CN110404509B - Preparation method of multilayer-structured ILs @ ZIF composite material similar to nano rectifying tower - Google Patents
Preparation method of multilayer-structured ILs @ ZIF composite material similar to nano rectifying tower Download PDFInfo
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Abstract
A preparation method of a quasi-nanometer rectifying tower composite material IL (a) -ZIF-IL (b) based on ILs @ ZIF multilayer structure belongs to the technical field of new materials. The material is a multilayer structure composite material similar to a nanometer rectifying tower formed by two different ionic liquids and ZIF-8 through a specific synthesis method, gas molecules undergo multiple adsorption separation similar to the rectification principle in the mass transfer process, and CO is realized2And N2The results show that CO is separated in a multi-stage step-by-step manner2/N2Has the highest selectivity at normal temperature and normal pressure. In ensuring considerable CO2On the premise of adsorption capacity (40 cc/g), the separation selectivity exceeds that of other conventional porous materials in CO2Performance in terms of separation. The specific synthesis method of the material has stronger innovation, and the material has the best separation performance after being successfully synthesized and tested by experiments. The composite material of the nanometer rectifying tower has important industrial application value in the aspect of gas utilization, and meanwhile, the composite material of the nanometer rectifying tower has important reference significance in the aspects of new material design and synthesis.
Description
Technical Field
The invention belongs to the technical field of new materials, and provides a preparation method of an ILs @ ZIF construction type nanometer rectifying tower composite material (IL (a) -ZIF-IL (b)).
Background
In recent years, carbon dioxide (CO) in air2) The average surface temperature of the earth is gradually increased year by year, the greenhouse effect is gradually increased, and a series of environmental problems caused by the increase of the average surface temperature of the earth are of great concern. To realize CO2The research and development of a clean and effective adsorption material have profound significance for the sustainable development of the future society.
CO commonly used in factories at present2The trapping method mainly depends on absorption by alkali liquor, and has the advantages of strong treatment capacity and high efficiency. But this methodThe method has serious corrosion to equipment, poor regeneration performance, difficult gas recovery and other problems, and limits the CO in the air2Is collected in large quantities. Therefore, there is a need to develop a clean and effective adsorbent for CO in industry2And (4) trapping. The adsorbent based on the novel porous solid material has the advantages of high adsorption quantity, high selectivity, no corrosion to equipment, good regeneration performance, simple and convenient operation and the like in the aspect of gas separation, and arouses the research interest of scientific workers. The composite material has the potential of gas adsorption and separation, such as zeolite, carbon nano tubes, activated carbon, lignin, metal-organic frameworks (MOFs) materials, covalent-organic frameworks (COFs) materials and the like, and particularly the MOFs materials are formed by self-assembling inorganic metal ions or metal clusters and organic ligands, so that the composite material has high specific surface area and porosity, pore channel height adjustability, stable structure and convenience in synthesis, and has potential application prospects in the fields of gas storage, adsorption and separation, chemical sensing, catalysis, absorption of heavy metal ions or organic dyes in wastewater, slow release of drugs and the like.
However, most MOFs are paired with CO2The adsorption capacity or selectivity of the MOFs material is not very high, the adsorption capacity and selectivity can be greatly improved by the MOFs material modified by amino groups, the conventional modification method is amino group grafting or amine impregnation, and the method can also face CO2Induced inactivation or thermodynamic stability. Ionic Liquids (ILs), salts of organic cations and anions which are liquid at ambient temperature or below 373K, are non-volatile and non-toxic, are referred to as green solvents, in CO2Has wide application potential in the aspect of trapping, and the amido functionalized ionic liquid has CO2Equimolar adsorption can be achieved. However, functionalized ILs tend to have a high viscosity, which severely affects the mass transfer rate of the gas. If the ILs are loaded into the MOFs material, the ILs in the nanometer range are formed, the adsorption quantity and the selectivity of the MOFs material are improved, and the mass transfer problem of the ILs is solved. Based on two different ionic liquids and ZIF-8, a multilayer structure composite material similar to a nanometer rectifying tower is synthesized by a specific synthesis method, and gas molecules experience a process similar to a rectifying raw material in the mass transfer processMultiple times of adsorption and separation of CO are realized2And N2The results show that CO is separated in a multi-stage step-by-step manner2 /N2Has the highest separation selectivity at normal temperature and normal pressure. The specific synthesis method of the material has stronger innovation, and experimental tests show that the material has the best separation performance. The composite material of the nanometer rectifying tower has important industrial application value in the aspect of gas utilization, and meanwhile, the composite material of the nanometer rectifying tower has important reference significance in the aspects of new material design and synthesis. .
Disclosure of Invention
The invention aims to provide a preparation method of a composite material similar to a nanometer rectifying tower. A zeolite imidazole framework material (ZIF-8) is used as a framework, and two different ILs are loaded on the inner side and the outer side of the cage-shaped framework respectively to construct a multilayer structure. Each layer structure is to CO2Has the functions of adsorption and separation, and the process of layer-by-layer mass transfer of gas from outside to inside is similar to the step-by-step separation process of each tower plate in the rectifying tower, so that the formed compound can be regarded as a similar nano rectifying tower, and the CO can be realized by constructing the similar nano rectifying tower2The gas is subjected to multi-stage separation to reach S at normal temperature and normal pressureCO2/N2Selectivity (iatt) of = 73148.
