CN106732519A - A kind of preparation method of soft lanthanium titanate fiber - Google Patents
A kind of preparation method of soft lanthanium titanate fiber Download PDFInfo
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- CN106732519A CN106732519A CN201611025211.6A CN201611025211A CN106732519A CN 106732519 A CN106732519 A CN 106732519A CN 201611025211 A CN201611025211 A CN 201611025211A CN 106732519 A CN106732519 A CN 106732519A
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- lanthanium titanate
- solution
- colloidal sol
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- ceramic fibre
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000000835 fiber Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 235000019441 ethanol Nutrition 0.000 claims abstract description 11
- 238000007711 solidification Methods 0.000 claims abstract description 11
- 230000008023 solidification Effects 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000002657 fibrous material Substances 0.000 claims abstract description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 6
- -1 isopropyl alcohol ester Chemical class 0.000 claims abstract description 6
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000009833 condensation Methods 0.000 claims description 15
- 230000005494 condensation Effects 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 238000005485 electric heating Methods 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000011282 treatment Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000004922 lacquer Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims 4
- 235000005979 Citrus limon Nutrition 0.000 claims 1
- 244000131522 Citrus pyriformis Species 0.000 claims 1
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N isopropyl alcohol Natural products CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 abstract 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-O isopropylaminium Chemical compound CC(C)[NH3+] JJWLVOIRVHMVIS-UHFFFAOYSA-O 0.000 abstract 1
- 229940039790 sodium oxalate Drugs 0.000 abstract 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 8
- 229910052573 porcelain Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 229960004543 anhydrous citric acid Drugs 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- IPGOVDXOBDFUBM-UHFFFAOYSA-N oxalic acid;sodium Chemical compound [Na].OC(=O)C(O)=O IPGOVDXOBDFUBM-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000011269 treatment regimen Methods 0.000 description 1
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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
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- 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
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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
- 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
- B01J35/58—Fabrics or filaments
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
A kind of preparation method of soft lanthanium titanate fiber, the first solution is synthesized in round-bottomed flask using absolute ethyl alcohol, acetone and paraxylene, metatitanic acid isopropyl alcohol ester, 25% ethanol solution of tri-tert isopropyl ammonium, directed agents ART 113.Second solution is synthesized with distilled water, lanthanum nitrate, ammonium chloride, sodium oxalate and dispersant TO 125.Mix the first solution and the second solution, form lanthanium titanate colloidal sol.Ceramic fibre is immersed in colloidal sol, dry solidification is carried out after lifting out.3 ~ 5 h are processed in 750 ~ 950 DEG C of calcined oxides in electric furnace, soft lanthanium titanate fibrous material is obtained, can synthesized that purity is higher on ceramic fibre, be evenly distributed, the lanthanium titanate material that adhesive strength is big.
Description
Technical field：
It is a kind of preparation of soft lanthanium titanate fiber the present invention relates to a kind of functional material that can be used for environmental pollution purification process
Method.
Background technology：
Photocatalysis purifying technology is applied to atmosphere and water pollution to be administered has unique using effect, is applied to many tools
Environmental pollution improvement's process of body.In past research process, main work is around novel high-activity catalysis material
Preparation and application.By semicentennial exploitation and improvement, current research emphasis are that the further industrialization of the technology should
With.In this process, the selection of material and the adaptability to specific embodiment are just particularly important.Photocatalysis technology and
Related product is mainly used in Small Civil product and Small Scale Industry production, the master applied in large-scale industrial production to it
It is catalysis material to want restraining factors.Titanium-containing compound is the main body of catalysis material, wherein most importantly titanium oxide, is subject to
The titanate that researcher pays close attention to is the class novel photocatalysis material that there is application potential current pole.Lanthanium titanate material is all kinds of
Environmental pollution purification process has gratifying performance, especially the utilization of visible luminous energy is made it have relatively low use into
This.
, it is necessary to catalysis material is made various special shapes to adapt to different works during specific pollution control
The requirement of skill process.Soft-filler has very strong adaptability in air and water process, can quickly and efficiently adsorb and degrade
Pollutant, and suitable for variously-shaped reactor.Fibrous material has high surface area and surface reaction activity, fits
It is suitable for flowable state purified treatment pattern.The present invention discloses a kind of preparation method of soft lanthanium titanate fiber, can prepare attachment
The soft fiber material of lanthanium titanate, with great application potential and use value.
The content of the invention：
For the problem that prior art is present, the present invention is intended to provide a kind of preparation method of soft lanthanium titanate fiber.
