CN111420640B - HKUST-1 composite material and preparation method thereof - Google Patents
HKUST-1 composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an HKUST-1 composite material and a preparation method thereof, wherein the method comprises the following steps: s1, adding deionized water and absolute ethyl alcohol into 7.3-29.3 parts of hydrotalcite powder and 4-7 parts of graphene oxide, and ultrasonically mixing uniformly to obtain slurry A; s2, adding 70-100 parts of copper nitrate trihydrate into deionized water, and stirring for dissolving to obtain solution B; s3, dissolving 30-50 parts of trimesic acid in DMF, and uniformly stirring to obtain solution C; s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and stirring for reaction; and S5, carrying out centrifugal separation to obtain the HKUST-1 composite material. The HKUST-1 composite material and the preparation method thereof have the advantages that the reaction speed is high, the mass production is easy, the reaction condition is simple, the reaction can be realized at normal temperature and normal pressure, and the obtained HKUST-1 has a larger microporous structure and can improve the adsorption capacity to benzene.
Description
Technical Field
The invention relates to the technical field of metal organic framework materials, in particular to an HKUST-1 composite material and a preparation method thereof.
Background
Metal-organic Frameworks (MOFs for short) are a class of crystalline materials, which are composed of coordination bonds between transition Metal cations and multidentate organic linkers to form porous materials with one-dimensional, two-dimensional or three-dimensional structures. Compared with other porous materials, the MOFs provide unique structural diversity, can successfully control framework topology, porosity and function, have large specific surface area and high porosity, can adjust pore size through a special preparation mode and are modified through functional groups, and therefore have wide application, such as gas storage, gas adsorption separation, asymmetric catalysis, biomedicine and luminescent materials, particularly HKUST-1, and are more advantageous due to high specific surface area.
The existing preparation methods of MOFs include hydrothermal synthesis methods, ultrasonic synthesis methods, mechanical synthesis methods and microwave synthesis methods, wherein the hydrothermal synthesis methods have high temperature and pressure and long time, the ultrasonic methods have short time but are difficult to control the product structure, the mechanical synthesis methods require special equipment, and the microwave synthesis methods can control the product shape and size but cannot realize mass production. In addition, most of the MOFs synthesized by the method are microporous materials, the pore diameter of micropores is small, the rapid diffusion of small molecules is not facilitated, the application of the MOFs materials to the aspect of macromolecular adsorption is limited, the pore volume is insufficient, and the chemical stability needs to be improved. Moreover, the existing synthesis methods are carried out under a certain temperature condition, and the reaction time is long. It is seen that improvements and enhancements in the prior art are needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a preparation method of an HKUST-1 composite material, and aims to overcome the defects that the existing preparation method of the HKUST-1 is long in time and cannot be carried out at normal temperature, the prepared HKUST-1 has small pore volume, and the adsorption capacity needs to be improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing an HKUST-1 composite, wherein the method comprises the steps of:
s1, adding deionized water and absolute ethyl alcohol into 7.3-29.3 parts of hydrotalcite powder and 4-7 parts of graphene oxide, and ultrasonically mixing uniformly to obtain slurry A;
s2, taking 70-100 parts of copper nitrate trihydrate, adding deionized water according to the weight ratio of the copper nitrate trihydrate to the deionized water of 1: 5, and stirring for dissolving to obtain solution B;
s3, dissolving 30-50 parts of trimesic acid in DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and stirring for reaction;
and S5, carrying out centrifugal separation to obtain the HKUST-1 composite material.
In the preparation method of the HKUST-1 composite material, the weight ratio of the graphene oxide to the copper nitrate trihydrate is 1-4: 10-13.7.
In the preparation method of the HKUST-1 composite material, the weight ratio of the hydrotalcite powder to the graphene oxide in the step S1 is 1.8-7.3: 1-1.75.
In the preparation method of the HKUST-1 composite material, the solid-to-liquid ratio of the hydrotalcite powder and the graphene oxide solid to the mixed solution of the deionized water and the absolute ethyl alcohol in the step S1 is 1-3.2: 90-130, and the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 2.
In the preparation method of the HKUST-1 composite material, the ultrasonic time in the step S1 is 10-15 min.
In the preparation method of the HKUST-1 composite material, the mass ratio of the trimesic acid to the DMF in the step S3 is 1: 40.
In the preparation method of the HKUST-1 composite material, the reaction time in the step S4 is 1-5 min.
In the preparation method of the HKUST-1 composite material, a purification step is further arranged after the step S5, and the purification step sequentially adopts absolute ethyl alcohol, DMF and methanol for multiple times of cleaning, then centrifugal separation and vacuum drying are carried out, so that the purified HKUST-1 composite material is obtained.
