CN112657554B - Preparation method of perovskite sensitized covalent triazine organic framework composite material - Google Patents
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Abstract
The invention discloses a preparation method of a perovskite sensitized covalent triazine organic framework composite material, belonging to the field of catalysts, which utilizes a perovskite material to sensitize CTF and add metal ions, thus widening the light absorption range of the composite material, simultaneously, the introduction of non-noble metal ions provides more catalytic active sites for the composite material, compared with the prior art, the catalytic activity of CTF for photocatalytic reduction of carbon dioxide is obviously improved, the preparation process has simple operation and low price, the technical route can be widely popularized due to lower cost, the preparation method has obvious practical application significance, and meanwhile, ice water is in a moving state during ice water bath through the use of ice balloons in the preparation process, thereby accelerating the heat exchange speed in the ice water and further accelerating the cooling speed of a mixed solution and B, so that the overall preparation efficiency of CsPbBr3/CTF (Fe) is improved.
Description
Technical Field
The invention relates to the field of catalysts, and in particular relates to a preparation method of a perovskite sensitized covalent triazine organic framework composite material.
Background
The exhaustion of fossil energy and the greenhouse gas effect are two major problems faced by human beings, and the conversion of solar energy into chemicals with high added value (such as the conversion of carbon dioxide into methane and the like) by using a catalyst and the storage of the chemicals are effective ways for solving the problems.
At present, TiO is the most widely used 2 Inorganic semiconductors of the type which readily recombine photogenerated electron and hole pairs with the semiconductor surface facing the CO 2 The molecular adsorption capacity is low, and the molecular adsorption capacity is low,and the use of some precious metals has also hindered their further commercial use. And a suitable CO 2 The reduced photocatalytic system should generally have a stable chemical structure, strong light harvesting capability, efficient electron transfer capability and CO 2 Adsorption activation capacity. Therefore, there is a need to develop non-noble metal materials with strong visible light absorption for photocatalysis.
The Covalent Organic Frameworks (COFs) have the advantages of high stability, high porosity, large surface area, easy synthesis, easy modification, adjustable amplitude and the like, and become a new CO 2 A photoreducible material. Also, such semiconductors have exhibited very excellent properties in the fields of gas adsorption, heterogeneous catalysis, photoconduction, and the like. Triazine covalent frameworks (CTFs) have attractive activity as nitrogen-rich porous COFs in photocatalysis. Recent studies have shown that triazine rings in CTFs can accelerate CO 2 Adsorption and activation in CO 2 Has achieved great success in terms of storage and separation.
Few reports on the aspect of photocatalytic reduction of carbon dioxide by using simple covalent triazine organic frameworks (CTFs) catalysts exist, and the catalytic performance of the simple CTF is low. The weak absorption of visible light and the lack of selective catalytic sites are mainly caused by two reasons.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a perovskite-sensitized covalent triazine organic framework composite material, which can realize the regulation and control of the photocatalytic activity of CTF (carbon nanotube) and obtain an inorganic cheap photocatalyst.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A preparation method of a perovskite sensitized covalent triazine organic framework composite material comprises the following steps:
s1, synthesizing CTF through acid gas assistance;
s2, adding a cesium source compound and oleic acid into octadecene, and heating to 150 ℃ in an argon atmosphere to obtain a mixed solution A;
s3, adding lead bromide, oleic acid and oleylamine into octadecene, and heating to 165 ℃ to obtain a mixed solution B;
s4, adding a proper amount of the mixed solution A obtained in the step 2 into the mixed solution B obtained in the step 3, stirring for 5 seconds, cooling in an ice-water bath, and performing centrifugal separation to obtain a solid, namely the cesium-lead-bromine quantum dot (CsPbBr) of the oil phase 3 -OL)；
S5, and mixing the CsPbBr prepared in the step 4 3 Dispersing OL quantum dots in ethyl acetate to obtain a mixed solution C;
s6, dissolving hexafluorophosphate in ethanol to obtain a mixed solution D;
