CN107442157A - 一种快速合成分子筛负载型纳米光催化剂的方法 - Google Patents
一种快速合成分子筛负载型纳米光催化剂的方法 Download PDFInfo
- Publication number
- CN107442157A CN107442157A CN201710691854.2A CN201710691854A CN107442157A CN 107442157 A CN107442157 A CN 107442157A CN 201710691854 A CN201710691854 A CN 201710691854A CN 107442157 A CN107442157 A CN 107442157A
- Authority
- CN
- China
- Prior art keywords
- molecular sieve
- sba
- tio
- mesoporous
- capillary force
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 40
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 14
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 230000005855 radiation Effects 0.000 claims abstract description 5
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical class CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims 1
- 229910052763 palladium Inorganic materials 0.000 claims 1
- 229910052703 rhodium Inorganic materials 0.000 claims 1
- 229910052707 ruthenium Inorganic materials 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000010931 gold Substances 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000001988 small-angle X-ray diffraction Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 210000005239 tubule Anatomy 0.000 description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- QRJOYPHTNNOAOJ-UHFFFAOYSA-N copper gold Chemical compound [Cu].[Au] QRJOYPHTNNOAOJ-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- CQBPOPVKDNHISM-UHFFFAOYSA-N propane-1,2,3-triol;propan-2-one Chemical compound CC(C)=O.OCC(O)CO CQBPOPVKDNHISM-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0325—Noble metals
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Optics & Photonics (AREA)
- Electromagnetism (AREA)
- Plasma & Fusion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
本发明公开了一种快速合成分子筛负载型纳米光催化剂的方法,属于光催化技术领域。利用分子筛介孔在负压环境下的毛细管力,吸附二氧化钛和金属纳米颗粒的前驱体,并配合微波辅助醇热还原法,快速获得高催化活性和高稳定性的分子筛负载型光催化剂。制备方法简单易行,有利于大规模推广。
Description
技术领域
本发明涉及环境治理领域的光催化技术,特别涉及一种快速合成分子筛负载型纳米复合光催化剂的方法。
背景技术
在众多的光催化材料中,二氧化钛无毒,化学稳定性好,光催化活性高,价廉易得,因此成为目前应用最广泛的半导体光催化材料。目前,在光催化反应中存在催化剂易失活、易凝聚和难回收的缺点,克服这些缺点的有效方法之一是将纳米材料进行负载化,与单一TiO2体系相比,负载型TiO2体系液固分离较为容易,可以回收并重复使用,有更高的应用价值。并且大量研究表明光催化过程中,有机物在TiO2表面的吸附是决定光催化降解动力学的关键因素之一。
分子筛SBA-15由于其特殊孔道结构、较大的比表面积和极强的吸附性能,在其结构中可以形成稳定的、分子尺寸的半导体纳米团簇。根据这一理念,研究人员报道了众多基于分子筛载体的光催化剂,其中,Schunemann等人报道一种新型的等离子体光催化剂,即把粒径2 nm的金铜合金负载在介孔材料(SBA-15,KIT-6和MCM-41)上,测试了该催化剂在可见光下对甘油催化氧化二甘油丙酮的反应活性。而福州大学的付贤智教授在中国专利(公开号CN101653732A)中提供了一种分子筛负载卤氧化铋光催化剂的制备及应用方法。他们通过引入分子筛为载体,增大了催化剂的比表面积,减小了晶粒尺寸,显著提高催化剂降解苯的活性。
