CN111644185A - Bi stripping by cell crusher3O4Method for Cl and in photocatalytic reduction of CO2Application of aspects - Google Patents

Bi stripping by cell crusher3O4Method for Cl and in photocatalytic reduction of CO2Application of aspects Download PDF

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CN111644185A
CN111644185A CN202010505296.8A CN202010505296A CN111644185A CN 111644185 A CN111644185 A CN 111644185A CN 202010505296 A CN202010505296 A CN 202010505296A CN 111644185 A CN111644185 A CN 111644185A
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stripping
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金晓丽
葛腾
徐怡雪
谢海泉
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Nanyang Normal University
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Abstract

本发明提出了一种利用细胞粉碎机剥离Bi3O4Cl的方法，其是以水为溶剂，以Bi(NO3)3·5H2O作为Bi源，盐酸四环素作为Cl源，采用水热法制备出Bi‑O‑Cl配合物，再通过烧结法制备出块体Bi3O4Cl光催化剂（B‑Bi3O4Cl），再将B‑Bi3O4Cl通过细胞粉碎机进行超声剥离制备超薄Bi3O4Cl纳米片（S‑Bi3O4Cl），以提高其光催化性能。本发明由水热和烧结法相结合制备出Bi3O4Cl光催化剂，所制备的Bi3O4Cl形貌呈不规则的块体结构，厚度约为200‑400 nm；利用细胞粉碎机对制备的块体Bi3O4Cl光催化剂进行超声剥离，使Bi3O4Cl由块体剥离为Bi3O4Cl纳米片，纳米片的厚度约为10‑50 nm，超薄纳米片使其光生载流子的迁移速率快，分离效率高，具备较好的光催化还原CO2性能。The invention proposes a method for peeling Bi 3 O 4 Cl by using a cell crusher, which uses water as a solvent, Bi(NO 3 ) 3 ·5H 2 O as a Bi source, tetracycline hydrochloride as a Cl source, and adopts hydrothermal treatment. The Bi-O-Cl complex was prepared by the sintering method, and the bulk Bi 3 O 4 Cl photocatalyst (B-Bi 3 O 4 Cl ) was prepared by the sintering method . Ultrathin Bi 3 O 4 Cl nanosheets (S‑Bi 3 O 4 Cl) were prepared by ultrasonic exfoliation to improve their photocatalytic performance. In the invention, the Bi 3 O 4 Cl photocatalyst is prepared by the combination of hydrothermal and sintering methods, and the prepared Bi 3 O 4 Cl has an irregular block structure and a thickness of about 200-400 nm; The prepared bulk Bi 3 O 4 Cl photocatalyst was subjected to ultrasonic exfoliation, so that Bi 3 O 4 Cl was exfoliated into Bi 3 O 4 Cl nanosheets from the bulk. The thickness of the nanosheets was about 10-50 nm, and the ultrathin nanosheets made The photogenerated carriers have fast migration rate, high separation efficiency, and good photocatalytic CO2 reduction performance.

Description

一种利用细胞粉碎机剥离Bi3O4Cl的方法及在光催化还原CO2 方面的应用A method for stripping Bi3O4Cl by using a cell pulverizer and reducing CO2 in photocatalysis applications

技术领域technical field

本发明涉及化学物质的制备，具体涉及一种利用细胞粉碎机剥离Bi3O4Cl的方法，本发明还涉及Bi3O4Cl在还原CO2方面的应用。The invention relates to the preparation of chemical substances, in particular to a method for stripping Bi 3 O 4 Cl by using a cell pulverizer, and also relates to the application of Bi 3 O 4 Cl in reducing CO 2 .

背景技术Background technique

能源是人类赖以生存与发展的物质基础，也是社会赖以生存与发展的物质基础。现如今，在能源结构中传统的化石能源仍处于主导地位，但由于化石能源的有限性和不可再生性，不久的将来全球将面临资源枯竭的问题。因此对新能源的开发与利用已成为人们研究的热点。在众多新能源中，太阳能因为其取之不竭，用之不尽的优势，成为研究焦点，而光催化技术就是通过半导体光催化剂直接利用太阳能，将其转化为化学能和电能，能够进行分解水制氢、CO2还原、光催化固氮等反应，这使得光催化技术在新能源领域显示出独特的优势和广阔的应用前景。Energy is the material basis for human survival and development, and it is also the material basis for society to survive and develop. Today, traditional fossil energy is still dominant in the energy structure, but due to the limited and non-renewable nature of fossil energy, the world will face the problem of resource depletion in the near future. Therefore, the development and utilization of new energy has become a research hotspot. Among many new energy sources, solar energy has become the focus of research because of its inexhaustible advantages. Photocatalysis technology directly utilizes solar energy through semiconductor photocatalysts to convert it into chemical energy and electrical energy, which can be decomposed. Reactions such as water hydrogen production, CO reduction, and photocatalytic nitrogen fixation make photocatalytic technology show unique advantages and broad application prospects in the field of new energy.

