CN105879855A - Graphene-gamma-bismuth molybdate nano-composite material, method for preparing same and application of graphene-gamma-bismuth molybdate nano-composite material - Google Patents
Graphene-gamma-bismuth molybdate nano-composite material, method for preparing same and application of graphene-gamma-bismuth molybdate nano-composite material Download PDFInfo
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Abstract
本发明公开了一种石墨烯‑γ‑钼酸铋纳米复合材料的制备方法，包括以下步骤：1)将石墨烯，硝酸铋和乙二醇一起溶剂热反应，再经过滤、洗涤、烘干得石墨烯‑乙二醇铋复合物；2)将所得复合物均匀分散在钼酸钠水溶液中，调节所得溶液体系的pH值为0‑3，然后进行水热反应，再经过滤、洗涤、烘干得石墨烯‑γ‑钼酸铋纳米复合材料。本发明以石墨烯、硝酸铋、钼酸钠，乙二醇为主要原料，采用溶剂热法和水热法相结合制备出石墨烯‑γ‑钼酸铋纳米复合材料，本法涉及的制备工艺设备简单、反应条件温和、能耗小，工艺新颖，制备的纳米复合材料比表面积大，可见光光催化性能优异。The invention discloses a preparation method of a graphene-γ-bismuth molybdate nanocomposite material, comprising the following steps: 1) solvothermally reacting graphene, bismuth nitrate and ethylene glycol together, and then filtering, washing and drying Obtain graphene-ethylene glycol bismuth compound; 2) Gained compound is uniformly dispersed in sodium molybdate aqueous solution, the pH value of adjusting gained solution system is 0-3, then carries out hydrothermal reaction, then through filtering, washing, Dry to obtain graphene-γ-bismuth molybdate nanocomposites. The present invention uses graphene, bismuth nitrate, sodium molybdate and ethylene glycol as main raw materials, adopts solvothermal method and hydrothermal method to prepare graphene-γ-bismuth molybdate nanocomposite material, and the preparation process equipment involved in this method Simple, mild reaction conditions, low energy consumption, novel process, large specific surface area of the prepared nanocomposite, and excellent visible light photocatalytic performance.
Description
技术领域technical field
本发明属于环保新材料领域，具体涉及一种石墨烯-γ-钼酸铋纳米复合材料及其制备方法和应用。The invention belongs to the field of new environmental protection materials, and in particular relates to a graphene-γ-bismuth molybdate nanocomposite material and its preparation method and application.
背景技术Background technique
环境污染的严重性，已成为一个直接威胁人类生存，亟需解决的焦点问题。光催化技术作为绿色化学的一个分支，该技术能使环境中的有机污染物发生氧化分解反应，最终降解为CO2、水和无机离子等小分子物质，无二次污染、降解程度高，被认为是最有前景的污染处理方法。但传统的TiO2光催化剂，带隙宽，主要吸收紫外光，只能利用太阳光中的紫外光，对太阳光的利用率低。开发能利用可见光光催化的纳米新材料作为高催化活性、能充分利用太阳光的光催化剂，是控制环境污染最具前景的方法之一。因此开发设计新型高效、稳定和可见光响应的半导体光催化剂是当前光催化研究的热点。The seriousness of environmental pollution has become a focal issue that directly threatens human existence and needs to be resolved urgently. As a branch of green chemistry, photocatalytic technology can oxidize and decompose organic pollutants in the environment, and finally degrade them into small molecules such as CO 2 , water and inorganic ions, without secondary pollution and high degree of degradation. It is considered to be the most promising pollution treatment method. However, the traditional TiO2 photocatalyst has a wide band gap, mainly absorbs ultraviolet light, and can only use ultraviolet light in sunlight, so the utilization rate of sunlight is low. The development of new nanomaterials that can utilize visible light photocatalysis as a photocatalyst with high catalytic activity and can fully utilize sunlight is one of the most promising methods for controlling environmental pollution. Therefore, the development and design of new semiconductor photocatalysts with high efficiency, stability and visible light response is a hot spot in current photocatalysis research.
