CN108993374B - Preparation method of one-dimensional mesoporous photocatalytic material - Google Patents
Preparation method of one-dimensional mesoporous photocatalytic material Download PDFInfo
- Publication number
- CN108993374B CN108993374B CN201810824656.3A CN201810824656A CN108993374B CN 108993374 B CN108993374 B CN 108993374B CN 201810824656 A CN201810824656 A CN 201810824656A CN 108993374 B CN108993374 B CN 108993374B
- Authority
- CN
- China
- Prior art keywords
- solution
- preparation
- solid
- photocatalytic material
- dimensional
- 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.)
- Active
Links
- 239000000463 material Substances 0.000 title claims abstract description 36
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000007669 thermal treatment Methods 0.000 claims description 5
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 5
- 239000011148 porous material Substances 0.000 abstract description 9
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 8
- 238000000746 purification Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- BITDBQPMTQEZRS-UHFFFAOYSA-N praseodymium titanium Chemical compound [Ti][Pr] BITDBQPMTQEZRS-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28095—Shape or type of pores, voids, channels, ducts
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Biomedical Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Catalysts (AREA)
Abstract
A preparation method of a one-dimensional mesoporous photocatalytic material belongs to the field of environmental purification materials; the preparation method comprises the following steps: 1) preparing a solution A and a solution B from the raw material mixture; 2) mixing the solution A and the solution B, carrying out hydrothermal reaction, and filtering and washing the obtained solid-liquid mixture; 3) after the solid is dried, high-temperature calcination is carried out, and the cooled particles are ground into powder to obtain the one-dimensional mesoporous photocatalytic material; the material obtained by the invention has a linear one-dimensional pore structure and a stable structure, can be used for adsorbing organic pollutants in water and atmosphere, can decompose adsorbed organic matters under the irradiation of visible light and ultraviolet light, and can conveniently and quickly remove various organic pollutants in the water and atmosphere environment.
Description
Technical Field
The invention belongs to the field of environment purification materials, and particularly relates to a preparation method of a one-dimensional mesoporous photocatalytic material.
Background
Various organic materials present in water and atmospheric environments are important pollutants in the environment and need to be removed in a variety of ways. The photocatalytic pollution purification technology is an advanced deep oxidation technology, is widely applied to the treatment process of water and atmospheric environmental pollution, plays a very significant role, and can purify most organic pollutants. In the course of research for almost half a century, in order to obtain a desired purification efficiency, efforts have been made to prepare advanced and highly efficient photocatalytic materials so as to have higher activity and be applicable to various complicated use environments including two different media of water and atmosphere. The photocatalytic material can generate substances with strong oxidation-reduction characteristics under the condition of illumination, so that the photocatalytic material is used for degrading organic pollutants. To achieve this, it is necessary to provide a new highly efficient photocatalytic material which not only can produce substances with redox ability, but also can be adapted to various specific practical conditions. Since organic substances can be removed from water and atmosphere by adsorption, a material having high adsorption capacity and strong photocatalytic efficiency is more suitable for the requirements of complex use environments. To achieve this, the pore structure of the photocatalytic material needs to be specially designed so as to be easy to adsorb organic pollutants and facilitate the subsequent photocatalytic purification treatment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a one-dimensional mesoporous photocatalytic material, which can be used for the adsorption-photocatalytic combined purification process of organic pollutants in water and atmosphere.
The technical scheme adopted by the invention is as follows:
a preparation method of a one-dimensional mesoporous photocatalytic material comprises the following process steps:
step 1: preparation of solutions (1) and (2) without sequence
(1) Sequentially adding 330-380 mL of absolute ethyl alcohol, 26-35 mL of ethylene glycol and 12-16 mL of isopropyl titanate into a flask, heating the solution to 65 ℃, refluxing for 20min, continuously adding 3-7 g of polyacrylamide with the molecular weight of 300 ten thousand, 2-3 g of emulsifier Span-60 and 5-7 mL of ethyl acetoacetate into the flask, and continuously refluxing for 30min at 65 ℃ to form a solution A;
(2) adding 100-120 mL of deionized water, 5-8 g of praseodymium nitrate and 3-4 g of sodium bicarbonate into a beaker, and stirring until a transparent solution B is formed;
step 2: pore-forming by crystallization
(1) Mixing the solution A and the solution B, placing the mixture in a stainless steel high-pressure reaction kettle, controlling the reaction temperature to be 190-210 ℃, controlling the system pressure to be less than 2.6MPa, reacting for 35-60 h, and cooling to room temperature to obtain a solid-liquid mixture;
(2) filtering the solid-liquid mixture, and washing with distilled water to obtain a solid A;
and step 3: thermal treatment
And drying the solid A at 160 ℃ for 20h, calcining at 630-750 ℃ for 3.5-5.5 h, cooling to room temperature, and grinding into powder with the particle size of less than 20 mu m to obtain the one-dimensional mesoporous photocatalytic material.