1. The invention relates to a quasi-nanometer rectifying tower, which comprises the following specific synthetic methods:
(1) weighing a certain amount of ionic liquid [ TETA ] L into a beaker, adding 5-30ml of anhydrous methanol until the ionic liquid is completely dissolved, then adding a certain amount of activated ZIF-8 powder into the beaker, and stirring at room temperature until the solvent is completely volatilized. The obtained product is put into a vacuum oven and dried for several hours under the condition of high temperature.
(2) The obtained solid powder was washed several times with anhydrous N, N-Dimethylformamide (DMF), and centrifuged until no residue remained after the filtrate was evaporated under high temperature vacuum condition. The solid material obtained after centrifugation was placed in a high temperature vacuum oven for several hours for drying.
(3) Weighing a certain amount of ionic liquid [ TEPA ] [ FV ] into a centrifuge tube with a certain specification, adding 1-10ml of anhydrous DMF until ILs are completely dissolved, adding the product obtained in the step (2), fully and uniformly mixing, and after a plurality of hours, putting the obtained product into a high-temperature vacuum oven to dry for a plurality of hours to obtain the target product.
2. The ratio of two ILs to ZIF-8 and the loading form of the inner layer and the outer layer are changed to prepare different forms of similar nanometer rectifying towers.
3. In the first step of loading process, different volatile solvents such as water, methanol, ethanol, acetone and the like are used for loading ILs.
4. Various forms of heating vacuum, etc. are used to remove the solvent during loading.
5. Different amino ILs and other materials of the ZIF series are combined to form composite materials in different forms.
The quasi-nanometer rectifying tower is used for CO2And trapping, including both batch adsorption and fixed bed adsorption.
Method for separating CO by using material batch adsorption method similar to nanometer rectifying tower2The method comprises the following steps:
(1) starting a physical adsorption instrument, adding the ground white nano rectifying tower composite material powder into a sample tube after accurate weighing, and degassing.
(2) The degassed sample was weighed again to obtain the total weight and the dry weight of the sample and placed in the adsorption apparatus test position.
(3) And setting relevant test parameters of the adsorption instrument and starting the test.
(4) The obtained material is used for treating CO at 298K2，N2Adsorption isotherm of (1).
(5) Through analysis, the separation performance data of the material can be obtained and evaluated.
Compared with the prior art, the invention has the following advantages:
experimental data of the batch adsorption method show that the material with the similar nanometer rectifying tower can treat CO under 298K2/N2The separation selectivity of the method is as high as 73148, far exceeding the traditional methodThe adsorbent material achieves the effect of molecular sieving.
Second, the intermittent adsorption method experiment shows that the composite material with the structure similar to the nanometer rectifying tower can efficiently separate CO at 298K2/N2。
The preparation method of the composite material is simple, can be synthesized in large batch, has low price of the synthetic raw materials, and can be widely applied to CO in industry2Absorption and separation.
Drawings
Fig. 1 is a schematic structural diagram of a composite material similar to a nanometer rectifying tower.
FIG. 2 is a physical diagram of a composite material similar to a nanometer rectifying tower.
FIG. 3 is a polycrystalline X-ray diffraction (PXRD) characterization plot of a "nano-rectifier" like composite material.
FIG. 4 is a class of 'nano-rectification tower' composite material to CO2/N2The separated adsorption capacity is plotted as a function of pressure.
FIG. 5 is a class of "nano-rectification column" composites vs. CO2/N2Selectivity of the separation as a function of pressure.
Detailed Description
The present invention is further illustrated by the following specific examples, but the invention is not limited thereto.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
(1) 0.4 g of ionic liquid [ TETA ] L is weighed into a beaker, 20 ml of absolute methanol is added until the ionic liquid is completely dissolved, then 0.6 g of activated ZIF-8 powder is added into the beaker, and stirring is carried out at room temperature until the solvent is completely volatilized. The obtained product was put into a vacuum oven and dried under 350K for 12 hours.
(2) The obtained solid powder was washed several times with anhydrous N, N-Dimethylformamide (DMF), and centrifuged until no residue remained after the filtrate was evaporated under high temperature vacuum condition. The solid material obtained after centrifugation was placed in a vacuum oven at 350K and dried for 12 hours.
(3) Weighing 0.25 g of ionic liquid [ TEPA ] [ FV ] in a 10ml centrifuge tube, adding 3 ml of anhydrous DMF until ILs are completely dissolved, adding the product obtained in the step (2), fully and uniformly mixing, and after 4 hours, putting the obtained product into a 350K vacuum oven for 12 hours to dry to obtain the target product.
