CN106799258A - A kind of method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst - Google Patents
A kind of method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst Download PDFInfo
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- CN106799258A CN106799258A CN201710029490.1A CN201710029490A CN106799258A CN 106799258 A CN106799258 A CN 106799258A CN 201710029490 A CN201710029490 A CN 201710029490A CN 106799258 A CN106799258 A CN 106799258A
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- 238000000034 method Methods 0.000 title claims abstract description 72
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 67
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000007385 chemical modification Methods 0.000 title claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000000889 atomisation Methods 0.000 claims abstract description 23
- 230000004048 modification Effects 0.000 claims abstract description 20
- 238000012986 modification Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 150000001413 amino acids Chemical class 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000000053 physical method Methods 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 4
- 229920005989 resin Polymers 0.000 abstract description 4
- 229920001002 functional polymer Polymers 0.000 abstract description 3
- 239000011858 nanopowder Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000003607 modifier Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000002096 quantum dot Substances 0.000 description 5
- 241001614291 Anoplistes Species 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
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- 238000010521 absorption reaction Methods 0.000 description 3
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- 235000011187 glycerol Nutrition 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000013386 optimize process Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
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- 235000009566 rice Nutrition 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
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Classifications
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0201—Oxygen-containing compounds
- B01J31/0202—Alcohols or phenols
-
- B01J35/39—
Abstract
The invention provides a kind of method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst, including, mechanical smashing, and ultrasonic high speed atomisation are carried out to sub- titanium oxide and/or miscellaneous element doping Asia titanium oxide；Air-flow smashing is carried out, Asia nano titanium oxide powder is obtained；Carry out surface modification.The method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst, by physical method it is simple, prepare nano-quantum point on a large scale, and surface modification is carried out to it to increase its stability and resin system compatibility, suppress its reunion behavior in systems such as resins, production efficiency is high, can large-scale application in industrialized production, be that the preparation of functional polymer and composite is laid a good foundation.
Description
Technical field
The invention belongs to the preparing technical field of function nano particle, and in particular to a kind of chemical modification method prepares nanoscale
The method of sub- titanium oxide composite photo-catalyst.
Background technology
Yardstick involved by this technology belongs to quantum point range, quantum dot also known as semiconductor nanocrystals, its three dimensions
Size all below 200 nanometers, outward appearance is all received just like a minimum pointing object, motion of its internal electron in all directions
To limitation.The special construction of quantum dot cause its have skin effect, quantum size effect, dielectric resistance meet effect and macroscopic quantum
Tunnel-effect etc., so as to show the physicochemical properties different from macroscopic material, there is larger application in terms of functional material
Potentiality.
By years of researches, establish the preparation method of various quantum dots so far, and chemically based on, including：
Synthesized in organic system using the method for colloid chemistry；It is directly synthesized in aqueous.But prepared by such method
Quantum dot yield is small, and kind is restricted, and quantum dot then rare report is prepared by physical method.Additionally, both at home and abroad
Prepared for nano-function powder, more using chemical technology, there is high cost, complex operation, be unfavorable for that industrialization should
With.
The content of the invention
The purpose of this part is to summarize some aspects of embodiments of the invention and briefly introduce some preferable implementations
Example.May be done in this part and the description of the present application summary and denomination of invention a little simplified or omitted to avoid making our department
Point, the purpose of specification digest and denomination of invention obscure, and this simplification or omission cannot be used for limiting the scope of the present invention.
In view of technological gap prepared by above-mentioned sub- titanium oxide composite photo-catalyst, it is proposed that the present invention.
Therefore, one of purpose of the invention is to solve deficiency of the prior art, there is provided a kind of chemical modification legal system
The method of standby nanoscale Asia titanium oxide composite photo-catalyst.