纳米γ-钼酸铋(Bi2MoO6)是近几年兴起的、受到广泛关注度一种可见光半导体催化剂，它在可见光下具有良好的光催化活性，可用于降解环境有机污染物、光催化制氧和光催化还原二氧化碳等。但其主要缺点是铋系半导体光催化剂均存在光生电子-空穴容易再结合，极大地限制了铋系光催化剂的大规模应用。因此，必须采取一定的措施来提高光生电子迁移效率，有效限制电子空穴再结合。石墨烯是一种高效的电子受体材料，其与γ-钼酸铋(Bi2MoO6)半导体复合有利于提高光照下电子-空穴的分离效率，降低电子空穴再结合，从而提高复合材料的光催化活性，因此石墨烯-γ-钼酸铋纳米复合材料具有比单纯纳米γ-钼酸铋更高的光催化效率。开发一种工艺简单的石墨烯-γ-钼酸铋纳米复合材料的制备方法具有重要意义。Nano γ-bismuth molybdate (Bi 2 MoO 6 ) is a kind of visible light semiconductor catalyst that has emerged in recent years and has received widespread attention. It has good photocatalytic activity under visible light and can be used to degrade environmental organic pollutants, photocatalytic Oxygen production and photocatalytic reduction of carbon dioxide, etc. However, its main disadvantage is that the photogenerated electrons and holes in bismuth-based semiconductor photocatalysts are easy to recombine, which greatly limits the large-scale application of bismuth-based photocatalysts. Therefore, certain measures must be taken to improve the transfer efficiency of photogenerated electrons and effectively limit the electron-hole recombination. Graphene is a high-efficiency electron acceptor material, and its compounding with γ-bismuth molybdate (Bi 2 MoO 6 ) semiconductor is beneficial to improve the separation efficiency of electrons and holes under light, reduce the recombination of electrons and holes, and thus improve the recombination efficiency. The photocatalytic activity of the material, so the graphene-γ-bismuth molybdate nanocomposite material has higher photocatalytic efficiency than pure nanometer γ-bismuth molybdate. It is of great significance to develop a preparation method of graphene-γ-bismuth molybdate nanocomposites with simple process.
发明内容Contents of the invention
本发明的目的是提供一种石墨烯-γ-钼酸铋纳米复合材料及其制备方法，该方法涉及的工艺设备简单、反应条件温和、能耗小，制备的石墨烯-γ-钼酸铋纳米复合材料比表面积大，可见光光催化性能优异。The object of the present invention is to provide a kind of graphene-γ-bismuth molybdate nanocomposite material and preparation method thereof, the processing equipment involved in this method is simple, reaction condition mildness, energy consumption is little, the prepared graphene-γ-bismuth molybdate The nanocomposite material has a large specific surface area and excellent visible light photocatalytic performance.
为实现上述目的，本发明采用的技术方案为：一种石墨烯-γ-钼酸铋纳米复合材料的制备方法，包括以下步骤：1)将石墨烯，硝酸铋和乙二醇一起溶剂热反应，再经过滤、洗涤、烘干得石墨烯-乙二醇铋复合物；2)将所得复合物均匀分散在钼酸钠水溶液中，调节所得溶液体系的pH值为0-3，然后进行水热反应，再经过滤、洗涤、烘干得石墨烯-γ-钼酸铋纳米复合材料。In order to achieve the above object, the technical scheme adopted in the present invention is: a kind of preparation method of graphene-γ-bismuth molybdate nanocomposite material, comprises the following steps: 1) with graphene, bismuth nitrate and ethylene glycol solvent thermal reaction together , and then filtered, washed, and dried to obtain a graphene-ethylene glycol bismuth composite; 2) the obtained composite is uniformly dispersed in an aqueous solution of sodium molybdate, and the pH value of the obtained solution system is adjusted to 0-3, and then the water thermal reaction, and then filtered, washed, and dried to obtain a graphene-γ-bismuth molybdate nanocomposite material.