s7, adding a proper amount of the mixed solution D obtained in the step 6 into the mixed solution C obtained in the step 5, and stirring for 30 minutes in the dark to obtain a solid CsPbBr 3 -PF 6 Quantum dots;
s8, obtaining CsPbBr in the step 7 3 -PF 6 Adding a proper amount of quantum dots into ethyl acetate solution of solid CTF, stirring in the dark for 30 minutes, adding a small amount of aqueous solution containing ferrous metal ions, stirring for 10 minutes, and centrifugally drying to obtain solid CsPbBr 3 /CTF(Fe)。
Further, the specific steps of acid gas assisted synthesis of CTF in S1 are as follows:
s11, respectively putting the monomer (1,4-Diacynobenzene (DCB)) and TfOH into glass bottles to obtain a bottle a and a bottle b;
s12, transferring the bottle a and the bottle b into a conical flask, degassing by using nitrogen gas, sealing, and heating to 100 ℃;
and S13, washing with an ammonia solution, deionized water and acetone after 24 hours, and drying in vacuum at 50 ℃ for 12 hours to obtain the light yellow solid CTF.
Further, the ratio of solid DCB in bottle a to TfOH liquid in bottle b was 100 mg: 0.3 ml.
Further, the cesium source compound is cesium carbonate, and the hexafluorophosphate salt is ammonium hexafluorophosphate.
Further, the ratio of the cesium source compound, oleic acid and octadecene in the mixed solution a is 0.23 mol: 0.2L: 3.8L; the proportion of lead bromide, oleic acid, oleylamine and octadecene in the mixed solution B is 1.88 mol: 5L: 5L: 50L.
Further, in the step 4, the ratio of the cesium source compound to the lead bromide is 1 mol: 8.17 mol.
Further, CsPbBr in the S5 3 -ratio of OL quantum dots to ethyl acetate 5 g: 5L of CsPbBr in the S8 3 -PF 6 The ratio of quantum dots to ethyl acetate was 5 g: 5L, CsPbBr in the S8 3 -PF 6 The ratio of quantum dots to CTF was 5 g: 5g, wherein the ratio of CTF to ethyl acetate in S8 is 5 g: 5L.
Further, the concentration of the ferrous metal ion aqueous solution is 0.06 mol/L.
Further, when the ice water bath in S4 is performed, a plurality of ice balloons are placed in ice water, each ice balloon includes a central water bag, a water filling pipe with a sealing cover is fixedly connected to the upper end of the central water bag, a dry ice layer wraps the outer side of the central water bag, a hard breathable layer wraps the outer end of the dry ice layer, and the water filling pipe sequentially penetrates through the dry ice layer and the hard breathable layer.
Furthermore, the hard breathable layer is made of a multi-pass through hole material, normal-temperature water is injected into the central water bag, when ice-water bath is carried out, the dry ice layer can quickly absorb heat of the normal-temperature water in the central water bag, so that heat is quickly absorbed and vaporized, the normal-temperature water overflows from the periphery of the hard breathable layer, and overflowed carbon dioxide can stir ice water, so that the ice water is in a dynamic state when the ice-water bath is carried out, compared with the static state in the prior art, the heat exchange speed between the ice water and the mixture of the mixed liquid A and the mixed liquid B can be accelerated when the ice water is in the dynamic state, the situation that the temperature of the ice water around the mixture of the mixed liquid A and the mixed liquid B is high is effectively relieved, the temperature difference of the ice water around the ice water is small, the cooling speed of the mixed liquid A and the mixed liquid B is accelerated, and the CsPbBr is enabled to be high 3 The overall preparation efficiency of the/CTF (Fe) is improved, and meanwhile, when carbon dioxide quickly overflows, certain driving force is generated on the ice balloon to enable the ice balloon to be in a dynamic state in ice waterThereby further increasing the magnitude of the ice water flow so that heat is more rapidly absorbed in the mixture of mixed liquor a and B.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) according to the scheme, the perovskite material is used for sensitizing the CTF and metal ions are added, so that the light absorption range of the CTF can be widened, meanwhile, the introduction of non-noble metal ions provides more catalytic active sites for the CTF, compared with the prior art, the catalytic activity of the CTFs for photocatalytic reduction of carbon dioxide is obviously improved, the preparation process is simple to operate and low in price, the technical route of the preparation process can be widely popularized due to low cost, and the preparation process has obvious practical application significance; meanwhile, by using the ice balloon in the preparation process, ice water is in a moving state during ice water bath, so that the heat exchange speed in the ice water is accelerated, the cooling speed of the mixed liquid A and the mixed liquid B is accelerated, and CsPbBr is ensured 3 The overall production efficiency of/CTF (Fe) is improved.
