CN106179303A - A kind of method preparing netted metatitanic acid gadolinium material - Google Patents
A kind of method preparing netted metatitanic acid gadolinium material Download PDFInfo
- Publication number
- CN106179303A CN106179303A CN201610577075.5A CN201610577075A CN106179303A CN 106179303 A CN106179303 A CN 106179303A CN 201610577075 A CN201610577075 A CN 201610577075A CN 106179303 A CN106179303 A CN 106179303A
- Authority
- CN
- China
- Prior art keywords
- precursor solution
- metatitanic acid
- titanium net
- colloidal sol
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002253 acid Substances 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 40
- 229910052688 Gadolinium Inorganic materials 0.000 title claims abstract description 32
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 56
- 239000010936 titanium Substances 0.000 claims abstract description 56
- 239000002243 precursor Substances 0.000 claims abstract description 46
- 238000010992 reflux Methods 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229960000583 acetic acid Drugs 0.000 claims abstract description 9
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 9
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 9
- 239000004922 lacquer Substances 0.000 claims abstract description 9
- 239000003973 paint Substances 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 8
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000003381 stabilizer Substances 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 238000003760 magnetic stirring Methods 0.000 claims description 16
- 238000005485 electric heating Methods 0.000 claims description 14
- 238000009833 condensation Methods 0.000 claims description 12
- 230000005494 condensation Effects 0.000 claims description 12
- 235000015165 citric acid Nutrition 0.000 claims description 8
- 239000002826 coolant Substances 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 239000008399 tap water Substances 0.000 claims description 7
- 235000020679 tap water Nutrition 0.000 claims description 7
- 239000011800 void material Substances 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 229920002538 Polyethylene Glycol 20000 Polymers 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 238000013019 agitation Methods 0.000 description 9
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000000746 purification Methods 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- YSLWUGPNJFSBON-UHFFFAOYSA-N [Ti].[Gd] Chemical compound [Ti].[Gd] YSLWUGPNJFSBON-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
A kind of method preparing netted metatitanic acid gadolinium material, prepares precursor solution 1: be heated to reflux preparation with dehydrated alcohol, acetone, pentanediol, stabilizer, positive four butyl esters of metatitanic acid, surfactant and directed agents；Preparation precursor solution 2: prepare with deionized water, citric acid, Gadolinium trinitrate, sodium carbonate, PEG20000 and glacial acetic acid；Prepare colloidal sol: by 2 precursor solution mixing post-heating backflows；Titanium net gel is covered with paint, lacquer, colour wash, etc.: titanium net lifts in colloidal sol preparation；Heat treatment: the titanium net scribbling gel is dried and calcines.Metatitanic acid gadolinium coating stability is good, metatitanic acid gadolinium active component is evenly distributed, it is high to be catalyzed activity.
Description
Technical field
The invention belongs to environmental purification function Material Field, be specifically related to a kind of method preparing netted metatitanic acid gadolinium material.
Background technology
The research and development that purification techniques have passed through nearly 50 years is polluted in photocatalysis, has been increasingly becoming a kind of rich potential
Multipurpose pollutes purification means, has outstanding application and performance in industrial and civilian various aspects.In order to improve photocatalysis
Purification efficiency, an important aspect is to use efficiently and meet the catalysis material of specific use needs.Industrialized photocatalysis
Purification reactor often shape to material has special requirement, and it is clean that simple powder body material can not meet successional pollutant
Change processing procedure.In order to avoid separating step with catalysis material after sewage disposal, the most often use load
Shaped material, and final material shape is generally restricted by carrier, to the selection of carrier it is contemplated that catalysis material system
The restriction of standby condition.In continuous flow reactor, need to use immobilized catalysis material, simultaneously it is contemplated that waste water
Or the flow process of waste gas.The basic characteristics of Web materials are can fully to receive the radiation of light source, disclosure satisfy that waste water simultaneously
Or the continuous flowing of waste gas.As the material that disclosure satisfy that commercial production needs, it is necessary to possess certain mechanical strength, it is possible to
Keep long service life.
Metatitanic acid gadolinium material has good heat stability and the most suitable energy gap, becomes current rich potential one
Class novel photocatalysis material.Research to such material is the most also in theoretical research stage, lacks its actual applied product
The development of product, does not the most prepare the metatitanic acid gadolinium material of special shape according to the specific requirement of conventional photo catalysis reactor.Pin
To the continuous flow reactor special requirement to catalysis material, this patent discloses a kind of side preparing netted metatitanic acid gadolinium material
Method.
