CN102502678A - Preparation method of nanometer TiO2-ATP (Adenosine Triphosphate) powder material - Google Patents
Preparation method of nanometer TiO2-ATP (Adenosine Triphosphate) powder material Download PDFInfo
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- CN102502678A CN102502678A CN2011102894838A CN201110289483A CN102502678A CN 102502678 A CN102502678 A CN 102502678A CN 2011102894838 A CN2011102894838 A CN 2011102894838A CN 201110289483 A CN201110289483 A CN 201110289483A CN 102502678 A CN102502678 A CN 102502678A
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Abstract
The invention discloses a preparation method of a nanometer TiO2-ATP (Adenosine Triphosphate) powder material, belonging to the technical field of preparation of nanometer powder materials. The method is characterized by comprising the following steps of: directly purifying attapulgite, wherein sodium hexametahposphate is taken as a dispersant, deionized water of which the temperature is 20 DEG C is used, the using amount of the sodium hexametahposphate is 3 percent that of the attapulgite, and an ultrasonic medium-speed stirring way is adopted; treating the attapulgite to obtain purified attapulgite and lower residues respectively, wherein the purified attapulgite is call ATP, and the content is nearly 100 percent; and preparing the nanometer TiO2-ATP powder material.
Description
Technical field
The invention belongs to the nano composite material preparing technical field, refer in particular to a kind of nano-TiO
2The preparation method of-ATP powder body material.
Background technology
Nano titanium oxide (nano-TiO
2) be to use one of the widest material in the nano material, compare with other nano materials, have that chemicalstability is good, photoetch take place after the illumination, resistance to acids and bases is strong, price is low, advantage such as nontoxic, simultaneously, nano-TiO
2Also have photocatalytic activity efficiently, can under UV-light even radiation of visible light, degrade all kinds of chemical substances or kill bacteria, thus receive increasing concern.At present, nano-TiO
2Many commerical prods have been widely used in, in pigment, coating, sun-proof class makeup, fuel cell etc.
Attapulgite clay mineral; Being called for short recessed soil, having the attribute of nano material, is the natural nano structure mineral material with nanochannel structure; Because they have very large specific surface area and certain ion exchangeable, therefore be widely used as sorbent material, support of the catalyst and antiseptic-germicide carrier etc.Attapulgite clay has unique physical and chemical performances such as absorption, decolouring, suspension, thixotroping, colloid, filling, rheological, thermostability and salt resistance, is described as " king of thousand soil, ten thousand kinds use soil ".Recent decades, recessed soil has obtained in fields such as oil, chemical industry, food-processing, environmental protection, light textile, agricultural chemicals using widely.
The present invention develops a kind of nano-TiO
2The preparation method of-ATP powder body material is with nano-TiO
2Process powder body material with ATP, for enlarging nano-TiO
2Lay a good foundation with the application of ATP.
Summary of the invention
The objective of the invention is to develop a kind of nano-TiO
2The preparation method of-ATP powder body material is characterized by, and directly recessed soil is purified, and selecting Sodium hexametaphosphate 99 for use is dispersion agent, uses 20 ℃ deionized water, and the consumption of Sodium hexametaphosphate 99 is 3% of a recessed native consumption, and alr mode is that UW adds the middling speed stirring.Concrete steps are: measure deionized water 200mL and place beaker, take by weighing recessed native 10g, accurately take by weighing certain dispersion agent an amount of (be that solid-to-liquid ratio is 1: 20, dispersant dosage be recessed soil property amount 3%); Dispersion agent is poured in the deionized water, and fully stirring is dissolved it fully, forms homogeneous phase solution; Under agitation, recessed soil slowly added in 20 ℃ the aqueous solution, fully stir the back and form suspension-s.After stirring 15min, this suspension-s is put concussion and stirring in the ultrasonic cleaner, the abundant aquation of recessed soil particle to suspension-s is disperseed; After leaving standstill 30min; System obviously is divided into the closely knit beds of precipitation of top suspension-s and bottom, pours out top suspension-s and centrifugal alcohol and washes, and with common loft drier the top and the bottom material is carried out drying; 150 ℃ of drying temperatures; Obtain the recessed soil and the bottom residue of purifying respectively, the recessed soil of purification is called ATP, and its content is close to 100%.