(2) When the ice water bath in S4 is carried out, a plurality of ice balloons are placed in ice water, each ice balloon comprises a central water bag, a water filling pipe with a sealing cover is fixedly connected to the upper end of the central water bag, a dry ice layer wraps the outer side of the central water bag, a hard breathable layer wraps the outer end of the dry ice layer, and the water filling pipe penetrates through the dry ice layer and the hard breathable layer in sequence.
(3) The hard breathable layer is made of a multi-pass through hole material, normal-temperature water is injected into the central water bag, when ice-water bath is carried out, the dry ice layer can quickly absorb heat of the normal-temperature water in the central water bag, so that heat is quickly absorbed and vaporized, the water overflows from the periphery of the hard breathable layer, overflowed carbon dioxide can stir ice water, and therefore the ice water is in a moving state when the ice-water bath is carried out, compared with the static state in the prior art, the heat exchange speed between the ice water and the mixture of the mixed liquid A and the mixed liquid B can be accelerated under the moving state of the ice water, the situation that the temperature of the ice water around the mixture of the mixed liquid A and the mixed liquid B is high is effectively relieved, the temperature difference of the ice water around the mixed liquid A and the mixed liquid B is small, the cooling speed of the mixed liquid A and the mixed liquid B is accelerated, and CsPbBr is enabled to be small 3 /CTF (Fe) is improved in overall preparation efficiency, and meanwhile, when carbon dioxide overflows rapidly, certain driving force is generated on the ice balloon to enable the ice balloon to be in a dynamic state in ice water, so that the ice water dynamic range is further improved, and heat in the mixture of the mixed liquid A and the mixed liquid B is absorbed more rapidly.
Drawings
FIG. 1 shows CsPbBr of the present invention 3 Schematic preparation of the catalyst;
FIG. 2 is a schematic representation of the catalytic conversion of carbon dioxide according to the present invention;
FIG. 3 shows CTF and CsPbBr of the present invention 3 And CsPbBr 3 XRD pattern of/CTF;
FIG. 4 shows CTF and CsPbBr of the present invention 3 And CsPbBr 3 FT-IR plot of/CTF;
FIG. 5 shows CsPbBr of the present invention 3 、CsPbBr 3 -PF 6 、CsPbBr 3 (ii) CTF and CsPbBr 3 Comparative graph of photocatalytic properties of/CTF (Fe);
FIG. 6 is a schematic structural view of an ice balloon of the present invention;
fig. 7 is a schematic structural view of the ice balloon surface of the present invention when carbon dioxide overflows.
