CN101164695A - Process for preparing supported nanometer titanium dioxide - Google Patents
Process for preparing supported nanometer titanium dioxide Download PDFInfo
- Publication number
- CN101164695A CN101164695A CNA2007100152150A CN200710015215A CN101164695A CN 101164695 A CN101164695 A CN 101164695A CN A2007100152150 A CNA2007100152150 A CN A2007100152150A CN 200710015215 A CN200710015215 A CN 200710015215A CN 101164695 A CN101164695 A CN 101164695A
- Authority
- CN
- China
- Prior art keywords
- preparation
- titania
- nano
- titanium
- porous
- 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.)
- Granted
Links
Images
Landscapes
- Catalysts (AREA)
Abstract
The present invention relates to a preparation method of load-type nano titanium dioxide, belonging to the field of inorganic functional material preparation technology. Said invention uses porous silica molecular sieve as host, and uses nano titanium dioxide as guest to prepare composite material, the size of guest material is limited by nano-grade pore channel of host material. Its concrete preparation method includes the following steps: firstly, preparing inorganic titanium salt aqueous solution whose concentration range is 6.25mmol/ml-375mmol/ml, using water or organic acid aqueous solution as solvent; adopting equivolume impregnation method to make them be introduced into porous material interior, storing the impregnated sample for 24hr at room temperature, moving the sample into a hydrothermal tank with Teflon liner, making hydrolysis for 0.5-4hr under the condition of temperature range with 80deg.C-120deg.C, then roasting at high temperature, roasting temperature is 500deg.C-700deg.C and roasting time is 2hr. so as to obtain the invented composite material with a certain photocatalytic activity. Said composite material can be used as organics photodegradation and catalyst carrier material.
Description
One, technical field
The present invention relates to a kind of preparation method of loading nano-titania, belong to the inorganic functional material preparation field.
Two, background technology
Nano titanium oxide is the environmentally friendly photochemical catalyst with good light catalytic activity, in order to improve the photocatalytic activity of titanium dioxide, its particle must be enough little so that the active site position to be provided, but this tiny nano material easily takes place to reunite and is difficult to and recycles.Nano particle is fixed in not only more to have in the duct of porous silica material by the back synthetic method disperses and be beneficial to recycling, and the size of pore size control nano particle that can be by porous material.
The introducing of titanium dioxide on the mesoporous carrier generally is by subject and object predecessor in the liquid phase.Realize that metallic compound fixing on mesoporous material generally has following three kinds of approach: ship construction method in direct grafting, indirect grafting, the bottle.Usually, the introducing of titanium dioxide nanoparticle is to utilize the hydrolysis of organic pure titanium salt in mesopore orbit to obtain, and this type of document has report frequently, and people such as Wei Wang are medium with the cyclohexane give, utilize titanium isopropoxide hydrolysis in the SBA-15 duct to make TiO
2Content is 24.4% material, and the multistep infusion process has effectively been controlled TiO
2Granular size also can improve TiO as far as possible
2Content, be applied to obtain good catalytic effect in the light degradation of estrogen and phenol.Human titanium isopropoxides such as A.M.Busuioc make nano-TiO as the hydrolysis in acid solution of titanium source
2, be applied in the Rhodamine 6G dyestuff degraded and analyzed the relation of absorption and the disposal efficiency.But as the titanium source, not only cost an arm and a leg, need organic solvent to be difficult to control with the organic titanium alkoxide, therefore select inorganic titanium salt to have low price, advantage such as easy and simple to handle as the hydrolysis predecessor as medium and hydrolysising condition.
Three, summary of the invention
At the deficiencies in the prior art, the invention provides the preparation method of a kind of inorganic titanium salt as the loading nano-titania of hydrolysis predecessor.
The present invention is based on the porous silicon molecular sieve, is the preparation method of the loading nano-titania of object with the nano titanium oxide, and the guest materials size is limited by the nanoscale duct of material of main part; Concrete steps are as follows:
The configuration concentration scope is the inorganic titanium saline solution of 6.25mmol/mL ~ 37.5mmol/mL, is solvent with water or aqueous solutions of organic acids; Adopt the incipient impregnation method will introduce porous material inside, the sample room temperature that dipping is good is transferred and was put 24 hours, immigration has in the hydro-thermal jar of poly-tetrafluoro liner, under 80 ℃ ~ 120 ℃ conditions of temperature range hydrolysis 0.5 ~ 4h hour, high-temperature roasting then, 500 ℃ ~ 700 ℃ of sintering temperatures, roasting time is 2 hours, must have the composite of certain photocatalytic activity.