The preparation nano-TiO
2The concrete technology of-ATP powder body material is following: (1) is measured the 10mL tetrabutyl titanate and is dissolved in the 30mL absolute ethyl alcohol, adds the 2mL trolamine, and stirring at room gets shallow yellow transparent solution A; (2) 10mL absolute ethyl alcohol, 2mL deionized water and 1.5mL nitric acid are mixed with solution B; (3) solution A stirs, and whole B drips of solution are added in the A liquid, forms the orange-yellow colloidal sol of homogeneous transparent; (4) A, the mixed solution of B are ultrasonicly being added that slowly to be added drop-wise to total amount under the condition of stirring be 80mL, containing in the aqueous solution of ATP20%, dripping off continued ultrasonic adding to stir 1 hour; (5) with pure water with TiO
2The presoma of-ATP material cleans and centrifugal 3 times; (6) again 80 ℃ dry 12 hours down, grind then, the powder that obtains 450 ℃ of calcinings 2 hours down, can be obtained nano-TiO
2-ATP powder body material.
Description of drawings
The stereoscan photograph of the recessed soil (ATP) before Fig. 1 purifies after recessed soil and the purification
(a) recessed native raw ore; (b) the recessed soil (ATP) after the purification
Can find out that from Fig. 1 (a) the recessed native shape before handling is all very irregular with distribution; And can find out that from Fig. 1 (b) the recessed soil (ATP) after the processing is loose fibres shape crystal, outward appearance meets the characteristic of pure recessed native perfect cystal.
Fig. 2 differing temps nano-TiO
2The SEM sem photograph of-ATP powder body material
(a)450℃；(b)850℃
Can find out that from Fig. 2 (a) ATP still is loose fibres shape crystal, this explanation also finds to have many granular TiO at the crystalline structure that 450 ℃ of following ATP do not have change itself among Fig. 2 (a)
2Accumulate in the surface of ATP, these TiO
2Attached to ATP surface, disperse more evenly, there is not tangible agglomeration.From granularity, its TiO
2Particle diameter at 20～30nm; But we do not find fibrous crystal among Fig. 2 (b), and this explanation attapulgite clay under 850 ℃ high temperature has lost original crystalline structure, and we still can see granular TiO on the surface of some blocks simultaneously
2Exist, and particle diameter is between 40～60nm, clearly, along with ATP adds, TiO
2The pure TiO that the particle diameter ratio same process obtains
2Little; This is consistent with XRD diffraction result.
Fig. 3 nano-TiO
2The TEM stereoscan photograph of-ATP powder body material
Visible by Fig. 3, ATP still is strip and is entrenched in nano-TiO
2In the particle, the about 7.5nm of width, nano-TiO
2The about 6.5nm of diameter, and it is more even to distribute.
ATP and nano-TiO that Fig. 4 purifies
2The XRD spectra of-ATP powder body material presoma
(001) crystal face characteristic diffraction peak of the ATP that as can be seen from Figure 4 purifies ° is located in 2 θ=8.34, can calculate according to Bragg equation λ=2dsin θ, and the spacing of ATP is 1.06nm; At nano-TiO
2On the XRD spectra of-ATP powder body material presoma, the diffraction peak that appears between 22～75 ° is non-crystalline state TiO
2Characteristic diffraction peak; In composite material precursor at the still visible significantly ATP characteristic diffraction peaks of (001) face 2 θ=8.34 °; Variation has not taken place in its spacing; Its spacing is for still being 1.06nm, and this explanation ATP is not a laminated structure completely, that is to say the intercalation phenomenon in powder body material, not occur.