In the preparation method of the HKUST-1 composite material, the vacuum drying step comprises the following steps: vacuum drying at 40 deg.C for 4 hr, and vacuum drying at 150 deg.C for 12 hr.
An HKUST-1 composite material prepared by the preparation method.
Has the beneficial effects that:
the invention provides an HKUST-1 composite material and a preparation method thereof, the method is simple to operate and easy to realize, the synthesis speed of HKUST-1 is greatly accelerated by adding hydrotalcite and graphene oxide, the preparation process can be completed in a short time, and industrial mass production is facilitated, in addition, the preparation process does not need heating and can be carried out under the conditions of normal temperature and normal pressure, the energy consumption is greatly reduced, the cost is saved, more importantly, the added graphene oxide can obtain a larger micropore structure, and the adsorption capacity of metal-organic materials to benzene is greatly improved.
Drawings
FIG. 1 is an XRD spectrum of HKUST-1 prepared in examples 1-3 of the present invention;
FIG. 2 is an SEM photograph of HKUST-1-a obtained in example 1;
FIG. 3 is an SEM photograph of HKUST-1-b obtained in example 2;
FIG. 4 is an SEM photograph of HKUST-1-c obtained in example 3;
FIG. 5 is a graph of adsorption isotherms for benzene.
Detailed Description
The invention provides an HKUST-1 composite material and a preparation method thereof, and in order to make the purposes, technical schemes and effects of the invention clearer and clearer, the invention is further described in detail by referring to the attached drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A method of preparing an HKUST-1 composite, the method comprising the steps of:
and S1, adding deionized water and absolute ethyl alcohol into 7.3-29.3 parts of hydrotalcite powder and 4-7 parts of graphene oxide, and ultrasonically mixing uniformly to obtain slurry A. In the step, the solid-to-liquid ratio of the hydrotalcite powder and the graphene oxide solid to the mixed solution of the deionized water and the absolute ethyl alcohol is 1-3.2: 90-130, and the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 2.
And S2, taking 70-100 parts of copper nitrate trihydrate, adding deionized water according to the weight ratio of the copper nitrate trihydrate to the deionized water of 1: 5, and stirring for dissolving to obtain solution B.
S3, dissolving 30-50 parts of trimesic acid, taking DMF according to the mass ratio of 1: 40 of trimesic acid to DMF, dissolving trimesic acid in DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and stirring for reaction for 1-5 min;
and S5, carrying out centrifugal separation, sequentially adopting absolute ethyl alcohol, DMF (dimethyl formamide) and methanol to carry out cleaning and purification for multiple times, then carrying out centrifugal separation and vacuum drying to obtain the purified HKUST-1 composite material.
In the preparation method of the HKUST-1 composite material, the preparation is carried out under the conditions of normal temperature and normal pressure, heating and special equipment are not needed, and the graphene oxide and the hydrotalcite are added in the preparation process, so that the reaction speed is greatly increased, the preparation time is shortened, the specific surface area and the porosity of the material are increased, the adsorption capacity is increased by 10% compared with the conventional HKUST-1 without the graphene oxide and the hydrotalcite, and the preparation method is simple to operate and easy to realize.
In the preparation method, the weight ratio of the graphene oxide to the copper nitrate trihydrate is 1-4: 10-13.7. Because the oxidized graphene is of a laminated structure and has special surface performance, and the oxidized graphene contains hydroxyl, carboxyl and carbonyl, the oxidized graphene is easily combined with copper, so that the metal organic framework material forms a multi-dimensional topological network structure, the pore diameter structure of the metal organic framework is richer, and the void ratio is improved. The addition amount of the graphene oxide affects the crystal structure of the composite material, can increase the pore size, and makes the porous structure of the crystal more complicated, but when the addition amount of the graphene oxide is too large, the graphene oxide competes with a multidentate organic substance, the formation of the structure of an organic-inorganic hybrid crystal is damaged, the crystallinity is reduced, and the adsorption amount is affected. When the weight ratio of the graphene oxide to the copper nitrate trihydrate is 1-4: 10-13.7, a better crystal structure can be obtained, the gaps are large, and the adsorption capacity is high.
In the preparation step, the weight ratio of the hydrotalcite powder to the graphene oxide in the step S1 is 1.8-7.3: 1-1.75. The hydrotalcite is a layered double hydroxide and is a layered compound formed by coordination of cation sheets and inorganic/organic anions. The structural characteristics of hydrotalcite make it have excellent anion exchange performance, and can exchange with various anions, including inorganic ions, organic ions, homogeneous ions, heteropoly acid ions and anions of coordination compounds. In the present inventionBy hydrotalcite and Cu (NO) 3 ) 2 ·3H 2 The rapid reaction of O enables copper ions to enter a layered structure, the structure has excellent ion exchange capacity and extremely high ion exchange rate, the capability of forming coordination bonds between metal ions and ligands can be enhanced, and the rapid synthesis of HKUST-1 is greatly promoted.