然而,分子筛负载的光催化剂在合成过程中,由于孔道的特殊性,易于被催化剂堵塞,导致大量的纳米颗粒团聚在分子筛的表面,降低了催化剂的活性。另外,传统的浸渍煅烧方法的合成过程耗时较长且能耗较大。为了解决以上问题,我们提出一种利用分子筛介孔的毛细管力吸附负载前驱体配合微波辅助水热合成法快速合成光催化剂。
发明内容
本发明提供一种快速合成分子筛负载型纳米光催化剂的方法,以期快速合成分子筛负载型光催化剂。
所述纳米复合光催化剂利用分子筛介孔的毛细管力吸附负载前驱体配合微波辅助水热合成法制备,其技术方案包括以下步骤:
(1)取SBA-15粉末置于烘箱内烘烤,以去除分子筛孔道内吸附的杂质;
(2)将烘烤后的SBA-15加入无水乙醇和冰乙酸中超声分散,之后逐滴加入二氧化钛前驱体。将混合液置于100 Pa真空系统中,利用分子筛介孔的毛细管力将二氧化钛前驱体吸入孔道中;
(3)将混合液体转移至聚四氟乙烯内衬水热反应釜中,随后放入微波消解仪中反应,合成TiO2/SBA-15;
(4)将一定量的1-己醇和金属纳米颗粒前驱体溶液(氯盐和硝酸盐)滴加至TiO2/SBA-15中,将混合液置于100 Pa真空系统中,,利用分子筛介孔的毛细管力将金属纳米颗粒的前驱体吸入孔道中;
(5)在氩气环境下,微波反应数分钟合成光催化剂。反应完成后,收集沉淀,用蒸馏水和无水乙醇分别洗涤,随后在烘箱内干燥后使用。
本发明的有益效果体现在以下三个方面:1. 利用分子筛介孔在负压力状态下的毛细管力将二氧化钛和金属纳米颗粒的前驱体吸入孔道中,防止纳米颗粒在分子筛表面生长团聚,堵塞分子筛孔道。2. 采用微波辅助醇热还原法,快速合成金属纳米颗粒。3. SBA-15的孔道结构可以抑制金属纳米颗粒和TiO2纳米颗粒的生长,并使高度分散的金属纳米颗粒在分子筛孔道中与TiO2紧密接触,形成肖特基势垒,有利于光生电子和光生空穴的传导,从而促进光催化反应的进行。
附图说明
图1 Au/TiO2/SBA-15样品的透射电镜图片。
图2 Au/TiO2/SBA-15样品的高角环形暗场-扫描透射电子显微镜图片。
图3 SBA-15和Au/TiO2/SBA-15两种粉末样品的小角度X射线衍射图。
图4 德固赛P25和Au/TiO2/SBA-15两种粉末样品对亚甲基蓝溶液的降解情况。
具体实施方式
下面结合附图和实施例对本发明做详细说明。
实施例1
取SBA-15粉末置于烘箱内烘烤,以去除分子筛孔道内吸附的杂质。将1g的SBA-15加入20 mL的无水乙醇和冰乙酸中超声分散10分钟,之后逐滴加入二氧化钛前驱体,将混合液置于负压系统中,利用分子筛介孔的毛细管力将二氧化钛前驱体吸入孔道中。在磁力搅拌条件下搅拌1小时后,将混合液体转移至70 mL聚四氟乙烯内衬水热反应釜中,随后放入微波消解仪中(MDS-6,上海,中国),在180oC温度下反应30分钟,合成TiO2/SBA-15。将一定量的1-己醇和氯金酸溶液(10 mg/mL)滴加至TiO2/SBA-15中,将混合液置于负压系统中,利用分子筛介孔的毛细管力将金属纳米颗粒的前驱体吸入孔道中。最后,在氩气环境下,微波反应5分钟合成Au1/TiO2/SBA-15光催化剂。对合成的Au/TiO2/SBA-15光催化剂进行透射电镜(图1)和扫描透射电镜(图2)拍摄照片后表明合成的Au/TiO2/SBA-15催化剂中,均可以观察到具有[100]方向高度有序的平行孔道,这表明随着Au纳米颗粒和TiO2的负载,并没有改变SBA-15载体介孔的长程有序结构,并且Au纳米颗粒和TiO2高度分散地分布在分子筛SBA-15的孔道中。小角度X射线衍射测试(图3)同样表明,两步法合成的Au/TiO2/SBA-15复合材料保留了原始SBA-15材料长程有序的介孔结构。Au/TiO2/SBA-15样品在180分钟内,在波长大于400 nm的可见光下对亚甲基蓝的降解率为99%,而商品德固赛P25为64%(图4)。
实施例2
取SBA-15粉末置于烘箱内烘烤,以去除分子筛孔道内吸附的杂质。将1g的SBA-15加入20 mL的无水乙醇和冰乙酸中超声分散10分钟,之后逐滴加入二氧化钛前驱体,将混合液置于负压系统中,利用分子筛介孔的毛细管力将二氧化钛前驱体吸入孔道中。在磁力搅拌条件下搅拌1小时后,将混合液体转移至70 mL聚四氟乙烯内衬水热反应釜中,随后放入微波消解仪中(MDS-6,上海,中国),在180oC温度下反应30分钟,合成TiO2/SBA-15。将一定量的1-己醇和氯铂酸溶液滴加至TiO2/SBA-15中,将混合液置于负压系统中,利用分子筛介孔的毛细管力将金属纳米颗粒的前驱体吸入孔道中。最后,在氩气环境下,微波反应5分钟合成Pt/TiO2/SBA-15光催化剂。
实施例3
取SBA-15粉末置于烘箱内烘烤,以去除分子筛孔道内吸附的杂质。将1g的SBA-15加入20 mL的无水乙醇和冰乙酸中超声分散10分钟,之后逐滴加入二氧化钛前驱体,将混合液置于负压系统中,利用分子筛介孔的毛细管力将二氧化钛前驱体吸入孔道中。在磁力搅拌条件下搅拌1小时后,将混合液体转移至70 mL聚四氟乙烯内衬水热反应釜中,随后放入微波消解仪中(MDS-6,上海,中国),在180oC温度下反应30分钟,合成TiO2/SBA-15。将一定量的1-己醇和硝酸银溶液滴加至TiO2/SBA-15中,将混合液置于负压系统中,利用分子筛介孔的毛细管力将金属纳米颗粒的前驱体吸入孔道中。最后,在氩气环境下,微波反应5分钟合成Ag/TiO2/SBA-15光催化剂。
Claims (5)
1.一种快速合成分子筛负载型纳米光催化剂的方法,其特征在于,利用分子筛介孔的毛细管力吸附负载前驱体,配合微波辅助醇热还原法,快速制备分子筛负载型光催化剂。
2.根据权利要求1所述光催化剂的制备方法,其特征在于,技术方案包括以下步骤:
(1)取分子筛SBA-15粉末置于烘箱内烘烤,以去除分子筛孔道内吸附的杂质;