Above-mentioned porous molecular sieve materials is SBA, MCM series mesopore molecular sieve, silica aerogel porous silica material.
Above-mentioned is that inorganic titanium salt is titanium sulfate and titanyl sulfate.
The above-mentioned loading nano-titania that makes is applied to organic light degradation and catalyst carrier material.
By means such as XRD, BET, TEM composite is characterized, the result shows that titanium dioxide granule is evenly distributed in porous material inside, and restriction is played to the growth of particle in the duct of rule.This composite is applied in the organic matter light degradation, respond well.
Four, description of drawings
Fig. 1 is main body SBA-15TEM figure, and Fig. 2 is single-steeping Ti: Si=1: composite TEM figure after 5, the 700 degree roastings, Fig. 3 are that complex carrier methyl orange light degradation effect commodity titanium dioxide P25 identical with Ti content and main body compare.
Five, the specific embodiment
Example 1:SBA-15 is a main body, and titanium sulfate solution is the object predecessor
Compound concentration is the titanium sulfate aqueous solution of 6g/10mL respectively, is designated as a) solution.With 1mL a) among the solution incipient impregnation 1gSBA-15, the SBA-15 that dipping is good transfers in the measuring cup, then measuring cup is put into and had 120 ℃ of hydrolysis 4h of teflon-lined hydro-thermal jar, in order to guarantee to be impregnated into the required moisture of titanium sulfate hydrolysis in the SBA-15 duct, in the hydro-thermal jar, pour in advance a small amount of with flood the identical titanium sulfate solution of used concentration.Getting titanium dioxide is 1: 5 sample with silica quality ratio.700 ℃ of roastings of sample of a load after two hours, are repeated above-mentioned dipping, hydrolysis, process again, carried titanium dioxide SBA-15 repeatedly, characterization result shows Ti: the Si ratio reaches at 2: 5 o'clock and still can not cause serious obstruction to the duct of main body own.
Example 2:SBA-15 is a main body, and titanium sulfate solution is the object predecessor
Compound concentration is the titanium sulfate solution of 3g/10mL respectively, is designated as a) solution.With 1mL a) the solution incipient impregnation in 1gSBA-15, the SBA-15 that dipping is good transfers in the measuring cup, then measuring cup is put into and had 120 ℃ of hydrolysis 4h of teflon-lined hydro-thermal jar, in order to guarantee to be impregnated into the required moisture of titanium sulfate hydrolysis in the SBA-15 duct, in the hydro-thermal jar, pour in advance a small amount of with flood the identical titanium sulfate solution of used concentration.700 ℃ of roastings of gained sample two hours, getting titanium dioxide is 1: 10 sample with silica quality ratio.
Example 3:SBA-15 is a main body, and titanyl sulfate solution is the object predecessor
Compound concentration is the titanyl sulfate solution of 4g/10mL respectively, is designated as a) solution.With 1mL a) among the solution incipient impregnation 1gSBA-15, the SBA-15 that dipping is good transfers in the measuring cup, then measuring cup is put into and had 120 ℃ of hydrolysis 4h of teflon-lined hydro-thermal jar, in order to guarantee to be impregnated into the required moisture of titanyl sulfate hydrolysis in the SBA-15 duct, in the hydro-thermal jar, pour in advance a small amount of with flood the identical titanium sulfate solution of used concentration.700 ℃ of roastings of gained sample two hours, getting titanium dioxide is 1: 5 sample with silica quality ratio.
Example 4:MCM-41 is a main body, and titanium sulfate solution is the object predecessor
Compound concentration is the titanium sulfate solution of 7.5g/10mL respectively, is designated as a) solution.With 0.8mL a) among the solution incipient impregnation 1gMCM-41, the MCM-41 that dipping is good transfers in the measuring cup, then measuring cup is put into and had 120 ℃ of hydrolysis 4h of teflon-lined hydro-thermal jar, in order to guarantee to be impregnated into the required moisture of titanium sulfate hydrolysis in the SBA-15 duct, in the hydro-thermal jar, pour in advance a small amount of with flood the identical titanium sulfate solution of used concentration.500 ℃ of roastings of gained sample two hours, getting titanium dioxide is 1: 5 sample with silica quality ratio.