按上述方案，所述石墨烯为硝酸铋质量的0.5-5％。According to the above scheme, the graphene is 0.5-5% of the mass of bismuth nitrate.
按上述方案，所述硝酸铋在乙二醇中的浓度为10-100g/L。According to the above scheme, the concentration of the bismuth nitrate in ethylene glycol is 10-100g/L.
按上述方案，所述溶剂热反应条件为：加热至160-180℃保温反应2-24小时，然后自然冷却至室温。According to the above scheme, the solvothermal reaction conditions are: heating to 160-180° C. for 2-24 hours, and then naturally cooling to room temperature.
按上述方案，所述钼酸钠与石墨烯-乙二醇铋复合物的质量为(0.35-0.5):1。According to the above scheme, the quality of the sodium molybdate and graphene-ethylene glycol bismuth compound is (0.35-0.5):1.
按上述方案，所述钼酸钠水溶液的浓度为20-100g/L。According to the above scheme, the concentration of the sodium molybdate aqueous solution is 20-100g/L.
按上述方案，所述水热反应条件为加热至150-200℃保温反应1-24小时。According to the above scheme, the hydrothermal reaction condition is heating to 150-200° C. for 1-24 hours.
按上述方案，步骤1)所述烘干温度为80-100℃；步骤2)所述烘干温度为80-120℃。According to the above scheme, the drying temperature in step 1) is 80-100° C.; the drying temperature in step 2) is 80-120° C.
上述所述制备方法制得的石墨烯-γ-钼酸铋纳米复合材料，其为纳米晶片状，晶片厚度为10-40nm，比表面积为30-60m2/g。The graphene-γ-bismuth molybdate nanocomposite material prepared by the above-mentioned preparation method is in the shape of a nano-chip, the thickness of the chip is 10-40 nm, and the specific surface area is 30-60 m 2 /g.
所述的石墨烯-γ-钼酸铋纳米复合材料作为光催化材料的应用。The application of the graphene-γ-bismuth molybdate nanocomposite material as a photocatalytic material.
本发明的机理：由于石墨烯具有单层二维结构，高导电性，优良的电子迁移率和极高的比表面积等特性，使其可以构筑半导体-石墨烯异质结来增强可见光催化活性。负载的石墨烯有利于电子的转移和存储，与γ-钼酸铋材料复合后能有效转移光生载流子，抑制光生电子-空穴对的复合，同时提供大的比表面积，改善的石墨烯-γ-钼酸铋纳米复合催化剂的光催化活性，并且石墨烯边界处的含氧功能团对有机物污染物有强吸附性，也能增强复合材料的光催化活性。Mechanism of the present invention: Since graphene has a single-layer two-dimensional structure, high electrical conductivity, excellent electron mobility and extremely high specific surface area, it can construct a semiconductor-graphene heterojunction to enhance visible light catalytic activity. The supported graphene is conducive to the transfer and storage of electrons. After being combined with γ-bismuth molybdate materials, it can effectively transfer photogenerated carriers, inhibit the recombination of photogenerated electron-hole pairs, and provide a large specific surface area. Improved graphene - The photocatalytic activity of the γ-bismuth molybdate nanocomposite catalyst, and the oxygen-containing functional groups at the graphene boundary have strong adsorption to organic pollutants, which can also enhance the photocatalytic activity of the composite material.
本发明的有益效果为：本发明以石墨烯、硝酸铋、乙二醇、钼酸钠为主要原料，采用溶剂热和水热法制备石墨烯-γ-钼酸铋纳米复合材料，得到的复合材料化学成分均一，石墨烯高度分散，由于石墨烯具有高的电子接受能力，γ-钼酸铋复合材料在光催化时，电子-空穴分离率高，光催化效果比复合相比显著提高。同时本制备工艺设备简单、反应条件温和、能耗低。The beneficial effects of the present invention are as follows: the present invention uses graphene, bismuth nitrate, ethylene glycol, and sodium molybdate as main raw materials, adopts solvothermal and hydrothermal methods to prepare graphene-γ-bismuth molybdate nanocomposites, and the obtained composite The chemical composition of the material is uniform, and the graphene is highly dispersed. Due to the high electron accepting ability of graphene, the γ-bismuth molybdate composite material has a high electron-hole separation rate during photocatalysis, and the photocatalytic effect is significantly improved compared with the composite. At the same time, the preparation process has simple equipment, mild reaction conditions and low energy consumption.
