CN108479775A - A kind of TiO2/Fe3O4The preparation method and application of loaded photocatalyst - Google Patents
A kind of TiO2/Fe3O4The preparation method and application of loaded photocatalyst Download PDFInfo
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- CN108479775A CN108479775A CN201810045396.XA CN201810045396A CN108479775A CN 108479775 A CN108479775 A CN 108479775A CN 201810045396 A CN201810045396 A CN 201810045396A CN 108479775 A CN108479775 A CN 108479775A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 17
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012153 distilled water Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003483 aging Methods 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 230000001699 photocatalysis Effects 0.000 claims abstract description 9
- 238000006237 Beckmann rearrangement reaction Methods 0.000 claims abstract description 7
- 150000001408 amides Chemical class 0.000 claims abstract description 6
- 238000007146 photocatalysis Methods 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 125000001931 aliphatic group Chemical group 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims 1
- 238000003980 solgel method Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000002253 acid Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- -1 Amides compound Chemical class 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- DLNKOYKMWOXYQA-APPZFPTMSA-N phenylpropanolamine Chemical compound C[C@@H](N)[C@H](O)C1=CC=CC=C1 DLNKOYKMWOXYQA-APPZFPTMSA-N 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J37/08—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B43/00—Formation or introduction of functional groups containing nitrogen
- C07B43/06—Formation or introduction of functional groups containing nitrogen of amide groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/10—Preparation of carboxylic acid amides from compounds not provided for in groups C07C231/02 - C07C231/08
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Dispersion Chemistry (AREA)
- Catalysts (AREA)
Abstract
A kind of TiO2/Fe3O4The preparation method and application of loaded photocatalyst, the preparation method prepare TiO using sol-gal process2/Fe3O4Compound specifically comprises the following steps:a)The preparation of solution A:The absolute ethyl alcohol of 1 mass parts is added in the distilled water of 3 mass parts, the Fe of 0.1 mass parts is added3O4, ultrasonic disperse, adjusting pH >=3 obtain A liquid;b)The preparation of B solution:Take 6 mass parts of butyl titanate in being vigorously stirred down in the absolute ethyl alcohol for being slowly added into 8 mass parts;c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues to stir 1h, 75 DEG C of agings obtain grey gel, continue freeze-day with constant temperature, are washed repeatedly with distilled water until pH=6.8, and TiO is made after 500 DEG C of calcinings2/Fe3O4Loaded catalyst;The TiO2/Fe3O4Loaded catalyst reacts synthesizing amide class compound for photocatalysis ketoxime Beckmann rearrangement.
Description
Technical field
The present invention relates to a kind of TiO2/Fe3O4The preparation method and application of loaded photocatalyst, belongs to catalyst
Preparing technical field.
Background technology
Amides compound can synthetic antibacterial agents, agrochemical, have broad application prospects.
Traditional Beckmann is reset(Ketoxime occurs to reset the reaction for generating N- hydrocarbyl amides in acid condition)It is used
Catalyst be mainly PCl5, H2SO4, PPA and metal oxide etc., these traditional catalyst system and catalyzings generate a large amount of acid
Waste water, it is seriously polluted.In recent years, as people's environmentally friendly, the attention degree of conservation-minded society increase, chemists
The reaction condition that begins one's study is mild, and operating process is easy, the environment amenable novel B eckmann that can be used for sustainable development
Rearrangement catalyst.The rapid development of Green Chemistry is but also the research that Beckmann is reset initially enters second stage, at this
Occur many high conversion rates, good, the environment amenable new catalyst of selectivity in stage.
Invention content
It is an object of the invention to overcome the shortcomings of the prior art, and provide a kind of amide yield it is higher, reaction item
Part is mild, catalyst easily recycles, and reusable TiO2/Fe3O4The preparation method and application of loaded photocatalyst.