Summary of the invention
The problem existed for prior art, it is desirable to provide a kind of method preparing netted metatitanic acid gadolinium material, can
Light catalytic purifying technical process for various ways.
A kind of method preparing netted metatitanic acid gadolinium material, it is characterised in that it comprises the following steps:
Step 1: preparation precursor solution 1；
Step 1.1: in 1000 mL three neck round bottom flasks add 170 ~ 200 mL dehydrated alcohol, 35 ~ 50 mL acetone, 25 ~ 30
ML pentanediol and 4 ~ 7 g stabilizer OP-9；
Step 1.2: described three neck round bottom flask be placed in precise temperature control electric heating bag, installs thermometric galvanic couple, overhead electric mixing
Mix machine and spherical condensation tube, condensing tube is passed through tap water as cooling medium；
Step 1.3: by adjusting the heating-up temperature of electric heating bag, make the temperature of solution in flask be maintained at 80 DEG C, electric blender
Mixing speed 200 r/min, be heated to reflux 20 min；
Step 1.4: add in flask 36 ~ 38 positive four butyl esters of mL metatitanic acid, 10 ~ 15 mL surfactant CR-6,15 ~ 18
ML directed agents AT-7, continues to be heated to reflux 60 min afterwards at a temperature of 80 DEG C, obtains precursor solution 1, standby；
Step 2: preparation precursor solution 2；
Step 2.1: add 51 ~ 56 mL deionized waters, 3.5 ~ 3.6 g citric acids and 15 ~ 17 g nitre in 200 mL glass beakers
Acid gadolinium, on magnetic stirring apparatus, stirring is allowed to fully dissolve；
Step 2.2: add 2.8 ~ 3.0 g sodium carbonate, 6.6 ~ 6.8 g PEG20000s and 4.1 again in the solution after dissolving
~ 4.3 mL glacial acetic acid, stir to being completely dissolved on magnetic stirring apparatus, prepare precursor solution 2；
Step 3: prepare colloidal sol；
Under conditions of stirring, precursor solution 2 is added in precursor solution 1, at a temperature of 50 DEG C, be heated to reflux 120
Min, until being transferred in 1000 mL beakers standby after forming transparent and slightly thickness colloidal sol；
Step 4: titanium net gel is covered with paint, lacquer, colour wash, etc.；
The titanium net of a size of 10 cm × 10 cm is immersed in the colloidal sol that step 3 beaker holds, after 10 min, slowly lift titanium net
Leave colloidal sol, at room temperature hang and place 3 h；
Step 5: heat treatment；
Step 5.1: be placed in air dry oven by the titanium net scribbling gel, is dried 12 h at a temperature of 130 DEG C；
Step 5.2: be placed in program control cabinet-type electric furnace by the titanium net being completely dried, the heating rate with 10 DEG C/min will calcining
Temperature rises to 630 ~ 1000 DEG C, and keeps calcining heat 3 ~ 7 h；Treat after calcining that electric furnace is cooled to room temperature, i.e. prepare netted metatitanic acid
Gadolinium material.
Described titanium net is made up of diameter 0.3 mm titanium silk, and between titanium silk, void size is 1mm × 1mm.
In described step 2, the rotating speed of magnetic stirring apparatus is 200 revs/min.
Compared with prior art, it is an advantage of the current invention that:
1, the technical problem underlying of the present invention is to solve to form metatitanic acid gadolinium coating on the net at titanium and improve its stability, the present invention with
Titanium net is matrix material, it is ensured that matrix will not produce with metatitanic acid gadolinium and influence each other；
2, the present invention selects positive four butyl esters of metatitanic acid, citric acid, Gadolinium trinitrate, sodium carbonate, PEG20000 and glacial acetic acid as master
Wanting raw material, by accurately controlling precursor solution preparation, colloidal sol synthesizes, titanium net gel is covered with paint, lacquer, colour wash, etc. and heat treatment process, prepares titanium
Gadolinium coating stability is good, metatitanic acid gadolinium active component is evenly distributed in acid, be catalyzed the netted metatitanic acid gadolinium catalysis material that activity is high；
3, the inventive method preparation technology is simple and clear, synthesis condition is gentle and is prone to repetition, material structure and stable performance, can be used for
Under the conditions of specific use, the photocatalysis of environmental contaminants is administered, and has broad application prospects at environmental area.