近年来，研究人员致力于研究新型高效、可见光响应的光催化剂，包括多元金属氧化物、层状化物、金属氢氧化物等，其中，BiOX（X=Cl，Br，I）属于新型铋基光催化剂，具有层状结构，其特征在于[Bi2O2]2+与双层卤素原子交错排列，能够显著降低光生载流子复合率，并且还具有低毒性、易合成等优点，引起了世界各国的广泛关注。但是由于其导带位置较低和还原能力弱，大部分BiOX只能应用于环境光催化，而在能源光催化方面应用不力。相关研究表明，富铋（脱卤）Bi x O y X z 基光催化剂具有和BiOX相似的层状结构和更负的导带位置，相比于BiOX，既保留了优势，又弥补其不足，是一种更具潜力的光催化剂。科研人员在研究Bi x O y X z 光催化过程中也发现了一些问题，Bi x O y X z 的载流子分离能较弱导致其光催化效率仍较低，因此，对Bi x O y X z 进行进一步改性来提高光催化活性是很有必要的。构建超薄的二维结构是优化光催化性能的有效途径之一。超薄纳米片通常比空间电荷层更薄，光生载流子可以通过简单的扩散从纳米片的内部迁移到表面，纳米薄片越薄，载体从内部扩散到表面的速度就越快。此外，超薄纳米薄片表面暴露的原子数量更多，这对提高太阳能吸收效率也很重要。因此，Bi x O y X z 厚度超薄化是获得优异光催化性能的一种有效途径。Bi3O4Cl作为一种Bi x O y X z 光催化剂，由于具有独特的晶体结构可以产生强大的内部电场，有助于光生电荷的有效分离，并且Bi3O4Cl具有很高的化学和光学稳定性，是一种理想的研究Bi x O y X z 厚度超薄化的光催化材料。In recent years, researchers have devoted themselves to the study of new high-efficiency, visible-light-responsive photocatalysts, including multi-component metal oxides, layered compounds, metal hydroxides, etc. Among them, BiOX (X=Cl, Br, I) belongs to a new type of bismuth-based photocatalyst The catalyst, with a layered structure, is characterized by the staggered arrangement of [Bi 2 O 2 ] 2+ and double-layer halogen atoms, which can significantly reduce the recombination rate of photogenerated carriers, and also has the advantages of low toxicity and easy synthesis, which has attracted worldwide attention. wide attention from all countries. However, due to its low conduction band position and weak reducing ability, most BiOX can only be used in ambient photocatalysis, but not in energy photocatalysis. Relevant studies have shown that Bi-rich (dehalogenated) Bi x O y X z -based photocatalysts have a layered structure similar to BiOX and a more negative conduction band position, which not only retains the advantages but also makes up for its shortcomings compared to BiOX. It is a more potential photocatalyst. Researchers also found some problems in the photocatalytic process of Bi x O y X z . The weak carrier separation energy of Bi x O y X z leads to its low photocatalytic efficiency. Therefore, for Bi x O y Further modification of X z is necessary to improve the photocatalytic activity. Constructing ultrathin 2D structures is one of the effective ways to optimize photocatalytic performance. Ultrathin nanosheets are usually thinner than space charge layers, and photogenerated carriers can migrate from the interior of the nanosheets to the surface by simple diffusion. The thinner the nanosheets, the faster the diffusion of carriers from the interior to the surface. In addition, the number of exposed atoms on the surface of ultrathin nanoflakes is higher, which is also important for improving solar energy absorption efficiency. Therefore, Bi x O y X z thickness ultrathinning is an effective way to obtain excellent photocatalytic performance. As a BixOyXz photocatalyst , Bi3O4Cl can generate a strong internal electric field due to its unique crystal structure, which facilitates the efficient separation of photogenerated charges, and Bi3O4Cl has a high chemical and optical stability, it is an ideal photocatalytic material to study the ultrathin thickness of Bi x O y X z .

发明内容SUMMARY OF THE INVENTION

本发明所要解决的技术问题是提供一种利用细胞粉碎机剥离块体Bi3O4Cl以获得纳米片的制备方法，还提供该纳米片应用于光催化还原CO2的用途。The technical problem to be solved by the present invention is to provide a preparation method for peeling off bulk Bi 3 O 4 Cl with a cell crusher to obtain nanosheets, and also to provide the application of the nanosheets in photocatalytic reduction of CO 2 .

为解决上述技术问题，本发明所采取的技术方案是：一种利用细胞粉碎机剥离Bi3O4Cl的方法，是以水为溶剂，以Bi(NO3)3·5H2O作为Bi源，盐酸四环素作为Cl源，采用水热法制备出Bi-O-Cl配合物，再通过烧结法制备出块体Bi3O4Cl光催化剂（即为B-Bi3O4Cl），再将B-Bi3O4Cl通过细胞粉碎机进行超声剥离制备超薄Bi3O4Cl纳米片（记为S-Bi3O4Cl），以提高其光催化性能；其方法步骤为：In order to solve the above-mentioned technical problems, the technical scheme adopted in the present invention is: a method for stripping Bi 3 O 4 Cl by using a cell crusher, using water as a solvent and Bi(NO 3 ) 3 .5H 2 O as a Bi source , tetracycline hydrochloride was used as Cl source, Bi-O-Cl complex was prepared by hydrothermal method, and then bulk Bi 3 O 4 Cl photocatalyst (ie B-Bi 3 O 4 Cl) was prepared by sintering method. Ultra-thin Bi 3 O 4 Cl nanosheets (referred to as S-Bi 3 O 4 Cl) are prepared by ultrasonic exfoliation of B-Bi 3 O 4 Cl through a cell crusher to improve its photocatalytic performance; the method steps are as follows:

⑴.称取0.4—1 g Bi(NO3)3·5H2O充分搅拌溶于30—35 ml去离子水中，接着加入0.2—0.5 g盐酸四环素，搅拌30—60 min，装入40 ml聚四氟乙烯内衬不锈钢釜水热釜中，在140—180 ℃下反应15—24 h；⑴. Weigh 0.4-1 g Bi(NO 3 ) 3 ·5H 2 O and dissolve it in 30-35 ml of deionized water, stir well, then add 0.2-0.5 g of tetracycline hydrochloride, stir for 30-60 min, and put 40 ml of poly In a tetrafluoroethylene-lined stainless steel kettle hydrothermal kettle, react at 140-180 ℃ for 15-24 h;

