CN114768713A - Photocatalytic microreactor and preparation method thereof - Google Patents
Photocatalytic microreactor and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/60—Reduction reactions, e.g. hydrogenation
- B01J2231/62—Reductions in general of inorganic substrates, e.g. formal hydrogenation, e.g. of N2
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2531/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- C07C2531/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups C07C2531/02 - C07C2531/24
Abstract
The invention provides a wood-based photocatalytic microreactor, which comprises a white wood and a photocatalytic nanomaterial compounded on the wall of a white wood channel, wherein the white wood is obtained by chemically treating wood. The application also provides a preparation method of the wood-based photocatalytic microreactor. This application regards porous timber after the chemical treatment as the load matrix of photocatalysis nano-material, utilizes the micropore passageway of white timber as catalytic reaction space, has promoted photocatalytic reaction efficiency.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to a wood-based photocatalysis microreactor and a preparation method thereof.
Background
In recent years, micro/nano-structured substrates with porous structures have become an important area for catalyst, filter, battery and sensor applications. Many of these applications require extensive gas/solid or fluid/solid contact to provide a porous structure. In view of the above, it has been proposed to combine a photocatalytic material with a porous matrix and firmly fix the nanomaterial to solve the above-mentioned problems. Porous matrices are attractive for photocatalysts because the porous material minimizes the distance between the photon absorption site and the electron/hole redox reaction, thereby improving efficiency. In addition, the combination of the photocatalytic nanomaterial and various porous macroscopic materials (such as wood, gel, and foam) also helps to further improve the recovery rate of the nano photocatalyst. These substrates can be classified into natural substrates such as zeolite, plant, etc., and synthetic substrates such as non-polar fibrous substrates, glass, cotton fabrics, bentonite, activated carbon, multi-walled carbon nanotubes, and metal organic frameworks. Most of substrates used in photocatalysis at present are artificially synthesized, the process is complicated and has certain harm to the environment.
Due to the high abundance and renewability of wood, as well as the high reactivity and unique structural characteristics of these materials, wood-based nanotechnology has received much attention in the field of photocatalytic degradation of organic pollutants in aquatic environments. However, most of the wood modification methods are to crush and refine wood, and then combine the wood with a photocatalytic material. Therefore, the procedure is complicated, the multi-level hierarchical structure and the micropore channels of the wood cannot be reserved, and all the characteristics of the wood are not fully utilized.
A monolithic wood material contains a complex hierarchical structure and micropore channels inside, and if the monolithic wood material can be used, the monolithic wood material is used as a photocatalytic reaction space, which is a purely natural microreactor and has great research significance. Lignin and other pigments can be removed from logs by chemical modification, a technique that is well established as a first step in wood multi-functional applications, such as transparent wood. After the wood logs are freed of lignin and other pigments, the whole body appears white, called white wood. After the modification, the internal micropore channel and the hierarchical structure can be completely reserved, the optical performance is improved, and the multifunctional modification of the wood can be realized by filling different materials. However, there is no technology to apply such monolithic wood to photocatalysis.
Disclosure of Invention
The invention aims to provide a wood-based photocatalytic microreactor which can improve the efficiency of photocatalytic reaction.
In view of the above, the present application provides a wood-based photocatalytic microreactor comprising a white wood and a photocatalytic nanomaterial composited on a wall of a white wood channel, wherein the white wood is obtained by chemically treating wood.
Preferably, the load factor of the photocatalytic nano material is 15-30 wt%; the porosity of the white wood is 80-90%.
Preferably, the photocatalytic nanomaterial is a photocatalytic nanoparticle material or a photocatalytic two-dimensional nanosheet material.
The application also provides a preparation method of the wood-based photocatalytic microreactor, which comprises the following steps:
titrating the photocatalytic nano material suspension into the white wood, drying, and repeating for multiple times to obtain the wood-based photocatalytic microreactor;
the white wood is obtained by chemically treating wood.
Preferably, the preparation process of the white wood comprises the following specific steps:
cutting the wood into a veneer sample along a direction perpendicular to the wood micropore channel;
mixing the veneer sample with glacial acetic acid, sodium chlorite and an acetic acid buffer solution, and reacting with hydrogen peroxide;
and (4) washing and drying the reacted sample to obtain the white wood.