具体实施方式detailed description
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明不仅仅局限于下面的实施例。In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the examples, but the present invention is not limited to the following examples.
以下实施例如无具体说明，采用的试剂市售化学试剂或工业产品。The following examples are not specifically described, and the reagents used are commercially available chemical reagents or industrial products.
实施例1Example 1
石墨烯-γ-钼酸铋纳米复合材料的制备方法，包括以下步骤：The preparation method of graphene-γ-bismuth molybdate nanocomposite material comprises the following steps:
1)将100g硝酸铋溶于1L乙二醇中，然后加入0.5g石墨烯粉搅拌混合均匀，得到稳定悬浊液，将此溶液转移到容积为2L的高压釜中，加热至160℃并保温24小时；待反应釜冷却至室温，过滤并用乙醇洗涤3次，然后在80℃下干燥12小时，得石墨烯-乙二醇铋粉体；1) Dissolve 100g of bismuth nitrate in 1L of ethylene glycol, then add 0.5g of graphene powder and mix evenly to obtain a stable suspension. Transfer this solution to an autoclave with a volume of 2L, heat to 160°C and keep it warm 24 hours; after the reactor is cooled to room temperature, filter and wash with ethanol for 3 times, and then dry at 80°C for 12 hours to obtain graphene-bismuth ethylene glycol powder;
2)取25g钼酸钠溶于250ml去离子水中，再将1)中制备石墨烯-乙二醇粉末50g加入上述钼酸钠水溶液中，超声波震荡搅拌使其分散均匀，用浓硝酸和浓盐酸调节溶液pH值至0-3之间，然后将所得混合液转移至容积为500mL的高压釜中，升温至200℃保温1小时，待反应釜冷却至室温，过滤后用去离子水和乙醇洗涤5次，再在120℃下干燥4小时，得石墨烯-钼酸铋钠纳米复合材料。2) Take 25g of sodium molybdate and dissolve it in 250ml of deionized water, then add 50g of the graphene-ethylene glycol powder prepared in 1) into the above-mentioned sodium molybdate aqueous solution, stir with ultrasonic vibration to make it evenly dispersed, and use concentrated nitric acid and concentrated hydrochloric acid Adjust the pH value of the solution to between 0-3, then transfer the resulting mixture to an autoclave with a volume of 500mL, raise the temperature to 200°C and keep it warm for 1 hour, wait for the reaction kettle to cool down to room temperature, filter and wash with deionized water and ethanol 5 times, and then dried at 120° C. for 4 hours to obtain a graphene-sodium bismuth molybdate nanocomposite material.
本实施例所得产物γ-钼酸铋纳米晶片平均厚度为10nm，比表面积为60m2/g，在浓度1.0g/L时，可见光照射下能在30min内完全降解0.02g/L罗丹明。The γ-bismuth molybdate nanochips obtained in this example have an average thickness of 10 nm and a specific surface area of 60 m 2 /g. When the concentration is 1.0 g/L, 0.02 g/L rhodamine can be completely degraded within 30 minutes under visible light irradiation.