In order to solve the above technical problems, the invention provides following technical scheme：A kind of chemical modification method prepares nanoscale
The method of sub- titanium oxide composite photo-catalyst, including, mechanical powder is carried out to sub- titanium oxide and/or miscellaneous element doping Asia titanium oxide
Essence, and ultrasonic high speed atomisation；Air-flow smashing is carried out, Asia nano titanium oxide powder is obtained；Carry out surface modification.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The sub- titanium oxide and/or miscellaneous element doping Asia titanium oxide, its particle size range is 500~20000nm.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The miscellaneous element is one or more in nitrogen, phosphorus or sulphur.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The particle diameter of the sub- nano titanium oxide powder is 10~200nm.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The ultrasonic high speed atomisation, wherein ultrasonic power be 200~250W, high speed atomisation rotating speed be 20000~
24000rpm。
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The air-flow crushing, its gas flow is 2~4m3/ min, gas pressure is 0.5~0.7MPa, gas temperature
Spend is 90~120 DEG C.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The machinery is smashed, and it smashes the time for 0.5~1h, and rotating speed is 250~350rpm.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The surface modification, the consumption of its dressing agent is the 1~10% of powder quality, its mass concentration is 4~
6wt.%.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The dressing agent, its atomization droplets diameter is 1~20 μm.
Prepared as chemical modification method of the present invention nanoscale Asia titanium oxide composite photo-catalyst method it is a kind of excellent
Scheme is selected, wherein：The dressing agent includes the one kind or several in silane coupler, titanate coupling agent or amino acids dressing agent
Kind.
The present invention is had the advantage that：
(1) method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst, passes through
Physical method is simple, prepare nano-quantum point on a large scale, and it is carried out surface modification to increase its stability and resin system
Compatibility, production efficiency is high, can large-scale application in industrialized production, be that the preparation of functional polymer and composite is established
Basis.
(2) method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst, uses
A small amount of coating material can be prepared by the more excellent nano-powder of performance.
(3) chemical modification method provided by the present invention is prepared prepared by the method for nanoscale Asia titanium oxide composite photo-catalyst
The nano-powder for obtaining, particle diameter is small and has excellent surface active index and dispersiveness in the base.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be to that will use needed for embodiment description
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill of field, without having to pay creative labor, other can also be obtained according to these accompanying drawings
Accompanying drawing.Wherein：
Fig. 1 is the sub- titanium oxide powder of a diameter of 100 ran of gained of embodiment 1；
Fig. 2 is the sub- titanium oxide powder of a diameter of 50 ran of gained of embodiment 3.
Specific embodiment
To enable the above objects, features and advantages of the present invention more obvious understandable, with reference to specific embodiment pair
Specific embodiment of the invention is described in detail.
Many details are elaborated in the following description in order to fully understand the present invention, but the present invention can be with
Other manner described here is different from using other to implement, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Secondly, " one embodiment " or " embodiment " referred to herein refers to that may be included at least one realization side of the invention
Special characteristic, structure or characteristic in formula." in one embodiment " that different places occur in this manual not refers both to
Same embodiment, nor the single or selective embodiment mutually exclusive with other embodiment.
Embodiment 1
3t Asias titanium oxide (particle diameter is 10000~20000nm) is weighed, is added in the mechanical crusher of 350rpm rotating speeds,
Crush 45 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power is 250W, and high speed atomisation rotating speed is
24000rpm, powder is gathered and weighed after smashing；Coating material Thioglycolic acid 0.15t is weighed in 5wt.% ratios, gas is adjusted
Stream disintegrating machine, gas flow is 3m3/ min, gas pressure is 0.6MPa, and air themperature is 100 DEG C, and dressing agent solution concentration is
5wt.%, the flow for modifying agent solution is 1ml/min, and it is 1~20 μm to be atomized, and starts to spray into dressing agent after crushing, and crushes and completes
After to obtain average diameter be 100 nanometers, surface modification, finely dispersed sub- nano titanium oxide powder.
This is sample 1.
Embodiment 2
3t Asias titanium oxide (particle diameter is 5000~10000nm) is weighed, is added in the mechanical crusher of 300rpm rotating speeds, powder
Broken 60 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power is 200W, and high speed atomisation rotating speed is
22000rpm, powder is gathered and weighed after smashing；Amino acids coating material 0.24t is weighed in 8wt.% ratios, gas is adjusted
Stream disintegrating machine, gas flow is 3m3/ min, gas pressure is 0.6MPa, and air themperature is 110 DEG C, and dressing agent solution concentration is
6wt.%, the flow for modifying agent solution is 1ml/min, and it is 1~20 μm to be atomized, and starts to spray into dressing agent after crushing, and crushes and completes
After to obtain average diameter be 100 nanometers, surface modification, finely dispersed sub- titanium oxide powder.
This is sample 2.