The one-dimensional mesoporous photocatalytic material prepared by the method has the technical characteristics that: the specific surface area is more than 300m2The aperture of the one-dimensional mesopore is 26-38 nm, the aperture length is 3-5 mu m, and the compressive strength is more than 5.6 multiplied by 104Pa, temperature-resistant range is more than 700 ℃.
Compared with the prior art, the preparation method of the one-dimensional mesoporous photocatalytic material has the advantages that:
the invention prepares the one-dimensional mesoporous photocatalytic material taking the titanium praseodymium composite oxide as the main component. The material has a linear one-dimensional pore structure and can be used for adsorbing organic pollutants in water and atmosphere. Meanwhile, the adsorbed organic matters can be decomposed under the irradiation of visible light and ultraviolet light, so that the synergistic effect of quick adsorption and decomposition is achieved, and various organic pollutants in water and the atmospheric environment can be conveniently and quickly removed. The material has stable structure and long service life, and is suitable for the requirements of various complex conditions on environment purification materials.
Detailed Description
The chemical raw materials used in the following examples are all pure materials.
Example 1
A preparation method of a one-dimensional mesoporous photocatalytic material comprises the following process steps:
step 1: preparation of solutions (1) and (2) without sequence
(1) Adding 330mL of absolute ethyl alcohol, 26mL of ethylene glycol and 12mL of isopropyl titanate into a flask in sequence, heating the solution to 65 ℃, refluxing for 20min, adding 3g of polyacrylamide with the molecular weight of 300 ten thousand, 2g of emulsifier Span-60 and 5mL of ethyl acetoacetate into the flask, and refluxing for 30min at 65 ℃ to form a solution A;
(2) adding 100mL of deionized water, 5g of praseodymium nitrate and 3g of sodium bicarbonate into a beaker, and stirring until a transparent solution B is formed;
step 2: pore-forming by crystallization
(1) Mixing the solution A and the solution B, placing the mixture in a stainless steel high-pressure reaction kettle, controlling the reaction temperature to be 190 ℃ and the system pressure to be 2.2MPa, reacting for 60 hours, and cooling to room temperature to obtain a solid-liquid mixture;
(2) filtering the solid-liquid mixture, and washing with distilled water to obtain a solid A;
and step 3: thermal treatment
And drying the solid A at 160 ℃ for 20h, calcining at 630 ℃ for 5.5h, cooling to room temperature, and grinding into powder with the particle size of less than 20 mu m to obtain the one-dimensional mesoporous photocatalytic material.
The specific surface area of the one-dimensional mesoporous photocatalytic material prepared in the embodiment is 450m2G, pore diameter of 26nm, pore length of 5 μm, and compressive strength of 5.8 × 104Pa, temperature-resistant range is more than 700 ℃.
Example 2
A preparation method of a one-dimensional mesoporous photocatalytic material comprises the following process steps:
step 1: preparation of solutions (1) and (2) without sequence
(1) Adding 350mL of absolute ethyl alcohol, 29mL of ethylene glycol and 14mL of isopropyl titanate into a flask in sequence, heating the solution to 65 ℃, refluxing for 20min, continuously adding 5g of polyacrylamide with the molecular weight of 300 ten thousand, 2.5g of emulsifier Span-60 and 6mL of ethyl acetoacetate into the flask, and continuously refluxing for 30min at 65 ℃ to form a solution A;
(2) adding 110mL of deionized water, 6g of praseodymium nitrate and 3.5g of sodium bicarbonate into a beaker, and stirring until a transparent solution B is formed;
step 2: pore-forming by crystallization
(1) Mixing the solution A and the solution B, placing the mixture in a stainless steel high-pressure reaction kettle, controlling the reaction temperature to be 200 ℃ and the system pressure to be 2.3MPa, reacting for 48 hours, and cooling to room temperature to obtain a solid-liquid mixture;
(2) filtering the solid-liquid mixture, and washing with distilled water to obtain a solid A;
and step 3: thermal treatment
And drying the solid A at 160 ℃ for 20h, calcining at 690 ℃ for 4.5h, cooling to room temperature, and grinding into powder with the particle size of less than 20 mu m to obtain the one-dimensional mesoporous photocatalytic material.
