CN106186052A - A kind of preparation method of macropore hollow Cerium titanate microsphere - Google Patents
A kind of preparation method of macropore hollow Cerium titanate microsphere Download PDFInfo
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- CN106186052A CN106186052A CN201610577086.3A CN201610577086A CN106186052A CN 106186052 A CN106186052 A CN 106186052A CN 201610577086 A CN201610577086 A CN 201610577086A CN 106186052 A CN106186052 A CN 106186052A
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- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 53
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 53
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000004005 microsphere Substances 0.000 title claims abstract description 24
- 239000012065 filter cake Substances 0.000 claims abstract description 36
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 26
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N isopropyl alcohol Natural products CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 8
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 8
- 239000008103 glucose Substances 0.000 claims abstract description 8
- 239000003381 stabilizer Substances 0.000 claims abstract description 8
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 56
- 238000005485 electric heating Methods 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- 239000004744 fabric Substances 0.000 claims description 14
- 239000004570 mortar (masonry) Substances 0.000 claims description 14
- 229910052573 porcelain Inorganic materials 0.000 claims description 14
- 230000001105 regulatory effect Effects 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 239000010959 steel Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000003760 magnetic stirring Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 7
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 239000008399 tap water Substances 0.000 claims description 7
- 235000020679 tap water Nutrition 0.000 claims description 7
- 230000005619 thermoelectricity Effects 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 2
- 238000011001 backwashing Methods 0.000 claims 2
- 239000006227 byproduct Substances 0.000 claims 2
- 239000002202 Polyethylene glycol Substances 0.000 claims 1
- 239000002826 coolant Substances 0.000 claims 1
- 229920001223 polyethylene glycol Polymers 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 229920002538 Polyethylene Glycol 20000 Polymers 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- -1 isopropyl alcohol ester Chemical class 0.000 abstract 1
- 238000004506 ultrasonic cleaning Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 5
- 238000000746 purification Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011796 hollow space material Substances 0.000 description 3
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 3
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- GMVLGJDMPCRIJK-CGZBRXJRSA-N benzyl n-[(2s)-1-[(3-hydroxyoxan-4-yl)amino]-4-methyl-1-oxopentan-2-yl]carbamate Chemical class N([C@@H](CC(C)C)C(=O)NC1C(COCC1)O)C(=O)OCC1=CC=CC=C1 GMVLGJDMPCRIJK-CGZBRXJRSA-N 0.000 description 1
- SEGBQNJGOCXIGC-FHERZECASA-N benzyl n-[(2s)-1-[(4-hydroxyoxolan-3-yl)amino]-4-methyl-1-oxopentan-2-yl]carbamate Chemical class N([C@@H](CC(C)C)C(=O)NC1C(COC1)O)C(=O)OCC1=CC=CC=C1 SEGBQNJGOCXIGC-FHERZECASA-N 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/12—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of actinides
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/651—50-500 nm
-
- 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
- B01J35/653—500-1000 nm
-
- 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
- B01J35/657—Pore diameter larger than 1000 nm
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The preparation method of a kind of macropore hollow Cerium titanate microsphere, prepares template presoma: prepare with n-butyl alcohol, glucose solution, PEG 20000, Dodecyl trimethyl ammonium chloride and stabilizer SY 5；Hydrothermal Synthesis macropore template: by template presoma 180 ~ 200 DEG C be incubated 36h, sonicated, filter, be dried prepare；Cerium titanate presoma: include metatitanic acid isopropyl alcohol ester, dehydrated alcohol, acetone and directed agents AP 3；Hydrothermal Synthesis Cerium titanate: Cerium titanate presoma is incubated 72h at 220 ~ 240 DEG C, then through ultrasonic cleaning, filtration and dry run；Heat treatment: filter cake is calcined 3 ~ 6h at 1200 ~ 1350 DEG C, grinds and get final product.Preparation process condition has operability, and product particle size is uniform, shape is complete, and product photocatalytic activity is high and stable.
Description
Technical field
The invention belongs to environmental purification function Material Field, be specifically related to the preparation side of a kind of macropore hollow Cerium titanate microsphere
Method.
