CN107352580A - One kind prepares black TiO using bean dregs2The method of nano material - Google Patents

One kind prepares black TiO using bean dregs2The method of nano material Download PDF

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Publication number
CN107352580A
CN107352580A CN201710644899.4A CN201710644899A CN107352580A CN 107352580 A CN107352580 A CN 107352580A CN 201710644899 A CN201710644899 A CN 201710644899A CN 107352580 A CN107352580 A CN 107352580A
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CN
China
Prior art keywords
nano material
bean dregs
black tio
tio
institute
Prior art date
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Pending
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CN201710644899.4A
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Chinese (zh)
Inventor
李兆乾
莫立娥
胡林华
戴松元
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Hefei Institutes of Physical Science of CAS
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Hefei Institutes of Physical Science of CAS
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Priority to CN201710644899.4A priority Critical patent/CN107352580A/en
Publication of CN107352580A publication Critical patent/CN107352580A/en
Pending legal-status Critical Current

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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
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses one kind black TiO is prepared using bean dregs2The method of nano material, by being added under being stirred after the grinding of the bean dregs after drying in the mixed liquor being made up of titanium source and absolute ethyl alcohol, lower natural drying is stirred, black TiO is then thermally treated resulting at 450 500 DEG C2Nano material.The preparation method of the present invention has the advantages of method is simple, yield is high.Black TiO prepared by the inventive method2Nano material is with a wide range of applications in fields such as photocatalysis, lithium ion battery, ultracapacitors.

Description

One kind prepares black TiO using bean dregs2The method of nano material
Technical field
The present invention relates to technical field of inorganic nanometer material, more particularly to one kind to prepare black TiO2 nanometer materials using bean dregs The method of material.
Background technology
Semiconductor energy band structure, band gap width etc. have decisive role for the optical property of semi-conducting material.Therefore, In recent years, narrow band gap, the semi-conducting material with visible light-responded performance cause the extensive concern of people.TiO2As most There are application prospect, the most commonly used semi-conducting material of research, due to its greater band gap (3.2eV), can only absorb that to account for sunshine total The ultraviolet light of energy 5%, cause the utilization rate of sunshine very low.Therefore, to TiO2Materials band structure is modified, and design is closed Into narrow band gap, continuous band gap TiO2Micro Nano material is TiO in the last few years2One important directions of research, organic to light degradation/ Inorganic pollution, photolysis water hydrogen etc. are significant.
Due to narrow band gap, all visible rays, recent years, black TiO can be absorbed2Excite the research heat of people Feelings.Such as Chen XB are in H2To TiO in atmosphere2Nano-particle material surface is modified processing, has obtained nano grain surface Disordering, the black TiO with continuous band gap2, its spectral response is extended to 1200 nm, and band gap is reduced to about 1eV, shown Fabulous light degradation and photocatalysis hydrogen production performance.Naldani etc. equally using H2 handle by the way of obtain band gap width ~ 1.85eV black TiO2Nano material, and have studied in detail its Crack cause and defect state distribution.Wang etc. is in different temperatures Under the conditions of to TiO2Nano wire carries out H2Processing has obtained the TiO that color is gradually changed by yellow to black2Nano-material, and Obtain good photocatalytic water performance.In the recent period, Zhao Dongyuan seminars are obtained black using the method for heat treatment hydrogenation presoma again The order mesoporous TiO of color2。
Prepare black TiO at present2Nano material method be all using surface hydriding processing by the way of, generally it is comparatively laborious and It is difficult to be prepared on a large scale, greatly hinders black TiO2Applications to nanostructures develops.Therefore, easy-to-use black is developed TiO2The preparation method of nano material is significant.Bean dregs are a kind of common life raw materials, safe and non-toxic, have biology Loose structure, itself is made up of organic matter, therefore can be using bean dregs come to TiO2Band structure is modified, design prepare it is narrow Band gap TiO2Nano material.In the present invention, we are prepared for black TiO using bean dregs householder method2Nano material, method letter Easy row, it can be prepared on a large scale.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided one kind prepares black TiO using bean dregs2Nanometer The method of material.
The present invention is achieved by the following technical solutions：
One kind prepares black TiO using bean dregs2The method of nano material, comprises the following steps：
It is added under being stirred after bean dregs grinding after drying in the mixed liquor being made up of titanium source and absolute ethyl alcohol, stirs lower nature Dry, be then heat-treated at 450-500 DEG C, produce black TiO2Nano material.
Described drying condition is 200-250 DEG C, 12-24h.
The mass ratio of the titanium source and absolute ethyl alcohol is 1：（1-2）.
The titanium source is tetraisopropyl titanate.
The bean dregs are yellow, and loose and porous structure, bean dregs grain diameter size is 1-100 μm.
The heat treatment time is 1-2h.
The black TiO that this method is obtained2Nano material is used for photocatalysis degradation organic contaminant, the purposes of photocatalytic water.
It is an advantage of the invention that：
Compared with present synthetic technology, the present invention prepares material using bean dregs as auxiliary, and ethanol is solvent, by simply mixed Close, stir, drying, heat treatment step can obtain black TiO2Nano material.Synthetic method of the present invention has technique simple, former Expect cheap and easily-available, nontoxic, the advantages of can preparing in batches.The black TiO that the present invention synthesizes2Nano material is in lithium ion battery, super The fields such as level capacitor, photocatalysis have a wide range of applications.
Brief description of the drawings
Fig. 1 is bean dregs raw material (a) used and gained sample (b)；
Fig. 2 is the SEM image of gained sample；
Fig. 3 is the XRD spectra of gained sample.
Embodiment
Embodiment 1：
After the bean dregs that yellow, loose and porous structure and the grain diameter size of the drying 12 hours at 200 DEG C are 1-100 μm are ground It is added under stirring in the mixed liquor being made up of 10g tetraisopropyl titanates and 10g absolute ethyl alcohols, stirs lower natural drying, then It is heat-treated 1 hour at 450 DEG C, obtains 4.5g samples.Fig. 1-3 shows the analysis test result of sample.Fig. 1 left sides are beans used Slag raw material, the right are gained sample, it can be seen that the color sample after processing is black.Fig. 2 shows the SEM figures of gained sample Picture.Fig. 3 is the XRD spectra of gained sample, itself and standard card is compared, it can be seen that gained sample is pure Anatase TiO2。