Preferably, the density of the veneer sample is 0.1-0.2 g/cm3。
Preferably, the concentration of the acetic acid buffer solution is 30-40%, in a system formed by the glacial acetic acid, the sodium chlorite and the acetic acid buffer solution, the volume ratio of the acetic acid buffer solution to the glacial acetic acid is 1:2, and the concentration of the sodium chlorite is 3-5 mg/mL; the concentration of the hydrogen peroxide is 30-40%.
Preferably, the concentration of the photocatalytic nano material suspension is 1-3 mg/mL, and the solvent is absolute ethyl alcohol.
Preferably, the drying temperature is 40-60 ℃ and the drying time is 10-20 min.
Preferably, the photocatalytic nanomaterial is selected from one or more of a semiconducting metal oxide and a photocatalytic two-dimensional material.
The application provides a wood-based photocatalytic microreactor, which comprises a white wood (DW) and photocatalytic nanomaterials compounded on the wall of a white wood channel, wherein the white wood is obtained by chemically treating wood; this application regards porous timber after the chemical treatment as the load matrix of photocatalysis nano-material, utilizes the micropore passageway of white timber as catalytic reaction space, has promoted photocatalytic reaction efficiency.
Drawings
FIG. 1 is a comparison of a raw wood and a white wood in example 1 of the present invention, wherein a is a raw wood and b is a white wood;
FIG. 2 is an SEM micro-characterization diagram of a wood-based photocatalytic microreactor prepared in example 1 of the present invention;
fig. 3 is a bar graph of the photocatalytic performance of the photocatalytic nanomaterials with different loading rates in example 2 of the present application.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The application adopts porous wood as the load matrix of the photocatalyst, provides a wood-based microreactor for photocatalysis, utilizes the micropore channel of wood as the catalytic reaction space, promotes the photocatalytic reaction efficiency, widens the application field of wood, and makes the wood have higher market value. Specifically, the embodiment of the invention discloses a wood-based photocatalytic microreactor, which comprises a white wood and a photocatalytic nanomaterial compounded on the wall of a white wood channel, wherein the white wood is obtained by chemically treating wood.
In the wood-based photocatalytic microreactor provided herein, the photocatalytic nanomaterial is specifically selected from semiconducting metal oxides such as TiO2ZnO and the like, two-dimensional materials such as LDH, TMDS, MOF, MXene and the like or a combination of the two, and the loading rate of the two-dimensional materials in the wood-based photocatalytic microreactor is 15-30 wt%, and more specifically, the loading rate of the photocatalytic nanomaterials in the wood-based photocatalytic microreactor is 17-27%; the photocatalytic nanomaterial described in the present application is in the form of particles or two-dimensional nanoplates. In the application, the porosity of the white wood is 80-90%.
The application also provides a preparation method of the wood-based photocatalytic microreactor, which comprises the following steps:
titrating the photocatalytic nano material suspension into the white wood, drying, and repeating for multiple times to obtain the wood-based photocatalytic microreactor;
the white wood is obtained by chemically treating wood.
In the present application, the preparation method of the white wood comprises the following specific steps:
cutting the wood into a veneer sample along a direction perpendicular to the wood micropore channel;
mixing the veneer sample with glacial acetic acid, sodium chlorite and an acetic acid buffer solution, and reacting with hydrogen peroxide;
and (4) cleaning and drying the reacted sample to obtain the white wood.
In the preparation process, the density of the veneer sample is 0.1-0.2 g/cm3(ii) a More specifically, the density of the veneer sample is 0.15-0.2 g/cm3。
Mixing the veneer sample with glacial acetic acid, sodium chlorite and an acetic acid buffer solution, reacting for 2-3 h, and then reacting with hydrogen peroxide for 2-3 h; delignification of logs by CIO2Under the action of glacial acetic acid, sodium chlorite and acetic acid buffer solution, aromatic ring is oxidized to produce ring-opening reaction, so that lignin is decomposed effectively. The hydrogen peroxide has strong bleachingAnd (4) white action, which can effectively remove residual pigment in the wood. Thus, the above process results in the removal of lignin and other pigments from the veneer sample, enhancing the porosity and optical properties of the wood. The concentration of the acetic acid buffer solution adopted by the application is 30-40%, and more specifically, the concentration of the acetic acid buffer solution is 35 wt%; in a system formed by the glacial acetic acid, the sodium chlorite and the acetic acid buffer solution, the volume ratio of the acetic acid buffer solution to the glacial acetic acid is 1:1, and the concentration of the sodium chlorite is 3-5 mg/mL. The concentration of the hydrogen peroxide is 30-40%, and more specifically, the concentration of the hydrogen peroxide is 30%.