The purpose of the present invention is by following technical solution to complete, a kind of TiO2/Fe3O4Loaded photocatalyst
Preparation method, the preparation method prepare TiO using sol-gal process2/Fe3O4Compound specifically comprises the following steps:
a)The preparation of solution A:The absolute ethyl alcohol of 1-5 mass parts is added in the distilled water of 3-7 mass parts, 0.1-1 matter is added
Measure the Fe of part3O4, ultrasonic disperse, adjusting pH >=3 obtain A liquid;
b)The preparation of B solution:6-10 mass parts of butyl titanate are taken to be slowly added into 8-12 mass parts in being vigorously stirred down
In absolute ethyl alcohol;
c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues 1-3h of stirring, it is solidifying that 75-85 DEG C of agings obtain grey
Glue continues freeze-day with constant temperature, is washed with distilled water and is made after pH=6.8-7.2,500-600 DEG C of 1.5-2.5h of calcining repeatedly
TiO2/Fe3O4Loaded catalyst.
As preferred:The step a)In, 3 mass parts absolute ethyl alcohols are added in 5 mass parts distilled water, are added 0.5
Mass parts Fe3O4, ultrasonic disperse, adjusting pH >=3 obtain A liquid;
The step b)In, take 8 mass parts of butyl titanate to be slowly added into 10 mass parts absolute ethyl alcohols in being vigorously stirred down
In;
The step c)In, solution A is slowly added dropwise in the B solution being vigorously stirred, continues to stir 2h, 80 DEG C of agings obtain grey
Color gel continues freeze-day with constant temperature, is washed repeatedly with distilled water until pH=7.0, and TiO is made after 550 DEG C of calcining 2h2/Fe3O4Load
Type catalyst.
As preferred:The TiO2/Fe3O4TiO in loaded catalyst2For Detitanium-ore-type, the TiO2/
Fe3O4Photocatalytic activity can be improved in loaded catalyst with doped metal ion.
A kind of TiO as described above2/Fe3O4The application of loaded photocatalyst, the TiO2/Fe3O4Loaded catalyst
Synthesizing amide class compound, the photocatalysis Beckmann rearrangement reactions bottom are reacted for photocatalysis ketoxime Beckmann rearrangement
Object can be aromatic series ketoxime, aliphatic ketoxime or aromatic series and aliphatic mixing ketoxime.
As preferred:The light-catalyzed reaction optimal conditions is:PH=3.0, V (H2O2):N(Substrate)=2.5
ML/1 mmol, N (Catalyst):N(Substrate)=1:100,60 DEG C of reaction temperature.
TiO prepared by the present invention2/Fe3O4Support type photocatalytic system, have amide yield is higher, reaction condition is mild,
The features such as catalyst easily recycles, and reusable is a kind of ideal catalyst.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be described in detail:A kind of TiO of the present invention2/Fe3O4It is negative
The preparation method of load type photochemical catalyst, the preparation method prepare TiO using sol-gal process2/Fe3O4Compound, it is specific to wrap
Include following steps:
a)The preparation of solution A:The absolute ethyl alcohol of 1-5 mass parts is added in the distilled water of 3-7 mass parts, 0.1-1 matter is added
Measure the Fe of part3O4, ultrasonic disperse, adjusting pH >=3 obtain A liquid;
b)The preparation of B solution:6-10 mass parts of butyl titanate are taken to be slowly added into 8-12 mass parts in being vigorously stirred down
In absolute ethyl alcohol;
c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues 1-3h of stirring, it is solidifying that 75-85 DEG C of agings obtain grey
Glue continues freeze-day with constant temperature, is washed with distilled water and is made after pH=6.8-7.2,500-600 DEG C of 1.5-2.5h of calcining repeatedly
TiO2/Fe3O4Loaded catalyst.
TiO of the present invention2/Fe3O4TiO in loaded catalyst2For Detitanium-ore-type, the TiO2/Fe3O4It is negative
Photocatalytic activity can be improved in supported catalyst with doped metal ion.