The specific surface area of the one-dimensional mesoporous photocatalytic material prepared in the embodiment is 410m2G, pore diameter of 32nm, pore length of 4 μm, and compressive strength of 6.2 × 104pa, temperature resistant range is more than 700 ℃.
Example 3
A preparation method of a one-dimensional mesoporous photocatalytic material comprises the following process steps:
step 1: preparation of solutions (1) and (2) without sequence
(1) Adding 380mL of absolute ethyl alcohol, 35mL of ethylene glycol and 16mL of isopropyl titanate into a flask in sequence, heating the solution to 65 ℃, refluxing for 20min, continuously adding 7g of polyacrylamide with the molecular weight of 300 ten thousand, 3g of emulsifier Span-60 and 7mL of ethyl acetoacetate into the flask, and continuously refluxing for 30min at 65 ℃ to form a solution A;
(2) adding 120mL of deionized water, 8g of praseodymium nitrate and 4g of sodium bicarbonate into a beaker, and stirring until a transparent solution B is formed;
step 2: pore-forming by crystallization
(1) Mixing the solution A and the solution B, placing the mixture in a stainless steel high-pressure reaction kettle, controlling the reaction temperature to be 210 ℃ and the system pressure to be 2.5MPa, reacting for 35 hours, and cooling to room temperature to obtain a solid-liquid mixture;
(2) filtering the solid-liquid mixture, and washing with distilled water to obtain a solid A;
and step 3: thermal treatment
And drying the solid A at 160 ℃ for 20h, calcining at 750 ℃ for 3.5h, cooling to room temperature, and grinding into powder with the particle size of less than 20 mu m to obtain the one-dimensional mesoporous photocatalytic material.
The specific surface area of the one-dimensional mesoporous photocatalytic material prepared in the embodiment is 390m2G, pore diameter of 38nm, pore length of 3 μm, and compressive strength of 6.5 × 104Pa, temperature-resistant range is more than 700 ℃.
Claims (1)
1. A preparation method of a one-dimensional mesoporous photocatalytic material is characterized in that the technical characteristics of the one-dimensional mesoporous photocatalytic material are as follows: the specific surface area is more than 300m2The aperture of the one-dimensional mesopore is 26-38 nm, the aperture length is 3-5 mu m, and the compressive strength is more than 5.6 multiplied by 104Pa, temperature-resistant range is more than 700 ℃, and the preparation method comprises the following process steps:
step 1: preparation of solutions (1) and (2) without sequence
(1) Sequentially adding 330-380 mL of absolute ethyl alcohol, 26-35 mL of ethylene glycol and 12-16 mL of isopropyl titanate into a flask, heating the solution to 65 ℃, refluxing for 20min, continuously adding 3-7 g of polyacrylamide with the molecular weight of 300 ten thousand, 2-3 g of emulsifier Span-60 and 5-7 mL of ethyl acetoacetate into the flask, and continuously refluxing for 30min at 65 ℃ to form a solution A;
(2) adding 100-120 mL of deionized water, 5-8 g of praseodymium nitrate and 3-4 g of sodium bicarbonate into a beaker, and stirring until a transparent solution B is formed;
step 2: pore-forming by crystallization
(1) Mixing the solution A and the solution B, placing the mixture in a stainless steel high-pressure reaction kettle, controlling the reaction temperature to be 190-210 ℃, controlling the system pressure to be less than 2.6MPa, reacting for 35-60 h, and cooling to room temperature to obtain a solid-liquid mixture;
(2) filtering the solid-liquid mixture, and washing with distilled water to obtain a solid A;
and step 3: thermal treatment