After the reaction, cleaning and drying the reacted sample to obtain the white wood; the cleaning is specifically carried out by using deionized water for cleaning, and then pure ethanol, mixed solution of ethanol and acetone and pure acetone are sequentially used for dehydration; in the process, the volume ratio of ethanol to acetone in the mixed solution of ethanol and acetone is (1-2): 1; the volume ratio of the pure ethanol to the mixed solution of the ethanol and the acetone to the acetone is 1:1: 1; the dehydration is three-step ultrasonic dehydration, and the dehydration in each step is repeated three times, each time for 5 min.
After the white wood is obtained, the photocatalytic nano material suspension is dripped into the white wood, the dried nano material is attached to the wall of a channel of the wood, titration is carried out again after drying, and the steps are repeated until the loading capacity meets the requirement, so that the wood-based photocatalytic microreactor is obtained. In the process, the concentration of the photocatalytic nano material suspension is 1-3 mg/mL, and the solvent is absolute ethyl alcohol; the ultrasonic wave treatment agent is obtained through ultrasonic treatment, and the ultrasonic treatment time is 30-40 min. The drying temperature is 40-60 ℃, and the drying time is 10-20 min; more specifically, the drying temperature is 40-50 ℃, and the drying time is 10-15 min.
The wood-based photocatalytic microreactor provided by the application is prepared by filling a photocatalytic nanomaterial in a gap channel of wood after lignin and other pigments are removed from raw wood, and preparing a natural integral photocatalytic microreactor; the method reserves the integral hierarchical structure of the wood, improves the optical performance of the wood, and realizes the application of natural environmental protection by taking the internal transmission channel of the wood as a reaction space.
In order to further understand the present invention, the following examples are provided to illustrate the wood-based photocatalytic microreactor and the method for making the same in detail, and the scope of the present invention is not limited by the following examples.
Example 1
The preparation method of the wood-based photocatalytic microreactor is characterized by comprising the following steps:
1) a sample (Barhama cunninghami, 25X 2mm in size) was placed in a reaction solution containing 20mL of 35% acetic acid buffer and 60mL of glacial acetic acid, 0.3g of sodium chlorite, and the reaction time was 3 hours. After 3 hours, putting the wood into a new reaction solution for repeated operation once, wherein the reaction time is 3 hours;
2) taking out a sample, putting the sample into 20mL of 30% hydrogen peroxide, and standing for 3h under visible light;
3) washing a sample with deionized water, then ultrasonically dehydrating with 40mL of pure ethanol, 40mL of ethanol-acetone mixed solution (1:1) and 40mL of pure acetone in sequence, repeating the dehydration for three times in each step, and drying to obtain the white wood; FIG. 1 is a comparison of a log and a white wood in this example, wherein a is the log and b is the white wood;
4) weighing 50mg of ZnAl-LDH powder into 50mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 30min to obtain a suspension;
5) titrating the suspension on the white wood by adopting a titration method, drying the suspension after the suspension penetrates into the interior of the white wood along the pore canal of the wood, wherein the drying temperature is 40 ℃, the drying time is 10min, and repeating the operation until the loading capacity of ZnAl-LDH is 20 percent, thus completing the preparation. Fig. 2 is an SEM microscopic representation of the wood-based photocatalytic microreactor prepared in this example; it can be seen that the photocatalytic nanomaterial is attached to the channel walls of the white wood.
Example 2
The preparation method is the same as in example 1, except that: the addition amount of ZnAl-LDH is changed; thus, wood-based photocatalytic microreactor samples having loading ratios of 17.5%, 21%, 24.8%, 26.57%, and 29.34%, respectively, were obtained.