The technical solution adopted by the present invention is：
A kind of preparation method of soft lanthanium titanate fiber, including following processing steps：
Step 1：Synthesis lanthanium titanate colloidal sol.
Step 1.1：500 mL three neck round bottom flask add 170 ~ 190 mL absolute ethyl alcohols, 75 ~ 85 mL acetone and 26 ~
33 mL paraxylene, then load onto agitator, temperature thermocouple and spherical condensation tube, and spherical condensation tube connection running water is played
Cooling effect, 500 mL three neck round bottom flask are placed in constant temperature electric heating bag.
Step 1.2：Solution temperature is 60 DEG C in keeping 500 mL three neck round bottom flask, continuous heating 30 min of backflow, together
When agitator speed of agitator be 60rpm, be subsequently added 36 ~ 39 mL metatitanic acid isopropyls alcohol esters, 3.7 ~ 3.9 mL tri-tert isopropyls
The 25% of ammonium（Mass percent）Ethanol solution and 3.1 ~ 3.3 mL directed agents ART-113, it is 60 DEG C to keep solution temperature, plus
Heat 30 min of backflow, while agitator speed of agitator is 60rpm, form the first solution.
Step 1.3：200 mL beakers are placed in magnetic-mixing constant temperature water bath boiler, to addition 61 ~ 65 in 200 mL beakers
ML distilled water, it is 60 DEG C to keep water-bath water temperature.By 6.1 ~ 6.3 g lanthanum nitrates, 2.5 ~ 2.6 g ammonium chlorides, 2.5 ~ 2.7 g oxalic acid
Sodium and 1.6 ~ 1.7 g dispersants TO-125 are separately added into distilled water, are continuously stirred until all substances are completely dissolved, and form the
Two solution.
Step 1.4：During the second solution is added into the first solution in 500 mL three neck round bottom flask, 0.1-0.3g is added
Anhydrous citric acid, installs agitator, temperature thermocouple and spherical condensation tube, 30 min is heated to reflux at 60 DEG C, while agitator
Speed of agitator is 60rpm, forms transparence lanthanium titanate colloidal sol.
Step 2：Ceramic fibre is covered with paint, lacquer, colour wash, etc..
Step 2.1：Lanthanium titanate colloidal sol prepared by step 1.4 is poured into large beaker, by ceramic fibre（300 mm long, directly
The mm of footpath 1）3 min in lanthanium titanate colloidal sol are immersed in, lanthanium titanate colloidal sol is then vertically lifted out.
Step 2.2：Ceramic fibre is vertically stood to surface solidification at ambient temperature, disk is circular on porcelain dish, so
After be put in 85 DEG C of constant temperature electric heating drying boxes, reach complete gel solidification through 24 h.
Step 3：Calcined oxide treatment.
Step 3.1：The ceramic fibre for having coated lanthanium titanate gel prepared by step 2.2 is put in program control box together with porcelain dish
In electric furnace, by program control cabinet-type electric furnace temperature control at 750 ~ 950 DEG C, calcined oxide processes 3 ~ 5 h in atmosphere.Calcining terminates
Taken out after material is cooled into room temperature, you can soft lanthanium titanate fibrous material is obtained.
The advantage is that：
By to the formula and preparation process in synthesis lanthanium titanate colloidal sol, ceramic fibre covering with paint and calcined oxide processing procedure
Optimization, be matrix from resistant to elevated temperatures ceramic fibre material, can synthesize that purity is higher on ceramic fibre, be evenly distributed,
The big lanthanium titanate material of adhesive strength.The material is applied under specific use condition（For example in sewage）Environmental contaminants suction
Light catalytic purifying Processing tecchnics are echoed, has the advantages that good stability, treatment effeciency are high.The invention provides a kind of novel material
Material preparation means, prepared lanthanium titanate fibrous material is administered field and is had wide practical use in atmosphere and water pollution.
Specific embodiment：
Embodiment 1
A kind of preparation method of soft lanthanium titanate fiber, including following processing steps：
Step 1：Synthesis lanthanium titanate colloidal sol.
Step 1.1：170 mL absolute ethyl alcohols, 75 mL acetone and 26 mL pairs are added in 500 mL three neck round bottom flask
Dimethylbenzene, then loads onto agitator, temperature thermocouple and spherical condensation tube, and spherical condensation tube connection running water plays cooling and makees
With.500 mL three neck round bottom flask are placed in constant temperature electric heating bag.
