CN108837833A - Fe adulterates TiO2The preparation of catalyst - Google Patents

Fe adulterates TiO2The preparation of catalyst Download PDF

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Publication number
CN108837833A
CN108837833A CN201810696749.2A CN201810696749A CN108837833A CN 108837833 A CN108837833 A CN 108837833A CN 201810696749 A CN201810696749 A CN 201810696749A CN 108837833 A CN108837833 A CN 108837833A
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China
Prior art keywords
beaker
product
glucose
hours
time
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Withdrawn
Application number
CN201810696749.2A
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杜佳璇
温沅楹
郝小萌
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Yantai Zhiben Intellectual Property Operation and Management Co Ltd
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Yantai Zhiben Intellectual Property Operation and Management Co Ltd
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Priority to CN201810696749.2A priority Critical patent/CN108837833A/en
Publication of CN108837833A publication Critical patent/CN108837833A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/745Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to a kind of Fe to adulterate TiO2The preparation of catalyst, the present invention adulterates a small amount of iron into nano-titanium dioxide, by the sample of doping compared with pure titinium dioxide, the absorption region of light widens into visible-range, the electron-hole recombination probability of generation is also because the doping of iron is effectively reduced, it is modified that iron ion doping is carried out to titanium deoxide catalyst, it can reach the purpose for improving photocatalytic activity of the titanium deoxide catalyst in visible-range, to verify the nano-titanium dioxide of Fe2O3 doping in visible-range, there is good photoresponse photocatalytic activities.