Embodiment 3
3t Asias titanium oxide (particle diameter is 500~5000nm) is weighed, is added in the mechanical crusher of 250rpm rotating speeds, crushed
45 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power is 250W, high speed atomisation rotating speed is 20000rpm,
Powder is gathered and weighed after smashing；Glycerine 0.18t is weighed in 6wt.% ratios, air-flow disintegrating machine is adjusted, gas flow is
3m3/ min, gas pressure is 0.6MPa, and air themperature is 100 DEG C, and dressing agent solution concentration is 4wt.%, modification agent solution
Flow is 1ml/min, and it is 1~20 μm to be atomized, and starts to spray into dressing agent after crushing, and average diameter is obtained after the completion of crushing for 50 receive
Rice, surface modification, finely dispersed sub- titanium oxide powder.
This is sample 3.
Embodiment 4
3t Asias titanium oxide (particle diameter is 500~5000nm) is weighed, is added in the mechanical crusher of 300rpm rotating speeds, crushed
30 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power is 200W, high speed atomisation rotating speed is 24000rpm,
Powder is gathered and weighed after smashing；Glycerine 0.33t is weighed in 10wt.% ratios, air-flow disintegrating machine is adjusted, gas flow is
2m3/ min, gas pressure is 0.7MPa, and air themperature is 120 DEG C, and dressing agent solution concentration is 5wt.%, modification agent solution
Flow is 1.2ml/min, and it is 1~20 μm to be atomized, and starts to spray into dressing agent after crushing, and it is 80 that average diameter is obtained after the completion of crushing
Nanometer, surface modification, finely dispersed sub- titanium oxide powder.
This is sample 4.
Embodiment 5
3t N dopings Asia titanium oxide (particle diameter is 500~5000nm) is weighed, the mechanical crusher of 300rpm rotating speeds is added to
In, crush 30 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power is 200W, and high speed atomisation rotating speed is
24000rpm, powder is gathered and weighed after smashing；Glycerine 0.33t is weighed in 10wt.% ratios, air-flow disintegrating machine, gas is adjusted
Body flow is 2m3/ min, gas pressure is 0.7MPa, and air themperature is 120 DEG C, and dressing agent solution concentration is 5wt.%, modification
The flow of agent solution is 1.2ml/min, and it is 1~20 μm to be atomized, and starts to spray into dressing agent after crushing, and obtains average after the completion of crushing
A diameter of 80 nanometers, surface modification, finely dispersed N doping Asia titanium oxide powder.
Embodiment 6
3t phosphorus dopings Asia titanium oxide (particle diameter is 5000~10000nm) is weighed, the mechanical crushing of 300rpm rotating speeds is added to
In machine, crush 60 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power is 200W, and high speed atomisation rotating speed is
22000rpm, powder is gathered and weighed after smashing；Amino acids coating material 0.24t is weighed in 8wt.% ratios, gas is adjusted
Stream disintegrating machine, gas flow is 3m3/ min, gas pressure is 0.6MPa, and air themperature is 110 DEG C, and dressing agent solution concentration is
6wt.%, the flow for modifying agent solution is 1ml/min, and it is 1~20 μm to be atomized, and starts to spray into dressing agent after crushing, and crushes and completes
After to obtain average diameter be 100 nanometers, surface modification, finely dispersed phosphorus doping Asia titanium oxide.
Embodiment 7：
Commercially available nano level modified sub- titanium oxide powder is taken, its amount of modifier is 15wt%, used as sample 5.
Separately sampled product 1,2,3,4,5 each 5.0g, add 200ml deionized waters, and magnetic agitation 5min stands, and removes drift
The powder bubbled through the water column, by the sample filtering for sinking under water, dries, weighs, and its quality is designated as M, is calculated according to equation below and activated
Index：
Concrete outcome such as following table
From result, the modified powder prepared by the present invention, in terms of activation index, with excellent effect.Inventor
It has been investigated that, when controlling amount of modifier in 1~10wt%, the activation index of modified powder can be remarkably reinforced, and stabilization
More than 90%.Although in commercially available modified powder, amount of modifier serious offense 10wt%, because it is in modifying process, go out
It is soft-agglomerated between existing original nano-powder and modified nano powder so as to be formed " aggregate particle size ", it is impossible to which that effectively optimization activation refers to
Number.The present invention is when machinery is smashed, while destroying the reunion between nano-powder with ultrasound or high speed atomisation, it is to avoid directly add
The soft-agglomerated phenomenon for entering modifying agent and producing, and in mechanical crushing, carrying out modification can corrode machine simultaneously, cause mechanical disorder.