(2)将烘烤后的SBA-15加入无水乙醇和冰乙酸中超声分散,之后逐滴加入二氧化钛前驱体,将混合液置于100 Pa真空系统中,利用分子筛介孔的毛细管力将二氧化钛前驱体吸入孔道中;
(3)将混合液体转移至聚四氟乙烯内衬水热反应釜中,随后放入微波消解仪中反应,合成TiO2/SBA-15;
(4)将一定量的1-己醇和金属纳米颗粒前驱体溶液(氯盐和硝酸盐)滴加至TiO2/SBA-15中,将混合液置于100 Pa真空系统中,利用分子筛介孔的毛细管力将金属纳米颗粒的前驱体吸入孔道中;
(5)在氩气环境下,微波反应数分钟合成光催化剂,反应完成后,收集沉淀,用蒸馏水和无水乙醇分别洗涤,随后在烘箱内干燥后使用。
3.根据权利要求2所述光催化剂的制备方法,其特征在于利用分子筛介孔的毛细管力,使其在负压力环境下吸附二氧化钛前驱体和金属纳米颗粒前驱体。
4.根据权利要求2所述光催化剂的制备方法,其特征在于采用微波辅助醇热还原法在分子筛内孔中负载金属纳米颗粒。
5.根据权利要求2所述光催化剂的制备方法,其特征在于,所述负载的金属纳米颗粒为Au、Ag、Pt、Pd、Ru、Ir、Rh。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710691854.2A CN107442157A (zh) | 2017-08-14 | 2017-08-14 | 一种快速合成分子筛负载型纳米光催化剂的方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710691854.2A CN107442157A (zh) | 2017-08-14 | 2017-08-14 | 一种快速合成分子筛负载型纳米光催化剂的方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN107442157A true CN107442157A (zh) | 2017-12-08 |
Family
ID=60492369
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710691854.2A Pending CN107442157A (zh) | 2017-08-14 | 2017-08-14 | 一种快速合成分子筛负载型纳米光催化剂的方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107442157A (zh) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108311094A (zh) * | 2018-03-02 | 2018-07-24 | 奥为(天津)环保科技有限公司 | 一种快速合成负载型金属纳米颗粒的方法 |
CN108360010A (zh) * | 2018-01-26 | 2018-08-03 | 济南大学 | 一种新型固体氧化物电解电池电极催化涂层的制备方法 |
CN108855206A (zh) * | 2018-06-01 | 2018-11-23 | 南京工程学院 | 一种微-介孔复合光催化材料及其制备方法 |
CN109701511A (zh) * | 2019-01-28 | 2019-05-03 | 广东朗研科技有限公司 | 一种分形结构氧化钛的制备方法 |
CN110404569A (zh) * | 2018-04-28 | 2019-11-05 | 奥为(天津)环保科技有限公司 | 一种金属负载g-C3N4光催化剂的制备方法 |
CN110560147A (zh) * | 2019-07-31 | 2019-12-13 | 广东工业大学 | 一种亚纳米级Pd颗粒负载Ti-SBA-15催化剂及其制备方法与应用 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1554481A (zh) * | 2003-12-26 | 2004-12-15 | 华东师范大学 | 介孔分子筛中杂多酸纳米粒子的组装方法 |
CN101698153A (zh) * | 2009-10-30 | 2010-04-28 | 湘潭大学 | 一种纳米贵金属催化剂及其制备方法 |
CN103691477A (zh) * | 2013-12-27 | 2014-04-02 | 天津城建大学 | 二元负载型TiO2/纳米铁/SBA-15催化剂的制备方法 |
-
2017
- 2017-08-14 CN CN201710691854.2A patent/CN107442157A/zh active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1554481A (zh) * | 2003-12-26 | 2004-12-15 | 华东师范大学 | 介孔分子筛中杂多酸纳米粒子的组装方法 |
CN101698153A (zh) * | 2009-10-30 | 2010-04-28 | 湘潭大学 | 一种纳米贵金属催化剂及其制备方法 |
CN103691477A (zh) * | 2013-12-27 | 2014-04-02 | 天津城建大学 | 二元负载型TiO2/纳米铁/SBA-15催化剂的制备方法 |
Non-Patent Citations (1)
Title |
---|
赵杰 等: "醋酸盐稳定的Pt/C纳米离子的微波合成及其对甲醇的电催化氧化", 《第十三次全国电化学会议论文摘要集(下集)》 * |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108360010A (zh) * | 2018-01-26 | 2018-08-03 | 济南大学 | 一种新型固体氧化物电解电池电极催化涂层的制备方法 |