⑵.取出步骤⑴所得水热反应后的样品，使用离心机在每次10000 r/min下离心3—10min，分别用蒸馏水和乙醇洗涤离心沉淀若干次，最后置于60—100 ℃烘箱内干燥12—24h，得到黑色Bi-O-Cl配合物前驱体；秤取0.2—2 g干燥后的前驱体放入马弗炉中在450—600 ℃下烧结2—10 h，升温速率为1-5 ℃/min，自然降至室温后收取样品，即得块体Bi3O4Cl光催化剂；⑵. Take out the sample after the hydrothermal reaction obtained in step 1, use a centrifuge at 10,000 r/min for 3-10 min each time, wash the centrifuged precipitate with distilled water and ethanol for several times, and finally place it in a 60-100 ℃ oven to dry 12-24h, the black Bi-O-Cl complex precursor was obtained; 0.2-2 g of the dried precursor was weighed and put into a muffle furnace for sintering at 450-600 °C for 2-10 h, and the heating rate was 1- 5 ℃/min, the sample was collected after the temperature was naturally lowered to room temperature, and the bulk Bi 3 O 4 Cl photocatalyst was obtained;

⑶.称取300 mg步骤⑵制备的块体Bi3O4Cl样品于1000 ml烧杯中，加入0—200 ml去离子水、0—500 ml无水乙醇和0—500 ml乙二醇，用细胞粉碎机进行超声剥离，超声功率为40—80%，每次超声15—30 min后待冷却至室温再进行超声，每次补充无水乙醇至溶液达到500 ml，累计超声4—8 h后，静置沉淀，将沉淀物用蒸馏水和乙醇洗涤沉淀若干次，最后置于60—100 ℃烘箱内干燥12—24 h，得到超薄化样品，通过XRD、SEM、DRS、光电流测试技术手段对Bi3O4Cl光催化剂的物相组成、微观形貌、电荷分离和光催化性能进行研究。(3) Weigh 300 mg of the bulk Bi 3 O 4 Cl sample prepared in step (2) into a 1000 ml beaker, add 0-200 ml deionized water, 0-500 ml absolute ethanol and 0-500 ml ethylene glycol, and use The cell crusher was used for ultrasonic peeling, and the ultrasonic power was 40-80%. After each ultrasonic wave for 15-30 minutes, it was cooled to room temperature before ultrasonication. Each time, anhydrous ethanol was added to the solution to reach 500 ml, and the cumulative ultrasonic wave was 4-8 hours later. , stand for precipitation, wash the precipitate with distilled water and ethanol for several times, and finally dry it in a 60-100 ℃ oven for 12-24 h to obtain an ultra-thin sample. Through XRD, SEM, DRS, and photocurrent testing techniques The phase composition, microstructure, charge separation and photocatalytic performance of Bi 3 O 4 Cl photocatalyst were studied.

所述乙二醇的含水量小于0.01%（V/V）。The water content of the ethylene glycol is less than 0.01% (V/V).

所述乙醇的含水量小于0.01%（V/V）。The water content of the ethanol is less than 0.01% (V/V).

所述水热温度为140-180 °C。The hydrothermal temperature is 140-180 °C.

所述Bi(NO3)3·5H2O与盐酸四环素摩尔比为1.8-2：1。The molar ratio of Bi(NO 3 ) 3 ·5H 2 O to tetracycline hydrochloride is 1.8-2:1.

所述去离子水，无水乙醇和乙二醇的总体积为500 ml。The total volume of the deionized water, absolute ethanol and ethylene glycol was 500 ml.

本发明采用上述技术方案所设计的一种利用细胞粉碎机剥离Bi3O4Cl的方法，首先由水热和烧结法相结合制备出Bi3O4Cl光催化剂，所制备的Bi3O4Cl形貌呈不规则的块体结构，厚度约为200-400 nm；接着利用细胞粉碎机对制备的块体Bi3O4Cl光催化剂进行超声剥离，使Bi3O4Cl由块体剥离为Bi3O4Cl纳米片，纳米片的厚度约为10-50 nm，超薄纳米片使其光生载流子的迁移速率快，分离效率高，具备较好的光催化还原CO2性能。The present invention adopts a method for peeling off Bi 3 O 4 Cl by using a cell crusher designed by the above technical scheme. First, a Bi 3 O 4 Cl photocatalyst is prepared by combining hydrothermal and sintering methods. The prepared Bi 3 O 4 Cl The morphology is an irregular bulk structure, and the thickness is about 200-400 nm; then the prepared bulk Bi 3 O 4 Cl photocatalyst is ultrasonically exfoliated by a cell pulverizer, so that Bi 3 O 4 Cl is exfoliated from the block into Bi 3 O 4 Cl nanosheets, the thickness of the nanosheets is about 10-50 nm, the ultrathin nanosheets enable the photogenerated carriers to have a fast migration rate, high separation efficiency, and good photocatalytic CO 2 reduction performance.

附图说明Description of drawings

图1为本发明实施例1和2所得样品的粉末X-射线衍射图；Fig. 1 is the powder X-ray diffraction pattern of the samples obtained in Examples 1 and 2 of the present invention;

图2为本发明实施例1和2所得样品的扫描电镜照片；Fig. 2 is the scanning electron microscope photograph of the obtained sample of the embodiment of the present invention 1 and 2;

图3为本发明实施例1和2所得样品的紫外可见漫反射光谱；Fig. 3 is the ultraviolet-visible diffuse reflectance spectrum of the samples obtained in the embodiments of the present invention 1 and 2;

图4为本发明实施例1和2所得样品的光电流响应；Fig. 4 is the photocurrent response of the samples obtained in Examples 1 and 2 of the present invention;

图5为本发明实施例1和2所得样品的光催化还原CO2性能。Figure 5 shows the photocatalytic CO 2 reduction performance of the samples obtained in Examples 1 and 2 of the present invention.