Embodiment 8：
Commercially available nano level modified titanium dioxide powder is taken, its amount of modifier is 15wt%, used as sample 5.
Separately sampled product 1,2,3,4,5, add carbon tetrachloride, are made into the dispersion liquid of 0.1wt%, and ultrasonic disperse 10min puts
In the graduated test tubes with grinding port plug of 10ml, stand at room temperature, record the solvent of supernatant liquor, its body with organic phase
Product (10ml) ratio, represents the sedimentation rate of nano-powder to evaluate its dispersiveness.
Timing 180 minutes, sedimentation rate data, the following chart of arrangement were recorded every 30 minutes：
From result, the modified powder prepared by the present invention, in terms of dispersiveness, with excellent effect.Nano-powder
Whether can embody uniformly dispersed in same matrix material stabilization amalgamation and matrix material, it is critical only that control nano powder
Body uniform particle sizes and nano-powder are fully modified.Inventor's research finds, unified by mechanical crushing by nano-powder particle
Control using ultrasound, high speed atomisation rather than adds modifier modification in below 200nm, and during this, more enough to avoid modifying process
Middle modified Nano particle is soft-agglomerated with original nano-particle, and then causes that particle diameter distribution is narrower, is not in existing " aggregate particle size "
As；Further smashed using air-flow, and with modifying agent do surface modification simultaneously, then in the case of particle diameter distribution is uniform, entered
Step refining particle diameter, and simultaneously, it is modified compared to mechanical smashing method, fully nano-particle is changed near " one-to-one "
Property.To sum up, method provided by the present invention, can control particle diameter of nanometer powder uniform and nano-powder is fully modified, and embody
Excellent dispersiveness in the base.
Embodiment 9：
Sample 1,2,3,4 is mixed with corresponding matrix, finished product 1~4 is made, carry out electric conductivity, ultraviolet radiation absorption,
Photothermal conversion, light degradation formaldehyde this four aspect aptitude tests.Result such as following table.
From result, the modified powder prepared by the present invention, in ultraviolet radiation absorption, conductive capability, photothermal conversion, light drop
Solution formaldehyde function aspects, with excellent effect.Function nano powder, if excellent functional effect can be embodied, be it is critical only that
1. whether nano-powder particle is fully modified in itself；2. whether nano-powder stablizes fusion in the base；3. whether nano-powder
It is uniformly dispersed in the base.This three, complements each other.Inventor's research is found, is crushed by the first wheel to nano-powder and same
Shi Chaosheng or high velocity fog are processed, and can prevent the soft-agglomerated phenomenon of nano-powder, and then cause that it will not be because of " secondary grain
Footpath " and occur that particle diameter distribution is wide, insufficient situation that is modified occurs.Consequently, it is possible in the particle diameter of effectively control nano-powder
In the case of distribution and the abundant degree that is modified, preparation-obtained nano-powder of the invention is allowed for, there can be work higher
Change index and dispersiveness excellent in the base.And then, even if compared with the common commercially available function powder that modifier content is higher,
Fabric prepared by obtained powder of the invention, can embody more excellent functional effect.
It is noted that being chemical method in the prior art is obtained nanoscale Asia titanium oxide powder, the present invention uses thing
Reason method has been made better powder.In having abandoned traditional preparation process, the method for now modifying post processing, using ultrasonic mist
Change aid in treatment, and preferably optimize process conditions, promote sub- titania surface atom and stretch to " dangling bonds " in space to sky
The absorption of gas, with the carrying out crushed and the facilitation of ultrasonic atomizatio, the three-dimensional periodic potential field inside sub- titanium oxide is continuous
On surface by very fast interruption, electronic state and the dramatic change of body phase, cause its in addition to the stabilization adsorption site such as bridging oxygen room
There is a certain degree of dissociation in the gas that he adsorbs, have impact on the hybrid ionic and covalent bond work existed in sub- titanium oxide system
With so that sub- titanium oxide stability dies down, and can be crushed to the lower order of magnitude.