Detailed description of the invention
Embodiment 1
A kind of method preparing netted metatitanic acid gadolinium material, mainly comprises the steps that
(1) preparation precursor solution 1:
Adding 180 mL dehydrated alcohol, 38 mL acetone and 26 mL pentanediols in 1000 mL three neck round bottom flasks, 4 g are stable
Agent OP-9；
Flask is placed in precise temperature control electric heating bag, thermometric galvanic couple, overhead electric blender and spherical condensation tube, condensation are installed
Pipe is passed through tap water as cooling medium；
By adjusting the heating-up temperature of electric heating bag, the temperature of solution in flask is made to be maintained at 80 DEG C, the stirring speed of electric blender
Spend 200 r/min, be heated to reflux 20 min；
In flask, add 36 positive four butyl esters of mL metatitanic acid, 10 mL surfactant CR-6,15 mL directed agents AT-7, continue
It is heated to reflux 60 min at 80 DEG C, obtains precursor solution 1, standby.
(2) preparation precursor solution 2:
51 mL deionized waters, 3.5 g citric acids and 15 g Gadolinium trinitrates are added, at magnetic stirring apparatus in 200 mL glass beakers
Upper stirring is allowed to fully dissolve；
2.8 g sodium carbonate, 6.6 g PEG20000s and 4.1 mL glacial acetic acid are added again, in magnetic agitation in above-mentioned solution
Stir on device to being completely dissolved, prepare precursor solution 2.
(3) colloidal sol is prepared:
Under agitation precursor solution 2 is added in precursor solution 1, is heated to reflux 120 min at 50 DEG C, formed transparent and
The slightly colloidal sol of thickness, is transferred in 1000 mL beakers standby.
(4) titanium net gel is covered with paint, lacquer, colour wash, etc.:
By the titanium net (being made up of diameter 0.3 mm titanium silk, between titanium silk, void size is 1mm × 1mm) of a size of 10 cm × 10 cm
Immersing in the colloidal sol held in beaker, after 10 min, slowly lifting titanium net leaves colloidal sol, at room temperature hangs and places 3 h.
(5) heat treatment:
The titanium net scribbling gel is placed in air dry oven, is dried 12 h at 130 DEG C；
The titanium net being completely dried is placed in program control cabinet-type electric furnace, with the heating rate of 10 DEG C/min, calcining heat is risen to
700 DEG C, and keep calcining heat 5 h；Treat after calcining that electric furnace is cooled to room temperature, i.e. prepare netted metatitanic acid gadolinium material.
It is 200 revs/min that the rotating speed of the magnetic stirring apparatus described in the present embodiment can all be selected.
Embodiment 2
A kind of method preparing netted metatitanic acid gadolinium material, mainly comprises the steps that
(1) preparation precursor solution 1:
Adding 190 mL dehydrated alcohol, 39 mL acetone and 27 mL pentanediols in 1000 mL three neck round bottom flasks, 5.3 g are steady
Determine agent OP-9；
Flask is placed in precise temperature control electric heating bag, thermometric galvanic couple, overhead electric blender and spherical condensation tube, condensation are installed
Pipe is passed through tap water as cooling medium；
By adjusting the heating-up temperature of electric heating bag, the temperature of solution in flask is made to be maintained at 80 DEG C, the stirring speed of electric blender
Spend 200 r/min, be heated to reflux 20 min；
In flask, add 37 positive four butyl esters of mL metatitanic acid, 12 mL surfactant CR-6,16 mL directed agents AT-7, continue
It is heated to reflux 60 min at 80 DEG C, obtains precursor solution 1, standby.
(2) preparation precursor solution 2:
53 mL deionized waters, 3.5 g citric acids and 16 g Gadolinium trinitrates are added, at magnetic stirring apparatus in 200 mL glass beakers
Upper stirring is allowed to fully dissolve；
2.9 g sodium carbonate, 6.6 g PEG20000s and 4.1 mL glacial acetic acid are added again, in magnetic agitation in above-mentioned solution
Stir on device to being completely dissolved, prepare precursor solution 2.
