WO2019051745A1 - Procédé de préparation d'un photocatalyseur composite à nanocristaux de carbone et dioxyde de titane à surface modifiée - Google Patents

Procédé de préparation d'un photocatalyseur composite à nanocristaux de carbone et dioxyde de titane à surface modifiée Download PDF

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Publication number
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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same
parts
oven
quantum dot
carbon quantum
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PCT/CN2017/101809
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English (en)
Chinese (zh)
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谢秋生
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谢秋生
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Publication of WO2019051745A1 publication Critical patent/WO2019051745A1/fr

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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

Definitions

  • 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)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé de préparation d'un photocatalyseur composite à nanocristaux de carbone et dioxyde de titane à surface modifié, le procédé comprenant les étapes suivantes : ajouter de 20 à 30 parties d'éthylène glycol à un réacteur qu'on place dans un four pour le chauffage puis qu'on soumet à une centrifugation, ajouter de 0,5 à 1,5 partie d'ammoniac aqueux à un surnageant, mélanger uniformément, et le maintenir à une certaine température pour une durée de 2 à 4 h, le refroidir et le soumettre à une centrifugation, puis éliminer le surnageant pour obtenir une solution de nanocristaux de carbone modifiés; ajouter de 5 à 7 parties de Ti(SO4)2 à 40 à 50 parties d'eau désionisée, ajuster le pH entre 1,5 et 2,5 avec de l'acide chlorhydrique concentré, sceller puis placer dans un four et chauffer pour une durée de 11 à 13 h, le retirer après réaction, effectuer une centrifugation, le laver avec de l'eau, assécher un précipité sous vide, puis le broyer finement à l'aide d'un mortier, y ajouter la solution préparée de nanocristaux, puis ajouter de 10 à 20 parties d'eau désionisée, effectuer une agitation magnétique, puis le transférer vers un four de séchage à air forcé pour le séchage, et le faire refroidir. Le procédé est simple et facile à utiliser, et peut produire un photocatalyseur composite ayant un excellent effet catalytique.
PCT/CN2017/101809 2017-09-14 2017-09-15 Procédé de préparation d'un photocatalyseur composite à nanocristaux de carbone et dioxyde de titane à surface modifiée WO2019051745A1 (fr)

Applications Claiming Priority (2)

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CN201710825578 2017-09-14
CN2017108255784 2017-09-14

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WO2019051745A1 true WO2019051745A1 (fr) 2019-03-21

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110180521A (zh) * 2019-06-05 2019-08-30 陕西科技大学 一种碳量子点/二氧化钛纳米复合材料的制备方法
CN110354845A (zh) * 2019-06-28 2019-10-22 广东工业大学 一种碳纳米点修饰的钨酸铋光催化剂及其制备方法和应用
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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060063667A1 (en) * 2004-09-20 2006-03-23 Tsai-Chuan Lu Photo-catalyst physical water molecule for medical purposes
CN102127431A (zh) * 2010-12-24 2011-07-20 苏州方昇光电装备技术有限公司 碳量子点的制法及应用该碳量子点制备光催化剂的方法
CN103480353A (zh) * 2013-10-01 2014-01-01 大连理工大学 一种用水热法合成碳量子点溶液制备复合纳米光催化剂的方法
US20150069295A1 (en) * 2013-09-09 2015-03-12 National University Of Singapore Hydrogel nanocomposite
CN104923202A (zh) * 2015-04-29 2015-09-23 东华大学 一种氮掺杂碳量子点/二氧化钛复合材料的制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060063667A1 (en) * 2004-09-20 2006-03-23 Tsai-Chuan Lu Photo-catalyst physical water molecule for medical purposes
CN102127431A (zh) * 2010-12-24 2011-07-20 苏州方昇光电装备技术有限公司 碳量子点的制法及应用该碳量子点制备光催化剂的方法
US20150069295A1 (en) * 2013-09-09 2015-03-12 National University Of Singapore Hydrogel nanocomposite
CN103480353A (zh) * 2013-10-01 2014-01-01 大连理工大学 一种用水热法合成碳量子点溶液制备复合纳米光催化剂的方法
CN104923202A (zh) * 2015-04-29 2015-09-23 东华大学 一种氮掺杂碳量子点/二氧化钛复合材料的制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LI, LEI ET AL.: "Preparation of the Surface Modified Carbon Quantum Dot/Titanium Dioxide Composite Photocatalyst", GUANGDONG CHEMICAL INDUSTRY, vol. 44, no. 14, 30 July 2007 (2007-07-30), ISSN: 1007-1865 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110180521A (zh) * 2019-06-05 2019-08-30 陕西科技大学 一种碳量子点/二氧化钛纳米复合材料的制备方法
CN110180521B (zh) * 2019-06-05 2022-07-26 陕西科技大学 一种碳量子点/二氧化钛纳米复合材料的制备方法
CN110354845A (zh) * 2019-06-28 2019-10-22 广东工业大学 一种碳纳米点修饰的钨酸铋光催化剂及其制备方法和应用
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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