The reference numbers in the figures illustrate:
1 dry ice layer, 2 hard breathable layers, 3 central water bags and 4 water filling pipes.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; but not all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, 3 and 4, a method for preparing and characterizing a perovskite-sensitized covalent triazine organic framework composite material includes the steps of:
s1, synthesizing CTF through acid gas assistance;
s11, putting the monomer (1,4-Diacynobenzene (DCB)) and TfOH into glass bottles respectively to obtain a bottle a and a bottle b;
s12, transferring the bottle a and the bottle b into a conical flask, degassing by using nitrogen gas, sealing, and heating to 100 ℃;
and S13, washing with an ammonia solution, deionized water and acetone after 24 hours, and drying in vacuum at 50 ℃ for 12 hours to obtain the light yellow solid CTF.
The ratio of solid DCB in vial a and TfOH liquid in vial b was 100 mg: 0.3 ml.
With CsPbBr 3 Inorganic perovskites sensitize CTFs and introduce metal ions:
s2, adding a cesium source compound and oleic acid into octadecene, and heating to 150 ℃ in an argon atmosphere to obtain a mixed solution A;
s3, adding lead bromide, oleic acid and oleylamine into octadecene, and heating to 165 ℃ to obtain a mixed solution B;
s4, adding a proper amount of the mixed liquid A obtained in the step 2 into the mixed liquid B obtained in the step 3, stirring for 5 seconds, cooling in an ice water bath, and performing centrifugal separation to obtain a solid, namely the cesium-lead-bromine quantum dots (CsPbBr) of the oil phase 3 -OL)；
S5, mixing the CsPbBr prepared in the step 4 3 Dispersing the-OL quantum dots in ethyl acetate to obtain a mixed solution C;
s6, dissolving hexafluorophosphate in ethanol to obtain a mixed solution D;
s7, adding a proper amount of the mixed solution D obtained in the step 6 into the mixed solution C obtained in the step 5, and stirring for 30 minutes in the dark to obtain a solid CsPbBr 3 -PF 6 Quantum dots;
s8, obtaining CsPbBr in the step 7 3 -PF 6 Adding a proper amount of quantum dots into ethyl acetate solution of solid CTF, stirring in the dark for 30 minutes, adding a small amount of aqueous solution containing ferrous metal ions, stirring for 10 minutes, and centrifugally drying to obtain solid CsPbBr 3 /CTF(Fe)。
The cesium source compound is cesium carbonate, and the hexafluorophosphate is ammonium hexafluorophosphate.
The ratio of the cesium source compound, oleic acid and octadecene in the mixed solution A is 0.23 mol: 0.2L: 3.8L; the proportion of lead bromide, oleic acid, oleylamine and octadecene in the mixed solution B is 1.88 mol: 5L: 5L: 50L.
In the step 4, the ratio of the cesium source compound to the lead bromide is 1 mol: 8.17 mol.
CsPbBr in S5 3 -ratio of OL quantum dots to ethyl acetate 5 g: CsPbBr in 5L, S8 3 -PF 6 The ratio of quantum dots to ethyl acetate was 5 g: CsPbBr in 5L, S8 3 -PF 6 The ratio of quantum dots to CTF was 5 g: 5g, the ratio of CTF to ethyl acetate in S8 was 5 g: 5L of the solution. The concentration of the ferrous metal ion aqueous solution was 0.06mol/L, and the amount added was 0.45 mL.