(3) colloidal sol is prepared:
Under agitation precursor solution 2 is added in precursor solution 1, is heated to reflux 120 min at 50 DEG C, formed transparent and
The slightly colloidal sol of thickness, is transferred in 1000 mL beakers standby.
(4) titanium net gel is covered with paint, lacquer, colour wash, etc.:
By the titanium net (being made up of diameter 0.3 mm titanium silk, between titanium silk, void size is 1mm × 1mm) of a size of 10 cm × 10 cm
Immersing in the colloidal sol held in beaker, after 10 min, slowly lifting titanium net leaves colloidal sol, at room temperature hangs and places 3 h.
(5) heat treatment:
The titanium net scribbling gel is placed in air dry oven, is dried 12 h at 130 DEG C；
The titanium net being completely dried is placed in program control cabinet-type electric furnace, with the heating rate of 10 DEG C/min, calcining heat is risen to
800 DEG C, and keep calcining heat 5 h；Treat after calcining that electric furnace is cooled to room temperature, i.e. prepare netted metatitanic acid gadolinium material.
It is 200 revs/min that the rotating speed of the magnetic stirring apparatus described in the present embodiment can all be selected.
Embodiment 3
A kind of method preparing netted metatitanic acid gadolinium material, mainly comprises the steps that
(1) preparation precursor solution 1:
In 1000 mL three neck round bottom flasks, add 190 mL dehydrated alcohol, 45 mL acetone and 30 mL pentanediols and 6 g are stable
Agent OP-9；
Flask is placed in precise temperature control electric heating bag, thermometric galvanic couple, overhead electric blender and spherical condensation tube, condensation are installed
Pipe is passed through tap water as cooling medium；
By adjusting the heating-up temperature of electric heating bag, the temperature of solution in flask is made to be maintained at 80 DEG C, the stirring speed of electric blender
Spend 200 r/min, be heated to reflux 20 min；
In flask, add 38 positive four butyl esters of mL metatitanic acid, 15 mL surfactant CR-6,18 mL directed agents AT-7, continue
It is heated to reflux 60 min at 80 DEG C, obtains precursor solution 1, standby.
(2) preparation precursor solution 2:
55 mL deionized waters, 3.6 g citric acids and 17 g Gadolinium trinitrates are added, at magnetic stirring apparatus in 200 mL glass beakers
Upper stirring is allowed to fully dissolve.
3.0 g sodium carbonate, 6.8 g PEG20000s and 4.3 mL glacial acetic acid are added again, at magnetic force in above-mentioned solution
Stir on agitator to being completely dissolved, prepare precursor solution 2.
(3) colloidal sol is prepared:
Under agitation precursor solution 2 is added in precursor solution 1, is heated to reflux 120 min at 50 DEG C, formed transparent and
The slightly colloidal sol of thickness, is transferred in 1000 mL beakers standby.
(4) titanium net gel is covered with paint, lacquer, colour wash, etc.:
By the titanium net (being made up of diameter 0.3 mm titanium silk, between titanium silk, void size is 1mm × 1mm) of a size of 10 cm × 10 cm
Immersing in the colloidal sol held in beaker, after 10 min, slowly colloidal sol is left in lifting, at room temperature hangs and places 3 h.
(5) heat treatment:
The titanium net scribbling gel is placed in air dry oven, is dried 12 h at 130 DEG C；
The titanium net being completely dried is placed in program control cabinet-type electric furnace, with the heating rate of 10 DEG C/min, calcining heat is risen to
900 DEG C, and keep calcining heat 3 h；Treat after calcining that electric furnace is cooled to room temperature, i.e. prepare netted metatitanic acid gadolinium material.
It is 200 revs/min that the rotating speed of the magnetic stirring apparatus described in the present embodiment can all be selected.
Embodiment 4
A kind of method preparing netted metatitanic acid gadolinium material, mainly comprises the steps that
(1) preparation precursor solution 1:
170 mL dehydrated alcohol, 35 mL acetone and 25 mL pentanediols, 7g stabilizer is added in 1000 mL three neck round bottom flasks
OP-9；
Flask is placed in precise temperature control electric heating bag, thermometric galvanic couple, overhead electric blender and spherical condensation tube, condensation are installed
Pipe is passed through tap water as cooling medium；
By adjusting the heating-up temperature of electric heating bag, the temperature of solution in flask is made to be maintained at 80 DEG C, the stirring speed of electric blender
Spend 200 r/min, be heated to reflux 20 min；
In flask, add 36 positive four butyl esters of mL metatitanic acid, 12 mL surfactant CR-6,16 mL directed agents AT-7, continue
It is heated to reflux 60 min at 80 DEG C, obtains precursor solution 1, standby.
