CN103028387A - Preparation method of graphene/titanium dioxide photocatalyst - Google Patents
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 28
- 239000011941 photocatalyst Substances 0.000 title abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 32
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims description 5
- 230000003287 optical effect Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
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- 230000001699 photocatalysis Effects 0.000 description 13
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- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 239000007772 electrode material Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
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- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明公开了一种石墨烯/二氧化钛光催化剂的制备方法，步骤如下：（1）配制溶液A：将钛酸四丁酯慢慢加入氯仿中，得到溶液A；（2）配制混合液B：将氧化石墨烯加入到去离子水和乙醇的混合溶液中，得到混合液B；（3）将混合液B边搅拌边滴加到溶液A中，搅拌均匀，得混合液；（4）将混合液装入水热釜中，水热后，自然冷却至室温后，分离洗涤，即得到石墨烯/二氧化钛光催化剂。采用该方法所制备的石墨烯/二氧化钛光催化剂对有机染料具有优异的光催化降解性能。
The invention discloses a preparation method of graphene/titanium dioxide photocatalyst. The steps are as follows: (1) preparing solution A: slowly adding tetrabutyl titanate into chloroform to obtain solution A; (2) preparing mixed solution B: Add graphene oxide into the mixed solution of deionized water and ethanol to obtain mixed solution B; (3) add mixed solution B dropwise to solution A while stirring, and stir evenly to obtain mixed solution; (4) mix The liquid is put into a hydrothermal kettle, after being hydrothermally cooled to room temperature naturally, separated and washed to obtain a graphene/titanium dioxide photocatalyst. The graphene/titanium dioxide photocatalyst prepared by the method has excellent photocatalytic degradation performance for organic dyes.
Description
技术领域 technical field
本发明涉及光催化功能材料无机合成技术领域，尤其是涉及一种石墨烯/二氧化钛光催化剂的制备方法。 The invention relates to the technical field of inorganic synthesis of photocatalytic functional materials, in particular to a method for preparing a graphene/titanium dioxide photocatalyst.
背景技术 Background technique
石墨烯由于其优异的光、电性能，已经受到了科研人员的广泛关注。它可以作为性能增强相与其它纳米半导体材料进行复合，制备出性能优异的的复合材料。通过将石墨烯与半导体纳米材料复合，当材料被光照射时，光生电子可以从半导体颗粒转移到石墨烯中，有效阻止光生电子和空穴的复合，提高光生电子和空穴的寿命，从而提高光催化效率，显著提高光催化材料的性能。这种复合材料在太阳能、锂电池电极材料和污水处理等领域有着潜在的应用。 Graphene has attracted extensive attention of researchers due to its excellent optical and electrical properties. It can be used as a performance-enhancing phase to compound with other nano-semiconductor materials to prepare composite materials with excellent performance. By combining graphene with semiconductor nanomaterials, when the material is irradiated by light, photogenerated electrons can be transferred from semiconductor particles to graphene, effectively preventing the recombination of photogenerated electrons and holes, improving the lifetime of photogenerated electrons and holes, thereby improving Photocatalytic efficiency, significantly improving the performance of photocatalytic materials. This composite material has potential applications in fields such as solar energy, lithium battery electrode materials and sewage treatment.
二氧化钛是一种半导体材料，由于其无毒、成本低等优点，作为光催化剂被广泛用于污水处理等领域。将二氧化钛和石墨烯复合将提高二氧化钛的光催化性能，得到性能优异的光催化材料。 Titanium dioxide is a semiconductor material, which is widely used as a photocatalyst in sewage treatment and other fields due to its advantages of non-toxicity and low cost. Combining titanium dioxide and graphene will improve the photocatalytic performance of titanium dioxide and obtain a photocatalytic material with excellent performance.
目前所报导的制备方法，有水热、溶剂热、化学沉积等方法。制备过程中采用肼等方法将氧化石墨烯还原，然后再与二氧化钛复合。虽然氧化石墨烯在水溶液中具有很好的分散性，但是在复合材料制备过程中，当氧化石墨烯被还原为石墨烯后，由于石墨烯具有很强的憎水性，导致所得石墨烯/二氧化钛光催化剂团聚严重，不易分散。 Currently reported preparation methods include methods such as hydrothermal, solvothermal, and chemical deposition. During the preparation process, graphene oxide is reduced by hydrazine and other methods, and then compounded with titanium dioxide. Although graphene oxide has good dispersibility in aqueous solution, when graphene oxide is reduced to graphene in the preparation process of composite materials, due to the strong hydrophobicity of graphene, the obtained graphene/titania light The catalyst agglomerates seriously and is not easy to disperse.