Step 1.2：Solution temperature is 60 DEG C in keeping 500 mL three neck round bottom flask, continuous heating 30 min of backflow, together
When agitator speed of agitator be 60rpm, be subsequently added 36 mL metatitanic acid isopropyls alcohol esters, the 25% of 3.7 mL tri-tert isopropyl ammoniums
（Mass percent）Ethanol solution and 3.1 mL directed agents ART-113, keep solution temperature for 60 DEG C are heated to reflux 30 min,
Agitator speed of agitator is 60rpm simultaneously, forms the first solution.
Step 1.3：200 mL beakers are placed in magnetic-mixing constant temperature water bath boiler, to adding 61 mL in 200 mL beakers
Distilled water, it is 60 DEG C to keep water-bath water temperature.By 6.1 g lanthanum nitrates, 2.5 g ammonium chlorides, 2.5 g sodium oxalates and 1.6 g dispersion
Agent TO-125 is separately added into distilled water, is continuously stirred up to all substances are completely dissolved, and forms the second solution.
Step 1.4：During the second solution is added into the first solution in 500mL three neck round bottom flask, 0.1g is added anhydrous
Citric acid, installs agitator, temperature thermocouple and spherical condensation tube, and 30 min are heated to reflux at 60 DEG C, while agitator is stirred
Rotating speed is 60rpm, forms transparence lanthanium titanate colloidal sol.
Step 2：Ceramic fibre is covered with paint, lacquer, colour wash, etc..
Step 2.1：Lanthanium titanate colloidal sol prepared by step 1.4 is poured into large beaker, by ceramic fibre（300 mm long, directly
The mm of footpath 1）3 min in lanthanium titanate colloidal sol are immersed in, lanthanium titanate colloidal sol is then vertically lifted out.
Step 2.2：Ceramic fibre is vertically stood to surface solidification at ambient temperature, by its on porcelain dish disk into circle
Shape, is then put in 85 DEG C of constant temperature electric heating drying boxes, and complete gel solidification is reached through 24 h.
Step 3：Calcined oxide treatment.
Step 3.1：The ceramic fibre for having coated lanthanium titanate gel prepared by step 2.2 is put in program control box together with porcelain dish
In electric furnace, by program control cabinet-type electric furnace temperature control at 750 DEG C, calcined oxide processes 3 h in atmosphere.Calcining terminates material
Taken out after being cooled to room temperature, you can soft lanthanium titanate fibrous material is obtained.
Embodiment 2
A kind of preparation method of soft lanthanium titanate fiber, including following processing steps：
Step 1：Synthesis lanthanium titanate colloidal sol.
Step 1.1：180 mL absolute ethyl alcohols, 80 mL acetone and 30 mL pairs are added in 500 mL three neck round bottom flask
Dimethylbenzene, loads onto agitator, temperature thermocouple and spherical condensation tube, and spherical condensation tube connection running water plays cooling effect.Will
500 mL three neck round bottom flask are in constant temperature electric heating bag.
Step 1.2：Solution temperature is 60 DEG C in keeping 500 mL three neck round bottom flask, continuous heating 30 min of backflow,
Agitator speed of agitator is 60rpm simultaneously, is subsequently added 37 mL metatitanic acid isopropyls alcohol esters, 3.8 mL tri-tert isopropyl ammoniums
25%（Mass percent）Ethanol solution and 3.2 mL directed agents ART-113, keep solution temperature for 60 DEG C are heated to reflux 30
Min, while agitator speed of agitator is 60rpm, forms the first solution.
Step 1.3：200 mL beakers are placed in magnetic-mixing constant temperature water bath boiler, to adding 63 mL in 200 mL beakers
Distilled water, it is 60 DEG C to keep water-bath water temperature.By 6.2 g lanthanum nitrates, 2.5 g ammonium chlorides, 2.6 g sodium oxalates and 1.6 g dispersion
Agent TO-125 is separately added into distilled water, is continuously stirred up to all substances are completely dissolved, and forms the second solution.
Step 1.4：During the second solution is added into the first solution in 500 mL three neck round bottom flask, 0.2g is added anhydrous
Citric acid, installs agitator, temperature thermocouple and spherical condensation tube, and 30 min are heated to reflux at 60 DEG C, while agitator is stirred
Rotating speed is 60rpm, forms transparence lanthanium titanate colloidal sol.
Step 2：Ceramic fibre is covered with paint, lacquer, colour wash, etc..
Step 2.1：Lanthanium titanate colloidal sol prepared by step 1.4 is poured into large beaker, by ceramic fibre（300 mm long, directly
The mm of footpath 1）3 min in lanthanium titanate colloidal sol are immersed in, lanthanium titanate colloidal sol is then vertically lifted out.