Background technology
Large pore material (Macroporous materials) aperture is more than 50 nm.Pore structure in large pore material can become
The passage of pore passage structure is entered for adsorption molecule.Large pore material have specific surface area compared with big, density is low, low-refraction and heat
The features such as the coefficient of expansion is relatively low so that macropore hollow material is widely used in catalyst carrier, radioprotective skin-material, chargeable
Battery etc..Macropore hollow material has unique excellent photocatalysis property, is not only due to the specific surface area increased, hollow simultaneously
Structure can stablize its active center.In hollow shell structure particles, its internal pore passage structure gap provides a large amount of suitable
Space is used for catalytic reaction.
Cerium titanate is a kind of titanate material with particular advantages, by the extensive concern of all circles it is considered to be one
The environmental pollution purification type catalysis material of great development prospect.Although powder body Cerium titanate has higher purification activity, but urges
The recycling of agent becomes people's issues that need special attention in actual application.Nano-powder Cerium titanate photocatalyst is used for disappearing
During except water pollutant, there is catalyst recovery difficulty, catalyst easily inactivates, need dependence power stirring to maintain catalyst
The shortcoming such as suspension.Novel nano structure catalyst such as nanometer macropore tiny balloon etc. has the characteristic of low-density, high-ratio surface,
The difference of condition can be used to make catalyst be prone to from solution separate according to catalyst simultaneously.Macropore hollow material is as one
Novel environmental purification function material has broad application prospects.This patent discloses the system of a kind of macropore hollow Cerium titanate microsphere
Preparation Method.
Summary of the invention
The problem existed for prior art, it is desirable to provide the preparation side of a kind of macropore hollow Cerium titanate microsphere
Method.
The technical solution used in the present invention is:
A kind of preparation method of macropore hollow Cerium titanate microsphere, including following processing step:
1, preparation template presoma
By 30 ~ 40 mL n-butyl alcohol, glucose solution 18 ~ 25 mL of 3 mol/L, 5.6 ~ 7.5 g PEG 20000s, 1.5 ~
2.7 mL Dodecyl trimethyl ammonium chloride and 0.5 ~ 1.2 g stabilizer SY-5 add in 100 mL twoport round-bottomed flasks；
Being placed in by flask in precise temperature control electric heating bag, in flask center, interface installs spherical condensation tube, is situated between with tap water for cooling
Matter, installs thermometric thermoelectricity corner at another interface of flask.By regulation electric heating bag heating-up temperature to control solution temperature in flask it is
60 DEG C, maintain the reflux for time 50 min in this temperature, be then cooled to room temperature, standby.
2, Hydrothermal Synthesis macropore template
The template presoma of preparation is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 100 mL, covers
Lid, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 180 ~ 200 DEG C, insulation
36 h；In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 90 DEG C, is dried 6 h, then clays into power in agate mortar, standby
With.
3, prepared by Cerium titanate presoma
5.2 ~ 6.3 mL metatitanic acid isopropyl alcohol esters, 30 ~ 35 mL dehydrated alcohol, 12 ~ 14 mL it are separately added in 100 mL beakers
Acetone and 1.2 ~ 1.3 g directed agents AP-3, stir 20 min, as A liquid on magnetic stirring apparatus；
500 mg macropore templates, 3.6 g Surfactant OP-3 and 30 mL dehydrated alcohol are added, at magnetic in 200 mL beakers
20 min are stirred, as B liquid on power agitator；
A drop is added in B liquid and continuously stirred 30 min during magnetic agitation, by mixed liquor in ultrasonic cleaner
With 45 MHz frequency supersound process 1 h, standby.
4, Hydrothermal Synthesis Cerium titanate
Cerium titanate presoma is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 200 mL, closes the lid
Son, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 220 ~ 240 DEG C, insulation
72 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 120 DEG C, is dried 6 h, standby.
5, heat treatment
Filter cake is put in porcelain crucible and be placed in program control cabinet-type electric furnace, with 10 DEG C/min heating rate, furnace temperature is risen to
1200 ~ 1350 DEG C, at this temperature calcination 3 ~ 6 h.Take out after electric furnace is cooled to room temperature, grind in porcelain mortar and prepare macropore
Hollow Cerium titanate microsphere.