(2) preparation precursor solution 2:
56 mL deionized waters, 3.4 g citric acids and 16g Gadolinium trinitrate is added, on magnetic stirring apparatus in 200 mL glass beakers
Stirring is allowed to fully dissolve；
2.8 g sodium carbonate, 6.6 g PEG20000s and 4.1 mL glacial acetic acid are added again, in magnetic agitation in above-mentioned solution
Stir on device to being completely dissolved, prepare precursor solution 2.
(3) colloidal sol is prepared:
Under agitation precursor solution 2 is added in precursor solution 1, is heated to reflux 120 min at 50 DEG C, formed transparent and
The slightly colloidal sol of thickness, is transferred in 1000 mL beakers standby.
(4) titanium net gel is covered with paint, lacquer, colour wash, etc.:
By the titanium net (being made up of diameter 0.3 mm titanium silk, between titanium silk, void size is 1mm × 1mm) of a size of 10 cm × 10 cm
Immersing in the colloidal sol held in beaker, after 10 min, slowly lifting titanium net leaves colloidal sol, at room temperature hangs and places 3 h.
(5) heat treatment:
The titanium net scribbling gel is placed in air dry oven, is dried 12 h at 130 DEG C；
The titanium net being completely dried is placed in program control cabinet-type electric furnace, with the heating rate of 10 DEG C/min, calcining heat is risen to
630 DEG C, and keep calcining heat 7 h；Treat after calcining that electric furnace is cooled to room temperature, i.e. prepare netted metatitanic acid gadolinium material.
It is 200 revs/min that the rotating speed of the magnetic stirring apparatus described in the present embodiment can all be selected.
Embodiment 5
A kind of method preparing netted metatitanic acid gadolinium material, mainly comprises the steps that
(1) preparation precursor solution 1:
Adding 200 mL dehydrated alcohol, 50 mL acetone and 28 mL pentanediols in 1000 mL three neck round bottom flasks, 6.8 g are steady
Determine agent OP-9；
Flask is placed in precise temperature control electric heating bag, thermometric galvanic couple, overhead electric blender and spherical condensation tube, condensation are installed
Pipe is passed through tap water as cooling medium；
By adjusting the heating-up temperature of electric heating bag, the temperature of solution in flask is made to be maintained at 80 DEG C, the stirring speed of electric blender
Spend 200 r/min, be heated to reflux 20 min；
In flask, add 37 positive four butyl esters of mL metatitanic acid, 12 mL surfactant CR-6,16 mL directed agents AT-7, continue
It is heated to reflux 60 min at 80 DEG C, obtains precursor solution 1, standby.
(2) preparation precursor solution 2:
55 mL deionized waters, 3.6 g citric acids and 16 g Gadolinium trinitrates are added, at magnetic stirring apparatus in 200 mL glass beakers
Upper stirring is allowed to fully dissolve；
3.0 g sodium carbonate, 6.7 g PEG20000s and 4.2 mL glacial acetic acid are added again, in magnetic agitation in above-mentioned solution
Stir on device to being completely dissolved, prepare precursor solution 2.
(3) colloidal sol is prepared:
Under agitation precursor solution 2 is added in precursor solution 1, is heated to reflux 120 min at 50 DEG C, formed transparent and
The slightly colloidal sol of thickness, is transferred in 1000 mL beakers standby.
(4) titanium net gel is covered with paint, lacquer, colour wash, etc.:
By the titanium net (being made up of diameter 0.3 mm titanium silk, between titanium silk, void size is 1mm × 1mm) of a size of 10 cm × 10 cm
Immersing in the colloidal sol held in beaker, after 10 min, slowly lifting titanium net leaves colloidal sol, at room temperature hangs and places 3 h.
(5) heat treatment:
The titanium net scribbling gel is placed in air dry oven, is dried 12 h at 130 DEG C；
The titanium net being completely dried is placed in program control cabinet-type electric furnace, with the heating rate of 10 DEG C/min, calcining heat is risen to
1000 DEG C, and keep calcining heat 4 h；Treat after calcining that electric furnace is cooled to room temperature, i.e. prepare netted metatitanic acid gadolinium material.