Example 1
A method of preparing an HKUST-1 composite, the method comprising the steps of:
s1, adding 7.3 parts of talcum powder and 7 parts of graphene oxide, adding 330 parts of deionized water and 660 parts of absolute ethyl alcohol, and ultrasonically mixing for 10min to obtain slurry A;
s2, taking 70 parts of copper nitrate trihydrate, adding 350 parts of deionized water, and stirring for dissolving to obtain solution B;
s3, dissolving 30 parts of trimesic acid in 1200 parts of DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and reacting for 5min under stirring;
s5, carrying out centrifugal separation on the mixture obtained in the step S4 to obtain a HKUST-1 composite material crude product;
s6, soaking and cleaning the crude HKUST-1 composite material by sequentially adopting absolute ethyl alcohol, DMF and methanol, repeatedly soaking each solvent for at least 5 times, performing centrifugal separation after each soaking, recycling the soaked liquid, performing vacuum drying on solid particles after the soaking and cleaning are completed, performing vacuum drying at 40 ℃ for 4 hours, and performing vacuum drying at 150 ℃ for 12 hours to obtain the HKUST-1 composite material.
Example 2
A method of preparing an HKUST-1 composite, the method comprising the steps of:
s1, taking 15 parts of talcum powder and 5.8 parts of graphene oxide, adding 400 parts of deionized water and 800 parts of absolute ethyl alcohol, and ultrasonically mixing for 12min to obtain slurry A;
s2, adding 440 parts of deionized water into 88 parts of copper nitrate trihydrate, and stirring for dissolving to obtain solution B;
s3, dissolving 42 parts of trimesic acid in 1600 parts of DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and reacting for 8min under stirring;
s5, carrying out centrifugal separation on the mixture obtained in the step S4 to obtain a HKUST-1 composite material crude product;
s6, soaking and cleaning the crude HKUST-1 composite material by sequentially adopting absolute ethyl alcohol, DMF and methanol, repeatedly soaking each solvent for at least 4 times, performing centrifugal separation after each soaking, recycling the soaked liquid, performing vacuum drying on solid particles after the soaking and cleaning are completed, performing vacuum drying at 40 ℃ for 4 hours, and performing vacuum drying at 150 ℃ for 12 hours to obtain the HKUST-1 composite material.
Example 3
A method of preparing an HKUST-1 composite, the method comprising the steps of:
s1, adding 29.3 parts of talcum powder and 4 parts of graphene oxide, adding 500 parts of deionized water and 1000 parts of absolute ethyl alcohol, and ultrasonically mixing for 15min to obtain slurry A;
s2, taking 100 parts of copper nitrate trihydrate, adding 500 parts of deionized water, and stirring for dissolving to obtain solution B;
s3, dissolving 50 parts of trimesic acid in 2000 parts of DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and reacting for 10min under the condition of stirring;
s5, carrying out mixed centrifugal separation on the mixture obtained in the step S4 to obtain a crude HKUST-1 composite material product;
s6, soaking and cleaning the crude HKUST-1 composite material by sequentially adopting absolute ethyl alcohol, DMF and methanol, repeatedly soaking each solvent for at least 4 times, performing centrifugal separation after each soaking, recycling the soaked liquid, performing vacuum drying on solid particles after the soaking and cleaning are completed, performing vacuum drying at 40 ℃ for 4 hours, and performing vacuum drying at 150 ℃ for 12 hours to obtain the HKUST-1 composite material.
Comparative example 1
A method for preparing HKUST-1, said method comprising the steps of:
s1, taking 15 parts of talcum powder, adding 400 parts of deionized water and 800 parts of absolute ethyl alcohol, and ultrasonically mixing for 10min to obtain slurry A;
s2, adding 88 parts of copper nitrate trihydrate, 440 parts of deionized water, and stirring for dissolving to obtain solution B;
s3, dissolving 42 parts of trimesic acid in 1600 parts of DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and reacting for 8min under the condition of stirring;
s5, carrying out centrifugal separation on the mixture obtained in the step S4 to obtain a HKUST-1 composite material crude product;
s6, soaking and cleaning the crude HKUST-1 composite material by sequentially adopting absolute ethyl alcohol, DMF (dimethyl formamide) and methanol, repeatedly soaking each solvent for at least 4 times, performing centrifugal separation after each soaking, recycling the soaked liquid, performing vacuum drying on solid particles after the soaking and cleaning are completed, performing vacuum drying at 40 ℃ for 4 hours, and performing vacuum drying at 150 ℃ for 12 hours to obtain the HKUST-1 material.
