE 1
FIG. 2 is an XRD pattern of all the materials prepared in examples and Cu-BTC, and it can be seen from the figure that all the materials show three characteristic diffraction peaks at 2 theta 6.8 degrees, 9.6 degrees and 11.8 degrees, which are substantially identical to the characteristic diffraction peaks reported in the literature for Cu-BTC (C.Petit, B.Mendoza, T.J.Bandosz, Reactive adsorption of amonia on Cu-based MOF/graphene composites [ J ], Langmuir,26(2010)15302-15309), indicating that the amino acid @ Cu-BTC prepared by the present invention has a similar crystal structure to the original Cu-BTC.
FIG. 3 is an SEM image of the materials prepared in all the examples and the Cu-BTC material, and it can be seen that these materials have a regular octahedral structure.
FIG. 4 is the CO at 298K for all the materials prepared in the examples and Cu-BTC2Adsorption isotherm plot. As can be seen from the figure, the example material is paired with CO compared to the original Cu-BTC2The adsorption capacity of (a) is higher.
Fig. 5 is an XRD pattern of Cu-BTC and Gly @ Cu-BTC obtained in example 1 after being left in an environment of 50% RH for 20 days. As can be seen from the figure, after being placed for 20 days, the XRD characteristic peak of the original Cu-BTC has basically disappeared, which indicates that the structure of the Cu-BTC has collapsed; the Gly @ Cu-BTC material prepared in example 1 is kept unchanged after being placed for 20 days, which indicates that the material still has a good crystal structure.
FIG. 6 shows the CO measured at 298K and 1bar for Cu-BTC and Gly @ Cu-BTC obtained in example 1 in an environment of 50% RH for different days2Adsorption amount change chart. As can be seen from the figure, the CO of Cu-BTC is observed after 20 days of standing2The adsorption amount is greatly reduced, and is only 9.12 percent of that of fresh Cu-BTC, which indicates that the water vapor stability of the Cu-BTC is poor; the Gly @ Cu-BTC material prepared in example 1 had CO content after being placed in an RH 50% environment for 20 days2The adsorption capacity is still 81.48 percent of the original adsorption capacity, which shows that the water vapor stability of the Gly @ Cu-BTC material is greatly enhanced.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of an amino acid @ Cu-BTC composite adsorbent is characterized by comprising the following preparation steps:
(1) adding nano ZnO into deionized water, performing ultrasonic dispersion, and adding DMF to obtain a ZnO nano slurry solution; adding Cu (NO)3)2·3H2Dissolving O and amino acid in deionized water to obtain Cu (NO)3)2And an amino acid mixture; dissolving trimesic acid in ethanol to obtain a trimesic acid solution;
(2) cu (NO) obtained in the step (1)3)2Adding the amino acid mixed solution into the ZnO nano slurry solution, stirring and mixing uniformly, adding a trimesic acid solution, stirring and reacting for 5-10 min to obtain a reaction product, filtering the reaction solution, and sequentially soaking, centrifuging and drying the solid product by using methanol to obtain blue solid powder;
(3) carrying out vacuum activation on the solid powder obtained in the step (2) to obtain an amino acid @ Cu-BTC composite adsorbent;
in the step (1), the ZnO and the Cu (NO) are3)2·3H2The molar ratio of O is 1 (1.25-2); the Cu (NO)3)2·3H2The molar ratio of O to amino acid is 1 (0.2-0.5);
the amino acid in the step (1) is glycine, β -alanine or gamma-aminobutyric acid.
2. The method for preparing the amino acid @ Cu-BTC composite adsorbent according to claim 1, wherein the method comprises the following steps: the volume ratio of the total amount of the deionized water in the step (1) to the DMF to the ethanol is (1-1.1) to (1-1.2) to (1-1.3).
3. The method for preparing the amino acid @ Cu-BTC composite adsorbent according to claim 1, wherein the method comprises the following steps: the filtration in the step (2) means filtration with an organic filter having an average pore size of 0.45. mu.m.
4. The method for preparing the amino acid @ Cu-BTC composite adsorbent according to claim 1, wherein the method comprises the following steps: the drying in the step (2) is drying for 4-8 hours at the temperature of 60-80 ℃.
5. The method for preparing the amino acid @ Cu-BTC composite adsorbent according to claim 1, wherein the method comprises the following steps: the vacuum activation in the step (3) is vacuum activation for 8-16 h at 120-150 ℃.
6. An amino acid @ Cu-BTC composite adsorbent, which is characterized in that: prepared by the method of any one of claims 1 to 5.
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