It is 200 revs/min that the rotating speed of the magnetic stirring apparatus described in the present embodiment can all be selected.
Claims (3)
1. the method preparing netted metatitanic acid gadolinium material, it is characterised in that it comprises the following steps:
Step 1: preparation precursor solution 1；
Step 1.1: in 1000 mL three neck round bottom flasks add 170 ~ 200 mL dehydrated alcohol, 35 ~ 50 mL acetone, 25 ~ 30
ML pentanediol and 4 ~ 7 g stabilizer OP-9；
Step 1.2: described three neck round bottom flask be placed in precise temperature control electric heating bag, installs thermometric galvanic couple, overhead electric mixing
Mix machine and spherical condensation tube, condensing tube is passed through tap water as cooling medium；
Step 1.3: by adjusting the heating-up temperature of electric heating bag, make the temperature of solution in flask be maintained at 80 DEG C, electric blender
Mixing speed 200 r/min, be heated to reflux 20 min；
Step 1.4: add in flask 36 ~ 38 positive four butyl esters of mL metatitanic acid, 10 ~ 15 mL surfactant CR-6,15 ~ 18
ML directed agents AT-7, continues to be heated to reflux 60 min afterwards at a temperature of 80 DEG C, obtains precursor solution 1, standby；
Step 2: preparation precursor solution 2；
Step 2.1: add 51 ~ 56 mL deionized waters, 3.5 ~ 3.6 g citric acids and 15 ~ 17 g nitre in 200 mL glass beakers
Acid gadolinium, on magnetic stirring apparatus, stirring is allowed to fully dissolve；
Step 2.2: add 2.8 ~ 3.0 g sodium carbonate, 6.6 ~ 6.8 g PEG20000s and 4.1 again in the solution after dissolving
~ 4.3 mL glacial acetic acid, stir to being completely dissolved on magnetic stirring apparatus, prepare precursor solution 2；
Step 3: prepare colloidal sol；
Under conditions of stirring, precursor solution 2 is added in precursor solution 1, at a temperature of 50 DEG C, be heated to reflux 120
Min, until being transferred in 1000 mL beakers standby after forming transparent and slightly thickness colloidal sol；
Step 4: titanium net gel is covered with paint, lacquer, colour wash, etc.；
The titanium net of a size of 10 cm × 10 cm is immersed in the colloidal sol that step 3 beaker holds, after 10 min, slowly lift titanium net
Leave colloidal sol, at room temperature hang and place 3 h；
Step 5: heat treatment；
Step 5.1: be placed in air dry oven by the titanium net scribbling gel, is dried 12 h at a temperature of 130 DEG C；
Step 5.2: be placed in program control cabinet-type electric furnace by the titanium net being completely dried, the heating rate with 10 DEG C/min will calcining
Temperature rises to 630 ~ 1000 DEG C, and keeps calcining heat 3 ~ 7 h；Treat after calcining that electric furnace is cooled to room temperature, i.e. prepare netted metatitanic acid
Gadolinium material.
A kind of method preparing netted metatitanic acid gadolinium material the most according to claim 1, it is characterised in that described titanium net be by
Diameter 0.3 mm titanium silk is made, and between titanium silk, void size is 1mm × 1mm.
