CN108097199A - BixFey-TiO2Nanocomposite and preparation method and application - Google Patents
BixFey-TiO2Nanocomposite and preparation method and application Download PDFInfo
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- CN108097199A CN108097199A CN201711362729.3A CN201711362729A CN108097199A CN 108097199 A CN108097199 A CN 108097199A CN 201711362729 A CN201711362729 A CN 201711362729A CN 108097199 A CN108097199 A CN 108097199A
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- 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
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- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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Abstract
The invention discloses a kind of BixFey‑TiO2Nanocomposite and preparation method and application, the BixFey‑TiO2Nanocomposite includes TiO2Base and it is entrained in TiO2Bi and Fe elements in base, wherein, x=0.01~0.20；And BixFey‑TiO2Nanocomposite is the mixing crystal form of anatase and rutile-type, wherein rutile content 50~90%, Detitanium-ore-type content 10~40%.Above-mentioned BixFey‑TiO2Nanocomposite specific surface area is more than routine TiO2, good dispersion, big specific surface area and good dispersiveness improve its ability in phosphorylating protein immobilization, and the metal ion of doping can generate chelation with phosphate groups, enrichment is played jointly with physical absorption.And it significantly improves phosphorylated polypeptide adsorbance in β caseins, being capable of effective as selective enriched phosphorus acidifying polypeptide.
Description
Technical field
Field of nanocomposite materials of the present invention, more particularly to BixFey-TiO2Nanocomposite.And preparation method and
Using.Especially also relate to BixFey-TiO2The preparation method and application of nanocomposite
Background technology
At present, mass-spectrometric technique is the prefered method of phosphorylating protein quantitative analysis and phosphorylation site positioning, still, by
It easily degrades in phosphorylating protein, the low shortcomings such as low with stoichiometry of content, so, study the phosphorylation egg before mass spectral analysis
The enrichment method of white matter is necessary.Now, for phosphorylating protein absorption carrier mainly have titanium dioxide, mesoporous silicon,
Polystyrene etc., wherein, nano-TiO2It is a kind of to possess excellent biocompatibility, chemical stability, cheap and nontoxic
Functional material is the ideal carrier for adsorbing large biological molecule.But conventional TiO2For specific surface area than low, agglomeration is bright
It is aobvious, limit to its application in terms of large biological molecule absorption to a certain extent.Therefore there is an urgent need for one kind have bigger serface,
The TiO of fine dispersion ability2Base novel functional nano-composites.
The content of the invention
Based on this, it is necessary to for conventional TiO2Specific surface area is than low, the problem of agglomeration is apparent, provides a kind of tool
There are bigger serface, the TiO of fine dispersion ability2Base novel functional nano-composites.
A kind of BixFey-TiO2Nanocomposite, BixFey-TiO2Nanocomposite includes TiO2It base and is entrained in
TiO2Bi and Fe elements in base, wherein, x=0.01~0.20, y=0.01~0.20；
And BixFey-TiO2Nanocomposite is anatase and the mixing crystal form of rutile-type, wherein rutile content
50~90%, Detitanium-ore-type content 10~40%.
Further, BixFey-TiO2The particle of nanocomposite is 20~60nm.
A kind of BixFey-TiO2The preparation method of nanocomposite, comprises the following steps：
Obtain the alcohol solution of tetra-n-butyl titanate, i.e. A liquid；
Bi source compounds and Fe source compounds are dissolved in water and alcohols mixed liquor, and control pH=1~2, obtains B liquid；
Under agitation, A drops are entered in B liquid, the reaction was continued 1~3h obtains wet gel, and is aged, and drying obtains
Xerogel, xerogel grinding, calcining obtain BixFey-TiO2Nanocomposite.
Further, the molar ratio of the Fe elements of the Bi elements in Bi source compounds and Fe source compounds is 1：0.5~
1.5, Bi source compounds are Bi (NO3)3·5H2O, Fe source compound are Fe (NO3)3·9H2O；
The alcohols used of water and alcohols mixed liquor is ethyl alcohol, and the volume ratio of water and ethyl alcohol is 3:20.
Further, the alcohol solution of tetra-n-butyl titanate is the ethanol solution of tetra-n-butyl titanate.
Further, the metering of the Fe elements of the Bi elements in tetra-n-butyl titanate, Bi source compounds and Fe source compounds
Than for：0.01~0.20：0.01~0.20.
Further, drying temperature is 60~120 DEG C, and calcining heat is 500~800 DEG C.
Further, digestion time is 2~3 days.
Bi made from a kind of above-mentioned preparation methodxFey-TiO2Nanocomposite answering in phosphorylating protein enrichment
With.
