WO2019051745A1 - 一种制备表面改性碳量子点-二氧化钛复合光催化剂方法 - Google Patents

一种制备表面改性碳量子点-二氧化钛复合光催化剂方法 Download PDF

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WO2019051745A1
WO2019051745A1 PCT/CN2017/101809 CN2017101809W WO2019051745A1 WO 2019051745 A1 WO2019051745 A1 WO 2019051745A1 CN 2017101809 W CN2017101809 W CN 2017101809W WO 2019051745 A1 WO2019051745 A1 WO 2019051745A1
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quantum dot
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谢秋生
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谢秋生
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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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon

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  • the invention relates to a method for preparing a surface modified carbon quantum dot-titanium dioxide composite photocatalyst.
  • titanium dioxide photocatalytic materials Since the discovery of titanium dioxide to decompose water into oxygen and hydrogen under visible light irradiation, titanium dioxide photocatalytic materials have received continuous and extensive attention.
  • the main methods for preparing the titanium dioxide photocatalyst include a sol-gel method, a hydrothermal method, a precipitation method, a dipping method, a microemulsion method, a meteorological hydrolysis method, a supergravity method, and the like.
  • the raw materials for preparing TiO 2 by hydrothermal method are mostly tetrabutyl titanate and TiCl 4 , and the research on hydrothermal synthesis using titanium sulfate is relatively rare. Titanium sulphate is weaker than liquid titanium salt, which is easier and more convenient to operate, and has a wide range of applications in industry.
  • Carbon quantum dots are a class of zero-dimensional carbon nanomaterials with a good fluorescence performance of less than 10 nm. When the single-walled carbon nanotubes were purified by electrophoresis in 2004, the particle size was only 1 to 10 nm. The large specific surface area, the surface modification by organic matter, makes the carbon quantum dots more stable, and the carbon quantum dots have up-conversion luminescence properties and semiconductor properties, and have important applications in the field of photocatalysis.
  • a method for preparing a surface-modified carbon quantum dot-titanium dioxide composite photocatalyst comprises the following steps: adding 20-30 parts of ethylene glycol to a reaction kettle, heating in an oven at 170-190 ° C for 3-5 hours, and taking it after centrifugation The supernatant is added with 0.5-1.5 parts of ammonia water, mixed uniformly, and incubated at 100-110 ° C for 2-4 h. After cooling, the supernatant is centrifuged to obtain a modified carbon quantum dot solution; 5-7 parts of Ti(SO 4 ) 2 Add 40-50 parts of deionized water, adjust to pH 1.5-2.5 with concentrated hydrochloric acid, seal, and then heat in the oven at 180-190 °C for 11-13h.
  • the method is placed in an oven and heated at 180 ° C for 4 h.
  • the temperature is maintained at 105 ° C for 3 h.
  • the pH is adjusted to 2 with concentrated hydrochloric acid.
  • the method is heated in an oven at 185 ° C for 12 h.
  • the precipitate is dried under vacuum at 42 °C.
  • the magnetic stirring is carried out for 3 h, and then it is transferred to a blast drying oven and dried at 75 ° C for 4 h.
  • the method provided by the invention is simple and easy to operate, and a composite photocatalyst excellent in catalytic effect can be obtained.
  • a method for preparing a surface-modified carbon quantum dot-titanium dioxide composite photocatalyst comprises the steps of: adding 25 parts of ethylene glycol to a reaction kettle, heating in an oven at 180 ° C for 4 hours, and taking the supernatant after centrifugation, adding 1 A portion of ammonia water, mixed evenly, kept at 105 ° C for 3h, cooled, centrifuged to remove the supernatant to obtain a modified carbon quantum dot solution; 6 parts of Ti (SO 4 ) 2 was added to 45 parts of deionized water, adjusted to pH with concentrated hydrochloric acid The value is 2, after sealing, it is heated in an oven at 185 ° C for 12 h.
  • the mixture is centrifuged, washed 4 times with water, and the precipitate is vacuum dried at 42 ° C, and then ground in a mortar to prepare a sample of nano TiO 2 ;
  • a good TiO 2 was placed in a beaker, the quantum dot solution prepared above was added, and then 15 parts of deionized water was added, magnetically stirred for 3 hours, and then transferred to a blast drying oven at 75 ° C for 4 hours, and cooled to obtain; All are parts by weight.
  • a method for preparing a surface-modified carbon quantum dot-titanium dioxide composite photocatalyst comprises the steps of: adding 20 parts of ethylene glycol to a reaction kettle, heating in an oven at 170 ° C for 3 hours, taking the supernatant after centrifugation, adding 0.5 A portion of ammonia water, mixed evenly, incubated at 100 ° C for 2h, cooled, centrifuged to remove the supernatant to obtain a modified carbon quantum dot solution; 5 parts of Ti (SO 4 ) 2 was added to 40 parts of deionized water, adjusted to pH with concentrated hydrochloric acid The value is 1.5, after sealing, it is heated in an oven at 180 ° C for 11 h.
  • the mixture is taken out and centrifuged, and washed three times with water.
  • the precipitate is vacuum dried at 40 ° C and then ground in a mortar to prepare a sample of nano TiO 2 ;
  • a good TiO 2 was placed in a beaker, the quantum dot solution prepared above was added, and then 10 parts of deionized water was added, and magnetically stirred for 2 hours, and then transferred to a blast drying oven at 70 ° C for 3 hours, and cooled to obtain; All are parts by weight.
  • a method for preparing a surface-modified carbon quantum dot-titanium dioxide composite photocatalyst comprises the following steps: adding 30 parts of ethylene glycol to a reaction kettle, heating in an oven at 190 ° C for 5 hours, centrifuging, taking the supernatant, and adding 1.5 A portion of ammonia water, mixed uniformly, kept at 110 ° C for 4h, cooled, centrifuged to remove the supernatant to obtain a modified carbon quantum dot solution; 5-7 parts of Ti (SO 4 ) 2 was added to 50 parts of deionized water, adjusted with concentrated hydrochloric acid After the pH is 2.5, after sealing, it is heated in an oven at 190 ° C for 13 h.
  • the mixture is taken out and centrifuged, and washed with water for 5 times.
  • the precipitate is vacuum dried at 45 ° C and then ground in a mortar to obtain a sample of nano TiO 2 ;
  • the prepared TiO 2 was placed in a beaker, the quantum dot solution prepared above was added, and then 20 parts of deionized water was added, and magnetically stirred for 4 hours, and then transferred to a blast drying oven at 80 ° C for 5 hours, and cooled; Each raw material is in parts by weight.
  • the method provided by the invention is simple and easy to operate, and a composite photocatalyst excellent in catalytic effect can be obtained.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