Referring to fig. 6 to 7, in the ice-water bath of S4, a plurality of ice balloons are placed in the ice water, the ice balloons include a central water bag 3, and a water-filled tube 4 with a sealing cover is fixedly connected to an upper end of the central water bag 3, and the center of the water-filled tube is located at the center of the central water bag 3The outer side of the water core bag 3 is wrapped with a dry ice layer 1, the outer end of the dry ice layer 1 is wrapped with a hard breathable layer 2, a water filling pipe 4 sequentially penetrates through the dry ice layer 1 and the hard breathable layer 2, the hard breathable layer 2 is made of a multi-pass through hole material, normal-temperature water is injected into the water core bag 3, when ice-water bath is carried out, the dry ice layer 1 can rapidly absorb the heat of the normal-temperature water in the water core bag 3, so that heat is rapidly absorbed and vaporized, the hard breathable layer 2 overflows from the periphery of the hard breathable layer, overflowed carbon dioxide can stir ice water, so that the ice water is in a moving state when the ice-water bath is carried out, compared with the static ice water in the prior art, the heat exchange speed between the ice water and the mixture of the mixed liquids A and B can be accelerated under the moving state, the occurrence of the condition that the temperature around the mixed liquids A and B is higher can be effectively relieved, and the temperature difference between the surrounding ice water can be effectively ensured to be smaller, the cooling speed of the mixed liquid A and B is accelerated, so that CsPbBr is ensured 3 The overall preparation efficiency of the/CTF (Fe) is improved, and meanwhile, when carbon dioxide overflows rapidly, certain driving force is generated on the ice balloon to enable the ice balloon to be in a dynamic state in ice water, so that the ice water dynamic range is further improved, and the heat absorption of the mixture of the mixed liquid A and the mixed liquid B is quicker.
Example 2:
the CTF catalyst is used for photocatalytic reduction of carbon dioxide:
5mg of CTF prepared in S1 was weighed out and dissolved in 5mL of ethyl acetate, and 30. mu.L of deionized water was added and transferred to a 30mL reactor. A300W xenon lamp is used as a light source to simulate sunlight to carry out a photocatalytic carbon dioxide reduction experiment, please refer to FIG. 5, the sampling is carried out at regular time, and the contents of the generated carbon monoxide and methane are analyzed through gas chromatography.
Example 3:
please refer to fig. 2, CsPbBr 3 the/CTF (Fe) catalyst is used for photocatalytic reduction of carbon dioxide:
weighing prepared CsPbBr 3 the/CTF (Fe) quantum dots 5mg dissolved in 5mL ethyl acetate, 30. mu.L deionized water was added and transferred to a 30mL reactor. A 300W xenon lamp is used as a light source, and sunlight is simulated to carry out a photocatalytic carbon dioxide reduction experiment; referring to FIG. 5, the samples are taken periodically through the gas phaseThe resulting carbon monoxide and methane contents were chromatographed. CO of composite photocatalyst sample by adopting photocatalytic system 2 The light conversion performance was evaluated, and a 300W xenon lamp was used as a light source.
Comparing the results of example 2 and example 3, the CTF was sensitized with perovskite material and metal ions were added to broaden the absorption range and introduce more catalytically active sites. The catalytic activity of the obtained composite material for photocatalytic reduction of carbon dioxide is improved by 7 times, compared with the prior art, the catalytic activity of CTFs is obviously improved, the preparation process is simple to operate and low in price, the technical route can be widely popularized due to the low cost, and the preparation method has obvious practical application significance.
The above; are merely preferred embodiments of the invention; the scope of the invention is not limited thereto; those skilled in the art can appreciate that the present invention is not limited to the specific embodiments disclosed herein; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.