And drying the solid A at 160 ℃ for 20h, calcining at 630-750 ℃ for 3.5-5.5 h, cooling to room temperature, and grinding into powder with the particle size of less than 20 mu m to obtain the one-dimensional mesoporous photocatalytic material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810824656.3A CN108993374B (en) | 2018-07-25 | 2018-07-25 | Preparation method of one-dimensional mesoporous photocatalytic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810824656.3A CN108993374B (en) | 2018-07-25 | 2018-07-25 | Preparation method of one-dimensional mesoporous photocatalytic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108993374A CN108993374A (en) | 2018-12-14 |
| CN108993374B true CN108993374B (en) | 2020-12-15 |
Family
ID=64597705
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810824656.3A Active CN108993374B (en) | 2018-07-25 | 2018-07-25 | Preparation method of one-dimensional mesoporous photocatalytic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108993374B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101485979A (en) * | 2009-02-23 | 2009-07-22 | 南开大学 | Preparation of multi-stage structure cerium doped titanium dioxide mesoporous material as well as applications thereof in photocatalysis and CO oxygenation |
| CN105170130A (en) * | 2015-09-02 | 2015-12-23 | 中国科学院新疆理化技术研究所 | Preparation method and application of high-dispersion CeO2 modified TiO2 meso-porous photocatalyst |
| CN105562122A (en) * | 2015-12-15 | 2016-05-11 | 中国科学院上海高等研究院 | Perovskite type core-shell structured metal oxide and preparation method and application thereof |
| CN106179304A (en) * | 2016-07-28 | 2016-12-07 | 南昌航空大学 | A kind of CeO possessing photo catalytic reduction performance2tiO2the preparation method of nano composite material |
| CN106238104A (en) * | 2016-08-30 | 2016-12-21 | 樊之雄 | A kind of photocatalysis composite dye gives up material for water treatment and preparation method thereof |
| CN106362726A (en) * | 2016-09-05 | 2017-02-01 | 上海应用技术大学 | Cerium/neodymium-doped titanium dioxide/carbon hybrid aerogel material, and preparation method and application thereof |
| CN107597092A (en) * | 2017-07-21 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | 3D patterns CeO2/TiO2Preparation method of catalyst |
| CN108246361A (en) * | 2018-01-08 | 2018-07-06 | 沈阳理工大学 | A kind of method for preparing molecular sieve type titanium cerium oxide catalysis material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9522387B2 (en) * | 2012-06-15 | 2016-12-20 | Lawrence Livermore National Security, Llc | Highly active thermally stable nanoporous gold catalyst |
-
2018
- 2018-07-25 CN CN201810824656.3A patent/CN108993374B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101485979A (en) * | 2009-02-23 | 2009-07-22 | 南开大学 | Preparation of multi-stage structure cerium doped titanium dioxide mesoporous material as well as applications thereof in photocatalysis and CO oxygenation |
| CN105170130A (en) * | 2015-09-02 | 2015-12-23 | 中国科学院新疆理化技术研究所 | Preparation method and application of high-dispersion CeO2 modified TiO2 meso-porous photocatalyst |
| CN105562122A (en) * | 2015-12-15 | 2016-05-11 | 中国科学院上海高等研究院 | Perovskite type core-shell structured metal oxide and preparation method and application thereof |
| CN106179304A (en) * | 2016-07-28 | 2016-12-07 | 南昌航空大学 | A kind of CeO possessing photo catalytic reduction performance2tiO2the preparation method of nano composite material |
| CN106238104A (en) * | 2016-08-30 | 2016-12-21 | 樊之雄 | A kind of photocatalysis composite dye gives up material for water treatment and preparation method thereof |
| CN106362726A (en) * | 2016-09-05 | 2017-02-01 | 上海应用技术大学 | Cerium/neodymium-doped titanium dioxide/carbon hybrid aerogel material, and preparation method and application thereof |
| CN107597092A (en) * | 2017-07-21 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | 3D patterns CeO2/TiO2Preparation method of catalyst |
| CN108246361A (en) * | 2018-01-08 | 2018-07-06 | 沈阳理工大学 | A kind of method for preparing molecular sieve type titanium cerium oxide catalysis material |
Non-Patent Citations (3)
| Title |
|---|
| 一维介孔氧化镨纳米材料的合成及其对刚果红的吸附性能研究;王珊珊等;《齐齐哈尔大学学报》;20151130;第31卷(第6期);第61-64页 * |
| 溶剂热合成法制备B 掺杂TiO2光催化剂;张文杰等;《材料热处理学报》;20130630;第34卷;第12-16页 * |