Embodiment 1:A kind of TiO of the present invention2/Fe3O4The preparation method of loaded photocatalyst, the preparation
Method prepares TiO using sol-gal process2/Fe3O4Compound specifically comprises the following steps:
a)The preparation of solution A:3 mass parts absolute ethyl alcohols are added in 5 mass parts distilled water, 0.5 mass parts Fe is added3O4, surpass
Sound disperses, and adjusts pH >=3, obtains A liquid;
b)The preparation of B solution:8 mass parts of butyl titanate are taken to be slowly added into 10 mass parts absolute ethyl alcohols in being vigorously stirred down
In;
c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues to stir 2h, 80 DEG C of agings obtain grey gel, continue permanent
Temperature is dry, is washed repeatedly with distilled water until pH=7.0, and TiO is made after 550 DEG C of calcining 2h2/Fe3O4Loaded catalyst.
Embodiment 2:A kind of TiO of the present invention2/Fe3O4The preparation method of loaded photocatalyst, the preparation
Method prepares TiO using sol-gal process2/Fe3O4Compound specifically comprises the following steps:
a)The preparation of solution A:The absolute ethyl alcohol of 1-5 mass parts is added in the distilled water of 3-7 mass parts, 0.1-1 matter is added
Measure the Fe of part3O4, ultrasonic disperse, adjusting pH >=3 obtain A liquid;
b)The preparation of B solution:6-10 mass parts of butyl titanate are taken to be slowly added into 8-12 mass parts in being vigorously stirred down
In absolute ethyl alcohol;
c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues 1-3h of stirring, it is solidifying that 75-85 DEG C of agings obtain grey
Glue continues freeze-day with constant temperature, is washed with distilled water and is made after pH=6.8-7.2,500-600 DEG C of 1.5-2.5h of calcining repeatedly
TiO2/Fe3O4Loaded catalyst.
Embodiment 3:A kind of TiO of the present invention2/Fe3O4The preparation method of loaded photocatalyst, the preparation
Method prepares TiO using sol-gal process2/Fe3O4Compound specifically comprises the following steps:
a)The preparation of solution A:The absolute ethyl alcohol of 1-5 mass parts is added in the distilled water of 3-7 mass parts, 0.1-1 matter is added
Measure the Fe of part3O4, ultrasonic disperse, adjusting pH >=3 obtain A liquid;
b)The preparation of B solution:6-10 mass parts of butyl titanate are taken to be slowly added into 8-12 mass parts in being vigorously stirred down
In absolute ethyl alcohol;
c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues 1-3h of stirring, it is solidifying that 75-85 DEG C of agings obtain grey
Glue continues freeze-day with constant temperature, is washed with distilled water and is made after pH=6.8-7.2,500-600 DEG C of 1.5-2.5h of calcining repeatedly
TiO2/Fe3O4Loaded catalyst.
Embodiment 4:A kind of TiO of the present invention2/Fe3O4The preparation method of loaded photocatalyst, the preparation
Method prepares TiO using sol-gal process2/Fe3O4Compound specifically comprises the following steps:
a)The preparation of solution A:3mL absolute ethyl alcohols are added in 5 mL distilled water, 0.5gFe is added3O4, ultrasonic disperse, adjusting pH
>=3, obtain A liquid;
b)The preparation of B solution:Butyl titanate 8mL is taken to be slowly added into 10mL absolute ethyl alcohols in being vigorously stirred down;
c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues to stir 2h, 80 DEG C of agings obtain grey gel, continue permanent
Temperature is dry, is washed repeatedly with distilled water until pH=7.0, and after 550 DEG C of calcining 2h, TiO2/Fe3O4 loaded catalysts are made.
A kind of TiO2/Fe3O4The application of loaded photocatalyst, the TiO2/Fe3O4Loaded catalyst is urged for light
Change ketoxime Beckmann rearrangement and react synthesizing amide class compound, the photocatalysis Beckmann rearrangement reactions substrate can be
Aromatic series ketoxime, aliphatic ketoxime or aromatic series and aliphatic mix ketoxime.
Light-catalyzed reaction optimal conditions of the present invention is:PH=3.0, V (H2O2):N(Substrate)=2.5 mL/1
Mmol, N (Catalyst):N(Substrate)=1:100,60 DEG C of reaction temperature.