发明内容 Contents of the invention
本发明要解决的技术问题是提供一种石墨烯/二氧化钛光催化剂的制备方法。采用该方法所制备的石墨烯/二氧化钛光催化剂对有机染料具有优异的光催化降解性能，可以广泛应用于污水处理等环保领域。 The technical problem to be solved by the present invention is to provide a preparation method of graphene/titanium dioxide photocatalyst. The graphene/titanium dioxide photocatalyst prepared by the method has excellent photocatalytic degradation performance for organic dyes, and can be widely used in environmental protection fields such as sewage treatment.
一种石墨烯/二氧化钛光催化剂的制备方法，步骤如下： A preparation method of graphene/titanium dioxide photocatalyst, the steps are as follows:
（1）配制溶液A：将钛酸四丁酯慢慢加入氯仿中，得到溶液A； (1) Prepare solution A: slowly add tetrabutyl titanate into chloroform to obtain solution A;
（2）配制混合液B：将氧化石墨烯加入到去离子水和乙醇的混合溶液中，得到混合液B； (2) Prepare mixed solution B: add graphene oxide into the mixed solution of deionized water and ethanol to obtain mixed solution B;
（3）将混合液B边搅拌边滴加到溶液A中，搅拌均匀，得混合液； (3) Add the mixed solution B dropwise to the solution A while stirring, and stir evenly to obtain the mixed solution;
（4）将混合液装入水热釜中，水热后，自然冷却至室温后，分离洗涤，即得到石墨烯/二氧化钛光催化剂。 (4) Put the mixed liquid into a hydrothermal kettle, after hydroheating, cool to room temperature naturally, separate and wash, and obtain the graphene/titanium dioxide photocatalyst.
前面所述的制备方法，优选的方案是，步骤（1）配制的溶液A为钛酸四丁酯浓度为0.8-4.5g/L的溶液。 In the above-mentioned preparation method, the preferred solution is that the solution A prepared in step (1) is a solution with a tetrabutyl titanate concentration of 0.8-4.5 g/L.
前面所述的制备方法，优选的方案是，步骤（2）配制混合液B时所用氧化石墨烯为用Hummers法制备的氧化石墨烯。 In the above-mentioned preparation method, the preferred solution is that the graphene oxide used in step (2) when preparing the mixed solution B is the graphene oxide prepared by the Hummers method.
前面所述的制备方法，优选的方案是，步骤（2）配制的混合液B为氧化石墨烯浓度为0.02-1.0 g/L的混合液。 In the above-mentioned preparation method, the preferred solution is that the mixed solution B prepared in step (2) is a mixed solution with a graphene oxide concentration of 0.02-1.0 g/L.
前面所述的制备方法，优选的方案是，步骤（3）溶液A与混合液B的用量是等体积。 In the above-mentioned preparation method, the preferred solution is that the volumes of solution A and mixed solution B used in step (3) are equal.
前面所述的制备方法，优选的方案是，步骤（4）水热温度为160-200℃。 In the aforementioned preparation method, the preferred solution is that the hydrothermal temperature in step (4) is 160-200°C.
前面所述的制备方法，优选的方案是，步骤（4）水热时间为5-20小时。 In the aforementioned preparation method, the preferred solution is that the hydrothermal time in step (4) is 5-20 hours.
本发明提供的是一种石墨烯/二氧化钛光催化剂的制备方法，包括如下步骤：(1)配制溶液A，将钛酸四丁酯慢慢加入氯仿中，得到钛酸四丁酯浓度为0.8-4.5g/L的溶液；配制混合液B，将适量用Hummers法制备的氧化石墨烯加入到去离子水和乙醇的混合溶液中，得到氧化石墨烯浓度为0.02-1.0 g/L的混合液。将一定体积的混合液B边搅拌边滴加到等体积的溶液A中，搅拌均匀。(2)最后，将所得混合液装入水热釜中，在160-200℃下水热5-20小时。自然冷却至室温后，分离洗涤，即得具有优异光催化性能的石墨烯/二氧化钛光催化剂。本发明所述方法通过产物在水和氯仿间的转移，可以有效防止光催化剂的团聚，大幅提高光催化剂的比表面积和光催化性能。 What the present invention provides is a kind of preparation method of graphene/titanium dioxide photocatalyst, comprises the following steps: (1) prepare solution A, slowly add tetrabutyl titanate in chloroform, obtain tetrabutyl titanate concentration and be 0.8- 4.5g/L solution; prepare mixed solution B, add an appropriate amount of graphene oxide prepared by the Hummers method into a mixed solution of deionized water and ethanol to obtain a mixed solution with a graphene oxide concentration of 0.02-1.0 g/L. Add a certain volume of mixed solution B dropwise to an equal volume of solution A while stirring, and stir evenly. (2) Finally, put the obtained mixed solution into a hydrothermal tank, and heat it at 160-200° C. for 5-20 hours. After natural cooling to room temperature, separation and washing, a graphene/titanium dioxide photocatalyst with excellent photocatalytic performance is obtained. The method of the invention can effectively prevent the agglomeration of the photocatalyst through the transfer of the product between water and chloroform, and greatly improve the specific surface area and photocatalytic performance of the photocatalyst.