一种制备表面改性碳量子点-二氧化钛复合光催化剂方法，步骤如下：将20-30份乙二醇加入反应釜中，放入烘箱中加热，离心后取上清液，加入0.5-1.5份氨水，混合均匀，保温2-4h，冷却后离心取出上清液得到修饰过的碳量子点溶液；将5-7份Ti(SO 4) 2加入40-50份去离子水中，用浓盐酸调至pH值为1.5-2.5，密封后，置于烘箱中加热11-13h，反应后取出离心，用水洗涤，将沉淀真空干燥后用研钵研细，加入上述制备的量子点溶液，然后再加入10-20份去离子水，磁力搅拌，然后将其移入鼓风干燥箱中干燥，冷却即得。该方法简便、易操作，可得到催化效果优异的复合光催化剂。

Description

一种制备表面改性碳量子点-二氧化钛复合光催化剂方法 技术领域
本发明涉及一种制备表面改性碳量子点-二氧化钛复合光催化剂方法。
背景技术
自发现二氧化钛在可见光照射下将水分解成氧气和氢气后，二氧化钛光催化材料得到持续和广泛的关注。制备二氧化钛光催化剂的主要方法有溶胶-凝胶法、水热法、沉淀法、浸渍法、微乳液法、气象水解法、超重力法等。目前采用水热法制备TiO2的原料多为钛酸四丁酯和TiCl4，使用硫酸钛进行水热合成的研究相对较少。硫酸钛吸水性弱于液态钛盐，操作上更加简便易行，在工业上也有广泛的应用。
为提高TiO2对光的利用率，可将TiO2与碳量子点进行复合。碳量子点(CQDs)是一类尺寸小于10nm具有良好荧光性能的零维碳纳米材料，于2004年通过电泳法净化单层碳纳米管时首次发现，其粒径仅为1～10nm，具有很大的比表面积，利用有机物可以进行表面改性，使碳量子点更为稳定，同时碳量子点具有上转换发光性质以及半导体性质，在光催化领域有重要应用。
发明内容
本发明的目的在于提供一种制备表面改性碳量子点-二氧化钛复合光催化剂方法。
本发明通过下面技术方案实现：
一种制备表面改性碳量子点-二氧化钛复合光催化剂方法，包括如下步骤：将20-30份乙二醇加入反应釜中，放入烘箱中于170-190℃加热3-5h，离心后取上清液，加入0.5-1.5份氨水，混合均匀，于100-110℃保温2-4h，冷却后离心取出上清液得到修饰过的碳量子点溶液；将5-7份Ti(SO4)2加入40-50份去离子水中，用浓盐酸调至pH值为1.5-2.5，密封后，置于烘箱中于180-190℃加热11-13h，反应后取出离心，用水洗涤3-5次，将沉淀在40-45℃真空干燥后用研钵研细，制得纳米TiO2样品；将制备好的TiO2置于烧杯中，加入上述制备的量子点溶液，然后再加入10-20份去离子水，磁力搅拌2-4h，然后将其移入鼓风干燥箱中70-80℃干燥3-5h，冷却即得；各原料均为重量份。
优选地，所述的方法中，放入烘箱中于180℃加热4h。
优选地，所述的方法中，于105℃保温3h。
优选地，所述的方法中，用浓盐酸调至pH值为2。
优选地，所述的方法中，置于烘箱中于185℃加热12h。
优选地，所述的方法中，将沉淀在42℃真空干燥。
优选地，所述的方法中，磁力搅拌3h，然后将其移入鼓风干燥箱中75℃干燥4h。
本发明技术效果：
本发明提供的方法简便、易操作，可得到催化效果优异的复合光催化剂。
具体实施方式
下面结合实施例具体介绍本发明的实质性内容。
实施例1
一种制备表面改性碳量子点-二氧化钛复合光催化剂方法，包括如下步骤：将25份乙二醇加入反应釜中，放入烘箱中于180℃加热4h，离心后取上清液，加入1份氨水，混合均匀，于105℃保温3h，冷却后离心取出上清液得到修饰过的碳量子点溶液；将6份Ti(SO4)2加入45份去离子水中，用浓盐酸调至pH值为2，密封后，置于烘箱中于185℃加热12h，反应后取出离心，用水洗涤4次，将沉淀在42℃真空干燥后用研钵研细，制得纳米TiO2样品；将制备好的TiO2置于烧杯中，加入上述制备的量子点溶液，然后再加入15份去离子水，磁力搅拌3h，然后将其移入鼓风干燥箱中75℃干燥4h，冷却即得；各原料均为重量份。