Step 2.2：Ceramic fibre is vertically stood to surface solidification at ambient temperature, by its on porcelain dish disk into circle
Shape, is then put in 85 DEG C of constant temperature electric heating drying boxes, and complete gel solidification is reached through 24 h.
Step 3：Calcined oxide treatment.
Step 3.1：The ceramic fibre for having coated lanthanium titanate gel prepared by step 2.2 is put in program control box together with porcelain dish
In electric furnace, by program control cabinet-type electric furnace temperature control at 800 DEG C, calcined oxide processes 4 h in atmosphere.Calcining terminates material
Taken out after being cooled to room temperature, you can soft lanthanium titanate fibrous material is obtained.
Embodiment 3
A kind of preparation method of soft lanthanium titanate fiber, including following processing steps：
Step 1：Synthesis lanthanium titanate colloidal sol.
Step 1.1：190 mL absolute ethyl alcohols, 85 mL acetone and 33 mL are added to two in 500 mL three neck round bottom flask
Toluene, loads onto agitator, temperature thermocouple and spherical condensation tube, and spherical condensation tube connection running water plays cooling effect.By 500
ML three neck round bottom flask is placed in constant temperature electric heating bag.
Step 1.2：Solution temperature is 60 DEG C in keeping 500 mL three neck round bottom flask, continuous heating 30 min of backflow,
Agitator speed of agitator is 60rpm simultaneously, is subsequently added 39 mL metatitanic acid isopropyls alcohol esters, 3.9 mL tri-tert isopropyl ammoniums
25%（Mass percent）Ethanol solution and 3.3 mL directed agents ART-113, keep solution temperature for 60 DEG C are heated to reflux 30
Min, while the rotating speed of agitator is 60rpm, forms the first solution.
Step 1.3：200 mL beakers are placed in magnetic-mixing constant temperature water bath boiler, to adding 65 mL in 200 mL beakers
Distilled water, it is 60 DEG C to keep water-bath water temperature.By 6.3 g lanthanum nitrates, 2.6 g ammonium chlorides, 2.7 g sodium oxalates and 1.7 g dispersion
Agent TO-125 is separately added into distilled water, is continuously stirred up to all substances are completely dissolved, and forms the second solution.
Step 1.4：During the second solution is added into the first solution in 500 mL three neck round bottom flask, 0.3g is added anhydrous
Citric acid, installs agitator, temperature thermocouple and spherical condensation tube, and 30 min are heated to reflux at 60 DEG C, while agitator is stirred
Rotating speed is 60rpm, forms transparence lanthanium titanate colloidal sol.
Step 2：Ceramic fibre is covered with paint, lacquer, colour wash, etc..
Step 2.1：Lanthanium titanate colloidal sol prepared by step 1.4 is poured into large beaker, by ceramic fibre（300 mm long, directly
The mm of footpath 1）3 min in lanthanium titanate colloidal sol are immersed in, lanthanium titanate colloidal sol is then vertically lifted out.
Step 2.2：Ceramic fibre is vertically stood to surface solidification at ambient temperature, by its on porcelain dish disk into circle
Shape, is then put in 85 DEG C of constant temperature electric heating drying boxes, and complete gel solidification is reached through 24 h.
Step 3：Calcined oxide treatment
Step 3.1：The ceramic fibre for having coated lanthanium titanate gel prepared by step 2.2 is put in program control cabinet-type electric furnace together with porcelain dish
In, by program control cabinet-type electric furnace temperature control at 950 DEG C, calcined oxide processes 5 h in atmosphere.Calcining terminates to cool down material
Taken out after to room temperature, you can soft lanthanium titanate fibrous material is obtained.
The agitator used in above three embodiment can be electric mixer.