Compared with prior art, it is an advantage of the current invention that:
1, the invention provides a kind of method preparing new macroporous hollow Cerium titanate microsphere, the key technology of the method is to system
Standby technique and the reasonably optimizing of composition of raw materials；
2, the solvent during the present invention reasonably have selected macropore template and Cerium titanate precursor solution and key component, to preparation work
The selection of skill procedure parameter also fully takes into account stability and the needs of activity of prepared material；
3, the preparation process condition that the present invention provides has operability, and product particle size is uniform, shape is complete, and product light is urged
Change activity high and stable.
Detailed description of the invention
Embodiment 1
A kind of preparation method of macropore hollow Cerium titanate microsphere, including following processing step:
Step 1: preparation template presoma
By 32 mL n-butyl alcohol, glucose solution 18 mL of 3 mol/L, 5.6 g PEG 20000s, 1.6 mL dodecyls
Trimethylammonium bromide and 0.7 g stabilizer SY-5 add in 100 mL twoport round-bottomed flasks；
Being placed in by flask in precise temperature control electric heating bag, in flask center, interface installs spherical condensation tube, is situated between with tap water for cooling
Matter, installs thermometric thermoelectricity corner at another interface of flask；By regulation electric heating bag heating-up temperature to control solution temperature in flask it is
60 DEG C, maintain the reflux for time 50 min in this temperature, be then cooled to room temperature, standby.
Step 2: Hydrothermal Synthesis macropore template
The template presoma of preparation is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 100 mL, covers
Lid, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 180 ~ 200 DEG C, insulation
36 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 90 DEG C, is dried 6 h, then clays into power in agate mortar, standby
With.
Step 3: prepared by Cerium titanate presoma
5.3 mL metatitanic acid isopropyl alcohol esters, 30 mL dehydrated alcohol, 12 mL acetone and 1.2 g it are separately added in 100 mL beakers
Directed agents AP-3, stirs 20 min on magnetic stirring apparatus, as A liquid；
500 mg macropore templates, 3.6 g Surfactant OP-3 and 30 mL dehydrated alcohol are added, at magnetic in 200 mL beakers
20 min are stirred, as B liquid on power agitator；
A drop is added in B liquid and continuously stirred 30 min during magnetic agitation, by mixed liquor in ultrasonic cleaner
With 45 MHz frequency supersound process 1 h, standby.
Step 4: Hydrothermal Synthesis Cerium titanate
Cerium titanate presoma is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 200 mL, closes the lid
Son, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 220 ~ 240 DEG C, insulation
72 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 120 DEG C, is dried 6 h, standby.
Step 5: heat treatment
Filter cake is put in porcelain crucible and be placed in program control cabinet-type electric furnace, with 10 DEG C/min heating rate, furnace temperature is risen to
1200 DEG C, at this temperature calcination 5 h.Take out after electric furnace is cooled to room temperature, grind in porcelain mortar and prepare the hollow metatitanic acid of macropore
Cerium microsphere.
The rotating speed of the magnetic stirring apparatus related in the present embodiment is 200 r/min.
Embodiment 2
A kind of preparation method of macropore hollow Cerium titanate microsphere, including following processing step:
Step 1: preparation template presoma
By 35 mL n-butyl alcohol, glucose solution 21 mL of 3 mol/L, 6 g PEG 20000s, 1.9 mL dodecyls three
Methyl bromide ammonium and 0.7 g stabilizer SY-5 add in 100 mL twoport round-bottomed flasks；
Being placed in by flask in precise temperature control electric heating bag, in flask center, interface installs spherical condensation tube, is situated between with tap water for cooling
Matter, installs thermometric thermoelectricity corner at another interface of flask.By regulation electric heating bag heating-up temperature to control solution temperature in flask it is
60 DEG C, maintain the reflux for time 50 min in this temperature, be then cooled to room temperature, standby.
Step 2: Hydrothermal Synthesis macropore template
The template presoma of preparation is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 100 mL, covers
Lid, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 180 ~ 200 DEG C, insulation
36 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 90 DEG C, is dried 6 h, then clays into power in agate mortar, standby
With.