实施例2Example 2
石墨烯-γ-钼酸铋纳米复合材料的制备方法，包括以下步骤：The preparation method of graphene-γ-bismuth molybdate nanocomposite material comprises the following steps:
1)将50g硝酸铋溶于1L乙二醇中，然后加入2.5g石墨烯粉搅拌混合均匀，得到稳定悬浊液，将此溶液转移到容积为2L的高压釜中，加热至180℃并保温2小时；待反应釜冷却至室温，过滤并用乙醇洗涤3次，然后在80℃下干燥6小时，得石墨烯-乙二醇铋粉体；1) Dissolve 50g of bismuth nitrate in 1L of ethylene glycol, then add 2.5g of graphene powder and mix evenly to obtain a stable suspension. Transfer this solution to an autoclave with a volume of 2L, heat to 180°C and keep it warm 2 hours; the reactor was cooled to room temperature, filtered and washed with ethanol for 3 times, and then dried at 80°C for 6 hours to obtain graphene-ethylene glycol bismuth powder;
2)取4g钼酸钠溶于200ml去离子水中，再将1)中制备石墨烯-乙二醇铋粉末10g加入上述钼酸钠水溶液中，超声波震荡搅拌使其分散均匀，用浓硝酸和浓盐酸调节溶液pH值至0-3之间，然后将所得混合液转移至容积为500mL的高压釜中，升温至150℃保温24小时，待反应釜冷却至室温，过滤后用去离子水和乙醇洗涤2次，再在80℃下干燥12小时，得石墨烯-钼酸铋钠纳米复合材料。2) Take 4g of sodium molybdate and dissolve it in 200ml of deionized water, then add 10g of the graphene-ethylene glycol bismuth powder prepared in 1) into the above sodium molybdate aqueous solution, stir with ultrasonic vibration to disperse evenly, and use concentrated nitric acid and concentrated Adjust the pH value of the solution to 0-3 with hydrochloric acid, then transfer the resulting mixture to an autoclave with a volume of 500mL, raise the temperature to 150°C and keep it warm for 24 hours. Wash twice, and then dry at 80° C. for 12 hours to obtain a graphene-sodium bismuth molybdate nanocomposite material.
本实施例所得产物γ-钼酸铋纳米晶片平均厚度为12nm，比表面积为55m2/g，在浓度1.0g/L时，可见光照射下能在30min内完全降解0.02g/L罗丹明。The product obtained in this example γ-bismuth molybdate nanochips has an average thickness of 12nm and a specific surface area of 55m 2 /g. When the concentration is 1.0g/L, 0.02g/L rhodamine can be completely degraded within 30min under visible light irradiation.
实施例3Example 3
石墨烯-γ-钼酸铋纳米复合材料的制备方法，包括以下步骤：The preparation method of graphene-γ-bismuth molybdate nanocomposite material comprises the following steps:
1)将50g硝酸铋溶于1L乙二醇中，然后加入2g石墨烯粉搅拌混合均匀，得到稳定悬浊液，将此溶液转移到容积为2L的高压釜中，加热至170℃并保温12小时；待反应釜冷却至室温，过滤并用乙醇洗涤3次，然后在100℃下干燥4小时，得石墨烯-乙二醇铋粉体；1) Dissolve 50g of bismuth nitrate in 1L of ethylene glycol, then add 2g of graphene powder and mix evenly to obtain a stable suspension. Transfer this solution to an autoclave with a volume of 2L, heat to 170°C and keep it warm for 12 Hours; the reactor was cooled to room temperature, filtered and washed 3 times with ethanol, then dried at 100°C for 4 hours to obtain graphene-ethylene glycol bismuth powder;
2)取3.5g钼酸钠溶于100ml去离子水中，再将1)中制备石墨烯-乙二醇铋粉末10g加入上述钼酸钠水溶液中，超声波震荡搅拌使其分散均匀，用浓硝酸和浓盐酸调节溶液pH值至0-3之间，然后将所得混合液转移至容积为200mL的高压釜中，升温至180℃保温12小时，待反应釜冷却至室温，过滤后用去离子水和乙醇洗涤3次，再在100℃下干燥12小时，得石墨烯-钼酸铋钠纳米复合材料。2) Take 3.5g of sodium molybdate and dissolve it in 100ml of deionized water, then add 10g of the graphene-ethylene glycol bismuth powder prepared in 1) into the above aqueous solution of sodium molybdate, stir with ultrasonic vibration to disperse evenly, and use concentrated nitric acid and Concentrated hydrochloric acid to adjust the pH value of the solution to between 0-3, then transfer the resulting mixed solution to an autoclave with a volume of 200mL, raise the temperature to 180°C and keep it for 12 hours, wait for the reaction kettle to cool to room temperature, filter it with deionized water and Washed with ethanol for 3 times, and then dried at 100° C. for 12 hours to obtain a graphene-sodium bismuth molybdate nanocomposite material.