具体实施方式Detailed ways

本发明一种利用细胞粉碎机剥离Bi3O4Cl的方法，是以水为溶剂，以Bi(NO3)3·5H2O作为Bi源，盐酸四环素作为Cl源，采用水热法制备出Bi-O-Cl配合物，再通过烧结法制备出块体Bi3O4Cl光催化剂（即为B-Bi3O4Cl），再将B-Bi3O4Cl通过细胞粉碎机进行超声剥离制备超薄Bi3O4Cl纳米片（记为S-Bi3O4Cl），以提高其光催化性能。The present invention is a method for peeling Bi 3 O 4 Cl by using a cell crusher. Water is used as a solvent, Bi(NO 3 ) 3 ·5H 2 O is used as Bi source, and tetracycline hydrochloride is used as Cl source, and the hydrothermal method is used to prepare Bi-O-Cl complex, and then prepare the bulk Bi 3 O 4 Cl photocatalyst (that is, B-Bi 3 O 4 Cl) by sintering method, and then sonicate the B-Bi 3 O 4 Cl through a cell crusher Ultrathin Bi 3 O 4 Cl nanosheets (denoted as S-Bi 3 O 4 Cl) were prepared by exfoliation to improve their photocatalytic performance.

本发明一种利用细胞粉碎机剥离Bi3O4Cl的方法实施例1，其方法步骤为：Embodiment 1 of a method for stripping Bi 3 O 4 Cl by using a cell pulverizer according to the present invention, the method steps are:

⑴.称取1 g Bi(NO3)3·5H2O充分搅拌溶于35 ml去离子水中，接着加入0.5 g盐酸四环素，搅拌30 min，将混合液转入40 ml聚四氟乙烯内衬不锈钢釜水热釜中，在160 ℃下反应16 h。取出水热反应后的样品，使用离心机，每次在10000 r/min下离心10 min。分别用蒸馏水和乙醇洗涤离心沉淀若干次，最后置于80 ℃烘箱内干燥24 h，得到黑色Bi-O-Cl配合物前驱体。秤取0.2 g干燥后的前驱体放入马弗炉中在550 ℃下烧结3 h，升温速率为5 ℃/min，自然降至室温后收取样品，即得块体Bi3O4Cl光催化剂；⑴. Weigh 1 g of Bi(NO 3 ) 3 ·5H 2 O and dissolve it in 35 ml of deionized water with full stirring, then add 0.5 g of tetracycline hydrochloride, stir for 30 min, and transfer the mixture into 40 ml of polytetrafluoroethylene lining The reaction was carried out at 160 °C for 16 h in a stainless steel kettle hydrothermal kettle. The samples after hydrothermal reaction were taken out and centrifuged at 10,000 r/min for 10 min each time using a centrifuge. The centrifuged precipitate was washed with distilled water and ethanol for several times, and finally dried in an oven at 80 °C for 24 h to obtain the black Bi-O-Cl complex precursor. Weigh 0.2 g of the dried precursor, put it into a muffle furnace, and sinter it at 550 °C for 3 h with a heating rate of 5 °C/min. The sample was collected after naturally cooling to room temperature to obtain a bulk Bi 3 O 4 Cl photocatalyst. ;

⑵.称取300 mg步骤（1）制备的块体Bi3O4Cl样品于1000 ml烧杯中，加入100 ml去离子水、200 ml无水乙醇和200 ml乙二醇。用细胞粉碎机进行超声剥离，超声功率为40%，每次超声20 min后待冷却至室温再进行超声，每次补充无水乙醇至溶液达到500 ml，累计超声4 h后，静置沉淀，将沉淀物用蒸馏水和乙醇洗涤沉淀若干次，最后置于60 ℃烘箱内干燥24 h，得到超薄化样品。⑵. Weigh 300 mg of the bulk Bi 3 O 4 Cl sample prepared in step (1) into a 1000 ml beaker, add 100 ml deionized water, 200 ml absolute ethanol and 200 ml ethylene glycol. Ultrasonic peeling was carried out with a cell crusher, and the ultrasonic power was 40%. After each ultrasonic wave for 20 min, it was cooled to room temperature and then ultrasonicated. Each time, anhydrous ethanol was added to the solution until the solution reached 500 ml. The precipitate was washed several times with distilled water and ethanol, and finally dried in an oven at 60 °C for 24 h to obtain an ultra-thin sample.

本发明一种利用细胞粉碎机剥离Bi3O4Cl的方法实施例2，其方法步骤为：Embodiment 2 of a method for stripping Bi 3 O 4 Cl by using a cell pulverizer according to the present invention, the method steps are:

⑴.称取0.8 g Bi(NO3)3·5H2O充分搅拌溶于33 ml去离子水中，接着加入0.35 g盐酸四环素，搅拌40 min，将混合液转入40 ml聚四氟乙烯内衬不锈钢釜水热釜中，在180 ℃下反应16 h。取出水热反应后的样品，使用离心机，每次在10000 r/min下离心8 min，分别用蒸馏水和乙醇洗涤离心沉淀若干次，最后置于60 ℃烘箱内干燥18 h，得到黑色Bi-O-Cl配合物前驱体。秤取0.2 g干燥后的前驱体放入马弗炉中在500 ℃下烧结5 h，升温速率为2℃/min，自然降至室温后收取样品，即得块体Bi3O4Cl光催化剂；⑴. Weigh 0.8 g Bi(NO 3 ) 3 ·5H 2 O and dissolve it in 33 ml of deionized water with full stirring, then add 0.35 g of tetracycline hydrochloride, stir for 40 min, and transfer the mixture into 40 ml of polytetrafluoroethylene lining In a stainless steel kettle hydrothermal kettle, the reaction was carried out at 180 °C for 16 h. The samples after hydrothermal reaction were taken out, centrifuged at 10,000 r/min for 8 min each time using a centrifuge, washed with distilled water and ethanol for several times, and finally dried in a 60 °C oven for 18 h to obtain black Bi- O-Cl complex precursor. Weigh 0.2 g of the dried precursor, put it into a muffle furnace, sinter it at 500 °C for 5 h, the heating rate is 2 °C/min, and collect the sample after naturally cooling to room temperature to obtain a bulk Bi 3 O 4 Cl photocatalyst. ;

⑵.称取300 mg步骤（1）制备的块体Bi3O4Cl样品于1000 ml烧杯中，加入300 ml无水乙醇和200 ml乙二醇。用细胞粉碎机进行超声剥离，超声功率为60%，每次超声15 min后待冷却至室温再进行超声，每次补充无水乙醇至溶液达到500 ml，累计超声6 h后，静置沉淀，将沉淀物用蒸馏水和乙醇洗涤沉淀若干次，最后置于60 ℃烘箱内干燥24 h，得到超薄化样品。⑵. Weigh 300 mg of the bulk Bi 3 O 4 Cl sample prepared in step (1) into a 1000 ml beaker, add 300 ml of absolute ethanol and 200 ml of ethylene glycol. Ultrasonic peeling was carried out with a cell crusher, and the ultrasonic power was 60%. After each ultrasonic wave for 15 min, it was cooled to room temperature and then ultrasonicated. Each time, anhydrous ethanol was added until the solution reached 500 ml. The precipitate was washed several times with distilled water and ethanol, and finally dried in an oven at 60 °C for 24 h to obtain an ultra-thin sample.

本发明一种利用细胞粉碎机剥离Bi3O4Cl的方法实施例3，其方法步骤为：Embodiment 3 of a method for stripping Bi 3 O 4 Cl using a cell crusher of the present invention, the method steps are:

⑴.称取0.5 g Bi(NO3)3·5H2O充分搅拌溶于33 ml去离子水中，接着加入0.28 g盐酸四环素，搅拌30 min，将混合液转入40 ml聚四氟乙烯内衬不锈钢釜水热釜中，在180 ℃下反应24 h。取出水热反应后的样品，使用离心机，每次在10000 r/min下离心8 min，分别用蒸馏水和乙醇洗涤离心沉淀若干次，最后置于60 ℃烘箱内干燥18 h，得到黑色Bi-O-Cl配合物前驱体。秤取0.2 g干燥后的前驱体放入马弗炉中在450℃下烧结5 h，升温速率为1℃/min，自然降至室温后收取样品，即得块体Bi3O4Cl光催化剂；⑴. Weigh 0.5 g Bi(NO 3 ) 3 ·5H 2 O and dissolve it in 33 ml of deionized water with full stirring, then add 0.28 g of tetracycline hydrochloride, stir for 30 min, and transfer the mixture into 40 ml of polytetrafluoroethylene lining In a stainless steel kettle hydrothermal kettle, the reaction was carried out at 180 °C for 24 h. The samples after hydrothermal reaction were taken out, centrifuged at 10,000 r/min for 8 min each time using a centrifuge, washed with distilled water and ethanol for several times, and finally dried in a 60 °C oven for 18 h to obtain black Bi- O-Cl complex precursor. Weigh 0.2 g of the dried precursor, put it into a muffle furnace and sinter it at 450 °C for 5 h, with a heating rate of 1 °C/min, and collect the sample after naturally cooling to room temperature to obtain a bulk Bi 3 O 4 Cl photocatalyst. ;

⑵.称取300 mg步骤（1）制备的块体Bi3O4Cl样品于1000 ml烧杯中，加入100 ml去离子水、300 ml无水乙醇和100 ml乙二醇。用细胞粉碎机进行超声剥离，超声功率为80%，每次超声20 min后待冷却至室温再进行超声，每次补充无水乙醇至溶液达到500 ml，累计超声7 h后，静置沉淀，将沉淀物用蒸馏水和乙醇洗涤沉淀若干次，最后置于60 ℃烘箱内干燥24 h，得到超薄化样品。⑵. Weigh 300 mg of the bulk Bi 3 O 4 Cl sample prepared in step (1) into a 1000 ml beaker, add 100 ml deionized water, 300 ml absolute ethanol and 100 ml ethylene glycol. Ultrasonic peeling was carried out with a cell crusher, and the ultrasonic power was 80%. After each ultrasonic wave for 20 min, it was cooled to room temperature before ultrasonication. Each time, anhydrous ethanol was added to the solution until the solution reached 500 ml. The precipitate was washed several times with distilled water and ethanol, and finally dried in an oven at 60 °C for 24 h to obtain an ultra-thin sample.