Step 3: prepared by Cerium titanate presoma
5.8 mL metatitanic acid isopropyl alcohol esters, 32 mL dehydrated alcohol, 12 mL acetone and 1.2 g it are separately added in 100 mL beakers
Directed agents AP-3, stirs 20 min on magnetic stirring apparatus, as A liquid；
500 mg macropore templates, 3.6 g Surfactant OP-3 and 30 mL dehydrated alcohol are added, at magnetic in 200 mL beakers
20 min are stirred, as B liquid on power agitator；
A drop is added in B liquid and continuously stirred 30 min during magnetic agitation, by mixed liquor in ultrasonic cleaner
With 45 MHz frequency supersound process 1 h, standby.
Step 4: Hydrothermal Synthesis Cerium titanate
Cerium titanate presoma is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 200 mL, closes the lid
Son, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 220 ~ 240 DEG C, insulation
72 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 120 DEG C, is dried 6 h, standby.
Step 5: heat treatment
Filter cake is put in porcelain crucible and be placed in program control cabinet-type electric furnace, with 10 DEG C/min heating rate, furnace temperature is risen to
1260 DEG C, at this temperature calcination 5 h.Take out after electric furnace is cooled to room temperature, grind in porcelain mortar and prepare the hollow metatitanic acid of macropore
Cerium microsphere.
The rotating speed of the magnetic stirring apparatus related in the present embodiment is 200 r/min.
Embodiment 3
A kind of preparation method of macropore hollow Cerium titanate microsphere, including following processing step:
Step 1: preparation template presoma
By 38 mL n-butyl alcohol, glucose solution 25 mL of 3 mol/L, 7.3 g PEG 20000s, 2.5 mL dodecyls
Trimethylammonium bromide and 1.1 g stabilizer SY-5 add in 100 mL twoport round-bottomed flasks；
Being placed in by flask in precise temperature control electric heating bag, in flask center, interface installs spherical condensation tube, is situated between with tap water for cooling
Matter, installs thermometric thermoelectricity corner at another interface of flask.By regulation electric heating bag heating-up temperature to control solution temperature in flask it is
60 DEG C, maintain the reflux for time 50 min in this temperature, be then cooled to room temperature, standby.
Step 2: Hydrothermal Synthesis macropore template
The template presoma of preparation is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 100 mL, covers
Lid, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 180 ~ 200 DEG C, insulation
36 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 90 DEG C, is dried 6 h, then clays into power in agate mortar, standby
With.
Step 3: prepared by Cerium titanate presoma
In 100 mL beakers, it is separately added into 6 mL metatitanic acid isopropyl alcohol esters, 35 mL dehydrated alcohol, 13 mL acetone and 1.2 g lead
To agent AP-3, magnetic stirring apparatus stirs 20 min, as A liquid；
500 mg macropore templates, 3.6 g Surfactant OP-3 and 30 mL dehydrated alcohol are added, at magnetic in 200 mL beakers
20 min are stirred, as B liquid on power agitator；
A drop is added in B liquid and continuously stirred 30 min during magnetic agitation, by mixed liquor in ultrasonic cleaner
With 45 MHz frequency supersound process 1 h, standby.
Step 4: Hydrothermal Synthesis Cerium titanate
Cerium titanate presoma is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 200 mL, closes the lid
Son, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 220 ~ 240 DEG C, insulation
72 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 120 DEG C, is dried 6 h, standby.
Step 5: heat treatment
Filter cake is put in porcelain crucible and be placed in program control cabinet-type electric furnace, with 10 DEG C/min heating rate, furnace temperature is risen to
1300 DEG C, at this temperature calcination 5 h.Take out after electric furnace is cooled to room temperature, grind in porcelain mortar and prepare the hollow metatitanic acid of macropore
Cerium microsphere.
The rotating speed of the magnetic stirring apparatus related in the present embodiment is 200 r/min.