The prepared five-gradient sample and 30mg of ZnAl-LDH material are used for photocatalytic reduction of CO2Experiment, the experimental conditions are specifically a photocatalytic reaction system: PerfectLight, Labsolar-6A photocatalytic system; light source type: PerfectLight, PLS-SXE300, full wavelength; power of light source: a 100W xenon lamp; the distance between the light source and the sample is 8 cm; the reaction temperature is controlled below 40 ℃;
when single ZnAl-LDH is adopted for testing, a certain amount of sample is dispersed in 1ml of water by ultrasonic waves, then the sample is completely dripped on a glass fiber filter membrane, the filter membrane is dried and then placed in a reactor, and then the reactor is vacuumized and is introduced with CO2The gas washing process was repeated 3 times, and finally a certain amount of water was added to the reactor to make H2O is volatilized into steam, with CO2Circulating the gas in the reactor, and then turning on the lamp for reaction;
when the composite sample (ZAL/DW) was used for the experiment, the glass fiber filter membrane was replaced with the prepared sample, and the other conditions were not changed.
Under the above experimental conditions, the reaction time was 1h, and the reaction product CH was detected4The result is shown in FIG. 3, which shows that 30mg of CH is present in the pure ZnAl-LDH material4The yield is 1.13378 (mu mol/g), which is weaker than other five pieces of composite wood (ZAL/DW) with different material loading rates, and the loading rate can reach the maximum at about 26.57 percent in the five loading rates, compared with the method without taking white wood (DW) as a carrier, the catalytic efficiency is obviously improved.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A wood-based photocatalytic microreactor comprises a white wood and photocatalytic nanomaterials compounded on the walls of the white wood channels, wherein the white wood is obtained by chemically treating wood.
2. The wood-based photocatalytic microreactor of claim 1, wherein the photocatalytic nanomaterial has a loading rate of 15-30 wt%; the porosity of the white wood is 80-90%.
3. The wood-based photocatalytic microreactor of claim 1, wherein the photocatalytic nanomaterial is a photocatalytic nanoparticle material or a photocatalytic two-dimensional nanosheet material.
4. The method of making a wood-based photocatalytic microreactor of claim 1, comprising the steps of:
titrating the photocatalytic nano material suspension into the white wood, drying, and repeating for multiple times to obtain the wood-based photocatalytic microreactor;
the white wood is obtained by chemically treating wood.
5. The preparation method according to claim 4, wherein the preparation process of the white wood is specifically as follows:
cutting wood into a veneer sample along a direction perpendicular to the wood micropore channel;
mixing the veneer sample with glacial acetic acid, sodium chlorite and an acetic acid buffer solution, and reacting with hydrogen peroxide;
and (4) cleaning and drying the reacted sample to obtain the white wood.
6. According to the claimThe method of claim 5, wherein the density of the veneer sample is 0.1 to 0.2g/cm3。
7. The preparation method according to claim 5, wherein the concentration of the acetic acid buffer solution is 30-40%, the volume ratio of the acetic acid buffer solution to the glacial acetic acid in a system formed by the glacial acetic acid, the sodium chlorite and the acetic acid buffer solution is 1:2, and the concentration of the sodium chlorite is 3-5 mg/mL; the concentration of the hydrogen peroxide is 30-40%.
8. The preparation method of claim 4, wherein the concentration of the photocatalytic nanomaterial suspension is 1-3 mg/mL, and the solvent is absolute ethyl alcohol.
9. The method according to claim 4, wherein the drying is carried out at a temperature of 40 to 60 ℃ for 10 to 20 min.
10. The preparation method according to any one of claims 4 to 9, wherein the photocatalytic nanomaterial is selected from one or more of a semiconductor metal oxide and a photocatalytic two-dimensional material.
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| CN116393126A (en) * | 2022-11-02 | 2023-07-07 | 东北林业大学 | Cu for adsorbing photocatalytic degradation pollutant 2 Preparation method of O-modified wood carbon skeleton material |
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| CN112959446A (en) * | 2021-02-01 | 2021-06-15 | 国际竹藤中心 | Metal organic framework/wood composite material and preparation method and application thereof |
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