CN107899560A - 石墨烯‑二氧化钛复合光催化剂的制备方法 - Google Patents
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Abstract
本发明公开一种石墨烯‑二氧化钛复合光催化剂的制备方法,包括以下步骤:(1)将石墨粉和NaNO3混合,微波反应,自然冷却至室温;(2)在冰水浴状态下,将步骤(1)得到的混合物加入到浓硫酸中,搅拌混合,然后加入KMnO4;(3)将步骤(2)的体系置于油浴中,然后加入过氧化氢溶液至体系无气泡产生,洗涤沉淀,真空干燥,得到氧化石墨;(4)将氧化石墨加入乙醇和水的混合溶液中,超声;(5)加入二氧化钛,搅拌反应,150℃下反应,自然冷却至室温,过滤,洗涤沉淀,然后真空干燥,即得到石墨烯‑二氧化钛复合光催化剂。本发明通过水热法制备得到了石墨烯‑二氧化钛复合光催化剂,光催化剂的产氢活性高。
Description
技术领域
本发明属于催化剂制备技术领域,具体涉及一种石墨烯-二氧化钛复合光催化剂的制备方法。
背景技术
TiO2作为一种重要的无机半导体材料,在能源和环境方面的快速发展和广泛应用,吸引了越来越多研究者的关注,由于其廉价,化学性质稳定,无毒等特点而成为广泛研究的光催化剂,但是由于其较大的能带隙(3.2eV),只能对紫外光有响应,同时光生电子一空穴对容易复合,光量子效率低,极大地限制了在实际中的应用范围,为此研究者们进行了各种尝试对其进行改性,如离子掺杂、贵金属沉积、半导体复合等。
近年来,石墨烯的发现及应用为TiO2的改性创造了条件,研究者利用其优异的电子传输性能,将其引入到光催化领域,制备出石墨烯/ TiO2复合材料,提高TiO2的光催化量子效率。
氢能源是一种理想的清洁能源,自1972年Fujishima等人发现光解水制氢以来,一直被认为是最有发展前景的方法。李越湘等制备出Pt负载TiO2光催化剂,以甲醛为电子给体提高了光催化制氢的活性,张晓艳等制备出TiO2/石墨烯复合材料,发现石墨烯的引入有效提高了光的利用率。但是,目前光催化制氢的活性依然较低。
发明内容
针对现有技术的缺陷,本发明提供一种石墨烯-二氧化钛复合光催化剂的制备方法。
石墨烯-二氧化钛复合光催化剂的制备方法,包括以下步骤:
(1)将石墨粉和NaNO3混合,在功率100-200W下微波反应20-30min,自然冷却至室温;
(2)在冰水浴状态下,将步骤(1)得到的混合物加入到浓硫酸中,搅拌混合,然后加入KMnO4,在3000r/min的状态下搅拌20min;
(3)将步骤(2)的体系置于35℃的油浴中反应30-50min,然后加入质量浓度为30%的过氧化氢溶液至体系无气泡产生,将沉淀洗涤至滤液的pH为7,然后真空干燥,得到氧化石墨;
(4)按照料液比1g:8mL将步骤(3)得到的氧化石墨加入乙醇和水的混合溶液中,超声反应1h;
(5)加入二氧化钛,搅拌反应30min,然后在150℃下反应5h,自然冷却至室温,过滤,沉淀用去离子水洗涤3次,然后在60℃下真空干燥5h,即得到石墨烯-二氧化钛复合光催化剂。
优选地,步骤(1)和步骤(2)中,石墨粉、NaNO3、浓硫酸、KMnO4的添加比例为1g:1g:23mL:3g。
优选地,步骤(3)中真空干燥的条件为在50℃下干燥3-4h。
优选地,步骤(4)中乙醇和水的混合溶液中乙醇和水的体积比为1:2。
优选地,步骤(4)中超声反应的条件为:先在100W的功率下超声反应20min,然后在200W的功率下超声反应40min。
本发明的优点:
本发明通过水热法制备得到了石墨烯-二氧化钛复合光催化剂,在水热过程中,石墨被还原成石墨烯,二氧化钛颗粒通过化学键负载在石墨烯上,有效提高了光催化分解C2H5OH和H2O溶液的产氢活性,石墨烯做为一种良好的电子导体,太阳光照射下,能快速把光生电子转移,有效抑制电子和空穴对的复合,从而提高光催化剂的产氢活性。
具体实施方式
实施例1
石墨烯-二氧化钛复合光催化剂的制备方法,包括以下步骤:
(1)将石墨粉和NaNO3混合,在功率100W下微波反应20min,自然冷却至室温;
(2)在冰水浴状态下,将步骤(1)得到的混合物加入到浓硫酸中,搅拌混合,然后加入KMnO4,在3000r/min的状态下搅拌20min,其中,步骤(1)和步骤(2)中,石墨粉、NaNO3、浓硫酸、KMnO4的添加比例为1g:1g:23mL:3g;
(3)将步骤(2)的体系置于35℃的油浴中反应30min,然后加入质量浓度为30%的过氧化氢溶液至体系无气泡产生,将沉淀洗涤至滤液的pH为7,然后在50℃下干燥3h,得到氧化石墨;
(4)按照料液比1g:8mL将步骤(3)得到的氧化石墨加入乙醇和水的混合溶液中,乙醇和水的混合溶液中乙醇和水的体积比为1:2,超声反应1h,超声反应具体为:先在100W的功率下超声反应20min,然后在200W的功率下超声反应40min;