Above-mentioned BixFey-TiO2Nanocomposite specific surface area is more than routine TiO2, good dispersion, big specific surface area
Its ability in phosphorylating protein immobilization, the metal ion meeting of doping and phosphate groups are improved with good dispersiveness
Chelation is generated, enrichment is played jointly with physical absorption.And it is apparent to phosphorylated polypeptide adsorbance in beta-casein
It improves, it being capable of effective as selective enriched phosphorus acidifying polypeptide.
Description of the drawings
Fig. 1 is the Bi of embodiment 1xFey-TiO2The XRD diagram of nanocomposite；
Fig. 2 a are the Bi of embodiment 1xFey-TiO2The SEM figures of nanocomposite；Fig. 2 b are the Bi of embodiment 1xFey-
TiO2The grain size distribution of nanocomposite；
Fig. 3 a are the Bi of embodiment 1xFey-TiO2Nanocomposite is to phosphorylated polypeptide adsorption effect in beta-casein
Figure；Fig. 3 b are commercialization TiO2To phosphorylated polypeptide the adsorption effect figure in beta-casein.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below in conjunction with the accompanying drawings to the present invention
Specific embodiment be described in detail.Many details are elaborated in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of BixFey-TiO2Nanocomposite, BixFey-TiO2Nanocomposite includes TiO2It base and is entrained in
TiO2Bi and Fe elements in base, wherein, x=0.01~0.20, y=0.01~0.20；And BixFey-TiO2Nano combined material
Expect the mixing crystal form for anatase and rutile-type, wherein rutile content 50~90%, Detitanium-ore-type content 10~40%.
As x=0.01~0.20, during y=0.01~0.20, concentration effect is optimal.Detitanium-ore-type is conducive in mixing crystal form
The preparation of small nano particle, increases material specific surface area, and rutile-type is conducive to the enrichment of phosphorylated polypeptide, mixing crystal form collection two
Person's collective effect.Preferably, rutile content 73%, Detitanium-ore-type content are 27%.
Above-mentioned BixFey-TiO2Nanocomposite specific surface area is more than routine TiO2, good dispersion, big specific surface area
Its ability in phosphorylating protein immobilization, the metal ion meeting of doping and phosphate groups are improved with good dispersiveness
Chelation is generated, enrichment is played jointly with physical absorption.And it is apparent to phosphorylated polypeptide adsorbance in beta-casein
It improves, it being capable of effective as selective enriched phosphorus acidifying polypeptide.
Further, BixFey-TiO2The particle of nanocomposite is 20~60nm, it is preferred that BixFey-TiO2Nanometer
The particle of composite material is 47nm.
A kind of BixFey-TiO2The preparation method of nanocomposite, comprises the following steps：
Obtain the alcohol solution of tetra-n-butyl titanate, i.e. A liquid.
Bi source compounds and Fe source compounds are dissolved in water and alcohols mixed liquor, and control pH=1~2, obtains B liquid.
Under agitation, A drops are entered in B liquid, the reaction was continued 1~3h obtains wet gel, and is aged, and drying obtains
Xerogel, xerogel grinding, calcining obtain BixFey-TiO2Nanocomposite.
Specific step can be：Tetra-n-butyl titanate (TBT) is added in a certain amount of anhydrous alcohols and is uniformly mixed, make its
Disperse on molecular level, obtain light yellow transparent solution, it is spare.Alcohols can be isopropanol, ethyl alcohol etc..
It weighs a certain amount of by Bi source compounds and Fe source compounds, adds in alcohols solvent, and add in suitable quantity of water, so that preceding
Face adds in nitrate dissolving and in entire solution is uniformly dispersed, and stirring is to being completely dissolved, at this point, pH is in acid (pH=1~2)
It is denoted as B liquid.PH=1~2 can control the hydrolysis rate of TBT, and too fast product is easily agglomerated into bulky grain, specific surface area is caused to reduce.
In the case where being stirred continuously, A liquid is slowly dropped into B liquid, continues to stir certain time, obtains wet gel, be aged, by gel
Xerogel, grinding are obtained after being placed in the drying of (100 DEG C) thermostatic drying chamber, (700 DEG C) calcinings of high temperature obtain BixFey-TiO2(referred to as
BFT) novel nanometer functional composite material.
Further, the molar ratio of the Fe elements of the Bi elements in Bi source compounds and Fe source compounds is 1：0.5~
1.5, Bi source compounds are Bi (NO3)3·5H2O, Fe source compound are Fe (NO3)3·9H2O；
The alcohols used of water and alcohols mixed liquor is ethyl alcohol, and the volume ratio of water and ethyl alcohol is 3:20.
Further, the alcohol solution of tetra-n-butyl titanate is the ethanol solution of tetra-n-butyl titanate.