Fig. 5 nano-TiO
2The XRD spectra of-ATP powder body material under different calcining temperatures
Visible by Fig. 5, rutile TiO does not only appear in 450 ℃ of incinerating matrix materials
2, present the crystal formation that mixes of anatase octahedrite and indefinite form on the contrary; To 700 ℃ the time, the climax is that 2 θ=25.32 ° just begin to become sharp-pointed gradually; In the time of 800 ℃, just be Detitanium-ore-type TiO in the matrix material fully
2Arrived in the time of 850 ℃, powder body material is main with a small amount of rutile TiO with the Detitanium-ore-type
2To 900 ℃ of major parts change rutile TiO into
2This explanation is along with the adding of ATP, TiO
2Raise about 300 ℃ from anatase octahedrite to the rutile-type transition temperature; Simultaneously in 450 ℃ of incinerating powder body materials, we still can be in 2 θ=8.34 ° see the characteristic diffraction peak of ATP, but along with the rising of temperature, the characteristic diffraction peak completely dissolve of ATP shows that the crystalline structure of ATP has taken place to change fully.
Research of the present invention shows: TiO
2Can form good powder body material, TiO with ATP
2Even in the ATP surface arrangement, TiO
2Do not reunite between nano particle; TiO in the powder body material
2Transformation temperature from the Detitanium-ore-type to the rutile-type is than pure TiO
2Approximately raise about 300 ℃; In 850 ℃ powder body material, TiO
2The mixing crystal formation that presents sharp titanium and rutile, but ATP loses original crystalline structure.
Embodiment
Directly recessed soil is purified, selecting Sodium hexametaphosphate 99 for use is dispersion agent, uses 20 ℃ deionized water, and the consumption of Sodium hexametaphosphate 99 is 3% of a recessed native consumption, and alr mode is that UW adds the middling speed stirring.Concrete steps are: measure deionized water 200mL and place beaker, take by weighing recessed native 10g, accurately take by weighing certain dispersion agent an amount of (be that solid-to-liquid ratio is 1: 20, dispersant dosage be recessed soil property amount 3%); Dispersion agent is poured in the deionized water, and fully stirring is dissolved it fully, forms homogeneous phase solution; Under agitation, recessed soil slowly added in 20 ℃ the aqueous solution, fully stir the back and form suspension-s.After stirring 15min, this suspension-s is put concussion and stirring in the ultrasonic cleaner, the abundant aquation of recessed soil particle to suspension-s is disperseed; After leaving standstill 30min; System obviously is divided into the closely knit beds of precipitation of top suspension-s and bottom, pours out top suspension-s and centrifugal alcohol and washes, and with common loft drier the top and the bottom material is carried out drying; 150 ℃ of drying temperatures; Obtain the recessed soil and the bottom residue of purifying respectively, the recessed soil of purification is called ATP, and its content is close to 100%.
The preparation nano-TiO
2The concrete technology of-ATP powder body material is following: (1) is measured the 10mL tetrabutyl titanate and is dissolved in the 30mL absolute ethyl alcohol, adds the 2mL trolamine, and stirring at room gets shallow yellow transparent solution A; (2) 10mL absolute ethyl alcohol, 2mL deionized water and 1.5mL nitric acid are mixed with solution B; (3) solution A stirs, and whole B drips of solution are added in the A liquid, forms the orange-yellow colloidal sol of homogeneous transparent; (4) A, the mixed solution of B are ultrasonicly being added that slowly to be added drop-wise to total amount under the condition of stirring be 80mL, containing in the aqueous solution of ATP20%, dripping off continued ultrasonic adding to stir 1 hour; (5) with pure water with TiO
2The presoma of-ATP material cleans and centrifugal 3 times; (6) again 80 ℃ dry 12 hours down, grind then, the powder that obtains 450 ℃ of calcinings 2 hours down, can be obtained nano-TiO
2-ATP powder body material.