实施例2
一种制备表面改性碳量子点-二氧化钛复合光催化剂方法，包括如下步骤：将20份乙二醇加入反应釜中，放入烘箱中于170℃加热3h，离心后取上清液，加入0.5份氨水，混合均匀，于100℃保温2h，冷却后离心取出上清液得到修饰过的碳量子点溶液；将5份Ti(SO4)2加入40份去离子水中，用浓盐酸调至pH值为1.5，密封后，置于烘箱中于180℃加热11h，反应后取出离心，用水洗涤3次，将沉淀在40℃真空干燥后用研钵研细，制得纳米TiO2样品；将制备好的TiO2置于烧杯中，加入上述制备的量子点溶液，然后再加入10份去离子水，磁力搅拌2h，然后将其移入鼓风干燥箱中70℃干燥3h，冷却即得；各原料均为重量份。
实施例3
一种制备表面改性碳量子点-二氧化钛复合光催化剂方法，包括如下步骤：将30份乙二醇加入反应釜中，放入烘箱中于190℃加热5h，离心后取上清液，加入1.5份氨水，混合均匀，于110℃保温4h，冷却后离心取出上清液得到修饰过的碳量子点溶液；将5-7份Ti(SO4)2加入50份去离子水中，用浓盐酸调至pH值为2.5，密封后，置于烘箱中于190℃加热13h，反应后取出离心，用水洗涤5次，将沉淀在45℃真空干燥后用研钵研细，制得纳米TiO2样品；将制备好的TiO2置于烧杯中，加入上述制备的量子点溶液，然后再加入20份去离子水，磁力搅拌4h，然后将其移入鼓风干燥箱中80℃干燥5h，冷却即得；各原料均为重量份。
本发明提供的方法简便、易操作，可得到催化效果优异的复合光催化剂。

Claims (7)

  1. 一种制备表面改性碳量子点-二氧化钛复合光催化剂方法，其特征在于包括如下步骤：将20-30份乙二醇加入反应釜中，放入烘箱中于170-190℃加热3-5h，离心后取上清液，加入0.5-1.5份氨水，混合均匀，于100-110℃保温2-4h，冷却后离心取出上清液得到修饰过的碳量子点溶液；将5-7份Ti(SO4)2加入40-50份去离子水中，用浓盐酸调至pH值为1.5-2.5，密封后，置于烘箱中于180-190℃加热11-13h，反应后取出离心，用水洗涤3-5次，将沉淀在40-45℃真空干燥后用研钵研细，制得纳米TiO2样品；将制备好的TiO2置于烧杯中，加入上述制备的量子点溶液，然后再加入10-20份去离子水，磁力搅拌2-4h，然后将其移入鼓风干燥箱中70-80℃干燥3-5h，冷却即得；各原料均为重量份。
  2. 根据权利要求1所述的方法，其特征在于：放入烘箱中于180℃加热4h。
  3. 根据权利要求1所述的方法，其特征在于：于105℃保温3h。
  4. 根据权利要求1所述的方法，其特征在于：用浓盐酸调至pH值为2。
  5. 根据权利要求1所述的方法，其特征在于：置于烘箱中于185℃加热12h。
  6. 根据权利要求1所述的方法，其特征在于：将沉淀在42℃真空干燥。
  7. 根据权利要求1所述的方法，其特征在于：磁力搅拌3h，然后将其移入鼓风干燥箱中75℃干燥4h。
PCT/CN2017/101809 2017-09-14 2017-09-15 一种制备表面改性碳量子点-二氧化钛复合光催化剂方法 WO2019051745A1 (zh)

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CN114195365A (zh) * 2021-12-16 2022-03-18 广州光联电子科技有限公司 一种基于分子筛的荧光玻璃及其制备方法与应用

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