Embodiment 4
A kind of preparation method of macropore hollow Cerium titanate microsphere, including following processing step:
Step 1: preparation template presoma
By 30 mL n-butyl alcohol, glucose solution 19 mL of 3 mol/L, 5.6 g PEG 20000s, 1.5 mL dodecyls
Trimethylammonium bromide and 0.5 g stabilizer SY-5 add in 100 mL twoport round-bottomed flasks；
Being placed in by flask in precise temperature control electric heating bag, in flask center, interface installs spherical condensation tube, is situated between with tap water for cooling
Matter, installs thermometric thermoelectricity corner at another interface of flask；By regulation electric heating bag heating-up temperature to control solution temperature in flask it is
60 DEG C, maintain the reflux for time 50 min in this temperature, be then cooled to room temperature, standby.
Step 2: Hydrothermal Synthesis macropore template
The template presoma of preparation is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 100 mL, covers
Lid, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 180 ~ 200 DEG C, insulation
36 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 90 DEG C, is dried 6 h, then clays into power in agate mortar, standby
With.
Step 3: prepared by Cerium titanate presoma
5.2 mL metatitanic acid isopropyl alcohol esters, 30 mL dehydrated alcohol, 12 mL acetone and 1.25 it are separately added in 100 mL beakers
G directed agents AP-3, stirs 20 min on magnetic stirring apparatus, as A liquid；
500 mg macropore templates, 3.6 g Surfactant OP-3 and 30 mL dehydrated alcohol are added, at magnetic in 200 mL beakers
20 min are stirred, as B liquid on power agitator；
A drop is added in B liquid and continuously stirred 30 min during magnetic agitation, by mixed liquor in ultrasonic cleaner
With 45 MHz frequency supersound process 1 h, standby.
Step 4: Hydrothermal Synthesis Cerium titanate
Cerium titanate presoma is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 200 mL, closes the lid
Son, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 220 ~ 240 DEG C, insulation
72 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 120 DEG C, is dried 6 h, standby.
Step 5: heat treatment
Filter cake is put in porcelain crucible and be placed in program control cabinet-type electric furnace, with 10 DEG C/min heating rate, furnace temperature is risen to
1200 DEG C, at this temperature calcination 6 h.Take out after electric furnace is cooled to room temperature, grind in porcelain mortar and prepare the hollow metatitanic acid of macropore
Cerium microsphere.
The rotating speed of the magnetic stirring apparatus related in the present embodiment is 200 r/min.
Embodiment 5
A kind of preparation method of macropore hollow Cerium titanate microsphere, including following processing step:
Step 1: preparation template presoma
By 40 mL n-butyl alcohol, glucose solution 18 mL of 3 mol/L, 7.5 g PEG 20000s, 2.7mL dodecyl three
Methyl bromide ammonium and 1.2 g stabilizer SY-5 add in 100 mL twoport round-bottomed flasks；
Being placed in by flask in precise temperature control electric heating bag, in flask center, interface installs spherical condensation tube, is situated between with tap water for cooling
Matter, installs thermometric thermoelectricity corner at another interface of flask；By regulation electric heating bag heating-up temperature to control solution temperature in flask it is
60 DEG C, maintain the reflux for time 50 min in this temperature, be then cooled to room temperature, standby.
Step 2: Hydrothermal Synthesis macropore template
The template presoma of preparation is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 100 mL, covers
Lid, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 180 ~ 200 DEG C, insulation
36 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 90 DEG C, is dried 6 h, then clays into power in agate mortar, standby
With.
Step 3: prepared by Cerium titanate presoma
6.3 mL metatitanic acid isopropyl alcohol esters, 35 mL dehydrated alcohol, 14 mL acetone and 1.3g it are separately added in 100 mL beakers
Directed agents AP-3, stirs 20 min on magnetic stirring apparatus, as A liquid；
500 mg macropore templates, 3.6 g Surfactant OP-3 and 30 mL dehydrated alcohol are added, at magnetic in 200 mL beakers
20 min are stirred, as B liquid on power agitator；
A drop is added in B liquid and continuously stirred 30 min during magnetic agitation, by mixed liquor in ultrasonic cleaner
With 45 MHz frequency supersound process 1 h, standby.