本发明一种利用细胞粉碎机剥离Bi3O4Cl的方法实施例4，其方法步骤为：Embodiment 4 of a method for stripping Bi 3 O 4 Cl using a cell crusher according to the present invention, the method steps are:

⑴.称取0.8 g Bi(NO3)3·5H2O充分搅拌溶于33 ml去离子水中，接着加入0.35 g盐酸四环素，搅拌40 min，将混合液转入40 ml聚四氟乙烯内衬不锈钢釜水热釜中，在180 ℃下反应16 h。取出水热反应后的样品，使用离心机，每次在10000 r/min下离心8 min。分别用蒸馏水和乙醇洗涤离心沉淀若干次，最后置于60 ℃烘箱内干燥18 h，得到黑色Bi-O-Cl配合物前驱体。秤取0.2 g干燥后的前驱体放入马弗炉中在550 ℃下烧结5 h，升温速率为5℃/min，自然降至室温后收取样品，即得块体Bi3O4Cl光催化剂；⑴. Weigh 0.8 g Bi(NO 3 ) 3 ·5H 2 O and dissolve it in 33 ml of deionized water with full stirring, then add 0.35 g of tetracycline hydrochloride, stir for 40 min, and transfer the mixture into 40 ml of polytetrafluoroethylene lining In a stainless steel kettle hydrothermal kettle, the reaction was carried out at 180 °C for 16 h. The samples after hydrothermal reaction were taken out and centrifuged at 10,000 r/min for 8 min each time using a centrifuge. The centrifuged precipitate was washed with distilled water and ethanol for several times, and finally dried in an oven at 60 °C for 18 h to obtain the black Bi-O-Cl complex precursor. Weigh 0.2 g of the dried precursor, put it in a muffle furnace, sinter at 550 °C for 5 h, the heating rate is 5 °C/min, and collect the sample after naturally cooling to room temperature to obtain a bulk Bi 3 O 4 Cl photocatalyst. ;

⑵.称取300 mg步骤（1）制备的块体Bi3O4Cl样品于1000 ml烧杯中，加入200 ml去离子水、150 ml无水乙醇和150 ml乙二醇。用细胞粉碎机进行超声剥离，超声功率为60%，每次超声18 min后待冷却至室温再进行超声，每次补充无水乙醇至溶液达到500 ml，累计超声6 h后，静置沉淀，将沉淀物用蒸馏水和乙醇洗涤沉淀若干次，最后置于60 ℃烘箱内干燥24 h，得到超薄化样品。⑵. Weigh 300 mg of the bulk Bi 3 O 4 Cl sample prepared in step (1) into a 1000 ml beaker, add 200 ml of deionized water, 150 ml of absolute ethanol and 150 ml of ethylene glycol. Ultrasonic peeling was carried out with a cell crusher, and the ultrasonic power was 60%. After each ultrasonic wave for 18 min, it was cooled to room temperature before ultrasonication. Each time, anhydrous ethanol was added to the solution until the solution reached 500 ml. The precipitate was washed several times with distilled water and ethanol, and finally dried in an oven at 60 °C for 24 h to obtain an ultra-thin sample.

本发明一种利用细胞粉碎机剥离Bi3O4Cl的方法实施例5，其方法步骤为：Embodiment 5 of a method for stripping Bi 3 O 4 Cl by using a cell pulverizer of the present invention, the method steps are:

⑴.称取1 g Bi(NO3)3·5H2O充分搅拌溶于33 ml去离子水中，接着加入0.48 g盐酸四环素，搅拌40 min，将混合液转入40 ml聚四氟乙烯内衬不锈钢釜水热釜中，在180 ℃下反应16 h。取出水热反应后的样品，使用离心机，每次在10000 r/min下离心8 min，分别用蒸馏水和乙醇洗涤离心沉淀若干次，最后置于60 ℃烘箱内干燥18 h，得到黑色Bi-O-Cl配合物前驱体。秤取0.2 g干燥后的前驱体放入马弗炉中在500 ℃下烧结5 h，升温速率为2 ℃/min，自然降至室温后收取样品，即得块体Bi3O4Cl光催化剂。⑴. Weigh 1 g of Bi(NO 3 ) 3 ·5H 2 O and dissolve it in 33 ml of deionized water with full stirring, then add 0.48 g of tetracycline hydrochloride, stir for 40 min, and transfer the mixture into 40 ml of polytetrafluoroethylene lining In a stainless steel kettle hydrothermal kettle, the reaction was carried out at 180 °C for 16 h. The samples after hydrothermal reaction were taken out, centrifuged at 10,000 r/min for 8 min each time using a centrifuge, washed with distilled water and ethanol for several times, and finally dried in a 60 °C oven for 18 h to obtain black Bi- O-Cl complex precursor. Weigh 0.2 g of the dried precursor, put it into a muffle furnace, sinter at 500 °C for 5 h, the heating rate is 2 °C/min, and then naturally drop to room temperature and collect the sample to obtain a bulk Bi 3 O 4 Cl photocatalyst. .

⑵.称取300 mg步骤（1）制备的块体Bi3O4Cl样品于1000 ml烧杯中，加入200 ml去离子水、100 ml无水乙醇和200 ml乙二醇，用细胞粉碎机进行超声剥离，超声功率为70%，每次超声16 min后待冷却至室温再进行超声，每次补充无水乙醇至溶液达到500 ml，累计超声5 h后，静置沉淀，将沉淀物用蒸馏水和乙醇洗涤沉淀若干次，最后置于80 ℃烘箱内干燥24 h，得到超薄化样品。⑵. Weigh 300 mg of the bulk Bi 3 O 4 Cl sample prepared in step (1) into a 1000 ml beaker, add 200 ml of deionized water, 100 ml of absolute ethanol and 200 ml of ethylene glycol, and use a cell crusher Ultrasonic peeling, the ultrasonic power is 70%, after each ultrasonic wave for 16 min, it will be cooled to room temperature before ultrasonication, and anhydrous ethanol will be added each time until the solution reaches 500 ml. The precipitates were washed several times with ethanol, and finally dried in an oven at 80 °C for 24 h to obtain ultrathin samples.