Description

Fe adulterates TiO2The preparation of catalyst
Technical field
The present invention relates to Fe to adulterate TiO2The preparation of catalyst belongs to chemical material field.
Technical background
Titanium dioxide is a kind of transition metal oxide, and crystal state, partial size and chemical component are to TiO2It is relatively close Degree has different influences.In three kinds of various forms of structures of titanium dioxide, most stable of rutile-type, compared with anatase facies pattern and The anatase titanium dioxide of plate has intensive structure feature, to show on hardness, density and index of refraction more preferable Characteristic.Rutile type titanium white is with good stability and relative density is larger, because this 2 titania molecules are constituted Rutile titanium dioxide elementary cell, and anatase titanium dioxide is made of 4 titania molecules.Rutile type titanium White powder has smaller, more compact elementary cell, refractive index with higher and dielectric constant and low heat conductivity.Titanium dioxide is certainly The design feature of body determines its dielectric constant with higher, so showing good characteristic in terms of electrology characteristic.When When semiconductor titanium dioxide is placed in external electric field, because of the interaction between its inner ion, very strong internal electric field is generated, from And lead to the deformation of electron orbit appearance largely outside ion, while ion itself is also affected and generates larger Position move.Rutile TiO2Dielectric constant it is related with the deviation of crystal, such as:Work as TiO2When crystal is parallel to c, Dielectric constant is 180;When crystal is in three shaft angles, dielectric constant 90, average crystalline powder is 114.
Summary of the invention
The present invention relates to a kind of Fe to adulterate TiO2The preparation of catalyst, preparation process include:2.7g glucose is accurately weighed, 35ml deionized water is added into the beaker for fill glucose, the beaker equipped with glucose solution is placed in ultrasonic cleaner Middle ultrasound 15-30min 0.25mmol titanium sulfate is first added into above-mentioned beaker, then again until glucose all dissolution 0.25mmol ferric nitrate is added into beaker, takes 50ml hydrothermal reaction kettle, take out polytetrafluoroethyllining lining cleaned with deionized water, Ultrasound is simultaneously dried, and prepared solution is fitted into the polytetrafluoroethyllining lining of 50ml, liner is fitted into hydrothermal reaction kettle simultaneously Close sealing, is put into 180 degrees Celsius of electric heating constant-temperature blowing drying box and is fired, and the control firing time is 16-22 hours, It is cooled to room temperature, is first cleaned with deionized water, is then then transferred in centrifuge tube, adjusting electric centrifuge revolving speed is 2500 turns, Centrifugation 3-5 minutes every time repeat aforesaid operations three times, and washing is washed secondary with dehydrated alcohol later three times, and centrifuge speed is 2000 turns, centrifugation 2-4 minutes, take out the precipitated product in centrifuge tube, are transferred in small beaker, product is existed with glass bar every time Beaker bottom tiling is come, and the small beaker for filling product is transferred in 80 DEG C of baking oven, is dried 12 hours, waits until drying time Terminate, take out product and be put into mortar, product is ground to powdered white powder in collection mortar, is poured into crucible, Crucible is placed in Muffle furnace and is fired 3 hours, temperature control is 500 DEG C, final to obtain white product.
The present invention adulterates a small amount of iron into nano-titanium dioxide, by the sample of doping compared with pure titinium dioxide, light Absorption region widens into visible-range, and the electron-hole recombination probability of generation is also because the doping of iron is effectively reduced. Iron ion doping is carried out to titanium deoxide catalyst to be modified, and be can reach and is improved titanium deoxide catalyst in visible-range The purpose of photocatalytic activity.To verify the nano-titanium dioxide of Fe2O3 doping in visible-range, there is good light to ring Answer photocatalytic activity.
Specific embodiment
Below in conjunction with specific embodiment in the present invention principle and feature be described, example is intended merely to pair Further explanation explanation of the present invention, is not supposed to be a limitation to the present invention.
Embodiment 1
2.7g glucose is accurately weighed, 35ml deionized water is added into the beaker for fill glucose, glucose will be housed The beaker of solution is placed in ultrasound 15min in ultrasonic cleaner, until glucose all dissolution, first into above-mentioned beaker 0.25mmol titanium sulfate is added, 0.25mmol ferric nitrate is then added into beaker again, takes 50ml hydrothermal reaction kettle, takes out poly- four Vinyl fluoride liner cleans with deionized water, ultrasound and dries, and prepared solution is fitted into the polytetrafluoroethyllining lining of 50ml, Liner is fitted into hydrothermal reaction kettle and is closely sealed, is put into 180 degrees Celsius of electric heating constant-temperature blowing drying box and is fired, Controlling the firing time is 16 hours, is cooled to room temperature, is first cleaned with deionized water, is then then transferred in centrifuge tube, adjusts electricity Dynamic centrifuge speed is 2500 turns, every time centrifugation 3 minutes, repeats aforesaid operations three times, is washed after washing three times with dehydrated alcohol Wash it is secondary, centrifuge speed be 2000 turns, every time centrifugation 2 minutes, take out centrifuge tube in precipitated product, be transferred to small beaker It is interior, product is come in beaker bottom tiling with glass bar, the small beaker for filling product is transferred in 80 DEG C of baking oven, is dried It 12 hours, until drying time terminates, takes out product and is put into mortar, product is ground to powdered, collect white in mortar Color powder, pours into crucible, and crucible is placed in Muffle furnace and is fired 3 hours, and temperature control is 500 DEG C, final to obtain white production Object.
Embodiment 2
2.7g glucose is accurately weighed, 35ml deionized water is added into the beaker for fill glucose, glucose will be housed The beaker of solution is placed in ultrasound 30min in ultrasonic cleaner, until glucose all dissolution, first into above-mentioned beaker 0.25mmol titanium sulfate is added, 0.25mmol ferric nitrate is then added into beaker again, takes 50ml hydrothermal reaction kettle, takes out poly- four Vinyl fluoride liner cleans with deionized water, ultrasound and dries, and prepared solution is fitted into the polytetrafluoroethyllining lining of 50ml, Liner is fitted into hydrothermal reaction kettle and is closely sealed, is put into 180 degrees Celsius of electric heating constant-temperature blowing drying box and is fired, Controlling the firing time is 22 hours, is cooled to room temperature, is first cleaned with deionized water, is then then transferred in centrifuge tube, adjusts electricity Dynamic centrifuge speed is 2500 turns, every time centrifugation 5 minutes, repeats aforesaid operations three times, is washed after washing three times with dehydrated alcohol Wash it is secondary, centrifuge speed be 2000 turns, every time centrifugation 4 minutes, take out centrifuge tube in precipitated product, be transferred to small beaker It is interior, product is come in beaker bottom tiling with glass bar, the small beaker for filling product is transferred in 80 DEG C of baking oven, is dried It 12 hours, until drying time terminates, takes out product and is put into mortar, product is ground to powdered, collect white in mortar Color powder, pours into crucible, and crucible is placed in Muffle furnace and is fired 3 hours, and temperature control is 500 DEG C, final to obtain white production Object.
Embodiment 3
2.7g glucose is accurately weighed, 35ml deionized water is added into the beaker for fill glucose, glucose will be housed The beaker of solution is placed in ultrasound 20min in ultrasonic cleaner, until glucose all dissolution, first into above-mentioned beaker 0.25mmol titanium sulfate is added, 0.25mmol ferric nitrate is then added into beaker again, takes 50ml hydrothermal reaction kettle, takes out poly- four Vinyl fluoride liner cleans with deionized water, ultrasound and dries, and prepared solution is fitted into the polytetrafluoroethyllining lining of 50ml, Liner is fitted into hydrothermal reaction kettle and is closely sealed, is put into 180 degrees Celsius of electric heating constant-temperature blowing drying box and is fired, Controlling the firing time is 20 hours, is cooled to room temperature, is first cleaned with deionized water, is then then transferred in centrifuge tube, adjusts electricity Dynamic centrifuge speed is 2500 turns, every time centrifugation 4 minutes, repeats aforesaid operations three times, is washed after washing three times with dehydrated alcohol Wash it is secondary, centrifuge speed be 2000 turns, every time centrifugation 3 minutes, take out centrifuge tube in precipitated product, be transferred to small beaker It is interior, product is come in beaker bottom tiling with glass bar, the small beaker for filling product is transferred in 80 DEG C of baking oven, is dried It 12 hours, until drying time terminates, takes out product and is put into mortar, product is ground to powdered, collect white in mortar Color powder, pours into crucible, and crucible is placed in Muffle furnace and is fired 3 hours, and temperature control is 500 DEG C, final to obtain white production Object.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention range, all in the present invention Spirit and principle within, any modification, equivalent substitution, improvement and etc. done be somebody's turn to do included in protection scope of the present invention Within.