Step 4: Hydrothermal Synthesis Cerium titanate
Cerium titanate presoma is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 200 mL, closes the lid
Son, is placed in rustless steel autoclave；
Autoclave is put in constant temperature electric heating drying baker, constant temperature electric heating drying baker temperature is risen to 220 ~ 240 DEG C, insulation
72 h.In the process, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa；
After device is cooled to room temperature, product is transferred in 200 mL beakers, with 45 MHz frequency in ultrasonic cleaner
Supersound process 20 minutes；
By gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times, then with dehydrated alcohol cyclic washing 3
Secondary, obtain solid filter cake；
Filter cake is placed in constant temperature electric heating drying baker, at 120 DEG C, is dried 6 h, standby.
Step 5: heat treatment
Filter cake is put in porcelain crucible and be placed in program control cabinet-type electric furnace, with 10 DEG C/min heating rate, furnace temperature is risen to
1350 DEG C, at this temperature calcination 3 h.Take out after electric furnace is cooled to room temperature, grind in porcelain mortar and prepare the hollow metatitanic acid of macropore
Cerium microsphere.
The rotating speed of the magnetic stirring apparatus related in the present embodiment is 200 r/min.
Claims (4)
1. the preparation method of a macropore hollow Cerium titanate microsphere, it is characterised in that include following processing step:
Step 1: preparation template presoma；
Step 1.1: by 30 ~ 40 mL n-butyl alcohol, glucose solution 18 ~ 25 mL of 3 mol/L, 5.6 ~ 7.5 g Polyethylene Glycol
20000,1.5 ~ 2.7 mL Dodecyl trimethyl ammonium chloride and 0.5 ~ 1.2 g stabilizer SY-5 add 100 mL twoport round bottoms burnings
In Ping；
Step 1.2: be placed in by flask in precise temperature control electric heating bag, in flask center, interface installs spherical condensation tube, with tap water
For cooling medium, at another interface of flask, thermometric thermoelectricity corner is installed；Molten to control in flask by regulation electric heating bag heating-up temperature
Liquid temp is 60 DEG C, maintains the reflux for time 50 min in this temperature, is then cooled to room temperature, and prepares template presoma, standby；
Step 2: Hydrothermal Synthesis macropore template；
Step 2.1: the template presoma of preparation is moved in the cup-shaped being made up of polytetrafluoroethylmaterial material that volume is 100 mL
In lining, close the lid, be placed in rustless steel autoclave；
Step 2.2: be put in by autoclave in constant temperature electric heating drying baker, rises to 180 ~ 200 by constant temperature electric heating drying baker temperature
DEG C, it is incubated 36 h；
Step 2.3: after autoclave is cooled to room temperature, transfers in 200 mL beakers, at ultrasonic cleaner by product
Middle supersound process 20 minutes；
Step 2.4: by gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times more anti-with dehydrated alcohol
After backwashing is washed 3 times, obtains solid filter cake；
Step 2.5: be placed in by filter cake in constant temperature electric heating drying baker, is dried 6 h at 90 DEG C, then wears in agate mortar
Powder, obtains macropore template, standby；
Step 3: prepared by Cerium titanate presoma；
Step 3.1: be separately added in 100 mL beakers 5.2 ~ 6.3 mL metatitanic acid isopropyl alcohol esters, 30 ~ 35 mL dehydrated alcohol,
12 ~ 14 mL acetone and 1.2 ~ 1.3 g directed agents AP-3, stir 20 min, as A liquid on magnetic stirring apparatus；
Step 3.2: add 500 mg macropore templates, 3.6 g Surfactant OP-the 3 and 30 anhydrous second of mL in 200 mL beakers
Alcohol, stirs 20 min on magnetic stirring apparatus, as B liquid；
Step 3.3: A drop is added in B liquid and continuously stirred 30 min during magnetic agitation, by mixed liquor at ultrasound wave
Supersound process 1 h in washer, obtains Cerium titanate presoma, standby；
Step 4: Hydrothermal Synthesis Cerium titanate；
Step 4.1: Cerium titanate presoma is moved in the cup-like liner being made up of polytetrafluoroethylmaterial material that volume is 200 mL,
Close the lid, be placed in rustless steel autoclave；
Step 4.2: autoclave is put in constant temperature electric heating drying baker, the temperature of constant temperature electric heating drying baker is risen to 220 ~
240 DEG C, it is incubated 72 h；In the process, pressure is controlled in autoclave not by regulating thermostatic electrically heated drying cabinet temperature
More than 3MPa；
Step 4.3: after autoclave is cooled to room temperature, transfers in 200 mL beakers, at ultrasonic cleaner by product
Middle supersound process 20 minutes；
Step 4.4: by gained solidliquid mixture by cloth funnel sucking filtration, after distilled water wash 3 times more anti-with dehydrated alcohol
After backwashing is washed 3 times, obtains solid filter cake；
Step 4.5: be placed in by filter cake in constant temperature electric heating drying baker, is dried 6 h at 120 DEG C, standby；
Step 5: heat treatment；
Filter cake is put in porcelain crucible and be placed in program control cabinet-type electric furnace, with 10 DEG C/min heating rate, furnace temperature is risen to
1200 ~ 1350 DEG C, at this temperature calcination 3 ~ 6 h；Take out after electric furnace is cooled to room temperature, grind in porcelain mortar and prepare macropore
Hollow Cerium titanate microsphere.