本发明利用细胞粉碎机剥离出的Bi3O4Cl在光催化还原CO2的应用，实施例6：The present invention utilizes the application of Bi 3 O 4 Cl exfoliated by a cell pulverizer in photocatalytic reduction of CO 2 , Example 6:

光催化还原CO2是利用催化剂通过光催化反应将CO2还原为CO和CH4等太阳能燃料，对缓解目前能源短缺和温室效应等问题具有重要意义。具体操作流程如下：采用北京泊菲莱科技有限公司的气体密封石英反应器，反应器的体积为350 mL，以300 W高压氙灯为光源，在离线***上进行光催化CO2还原实验。将0.05 g的光催化剂Bi3O4Cl均匀地分散在28.26 cm2的圆形石英片上，在反应器底部加入1.7 g NaHCO3，在照射之前，对上述***进行真空处理，以完全去除反应器内的空气。随后将4 M H2SO4（5 mL）注入反应池，与NaHCO3反应生成1atm CO2气体。采用DC-0506低温恒温槽***，使光反应装置温度保持在20 ℃。在给定的时间间隔内，使用注射器抽取约1 ml气体，用气相色谱仪对CO2还原产物进行测定，色谱检测到的气体为CO，CH4和CO2，生成量通过标准曲线进行量化。Photocatalytic reduction of CO2 is the use of catalysts to reduce CO2 to solar fuels such as CO and CH4 through a photocatalytic reaction, which is of great significance for alleviating the current problems of energy shortage and greenhouse effect. The specific operation process is as follows: A gas-sealed quartz reactor of Beijing Bofeilai Technology Co., Ltd. with a volume of 350 mL was used, and a 300 W high-pressure xenon lamp was used as the light source, and the photocatalytic CO reduction experiment was carried out on an offline system. 0.05 g of the photocatalyst Bi3O4Cl was uniformly dispersed on a 28.26 cm2 circular quartz plate, 1.7 g NaHCO3 was added at the bottom of the reactor, and before irradiation, the above system was subjected to vacuum treatment to completely remove the reactor air inside. Then 4 MH 2 SO 4 (5 mL) was injected into the reaction cell to react with NaHCO 3 to generate 1 atm CO 2 gas. The temperature of the photoreaction device was maintained at 20 °C using a DC-0506 low temperature thermostatic bath system. At a given time interval, about 1 ml of gas was drawn using a syringe, and the CO 2 reduction products were determined with a gas chromatograph. The gases detected by chromatography were CO, CH 4 and CO 2 , and the production was quantified by a standard curve.

本发明图1为实施例1和2所得样品的粉末X-射线衍射图，从图中可以看出，S-Bi3O4Cl样品的衍射谱图在2θ=24.0 º、29.1 º、29.7 º、31.4 º、31.6 º和45.3 º处出现几个强峰，这些峰位与Bi3O4Cl标准PDF（36-0760）卡片所出现的峰位一致，这几处峰位对应着Bi3O4Cl的单斜晶系结构，且其XRD衍射谱图与Bi3O4Cl标准PDF（36-0760）卡片相比没有其它杂峰，峰位也无偏移，说明细胞粉碎机对Bi3O4Cl进行超声剥离并为改变其物相组成，所得超薄化样品仍为Bi3O4Cl纯相，且样品的晶型较好。图2为实施例1和2所得样品的扫描电镜图片，（a）B-Bi3O4Cl；（b）S-Bi3O4Cl，所制备的B-Bi3O4Cl形貌呈不规则的块体结构，厚度约为200-400 nm，而超声剥离后的样品S-Bi3O4Cl形貌大部分为块体剥离成的超薄纳米片，纳米片的厚度约为10-50 nm，说明利用细胞粉碎机对样品成功进行了剥离。图3为实施例1和2所得样品的紫外可见漫反射光谱，从图中可以看出，与B-Bi3O4Cl相比，S-Bi3O4Cl样品在可见光区的吸光强度更高，且吸光范围扩展至整个可见光区。图4为实施例1和2所得样品的光电流响应，从图中可以看出S-Bi3O4Cl具有比B-Bi3O4Cl更强的光电流强度，其光电流强度比B-Bi3O4Cl提升了约2 μA·cm-2。Figure 1 of the present invention is the powder X-ray diffraction pattern of the samples obtained in Examples 1 and 2. It can be seen from the figure that the diffraction pattern of the S-Bi 3 O 4 Cl sample is at 2θ=24.0 º, 29.1 º, 29.7 º , 31.4 º, 31.6 º and 45.3 º appeared several strong peaks, these peak positions are consistent with the peak positions of Bi 3 O 4 Cl standard PDF (36-0760) card, these peak positions correspond to Bi 3 O The monoclinic crystal structure of 4 Cl, and its XRD diffraction pattern has no other impurity peaks compared with the Bi 3 O 4 Cl standard PDF (36-0760) card, and the peak position is not shifted, indicating that the cell crusher has no effect on Bi 3 Ultra-thin samples obtained by ultrasonic exfoliation of O 4 Cl are still pure Bi 3 O 4 Cl, and the crystal form of the samples is better in order to change its phase composition. Figure 2 is the scanning electron microscope pictures of the samples obtained in Examples 1 and 2, (a) B-Bi 3 O 4 Cl; (b) S-Bi 3 O 4 Cl, the prepared B-Bi 3 O 4 Cl has a morphology The irregular bulk structure has a thickness of about 200-400 nm, while the morphology of the S-Bi 3 O 4 Cl sample after ultrasonic exfoliation is mostly ultra-thin nanosheets exfoliated from the bulk, and the thickness of the nanosheets is about 10 nm. -50 nm, indicating that the sample was successfully peeled off with a cell crusher. Fig. 3 is the UV-Vis diffuse reflectance spectra of the samples obtained in Examples 1 and 2. It can be seen from the figure that the S-Bi 3 O 4 Cl sample has a higher light absorption intensity in the visible light region than that of the B-Bi 3 O 4 Cl sample. high, and the absorption range extends to the entire visible light region. Figure 4 shows the photocurrent responses of the samples obtained in Examples 1 and 2. It can be seen from the figure that S-Bi 3 O 4 Cl has a stronger photocurrent intensity than B-Bi 3 O 4 Cl, and its photocurrent intensity is stronger than that of B-Bi 3 O 4 Cl -Bi 3 O 4 Cl increased by about 2 μA·cm −2 .