Claims (8)

1. one kind prepares black TiO using bean dregs2The method of nano material, it is characterised in that comprise the following steps：
It is added under being stirred after bean dregs grinding after drying in the mixed liquor being made up of titanium source and absolute ethyl alcohol, stirs lower nature Dry, be then heat-treated at 450-500 DEG C, produce black TiO2Nano material.
2. one kind according to claim 1 prepares black TiO using bean dregs2The method of nano material, it is characterised in that institute The drying condition stated is 200-250 DEG C, 12-24h.
3. one kind according to claim 1 prepares black TiO using bean dregs2The method of nano material, it is characterised in that institute The mass ratio for stating titanium source and absolute ethyl alcohol is 1：（1-2）.
4. one kind according to claim 1 prepares black TiO using bean dregs2The method of nano material, it is characterised in that institute It is tetraisopropyl titanate to state titanium source.
5. one kind according to claim 1 prepares black TiO using bean dregs2The method of nano material, it is characterised in that institute It is yellow to state bean dregs, and loose and porous structure, bean dregs grain diameter size is 1-100 μm.
6. one kind according to claim 1 prepares black TiO using bean dregs2The method of nano material, it is characterised in that institute It is 1-2h to state heat treatment time.
7. black TiO prepared by claim 1-6 method2Nano material, it is characterised in that the nano-grain particle diameter chi Very little is 100nm-10 μm.
8. the black TiO described in claim 72Nano material is used for photocatalysis degradation organic contaminant, the purposes of photocatalytic water.
CN201710644899.4A 2017-08-01 2017-08-01 One kind prepares black TiO using bean dregs2The method of nano material Pending CN107352580A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710644899.4A CN107352580A (en) 2017-08-01 2017-08-01 One kind prepares black TiO using bean dregs2The method of nano material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710644899.4A CN107352580A (en) 2017-08-01 2017-08-01 One kind prepares black TiO using bean dregs2The method of nano material

Publications (1)

Publication Number Publication Date
CN107352580A true CN107352580A (en) 2017-11-17

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4284521A (en) * 1979-03-26 1981-08-18 Ferro Corporation Reduced alkaline earth metal powders and process for producing same
CN1169956A (en) * 1996-07-08 1998-01-14 同济大学 Manufacture of black titanium oxide
CN1930250A (en) * 2004-04-07 2007-03-14 克罗内斯国际公司 Carbon-containing, titanium dioxide-based photocatalyst, and process for producing the same
CN1974000A (en) * 2006-12-21 2007-06-06 天津大学 Method of preparing C-doped porous nanometer TiO2 photocatalyst with egg shell membrane as template
CN105126796A (en) * 2015-07-13 2015-12-09 华北电力大学 Preparation method of fluorine-doped lamellar black titanium dioxide nano material
CN106745222A (en) * 2017-03-14 2017-05-31 上海友兰科技有限公司 A kind of method that black titanium dioxide is largely uniformly prepared
CN106892482A (en) * 2017-01-04 2017-06-27 浙江工业大学 A kind of black TiO2Nano material and preparation method and application

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4284521A (en) * 1979-03-26 1981-08-18 Ferro Corporation Reduced alkaline earth metal powders and process for producing same
CN1169956A (en) * 1996-07-08 1998-01-14 同济大学 Manufacture of black titanium oxide
CN1930250A (en) * 2004-04-07 2007-03-14 克罗内斯国际公司 Carbon-containing, titanium dioxide-based photocatalyst, and process for producing the same
CN1974000A (en) * 2006-12-21 2007-06-06 天津大学 Method of preparing C-doped porous nanometer TiO2 photocatalyst with egg shell membrane as template
CN105126796A (en) * 2015-07-13 2015-12-09 华北电力大学 Preparation method of fluorine-doped lamellar black titanium dioxide nano material
CN106892482A (en) * 2017-01-04 2017-06-27 浙江工业大学 A kind of black TiO2Nano material and preparation method and application
CN106745222A (en) * 2017-03-14 2017-05-31 上海友兰科技有限公司 A kind of method that black titanium dioxide is largely uniformly prepared

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
徐蕾等: "《负载型多酸光催化材料及其应用》", 31 March 2015, 东北师范大学出版社 *

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Application publication date: 20171117