Comparative example 2
A method for preparing HKUST-1, comprising the steps of:
s1, taking 5.8 parts of graphene oxide, adding 400 parts of deionized water and 800 parts of absolute ethyl alcohol, and ultrasonically mixing for 12min to obtain slurry A;
s2, adding 88 parts of copper nitrate trihydrate, 440 parts of deionized water, and stirring for dissolving to obtain solution B;
s3, dissolving 42 parts of trimesic acid in 1600 parts of DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and reacting for 60min under stirring;
and S5, carrying out centrifugal separation on the mixture obtained in the step S4 to obtain the HKUST-1 product.
It can be seen that, when talc was not added, the HKUST-1 product could not be obtained at all by producing it in a shorter time under conventional conditions, and thus it can be seen that hydrotalcite is a key factor for accelerating the reaction.
The HKUST-1 composite material obtained in the above examples 1-3 was subjected to structural characterization and performance tests, and the results were as follows:
(1) XRD analysis: the HKUST-1 composites obtained in examples 1-3 were designated HKUST-1-a, HKUST-1-b, HKUST-1-c, and then subjected to XRD test, the results of which are shown in FIG. 1.
As can be seen from figure 1, HKUST-1-a, HKUST-1-b and HKUST-1-c all show strong crystallinity, the peak position of each peak is consistent with the characteristic peak of the simulated HKUST-1, and the obtained crystal is proved to be the HKUST-1 crystal.
(2) SEM analysis: scanning electron microscope analysis is carried out on HKUST-1-a, HKUST-1-b and HKUST-1-c, and the test results are shown in figure 2, figure 3 and figure 4. As can be seen from FIGS. 2, 3 and 4, HKUST-1-a, HKUST-1-b and HKUST-1-c each exhibited a typical regular octahedral morphology and increased with the addition of hydrotalcite.
(3) Analysis of pore structure parameters: the structural parameters of HKUST-1-a, HKUST-1-b and HKUST-1-c were determined, and the results are shown in Table 1.
TABLE 1 pore Structure parameters of HKUST-1
As can be seen from Table 1, HKUST-1-a, HKUST-1-b and HKUST-1-c are larger than those of comparative example 1, and the pore volume thereof can reach 0.7cm 3 Comparative example 1, which is above/g, without the addition of graphene oxide, has significantly smaller pore volume.
(4) Adsorption property to benzene
Adsorption tests of benzene were carried out at 25 ℃ for HKUST-1-c and comparative example 1, and each adsorption isotherm is shown in FIG. 5. As can be seen from FIG. 5, the saturated adsorption amount of comparative example 1 was 6.43mmol/g, while that of HKUST-1-b was 7.22mmol/g, which is an improvement of almost 10%. The oxygen-containing functional groups of the composite graphite oxide are rich, so that adsorption sites are increased, and the benzene adsorption capacity is improved.
It should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (8)
1. A method for preparing HKUST-1 composite material, which is characterized by comprising the following steps:
s1, adding deionized water and absolute ethyl alcohol into 7.3-29.3 parts of hydrotalcite powder and 4-7 parts of graphene oxide, wherein the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 2, and ultrasonically mixing uniformly to obtain slurry A;
s2, taking 70-100 parts of copper nitrate trihydrate, adding deionized water according to the weight ratio of the copper nitrate trihydrate to the deionized water of 1: 5, and stirring for dissolving to obtain solution B;
s3, dissolving 30-50 parts of trimesic acid in DMF, and uniformly stirring to obtain solution C;
s4, under the condition of stirring, sequentially adding the solution B and the solution C into the mixed solution A, and stirring for reaction for 1-5 min;
and S5, carrying out centrifugal separation to obtain the HKUST-1 composite material.
2. The preparation method of the HKUST-1 composite material according to claim 1, wherein the weight ratio of the graphene oxide to the copper nitrate trihydrate is 1-4: 10-13.7.
3. The preparation method of the HKUST-1 composite material according to claim 1, wherein the weight ratio of the hydrotalcite to the graphene oxide in the step S1 is 1.8-7.3: 1-1.75.
4. The method for preparing HKUST-1 composite material according to claim 1, wherein the time of the ultrasound in step S1 is 10-15 min.
5. The method for preparing HKUST-1 composite material according to claim 1, wherein the mass ratio of trimesic acid to DMF in step S3 is 1: 40.
6. The preparation method of the HKUST-1 composite material according to claim 1, wherein a purification step is further provided after the step S5, and the purification step sequentially comprises washing with absolute ethanol, DMF and methanol for multiple times, centrifuging and vacuum drying to obtain the purified HKUST-1 composite material.
7. The process for the preparation of HKUST-1 composite according to claim 6, characterized in that said step of vacuum drying is: vacuum drying at 40 deg.C for 4 hr, and vacuum drying at 150 deg.C for 12 hr.
8. An HKUST-1 composite material prepared by the method as claimed in any one of claims 1 to 7.
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