图5为本发明实施例1和2所得样品的光催化还原CO2性能，图中可看出，S-Bi3O4Cl样品相比于块体的B-Bi3O4Cl样品，其在CO2转化为CO反应中显示出更高的光催化效率和选择性。所制备的样品生成的CO气体的产率随着照射时间而增加，并且随时间线性累积。S-Bi3O4Cl的CO生成速率为1.89 μmol g-1 h -1，相比于B-Bi3O4Cl的CO生成速率0.30 μmol g-1h-1，性能高出近6倍。Figure 5 shows the photocatalytic CO 2 reduction performance of the samples obtained in Examples 1 and 2 of the present invention. It can be seen from the figure that the S-Bi 3 O 4 Cl sample has a better performance than the bulk B-Bi 3 O 4 Cl sample. showed higher photocatalytic efficiency and selectivity in the CO2 -to-CO reaction. The yield of CO gas generated by the prepared samples increased with irradiation time and accumulated linearly with time. The CO generation rate of S-Bi 3 O 4 Cl is 1.89 μmol g -1 h -1 , which is nearly 6 times higher than the CO generation rate of B-Bi 3 O 4 Cl 0.30 μmol g -1 h -1 . .

Claims (7)

1. Bi stripping by cell crusher3O4Cl process, characterized in that it uses water as solvent and Bi (NO)3)3·5H2O is used as a Bi source, tetracycline hydrochloride is used as a Cl source, a hydrothermal method is adopted to prepare a Bi-O-Cl complex, and a sintering method is adopted to prepare a bulk Bi3O4Cl photocatalyst (B-Bi)3O4Cl), and then adding B-Bi3O4Cl is ultrasonically stripped through a cell crusher to prepare ultrathin Bi3O4Cl nanosheet (S-Bi)3O4Cl) to improve its photocatalytic properties; the method comprises the following steps:
⑴ weighing 0.4-1 g Bi (NO)3)3·5H2Fully stirring and dissolving O in 30-35 ml of deionized water, then adding 0.2-0.5 g of tetracycline hydrochloride, stirring for 30-60 min, putting into a 40 ml stainless steel kettle hydrothermal kettle with a polytetrafluoroethylene lining, and reacting for 15-24 h at 140-180 ℃;
⑵, taking out the sample after the hydrothermal reaction obtained in the step ⑴, centrifuging for 3-10 min at 10000 r/min each time by using a centrifuge, washing and centrifuging and precipitating for a plurality of times by using distilled water and ethanol respectively, finally drying in an oven at 60-100 ℃ for 12-24 h to obtain a black Bi-O-Cl complex precursor, weighing 0.2-2 g of the dried precursor, putting the dried precursor into a muffle furnace, sintering for 2-10 h at 450-600 ℃, raising the temperature at the rate of 1-5 ℃/min, naturally cooling to room temperature, and collecting the sample to obtain the block Bi3O4A Cl photocatalyst;
⑶ weighing 300 mg of the bulk Bi prepared in step ⑵3O4Adding 0-200 ml of deionized water, 0-500 ml of absolute ethyl alcohol and 0-500 ml of ethylene glycol into a Cl sample in a 1000 ml beaker, carrying out ultrasonic stripping by using a cell crusher, wherein the ultrasonic power is 40-80%, carrying out ultrasonic treatment after cooling to room temperature after 15-30 min of each ultrasonic treatment, supplementing absolute ethyl alcohol each time until the solution reaches 500 ml, accumulating the ultrasonic treatment for 4-8 h, standing and precipitating, washing and precipitating the precipitate by using distilled water and ethanol for a plurality of times, finally drying in an oven at 60-100 ℃ for 12-24 h to obtain an ultrathin sample, and carrying out XRD, SEM, DRS and photocurrent test on Bi by using the technical means of3O4The phase composition, the micro morphology, the charge separation and the photocatalytic performance of the Cl photocatalyst are researched.
2. The method of claim 1 for stripping Bi by using a cell crusher3O4Cl, characterized in that said ethylene glycol has a water content of less than 0.01% (V/V).
3. The method of claim 1 for stripping Bi by using a cell crusher3O4Cl, characterized in that the ethanol has a water content of less than 0.01% (V/V).
4. The method of claim 1 for stripping Bi by using a cell crusher3O4The Cl method is characterized in that the hydrothermal temperature is 140-180 ℃.
5. The method of claim 1 for stripping Bi by using a cell crusher3O4Cl, characterized in that said Bi (NO)3)3·5H2The molar ratio of O to tetracycline hydrochloride is 1.8-2: 1.
6. the method of claim 1 for stripping Bi by using a cell crusher3O4Cl, characterized in that the total volume of said deionized water, absolute ethanol and ethylene glycol is 500 ml.
7. The Bi of claim 1 exfoliated using a cell disruptor3O4Photocatalytic reduction of CO with Cl2Application of the aspect.
CN202010505296.8A 2020-06-05 2020-06-05 Bi stripping by cell crusher3O4Method for Cl and in photocatalytic reduction of CO2Application of aspects Pending CN111644185A (en)

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