本发明采用了一种水和氯仿两相水热法制备出了分散性好的石墨烯/二氧化钛光催化材料。该方法中，在氧化石墨烯被水热之前，可以很好地分散在水中，与分散氯仿中的钛酸四丁酯在两相界面上进行反应；当氧化石墨烯被水热为石墨烯后，生成的憎水性的石墨烯/二氧化钛复合材料将从水中转移到氯仿中，从而避免了在单一水相中的团聚情况，从而提高了光催化剂的比表面积和性能。采用该方法所制备的石墨烯/二氧化钛光催化剂对有机染料具有优异的光催化降解性能。 The invention adopts a two-phase hydrothermal method of water and chloroform to prepare the graphene/titanium dioxide photocatalytic material with good dispersibility. In this method, before graphene oxide is hydroheated, it can be well dispersed in water and react with tetrabutyl titanate in dispersed chloroform on the two-phase interface; when graphene oxide is hydrothermally converted into graphene , the resulting hydrophobic graphene/titania composite material will be transferred from water to chloroform, thereby avoiding the agglomeration situation in a single aqueous phase, thereby improving the specific surface area and performance of the photocatalyst. The graphene/titanium dioxide photocatalyst prepared by the method has excellent photocatalytic degradation performance for organic dyes.
本发明具有如下有益效果： The present invention has following beneficial effects:
(1)过程简单，易于实施，可以减少引入杂质的机会，从而不会影响产品的纯度。 (1) The process is simple and easy to implement, which can reduce the chance of introducing impurities, thereby not affecting the purity of the product.
(2)制备过程温和，不需要特殊气氛保护，所需设备简单，反应速度快，适于规模生产。 (2) The preparation process is mild, no special atmosphere protection is required, the required equipment is simple, the reaction speed is fast, and it is suitable for large-scale production.
(3) 避免了复合材料的团聚，使所得石墨烯/二氧化钛光催化剂具有优异的光催化降解性能，可以广泛应用于污水处理等环保领域。 (3) The agglomeration of composite materials is avoided, so that the obtained graphene/titanium dioxide photocatalyst has excellent photocatalytic degradation performance, and can be widely used in environmental protection fields such as sewage treatment.
附图说明 Description of drawings
图1是实例1所制备的石墨烯/二氧化钛光催化剂的透射电子显微镜照片； Fig. 1 is the transmission electron micrograph of the prepared graphene/titania photocatalyst of example 1;
图2是实例1所制备的石墨烯/二氧化钛光催化剂，在紫外照射下对甲基橙的光催化效果图。 Fig. 2 is the graphene/titanium dioxide photocatalyst prepared in Example 1, the photocatalytic effect figure to methyl orange under ultraviolet irradiation.
具体实施方式 Detailed ways
为了显示本发明的实质性特点和显著进步，用下列非限定性实施例进一步说明实施方式及效果。 In order to show the substantive characteristics and remarkable progress of the present invention, the following non-limiting examples are used to further illustrate the implementation and effects.
实施例1Example 1
一种石墨烯/二氧化钛光催化剂的制备方法，包括如下步骤： A kind of preparation method of graphene/titanium dioxide photocatalyst, comprises the steps:
(1)配制溶液A，将0.07 g钛酸四丁酯慢慢加入到40 mL氯仿中，浓度为1.75 g/L；配制溶液B，将0.024 g用Hummers法制备的氧化石墨烯加入到40 mL去离子水和乙醇的混合液中，氧化石墨烯的浓度为0.6 g/L。将所得到的混合溶液B边搅拌边滴加到溶液A中，搅拌均匀，得到A和B的混合溶液。 (1) To prepare solution A, slowly add 0.07 g of tetrabutyl titanate to 40 mL of chloroform at a concentration of 1.75 g/L; to prepare solution B, add 0.024 g of graphene oxide prepared by the Hummers method to 40 mL In the mixture of deionized water and ethanol, the concentration of graphene oxide was 0.6 g/L. The obtained mixed solution B was added dropwise into the solution A while stirring, and stirred evenly to obtain a mixed solution of A and B.
(2)将A和B的混合溶液装入水热釜中，在180℃下保温12小时；自然冷却至室温后，分离洗涤即得具有优异光催化性能的石墨烯/二氧化钛光催化剂。 (2) Put the mixed solution of A and B into a hydrothermal kettle and keep it warm at 180°C for 12 hours; after natural cooling to room temperature, separate and wash to obtain a graphene/titanium dioxide photocatalyst with excellent photocatalytic performance.