CN108360010B (zh) * | 2018-01-26 | 2019-09-06 | 济南大学 | 一种固体氧化物电解电池电极催化涂层的制备方法 |
CN108311094A (zh) * | 2018-03-02 | 2018-07-24 | 奥为(天津)环保科技有限公司 | 一种快速合成负载型金属纳米颗粒的方法 |
CN110404569A (zh) * | 2018-04-28 | 2019-11-05 | 奥为(天津)环保科技有限公司 | 一种金属负载g-C3N4光催化剂的制备方法 |
CN108855206A (zh) * | 2018-06-01 | 2018-11-23 | 南京工程学院 | 一种微-介孔复合光催化材料及其制备方法 |
CN108855206B (zh) * | 2018-06-01 | 2021-06-11 | 南京工程学院 | 一种微-介孔复合光催化材料及其制备方法 |
CN109701511A (zh) * | 2019-01-28 | 2019-05-03 | 广东朗研科技有限公司 | 一种分形结构氧化钛的制备方法 |
CN110560147A (zh) * | 2019-07-31 | 2019-12-13 | 广东工业大学 | 一种亚纳米级Pd颗粒负载Ti-SBA-15催化剂及其制备方法与应用 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107442157A (zh) | 一种快速合成分子筛负载型纳米光催化剂的方法 | |
Liu et al. | A novel step-scheme BiVO4/Ag3VO4 photocatalyst for enhanced photocatalytic degradation activity under visible light irradiation | |
Xu et al. | Simple synthesis of ZnO nanoflowers and its photocatalytic performances toward the photodegradation of metamitron | |
WO2015146830A1 (ja) | 光触媒およびその製造方法 | |
CN102350346B (zh) | 具有表面等离子体效应的可见光催化剂制备方法及其应用 | |
CN111514882B (zh) | 一种Ag-AgCl/三氧化钨/类石墨相氮化碳三元复合光催化剂及其制备方法和应用 | |
CN109482179A (zh) | TiO2/石墨烯/纳米银复合光催化剂的制备及其对甲醛的降解 | |
CN109046389B (zh) | 金纳米棒-铂纳米粒子-CdS复合光催化剂及其制备和应用 | |
CN103263920B (zh) | 一种TiO2负载的高分散金属催化剂及其制备方法 | |
CN103599776A (zh) | 一种Pd/CeO2可见光光催化剂及其制备方法和应用 | |
CN110227453B (zh) | 一种AgCl/ZnO/GO复合可见光催化剂的制备方法 | |
CN108514887A (zh) | 一种空心纳米颗粒二氧化钛/黑磷烯光热催化剂及其制备方法与应用 | |
CN102764649B (zh) | 一种金属银负载型二氧化钛光催化剂及其制备方法 | |
CN109331817A (zh) | 一种用于分解空气中有机物的光催化材料及制备方法 | |
Liu et al. | Metal-organic frameworks derived TiO2/carbon nitride heterojunction photocatalyst with efficient catalytic performance under visible light | |
CN107790129A (zh) | 氧化亚铜/石墨烯可见光光催化剂的制备方法及其产品和应用 | |
CN102101051B (zh) | 一种能降解氮氧化物的碳纳米管负载型纳米光催化材料的制备方法 | |
CN111482169B (zh) | 负载贵金属的纳米光催化剂及其制备方法和应用 | |
Duan et al. | The composite of Zr-doped TiO2 and MOF-derived metal oxide for oxidative removal of formaldehyde at the room temperature | |
Lian et al. | Hydrogen-terminated silicon nanowire photocatalysis: Benzene oxidation and methyl red decomposition | |
CN102553562A (zh) | 多重改性复合光催化剂及其制备方法 | |
CN109046308A (zh) | 一种石墨烯微米花/纳米氧化锌光催化材料及其制备方法 | |
CN104645980B (zh) | 一种贵金属‑氧化锌复合材料及其制备方法和应用 | |
CN106693956B (zh) | 一种贵金属-二氧化钛复合催化剂的制备方法 | |
CN108187701B (zh) | 一种管状AgCl结构的AgCl/BiOCl光催化剂制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171208 |
|
WD01 | Invention patent application deemed withdrawn after publication |