Claims (10)
1. A preparation method of a perovskite sensitized covalent triazine organic framework composite material is characterized by comprising the following steps: the method comprises the following steps:
s1, synthesizing CTF through acid gas assistance;
s2, adding a cesium source compound and oleic acid into octadecene, and heating to 150 ℃ in an argon atmosphere to obtain a mixed solution A;
s3, adding lead bromide, oleic acid and oleylamine into octadecene, and heating to 165 ℃ to obtain a mixed solution B;
s4, adding the mixed solution A obtained in the step 2 into the mixed solution B obtained in the step 3, stirring for 5 seconds, cooling in an ice-water bath, and performing centrifugal separation to obtain a solid, namely the cesium-lead-bromine quantum dot (CsPbBr) of the oil phase 3 -OL)；
S5, and mixing the CsPbBr prepared in the step 4 3 Dispersing the-OL quantum dots in ethyl acetate to obtain a mixed solution C;
s6, dissolving hexafluorophosphate in ethanol to obtain a mixed solution D;
s7, adding a proper amount of the mixed solution D obtained in the step 6 into the mixed solution C obtained in the step 5, and stirring for 30 minutes in the dark to obtain a solid CsPbBr 3 -PF 6 Quantum dots;
s8, obtaining CsPbBr in the step 7 3 -PF 6 Adding a proper amount of quantum dots into ethyl acetate solution of solid CTF, stirring in the dark for 30 minutes, adding aqueous solution of ferrous metal ions, stirring for 10 minutes, and centrifugally drying to obtain solid CsPbBr 3 /CTF(Fe)。
2. The method for preparing a perovskite sensitized covalent triazine organic framework composite material according to claim 1, wherein the method comprises the following steps: the CTF synthesis method in the S1 through the assistance of acid gas comprises the following specific steps:
s11, respectively putting the monomer 1,4-diacynobenzene, namely DCB and TfOH into glass bottles to obtain a bottle a and a bottle b;
s12, transferring the bottle a and the bottle b into a conical flask, degassing by using nitrogen gas, sealing, and heating to 100 ℃;
and S13, washing with an ammonia solution, deionized water and acetone after 24 hours, and drying in vacuum at 50 ℃ for 12 hours to obtain the light yellow solid CTF.
3. The method for preparing a perovskite sensitized covalent triazine organic framework composite material according to claim 2, wherein the method comprises the following steps: the ratio of solid DCB in bottle a to TfOH liquid in bottle b was 100 mg: 0.3 mL.
4. The method for preparing a perovskite sensitized covalent triazine organic framework composite material according to claim 1, wherein the method comprises the following steps: the cesium source compound is cesium carbonate, and the hexafluorophosphate is ammonium hexafluorophosphate.
5. The method for preparing a perovskite sensitized covalent triazine organic framework composite material according to claim 1, wherein the method comprises the following steps: the proportion of the cesium source compound, the oleic acid and the octadecene in the mixed solution A is 0.23 mol: 0.2L: 3.8L; the proportion of lead bromide, oleic acid, oleylamine and octadecene in the mixed solution B is 1.88 mol: 5L: 5L: 50L.
6. The method of preparing a perovskite-sensitized covalent triazine organic framework composite material as claimed in claim 1, wherein: in the step 4, the ratio of the cesium source compound to the lead bromide is 1 mol: 8.17 mol.
7. The method of preparing a perovskite-sensitized covalent triazine organic framework composite material as claimed in claim 1, wherein: CsPbBr in the S5 3 -ratio of OL quantum dots to ethyl acetate 5 g: 5L, CsPbBr in the S8 3 -PF 6 The ratio of quantum dots to ethyl acetate was 5 g: 5L, CsPbBr in the S8 3 -PF 6 The ratio of quantum dots to CTF was 5 g: 5g, wherein the ratio of CTF to ethyl acetate in S8 is 5 g: 5L.
8. The method of preparing a perovskite-sensitized covalent triazine organic framework composite material as claimed in claim 1, wherein: the concentration of the ferrous metal ion aqueous solution is 0.06 mol/L.
9. The method of preparing a perovskite-sensitized covalent triazine organic framework composite material as claimed in claim 1, wherein: when the ice water bath in the S4 is carried out, a plurality of ice balloons are placed in ice water, each ice balloon comprises a central water bag (3), the upper end of each central water bag (3) is fixedly connected with a water filling pipe (4) with a sealing cover, the outer side of each central water bag (3) is wrapped with a dry ice layer (1), the outer end of each dry ice layer (1) is wrapped with a hard breathable layer (2), and each water filling pipe (4) penetrates through the dry ice layer (1) and the hard breathable layer (2) in sequence.
10. The method of preparing a perovskite-sensitized covalent triazine organic framework composite material as claimed in claim 9, wherein: the hard breathable layer (2) is made of a material with multiple through holes, and normal-temperature water is injected into the central water bag (3).
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