Further, the metering of the Fe elements of the Bi elements in tetra-n-butyl titanate, Bi source compounds and Fe source compounds
Than for：0.01~0.20：0.01~0.20.
Further, drying temperature is 60~120 DEG C, and calcining heat is 500~800 DEG C.Preferably, drying temperature is
100 DEG C, calcining heat is 700 DEG C.
Further, digestion time is 2~3 days.
Bi made from a kind of above-mentioned preparation methodxFey-TiO2Nanocomposite answering in phosphorylating protein enrichment
With.
Embodiment 1
By a certain amount of tetra-n-butyl titanate (TBT；20mL) it is added to a certain amount of absolute ethyl alcohol (EtOH；Mixing is equal in 30mL)
It is even, light yellow transparent solution is obtained, is denoted as A liquid, is placed it in for use in separatory funnel；Then, 2.1392g Bi are weighed
(NO3)3·5H2O and 1.7816g Fe (NO3)3·9H2O is placed in 100mL beakers, adds in 20mL absolute ethyl alcohol EtOH, is added in suitable
Water is measured, stirring, at this point, pH is in acid (pH=1~2), is denoted as B liquid to being completely dissolved；In the case where being stirred continuously, A liquid is slowly dripped
Enter in B liquid, continue to stir certain time (2h), obtain wet gel, be aged, after gel is placed in the drying of (100 DEG C) thermostatic drying chamber
Xerogel, grinding are obtained, (700 DEG C) calcinings of high temperature obtain BixFey-TiO2(abbreviation BFT) novel nanometer functional composite material.
Take the Bi of preparationxFey-TiO2Functional nano-composites carry out XRD and SEM tests, as a result such as Fig. 1 and 2, XRD：
Pattern：Spheric granules is uniformly dispersed；Average grain diameter：Scherrer (Scherrer) formula expression is D=K λ/(β cos θ) (K is normal
Number 0.89；λ is X-ray wavelength；β is diffraction peak width；θ is the angle of diffraction).It calculates and understands that granular size is about 34nm；It is brilliant
Type content ratio：Rutile content 50~90%, Detitanium-ore-type content 10~40%.SEM：Average grain diameter：47nm or so, with
Scherrer formula calculation formula result is coincide substantially.
By material in the N of 300 DEG C of degassing 3h, the then opposite pressure 0.01~1.0 of selection2Adsorption-desorption curve is counted
It calculates, measures material specific surface area 6.8m2·g-1, more than German (degussa) Degussa P25 mixed crystal types (4.7m2·g-1).Big
Specific surface area and good dispersiveness improve its ability in phosphorylating protein immobilization, the metal ion meeting of doping and phosphorus
Sulfonate groups generate chelation, and enrichment is played jointly with physical absorption
Take BixFey-TiO2Nanocomposite and Germany's (degussa) Degussa P25 mixed crystal types (anatase 80%, gold
Red stone 20%) nano-titanium dioxide by dithiothreitol (DTT) at 60 DEG C respectively to reducing, iodoacetamide subsequently and trypsase
The beta-casein (containing trace alpha-casein) of enzymolysis.The Bi prepared with reference to Fig. 3, the present inventionxFey-TiO2Nanocomposite pair
Phosphorylated polypeptide adsorbance significantly improves in beta-casein (containing trace alpha-casein), and phosphoric acid site is respectively：α-junket egg
In vain:1952.9；Beta-casein:2061.8th, 2432.0,2554.1,3122.2, and with repeatability well.The material energy
Enough effective as selective enriched phosphorus acidifying polypeptides.And business TiO2Enrichment does not find corresponding phosphoric acid site.
Embodiment 2
By a certain amount of tetra-n-butyl titanate (TBT；20mL) it is added to a certain amount of absolute ethyl alcohol (EtOH；Mixing is equal in 30mL)
It is even, light yellow transparent solution is obtained, is denoted as A liquid, is placed it in for use in separatory funnel；Then, 2.1392g Bi are weighed
(NO3)3·5H2O and 0.8908g Fe (NO3)3·9H2O is placed in 100mL beakers, adds in 20mL absolute ethyl alcohol EtOH, is added in suitable
Water is measured, stirring, at this point, pH is in acid (pH=1~2), is denoted as B liquid to being completely dissolved；In the case where being stirred continuously, A liquid is slowly dripped
Enter in B liquid, continue to stir certain time (1h), obtain wet gel, be aged, obtained after gel is placed in the drying of (60 DEG C) thermostatic drying chamber
Xerogel, grinding, (500 DEG C) calcinings of high temperature obtain BixFey-TiO2(abbreviation BFT) novel nanometer functional composite material.