Claims (2)
1. directly recessed soil is purified, selecting Sodium hexametaphosphate 99 for use is dispersion agent, uses 20 ℃ deionized water, and the consumption of Sodium hexametaphosphate 99 is 3% of a recessed native consumption, and alr mode is that UW adds the middling speed stirring.Concrete steps are: measure deionized water 200mL and place beaker, take by weighing recessed native 10g, accurately take by weighing certain dispersion agent an amount of (be that solid-to-liquid ratio is 1: 20, dispersant dosage be recessed soil property amount 3%); Dispersion agent is poured in the deionized water, and fully stirring is dissolved it fully, forms homogeneous phase solution; Under agitation, recessed soil slowly added in 20 ℃ the aqueous solution, fully stir the back and form suspension-s.After stirring 15min, this suspension-s is put concussion and stirring in the ultrasonic cleaner, the abundant aquation of recessed soil particle to suspension-s is disperseed; After leaving standstill 30min; System obviously is divided into the closely knit beds of precipitation of top suspension-s and bottom, pours out top suspension-s and centrifugal alcohol and washes, and with common loft drier the top and the bottom material is carried out drying; 150 ℃ of drying temperatures; Obtain the recessed soil and the bottom residue of purifying respectively, the recessed soil of purification is called ATP, and its content is close to 100%.
2. according to the said a kind of nano-TiO of claim 1
2The preparation method of-ATP powder body material is measured the 10mL tetrabutyl titanate and is dissolved in the 30mL absolute ethyl alcohol, adds the 2mL trolamine, and stirring at room gets shallow yellow transparent solution A; 10mL absolute ethyl alcohol, 2mL deionized water and 1.5mL nitric acid are mixed with solution B; Solution A stirs, and whole B drips of solution are added in the A liquid, forms the orange-yellow colloidal sol of homogeneous transparent; A, the mixed solution of B are ultrasonicly being added that slowly to be added drop-wise to total amount under the condition of stirring be 80mL, containing in the aqueous solution of ATP20%, dripping off continued ultrasonic adding to stir 1 hour; With pure water with TiO
2The presoma of-ATP material cleans and centrifugal 3 times; Again 80 ℃ dry 12 hours down, grind then, the powder that obtains 450 ℃ of calcinings 2 hours down, can be obtained nano-TiO
2-ATP powder body material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102886254A (en) * | 2012-11-02 | 2013-01-23 | 镇江忆诺唯记忆合金有限公司 | Preparation of attapulgite compound type ATP-SnO2-TiO2 photocatalyst |
| CN104624026A (en) * | 2015-01-31 | 2015-05-20 | 龚娟 | Air purifying agent and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3790034B2 (en) * | 1998-02-06 | 2006-06-28 | 朝日化学工業株式会社 | Antioxidant paint for steel |
| CN101000809A (en) * | 2006-12-31 | 2007-07-18 | 江苏工业学院 | Preparation method of nano-conducting attapulgite material |
| CN101497039A (en) * | 2009-01-16 | 2009-08-05 | 淮阴工学院 | Air purification agent of high activity based on visible light and preparation method thereof |
| CN101914248A (en) * | 2010-09-02 | 2010-12-15 | 淮阴工学院 | Preparation method of PS-TiO2-ATP organic/inorganic composite film |
| CN101947464A (en) * | 2010-08-06 | 2011-01-19 | 淮阴工学院 | Preparation method of attapulgite clay composite visible light catalyst |
-
2011
- 2011-09-21 CN CN2011102894838A patent/CN102502678A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3790034B2 (en) * | 1998-02-06 | 2006-06-28 | 朝日化学工業株式会社 | Antioxidant paint for steel |
| CN101000809A (en) * | 2006-12-31 | 2007-07-18 | 江苏工业学院 | Preparation method of nano-conducting attapulgite material |
| CN101497039A (en) * | 2009-01-16 | 2009-08-05 | 淮阴工学院 | Air purification agent of high activity based on visible light and preparation method thereof |
| CN101947464A (en) * | 2010-08-06 | 2011-01-19 | 淮阴工学院 | Preparation method of attapulgite clay composite visible light catalyst |
| CN101914248A (en) * | 2010-09-02 | 2010-12-15 | 淮阴工学院 | Preparation method of PS-TiO2-ATP organic/inorganic composite film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102886254A (en) * | 2012-11-02 | 2013-01-23 | 镇江忆诺唯记忆合金有限公司 | Preparation of attapulgite compound type ATP-SnO2-TiO2 photocatalyst |
| CN104624026A (en) * | 2015-01-31 | 2015-05-20 | 龚娟 | Air purifying agent and preparation method thereof |
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