(5)加入二氧化钛,搅拌反应30min,然后在150℃下反应5h,自然冷却至室温,过滤,沉淀用去离子水洗涤3次,然后在60℃下真空干燥5h,即得到石墨烯-二氧化钛复合光催化剂。
实施例2
石墨烯-二氧化钛复合光催化剂的制备方法,包括以下步骤:
(1)将石墨粉和NaNO3混合,在功率200W下微波反应30min,自然冷却至室温;
(2)在冰水浴状态下,将步骤(1)得到的混合物加入到浓硫酸中,搅拌混合,然后加入KMnO4,在3000r/min的状态下搅拌20min,其中,步骤(1)和步骤(2)中,石墨粉、NaNO3、浓硫酸、KMnO4的添加比例为1g:1g:23mL:3g;
(3)将步骤(2)的体系置于35℃的油浴中反应50min,然后加入质量浓度为30%的过氧化氢溶液至体系无气泡产生,将沉淀洗涤至滤液的pH为7,然后在50℃下干燥4h,得到氧化石墨;
(4)按照料液比1g:8mL将步骤(3)得到的氧化石墨加入乙醇和水的混合溶液中,乙醇和水的混合溶液中乙醇和水的体积比为1:2,超声反应1h,超声反应具体为:先在100W的功率下超声反应20min,然后在200W的功率下超声反应40min;
(5)加入二氧化钛,搅拌反应30min,然后在150℃下反应5h,自然冷却至室温,过滤,沉淀用去离子水洗涤3次,然后在60℃下真空干燥5h,即得到石墨烯-二氧化钛复合光催化剂。
实施例3
石墨烯-二氧化钛复合光催化剂的制备方法,包括以下步骤:
(1)将石墨粉和NaNO3混合,在功率100W下微波反应30min,自然冷却至室温;
(2)在冰水浴状态下,将步骤(1)得到的混合物加入到浓硫酸中,搅拌混合,然后加入KMnO4,在3000r/min的状态下搅拌20min,其中,步骤(1)和步骤(2)中,石墨粉、NaNO3、浓硫酸、KMnO4的添加比例为1g:1g:23mL:3g;
(3)将步骤(2)的体系置于35℃的油浴中反应40min,然后加入质量浓度为30%的过氧化氢溶液至体系无气泡产生,将沉淀洗涤至滤液的pH为7,然后在50℃下干燥3.5h,得到氧化石墨;
(4)按照料液比1g:8mL将步骤(3)得到的氧化石墨加入乙醇和水的混合溶液中,乙醇和水的混合溶液中乙醇和水的体积比为1:2,超声反应1h,超声反应具体为:先在100W的功率下超声反应20min,然后在200W的功率下超声反应40min;
(5)加入二氧化钛,搅拌反应30min,然后在150℃下反应5h,自然冷却至室温,过滤,沉淀用去离子水洗涤3次,然后在60℃下真空干燥5h,即得到石墨烯-二氧化钛复合光催化剂。
Claims (5)
1.石墨烯-二氧化钛复合光催化剂的制备方法,其特征在于:包括以下步骤:
(1)将石墨粉和NaNO3混合,在功率100-200W下微波反应20-30min,自然冷却至室温;
(2)在冰水浴状态下,将步骤(1)得到的混合物加入到浓硫酸中,搅拌混合,然后加入KMnO4,在3000r/min的状态下搅拌20min;
(3)将步骤(2)的体系置于35℃的油浴中反应30-50min,然后加入质量浓度为30%的过氧化氢溶液至体系无气泡产生,将沉淀洗涤至滤液的pH为7,然后真空干燥,得到氧化石墨;
(4)按照料液比1g:8mL将步骤(3)得到的氧化石墨加入乙醇和水的混合溶液中,超声反应1h;
(5)加入二氧化钛,搅拌反应30min,然后在150℃下反应5h,自然冷却至室温,过滤,沉淀用去离子水洗涤3次,然后在60℃下真空干燥5h,即得到石墨烯-二氧化钛复合光催化剂。
2.根据权利要求1所述的石墨烯-二氧化钛复合光催化剂的制备方法,其特征在于:步骤(1)和步骤(2)中,石墨粉、NaNO3、浓硫酸、KMnO4的添加比例为1g:1g:23mL:3g。
3.根据权利要求1所述的石墨烯-二氧化钛复合光催化剂的制备方法,其特征在于:步骤(3)中真空干燥的条件为在50℃下干燥3-4h。
4.根据权利要求1所述的石墨烯-二氧化钛复合光催化剂的制备方法,其特征在于:步骤(4)中乙醇和水的混合溶液中乙醇和水的体积比为1:2。
5.根据权利要求1所述的石墨烯-二氧化钛复合光催化剂的制备方法,其特征在于:步骤(4)中超声反应的条件为:先在100W的功率下超声反应20min,然后在200W的功率下超声反应40min。
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CN110511509A (zh) * | 2019-09-03 | 2019-11-29 | 海南师范大学 | 一种可光催化降解的聚氯乙烯塑料薄膜及其制备方法 |
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CN110511509A (zh) * | 2019-09-03 | 2019-11-29 | 海南师范大学 | 一种可光催化降解的聚氯乙烯塑料薄膜及其制备方法 |
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