| 钛酸镧纳米材料的水热制备及其光解水性能研究;宋海波等;《2006年全国功能材料学术年会专辑》;20061130;第471-472页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108993374A (en) | 2018-12-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107321341B (en) | diatomite/(GR + TiO)2) Preparation method of composite photocatalyst | |
| CN108654586B (en) | Graphitized mesoporous carbon-TiO2Composite photocatalytic material and preparation method and application thereof | |
| CN108620113B (en) | Preparation method of nitrogen-doped carbon-cerium composite nanosheet | |
| CN108069497B (en) | Method for treating organic wastewater by catalytic wet oxidation | |
| CN105126797A (en) | Honeycomb ceramic-supported nano titanium dioxide photo-catalyst and preparation method of same | |
| CN112892521A (en) | Oxygen-enriched vacancy echinoid tungsten oxide and preparation method and application thereof | |
| CN114797942A (en) | Porous metal (iron, nickel and cobalt) doped graphite phase carbon nitride photocatalyst and preparation method and application thereof | |
| CN108311130B (en) | Gradient-pore macroporous-mesoporous alumina carrier and preparation method thereof | |
| CN114984942B (en) | Catalyst for VOC catalytic combustion and preparation method and application thereof | |
| CN115212869A (en) | CeO preparation based on Ce-MOF precursor 2 /TiO 2 Preparation method of composite thermal catalytic material | |
| CN113680343B (en) | Three-dimensional cubic CeO 2 /Mn 2 O 3 Preparation method and application of composite photo-thermal catalyst | |
| CN108993374B (en) | Preparation method of one-dimensional mesoporous photocatalytic material | |
| KR20140110145A (en) | Complex adsorbent and manufacuring method of complex adsorbent | |
| Castilhos et al. | Assessment comparison of commercial TiO 2 and TiO 2 sol-gel on the degradation of caffeine using artificial radiation | |
| CN113842938A (en) | Novel g-C3N4Method for preparing derived carbonaceous adsorbent and photocatalytic material | |
| CN108435129B (en) | Method for preparing Sr-Ti-In ternary oxide molecular sieve | |
| CN111001433A (en) | Mesoporous zeolite loaded with palladium-copper alloy nanoparticles and preparation method and application thereof | |
| CN108502898B (en) | A method of preparing titanium germanium molecular sieve | |
| CN114749151A (en) | Formaldehyde adsorbent for air purification and preparation method and application thereof | |
| CN109399726B (en) | Preparation method of iron lanthanum oxide molecular sieve type purification material | |
| CN109012650B (en) | Preparation method of rare earth porcelain sand purification material | |
| CN106563415A (en) | Method for preparing MIL-100Al-based porous carbon material for carbon dioxide adsorption and separation | |
| CN112755953A (en) | Adsorbent for removing nitrogen oxide in fluid, preparation method and application | |
| CN109439331B (en) | Preparation method of material for soil pollution treatment | |
| CN108837806B (en) | Preparation method of water treatment ceramsite filter material |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221020 Address after: 230000 Woye Garden Commercial Building B-1017, 81 Ganquan Road, Shushan District, Hefei City, Anhui Province Patentee after: HEFEI JINGLONG ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Address before: 110159 No. 6 Nanping Road, Hunnan New District, Shenyang, Liaoning Patentee before: SHENYANG LIGONG University |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240914 Address after: No. 69-7-1, 1st Floor, Courtyard 69-7-1, Linxiao Road, Huangcun Town, Daxing District, Beijing 102611 Patentee after: Guangzhishui (Beijing) Environmental Protection Co.,Ltd. Country or region after: China Address before: 230000 Woye Garden Commercial Building B-1017, 81 Ganquan Road, Shushan District, Hefei City, Anhui Province Patentee before: HEFEI JINGLONG ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Country or region before: China |