The preparation method of a kind of macropore the most according to claim 1 hollow Cerium titanate microsphere, it is characterised in that described magnetic force
The rotating speed of agitator is 200 r/min.
The preparation method of a kind of macropore the most according to claim 1 hollow Cerium titanate microsphere, it is characterised in that described step
In the insulating process of 2.2, control pressure in autoclave by regulating thermostatic electrically heated drying cabinet temperature and be not more than 3MPa.
The preparation method of a kind of macropore the most according to claim 1 hollow Cerium titanate microsphere, it is characterised in that
Described ultrasonic cleaner all carries out supersound process with 45 MHz frequency.
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| CN201610577086.3A CN106186052A (en) | 2016-07-21 | 2016-07-21 | A kind of preparation method of macropore hollow Cerium titanate microsphere |
| CN201710286590.2A CN107082447B (en) | 2016-07-21 | 2017-04-27 | A kind of preparation method of the hollow Cerium titanate microballoon of macropore |
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| 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 |
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| CN108033483B (en) * | 2017-12-19 | 2019-08-23 | 沈阳理工大学 | It is a kind of can floating type metatitanic acid praseodymium material preparation method |
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|---|---|---|---|---|
| US4313925A (en) * | 1980-04-24 | 1982-02-02 | The United States Of America As Represented By The United States Department Of Energy | Thermochemical cyclic system for decomposing H2 O and/or CO2 by means of cerium-titanium-sodium-oxygen compounds |
| CN1476929A (en) * | 2003-07-08 | 2004-02-25 | 浙江大学 | Denitration catalyst using CeTi2Ob as carrier and its preparation method |
| CN103482694A (en) * | 2013-09-29 | 2014-01-01 | 安徽工业大学 | Cerium titanate nanorod and preparation method thereof |
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| JPS5659672A (en) * | 1979-10-16 | 1981-05-23 | Matsushita Electric Ind Co Ltd | Piezoelectric ceramic material |
| CN102502798A (en) * | 2011-11-09 | 2012-06-20 | 南京航空航天大学 | Preparation method for monodisperse barium titanate nanopowder |
| CN103447022B (en) * | 2013-09-09 | 2015-03-11 | 桂林理工大学 | Visible-light-responsive photocatalyst Ca6Ce2Ti9O28 and preparation method thereof |
| CN106115779B (en) * | 2016-07-07 | 2017-10-31 | 西安交通大学苏州研究院 | A kind of hollow nano-TiO2The preparation method of bag carbon Yolk shell structures |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4313925A (en) * | 1980-04-24 | 1982-02-02 | The United States Of America As Represented By The United States Department Of Energy | Thermochemical cyclic system for decomposing H2 O and/or CO2 by means of cerium-titanium-sodium-oxygen compounds |
| CN1476929A (en) * | 2003-07-08 | 2004-02-25 | 浙江大学 | Denitration catalyst using CeTi2Ob as carrier and its preparation method |
| CN103482694A (en) * | 2013-09-29 | 2014-01-01 | 安徽工业大学 | Cerium titanate nanorod and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108246361B (en) * | 2018-01-08 | 2020-10-30 | 沈阳理工大学 | Method for preparing molecular sieve type titanium cerium oxide photocatalytic material |
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