Claims (1)
1. a kind of preparation method of soft lanthanium titanate fiber, it is characterised in that：Including following processing steps：
Step 1：Synthesis lanthanium titanate colloidal sol；
Step 1.1：170 ~ 190 mL absolute ethyl alcohols, 75 ~ 85 mL acetone and 26 ~ 33 mL pairs are added in three neck round bottom flask
Dimethylbenzene, then loads onto agitator, temperature thermocouple and spherical condensation tube, and spherical condensation tube connection running water, three mouthfuls of round bottoms burn
Bottle is placed in constant temperature electric heating bag；
Step 1.2：Solution temperature is 60 DEG C in keeping three neck round bottom flask, continuous heating 30 min of backflow, while stirring, with
36 ~ 39 mL metatitanic acid isopropyls alcohol esters, 25% ethanol solution and 3.1 ~ 3.3 of 3.7 ~ 3.9 mL tri-tert isopropyl ammoniums are added afterwards
ML directed agents ART-113, are heated to reflux 30 min, while stirring, forms the first solution；Described percentage is quality percentage
Number；
Step 1.3：Beaker is placed in magnetic-mixing constant temperature water bath boiler, to 61 ~ 65 mL distilled water are added in beaker, water is kept
Bath water temperature is 60 DEG C；By 6.1 ~ 6.3 g lanthanum nitrates, 2.5 ~ 2.6 g ammonium chlorides, 2.5 ~ 2.7 g sodium oxalates and 1.6 ~ 1.7 g points
Powder TO-125 is separately added into distilled water, and stirring forms the second solution to being completely dissolved；
Step 1.4：During the second solution is added into the first solution in three neck round bottom flask, the anhydrous lemons of 0.1-0.3g are added
Acid, installs agitator, temperature thermocouple and spherical condensation tube, and 30 min are heated to reflux at 60 DEG C, while stirring, forms transparent
Shape lanthanium titanate colloidal sol；
Step 2：Ceramic fibre is covered with paint, lacquer, colour wash, etc.；
Step 2.1：Lanthanium titanate colloidal sol prepared by step 1.4 is poured into beaker, and ceramic fibre is immersed in 3 in lanthanium titanate colloidal sol
Min, then vertically lifts out lanthanium titanate colloidal sol；
Step 2.2：Ceramic fibre is vertically stood to surface solidification at ambient temperature, 85 DEG C of constant temperature electric heatings is then put in and is done
In dry case, complete gel solidification is reached through 24 h；
Step 3：Calcined oxide treatment；
Step 3.1：The ceramic fibre for having coated lanthanium titanate gel prepared by step 2.2 is put in electric furnace, by furnace temperature control
At 750 ~ 950 DEG C, calcined oxide processes 3 ~ 5 h to system in atmosphere；Calcining terminates to be taken out after material is cooled into room temperature, you can
Soft lanthanium titanate fibrous material is obtained.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107096522A (en) * | 2017-06-05 | 2017-08-29 | 沈阳理工大学 | A kind of preparation method and applications for the ceramic fiber cloth for covering with paint, lacquer, colour wash, etc. bismuth titanates |
| 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 |
| CN108314079A (en) * | 2018-04-10 | 2018-07-24 | 四川大学 | A kind of regulation and control lanthanium titanate La2Ti2O7（LTO）The method of powder size |
| CN108435125A (en) * | 2018-05-17 | 2018-08-24 | 沈阳理工大学 | A kind of preparation method of self-cleaning ceramic cordage |
| CN109382089A (en) * | 2018-11-15 | 2019-02-26 | 沈阳理工大学 | A kind of preparation method of automatically cleaning fiber |
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| CN105797707A (en) * | 2016-04-14 | 2016-07-27 | 沈阳理工大学 | Method for preparing mesoporous titanic acid lanthanum zinc photocatalyst |
| CN105944710A (en) * | 2016-05-20 | 2016-09-21 | 沈阳理工大学 | Quartz sand supported lanthanum titanate photocatalyst and method for preparing same |
| CN106040225A (en) * | 2016-05-24 | 2016-10-26 | 沈阳理工大学 | Thin-layered bismuth titanate material and preparation method thereof |
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| CN105797707A (en) * | 2016-04-14 | 2016-07-27 | 沈阳理工大学 | Method for preparing mesoporous titanic acid lanthanum zinc photocatalyst |
| CN105944710A (en) * | 2016-05-20 | 2016-09-21 | 沈阳理工大学 | Quartz sand supported lanthanum titanate photocatalyst and method for preparing same |
| CN106040225A (en) * | 2016-05-24 | 2016-10-26 | 沈阳理工大学 | Thin-layered bismuth titanate material and preparation method thereof |
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| CN107096522A (en) * | 2017-06-05 | 2017-08-29 | 沈阳理工大学 | A kind of preparation method and applications for the ceramic fiber cloth for covering with paint, lacquer, colour wash, etc. bismuth titanates |
| 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 |
| CN108314079A (en) * | 2018-04-10 | 2018-07-24 | 四川大学 | A kind of regulation and control lanthanium titanate La2Ti2O7（LTO）The method of powder size |
| CN108435125A (en) * | 2018-05-17 | 2018-08-24 | 沈阳理工大学 | A kind of preparation method of self-cleaning ceramic cordage |
| CN109382089A (en) * | 2018-11-15 | 2019-02-26 | 沈阳理工大学 | A kind of preparation method of automatically cleaning fiber |
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