Claims (4)
1. the preparation method of a loading nano-titania is characterized in that based on the porous silicon molecular sieve, is the method for the composite of object with the nano titanium oxide, and the guest materials size is limited by the nanoscale duct of material of main part; Concrete steps are as follows: the configuration concentration scope is the inorganic titanium saline solution of 6.25mmol/mL ~ 37.5mmol/mL, is solvent with water or aqueous solutions of organic acids; Adopt the incipient impregnation method will introduce porous material inside, the sample room temperature that dipping is good is transferred and was put 24 hours, immigration has in the hydro-thermal jar of poly-tetrafluoro liner, under 80 ℃ ~ 120 ℃ conditions of temperature range hydrolysis 0.5 ~ 4h hour, high-temperature roasting then, 500 ℃ ~ 700 ℃ of sintering temperatures, roasting time is 2 hours, must have the composite of certain photocatalytic activity.
2. the preparation method of a kind of loading nano-titania as claimed in claim 1 is characterized in that porous molecular sieve materials is SBA, MCM series mesopore molecular sieve, silica aerogel porous silica material.
3. the preparation method of a kind of loading nano-titania as claimed in claim 1 is characterized in that inorganic titanium salt is titanium sulfate and titanyl sulfate.
4. the preparation method of a kind of loading nano-titania as claimed in claim 1 is characterized in that the loading nano-titania that makes is applied to organic light degradation and catalyst carrier material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100152150A CN100556541C (en) | 2007-06-27 | 2007-06-27 | A kind of preparation method of loading nano-titania |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100152150A CN100556541C (en) | 2007-06-27 | 2007-06-27 | A kind of preparation method of loading nano-titania |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101164695A true CN101164695A (en) | 2008-04-23 |
| CN100556541C CN100556541C (en) | 2009-11-04 |
Family
ID=39333629
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100152150A Expired - Fee Related CN100556541C (en) | 2007-06-27 | 2007-06-27 | A kind of preparation method of loading nano-titania |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100556541C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102909045A (en) * | 2012-07-20 | 2013-02-06 | 天津城市建设学院 | Preparation method of micron-order load type TiO2 catalyst |
| CN104056656A (en) * | 2014-06-26 | 2014-09-24 | 沈阳理工大学 | Molecular sieve with photocatalystic purification function and preparation method thereof |
| CN104056616A (en) * | 2014-07-01 | 2014-09-24 | 崔洁心 | Method for preparing silica aerogel photocatalyst formed by compounding nanometer titanium oxide and rare earth solid solution |
| CN104138752A (en) * | 2014-07-01 | 2014-11-12 | 崔洁心 | Production device of nanometer titanium oxide and rare earth solid solution composite silica aerogel photocatalyst |
| CN105435764A (en) * | 2015-11-19 | 2016-03-30 | 上海应用技术学院 | Compound mesoporous photocatalyst and preparation method thereof |
| CN106540706A (en) * | 2016-10-26 | 2017-03-29 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of support type ozone catalyst and its preparation method and application |
| CN107537437A (en) * | 2017-09-29 | 2018-01-05 | 天津大学 | A kind of support type bi-component nano-oxide adsorbent, its preparation method and its application |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106423118A (en) * | 2016-11-08 | 2017-02-22 | 嘉善君圆新材料科技有限公司 | Photocatalytic composite material and preparation method thereof |
-
2007
- 2007-06-27 CN CNB2007100152150A patent/CN100556541C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102909045A (en) * | 2012-07-20 | 2013-02-06 | 天津城市建设学院 | Preparation method of micron-order load type TiO2 catalyst |
| CN104056656A (en) * | 2014-06-26 | 2014-09-24 | 沈阳理工大学 | Molecular sieve with photocatalystic purification function and preparation method thereof |
| CN104056616A (en) * | 2014-07-01 | 2014-09-24 | 崔洁心 | Method for preparing silica aerogel photocatalyst formed by compounding nanometer titanium oxide and rare earth solid solution |
| CN104138752A (en) * | 2014-07-01 | 2014-11-12 | 崔洁心 | Production device of nanometer titanium oxide and rare earth solid solution composite silica aerogel photocatalyst |