In sum, chemical modification method provided by the present invention prepares the side of nanoscale Asia titanium oxide composite photo-catalyst
Method, by physical method it is simple, prepare nano-quantum point on a large scale, and it is carried out surface modification to increase its stability and tree
Resin system compatibility, production efficiency is high, can large-scale application in industrialized production, be the preparation of functional polymer and composite
Lay a good foundation；The method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst, uses
A small amount of coating material can be prepared by the more excellent nano-powder of performance；Chemical modification method provided by the present invention prepares nanoscale
The preparation-obtained nano-powder of method of sub- titanium oxide composite photo-catalyst, particle diameter is small and has excellent surface in the base
Activation index and dispersiveness.
It should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to preferably
Embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to technology of the invention
Scheme is modified or equivalent, and without deviating from the spirit and scope of technical solution of the present invention, it all should cover in this hair
In the middle of bright right.
Claims (10)
1. a kind of method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst, it is characterised in that：Including,
Mechanical smashing, and ultrasonic high speed atomisation are carried out to sub- titanium oxide and/or miscellaneous element doping Asia titanium oxide；
Air-flow smashing is carried out, Asia nano titanium oxide powder is obtained；
Carry out surface modification.
2. the method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst according to claim 1, its feature
It is：The sub- titanium oxide and/or miscellaneous element doping Asia titanium oxide, its particle size range is 500~20000nm.
3. the method that chemical modification method according to claim 1 or claim 2 prepares nanoscale Asia titanium oxide composite photo-catalyst, it is special
Levy and be：The miscellaneous element is one or more in nitrogen, phosphorus or sulphur.
4. the method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst according to claim 1, its feature
It is：The particle diameter of the sub- nano titanium oxide powder is 10~200nm.
5. the chemical modification method according to any one of claim 1,2 or 4 prepares nanoscale Asia titanium oxide composite photo-catalyst
Method, it is characterised in that：The ultrasonic high speed atomisation, wherein ultrasonic power are 200~250W, and high speed atomisation rotating speed is
20000~24000rpm.
6. the method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst according to claim 5, its feature
It is：The air-flow crushing, its gas flow is 2~4m3/ min, gas pressure be 0.5~0.7MPa, gas temperature be 90~
120℃。
7. the chemical modification method according to any one of claim 1,2,4 or 6 prepares nanoscale Asia titanium oxide composite photocatalyst
The method of agent, it is characterised in that：The machinery is smashed, and it smashes the time for 0.5~1h, and rotating speed is 250~350rpm.
8. the chemical modification method according to any one of claim 1,2,4 or 6 prepares nanoscale Asia titanium oxide composite photocatalyst
The method of agent, it is characterised in that：The surface modification, the consumption of its dressing agent is the 1~10% of powder quality, its mass concentration
It is 4~6wt.%.
9. the method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst according to claim 8, its feature
It is：The dressing agent, its atomization droplets diameter is 1~20 μm.
10. the method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst according to claim 9, its feature
It is：The dressing agent includes one or more in silane coupler, titanate coupling agent or amino acids dressing agent.
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| US20120040254A1 (en) * | 2010-08-10 | 2012-02-16 | Steven Amendola | Bifunctional (rechargeable) air electrodes |
| CN102496704A (en) * | 2011-12-08 | 2012-06-13 | 中信国安盟固利电源技术有限公司 | Lithium titanate/titanium black anode material and preparation method thereof |
| CN103991904A (en) * | 2014-06-10 | 2014-08-20 | 中山大学 | Magneli phase titanium oxide nanowire array and preparation method thereof |
| CN106242585A (en) * | 2016-09-29 | 2016-12-21 | 四川大学 | A kind of sub-titanium oxide spherical powder and preparation method thereof |
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| US20120040254A1 (en) * | 2010-08-10 | 2012-02-16 | Steven Amendola | Bifunctional (rechargeable) air electrodes |
| CN102496704A (en) * | 2011-12-08 | 2012-06-13 | 中信国安盟固利电源技术有限公司 | Lithium titanate/titanium black anode material and preparation method thereof |
| CN103991904A (en) * | 2014-06-10 | 2014-08-20 | 中山大学 | Magneli phase titanium oxide nanowire array and preparation method thereof |
| CN106242585A (en) * | 2016-09-29 | 2016-12-21 | 四川大学 | A kind of sub-titanium oxide spherical powder and preparation method thereof |
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