Embodiment 3
By a certain amount of tetra-n-butyl titanate (TBT；20mL) it is added to a certain amount of absolute ethyl alcohol (EtOH；Mixing is equal in 30mL)
It is even, light yellow transparent solution is obtained, is denoted as A liquid, is placed it in for use in separatory funnel；Then, 2.1392Bi (NO are weighed3)3·
5H2O and 2.6742g Fe (NO3)3·9H2O is placed in 100mL beakers, adds in 20mL absolute ethyl alcohol EtOH, is added in suitable quantity of water, is stirred
It mixes to being completely dissolved, at this point, pH is in acid (pH=1~2), is denoted as B liquid；In the case where being stirred continuously, A liquid is slowly dropped into B liquid,
Continue to stir certain time (3h), obtain wet gel, be aged, xerogel is obtained after gel is placed in the drying of (120 DEG C) thermostatic drying chamber,
Grinding, (800 DEG C) calcinings of high temperature, obtains BixFey-TiO2(abbreviation BFT) novel nanometer functional composite material.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. a kind of BixFey-TiO2Nanocomposite, which is characterized in that the BixFey-TiO2Nanocomposite includes TiO2
Base and it is entrained in TiO2Bi and Fe elements in base, wherein, x=0.01~0.20, y=0.01~0.20；
And the BixFey-TiO2Nanocomposite is anatase and the mixing crystal form of rutile-type, wherein rutile content
50~90%, Detitanium-ore-type content 10~40%.
2. Bi according to claim 1xFey-TiO2Nanocomposite, which is characterized in that the BixFey-TiO2Nanometer
The particle of composite material is 20~60nm.
3. a kind of Bi described in claim 1 or 2xFey-TiO2The preparation method of nanocomposite, which is characterized in that including
Following steps：
Obtain the alcohol solution of tetra-n-butyl titanate, i.e. A liquid；
Bi source compounds and Fe source compounds are dissolved in water and alcohols mixed liquor, and control pH=1~2, obtains B liquid；
Under agitation, the A drops are entered in the B liquid, the reaction was continued 1~3h obtains wet gel, and is aged, and dries
Xerogel, the xerogel grinding are obtained, calcining obtains BixFey-TiO2Nanocomposite.
4. Bi according to claim 3xFey-TiO2The preparation method of nanocomposite, which is characterized in that the Bi sources
The molar ratio of the Fe elements of Bi elements and Fe source compounds in compound is 1：0.5~1.5, the Bi source compounds are Bi
(NO3)3·5H2O, the Fe source compounds are Fe (NO3)3·9H2O；
The alcohols used of the water and alcohols mixed liquor is ethyl alcohol, and the volume ratio of the water and the ethyl alcohol is 3:20.
5. Bi according to claim 3xFey-TiO2The preparation method of nanocomposite, which is characterized in that the metatitanic acid
The alcohol solution of four N-butyls is the ethanol solution of tetra-n-butyl titanate.
6. Bi according to claim 4xFey-TiO2The preparation method of nanocomposite, which is characterized in that the metatitanic acid
The metering of the Fe elements of four N-butyls, the Bi elements in the Bi source compounds and Fe source compounds is compared for 1：0.01~0.20：
0.01~0.20.
7. Bi according to claim 3xFey-TiO2The preparation method of nanocomposite, which is characterized in that the drying
Temperature is 60~120 DEG C, and the calcining heat is 500~800 DEG C.
8. Bi according to claim 3xFey-TiO2The preparation method of nanocomposite, which is characterized in that the ageing
Time is 2~3 days.
9. Bi made from a kind of any one of claim 3~8 preparation methodxFey-TiO2Nanocomposite is in phosphorylation egg
Application in white matter enrichment.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103495376A (en) * | 2013-10-08 | 2014-01-08 | 江南大学 | Preparation and phosphoeptide enrichment methods of titanium dioxide/ferroferric oxide nanoparticles |
| CN105018553A (en) * | 2015-06-25 | 2015-11-04 | 江南大学 | Phosvitin phosphopeptide enrichment method |
-
2017
- 2017-12-18 CN CN201711362729.3A patent/CN108097199A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103495376A (en) * | 2013-10-08 | 2014-01-08 | 江南大学 | Preparation and phosphoeptide enrichment methods of titanium dioxide/ferroferric oxide nanoparticles |
| CN105018553A (en) * | 2015-06-25 | 2015-11-04 | 江南大学 | Phosvitin phosphopeptide enrichment method |
Non-Patent Citations (1)
| Title |
|---|
| QIONGZHI GAO, ET AL.: "Fabrication and photocatalytic properties of TiO2 Nanofilms co-doped with Fe3+ and Bi3+ ions", 《SURFACE REVIEW AND LETTERS》 * |
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Application publication date: 20180601 |