A kind of method preparing netted metatitanic acid gadolinium material the most according to claim 1, it is characterised in that in described step 2
The rotating speed of magnetic stirring apparatus is 200 revs/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610577075.5A CN106179303A (en) | 2016-07-21 | 2016-07-21 | A kind of method preparing netted metatitanic acid gadolinium material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610577075.5A CN106179303A (en) | 2016-07-21 | 2016-07-21 | A kind of method preparing netted metatitanic acid gadolinium material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106179303A true CN106179303A (en) | 2016-12-07 |
Family
ID=57491835
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610577075.5A Pending CN106179303A (en) | 2016-07-21 | 2016-07-21 | A kind of method preparing netted metatitanic acid gadolinium material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106179303A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984295A (en) * | 2017-03-28 | 2017-07-28 | 沈阳理工大学 | A kind of method for preparing two-dimentional strontium titanates Web materials |
| CN108301253A (en) * | 2018-01-08 | 2018-07-20 | 沈阳理工大学 | A kind of preparation method of the ceramic fiber paper of surface cladding titanium boron oxide compound coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102059110A (en) * | 2010-12-02 | 2011-05-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of double-rare earth co-doped nanometer titanium dioxide photocatalyst |
| CN102784636A (en) * | 2012-07-17 | 2012-11-21 | 上海交通大学 | Preparation method of spherical gadolinium-doped titanium dioxide photocatalyst |
| CN103100414A (en) * | 2013-01-31 | 2013-05-15 | 沈阳理工大学 | Molecular sieve with photocatalysis function, and preparation method thereof |
-
2016
- 2016-07-21 CN CN201610577075.5A patent/CN106179303A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102059110A (en) * | 2010-12-02 | 2011-05-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of double-rare earth co-doped nanometer titanium dioxide photocatalyst |
| CN102784636A (en) * | 2012-07-17 | 2012-11-21 | 上海交通大学 | Preparation method of spherical gadolinium-doped titanium dioxide photocatalyst |
| CN103100414A (en) * | 2013-01-31 | 2013-05-15 | 沈阳理工大学 | Molecular sieve with photocatalysis function, and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984295A (en) * | 2017-03-28 | 2017-07-28 | 沈阳理工大学 | A kind of method for preparing two-dimentional strontium titanates Web materials |
| CN108301253A (en) * | 2018-01-08 | 2018-07-20 | 沈阳理工大学 | A kind of preparation method of the ceramic fiber paper of surface cladding titanium boron oxide compound coating |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103977826B (en) | Modified TiO2 coating and preparation method thereof | |
| CN107362793B (en) | A kind of CeVO4-La2O3The preparation method and purposes of@HNTs composite photo-catalyst | |
| CN105944710A (en) | Quartz sand supported lanthanum titanate photocatalyst and method for preparing same | |
| CN107754819B (en) | Synthesis of photocatalyst SnS with visible light response2/Bi2WO6Preparation method of nanosheet | |
| CN101733087A (en) | Floating type TiO2/floating bead composite photochemical catalyst and preparation method and application thereof | |
| CN102674452A (en) | Method for preparing nano titanium dioxide by sol process at low temperature | |
| CN106732519A (en) | A kind of preparation method of soft lanthanium titanate fiber | |
| CN106179303A (en) | A kind of method preparing netted metatitanic acid gadolinium material | |
| CN105129806A (en) | High-specific surface area silica for washing powder and its preparation method and use | |
| CN106268907B (en) | A kind of two dimension Conductive mica load carbonitride catalysis material and preparation method thereof | |
| CN103933957B (en) | Porous monocrystalline nano titanium dioxide photocatalyst that a kind of high crystallization, size are controlled, high-energy surface exposes and its preparation method and application | |
| CN103846099B (en) | A kind of support type polyoxometallate and preparation method thereof | |
| CN105797707A (en) | Method for preparing mesoporous titanic acid lanthanum zinc photocatalyst | |
| CN108033485A (en) | A kind of one-step synthesis method TiO2The efficient hydrogen manufacturing of microballoon and the method for degradation of contaminant | |
| CN108816266B (en) | YF/g-C3N4Composite material and application thereof in photocatalysis | |
| CN106040225A (en) | Thin-layered bismuth titanate material and preparation method thereof | |
| CN106861667B (en) | A kind of TiO to suspend in water2The preparation method of microballoon | |
| CN110270355A (en) | A kind of preparation method of glass fabric load bismuth oxyiodide photocatalyst film | |
| CN100357186C (en) | Zinc oxide hollow microsphere preparation method | |
| CN107335432A (en) | A kind of BiVO4/TiO2The preparation method of nucleocapsid composite photo-catalyst | |
| CN107062154A (en) | Monoblock type photocatalysis light fixture and the preparation method of monoblock type catalysis material for air cleaning | |
| CN106622310A (en) | Preparation method of silver phosphate-titanium dioxide composite photocatalyst | |
| CN108285174B (en) | WO (WO)3-ZrO2Preparation method of photocatalytic sewage treatment membrane | |
| CN103816856B (en) | For the material and its preparation method and application of micro quantity organic pollutant in degradation water | |
| CN107640801A (en) | A kind of method of photocatalysis coupled filtering integral PROCESS FOR TREATMENT phenol wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161207 |