经透射电子显微镜分析可以看出二氧化钛纳米颗粒分散在石墨烯片层上，如图1所示。图2给出了实例1所制备复合材料在紫外光照射下的催化剂对甲基橙的催化效果图。结果表明，紫外光照射下40分钟可以将浓度为20 mg/L的甲基橙溶液完全降解，说明所得催化剂具有优异的光催化性能。 It can be seen from transmission electron microscope analysis that titanium dioxide nanoparticles are dispersed on graphene sheets, as shown in Figure 1. Fig. 2 shows the catalytic effect diagram of the catalyst of the composite material prepared in Example 1 on methyl orange under the irradiation of ultraviolet light. The results show that the methyl orange solution with a concentration of 20 mg/L can be completely degraded under ultraviolet light irradiation for 40 minutes, indicating that the obtained catalyst has excellent photocatalytic performance.
实施例2Example 2
一种石墨烯/二氧化钛光催化剂的制备方法，包括如下步骤： A kind of preparation method of graphene/titanium dioxide photocatalyst, comprises the steps:
(1)配制溶液A，将0.17 g钛酸四丁酯慢慢加入到40 mL氯仿中，浓度为4.2 g/L；配制混合液B，将0.008 g用Hummers法制备的氧化石墨烯加入到40 mL去离子水和乙醇的混合液中，氧化石墨烯的浓度为0.02 g/L。将混合液B边搅拌边滴加到溶液A中，继续搅拌混合均匀，得到A和B的混合溶液。 (1) Prepare solution A, slowly add 0.17 g tetrabutyl titanate into 40 mL chloroform, the concentration is 4.2 g/L; prepare mixed solution B, add 0.008 g graphene oxide prepared by Hummers method to 40 mL In the mixed solution of deionized water and ethanol, the concentration of graphene oxide was 0.02 g/L. Add the mixed solution B dropwise to the solution A while stirring, and continue to stir and mix evenly to obtain a mixed solution of A and B.
(2)将A和B的混合溶液装入水热釜中，在160℃下保温20小时；自然冷却至室温后，分离洗涤即得具有优异光催化性能的石墨烯/二氧化钛光催化剂。 (2) Put the mixed solution of A and B into a hydrothermal kettle and keep it warm at 160°C for 20 hours; after natural cooling to room temperature, separate and wash to obtain a graphene/titanium dioxide photocatalyst with excellent photocatalytic performance.
实施例3Example 3
一种石墨烯/二氧化钛光催化剂的制备方法，包括如下步骤： A kind of preparation method of graphene/titanium dioxide photocatalyst, comprises the steps:
(1)配制溶液A，将0.034 g钛酸四丁酯慢慢加入到40 mL氯仿中，浓度为0.85 g/L；配制混合液B，将0.032 g用Hummers法制备的氧化石墨烯加入到40 mL去离子水和乙醇的混合液中，氧化石墨烯的浓度为0.8 g/L。将所得到的混合溶液B边搅拌边滴加到溶液A中，搅拌均匀，得到A和B的混合溶液。 (1) Prepare solution A, slowly add 0.034 g tetrabutyl titanate into 40 mL chloroform, the concentration is 0.85 g/L; prepare mixed solution B, add 0.032 g graphene oxide prepared by Hummers method to 40 mL In the mixed solution of deionized water and ethanol, the concentration of graphene oxide was 0.8 g/L. The obtained mixed solution B was added dropwise into the solution A while stirring, and stirred evenly to obtain a mixed solution of A and B.
(2)将A和B的混合溶液装入水热釜中，在200℃下保温5小时；自然冷却至室温后，分离洗涤即得具有优异光催化性能的石墨烯/二氧化钛光催化剂。 (2) Put the mixed solution of A and B into a hydrothermal kettle and keep it warm at 200°C for 5 hours; after natural cooling to room temperature, separate and wash to obtain a graphene/titanium dioxide photocatalyst with excellent photocatalytic performance.
the
显然，本发明的上述实施例仅为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述举例的基础上还可以做其他不同形式的变化或变动。这里无法对所有的实施方式予以穷举。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。 Apparently, the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, rather than limiting the implementation of the present invention. For those of ordinary skill in the art, on the basis of the above examples, other changes or changes in different forms can also be made. All the implementation manners cannot be exhaustively listed here. All obvious changes or changes derived from the technical solutions of the present invention are still within the protection scope of the present invention.
该专利申请受到国家自然科学基金项目（51002069）的资金资助。 This patent application is funded by the National Natural Science Foundation of China (51002069).
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