本实施例所得产物γ-钼酸铋纳米晶片平均厚度为20nm，比表面积为40m2/g，在浓度1.0g/L时，可见光照射下能在30min内完全降解0.02g/L罗丹明。The γ-bismuth molybdate nanochips obtained in this example have an average thickness of 20nm and a specific surface area of 40m 2 /g. When the concentration is 1.0g/L, 0.02g/L rhodamine can be completely degraded within 30min under visible light irradiation.
实施例4Example 4
石墨烯-γ-钼酸铋纳米复合材料的制备方法，包括以下步骤：The preparation method of graphene-γ-bismuth molybdate nanocomposite material comprises the following steps:
1)将10g硝酸铋溶于1L乙二醇中，然后加入0.5g石墨烯粉搅拌混合均匀，得到稳定悬浊液，将此溶液转移到容积为2L的高压釜中，加热至160℃并保温24小时；待反应釜冷却至室温，过滤并用乙醇洗涤3次，然后在100℃下干燥4小时，得石墨烯-乙二醇铋粉体；1) Dissolve 10g of bismuth nitrate in 1L of ethylene glycol, then add 0.5g of graphene powder and mix evenly to obtain a stable suspension. Transfer this solution to an autoclave with a volume of 2L, heat to 160°C and keep it warm 24 hours; after the reactor is cooled to room temperature, filter and wash with ethanol for 3 times, and then dry at 100°C for 4 hours to obtain graphene-bismuth ethylene glycol powder;
2)取2.5g钼酸钠溶于100ml去离子水中，再将1)中制备石墨烯-乙二醇铋粉末5g加入上述钼酸钠水溶液中，超声波震荡搅拌使其分散均匀，用浓硝酸和浓盐酸调节溶液pH值至0-3之间，然后将所得混合液转移至容积为200mL的高压釜中，升温至200℃保温24小时，待反应釜冷却至室温，过滤后用去离子水和乙醇洗涤3次，再在100℃下干燥12小时，得石墨烯-钼酸铋钠纳米复合材料。2) Take 2.5g of sodium molybdate and dissolve it in 100ml of deionized water, then add 5g of the graphene-ethylene glycol bismuth powder prepared in 1) into the above aqueous solution of sodium molybdate, stir with ultrasonic vibration to disperse evenly, and use concentrated nitric acid and Concentrated hydrochloric acid to adjust the pH value of the solution to between 0-3, then transfer the resulting mixture to a 200mL autoclave, raise the temperature to 200°C and keep it warm for 24 hours. After the reaction kettle is cooled to room temperature, filter it with deionized water and Washed with ethanol for 3 times, and then dried at 100° C. for 12 hours to obtain a graphene-sodium bismuth molybdate nanocomposite material.
本实施例所得产物γ-钼酸铋纳米晶片平均厚度为40nm，比表面积为30m2/g，在浓度1.0g/L时，可见光照射下能在60min内完全降解0.02g/L罗丹明。The γ-bismuth molybdate nanochips obtained in this example have an average thickness of 40nm and a specific surface area of 30m 2 /g. When the concentration is 1.0g/L, 0.02g/L rhodamine can be completely degraded within 60min under visible light irradiation.
本发明所列举的各原料配比都能实现本发明，以及各原料的上下限取值、区间值都能实现本发明，本发明的工艺参数的上下限取值以及区间值都能实现本发明，在此不一一列举实施例。The ratio of each raw material listed in the present invention can realize the present invention, and the upper and lower limits and interval values of each raw material can realize the present invention, and the upper and lower limits and interval values of the process parameters of the present invention can realize the present invention , not enumerating the examples one by one here.
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