Example 2
(1) 0.4 g of ionic liquid [ TEPA ] was weighed][FV]In a beaker, 20 ml of anhydrous methanol was added to completely dissolve. 3 g Zn (NO)3)2·6H2The methanol solution of O is added and stirred uniformly. 6.6 g of 2-methylimidazole in methanol was added, and the mixture was stirred at room temperature for 2 hours, centrifuged, and vacuum-dried to obtain ZIF-8 as a white powder.
(2) The obtained solid powder was washed several times with anhydrous N, N-Dimethylformamide (DMF), and centrifuged until no residue remained after the filtrate was evaporated under high temperature vacuum condition. The solid material obtained after centrifugation was placed in a vacuum oven at 350K and dried for 12 hours.
(3) Weighing 0.25 g of ionic liquid [ TETA ] L into a 10ml centrifuge tube, adding 3 ml of anhydrous DMF until ILs are completely dissolved, adding the product obtained in the step (2), fully and uniformly mixing, and after 4 hours, putting the obtained product into a 350K vacuum oven for drying for 12 hours to obtain the target product.
Example 3
(1) 0.4 g of ionic liquid [ TETA ] L is weighed into a beaker, 20 ml of deionized water is added until the ionic liquid is completely dissolved, then 0.6 g of activated ZIF-8 powder is added into the beaker, and stirring is carried out at room temperature until the solvent is completely volatilized. The obtained product was put into a vacuum oven and dried under 350K for 12 hours.
(2) The solid powder obtained was washed several times with anhydrous N, N-Dimethylacetamide (DMA) and centrifuged until no residue remained after the filtrate was evaporated under high temperature vacuum. The solid material obtained after centrifugation was placed in a vacuum oven at 350K and dried for 12 hours.
(3) Weighing 0.25 g of ionic liquid [ TEPA ] [ FV ] in a 10ml centrifuge tube, adding 3 ml of anhydrous DMF until ILs are completely dissolved, adding the product obtained in the step (2), fully and uniformly mixing, and after 4 hours, putting the obtained product into a 350K vacuum oven for 12 hours to dry to obtain the target product.
Claims (5)
1. A preparation method of a multilayer-structured nano rectifying tower-like composite material composed of two different ILs and ZIF-8 is characterized by comprising the following steps of:
(1) weighing a certain amount of ionic liquid [ TETA ] L into a beaker, adding 5-30mL of volatile solvent until the ionic liquid is completely dissolved, then adding a certain amount of activated ZIF-8 powder into the beaker, stirring at room temperature until the solvent is completely volatilized, putting the obtained product into a vacuum oven, and drying for a plurality of hours at high temperature; the volatile solvent is water, anhydrous methanol, ethanol or acetone;
(2) washing the obtained solid powder with anhydrous N, N-Dimethylformamide (DMF) for several times, centrifuging until no residue exists after the filtrate is volatilized under the high-temperature vacuum condition, and drying the solid substance obtained after centrifuging in a high-temperature vacuum oven for several hours;
(3) weighing a certain amount of ionic liquid [ TEPA ] [ FV ] into a centrifuge tube with a certain specification, adding 1-10mL of anhydrous DMF until ILs are completely dissolved, adding the product obtained in the step (2), fully and uniformly mixing, and after a plurality of hours, putting the obtained product into a high-temperature vacuum oven to dry for a plurality of hours to obtain the target product.
2. A preparation method of a multilayer-structured nano rectifying tower-like composite material composed of two different ILs and ZIF-8 is characterized by comprising the following steps of:
(1) weighing a certain amount of ionic liquid [ TEPA ] [ FV ] into a beaker, adding 5-30mL of volatile solvent until the ionic liquid is completely dissolved, then adding a certain amount of activated ZIF-8 powder into the beaker, stirring at room temperature until the solvent is completely volatilized, putting the obtained product into a vacuum oven, and drying for a plurality of hours at high temperature; the volatile solvent is water, anhydrous methanol, ethanol or acetone;
(2) washing the obtained solid powder with anhydrous N, N-Dimethylformamide (DMF) for several times, centrifuging until no residue exists after the filtrate is volatilized under the high-temperature vacuum condition, and drying the solid substance obtained after centrifuging in a high-temperature vacuum oven for several hours;
(3) weighing a certain amount of ionic liquid [ TETA ] L into a centrifuge tube with a certain specification, adding 1-10mL of anhydrous DMF until ILs are completely dissolved, adding the product obtained in the step (2), fully and uniformly mixing, and after a plurality of hours, putting the obtained product into a high-temperature vacuum oven to dry for a plurality of hours to obtain the target product.
3. The multilayer structured nano rectifying tower-like composite material composed of two different ILs and ZIF-8 prepared by the preparation method according to claim 1 or 2, wherein the two different ILs are loaded on the inner and outer sides of the ZIF-8, respectively.
4. The composite material of claim 3 in CO2Use in capture, of said composite material for CO2/CH4/N2/H2The separation is efficient.
5. The use according to claim 4, wherein the separation method comprises batch adsorption separation and fixed bed continuous adsorption separation.
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