Claims (5)
1. a kind of TiO2/Fe3O4The preparation method of loaded photocatalyst, it is characterised in that the preparation method uses colloidal sol
Gel method prepares TiO2/Fe3O4Compound specifically comprises the following steps:
a)The preparation of solution A:The absolute ethyl alcohol of 1-5 mass parts is added in the distilled water of 3-7 mass parts, 0.1-1 matter is added
Measure the Fe of part3O4, ultrasonic disperse, adjusting pH >=3 obtain A liquid;
b)The preparation of B solution:6-10 mass parts of butyl titanate are taken to be slowly added into 8-12 mass parts in being vigorously stirred down
In absolute ethyl alcohol;
c)Solution A is slowly added dropwise in the B solution being vigorously stirred, continues 1-3h of stirring, it is solidifying that 75-85 DEG C of agings obtain grey
Glue continues freeze-day with constant temperature, is washed with distilled water and is made after pH=6.8-7.2,500-600 DEG C of 1.5-2.5h of calcining repeatedly
TiO2/Fe3O4Loaded catalyst.
2. TiO according to claim 12/Fe3O4The preparation method of loaded photocatalyst, it is characterised in that:
The step a)In, 3 mass parts absolute ethyl alcohols are added in 5 mass parts distilled water, 0.5 mass parts Fe is added3O4, surpass
Sound disperses, and adjusts pH >=3, obtains A liquid;
The step b)In, take 8 mass parts of butyl titanate to be slowly added into 10 mass parts absolute ethyl alcohols in being vigorously stirred down
In;
The step c)In, solution A is slowly added dropwise in the B solution being vigorously stirred, continues to stir 2h, 80 DEG C of agings obtain grey
Color gel continues freeze-day with constant temperature, is washed repeatedly with distilled water until pH=7.0, and TiO is made after 550 DEG C of calcining 2h2/Fe3O4Load
Type catalyst.
3. TiO according to claim 1 or 22/Fe3O4The preparation method of loaded photocatalyst, it is characterised in that described
TiO2/Fe3O4TiO in loaded catalyst2For Detitanium-ore-type, the TiO2/Fe3O4It can be mixed in loaded catalyst
Miscellaneous metal ion improves photocatalytic activity.
4. one kind TiO as described in claims 1 or 2 or 32/Fe3O4The application of loaded photocatalyst, it is characterised in that described
TiO2/Fe3O4Loaded catalyst reacts synthesizing amide class compound, the light for photocatalysis ketoxime Beckmann rearrangement
Catalytic Beckmann rearrangement reaction substrate can be aromatic series ketoxime, aliphatic ketoxime or aromatic series and aliphatic mixing ketoxime.
5. TiO according to claim 42/Fe3O4The application of loaded photocatalyst, it is characterised in that the photocatalysis is anti-
The optimal conditions is answered to be:PH=3.0, V (H2O2):N (Substrate)=2.5 mL/1 mmol, N (Catalyst):N
(Substrate)=1:100,60 DEG C of reaction temperature.
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101816937A (en) * | 2009-07-29 | 2010-09-01 | 兰州理工大学 | Method for manufacturing magnetic loading type nanometer catalyst TiO2/Fe2O4 |
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2018
- 2018-01-17 CN CN201810045396.XA patent/CN108479775A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101816937A (en) * | 2009-07-29 | 2010-09-01 | 兰州理工大学 | Method for manufacturing magnetic loading type nanometer catalyst TiO2/Fe2O4 |
Non-Patent Citations (2)
Title |
---|
HASHEM SHARGHI等: "Titanium oxide (TiO2) catalysed one-Step Beckmann rearrangement of aldehydes and ketones in solvent free conditions", 《J. CHEM. RESEARCH (S)》 * |
栾江月等: "Fe3O4-TiO2磁性光催化剂的制备与性能", 《大连工业大学学报》 * |
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Application publication date: 20180904 |