Claims (2)

1.Fe adulterates TiO2The preparation of catalyst, which is characterized in that preparation process includes:2.7g glucose is accurately weighed, to filling 35ml deionized water is added in the beaker of glucose, the beaker equipped with glucose solution is placed in ultrasonic cleaner ultrasonic 15-30min 0.25mmol titanium sulfate is first added into above-mentioned beaker, then again to beaker until glucose all dissolution Middle addition 0.25mmol ferric nitrate, takes 50ml hydrothermal reaction kettle, take out polytetrafluoroethyllining lining clean with deionized water, it is ultrasonic simultaneously Drying, prepared solution is fitted into the polytetrafluoroethyllining lining of 50ml, liner is fitted into hydrothermal reaction kettle and is closely sealed Mouthful, it is put into 180 degrees Celsius of electric heating constant-temperature blowing drying box and is fired, the control firing time is 16-22 hours, is cooled to Room temperature is first cleaned with deionized water, is then then transferred in centrifuge tube, adjust electric centrifuge revolving speed be 2500 turns, every time from The heart 3-5 minutes, repeat aforesaid operations three times, washing three times after wash with dehydrated alcohol it is secondary, centrifuge speed be 2000 turns, Centrifugation 2-4 minutes every time are taken out the precipitated product in centrifuge tube, are transferred in small beaker, with glass bar product in bottom of the beaker Portion's tiling is come, and the small beaker for filling product is transferred in 80 DEG C of baking oven, is dried 12 hours, until drying time terminates, It takes out product to be put into mortar, product is ground to powdered white powder in collection mortar, is poured into crucible, by earthenware Crucible is placed in Muffle furnace and fires 3 hours, and temperature control is 500 DEG C, final to obtain white product.
2. preparation method according to claim 1, which is characterized in that burning the only time is 16-22 hours.
CN201810696749.2A 2018-06-29 2018-06-29 Fe adulterates TiO2The preparation of catalyst Withdrawn CN108837833A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115073119A (en) * 2022-06-24 2022-09-20 昆明理工大学 Visible light catalytic light-transmitting concrete material and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102794164A (en) * 2012-07-19 2012-11-28 湖南先科环保有限公司 Preparation method of magnetic doped nano titanium dioxide
CN103537286A (en) * 2013-10-28 2014-01-29 湛江师范学院 Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder
CN107335434A (en) * 2017-06-15 2017-11-10 河南科技学院 A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method
CN107552051A (en) * 2017-10-09 2018-01-09 河南科技学院 The nano-TiO of Fe doping2Application of the photochemical catalyst in p-nitrophenol of degrading

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102794164A (en) * 2012-07-19 2012-11-28 湖南先科环保有限公司 Preparation method of magnetic doped nano titanium dioxide
CN103537286A (en) * 2013-10-28 2014-01-29 湛江师范学院 Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder
CN107335434A (en) * 2017-06-15 2017-11-10 河南科技学院 A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method
CN107552051A (en) * 2017-10-09 2018-01-09 河南科技学院 The nano-TiO of Fe doping2Application of the photochemical catalyst in p-nitrophenol of degrading

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115073119A (en) * 2022-06-24 2022-09-20 昆明理工大学 Visible light catalytic light-transmitting concrete material and preparation method and application thereof

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