| CN104138752B (en) * | 2014-07-01 | 2016-05-18 | 崔洁心 | The process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide and rare earth solid solution |
| CN105435764A (en) * | 2015-11-19 | 2016-03-30 | 上海应用技术学院 | Compound mesoporous photocatalyst and preparation method thereof |
| CN105435764B (en) * | 2015-11-19 | 2017-09-29 | 上海应用技术学院 | A kind of compound mesoporous photocatalytic agent and preparation method thereof |
| CN106540706A (en) * | 2016-10-26 | 2017-03-29 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of support type ozone catalyst and its preparation method and application |
| CN106540706B (en) * | 2016-10-26 | 2019-04-16 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of support type ozone catalyst and its preparation method and application |
| CN107537437A (en) * | 2017-09-29 | 2018-01-05 | 天津大学 | A kind of support type bi-component nano-oxide adsorbent, its preparation method and its application |
| CN107537437B (en) * | 2017-09-29 | 2020-08-04 | 天津大学 | Supported bi-component nano oxide adsorbent, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100556541C (en) | 2009-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100556541C (en) | A kind of preparation method of loading nano-titania | |
| CN103028352B (en) | Preparation method for synthesizing MoS2/Fe3O4 nano composite material | |
| Kominami et al. | Correlation between some physical properties of titanium dioxide particles and their photocatalytic activity for some probe reactions in aqueous systems | |
| CN101293669B (en) | Method for preparing nano-titanium dioxide powder with controllable phase ratio of anatase and rutile | |
| Guo et al. | Biogenic Pt/CaCO3 nanocomposite as a robust catalyst toward benzene oxidation | |
| CN108295907B (en) | Composite visible light photocatalystAgent Ag2CO3/TiO2/UiO-66-(COOH)2Preparation method and application thereof | |
| CN105797762B (en) | A kind of photocatalysis haydite and preparation method and application | |
| CN103521163A (en) | Method for preparing nanometer composite with chrysanthemum structure | |
| CN103172030A (en) | Oxide powder and preparation method thereof as well as catalyst and carrier thereof | |
| CN106745226A (en) | Micro-nano titanium dioxide and preparation method and application based on eutectic solvent synthesis | |
| CN107456983A (en) | A kind of Ag/AgCl/TiO2Composite photocatalyst material and its preparation method and application | |
| CN101711977A (en) | Method for preparing mesoporous titanium dioxide photocatalyst by using microbes and algae as templates | |
| CN101791547A (en) | Method for preparing TiO2 nanocryatal/nanotube composite photocatalyst | |
| Palas et al. | Bioinspired metal oxide particles as efficient wet air oxidation and photocatalytic oxidation catalysts for the degradation of acetaminophen in aqueous phase | |
| CN104927097B (en) | A kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites | |
| CN102784632A (en) | Preparation method for infusorial earth/ titanium dioxide composite photocatalyst with nuclear/shell structure | |
| CN106423120A (en) | Preparation method of nanometer needle-shaped titanium dioxide B photocatalyst | |
| CN107983353A (en) | A kind of TiO2-Fe2O3The preparation method and applications of composite granule | |
| CN110227515B (en) | Bi2MoO6/BiPO4P-n heterojunction photocatalyst, preparation method and application thereof | |
| CN101863509A (en) | Rutile TiO2 nanowire array synthesized by soft chemistry and hydrothermal technology and preparation method thereof | |
| CN114602508A (en) | Preparation and application of MnS @ ZnS core-shell hollow sphere with photocatalytic performance | |
| CN103418416A (en) | Preparation method of nitrogen doping titanium dioxide powder, prepared titanium dioxide powder material and purpose thereof | |
| CN106000440A (en) | Preparation method of g-C3N4 quantum dot-loaded titanium dioxide nanoparticles | |
| CN104098133B (en) | Preparation method for high-efficient photocatalyst-nanometer titanium dioxide water-based colloid | |
| CN103214033B (en) | The preparation method of the controlled spherical mesoporous titanium dioxide of size |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091104 Termination date: 20120627 |